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PRODUCTION OF ETHANOL USING MOLASSES AND ITS EFFLUENT TREATMENT

CONTENTS

1. Introduction

A Chronological profile of Mohan Meakin Introduction Organizational Structure

2. Fermentation

Introduction Raw Materials

Responsible micro-organisms for Alcoholic Fermentation Media for Fermentation

Process Description of Fermentation unit Lab tests conducted at Fermentation unit Properties of Ethyl Alcohol Treatment of by product CO2

3. Distillation

Introduction Process Reflux Ratios

4. Production of Liquor

Production of Liquor Bottling

5. Effluent Treatment Plant

Introduction Characteristics of Spent wash Problems created by Untreated wash Process Lab tests conducted at E.T.P

Uses of Treated wash

6. Brewery House

Introduction Medium Components Manufacturing Process of Beer

7. Water Treatment Plant

Water Treatment Plant

8. Products of Mohan Meakin Limited

Alcoholic products Non-Alcoholic products Exports of Mohan Meakin

9. Conclusion

Major Engineering Problems Quality Control Market Reach Conclusion

10. References

A CHRONOLOGICAL PROFILE OF MOHAN MEAKIN

The history of mohan meakin goes back as far as the Lucknow DISTILLERY which although officially established in 1855 was probably has its existence in 1820. The evidence is in the form of bricks dated 1820 were discovered during maintenance work some years ago.

In 1855, an Englishmen named EDWARD DRYER established a brewery at KASOULI and gave INDIANS first thrills of the modern beer. Riding on the wave of his successful venture, DRYER went on to start distilleries at SHIMLA, SOLAN (both in HIMACHAL PRADESH), LUCKNOW MANDALAVA, BURMA. During this time another Englishmen H.G.MEAKIN who bought the old SHIMLA and KASOULI breweries and constructed others at DALHOUSIE, RANIKHET, CHAKARATA, DARJEELING and KIRKEE.

Both these firms DRYER & Co. and MEAKIN & Co. continued separate business dealing till 1920s. During World War I, when importing beer was a hard task, after the First World War the two firms merged together and formed DRYER MEAKIN & COMPANY. In 1935, when BURMA was separated from INDIA, the company was recognized with its Indian assets and named DRYERS MEAKIN BREWERIES LIMITED. In 1947, when India got its independence the company went through a major change in its management. Padamshree late N.N.MOHAN the founding father of MOHAN MEAKIN HOUSE overtook its management. In 1967, DRYER MEAKIN BREWERIES LIMITED was named MOHAN MEAKIN BREWERIES LIMITED under the leadership of late N.N.MOHAN.

In 1969, due to passing away of Mr. N.N.MOHAN his eldest son COL. V.R.MOHAN took over as the managing director of the company. He introduced a number of new products that are grand leaders even today.

In 1973, after passing away of COL V.R.MOHAN, BRIG. KAPIL MOHAN became the managing director of the company. Under his guidance, the manufacturing activities of the company were diversified into other fields. Subsequently, in 1982, to remove the impression that the company is engaged only in beer making, the brewery word was dropped from its name.

Now, MOHAN MEAKIN LIMITED entered the international market and started exporting beverages to many countries such as U.S.A., U.K., JAPAN, and WEST EUROPEAN COUNTRIES & MIDDLE EAST. The company also began of man power & technical knowledge overseas especially where collaborations existed. A distillery and a glass factory were set up by MEAKIN PERSONAL at NAIROBI & KENYA a breweries set up in NEPAL & BHUTAN.

Apart of liquor, the other MEAKIN products which began for good profile were mineral water, cornflakes, mango nectar & apple juice. Among the companys diversification plans there are proposals to enter the cement, steel metal & allied products. It was there transformative inclination that leads the company to rename itself in 1982 as MOHAN MEAKIN LIMITED.

A saga that began over a century and half ago continues on its path of service to the nation with dedication, courage and unflinching commitment to quality. Over the years the company has embraced modernity and adapted to changing times. Yet its basic values remain the same integrity, craftsmanship, tradition.

INTRODUCTION

There are two types of distilleries: 1. Potable 2. Non potable

Potable: The distillery which produces first of all alcohol in the form of spirit etc. and then after maturation blending is done to make liquor. M/s MOHAN MEAKIN LIMITED, LUCKNOW is leading manufacture of beverage of the sort country liquor, foreign liquor, beer and denatured spirit. Hence this is a potable distillery.

Non Potable: In non potable ones distillery only alcohol is manufactured in the form of spirit etc.

Lucknow distillery is one of the manufacturing units of Mohan Meakin Limited. It was set up by the Dyer Meakin and Company in the historic city of NAWABS (Lucknow) on the perennial river Gomti. The distillery is housed in a building built about 480 years back by the Nawabs of Awadh which covers a carpet area of about 1 sq. km. approx. It is located at DALIGANJ, 10 k.m. far from LUCKNOW central railway station.

Molasses is used as a raw material here. This is processed through different channels (prefermentation, fermentation and distillation) for the formation of alcohol.

Rail and road are the two modes of transportation used here. The nearby located sugar factories supply molasses to it. It has two separated storage tanks. One located near the city station acquiring molasses through rail and other one is located in the factory storing molasses through road transportation.

Alcoholic beverages manufactured are of two types:

1. Undistilled beverages: beverages produced after fermentation and purification and no distillation is done after fermentation is called as undistilled beverages. These beverages have low alcohol content. E.g. beers, champanege, cider, port, sherry.

2. Distilled beverages: if the fermented liquid is distilled then they fall in this category. These beverages have high alcohol content as high as 50%. E.g. whisky, brandy,rum,gins.

The processing of molasses produces large quantity of liquid effluent called SPENT WASH. The treatment of spent wash takes place in the EFFLUENT TREATMENT PLANT.

The units of MOHAN MEAKIN LIMITED as follows:

SOLAN : Brewery, Distillery and Bottling.

KASAULI : Distillery.

LUCKNOW : BREWERY, Distillery and Bottling.

MOHAN NAGAR : Brewery, Distillery, Glass factory and Fruits production.

FERMENTATION

Introduction

The fermentation is derived from the Latin word fervrve, which means boiling. However, events of boiling came into existence from the fact that during the alcoholic fermentation the bubble of CO2 gas bursts at the surface of boiling liquid and give the watery appearance.

The action of specific micro-organism on a complex organic substrate and degrade it to produce the desired chemical compound is termed as Fermentation.

The majorities of processes require oxygen and classified as Aerobic. The other few processes carried out in the absence of air are classified as Anaerobic.

Fermentation process utilizes microbiology in producing chemical compounds. The process involves addition of a specific culture of microorganism to a sterilized liquid substrate or both in a well designed gas liquid contraction and carrying out the fermentation to grow micro-organism.

The general equation of fermentation is as follows:

Substrate + Micro-organism ==== More microbial cells + Metabolic products

Raw materials

The raw materials employed are among the most important materials of production process, to a large degree they determine the economics of the process, the production method and the quality of the product. Raw materials are naturally occurring substances utilized manufacturing industries. A fermentation substrate must be readily available throughout most of the year. Raw materials produced seasonally are not desired to have contamination and spoilage. Thus many industries need a substrate which is relatively stable and stored for 6 to 9 months without decomposition. Apart from bagasse, pulp and molasses most of the raw materials produced in sugar factory as are intermediated products of the sugar recovery process which are subsequently treated to crystal sugar. For cost reason, the use of non refined carbohydrates substrate often becomes mandatory in bulk fermentation. Thus less pure crystal sugar (after product sugar, raw sugar) or even sugar containing raw materials seems to be advisable.

Transport cost have to be taken care of, they become significant and prohibitive if too much is present and will prohibit the use of some waste materials at sites removed from their place production.

Some of raw materials are listed below:

1. Sugar crop:

1. Sugar cane: Although sugar cane is grown primarily for sucrose production, it is also used as raw material in alcoholic fermentation. The fermentable carbohydrates, from sugar cane may be directly utilized in the form of cane juice or in conjunction with a sugar factory from a black

strap molasses.

2. Sugar beets: as for sugar cane, beat molasses is generated in large volume from sucrose recovery operation. These raw materials contain sufficient nitrogen, other organic and inorganic nutrients such that, if any, fortification is required for fermentation.

2. Fruit crop:

Fruit with high fructose and sucrose content are grapes, peaches, apricots, peas, pineapples and apple.

3. Starches:

A variety o starches can be used for ethanol production by fermentation.

1. Corn: According to Miranowski(1981) corn is the most viable feed stock for the manufacture of ethanol in United States.

2. Cassava: Also called Manioc or Tapioca is cultivated in many tropical countries. Brazil, Indonesia and Zaire are the most important producers. It has starch content of 20-35 wt% and 1-2 wt% protein.

3. Sweet potato: Sweet potato powder (S.P.P.) generated by freeze drying, then grinding and screening the tubers. It has starch content of 64.4 wt %.

Keeping all facts in mind, black strap molasses are economically feasible and best result oriented in alcohol industries. So, widely used in INDIA.

Molasses: Molasses is generally used because it is rich in all salts except nitrogen which is normally employed in the actual growth of yeast cells.

It is defined as it is waste product of sugar industry of which further extraction of sugar is uneconomical.

Hence molasses is a solution of sugar, organic matter and inorganic matter in water. Even if all known components of molasses were added synthetically the result would not be molasses. Thus in accordance with the statement of three experts of sugar analysis nobody really knows what molasses exactly is?

We can say that molasses are the final effluent (final molasses) and byproducts of sugar manufacture. Due to their origin sugar cane and molasses are different. Black strap molasses are molasses produced from raw sugar factories from cane or beet. Often only term molasses is used for molasses from a beet factory where as black strap is preferably used for cane molasses.

Refinery (final) molasses (refinery black strap, barrel syrup), is derived mainly from cane refineries, where (high grade) white sugar is produced from raw sugar.

General composition of cane molasses: Molasses is an agricultural product and its composition varies with the variety of maturity of cane with the climate and soil condition. In addition processing condition in the sugar factory may also bring about changes in the composition of molasses. So, only average values of main components of cane black strap molasses given below.

Composition Sugars Sucrose Invert sugar Other Organic Glutamic acid and pyrollidine carboxylic acid Other N Organic acids Pectin etc. Inorganic

percentage 73.1 45.5 22.1 5.5 15.5

2.4 3.1 7.0 2.7 11.7

K2O Na2O CaO MgO

5.3

0.1 0.2 1.0

SO2+SO3

2.3

P2O5 Others

0.8 0.9

Physical characteristics of molasses: Molasses is a dark reddish colored jelly like viscous material. The pH of molasses varies from 6.8 to 8.5. The high osmotic pressure of molasses protects it from microbial spoilage, and it can be easily transported by barge and tankers etc. Molasses can be pumped easily. For production of ethanol in non sugar producing areas, and particularly in areas with suitable waterways for barge shipment, molasses may be the best suitable raw material for fermentation.

Classification of Molasses: Molasses are classified into following three grades: a) First grade Molasses: It contains more than 50%TRS. b) Second grade Molasses: It contains 40%to 50% TRS. c) Third grade Molasses: It contains less than 40% TRS.

Responsible Micro-organism for Alcoholic Fermentation

The choice of fermentation micro-organism for industrial alcohol production depends on the type of carbohydrate present in the medium.

Yeast is usually used in alcoholic fermentation. Many yeast strains present, which are responsible for alcoholic fermentation. Some of them are listed below.

Saccharomyces Cerevisae Saccharomyces Ellypriodes Saccharomyces Carlbergensis Saccharomyces Fragillis Saccharomyces Oviformis Saccharomyces Saki

Saccharomyces Cerevisae is the yeast strain now a day used widely in alcoholic fermentation because of having many of properties listed below:

1. High ethanol yield 2. Osmotolerance 3. High growth & fermentation rate 4. High temperature fermentation Low pH fermentation optimum

5. Ethanol and glucose tolerance 6. General hardness under physical and chemical stress.

High growth and fermentation rate allows the use of fermentation equipment. Ethanol and glucose tolerance allows the conversion of concentrated feeds to concentrated products reducing energy requirements for distillation and spillage handling.

Osmotolerance allows the handling relatively dirty raw material, such as black strap molasses with its high salt content.

Low pH fermentation combats contamination by completing organism.

High temperature tolerance simplifies fermenter cooling.

General hardiness allows yeast to survive both the ordinary stress of handling such as centrifugation as well as arising from a plant upset, the improvement process consists of modification to the medium & fermentation conditions used, So as to increase the yield of end products. Other common method is mutation brought about by exposure of organism to

Ultra-violet Radiation

X-rays Chemicals such as Nitrogen, Mustard etc.

Cultures are to be preserved so as to ensure their viability and reproducibility from batch to batch. They are lyophilized or kept on Agar improvement of microorganism for industrial purposes.

Some of micro-organisms used in alcoholic fermentation are as follows:

Bacteria

Zymomonas mobilis Clostridium actobutylicum Sarcina ventriculi Leuco-nsotoc mesenteroides

Fungi

Aspergillus orygae Endomyces lactis Nurospora crassa Rhizopus SP Mucor SP

In spite of these fungi and bacteria, yeast group is most widely used in fermentation process.

Media for Fermentation

The principal media for the commercial production of fermentation involves following:

Molasses: the main raw material is the wastes produced in the sugar mills. It is a dark brown color viscous syrupy liquid obtained as a byproduct in both by vacuum pass process and khandsari process of manufacturing. The bulk of the supply is obtained by vacuum pass process. The molasses contains reducing sugar up to 50%.

Urea (NH2CONH2): Urea is added to fulfill the requirement of nitrogen for good fermentation.

Sulphuric Acid: Sulphuric acid is added to bring down the pH value to an optimum level (4.2 - 4.8). pH plays a vital role in good fermentation.

Yeast: Certain types of yeast strains are desirable which are able to produce and tolerate high concentrations of ethyl alcohol. It should also possess uniform and stable characteristics. The most popular yeast strain used for this purpose is Saccharomyces Cerevisiae.

Di Amonium Phosphate(DAP): Phosphoric Acid: Antibiotic: To prevent the contamination (growth of other bacteria) an antibiotic Benzyl Penicillin is used.

Fermentation conditions

Temperature during fermentation

28-34 0C

Settling gravity of yeast vessels

1.045

Settling pH of yeast vessels

4.5 4.9

Settling gravity of prefermenters

1.05

Final gravity after complete fermentation

1.031.00

Duration of fermentation

24 hours

% alcohol after completion

5-8%

PROCESS

The process adapted in the manufacture of industrial alcohol is as follows:

Yeast Vessel: Yeast vessel is a metallic cylindrical vessel having capacity (1500 BL). It is mainly inoculums of S.cervisiae preparation tank. Inoculums preparation is a critical stage in an industrial fermentation process which usually differs in composition from production media. Inoculums media are compounded to quickly yield numbers of microbial cells in their proper physiological and morphological states, but without sacrificing genetic stability of the cells. The utilization of some component of the production medium i.e. molasses requires, the cells to be enzymatic ally adapted to this substrate, then this particular component should also be include in the inoculums medium. This precaution prevents deadaptation, if the cells already are adapted, or eliminates the leg period during the initial stage of production which may occur while adaptation is being accomplished. Here we are not interested in the accumulation of fermentation product other than cells in the inoculums medium and, hence, the inoculums medium is not balanced for product formation due to lack of carbon source.

Inoculum is prepared as a stepwise sequence employing increasing volumes of media. All steps, except that of initial inoculums from a stock culture, require the transfer of approximately 0.5 to 5% inoculums by volume from the preceding step in the sequence. At each step, the organism should grow quickly and in high numbers so that the period of incubation required is relatively short. Little, if any, fermentation product is accumulated during the inoculums stages, because the cells to be transferred their logarithmic growth phases and before accumulation of product would normally occur. In fact, inoculums media usually are balanced for rapid cell growth and lot for product formation.

Growth Curve of Yeast:

The growth curve of yeast occurs in the above manner following the four major phases:

1. Lag phase ( shown by AB) 2. Log or exponential phase (shown by CD) 3. Stationary phase (shown by EF) 4. Death or decline phase (shown by FG)

Also part BC and DE is considered as acceleration and deceleration phases respectively.

As mentioned earlier we are always interested to reduce part AB so substrate is added for adaptation of the cells.

In the yeast vessel, growth occurs exponentially and is shown by phase CD. The growth of the yeast can be expressed mathematically in the following manner:

dN KN dt

If initial population of cells is N0 and after time t it becomes N then

Nt

dN = Kdt
N0

N0

N LogeN = Kt N0

Loge N = Kt N0

N = ekt N0

N = N0 eKt

Prefermenter:

Here we are not concern with the alcohol production, we are concerned mainly with the growth of yeast culture and adaptation of cells in a large cylindrical metallic vessels having capacity 86230 BL. Thats why low dilution is maintained to avoid alcohol formation for 7 to 8 hours in anaerobic conditions. The specific gravity of the medium is 1.050 and optimum temperature for the growth of S.cerevisiae is 300C but somewhat higher temperatures (35 - 380C) are tolerated. Yeast growth is inhibited by solution of high osmotic pressure and high concentration of ethanol. Molasses contain variable amounts of nitrate which can be reduced to nitrate by bacterial action during the production of yeast. A considerable loss in yield has been reported for concentrations of 0.004 to 0.001% nitrite.

Many products have been reported to be activators or inhibitors of yeast growth. Flour milling waste, sludge from aerobic digesters etc. are considered as activators while SO2 inhibits yeast growth but concentrations up to 800 ppm molasses can be well tolerated. S.cerevisiae adapts well to the presence of even higher concentrations of SO2 as is known from the use of this species in the wine industry where fermentation is often carried out in the presence of 80 to 100 ppm of SO2.

Fermentation:

Fermentation applies to both the aerobic and anaerobic metabolic activities of micro-organisms in which specific chemical changes are brought about in an organic substrate due to the enzymes secreted by those microbes.

Fermentation is the core part of distillery which is carried out in large cylindrical vessel generally made of stainless steel having thickness 5-6 mm and capacity (46300 BL) is called as fermenter. The media which has been prepared is introduced in the prefermenter and after 7 8 hours it is transferred into fermenter where fermentation is carried out. Here batch fermentation is carried out without establishing pure culture conditions and without maintenance of complete sterility of equipment. However, this pre supposes a rapid start of the yeast fermentation. This fermentation inhibits the growth of other microbes by depleting the available nutrients, by lowering the pH and most importantly by the formation of ethanol. To reduce the pH H2SO4 is usually added.

Reactions in the fermentation:

As we know molasses contain approximately 50% invert sugar i.e. sucrose. It is converted into glucose and fructose in the presence of yeast and invertase enzyme.

S.cerevisiae C12H22O11 + H2O =============== C6H12O6 + C6H12O6 Invertase (enzyme) Glucose Fructose

Glucose is converted into ethyl alcohol and carbon dioxide in further reaction in the presence of yeast and zymase enzyme.

S.cerevisiae C6H12O6=============== 2C2H5OH + CO2 + Heat Zymase (enzyme) ethyl alcohol

As shown in the chemical reaction it is an exothermic reaction so cooling is required, cooling is done by external cooling, which releases cold water over the surface of fermenter to maintain the temperature of the fermentation which is set initially in between 21 to 270C usually, but as mentioned earlier heat evolution during the fermentation raises the temperature to 28 30 0C, with the temperature

being held in this range through the use of cooling coils. Although ethanol evaporation from the fermentation can become serious problem at temperature much over approximately 300C. The pH of the fermentation medium is maintained 4.5 6 by addition of sulphuric acid time to time. The fermentation lasts approximately 24 48 hours, with the actual time period being dependent on the substrate utilized and on the temperature of incubation.

Types of Fermentation operations:

Fermentation operation can be done in following three ways:

1) Continuous Fermentation process: It is an open type system. Here the formation of chemo state via steady state occurs.

If the medium is added continuously to a system at suitable rate the displacement of a culture may be balanced by the production of new bio-mass and thus a steady state may be achieved.

The growth of the cell in a continuous culture is controlled by the availability of the growth limiting chemical component in the medium and the medium is described as chemo state. 2) Semi-Continuous Fermentation process: The characteristic of this process is continuous feed liquid flow after addition of nutritive wort and of he seeding culture, such as S.cerevisiae. The treated medium flows by gravity or is pumped as a seeding culture from the first vessel into second, while fermentation is continued in the first. This is successive process continued till all the vessels are charged.

3) Batch Fermentation process: Today, most of ethanol produced by batch Fermentation process in the beverage industry developed more than 100 years ago.

In this type of fermentation process, substrate and microbes are added together to the start of the reaction. The reaction is carried out till the process of fermentation ceases or optimum yield of the product is obtained.

S + m =============== p + m (Substrate) (Microbe) (Product) (Microbe)

The general characteristics of batch system are well known. Usually the time required to completely utilize the substrate in 36 72 hours. The temperature is held at 23 300C and initial pH is adjusted to 4.5 depending upon the nature of the carbohydrate material. The conversion efficiency lies in the range of 90 95% of the theoretical value, a final ethanol concentration of 5-8% (w/v).

Batch technology has been preferred in the past and now days due to ease of operation, low requirements for complete sterilization insusceptibility to the contaminants, use of unskilled labor, low risk of financial loss and easy management of feed stocks. In an effort to increase fermentation productivity yet retain the simplicity of the batch process, cell recycle has been employed in many cases. This technique does not increase the alcohol conversion; however the time required for the fermentation to run its completion is reduced as much as 60 70% over traditional batch methods. The sugar supplemented with yeast nutrients is added to fermenter and the fermenter is inoculated with a rapidly growing culture of yeast from the seed

tank. A maximum in ethanol productivity is reached after 14 -20 hours. An ethanol production then continues at a decreasing rate unit about 95% of the sugar is utilized.

Usually several fermenter are operated at staggered intervals to provide a continuous feed to the distillation system.

Requirements for batch operation:

For the fermentation we require standing cylindrical fermenter designed to have larger height than the diameter of vessel, having following characteristics: 1. Made from stainless steel because corrosion problem and necessity for cleanliness and sterility. 2. Fitted with manholes at the bottom and top of the fermenter. 3. Inspection glass above the bottom manhole. 4. Thermometer and CO2 collection tube at the top. 5. Cooling coil for the hot temperature control during fermentation. 6. By pass valve in the air system allowing diversion of the air so that the foaming is not excessive and the Redox potential is not high during the early stage of fermentation. 7. Anti-foam is added when reached up to capacitive probe.

Merits of fermentation process over the chemical synthesis:

1. Cheaper raw material may be used. 2. Desired changes may be brought about in one step, which would be otherwise produced by a lengthy process. 3. Fermentation is only process for synthesizing some complex

compounds. 4. It works under less drastic conditions compared to chemical process. 5. Unwanted compound may be removed from the products.

Description of Fermentation Unit

Specific gravity of molasses in storage tanks is around 1.4. It is brought into fermentation section through pumps and it is diluted to specific gravity of around 1.05 as per the requirement. Molasses (specific gravity 1.4) is sterilized in preparatory tanks by air. Contamination of pure cultures used in fermenters is avoided by heat sterilization of air. This is accomplished by compressing it at high temperature and removing all the dust by passing through Potassium Permanganate.

Now water is added to the molasses to bring down its specific gravity up to 1.05 now yeast (S.cerevisiae) is added. To provide food for the yeast and proper functioning of the process Urea and Orthophosphoric acid is mixed. To maintain its pH 4.5 5 Sulphuric acid is added. It is kept in preparatory for 5 8 hours. Benzene Penicillin is added so that only yeast remains and other harmful bacteria are killed. Now it is sent to prefermenter molasses of specific gravity around 1.10 is mixed in it. It is kept here for around 7 8 hours. Then it is processed to fermentation vat. Anti-foam agent is added to prevent vigorous overflowing. It is then closed and kept for 24 hours. Carbon dioxide produced as by product is sent to cooling section and the fermented molasses is sent to distillation column as the feed. The fermented liquid is technically called wash.

Lab tests Conducted at Fermentation Unit

As the alcohol production is an extensive and time consuming process also it is concern with the life of human being and biological system, so testing of various types is necessary during the accomplishment or industrial alcohol production process. Also testing fulfills the economic consideration. Thats why the following experiments are carried out during the manufacturing of ethanol.

Estimation of brix in the molasses:

Estimation of brix in the molasses is necessary because it indicates that if brix is more, more are total solids inside the molasses or in other words more is sugar content in the molasses, but is not a condition. By weighing, 100 gm of molasses is taken in flask and is mixed with water. The mixture is shaken well. Now the volume of the prepared solution increase up to the 1000 ml to make it dilute. The specific gravity of the solution is now measured by balling hygrometer and the brix is measured by brixometer.

Analysis:

Reading of brixometer = 8.70 Temperature = 28C Correction factor = 0.06

Therefore brix = 8.70 + 0.06 = = = 8.76 total brix in the original molasses = (8.76 10) 87.6

Estimation of total reducing sugar (TRS) in the molasses:

The fermentable part of the total reducing sugar is converted into the glucose and fructose. The glucose then produces ethanol through enzyme zymase. So it is necessary to estimate total reducing sugar present in the molasses. 10 ml. of first molasses solution is taken in a 100 ml. measuring flask and 2 ml. of HCL is added. Then it is kept on water, both at 70-80C for approximately 15 minutes. After conversion it is cooled at room temperature then water is added to make solution up to 100 ml. now Na2CO3 is added to neutralize it and kept t 25C for 5 minutes. This solution is now ready to fill into the burette.

Now titrate is prepared. 5 ml. of each Fehling solution i.e. Fehling solution (A) and Fehling solution (B) are taken and then water is added up to 50 ml. . . . This solution is prepared in two 100 ml. measuring flasks, one for primary titration while another for final titration. This solution is now heated at heat plate and is titrated with neutral molasses solution. Methylene blue is used as an indicator. On completion it gives brick red color at certain burette reading. Now methylene blue again is added which turns solution into blue color. Again pour the neutral molasses solution, blue color is disappeared.

Analysis:

Molasses taken = 100 gm Dilution = 10 X 10 = 100


Fehling factor = 0.0535 Burette reading = 12.2

TRS = (gm of molasses) x (Dilution) x Fehling factor Burette Reading = 12.2 = 43.85 gm / l (100) x (100) x (0.0535)

Result: total reducing sugar present in the solution is 43.85 gm/l.

Estimation of alcohol percentage in the fermented wash:

The main raw material of distillery is molasses and when it is fermented, the main product is alcohol. Now estimation of alcohol becomes necessary for economic consideration in industry.

500 ml fermented wash and150 ml water is taken in a 1000 ml measuring flask. The top of the flask is fitted with inlet of condenser. This solution is now heated on the heat plate to create alcoholic vapors which are then cooled by condenser and stored in another flask fitted at the other end of condenser. This solution gives approximately 300 ml of alcohol. Again we increase the volume of wash by adding water and get approximately 300 ml of alcohol in another flask in the same manner. The volume of this alcohol is made up to the 500 ml, by adding water in it. Now both flasks a kept at temperature 27C in the refrigerator to reduce the temperature of the alcohol.

Now alcohol meter is introduce into the flask to get reading at temperature 27C. A reading for the proof of spirit (PS) at temperature 27C is achieved from the booklet for corresponding alcohol meter reading. The reading which we get from booklet is

subtracted from 100, gives the actual proof of spirit (PS). Then applying the following formula we get alcohol percentage in the fermented wash.

Alcohol % (v / v) = (PS 4) / 7

Analysis:

Temperature = 28C

= 301 k

Indication i.e. alcohol meter reading = 94.2

Booklet reading = 88.6

Proof of spirit = (100 - booklet reading)

= (100 88.6)

= 11.4

Alcohol % (v / v) = (11.4 4) / 7

= 6.52%

Result: the alcohol percentage in the fermented wash is 6.52% (v / v)

Properties of ethyl alcohol

Formula

C2H5OH

Molecular Weight

46

Boiling Point

78.30C

Melting Point

1120C

Density

0.791 @ 200C

Flash Point

210C

Ignition temperature

3720C

Explosive limit

Lower (3.5% by volume) Upper (19% by volume)

Toxicity

1000 P.P.M.

Grades

Anhydrous (95%)

Denatured

Treatment of by product CO2

Co2 obtained from fermentation tank contains the smell of molasses, moisture etc. and therefore treated through number of stages before storage.

FERMENTATION TANK--------H2SO4 -------- C OA L--------CYLINDER H20-------- SILICA

GAS HOLDER--------- COMPRESSOR--------- KMNO4--------- N a N O 3 - -- -- -- -- LIME STONE-------- WATER--------- COMPRESSOR--------- MASTER

DISTILLATION

INTRODUCTION

In the fermentation unit product received has 5-8% ethyl alcohol by volume. To get ethyl alcohol concentration as high as 95% by volume we send the product to the distillation unit.

Distillation is the method of separating two miscible volatile liquids by vaporization given that both the liquid exist in both the phases. Class of mass transfer devices consists of assemblies of individual units. These units are interconnected so that the material being processed pass through the assembly in stage they are brought into contact, mixed and then separated such stage system are called cascades.

In practice distillation may be carried out either of two principle methods. The first method is based on production of a vapor by boiling the liquid mixture to be separated and condensing the vapor without allowing any liquid to return to the still, and then there will be no reflux.

The second method is based on the return of part of the condensate to the still under such condition that this returning liquid is brought into intimate contact with the vapors on their way to the condenser either of these methods may be conducted as a continuous or batch process.

Ethanol is separated from the fermentation broth in continuous stills resembling those utilized for the recovery of 95% concentration is obtained by successive distillation in these stills. So the distilling process is divided into the distillation proper, which separates the volatile components of the fermented liquid from the insoluble solids and which concentrates the ethanol to a distillate containing 30-95% ethanol by volume. Ethanol has lower boiling point then water and the vapor phase in equilibrium with a vapor alcoholic solution has a higher concentration of ethanol. Suppose a solution containing 10% of ethanol by volume, is in equilibrium with a vapor containing about 50% of ethanol by volume. Therefore, the concentration of ethanol is greatly

enriched, in the distillate. Water and ethanol form an azeotrope. This is a mixture of volatile substance which at a given concentration has identical liquid and vapor compositions. For water and ethanol this concentration is 95% by volume of ethanol, and the boiling point of azeotrope is 78.2C. Therefore, ethanol can be concentrated by distillation to 95% by volume, but not to higher concentration.

By product of this section are aldehydes and spent wash. Aldehydes are removed in aldehyde section and spent wash is sent to E.T.P.

Process

The fermented wash which we get from fermentation vat having alcohol percentage approximately 7% is pumped to the overhead tank through the pumps fitted at the ground near the bottom of fermenter. This wash then comes into the beer heater what are actually condenser in which the temperature of the wash is rose up due to the vapor coming into the beer heater. This wash is then passed through a plate type heat exchanger where its temperature rises upto 70-100C due to the spent less passing in cross current manner in another plate having temperature 108 C. this wash is now ready to introduce in the analyzer column.

(a) Analyzer: analyzer is a long metallic column vessel having plate thickness 6 mm. there are 21 plates inside an analyzer and each segment provides inside vision facility through the glasses fitted onside the wall of it. The diameter of the analyzer is 1.60 meter; the fermented wash is introduced at top of the analyzer. To heating the wash and effective distillation steam is provided at the bottom of analyzer and the fractional distillation process takes place. The bottom and top temperature are 107 C and 100101C respectively. The temperature difference at the top and the bottom is due to alcohol present in excess quantity at the top and having lower boiling point. This process takes 30 minutes and gives spirit of 20% strength.

(b) Rectifier: it is another column for further distillation of the spirit. It is also a cylindrical column having 56 plates which do not provide inside facility. The pressure gauge and temperature measuring instruments are fitted onside the wall of the rectifier. The spirit which we get from analyzer is introduced here at 12th plate from bottom of the rectifier. Steam is provided at the bottom of the column. Due to high temperature or steam alcohol is vaporized, while water vapors come towards bottom. These vapors consist somewhat percentage of the alcohol also. So these are recycled into the analyzer for further processing. The bottom temperature of the rectifier is 100- 101C while top temperature is 80C. this column releases four types of spirit i.e. silent and neutral spirit, country made spirit, aldehyde and head product spirit, plane and rectified spirit. Aldehydes and head product spirit is removed here by another column fitted on top of the rectifier. The spirit which we get here is called rectified spirit and having strength of 95% and the strength of plain is 80% or more. Spent wash is obtained from bottom of the rectifier which is piped towards the effluent treatment plan.

(c) Purifier: This is the third main column of distillation plant. It is used to increase the concentration of rectified spirit and is having 25 plates in it. It is also a metallic column vessel whose temperature is 82-83C. The rectified spirit is provided at middle of the purifier and steam is introduced in it at above the spirit inlet. Purified spirit of strength 98% is obtained at the top of the purifier. While some part of the spirit is vaporized at the top, which is recycled into the purifier by colonizers fitted over the purification

column.

(d) Silent column or rectifier: it is the fourth main column used for further purification or rectification of the rectified spirit. Steam is provided here also at bottom of the column. The spirit in the vapor form which we get from the top of the purifier together with the spent of it is introduced to the silent column at somewhat above from bottom of it. Temperature of the column is 100-101C at bottom while 80C at top of it. The vapors of the alcohol are achieved at top of the silent column and are recycled into the column. Cooler is a plate type heat exchanger in which cold water passes as cross current or antiparallel with the rectified spirit. Ultimately the spirit is cool down and then stored into the storage receivers.

REFLUX RATIOS

Infinite Reflux Ratio or Total Reflux Ratio:

In this case, enough is charged to distillation assembly and column is operated under total reflux. During the operation of the column, vapory issuing from top are condensed and all condensed steam is fed back to the column as reflux. Also all liquid going to the recoiled is vaporized and is fed to the column. Thus under condition of total reflux D=0 and w=0, therefore v=Ln throughout the column. The slope (L/V) of both the operation lines becomes unity and hence both the operating lines coincides with diagonal and minimum number of stages are then required for desired degree of separation ( ).

Minimum Reflux Ratio:

At total reflux, operation lines coincide with the diagonals and to effect desired separation number of stages required is minimum. As the reflux ratio is reduced, operation lines moves towards equilibrium curve along feed line and the number of stages increases.

Ultimately, further reduction in reflux ratio results into condition where in top operation line touches the equilibrium curve. The point of intersection of operating lines lies on the equilibrium curve and at this point step become very close together, so that a zone of nearly constant composition is formed near the feed plate. Infinite number of plates are then required. This represents a condition of minimum reflux. Thus, a minimum reflux ratio is that ratio at which infinite number of plates is required for desired separation. At minimum reflux ratio, required heat supply for reboiler and coolant supply for condenser are minimum. For liquid at its bubble point, feed time is vertical (parallel o y-axis) and point C lies on equilibrium curve.

Optimum reflux ratio:

Any reflux ratio between infinite reflux ratio requiring minimum number of plates and minimum reflux ration requiring infinite number of plates is a work able system which requires finite stages for desired degree separation. As the reflux ratio is increased the number of plates decreases and the fixed cost decreases at first , passes through a minimum and then increases as with higher reflux ratio the diameter of the column and sizes of recoiled and condenser increases . The operation cost increases continuously as reflux ratio is increased, as it is directly proportional to R at total reflux. Though the number of plates is minimum, and also large capacity recoiled and condenser is needed. The total cost which is sum of fixed cost and operation cost also decreases to a minimum and then increases with reflux ratio. The optimum reflux ratio occurs at the point where the sum of the fixed cost and operating cost is minimum.

Production of Liquor

After the formation of spirit (ethyl alcohol 94%) it is kept in teak wood vats for maturation. Teak wood helps in removing impurities, provides some color, and some essence. Spirit is kept in maturation vats for different number of years. The higher the numbers of years better the quality of spirit. MOHAN MEAKIN in its teak vats have spirit ranging from current till more than 50 years ago spirit. From here the spirit is sent to following two departments:

1) Country Liquor (Single distilled spirit): Country liquor produced here are of two types:

a) Plain country liquor: It is produced by mixing alcohol (85 90%) strength with de-mineralized water in such a volume by volume basis that the final strength of alcohol is 25%.

b) Spice (Masala) country liquor: It is made by mixing alcohol with water such that alcohol is around 36% along with Malta essence and caramel which gives it the unique brownish color.

2) Foreign Liquor: under the foreign liquor following products are produced:

a) Whisky: Whisky is made from malt spirit (malt is technical name for dried and germinated barley), has 40 50% v /v alcohol. Whisky is of three types:

i) Pure: it is made from 100% malt alcohol.

ii) Blended: it is made by blending malt alcohol with molasses alcohol.

iii) Essence blended: it is made by molasses alcohol and malt essence.

b) Brandy: Brandy is made from grapes, leaches, cherries or apples and has alcohol 40 50% v/v.

c) Rum: Rum is produced from molasses spirit and has alcohol 40 50% v/v.

d) Gin: Gin is made from maize, barley, has alcohol 40 45 % v/v alcohol.

In India, owing to large population and economic viability brandies, Whiskies etc. are available in blended form. It is not possible to supply pure form to such a large population. Old monk rum produced at Mohan Meakin Limited, Lucknow is one of the most sold and sought after in the Indian market.

It is prepared by mixing the E.N.A. (Extra Neutral Alcohol) from spent column with the matured spirit of different periods in a certain ratio (older the spirit lesser it is added). The blended spirit is now mixed with demineralised water, essence, color (caramel) and tinctures.

Bottling: After addition of everything required it is sent to bottling unit which is fully automatic unit. Here mixture is filled in bottles then cap is put on it. All the air is sucked out then they are labeled and packed. So now it is ready to be delivered and sold.

ELLFLUENT TREATMENT

INTRODUCTION

The main raw material of Distillery is Molasses and when it is distilled after fermentation to get alcohol. The residual liquor remaining after the recovery of the alcohol is termed as Spent wash and discharged as waste. A sludge settling at the bottom of fermented is termed as yeast sludge is also discharged as waste.

If this waste is directly (untreated) discharged either in river Gomti or to a land will cause severe Pollution and environment will not be suitable for people to live.

Therefore MOHAN MEAKIN LIMITED LUCKNOW set up Effluent Treatment plant in March 1988. The treatment of effluent takes place in the following steps.

1. Anaerobic treatment i.e.: biogas generation. 2. Aerobic treatment i.e.: secondary treatment. 3. Classification unit with chemical treatment. 4. Extended (secondary treatment. stage) aeration unit with chemical

5. Sludge decanter (press leg dewatering machine). 6. Classification by two M.S. classifiers.

7. Ferti irrigation in the zeal of zero discharge 8. Fountain with atomization technique. 9. Flocculation unit with R.C.C classifiers for chemical treatment. 10) Recycling of treated trade effluent for cooling purpose.

Characteristics of Spent Wash

Spent wash has following characteristics:

1. The spent wash is a viscous liquid, reddish brown in color having a characteristic unpleasant smell. 2. It is acidic in nature having pH ranging from 3.5 4.5. 3. It has B.O.D (biological oxygen demand) ranging from 30,000 to 50,000 ppm. With the total solid content exceeding 10% by weight. These solids are mainly inorganic in nature which includes dead yeast and other organic debris in the suspension. 4. It contains a high percentage of organic and inorganic matter, which are added in two stages 1. Sugar cane industry for extraction of sugar 2. In fermentation process in Distillery. 5. It has C.O.D ( chemical - biological oxygen demand) ranging from 90,000 to 1,20,000 ppm. 6. This organic matter is readily decomposed by biological action.

General Composition of Spent wash

characteristic

value

Color

Dark brown

Odor

Characteristic

pH

3.5 4.5

C.O.D

80,00 0 1,20,000 ppm

B.O.D 3 days at 27.50C

30,00 0 45,000 ppm

Total solids

75,00 0 1,00,000 mg/ltr

Suspended solids

300 400 mg/ltr

Dissolved solids

74,500 1,00,000 mg/ltr

Total Nitrogen

1,000 1,500 mg/ltr

Free ammonia

25 30 mg/ltr

Chloride

3,000 5,000 mg/ltr

Sulphate

3,000 4,000 mg/ltr

Total acidity

15,000 18,000 mg/ltr

Mineral acidity

100 300 mg/ltr

Calcium

2,000 3,500 mg/ltr

Magnesium

2,000 3,000 mg/ltr

Problems Created by Untreated Spent wash

If spent wash is directly discharged as effluent without treatment then it can cause following problems:

1. problems created in natural water streams: 1. Lowering of pH value of the stream. 2. Increase in organic load.
3. Discoloration of the stream causing aesthetic problems and improved vision.

4. Bad smell. 5. Depletion of Oxygen content. 6. Heavy Fish mortality by interference in the respiratory metabolism.
Discharge of spent wash into fresh water stream cause precipitation of iron (F3+). Which affect respiratory activity in fish by choking their gills through fine deposition. Suspended solids present in the effluent affect the fish life adversely by causing mechanical injury to the fish and disturbed the osmotic regulation and result in suffocation event in the presence of adequate DO

2. Problems created by untreated spent wash on land: 1. Charring of vegetation crops. 2. Accumulation of salts. 3. Increase of salt content. 4. Increase in cropping period.

5. Increase in electrical conductivity of soil. 6. Increased bad smell.

3) Odor nuisance: It causes psychological stress to human. Offensive odour can cause poor appetite for good lowered water consumption. Impaired respiration, nausea, and vomiting & mental perturbation.

4) Color related problems and their disadvantages:

1. It is found that many colored bodies are colloidal in nature and they behave as absorbents. Thus they concentrate on many trace metal exert toxicity to the aquatic life. 2. The colored water is unsuitable for certain industries dairy production, papermaking, laundering, textile etc. 3. The receiving water polluted with color restricts the penetration of light subsequently retards the photosynthetic reaction. It also indirectly affects the reoxygenating capacity of receiving water. 4. The trees colors caused by organic compound create a chloride demand and hence it is the quantity of chloride required for disinfections of water.

PROCESS

Process of effluent treatment plant is as follows:

Plate heat exchanger (P.H.E): The fresh spent wash let out by distillery unit is quite warm (70 1000C), which is not fit for microbes or microbial treatment. Therefore to maintain temperature spent wash is passed through a plate heat exchanger, which is devised, on the principal greater the surface area, faster would be cooling. Here temperature is brought down to 400C and sent to next unit for further process.

Digester/ methane reactor (Anaerobic treatment): Once the spent wash cool down their next important factor, which can reduce the process, is pH of spent wash is extremely acidic. This acidic pH is harmful for bacteria in digester, which can reduce the activity of microorganism or kill them. To maintain the pH cooled spent wash is mixed with a portion of digester overflow in such a ratio that pH maintain 6.22 7.2.

Digester is also called methane reactor because, main product of anaerobic digestion is methane. Anaerobic digestion is partial conversion by microorganism of organic substrate into gases in the absence of air, the gases produce are collectively known as BIOGAS.

Mechanism of methane formation:

1. The primary reaction in which carbon dioxide formation takes place is as follows:

CO+H2OCO2+ H2

1. The secondary reaction takes place in presence of sufficient hydrogen. CO2+6HCH4+H2O

Important genra responsible for methane production is as follows:

1. Methanobacterium example: Autotropicum. Mb. Omelianskil. 2. Methanococcus example: Mc. Mezei Mc. vaniellii etc.

Mb.

Capacity of the digestion tank of M/S Mohan Meakin E.T.P is 4260 metric cubes. The expected drop in the level of BOD is 90% and COD is 70%.

Gas holder: Collection of methane, produce, as by product of anaerobic digestion is take place in gasholder. It is cost effective fuel and used in furnaces.

Biogas produced at digester is use in boiler for energy.

Aeration Tank:

(Anaerobic Treatment): The overflow of methane digester is sent to aeration tank having three surfaces. The growth of aerobic bacteria responsible for further degradation of BOD. Water used for bottle washing is directly sent to the aeration tank. This basin has been designed for 90% reduction in BOD.

RCC Clarifier/ Secondary Clarify: From aeration tank 1 effluent goes to final clarifies here sludge separated through SLUDGE DECANTER & sun dried is sludge drying beds. Apart of sludge as required, if reticulated to the aeration basin to maintain the desired number of bacteria in the aeration tank.

Aeration Tank: 2: The overflow effluent from the secondary clarifies further taken to second aeration unit for further reduction of BOD and COD.

M.S Clarifier: Here the overflow comes from aeration tank 2 and further separations of sludge take place.

Atomization Unit: Over flow of M.S clarifiers sent to atomization unit having fountain technique. In this technique each drop of water is broken down into several droplets thus enhancing their surface area allowing dissolution of more oxygen. This further reduced the BOD and COD.

Chemical Treatment Tank: effluent coming from atomization unit is treated in chemical treatment tank by the addition of suitable chemicals like alum &polyelectrolyte.

The main function of chemical treatment is to reduce or decrease the load of Nitrogen.

Final Clarifier: Finally effluent taken into final clarifier. Treatment is completed in final clarifier.

From final clarifier effluent is sent to cooling tower and is use for cooling purpose in distilling chamber and last effluent is finally discharged into river Gomti or some amount is used in PHE and atomization tank.

Lab tests conducted at E.T.P.

For the study purpose effluent of MOHAN MEAKIN LIMITED is taken at various steps and different tests are conducted daily in E.T.P lab and central lab daily. The tests that are conducted are as follows:

Test for pH:

Apparatus- pH meter, pH table of 4.7 & 9.2 pH

Procedure1. Prepare std. pH solution OF 4.7 & 9.2 pH using pH tables. 2. Standardize the pH meter is std. PH solution. 3. Determine the pH of the sample of water on waste water. 4. Standardize the pH meter every day.

Test for COD:

Apparatus- Reflux apparatus (flat bottom, COD flask of 500ml capacity & condenser).

Reagents1. Potassium dichromate solution (0.025N) Dissolve 12.56 gm. Dried K2Cr2O7 in/It. D/W. 2. Fe (NH4)2SO4 6H2O-98 gm/It. With 210 ml. Conc. H2SO4 3. Silver sulphaete - AgSO4 crystal, analytical grade. 4. Conc. : H2SO4 5. Ferro in indicator- Dissolve 1.48 gm. Phenethroline monohydrate +0.7 gm. FeSO4H2O in 100 ml. Distill water +Conc. H2SO4.

Procedure1. Use 0.4 gm. Ag SO4 in COD flask and add 25ml. Of K2Cr2O7 and volume of sample and make volume 50ml. of sample. 2. Add slowly 75ml. of conc. H2SO4 reagents & mix well its color turn green 3. Reflux for 2hr. wash down condenser with 50ml. D/W & cool it. 4. Titrate with 0.25 Fe (NH4) 2SO4 using ferroin indicator till wine red color appears. 5. Reflux blank in the same manner using D/W instead of sample.

Calculation-

COD mg/l = (a-b) *8000*N

V ml. Sample

Where, a) = ml [Fe (NH4)2SO4] consumed for blank b) = ml [Fe (NH4)2SO4] consumed for sample

Test for BOD:

Chemicals used-

1. PO4 Buffer a) Potassium dihydrogen Phosphate KH2PO4-0.85 gm. b) Dipotassium hydrogen Phosphate K2HPO4-2.175 gm. c) Disodium hydrogen Phosphate Na2HPO42H2O-0.22 gm. d) Ammonium Chloride (NH4Cl)-0.17 gm. Dissolute an altogether in 100ml 2. Starch indication 1% W/V 3. N/40 Sodiumthio Sulphaete. 4. Cacl2-2.7 gm/100ml of water. 5. Mgso4.7H2O-2.25gm.NaoH or 70 gm. 6. a) Sodium azide-a 50 gm. NaOH or 70gm. KOH + 13.54 gm. Nal or 15.0 gm. Kl

Dissolve in 70ml. of water. b) Sodium azide Na3N3 -1gm. In100ml. Mix a & b and make up volume 100ml. 7. FeCl3.6H2O-0.25 gm/It. 8. MnSO4.2H2O-3.64 gm/100ml. 9. Conc.H2SO4 Analytical

Method- One lit of D.M. water for blank determinant. On and one let each for individual sample. Aerate the water at least for 6 hr continuously by an aquarium.

For One sample- Take 2 It. aerated water and add appropriate quantity of seed about 2ml. /It. Add 2ml. each FeCl3, Cacl2, MgSO4 PO4 Buffer. To it mix thoroughly, separate out 1 ltr. Of it in that replacing the same quantity of sample by replacing the same quantity of water (volume should be 1 ltr.). In case of minor quantity sample it does not matter. Take 4 B.O.D. bottles properly in autoclave and sterilize. Fill each to with blank and sample being very cautious no air bubble should be trapped in it, keep each of bottle properly air sealed for incubation.

For initial titration: In remaining B.O.D bottle add 1 ml. each strictly in the sequence MnSO4, then Sodium azide Na2N3 shake vigorously allow to settle the ppt again shake ppt should be completely settle and the remaining liquid should be all clear without any suspension Add 1ml. Conc. H2SO4 in each dissolve the ppt properly. Shaken should be

done very carefully to avoid any personal damage.

Note- At the addition of Na azide it ppt appear in white color it clearly indicated that sample is overdose so discard it.

Titration- Take 100ml. the sample and titrate it against N/40 Na2S2O3 solution using indicator (starch).Titrate the same after incubation.

Calculation- Dilution factor- sample quantity in ml divided by 1000 ml. of water is dilution factor. Titration reading B0 before incubation

For blank incubated reading- B 3 After 3 days For sample S0 or S0

B=B0-b3 S0-S3=S

BOD mg/It. = (B-S) * Dilution factor * 2 As we are using N/40 Na2SO3 instead of N/20 we do it more accuracy in titration.

Test for Nitrogen:

Reagents-

a) Concentrate Sulphuric acid- 98%

b) Sodium hydroxide- 40% c) Boric acid- 2% W/V d) Hydrochloric acid or Sulphuric acid- N/10 e) Catalyst- Potassium sulphate, Copper sulphate(CuSO4.5H2O), Selinium Powder 100:6:1(gm)
f) Indicator- (a) Bromo cresol screen green indicator- 1% W/V in ethanol.

b) .1% methyl red in ethanol in the ratio 10:1 It shall give color pink in acid grey at end point and blue in alkaline. Procedure- Take appropriate quantity of sample in an 800ml. capacity Kjeldlhal flask add few drops of conc. Sulphuric acid. Gently evaporate to almost dryness, avoid charring. Cool and add 20ml. conc. Sulphuric acid +10gm. Catalyst and digested till the frotlling at low temperature further increase the temperature and digest till brown color disappear. Continue the heating strongly till slightly greenish color with clear appearance remains, cool and dilute it with 2.50ml.distill water transfer to a round bottom distillation flask add some glass pieces anti bombing agent and slowly add 70ml. NaOH solution so two distinct layer should form. Without disturbing the layer connects the condenser until the collection point dips below the surface of boric acid solution in beaker.

Swirl the content and apply full heat heater should be on before connecting the flask to minimize the danger of back suction. Immediately after the mixing of two layers remove the collecting beaker momently to let the exact tube and to equalize the pressure in distillation flask. Distill the ammonia in excess of 25 ml boric acid solution containing about 0.5 ml of screened indicator collect about 180 ml of distillate and titrate against standard acid to the grey end point.

Calculation- Total Soluble Nitrogen = x * 5.6 . Dry matter %

Test for total Alkali compound-T.A.C.:

T.A.C. refers to total alkali compound present in 1 lt. effluent in the form of Calcium Carbonate.

Procedure- First of all take 25 ml of sample in a beaker then pH electrode was set. For shaking the sample magnetic stirrer was applied, temperature was maintained at 35 0C and N/5 sulphuric acid was added till pH becomes 4 with constant stirring; final reading was noted; which will give the amount of sulphuric acid consumed.

Calculation- T.A.C = volume of H2SO4 (N/5) used * 400 (mg/l)

Test for total Volatile acid- TVA:

It refers to total volatile acid present as acetic acid in 1 lt. of effluent.

Procedure- 25 ml. of the sample is taken in a beaker, pH electrode was set up for constant monitoring of pH and magnetic stirrer was applied for proper mixing. N/5 sulphuric acid was added till the pH becomes 4. Reading (a) is noted and sample was heated for 3 minutes on hot plate. Further pH was increased to 7 with the help of N/5 NaOH. The final reading was noted as (b).

Calculation- TVA= volume of NaOH used * (b-a) * 480 mg/l

Test for Total Solids-TS:

Procedure- A clean and dry silica crucible was taken and after repeated heating at 105 0C, samples is then cooled in desiccators and weighed. 100 ml of the sample is taken in it and dried and evaporated in water bath followed by oven. Crucible is weighed along sample.

Calculation- Total solids = W * 106 mg/l V

W= weight in grams of residue obtained V= volume of sample in ml.

Test for total Dissolved Solids- T.D.S:

Procedure- Known amount of filtered sample is taken in silica crucible; dry it with the help of water bath followed by oven. Material remained in the crucible is weighed.

Calculation- T.D.C = W

Test for total Suspended Solids- T.S.S. :

Calculation- T.S.S = T.D.S T.S.

Uses of Treated wash

Distillery effluent if treated properly or diluted to reduce the toxic level of pollutants to tolerance limits before discharge may act synergistically to promote growth and developments of plants and animals.

Distillery effluent (diluted) is being gainfully used in many countries. Besides reducing environmental hazards, they provide substantial ecological and recreational benefits are as follows:

1) Anaerobic sludge, produced in the aerobic treatment is finally recovered from the sludge decanter machine where water is removed from the sludge by centripetal course and concentrated sludge is obtained which has following nutrients:

a) Nitrogen (N) 19% b) Phosphate (P) 14% c) Potassium (K) 21% d) Organic matter 5.86%

Due to rich organic matter content and other inorganic constituents sludge is used, as manure of good quality and it has shown good result in the fields.

2) Biogas/Marsh gas produced in a methane reactor has a high calorific value and is utilized in the place of coal in boiler. It replaced coal burnt in the boiler leading to reduce air pollution.

3) Along saving environment from being polluted, it also saves money.

4) High temperature of spent wash is used to increase the temperature of water so that preheated water is easily converted into steam in boiler leading to energy saving.

5) Treated spent wash is mixed with waste water from the units of the distillery in the cooling tower and is utilized for condensing the alcohol vapors.

6) Treated water is successfully utilized in the E.T.P. for irrigation purpose. Plants like Peepal, Ashok and Neem are grown here utilizing the treated water.

7) Spent wash may also be use for production of yeast or fungal biomass. Some distilleries in India are practicing recovery of dried yeast powder of pharmaceutical quality from spent wash yeast sludge mixture.

BREWERY HOUSE

Introduction

MOHAN MEAKIN LIMITED also has a brewery unit known as Mohan Goldwater Breweries situated in the same premises, manufacturing BEER.

Brewing, the production of malt beverages is one of the oldest fermentations, dating back thousands of years and probably originating in Nile Valley.

Brewing is a complex fermentation process, because multitude of products must be considered, because several of these products do not result from microbial activity and because the exact nature of certain of the latter products still not known. The fermentative products of yeast, however, are known, and these include ethanol, carbon dioxide, glycerol, acetic acid and higher alcohols and acids,

Brewing also differs from most other industrial fermentations, because flavor, aroma, clarity, color, foam production, foam stability, percentage of alcohol, and satiety all are associated with the finished product. Thus, since people differ in their likes as to the relative balance of these factors in the finished product, the resulting variations in the brewing process, all are commercially profitable. Typically beer contains 4-8% alcohol. LAGER BEER the type most commonly produced, refers to a fermented beer that has been allowed to age in the cold. For this beer, bottom fermenting yeasts are utilized in.

Medium Components

The compounding of the medium for brewing of beer presents special problems, since the medium must supply not only the carbon and nitrogen substrates, vitamins, growth factors, and so forth for the yeast but, in addition, must contribute to the aroma, flavor, foam characteristics, color, clarity, stability, and so forth of the finished product. This picture is further complicated by the fact that yeast is not able to directly utilize certain of the nutrients of the medium. For instance, starch is the primary carbon source of the medium, but its carbon become available to the yeast only after it has been totally degraded to maltose and glucose through the action of malt amylase. However, the latter enzymic reaction, in addition to the maltose and glucose, also yields dextrins, which are partial degradation products of the starch. These dextrins are not available to the yeast, but they are important, nevertheless, because of their association with the flavor of the product. These dextrins are not available to the yeast, but they are important, nevertheless, because of their association with the flavor of the product. The nitrogen source of the medium can also be classed in the yeast nonavilability category, since it is supplied mainly as protein, and the yeast does not possess proteolytic activity. Thus, the protein, through malt proteolytic activity, first must be degraded totally to amino acids and short chained peptides for utilization by the yeast but, as with the carbon source of the medium, a portion of the protein must remain only partially degraded to peptones and larger peptides so as to contribute flavor, foam characteristics, and so forth to the final product. Thus, these partial and total degradations of both the carbon and nitrogen substrates of the medium are accomplished by employing the amylase and protease enzymes, respectively, of malt as prepared from barley. However, the malt, in addition to these enzymes, also provides the protein nitrogen compounds and, in most instances, part to all of the starch of the medium, although some of the starch may be supplied as malt adjuncts, Hops also are added to the medium to provide various of the characteristics of the finished product, although the extractives from the hops, for the most part, are in themselves substrates for yeat activity.

Malt: Malt is prepared from carefully selected barley. This barley is first cleaned and then steeped in water for periods of up to two days.

The malt contributes amylases, proteases, starch, protein, additional yeast nutrients and growth factors, and flavor characteristics, to this medium.

Malt adjuncts: Barley contains considerable protein. If these barleys are employed

in the medium as the only source of carbon and nitrogen, the resulting beer is dark colored, some what unstable, and too filling for the average taste. This situation is corrected by diluting the malt protein with additional starch added as starch containing malt adjuncts. This additional starch does not present a problem, as might be expected, because the malt produced from barley contains enough amylase activity for hydrolysis of this extra starch.
Hops: Hops are the dried female flowers of the hop plant. The hops provide the beer

with its aromatic and pungent character, as well as having stabilizing effect.

Water: Large amounts of water are employed in the production of beer. Only a small amount of this water ends up in the finished product; the rest is utilized in various fermentation and processing steps. The composition of the water is of extreme importance as regards its effects on flavor and other properties of the finished product.

The characteristics of good water for brewing are a pH of 6.5 7, less than 100 ppm calcium and magnesium carbonates.

Manufacturing Process of Beer

Preparation of medium: The fermentation medium, or wort, is prepared in four successive operations 1. Adjuncts are cooked to gelatinize their starch. 2. They are added to water along with malt in as approximate ratio 2/3 malt to 1/3 adjuncts. 3. The mixture is subjected to mashing, a procedure by which the various enzymes of the malt are allowed to act over a range of temperature.
4. On completion of mashing, the wort is separated from the undissolved husks and insoluble protein malt and then boiled with hops at 1/4 lb per barrel of wort.

Microorganism: Brewing utilizes strains of saccharomyces cerevisiase, both bottom and top yeast strains .Yeast strains are specially selected for their fermenting ability and for their ability to flocculate at the proper time near the end of the fermentation.

Fermentation: The aerated wort is cooled approximately 10 to 11 0c and then placed in a closed fermentation tank containing cooling coils. Although an open tank can be used, the closed tank is preferred so that evolved CO2 can be collected for later carbonation of the product. After addition of yeast within 24 hours after pitching, foam begins to appear on the surface of the medium, first along the wall of the tank and then gradually across the surface. The CO2 evolution then increases so that the yeast cells become suspended in the medium.

From seven to nine days, the last phase of the fermentation the yeasts became inactive and flocculate.

Cold storage Maturation: The completed fermentation is transferred to storage tanks and held at approximately 00C for a period of time. During this Cold storage maturation coagulated nitrogenous substances, resins, insoluble phosphates,

and yeast cell sediment from the beer. In addition, esters are formed, and the beer matures so that if loses its harshness.

During this maturation process,Chill proofing is commonly practiced to help prevent turbidity development on later exposure of the finished beer to cold.

Antioxidants also usually are added during cold storage maturation to prevent oxidative changes in the beer which affect flavor SO2 and ascorbic acid are commonly used to accomplish this end.

Carbonation: Carbonation of the beer is accomplished by injection of cleaned CO2 recovered from evolved fermentation gas. This method provides a final dissolved CO2 content of approximately 0.5 % in the beer. This CO2 displaces dissolved oxygen, which is detrimental to the stability of the beer, and helps in the production and retention of foam in the preservation of beer.

Packaging: After cold storage maturation, the beer again is passed through cooling pipes and through a diatomaceous earth filter before being packed in bottles. Air is rigorously excluded during this packaging to prevent oxidative changes in the product. Beer packaged in bottles is not pasteurized and hence, has a relatively short storage life therefore pasteurization is done.

By products: The spent grains along with spent wash are sent to E.T.P.

WATER TREATMENT PLANT

MOHAN MEAKIN LIMITED is one of the leading manufacturers of alcoholic beverages. MOHAN MEAKIN sets up high standards and as the distillery needs different types of water for different purposes. MOHAN MEAKIN has set up a WATER TREATMENT PLANT in the same premises.

Tap water or source of water can not provide water as required for different units. Some of the requirements of different units are as follows:

1. Boiler requires water without having hardness to avoid scaling problems. 2. Foreign and country liquor requires demineralised water.
3. Brew house requires water having pH around 6 and hardness around 4-5 ppm.

As the water required for different purposes is different water treatment plant produces water of different qualities and supply it to different units.

Water treatment plant requires to remove or adjust hardness, free mineral acid, pH, Cl2, SO4, alkalinity etc. to required values. Water treatment plant uses ion exchange mechanism.

Ion exchange mechanism: Ion exchange operations are essentially metathetical chemical reactions between an electrolyte in solution and an insoluble electrolyte with which the solution is contacted. The mechanisms of these reactions and the techniques used to bring them about resemble those of adsorption so closely that

for most engineering purposes ion exchange can simply be considered as a special case of adsorption application.

Principle of ion exchange: the ion exchange solids first used were porous, natural or synthetic minerals containing silica, the zeolites, such as the mineral Na2O. Al2O3.4SiO2. 2H2O, for example. Positively charged ions (cations) of a solution which are capable of diffusing through the pores will exchange with the Na+ ions of such a mineral, which is therefore called a calcium exchangers. For example,

Ca2+ + Na2R========= CaR + Na+

Where R represents the residual material of a zeolite. In this manner hard water containing Ca2+ can be softened by contact with zeolite, the less objectionable Na+ replacing the Ca2+ in solution and the latter becoming immobilized in the solid. The reaction is reversible, and after saturation with Ca2+ the zeolite can be regenerated by contact with a solution of salt,

CaR + 2 NaCl ============ Na2R + CaCl2

Later certain carbonaceous cation exchangers were manufactured by treating substances such as coal with reagents such as fuming sulphuric acid, and the like. The resulting exchangers can be regenerated to hydrogen from, HR, by treatment with acid rather than salt. Thus hard water containing Ca(HCO3)2 would contain H2CO3 after removal of the Ca2+ by exchange, and since the carbonic acid is readily removed by degasification procedures, the total solids, content of the water can be reduced in this manner. This method is limited to water softening only.

In addition to water softening applications mentioned above, the complete deionization of water can be accomplished by percolation first through a cation exchanger and then through anion exchanger. After passing through cation exchanger it is passed through degasification. Water from anion exchanger and degasification is passed through mixed bed. This is done in Fixed bed exchangers.

Products of Mohan Meakin Limited

Alcoholic Products:

1) Whiskies:

Solan No.1 whisky Solan Imperial whisky Solan No.1 premium whisky Mike and Butler malt whisky Col. Spl. Premium whisky Chck-neck deluxe malt whisky Saaqi malt whisky Coller 117 matured whisky M.B fine whisky Meakins whisky Blue Bell whisky Black Beaury fine malted whisky Grand master malt blended whisky

India king deluxe whisky King castle special rescue whisky Red dog fine whisky Diplomate deluxe whisky Knight rider whisky John white whisky Old master whisky Cary house malted whisky

2) Brandies:

Triple Crown pure grape whisky Doctors reserve no.1 brandy D.M brandy M.M.B brandy Golden eagle doctors brandy

3) Rum:

Old monk supreme rum Old monk white rum

Old monk gold reserve rum Old monk xxx rum


Gorkha rum Tusker xxx rum Black beauty rum

M.M.B. xxx rum

4) Vodka:

Kaplansky vodka

5) Beers:

Golden eagle lager beer Golden eagle deluxe lager beer Golden lager beer (herbal beer) Asla - 72 lager beer

black night super strong beer Solan no.1 special larger beer Gymkhana pilsner beer
Lion larger beer Meakins larger beer Crown light pilsner beer

Solan no.1 extra strong beer Grand master black lable beer Black knight deluxe beer

7) Gins:

Big ben Landon dry gin Meakin dry gin M.M.B. gin

8) Cider:

Mohan apple cider Beside liquor division, Mohan Meakin Ltd. has also expanded its activity in the area of food products like: a) Break fast food b) Vinegar c) Juices d) Sauces

e) Jam & Jallies f) Canned products g) Mineral water

The production of food products is seasonal and production is stopped in different seasons for different products,depending upon the seasonal demand

None alcoholic products:

Juices:

Mohans gold wine apple juice Mohans mango tonic Mohans pine apple juice Mohans pine apple juice necter Mohans marri nector Mohans sfruit punch Mohans guava juice

James & jellies

Mohans mango jam Mohans apple jam Mohans mixed fruit jam Mohans smelon ginger jam Mohans pine apple jam

Canned products:

Mohans mango pulp Mohans chutney Mohans green peas

Sauces:

Mohans tomato ketch up

Vinegar:

Mohans pure malt vinegar Mohans synthetic vinegar

Mineral water:

Golden eagle mineral water Mohans mineral water Golden eagle natural mineral water Golden eagle auqa mineral water

Breakfast foods:

Mohans new life corn flakes Mohans new life wheat flakes

Extracts:

Brewers years Malt extract Compressed pakers yeast

Exports of Mohan Meakin Limited

Mango pulp Mango juice Mango slices Guava juice Pine apple juice Corn flakes Beers

Rums Whiskies Brandies Gins

MAJOR ENGINEERING PROBLEMS

1. Batch vs. Continuous Process

Continuous molasses dilution in the head end of the process and continuous distillation are incorporated to save space, equipment and operation cost. But for fermentation batch process is usually preferred for long residence time process and because of the hazards of contamination and mutation of the specific microorganism.

2. Waste disposal problem

According to pollution board norms the B.O.D level should be around 30. The Spent wash processed by distillation column have B.O.D. around 35000. This spent wash contains organic matter in the effluent is therefore, required to be removed. So that it can be discharged safely into the environment.

3. Fuel economy

To save energy cost, preheat exchangers are employed in Distillation as well as in E.T.P. Section. During the processing of spent wash in E.T.P. section, methane gas produced in gas boiler which is used as a fuel.

4. Collection & storage of molasses

Due to high viscosity of molasses, its transportation and storage is problematic

5. Other problem

Maintenance of sterile and specific yeast culture condition for the proper functioning of culture conditions, for the proper functioning of yeast temperature should be maintained around 25 0C. Contamination of pure cultures used in fermenter avoided by heat sterilization of air which removes all dust and oil by passage through fibrous filters.

MARKET REACH

After the final product is produced the next important process is the marketing reach of the product. Some exclusively deal in the marketing of these beverages and make these footrests in the near reach of the consumers. Some of these companies are like Kedia, McDowells and so on. These companies are licensed from the government to purchase this coverage in the wholesale rate from the manufacturing units and all these products under these known names and with the help of their distribution channel. And all the rights are exclusively with these firms that how they should do the marketing and do the distribution of these products and manufacturing units have nothing to do with it.

CONCLUSION

MOHAN MEAKIN LIMITED situated in Lucknow is a potable distillery producing alcoholic beverages of both types i.e. distilled and undistilled has been an example for others to follow.

MOHAN MEAKIN has adapted the modernity still keeping the same old taste & quality. Its OLD MONK one of the oldest RUM is still numero uno of its type.

MOHAN MEAKIN LIMITED works in such a way that they try to maximize output with minimum input. Company has worked on different aspects of energy saving so that this not only helped them to bring down the cost of manufacture but also helped in saving non renewable energy sources from being depleted. Company also utilizes its by products in different sectors as useful product.

In 1988 company set up the Effluent treatment plant so that the company can meet the new standards of Environmental pollution control. This helped the company to still remain in the heart of city when all the industries are being thrown into outskirts of the city. Company discharges their waste into Gomti River with all the standards being fulfilled. New USB reactor set here is an example of modernity.

Company has well equipped labs in different units and there is also central lab. Company has a well qualified staff which works for the company with dedication, courage and unflinching commitment. Company also takes care of the welfare and interests of the staff. All the units of the company though working separately have proper coordination within them. A great thing about the company is that all the

units and their staff live like a family striving hard for success.

A saga that began over a century and half ago continues on its path of service to the nation with dedication, courage and unflinching commitment to quality. Over the years the company has embraced modernity and adapted to changing times. Yet its basic values remain the same integrity, craftsmanship, tradition.

REFERENCES

Outlines of Chemical Technology: Dryden

Mass Transfer Operations: Trebyal

Journals of Mohan Meakin

Unit Operation of Chemical Engineering: McCabe Smith