Method and apparatus for purifying vitamin A intermediate mynistic aldehyde

Abstract

This invention relates to purification method of intermedium myristic aldehyde and device. The device has set heater, fractionating tower, falling film reboiler, falling film evaporator and condenser. Raw myristic aldehyde outlet of heater connect with fractionating tower inlet; steam outlet of fractionating tower top connect with condenser steam inlet; one way of first condenser condensed fluid outlet connect with reflux liquid inlet of fractionating tower top, the other way outflow low boiler of beta - ionone. Dephlegmation tower bottom outlet respectively connect with falling film reboiler overhead entrance and falling film evaporator overhead entrance; falling film reboiler bottom outlet connect with fractionating tower bottom entrance; one way of falling film evaporator outlet connect with second condenser entrance, the other way is outlet of high boil thing; second condenser outlet is outlet of refine myristic aldehyde. Whil purification first send raw myristic aldehyde to fractionating tower, gain distillate from fractionating tower top. The distillate enter fractionating tower bottom tower kettle, pass through falling film evaporator to remove high boil thing.

Description

technical field [0001] The invention relates to a vitamin A intermediate, in particular to a method for purifying the vitamin A intermediate tetradecaldehyde. Background technique [0002] β-tetradecaldehyde (tetradecaldehyde for short) is an important intermediate for the synthesis of vitamin A, and its structural formula is as follows: [0003] [0004] Tetradecaldehyde is usually prepared by condensation reaction of β-ionone, and the crude tetradecaldehyde generally contains 80% to 86% of tetradecaldehyde, 4% to 8% of β-ionone, 8% to 12 % of high boilers and 1% to 2% of other substances. [0005] Ionone is a reactant for preparing myristal, and its physical and chemical properties have certain similarities with myristal. The publication number is CN1348949, which provides a production method of β-ionone in the patent application of CN1348949. The cyclization reaction is carried out under the action of strong acid. After mixing pseudoionone and chloromethane, the cycl...

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Problems solved by technology

The problem that this method exists is: (1) intermittent distillation is a kind of unstable process, can not separate tetradecaldehyde and β-ionone completely, and the purity of the tetradecaldehyde obtained by final refining is not high, generally only has 90%~94 %; (2) Tetradecaldehyde material is heated at high temperature for a long time in the distillation kettle, which produces unnecessary decomposition side reactions, so the refining yield is not high

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