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A kind of synthesis technique of trimellitic acid triglycidyl ester

A technology of triglycidyl ester and trimellitic acid, applied in the direction of organic chemistry and the like, can solve the problems of affecting product yield and product quality, complex reaction products, and high production costs

Active Publication Date: 2020-04-28
JIANGSU ZHENGDAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The transesterification method needs to prepare the methyl ester intermediate first, and there is a problem of high production cost
Esterification-ring-closing two-step method is currently a method that has attracted much attention for the preparation of epoxy resin compounds. Although this method needs to go through two steps of epoxy ring-opening and ring-closing, the actual intermediate product does not need to be purified; Ring-opening esterification is a heterogeneous reaction, coupled with the use of catalysts, and the hydrolysis of esters under basic conditions during ring closure. At the same time, self-polymerization or mutual polymerization of epoxy compounds will cause complex reaction products, which will affect product yield and product quality. Quality, so the synthesis process route needs to be improved and the new reactor design

Method used

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  • A kind of synthesis technique of trimellitic acid triglycidyl ester
  • A kind of synthesis technique of trimellitic acid triglycidyl ester
  • A kind of synthesis technique of trimellitic acid triglycidyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Put 40kg of trimellitic acid, 62.2L of acetone, 50L of epichlorohydrin, and 0.2kg of cetyltrimethylammonium bromide into the reactor in turn, stir, and heat up to 85°C. Promote the reflux of epichlorohydrin, and add 100 L of epichlorohydrin in two equal portions. Reaction 7h. Then epichlorohydrin and co-solvent were removed under reduced pressure to obtain a concentrated reaction solution.

[0058] 60 L of dichloromethane was added to the reaction liquid, and the temperature was raised to 50°C. Slowly add 53.4kg of 50% sodium hydroxide solution through a constant pressure dripping device, vacuumize the reaction system (-0.1MPa) and remove the water therein through reflux condensation with a water separator, and control the dripping within 1h. Then continue to keep warm for 7h.

[0059] Cool to room temperature after the reaction, filter off sodium chloride, and wash the filtrate with water until the organic layer is neutral. The organic phase is distilled to remove ...

Embodiment 2

[0061] Put 40kg of trimellitic acid, 66.6L of N,N-dimethylformamide, 64L of epichlorohydrin, and 0.6kg of octadecyltrimethylammonium chloride into the reactor in sequence, stir, and heat up to 85°C. During the reaction process, the reflux of epichlorohydrin was continuously promoted through the reflux condenser, and 130 L of epichlorohydrin was added in two equal parts. Reaction 6h. Then epichlorohydrin and co-solvent were removed under reduced pressure to obtain a concentrated reaction solution.

[0062] 71 L of dichloromethane was added to the reaction liquid, and the temperature was raised to 45°C. Slowly add 57.2kg of 50% sodium hydroxide solution through a constant pressure dripping device, vacuumize the reaction system (-0.1MPa) and remove the water therein through reflux condensation with a water separator, and control the dripping within 1h. Then continue to keep warm for 6.5h.

[0063] Cool to room temperature after the reaction, filter off sodium chloride, and was...

Embodiment 3

[0065] Put 36.5kg of trimellitic anhydride, 15.4L of water, 89L of epichlorohydrin, and 0.8kg of hexadecyltrimethylammonium bromide into the reactor in turn, stir, and raise the temperature to 95°C. During the reaction, pass through the reflux condenser Continuously impel epichlorohydrin to reflux, and epichlorohydrin 180L is added in two equal parts. Reaction 5h. Then epichlorohydrin and co-solvent were removed under reduced pressure to obtain a concentrated reaction solution.

[0066] 127 L of dichloromethane was added to the reaction liquid, and the temperature was raised to 45°C. Slowly add 61 kg of 50% potassium hydroxide solution through a constant pressure dripping device, vacuumize the reaction system (-0.1 MPa) and remove the water therein through reflux condensation with a water separator, and control the dripping within 1 hour. Then continue to keep warm for 5h.

[0067] After the reaction was completed, it was cooled to room temperature, potassium chloride was f...

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Abstract

The invention provides a synthetic process of triglycidyl trimellitate. The synthetic process comprises the following steps: (1) performing the esterification step by step: adding trimellitic acid ortrimellitic anhydride, co-solvent, epichlorohydrin and a catalyst into a reactor, preserving the heat, reacting, and after the esterification reaction is completed, removing the epichlorohydrin and the co-solvent in a decompression evaporation manner; (2) eliminating a closed loop: adding a closed-loop solvent, heating the reactor to a reaction temperature, slowly dropwise adding an aqueous solution of inorganic base, reacting for an appropriate time by preserving the needed reaction temperature, and removing the water of the reactor at a negative pressure state by using a water separator at the same time; and (3) refining: filtering, washing with water, separating, and distilling. By adopting the measures provided by the invention, the continuous reaction of epichlorohydrin and an intermediate product can be effectively prevented from generating a bipolymer or polymer, and the hydrolysis of a target product can be effectively prevented. The reaction temperature is moderate, the reaction time is short, few side products are generated, the after-treatment is simple and environmentally friendly, the product quality is good, the industrialized production is realized, and the economicbenefit is good.

Description

technical field [0001] The invention relates to a method for synthesizing trimellitic acid triglycidyl ester, specifically, trimellitic acid or trimellitic anhydride and epichlorohydrin are synthesized in three steps of trimellitic acid or trimellitic anhydride and epichlorohydrin through stepwise esterification-eliminating ring closure-refining three-step method Glyceride; belongs to the field of organic chemical industry. Background technique [0002] Triglycidyl trimellitate, chemical name is 1,2,4-benzenetricarboxylate tris(oxiranylmethyl)ester, CAS number is 7237-83-4, molecular formula: C18H18O9, molecular weight: 378.33g / mol, boiling point: 278°C, melting point: -21.5°C, density heavier than water, light yellow transparent liquid, slightly soluble in water, methanol, easily soluble in organic solvents such as ethyl acetate, acetonitrile, acetone, etc. In terms of structure, because it contains highly active epoxy groups in its molecules, it can carry out a series of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/26C07D303/16
CPCC07D301/26C07D303/16
Inventor 曹正国李江华王福荆晓平张小平冯龙海陈佳佳
Owner JIANGSU ZHENGDAN CHEM IND CO LTD