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Integrated utilization method for byproduct of vanillin production

A by-product, vanillin technology, applied in the direction of organic chemistry

Inactive Publication Date: 2008-08-06
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to solve the problem of comprehensive utilization of glyoxylic acid and guaiacol reaction by-products

Method used

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  • Integrated utilization method for byproduct of vanillin production
  • Integrated utilization method for byproduct of vanillin production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 156.6 g of industrial guaiacol (1.2 mol) with a content of 95% was dissolved in 1200 ml of 4% sodium hydroxide solution to obtain a light red sodium guaiacol solution. 1000ml of 10% sodium carbonate solution was added into 222g of 40% glyoxylic acid solution (1.2mol) under stirring to obtain light yellow sodium glyoxylate solution. Use a 3000ml four-necked bottle equipped with a stirrer, a thermometer and a dropping funnel as the reactor, first add the sodium guaiacol solution, then add the sodium glyoxylate solution dropwise at 15-25°C under stirring, and complete the addition in about 8 hours , Then continue to stir and react for about 8 hours to make all sodium glyoxylate in the solution convert. The total volume of the reaction mother liquor is about 2400ml, and liquid chromatography analysis contains 190g (0.96mol) of 3-methoxyl-4-p-hydroxymandelic acid and 45.4g of 3-methoxyl-4-p-hydroxymandelic acid dimer (0.12 mol). Concentrate the reaction solution in vacuo t...

Embodiment 2

[0014] Add 45.4g (0.12mol) of 3-methoxy-4-p-hydroxymandelic acid dimer into a 250ml four-necked bottle equipped with a stirrer, a thermometer and a dropping funnel, and add 37% formaldehyde solution under stirring 19.5 g (0.24 mol). Heat to 65°C with an electric heating mantle, add dropwise 10% hydrochloric acid solution, control the pH of the solution to 1.5-2.5, and stop the condensation reaction after reacting for 3 hours. Concentrate in vacuo, and remove the upper layer of water after cooling to obtain 48.1 g of modified phenolic resin.

Embodiment 3

[0016] Add 45.4g (0.12mol) of 3-methoxy-4-p-hydroxymandelic acid dimer into a 250ml four-necked bottle equipped with a stirrer, a thermometer and a dropping funnel, and add epichlorohydrin under stirring 33.6 g (0.36 mol). 25ml of 30% sodium hydroxide solution was added dropwise, and the temperature was controlled at 75°C. After the alkali solution was added dropwise, the reflux reaction was continued for 1.5h, and then the condensation reaction was stopped by cooling. Separate the organic phase by extracting three times with 150 ml of benzene, and wash the organic phase with warm water. Excess epichlorohydrin was recovered by distillation to obtain 50.1 g of modified epoxy resin.

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Abstract

The invention relates to a comprehensive utilization method of vanillin production byproduct, which comprises effectively separating 3-methoxy-4-hydroxy benzene glycollic acid dimmer from product to replace part or total phenol to be condensed with formaldehyde to prepare modified phenol resin, replacing part or total bisphenol A to be condensed with epichlorohydrin to prepare modified epoxy resin, replacing part or total benzene dicarboxylic acid to be condensed with maleic acid and methyl glycol to prepare unsaturated alkide resin. The modified resin has wide application in paint, adhesive and plastic to reduce vanillin production cost and eliminate waste liquid pollution in production.

Description

technical field [0001] The invention relates to a method for comprehensive utilization of by-products of vanillin production, in particular, phthalic acid, phenol and The invention discloses a method for synthesizing modified resin from raw materials such as bisphenol A, and belongs to the fields of polymer chemical industry and polymer materials. Background technique [0002] Glyoxylic acid and phenolic compounds undergo condensation reaction to produce p-hydroxyphenylglycolic acid derivatives, through which a series of fine chemicals can be synthesized simply and efficiently, and have a wide range of applications in medicine, pesticides and daily chemicals. The main varieties that have been industrialized at home and abroad are summarized as follows: [0003] [0004] The process of preparing vanillin with glyoxylic acid and guaiacol has been applied on a large scale industrially. The inventor of the basic process has introduced it in detail in "Jiangsu Chemical Indust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/28C08G59/12C08G63/60C07C47/58
Inventor 李建生朱虹朱振赵斌斌
Owner TIANJIN VOCATIONAL INST
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