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Synthetic method of diphenyl iso-phthalate

A technology of diphenyl isophthalate and a synthesis method, which is applied in the field of synthesis of diphenyl isophthalate, can solve the problems of large environmental pollution, uneconomical application, and high cost of phenol-containing wastewater treatment, and overcome product belts. Color, overcoming the effect of incomplete reaction

Active Publication Date: 2013-12-18
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the quality and cost of the product, it is uneconomical to apply mechanically; and the phenol-containing wastewater is very polluting to the environment. The country has strict restrictions on the content of phenol in the sewage discharged from the factory: ≤2.0mg / L, and the treatment of phenol-containing wastewater higher cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 203g of isophthaloyl chloride and 200ml of anhydrous cyclohexane into a 1000ml reaction bottle, and dissolve for later use. In a 2000ml stirred four-neck reaction flask, add 100g of phenol, 1000ml of cyclohexane water azeotrope, and 1.0g of benzyltriethylammonium chloride. Start stirring, add the acid chloride solution dropwise at 10°C, continue to stir for 2 hours after dropping, then raise the temperature to reflux for 3 hours, take a sample for detection, and the reaction is over. The cyclohexane water azeotrope 950ml and 215ml of anhydrous cyclohexane recovered under normal pressure were respectively used in the next batch of production. After vacuum distillation, 312.37g of diphenyl isophthalate was obtained, and the gas chromatography content was 99.83%. The yield is 98.14%.

Embodiment 2

[0023] Add 203g of isophthaloyl chloride and 200ml of anhydrous cyclohexane into a 1000ml reaction bottle, and dissolve for later use. In a 2000ml stirred four-neck reaction flask, 100g of phenol, 500ml of cyclohexane water azeotrope recovered in Example 1, and 0.4g of benzyltriethylammonium chloride were added. Start stirring, add the acid chloride solution dropwise at 25°C, continue stirring for 4 hours after the drop is complete, then raise the temperature to reflux for 2 hours, and take a sample for detection. After the reaction was completed, 468ml of the cyclohexane water azeotrope recovered under normal pressure and 210ml of anhydrous cyclohexane were distilled under reduced pressure to obtain 314.09g of diphenyl isophthalate with a gas chromatography content of 99.52% and a yield of 98.68%.

Embodiment 3

[0025] Add 203g of isophthaloyl chloride and 200ml of anhydrous cyclohexane into a 1000ml reaction bottle, and dissolve for later use. In a 2000ml stirred four-necked reaction flask, 100g of phenol, 300ml of cyclohexane water azeotrope recovered in Example 1, and 0.2g of tetraethylammonium bromide were added. Start stirring, add the acid chloride solution dropwise at 15°C, continue stirring for 3 hours after dropping, then raise the temperature to reflux for 6 hours, and take samples for detection. After the reaction was completed, 270ml of the cyclohexane water azeotrope recovered under normal pressure and 208ml of anhydrous cyclohexane were distilled under reduced pressure to obtain 312.00g of diphenyl isophthalate with a gas chromatography content of 99.71% and a yield of 98.02%.

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Abstract

The invention belongs to the field of fine chemical engineering and relates to a synthetic method of diphenyl iso-phthalate. Under the catalytic effect of double catalysts, isophthaloyl dichloride and phenol are subjected to reaction, the reduced pressure distillation is carried out, and high-purity diphenyl iso-phthalate is obtained. Under the catalytic effect of the double catalysts, the isophthaloyl dichloride and the phenol take reaction, the reduced pressure distillation is carried out, and the high-purity diphenyl iso-phthalate is obtained. The synthetic method has the advantages that the adverse influence on the next step polymerization reaction caused by free acid groups because of reaction incompletion in the direct esterification method is avoided; the problem of product coloring in an ester exchange method is also solved; and meanwhile, the problem of treatment difficulty of phenol-containing wastewater generated in the traditional phase transfer catalysis method is also solved. The synthetic method is safe and environment-friendly and is suitable for industrial production. The diphenyl iso-phthalate prepared by the synthetic method has the advantages that the chromatographic content is higher than 99.5 percent, and the average yield is higher than 98 percent.

Description

technical field [0001] The invention belongs to the field of fine chemicals and relates to a method for synthesizing diphenyl isophthalate. Background technique [0002] Diphenyl isophthalate can be used in organic synthesis, as a plasticizer for nylon resins, as a toughening agent for polyamide engineering plastics, and as an aromatic heterocyclic high-temperature-resistant polymer (such as polyphenylene And imidazole, polybenzothiazole, etc.) one of the monomers of PBT. PBT has good thermal oxidation stability, toughness, fatigue resistance, acid and alkali resistance, extremely low water absorption, good electrical insulation, and certain self-lubricating engineering plastics. It is mainly used in automobiles, electronic appliances, Instrumentation, aerospace technology pressure valves and space structure frames, etc. In the "High-tech Fields Supported by the State" issued by the Ministry of Science and Technology in 2008, the "Key Polymer Monomer Manufacturing Technolo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/80C07C67/14
Inventor 张善民孙丰春张振霞薛居强李文娟
Owner SHANDONG KAISHENG NEW MATERIALS
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