Semi-Boiled Soap Production Systems

Boris Radic and Luis Spitz

Souptecsrl, Iruly; IL. Spitz, Inc., Highlund Pork, Illinois, USA

Introduction
Semi-boiled saponification is a glycerine removal free process which produces neat soap with all the glycerine that is contained in the starting fats and oils. Semi-boiled saponification does not require the washing and fitting steps of the traditional fullboiled kettle-soap process or the washing and neutralization of the continuous saponification systems which produce neat soap with only a small quantity of glycerine. The traditional market for Semi-boiled soaps was mainly for different laundry soaps. Currently, Semi-boiled soap manufacturing is also gaining importance for toilet soaps due to: the fluctuating cost of refined glycerine the increasing cost of many raw materials, especially those for spent-lye treatment the availability of complete glycerine processing plants Semi-boiled soap making is a simple, single-step operation which offers these advantages: savings in energy consumption reduced capital investment compared to other systems lower environmental impact (no by-products) requirement of less-skilled personnel due to process simplicity less and simpler quality-control requirements. The high-glycerine content of Semi-boiled soap alters the soaps appearance, and results in a harder finished product at given moisture content due to the increased viscosity of the liquid phase of the soap. To account for this, Semi-boiled soaps are usually produced with 5 8 4 0 % of Total Fatty Matter (TFM) content, in contrast to the full-boiled or continuously made neat soap with 6 2 4 3 % of TFM content. For comparison between the two types ofsoaps, the term virtual TFM is introduced to predict the behavior of the Semi-boiled soap in full-boiled terms (more details in the Definitions and Calculations section of this chapter). In the full-boiled process, some or most of the glycerine and impurities are removed from the neat soap by washing andlor fitting. These procedures include the addition of water and electrolytes, some kind of mixing to assure contact between newly added material and preformed soap, and then settling to separate the neat soap from the waste (in the case of washing, spent lye; and in the case of fitting, seat soap and lye). For more details, refer to Chapters 7 and 8 in this book.

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The purpose of washing is twofold: (i) to recover the glycerine liberated by the saponification reaction and (ii) to remove the lye-soluble impurities. Washing in the kettle process is time-consuming and less efficient than in the continuous systems with the commonly used countercurrent, highefficiency, multistage washing columns [rotating disc contactor (RDC)]. phase diagram shows that The washing is conducted inside the neat soaplye region.

Electrolyte as Sodium Chloride, %

Fig. 9.1. Washing.

The purposes for fitting the last processing step in the kettle process are to: remove soap-soluble color bodies remove the minor impurities lower the electrolyte content raise the fatty-acid content. When producing semiboiled soap, the process cannot be manipulated by physical means, only by chemical means; therefore, important points to bear in mind are: Semi-boiled soap is produced directly inside the neat soap region: no separation or washing of any kind.

All of the ingredients present at the beginning of the process remain inside the finished product.
The quality of the finished soap directly depends on the quality of the raw materials used.

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mb

Electrolyte as Sodium Chloride, %

Fig. 9.2. Fitting.

Electrolyte as Sodium Chloride, %

Fig. 9.3. Semi-boiled Neat Soap Phase Region

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Crutcher-MixedReactor
Semi-boiled soap production requires a fair amount of mechanical mixing. Open-steam mixing, typical in kettle saponification, would lower the percentage ofTFM and introduce the risk of the formation of middle or seat soap. Acrutcher, a very efficient mixedreactor, was and still is the first choice for Semi-boiled saponification systems. It also serves very well for mixing minor additives and fillers into all types of soap. The crutcher is a jacketed vessel with a screw-type agitator in a draft tube. The rotating screw induces a vigorous flow of the materials across the vessel, resulting in very good mixing. The crutchers versatility is limited by its inability to handle high viscosities: for this reason it is used mostly for atmospheric-pressure applications.

Fig. 9.4. Crutcher.

At m0spheric Systems
Batch Process
All the fats and oils are fed into the crutcher (Fig. 9.4.).Then caustic soda is fed gradually through a
distributor ring (on top of the fats and oils) under constant agitation. A rule of thumb is that about three hours are needed for the preparation of a batch of Semi-boiled soap. This time includes the filling of all materials, the reaction time, and the discharge of the product. A detailed sample for the preparation of one batch follows: Feed the fats and oils into the crutcher, and heat to 70C by heating the water in the crutchers jacket to 85C: 30-45 minutes. When this temperature is reached, two-thirds of the caustic soda is added slowly at room temperature and at a predetermined strength.

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Keep the batch under constant agitation because the mixture will begin to thicken, and then add the rest of the caustic soda until the saponification reaction is completed in 90 to 120 minutes. Analyze for free alkalinity to determine if more caustic soda or fatdoils are needed. Adjust if required: 10 to 20 minutes. Discharge the finished Semi-boiled neat soap to storage: 20 to 30 minutes. Total time is from 150-215 minutes.

Semi-continuous Process
The most commonly used Semi-boiled soap-production system consists of two crutchers. This plant consists of two batch systems (two crutchers) working in tandem to allow for the continuous operation of a downstream drying system. While in one crutcher a batch is saponified, the other crutcher is discharging an already finished batch of Semi-boiled soap.

Fig. 9.5. Atmospheric Semi-continuous System.

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High Shear Mixer

Fig. 9.6. Atmospheric Continuous System.

Continuous Process
The addition of a high-shear mixer (turbodisperser) and a recycle pump to the crutcher converts a batch system into a fully continuous process. The high-shear mixer assures very good contact between all the reagents. Further vigorous mixing by the crutcher (combined with the enhanced action of the recycle pump) speeds up and completes the reaction. Also,since a reasonably small quantity of fresh reagent is injected in a stream of already formed soap, no separation occurs so that fadoils and caustic remain in contact for the time necessary. A nominal production rate is discharged continuously by the incoming fresh raw materials through a siphon pipe. In many cases, especially when no intermediate storage occurs before drying, the first crutcher is followed by another one, called the maturator, which serves to assure the completion of the reaction by allowing a longer residence time. The maturator is also handy for the addition of various minor ingredients that are used in many soap formulations.

Pressurized Systems
Stirred Vessel Reactor (Autoclave)
Stirred-vessel reactors, also called autoclaves, were developed for continuous saponification systems of full-boiled neat soaps, and only recently have been used for the Semi-boiled saponification of toilet soaps. Figure 9.7 shows a typical stirred-vessel reactor inside a continuous saponification plant (full-boiled type) *

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Fig. 9.7. Stirred Vessel Reactor (Autoclave) Pressurized System.

Vertical- or horizontal-type stirred-vessel reactors come with internal baffles, tubes, or mixing blades. 'These reactors are used in combination with a centrifugal recycle pump. All previously described effects take place here as well. The good mixing action of the recycle pump and the preformed soap acting as an emulsifier will, given enough residence time, result in a complete reaction between the reagents. Important to notice is that the newly formed soap is not simply displaced by incoming raw materials, but has to go through a pressure-control valve. This allows a degree of control over pressure and temperature inside the reactor which, in turn, allows one to control the speed of the reaction and the viscosity of the finished neat soap. 'These reactors are used for the production of neat soaps of regular viscosity: their design and the use of a centrifugal pump for recirculation are not well-suited for handling concentrated materials.

High Shear Mixer/Reactor

The high-shear mixedreactor has an internal multiblade mixer shah with large contact surfaces which assure quick and complete saponificationlneutralization (Fig. 9.8). It can be offered with or without a recycle loop. The system with a recycle loop is more efficient, more flexible, and can process materials of higher viscosity. These units can handle both regular and semiconcentrated neat soaps. This type of reactor utilizes the thixotropic characteristic of soap to its advantage by a constant, intense mixing action, allowing one to obtain high TFM content neat soap that would otherwise be too viscous to produce.

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Fig. 9.8. High Shear Mixer-reactor Pressurized System.

SemiconcentratedSaponification Systems
Various pressurized systems exist that are designed to produce semiconcentrated soaps up to 70-72% of TFM content by using concentrated caustic soda. The efficiency of the reaction is greatly enhanced by a higher concentration of reagents, allowing for shorter residence times and/or resulting in very complete saponification. Furthermore, this extra efficiency of reaction, when combined with longer residence times, allows for the successful processing of a wide variety of raw materials; hence, increased flexibility of operation results. This implies that commercially available plants are a trade-off between the compactness of the installation (easier cleaning, smaller investment, smaller footprint but a more narrow range of processible raw materials) and residence time (a wider range of processible raw materials but more equipment o r a bigger installation, a bigger investment). Figures 9.9 and 9.10 show two typical commercially offered plants: the compact Mazzoni LB SSCT plant with a tubular reactor (Fig. 9.9) and Binacchis CHBS plant (Fig. 9.10) utilizing two high-capacity (high residence time) reactors capable of processing a very wide variety of raw materials.

Combination (Integrated) SaponificationDrying Plants

The most interesting development of the semiconcentrated system is a combination saponification/drying plant where the saponification plant is directly coupled to the spray chamber of the vacuum spray-dyer atomizer without the use of an intermediate storage or feed tank and a heat exchanger (Fig. 9.1 1).

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Fig. 9.9. Mazzoni LB "SSCT" Semi-boiled Soap Production Plant. Courtesy of Mauoni LB, S.p.A.

Fig. 9.1 0. Binacchi "CHBS"Semi-boiled Soap Production Plant. Courtesy of Binacchi & Co.

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Fig. 9.1 1. Combination Semi-concentrated Saponificationand Drying Plant.

Apart from obvious investment savings due to the reduced number of equipment pieces involved (at least a couple of pumps, a filter, a service tank, and a heat exchanger), this kind of setup delivers a series of hrther advantages: Exothermic nature of reaction is used to heat the soap without the need for external energy sources. The hot neat soap produced is sprayed directly into the vacuum-spray chamber of the dryer where the exact amount of water is flashed offto obtain the desired final moisture content of the dried soap pellets. Steam-saving of up to 60% with respect to the traditional plants. Reduced fines formation due to the reduced quantity of moisture to be removed (single liquid phase flow through the system). This permits one to utilize only one soap-fines recovery cyclone for medium-size plants.

No intermediate storage tank and no heat exchanger eliminate the exposure of the soap to air and local overheating, resulting in improved quality of the final product.
Figures 9.12 and 9.13 show two typical commercially available combination (integrated) plants.

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SAPONIFICATION

VACUUM SPRAY DRYING

Fig. 9.1 2. Binacchi'CHBS-VSD"Combination Semi-concentrated Saponification and Drying Plant. Courtesy of Binacchi & Co.

Fig. 9.1 3. Mauoni LB"SSCT-C"Semi-concentrated Combination Saponification and Drying Plant. Courtesy of Mauoni LB, SPA.

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An Atmospheric- and a Pressurired-system Comparison

Atmospheric Batch Systems
These were the first systems, and are still widely used due to their operational simplicity. O n e does not need to bother with pressure control. Mixing is continued until the reaction is completed. The soap is sampled periodically by the laboratory, and minor adjustments are made based on the analysis and the desired final-product specifications.

Atmospheric Continuous Systems

The atmospheric continuous systems are more complex, mostly due to the importance of avoiding incorporation of air during mixing. A vent valve on the crutcher eliminates the air during the filling stage and the produced soap leaves the crutcher through the siphon pipe, ensuring that the vessel is always full. Keeping the vessel full at all times requires good temperature control of the raw materials. The newly formed soap inside the crutcher must not boil; its temperature must be kept under 100C. The residence time given to the soap is fixed in the function of a production rate. If a problem occurs with the efficiency of saponification and the temperature cannot be increased, the residence time can, but this will result in a decreased production rate. Important to note is that atmospheric systems cannot produce semiconcentrated soap.

Pressurized Systems
Pressurized systems allow the use of increased pressure and temperature, resulting in a faster and a more complete reaction. Increasing temperature and pressure can also fix viscosity problems. Pressurized systems are more complex and are normally more expensive. The use of pressurized systems-the new combination (integrated) of saponification and drying plants for semiconcentrated soap productionrepresents the latest and most exciting advance in soapprocessing technology in a long time. From the above descriptions, the main characteristics of the atmospheric and pressurized systems are summarized as:

Atmospheric Systems
Low investment cost (batch version) Ease of use and maintenance Best suited for batch-type production.

Pressurized Systems
Require tighter control Very flexible and efficient Best suited for continuous production.

Continuous Saponification Plant Use for Semi-boiled Soap Production

The main components of the widely used, continuous, neutral fats-and-oils saponification process for the production of62-63% ofTFM neat soap are shown in Fig. 9.14. For more details on the continuous saponification plants, please refer to Chapter 8.

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Fig. 9.14. Continuous Neutral Fats and Oils Saponification Plant.

O n e can utilize a continuous saponification plant for Semi-boiled soap production by using either the reactor route (pressurized system) or the neutralizer route (atmospheric system).

Reactor Route-Pressurized System

A pressurized system requires the use of the reactor. O n e can apply any type of horizontal, vertical, stirred, or not stirred reactor that performs well for a full-boiled soap operation for a Semi-boiled soap production. A bypass must be installed from the cooler to the holding tank from where the finished Semi-boiled soap is transferred by using the existing transfer pump and piping. Normally, continuous, neutral fats and oils saponification works with a mass balance that avoids pumping the water into the reactor. Therefore, the usual dosing set-up does not have a water to reactor pump, or if it does, it is only a small emergency pump. For Semi-boiled soap production, water is required. A half-spent lye pump has the capacity required, and is therefore used for dosing the water into the reactor. Alternatively, Semi-boiled neat soap produced in the reactor and passed through the cooler is fed into the neutralizer. This operation allows for a longer residence time. Also, already installed pipes, valves, transfer pumps, etcetera of the plant can perform the eventual addition of minors.

Neutralizer Route-Atmospheric System

In the atmospheric pressure-type operation, the neutralizers group components are the key units. Raw materials are pumped into the recycle loop of the neutralizer, and are reacted there until the completion of saponification. Two main issues reside with this solution: (i) one needs to repipe the dosing section and bring all the raw materials to the neutralizer (water by using Half Spent Lye (HSL) pump included) and (ii) one will suffer some loss of the production due to the inferior efficiency of the neutralizer (when compared to the reactor).

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Fig. 9.1 5. Continuous Saponification Plant Utilization for Semi-boiled Soap Production Using the Reactor, Cooler, and Additional Water.

Fig. 9.16. Continuous Saponification Plant Utilization for Semi-boiled Soap Production Using the Reactor, Cooler, and the Neutralization Section.

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Fig. 9.1 7. Continuous Saponification Plant for Semi-boiled Soap Productionvia the NeutralizingSection.

High Shear-Mixer
Fig. 9.1 8. Neat Soap NeutralizationSystem.

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Other than that, the system is already piped properly, and no bypasses are to be added. The inlet that receives the neat soap from the centrifuges should be blanketed off. The neutralization sections details are shown in Fig. 9.18. The comparison with the atmospheric continuous system (Fig. 9.6) shows the similarity between these two systems-crutcher with a recycle loop, recycle pump, high-shear mixer, siphon pipe, and a second vessel to receive the finished product.

Definitions and Calculations

Sample Calculation for a Batch of Semi-boiled Soap
The production of 10 tons 0f6O% ofTFM, 80:20 tallow/coco-blend neat soap with a residual of 0.05% of free NaOH, and of 0.5% of NaCl follows: Tallow-saponification value (SV): 200 Coconut oil- Saponification Value (SV): 250 48% of NaOH (caustic soda) 20% of NaCl (brine) Desired: Quantity (kg) TFM (%) Residual NaOH (Yo) NaCl (%) At our disposition: Oil blend 80:20 SV NaOHYo in caustic NaCI% in brine TFM% in oils Glycerine% in oils 10,000 60 0.05 0.5 210 48 20 94.63 11

ID Letter A B C D E F G H I
x

Oils required = A x B/H = 10,000 x 60194.6 = 6340.5 kg (= J) Caustic soda required = [(J x E x 0.0713) + C x A]/F = [(6340.5 x 210 x 0.0713) + 0.05 = [(94936.3) + 500]/48 = 1988.25 kg (= M) Brine required = A x D/G = 10.000 x 0.5/20 = 250 kg (= K) Water required = A-J-M-K = 10,000 - 6340.5 -1988.25 -250 = 1421.25 kg (= L)

10,000]/48

The final formula is: 6340.5 kg of oil blend + 1988.25 kg of caustic soda + 250 kg of brine + 1421.25 kg of water.
?he soap produced will contain:

Anhydrous soap .................65.22% Glycerine .......................... 7.28% 26.95% Water ............................... 63.64% Virtual TFM ..................... (The real TFM value is 60%, but the increased glycerine content will make this soap behave as if it had 63.64% ofTFM, thus Virtual TFM.) Residual NaOH and NaCl should be as per-desired specs, that is, 0.05% and 0.5%, respectively.

All the calculations must be controlled via analysis. When comparing the analysis with calculated results, one can make the necessary corrections.

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46 TFM
Real Virtual

56 59.40 57 60.46 58 6 -52 1 59 62.58 60 63.64 6 1 64.70 62 65.76 63 66.82 Valid for 8020tallowkoconut mixture with 200 SV for tallow and 250 SV for coconut.

Glycerine Content Finder Diagram

52

52 d
a4

Theoretical Glycerine in Neat Soap, %

Note: Calculated for Tallow (PO) with SV of 250 and COCO (PKO) with SC of 250

Fig. 9.19. Glycerine Content Finder Diagram.