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Method for preparing crotonic acid through catalytic conversion of poly-3-hydroxybutyrate by using solid catalyst

A technology of hydroxybutyrate and solid catalyst, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problems of difficult recovery, volatile loss, high vapor pressure, etc., and achieve simple and convenient process operation Effect

Active Publication Date: 2019-05-03
DONGGUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcoming that crotonaldehyde, the raw material required for crotonic acid synthesis in conventional industrial methods, is highly toxic and harmful to the environment, and overcomes the difficulty in recovering the homogeneous acid-base catalyst used when poly-3-hydroxybutyrate is used as raw material , It is easy to cause environmental pollution and equipment corrosion problems, and the reaction solvent has the disadvantages of low boiling point, easy volatilization loss and high vapor pressure, and provides a method for preparing crotonic acid by catalytic conversion of poly-3 hydroxybutyrate with solid catalyst

Method used

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  • Method for preparing crotonic acid through catalytic conversion of poly-3-hydroxybutyrate by using solid catalyst
  • Method for preparing crotonic acid through catalytic conversion of poly-3-hydroxybutyrate by using solid catalyst
  • Method for preparing crotonic acid through catalytic conversion of poly-3-hydroxybutyrate by using solid catalyst

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Effect test

Embodiment 1

[0034] A kind of method utilizing solid catalyst catalytic conversion poly-3 hydroxybutyrate to prepare crotonic acid, specifically as follows:

[0035] 6.0g poly-3 hydroxybutyrate, 3g solid acid HND-58 catalyst and 60mL gamma valerolactone were placed in a 250mL three-necked flask reaction system with mechanical stirring and condensation (see figure 1 ), turn on the mechanical stirring (300rpm), the reaction system is heated from room temperature to 170°C at a rate of 8°C / min, and react at 170°C for 12 hours, and the poly-3-hydroxybutyrate is completely converted. Cool to room temperature after completion of the reaction, add 3.0g internal standard n-butanol to the reaction solution, and quantitatively analyze by GC-FID (see figure 2 ) detected that the content of crotonic acid in the product was 5.1 g, thus the productive rate of crotonic acid was 85%. Crotonic acid can be separated from gamma valerolactone by salting out or rectification, and the separated gamma valerolac...

Embodiment 2

[0038] A method for preparing crotonic acid by catalytic conversion of poly-3 hydroxybutyrate with solid catalyst, specifically as follows:

[0039] 6.0g poly-3 hydroxybutyrate, 3g solid superbase HND-63 catalyst and 60mL gamma valerolactone were placed in a 250mL three-necked flask reaction system with mechanical stirring and condensation (see figure 1 ), turn on the mechanical stirring (300rpm), the reaction system was heated from room temperature to 150°C at a rate of 8°C / min, and reacted at 150°C for 4 hours, and the poly-3-hydroxybutyrate was completely converted. Cool to room temperature after completion of the reaction, add 3.0g internal standard n-butanol to the reaction solution, and quantitatively analyze by GC-FID (see Figure 4 ) detects that the content of crotonic acid in the product is 3.9g, thus the productive rate of crotonic acid is 65%. Crotonic acid can be separated from gamma valerolactone by salting out or rectification.

[0040] The solid superbase HND...

Embodiment 3

[0042] A method for preparing crotonic acid by catalytic conversion of poly-3 hydroxybutyrate with solid catalyst, specifically as follows:

[0043] Put 6.0g poly-3 hydroxybutyrate, 3g solid acid NR50 catalyst and 60mL gamma valerolactone were placed in a 250mL three-necked flask reaction system with a mechanical stirring and condensation device (see figure 1), turn on the mechanical stirring (300rpm), the reaction system is heated from room temperature to 160°C at a rate of 8°C / min, and react at 160°C for 12 hours, and the poly-3 hydroxybutyrate is completely converted. After the reaction was completed, it was cooled to room temperature, and 3.0 g of internal standard n-butanol was added to the reaction solution, and the content of crotonic acid in the product was detected to be 3.7 g by GC-FID quantitative analysis, thus the yield of crotonic acid was 62%.

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Abstract

The invention relates to a method for preparing crotonic acid through catalytic conversion of poly-3-hydroxybutyrate by using a solid catalyst. The method comprises the following steps: poly-3-hydroxybutyrate, the solid catalyst and a gamma valerolactone solvent are mixed, and stirred and react for 1 to 24 hours at 120 to 180 DEG C to obtain crotonic acid; wherein the solid catalyst is one or moreof a solid acid catalyst or a solid base catalyst. The invention takes stable and high boiling point gamma valerolactone as solvent, solid acids and solid bases which are easy to separate and recoverand reusable are used as catalysts, so as to convert environmentally friendly and renewable poly-3-hydroxybutyrate into crotonic acid, and that yield of crotonic acid is as high as 85%, which has theprospect of industrialization. In addition, gamma valerolactone is used as the reaction solvent and has high stability and negligible loss in the preparation of crotonic acid. The separation and recovery process of solid catalyst after reaction is simple and has good reusability.

Description

technical field [0001] The invention belongs to the field of crotonic acid preparation, and in particular relates to a method for preparing crotonic acid by catalytically converting poly-3-hydroxybutyrate with a solid catalyst. Background technique [0002] Crotonic acid, scientific name 2-butenoic acid, is an unsaturated C 4 organic acids. The application of crotonic acid is extremely extensive, and can be used in the preparation of synthetic resins, hair sprays, fungicides, plasticizers and medicines. For example, the copolymer of crotonic acid and vinyl acetate can be used as hot-melt adhesive for binding books, coating and paper for wallpaper, adhesive for laminates, film developer and electrostatic copying solution components, etc. At present, the process route adopted by industrial production of crotonic acid at home and abroad is to use crotonaldehyde as raw material to prepare crotonic acid through selective oxidation (such as CN200710019294.2). Crotonaldehyde is ...

Claims

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Application Information

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IPC IPC(8): C07C57/08C07C51/09
Inventor 康世民周海平吴旋华钟颖严明丽谢秀卿徐勇军肖雨葵
Owner DONGGUAN UNIV OF TECH
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