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INSTRUCTION MANUAL.
PLUG FLOW REACTOR
SET UP DESCRIPTION SPECIFICATIONS INSTALLATION REQUIRMENTS INSTALLATION AND CONNECTIONS PRECAUTIONS TROUBLE SHOOTING
EXPREMENTATION THEORY OPERATING PROCEDURE’ SYSTEM CONSTANTS OBSERVATION TABLE CALCULATIONS PLUG FLOW REACTOR AIM: To study the saponification of ethyl acetate in a plug flow reactor and to determine percentage conversion and theoretical conversion.
APPRATUS: A plug flow reactor, burette, pipette, conical flasks, measuring cylinders etc.
CHEMICALS: Ethyl acetate, NaOH, oxalic acid, HCl
THEORY: Saponification of ethyl acetate undergoes as follows: CH3COOC2H5 + NaOH → CH3COONa + C2H5OH B + A → P
Reaction is made homogeneous and is first order with respect to ester and alkali. The rate of reaction can therefore be written as, -rA= KCA CB K = 10 lit/g-mole. min at25 deg. C Performance equation of the constant Plug flow reactor is (V CAO’/FAO) = = CAO’ ∫DxA/-rA K CAO’ = [1/(M-1)] X ln[(M-XA)/M(1-XA)] ------ (1) M= CBO’/CAO’ When m ≠ 1 When M = 1 K CAO’ = XA/ 1-XA.
PROCEDURE: Prepare the following solutions: Ethyl acetate – 0.1 N, NaOH – 0.05N, HCl/Acetic acid -0.05 N All solutions are prepared freshly and standardize NaOH with oxalic acid. The experiment is to be carried out at room temperature. Fill up the overhead tanks with 30 lts of NaOH and ethyl acetate. Find out the volume of the reactor. Adjust total flow rate into the reactor in such a way to have residence time of 4-5 min. Keep the bottom valve closed until the reactor is filled. Once the reactor is filled open the bottom valve and maintain the level. Collect the samples after 2—time. Titrate the sample against HCl immediately (as the reaction is very fast and experiment is carried out without arrestation.) For steady state to be approached a low 2 – to 3 – time to be elapsed before taking samples for titration.
Operating procedure 1. Feed tanks – open small air vent valve and insure that bottom valves are closed. Fill up feed tanks slowly. Close all valves of feed tank. 2. Start air supply to both the tanks through air regulator, assuring that the air pressure from regulator to feed tanks will not exceed 1 to 1.5 kg/cm². 3. Slowly open feed valve say 25% open. 4. Adjust rota meter valves to desired flows and ensure steady-state flow rate. 5. Initially keep minimum flow rates possible. 6. After reaching to steady-state of process conditions start to withdraw samples. 7. After experimentation first close air supply valve to tanks. 8. Drain all tanks slowly. 9. Flush all system tanks and reactor by circulating water through it. 10. important note: during pneumatic conveying, don’t allow air to pass through Rota meters from feed tank. It may damage Rota meter tube. So ensure sufficient quantity of feed material in feed tanks. OBSERVATION: Volume of reactor = V = 1.170 liter. Vol. Flow rate of ester = vB Vol. flow rate of NaOH = vA Normality of ester = CBO Normality of NaOH = CAO Normality of oxalic acid = NOX Normality of HCl = NHCl Sr. No. Time ( min) Burette reading ( VHCl)
CALCULATIONS: = V / (VA + VB) CA = NHCl VHCl / V sample CAO’ = CAO . vA / ( vA + vB ) XA = (CAO’ CA) / CAO’. Theoretical conversion can be calculated by following equation K CAO’ = [1/(M-1)] X ln[(M-XA)/M(1-XA)] RESULT: The saponification of ethyl acetate in PFR is studied and 1. Experimental conversion = 2. Theoretical conversion =
