Synthesis method of diphenyl isophthalate

A technique for diphenyl isophthalate and a synthesis method, which is applied in the field of synthesis of diphenyl isophthalate, can solve problems such as harsh reaction conditions, difficult esterification, and long reaction process, and achieve conversion and yield High, easy reactivity, and mild reaction conditions

Inactive Publication Date: 2012-08-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the reaction process is long and the yield is low, and the operation is cumbersome and increases the amount of labor; 2. Using isophthalic acid and diphenyl carbonate, under the condition of stannous oxide as a catalyst, the temperature is 250-300 ° C, Reaction 30 minutes to several hours, this method reaction condition is harsh, energy consumption is big and yield is low; 3. organic acid and phenol are in catalyst A1C1 3 and dehydrating agent ZnC1 2 Under the condition of room temperature, react for 7~10h
Because phenol itself is difficult to esterify, the carrying out of this reaction is more difficult, and conversion rate is lower; Sodium hydroxide is used as a raw material to synthesize diphenyl terephthalate (DPT) and diphenyl isophthalate (DPI) through interfacial reactions, but the cost of this method is relatively high, and the phase transfer catalyst cannot be recycled and reused
[0006] According to the previous analysis, in order to solve the problems of long reaction process, harsh reaction conditions, low yield and high energy consumption in the synthesis of diphenyl isophthalate, it is necessary to develop a new synthetic method to realize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Under the condition of 5°C, dissolve 0.05mol of isophthaloyl chloride with 100ml of dichloroethane, add to the reactor, then add 0.13mol of sodium phenoxide, stir and react for 12 hours, sample and analyze the reaction liquid isophthalic acid dichloride The content of phenyl ester is 95.66%. The reaction solution is washed with water, separated, solvent distilled, and recrystallized to obtain the finished product of diphenyl isophthalate. The finished product weighs 14.9g, has a purity of 99%, and a yield of 93.7%.

Embodiment 2

[0022] The operating conditions are the same as in Example 1. Dissolve 0.0547 mol of isophthaloyl chloride with 70 ml of ethylene dichloride, add to the reactor, then add 0.121 mol of sodium phenoxide, stir and react for 8 hours, and analyze the isophthalic acid diphenyl The content of the ester is 95.12%. The reaction solution is washed with water, separated, and the solvent is distilled. The finished product of diphenyl isophthalate is obtained without recrystallization. The finished product weighs 16.3g, has a purity of 96.77%, and a yield of 93.7%.

Embodiment 3

[0024] The operating conditions are the same as in Example 2. Dissolve 0.0507 mol of isophthaloyl chloride with 70 ml of dichloroethane, add to the reactor, then add 0.129 mol of sodium phenoxide, heat up to 30° C., stir and react for 5 hours, and take samples for analysis. The content of diphenyl phthalate is 96.11%. The reaction solution is washed with water, separated, and the solvent is distilled. The finished product of diphenyl isophthalate is obtained without recrystallization. The weight of the finished product is 14.8g, the purity is 97.34%, and the yield is 83.75% %.

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of diphenyl isophthalate. The method comprises the steps of: directly reacting sodium salt of phenol with isophthaloyl chloride in dichloroethane as a solvent at the temperature of 5-30 DEG C under stirring for multiple hours, washing reaction liquid with water after reaction is finished, separating, distilling to remove solvent, recrystallizing and the like to obtain a diphenyl isophthalate finished product. The method is a green environment-friendly synthesis method, is high in reaction conversion rate and yield, and simple and convenient in operation of the whole synthesis process.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for synthesizing diphenyl isophthalate. Background technique [0002] The appearance of diphenyl isophthalate is white crystal. It is used in organic synthesis and is one of the monomers of PBT (polybenzothiazole) heat-resistant polymer. It is used as a raw material for aromatic heterocyclic polymers (such as polybenzimidazole, polybenzothiazole and other high-temperature-resistant polymers), and can also be used as a toughener for polyamide engineering plastics and a plasticizer for nylon resins . [0003] Poly2,2′-m-phenylene-5,5′-bisbenzimidazole fibers (PBI for short in English, trade name Togylen). It is a typical heterocyclic polymer heat-resistant fiber. It is mainly used in fields requiring fiber flame retardancy, high temperature resistance, smokeless and low toxicity. It can be used to make protective clothing (fire-fighting clothing, anti-high t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/80C07C67/14
Inventor 张蓉蓉王培兰邹宁芬张帆
Owner CHINA PETROLEUM & CHEM CORP
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