Basic Parameters 1.1.

.1. Retention time in destillation column Minimum allowable flow reactant Maximum unit operation Volume and retention time of reactor

The destillation column tested in the literature (He,Singh et al. 2005; He, Singh et al. 2006; He, Singh et al. 2007) had good biodiesel yield with retention times inside the column varying from 2 to 10 minutes. A 1500 L reactor was chosen, which therefore gave overall flows varying between 10 and 50 L/min and a minimal methanol flow of 1.1 mL/min. Qmax Qmin = = = = = =

Flow (L/min) Reactor Volume 1000 1100 1200 1300 1400 1500 1600 2 500 550 600 650 700 750 800 10 100 110 120 130 140 150 160

Tabel 1-1. Flow in function of reactor volume 1.2. Unit operation time

First hour : the unit is expected to stabilize and reach its maximum conversion capacity. Last 2 hours : the unit should work under its full potential and samples could be taken. At 3 hours : the unit having a maximum production time and allows the separation process to be done in decanters instead of using centrifugal pumps.

1.3.

Required volume for pre-reactor

The range of retention time in the pre-reactor should be between 1 and 4 minutes as cited in the literature (Singh, Thompson et al. 2004; He, Singh et al. 2006). Such a retention time should belong enough to heat the solution to 55C and allow for adequate mixing. The reaction is expected to start in the pre-reactor. By trial and error and by considering the overall flow, the ideal working volume was fixed at 50 mL. RTmin at pre-reactor = =
retention time (minute) Volume for prereactor 500 600 700 750 800 900 1000
Qmin (150 L/min) Qmax (750 L/min)

= 5 minutes

3,333 4 4,67 5 5,33 6 6,66

0,66 0,8 0,93 1 1,06 1,2 1,33

Tabel 2. Retention time in the reactor based on the working volume 1.4. Required range of pumping rates

Based on the literature(He, Singh et al. 2005), the expected methanol to oil molar ratio for this research unit will varies between 3:1 and 6:1. Step 1: Find the molar volume of reactants at room temperature The unit is located in Coimbatore in an open environment without air conditioning. Therefore the room temperature was set to 30C.

Tabel 3. Molar volumes for all chemicals involved in the reaction at different temperatures (mL/mol)

Step 2: Find the volume ratio Based on the molar volume, the quantity of methanol solution that should be supplied to the system for every mL of oil entering the system can be calculated. Here after, this value will be called Volume Ratio. Volume Ratio = =

Tabel 4. Volume ratio Step 3: Find the pumping rates This calculation is crucial since it allows for the proper sizing of the initial containers as well as the volume of the reactor. minimum pumping rate of oil [with molar ratio of 3:1 & flow of 150 L/min]

Tabel 5. Pumping rate for oil and methanol

1.5.

Required size for containers

The main systems driving force is gravity, and the flows are regulated by valves only. To size the oil container, a certain portion ofthe volume was dedicated to the upper cylinder part and the remaining portion to the lower conicalpart. This is done partly to ensure shallow container. Sizing the Methanol & NaOH Container:

Sizing the Jatropha Oil Container:

The use of a bag to contain the methanol isvery convenient since it reduces the vapor emanation. 1.6. Required mass of NaOH

In the literature, the quantity of NaOH to use for biodiesel production with Jatropha seed oil should vary between 0.5 and 1.5% of the oil mass (Chitra, Venkatachalam et al. 2005). Therefore, the maximum mass is obtained under a ratio of 1.5%, maximal flow rate, and a methanol to oil molar ratio of 3 to 1. [
[

]
]

1.7.

Reactor

The reactor consists of a reactive distillation column. A working volume of 1500 L is desired, distributed over 10 plates (Singh, Thompson et al. 2004; He, Singh et al. 2005; He, Singh et al. 2006). Hence, each plate holds 150 L of solution. The distance between the plates is selected at 25 cm based on information found in the literature (Singh, Thompson et al. 2004; He, Singh et al. 2006; He, Singh et al. 2007).

Step 1: Find the plate working area (plate area which holds the solution)

Step 2: Find the total plate area As mentioned earlier, the weir should represent 5% of the total plate area. Therefore, the working area represents 95% of the total plate area.

1.8. Methanol evaporator

The evaporator is designed for the worst case scenario, which occurs under the highest flow, the highest expected evaporator temperature, the highest methanol to oil molar ratio, and the lowest system efficiency. This translates into: Flow of 750 L/min Temperature of the solution entering the evaporator is around 60C and temperature of the solution leaving is around 130C Methanol to oil molar ratio of 6 to1 60% reaction efficiency

The balanced chemical equation under reaction efficiency of 60% becomes: 1 mol oil + 6 mol methanol 0.4 mol oil + 4.2 mol methanol + 1.8 mol + 0.6 mol glycerol

Since the efficiency is 60%, only 0.6 mol of oil is converted to biodiesel. Therefore the final quantities are:

oil methanol biodiesel glycerol

: 0.4 mol = 1 mol - 0.6 mol reacted : 4.2 mol = 6 mol - (0.6 mol x 3)reacted : 1.8 mol = (0.6 x 3) mol : 0.6 mol = (0.6 x 1) mol

To have complete methanol evaporation in the evaporator, one needs to know the minimal evaporator volume required. To do so, the energyand the mass transfer need to be quantify. Step 1: Mass flow of each component entering the evaporator When the solution gets to the condenser, the reaction has occurred and therefore the nature of the initial solution has changed. Consequently, the mass flow rate of each component (oil, methanol, biodiesel, and glycerol) has changed from the initial known mass flow rate. The mass flow rate of each component entering the evaporator is determined using molar flow. The molar flow of each component entering the evaporator is found using stoechiometric coefficients from the balanced reaction equation under worst case conditions. Therefore, the reaction of one mole of oil will translate into products formation accordingly to the stoechiometric coefficients. Since the initial mass flow of oil is known, it is possible to find the oil molar flow. Masa oil yang masuk ke reactor :

Ini pada kondisi effisiensi reaktor sebesar 60% (berdasarkan satuan molar ) maka :

Maka laju aliran masa oil yang masuk ke evaporator adalah :

Therefore, it is possible to calculate the number of moles of all components entering the evaporator using the stoechiometric coefficients, and consequently to find their mass flow rate. [Note that the properties are evaluated at 60C.]

Tabel 6. Mass flow rate of each component entering the evaporator

Step 2: Energy Balance The following schematic is a representation of the evaporator energy situation.

Gambar 1. Energy balance in methanol evaporator From the Energy Equation:

In this system, it is assumed that heat lost is negligible. Therefore, Qout = 0 Consequently,

Where:

(applicable when no phase change occurs) Example :

(Applicable when there is phase change) Example :

[ [ ] [ ] ]

Therefore,

Tabel 7. Energy for each component

Step 3: Find the minimal evaporator volume required The methanol evaporates quickly from the solution. Hence, the properties of the remaining solution are taken assuming no methanol is present.

1- Find the density of the solution:

Where the ratio volume is determine as follow:

Example :

Tabel 8. Volume ratio of each component entering the evaporator 2- Find the specific heat of solution:

Where: Mass ratio is established from previous calculations see step one :

Tabel 9. Mass flow of each component leaving the evaporator

This result can be interpreted as the quantity of incoming solution at 55C that can be heated to 130C in one minute. Considering that the maximum flow is 750 L/min, it can be expected that all methanol will evaporate.

The evaporator working volume is chosen to be 200 mL. Hence, with Qmax at 20 mL/sec, it will take about 13 seconds to heat the entering solution to the desired temperature (130C). 1.9. Decanter

the volume of biodiesel produced varies proportionally with the oil flow. Assuming maximum flow conditions and all the oil isconverted to biodiesel and glycerol (100% efficiency), one can size the decanter. As mentioned earlier, the maximum working time of the unit is 3 hours. For each mole of oil entering the system, 3 mol of biodiesel and 1 mol of glycerol is yield.

From this, it is possible to find the minimum volume required for the decanter. Step 1: Find the maximum number of moles of oil entering the system during a 3 hours period.

Step 2: Find the number of moles of biodiesel and glycerol thatcan be produced under maximum flow and assuming 100% efficiency.

Step 3: Find the total volume produced

Hampir semua biodiesel diproduksi dengan metode transesterifikasi dengan katalisator basa karena merupakan proses yang ekonomis dan hanya memerlukan suhu dan tekanan rendah. Hasil

konversi yang bisa dicapai dari proses ini adalah bisa mencapai 98%. Proses ini merupakan metode yang cukup krusial untuk memproduksi biodiesel dari minyak/lemak nabati. Proses transesterifikasi merupakan reaksi dari trigliserin (lemak/minyak) dengan bioalkohol (methanol atau ethanol) untuk membentuk ester dan gliserol. Minyak nabati dengan kadar asam lemak bebas (ALB)-nya rendah (< 1%), bila lebih, maka perlu pretreatmentkarena berakibat pada rendahnya kinerja efisiensi. Padahal standar perdagangan dunia kadar ALB yang diijinkan hingga 5%. Jadi untuk minyak nabati dengan kadar ALB >1%, perlu dilakukan deasidifikasi dengan reaksi metanolisis atau dengan gliserol kasar. Secara sederhana reaksi transesterifikasi dapat digambar sebagai berikut : 100 lbs Minyak Nabati + 10 lbs Methanol -"100 lbs Biodiesel + 10 lbs gliserol R1, R2, dan R3 adalah alkil dari ester. Selama proses esterifikasi, trigliserin bereaksi dengan alkohol dengan katalisator alkalin kuat (NaOH, KOH atau sodium silikat). Jumlah katalisator yang digunakan dalam proses titrasi ini adalah cukup menentukan dalam memproduksi biodiesel. Secara empiris, 6,25gr/l NaOH adalah konsentrasi yang memadai. Reaksi antara biolipid dan alkohol adalah reaksi dapat balik (reversible) sehingga alkohol harus diberikan berlebih untuk mendorong reaksi kekanan dan mendapatkan konversi yang sempurna.