Combination step batch operation

In this representation the FeCl2 which takes part in the first step of the reaction is not a tme catalyst, but is continuously formed from HQ. and iron. This is a highly exothermic process with a heat of reaction of 546 kj /mol (130 kcal/mol) for the combined charging and reaction steps (50). Despite the complexity of the Bnchamp process, yields of 90—98% are often obtained. One of the major advantages of the Bnchamp process over catalytic hydrogenation is that it can be mn at atmospheric pressure. This eliminates the need for expensive high pressure equipment and makes it practical for use in small batch operations. The Bnchamp process can also be used in the laboratory for the synthesis of amines when catalytic hydrogenation caimot be used (51). 

Mode 2. With this operation model, the mixture is separated by distUlalion to obtain some of the heteroazeotrope in the decanter, and the liquid-liquid split takes place during distillation with withdrawal or accumulation of the entrainer-lean phase and reflux of aU or part of the entrainer-rich phase. A start-up period is needed for Mode 2 as stated in Skouras et al., " where all the mixed phases are refluxed. In our study, this Mode 2 operation will be used to combine two different separation methods (distUlation and liquid-liquid splitting) simultaneously. The batch operating sequence was further modified to combine the start-up period with the next batch operating step to save the total batch time. 

An excess of crotonaldehyde or aUphatic, ahcyhc, and aromatic hydrocarbons and their derivatives is used as a solvent to produce compounds of molecular weights of 1000—5000 (25—28). After removal of unreacted components and solvent, the adduct referred to as polyester is decomposed in acidic media or by pyrolysis (29—36). Proper operation of acidic decomposition can give high yields of pure /n j ,/n7 j -2,4-hexadienoic acid, whereas the pyrolysis gives a mixture of isomers that must be converted to the pure trans,trans form. The thermal decomposition is carried out in the presence of alkaU or amine catalysts. A simultaneous codistillation of the sorbic acid as it forms and the component used as the solvent can simplify the process scheme. The catalyst remains in the reaction batch. Suitable solvents and entraining agents include most inert Hquids that bod at 200—300°C, eg, aUphatic hydrocarbons. When the polyester is spHt thermally at 170—180°C and the sorbic acid is distilled direcdy with the solvent, production and purification can be combined in a single step. The solvent can be reused after removal of the sorbic acid (34). The isomeric mixture can be converted to the thermodynamically more stable trans,trans form in the presence of iodine, alkaU, or sulfuric or hydrochloric acid (37,38). 

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