Preparation method of 2, 4-hexadienoic acid polyester

A technology of hexadienoic acid polyester and ketene, applied in 2 fields, can solve the problems of low conversion rate and low yield of beta-methacrolein, and achieve the effects of improving the conversion rate of beta-methacrolein and reducing the amount of waste water

Active Publication Date: 2014-03-05
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is: in terms of catalyst selection, the main catalysts used are zinc acetate, zinc methacrylate, α-picoline, zinc chloride, aluminum chloride, etc., so that the conversion rate of raw material β-methacrolein Low, the conversion rate of raw material β-methacrolein is only 80%; the yield of 2,4-hexadienoic acid polyester is low, and the yield of 2,4-hexadienoic acid polyester is only 85%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: the preparation method of titanium dioxide-silicon dioxide-caprolactam composite catalyst:

[0036] Hydrolyze 8.8083g butyl titanate in 103.6ml0.1mol / L hydrochloric acid to obtain TiO2 sol A; then hydrolyze 21.5544g ethyl orthosilicate in a mixed solution of 12.8ml0.2mol / L hydrochloric acid and 15.4ml ethanol to obtain SiO2 Sol B; mix A and B and stir for 0.5 hours to obtain a colorless, clear and transparent TiO2 / SiO2 sol C; dissolve 11.7099g caprolactam in 780g water to obtain solution D, drop sol C into solution D, wash and dry , to obtain a titanium dioxide-silicon dioxide-caprolactam composite catalyst.

Embodiment 2

[0037] Embodiment 2: the preparation method of 2,4-hexadienoic acid polyester

[0038] Add 550Kg β-methacrolein and 5Kg titanium dioxide-silicon dioxide-caprolactam composite catalyst into a 1500L reactor, start stirring, raise the temperature to 40°C, and control the temperature between 40±1°C and feed 330Kg ketene gas to react After the reaction is completed, the catalyst is filtered, and the reaction liquid is rectified by negative pressure (vacuum degree 0.098MPa) to recover 27Kg of β-methacrolein (one-pass conversion rate 95.1%) and apply it to the next batch to obtain high-viscosity 2,4- Hexadienoic acid polyester 757.3Kg, one-way yield 90.5%.

Embodiment 3

[0039] Embodiment 3: the preparation method of 2,4-hexadienoic acid polyester

[0040]Add 580Kg β-methacrolein and 7Kg titanium dioxide-silicon dioxide-caprolactam composite catalyst into a 1500L reactor, start stirring, raise the temperature to 45°C, and control the temperature between 45±1°C and feed 345Kg ketene gas to react After the reaction is completed, the catalyst is filtered, and the reaction liquid is rectified by negative pressure (vacuum degree 0.099MPa) to recover 24.4Kg of β-methacrolein (one-pass conversion rate 95.8%) and apply it to the next batch to obtain high viscosity 2,4 - 809.8Kg of hexadienoic acid polyester, the yield per pass is 91.1%.

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Abstract

The invention provides a preparation method of 2, 4-hexadienoic acid polyester. The preparation method comprises the following steps of adding 500-650 parts by weight of beta-methyl acrolein and 3-15 parts by weight of titanium dioxide-silicon dioxide-caprolactam composite catalyst into a reaction kettle, stirring, introducing ketene gas at the temperature of 35-50 DEG C for reaction, filtering after the completion of the reaction, and performing negative pressure rectification on a reaction solution to obtain 2, 4-hexadienoic acid polyester. The condensation catalyst used in the method adopts the titanium dioxide-silicon dioxide-caprolactam composite catalyst, so that the conversion rate of beta-methyl acrolein is improved, the yield of the product 2, 4-hexadienoic acid polyester is simultaneously improved, and the waste water amount produced by production is also reduced; by using the method, the single-pass conversion rate of the raw material beta-methyl acrolein can achieve 95%, and the single-pass yield of the 2, 4-hexadienoic acid polyester can be above 90%.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a preparation method of 2,4-hexadienoic acid polyester. Background technique [0002] 2,4-Hexadienoic acid polyester is an important intermediate in the production of 2,4-hexadienoic acid. 2,4-Hexadienoic acid is white needle-like or powdery crystal, slightly soluble in water and soluble in many organic solvents. Molecular weight of 2,4-hexadienoic acid: 112.13; Melting point: 132-135°C; Boiling point: 228°C (decomposition); Density: 1.204 (19°C); [0003] Flash point: 127°C. 2,4-Hexadienoic acid is a kind of unsaturated fatty acid with conjugated diene, it can effectively inhibit the activity of mold, yeast and aerobic bacteria, and its effect of inhibiting the development and reproduction of harmful microorganisms is stronger than that of bactericidal, It is a preservative recommended by the Food Organization of the United Nations to countries all over the worl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/52C08G63/85
Inventor 丁彩峰朱小刚刘芳姚俊生
Owner NANTONG ACETIC ACID CHEM
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