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Preparation method of tetraphenyl resorcinol bis(diphenylphosphate)

A technology of resorcinol tetraphenyl diphosphate and triphenyl phosphate, which is applied in the field of phosphate preparation, can solve the problems of low activity, long reaction time, and insufficient deactivation resistance of catalysts.

Active Publication Date: 2017-05-10
山东瑞兴阻燃科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with enzyme catalysts and liquid catalysts, solid catalysts, especially solid base catalysts, have the advantages of simple process, less environmental pollution, and easy recycling, but the activity of solid base catalysts is still low, and the reaction time required to achieve a higher conversion rate of glycerin too long; at the same time, the deactivation resistance of the catalyst is not good enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) preparation of solid catalyst

[0019] The well-known D001 macroporous styrene-based ion exchange resin production standard process formula, heating method and reaction time are selected. The difference is: add 2 parts of 6-(2,2-dicyanide to 100 parts of total monomer weight Vinyl)-N-(2-hydroxyethyl)-1,2,3,4-tetrahydroquinoline, add 0.06 parts of 2-[[4-(2,2-dicyanovinyl)-3- Methylphenyl]ethylamino]ethyl-1,4-phthalic acid methyl ester as comonomer, add 0.03 part of 2,4-diphenyl-4-methyl-1-pentene as chain transfer agent , the polymerized white balls are formed through the polymerization reaction, and after drying, the porogen is extracted and dried for use. The solid catalyst can be obtained by carrying out sulfonation reaction according to the known sulfonation process of D001 macroporous cation exchange resin.

[0020] (2) transesterification reaction

[0021] According to parts by weight, 100 parts of triphenyl phosphate and 40 parts of resorcinol are added to ...

Embodiment 2

[0023] (1) Preparation of solid catalyst

[0024] The well-known D201 macroporous styrene-based ion-exchange resin polymerization production standard formula, heating method and reaction time are selected. The difference is: add 0.5 part of 6-(2,2-di Cyanovinyl)-N-(2-hydroxyethyl)-1,2,3,4-tetrahydroquinoline, add 0.01 part of 2-[[4-(2,2-dicyanovinyl)-3 -Methylphenyl]ethylamino]ethyl-1,4-phthalic acid methyl ester as comonomer, add 0.01 part of 2,4-diphenyl-4-methyl-1-pentene for chain transfer agent, polymerized white balls are formed by polymerization reaction, after drying, the porogen is extracted and dried for use. The solid catalyst can be obtained by carrying out sulfonation reaction according to the known sulfonation process of D001 macroporous cation exchange resin.

[0025] (2) transesterification reaction

[0026] According to parts by weight, add 100 parts of triphenyl phosphate and 20 parts of resorcinol into the reactor; the amount of solid catalyst is 5 parts;...

Embodiment 3

[0028] (1) preparation of solid catalyst

[0029] The well-known D001 macroporous styrene-based ion exchange resin production standard process formula, heating method and reaction time are selected. The difference is: add 2 parts of 6-(2,2-dicyanide to 100 parts of total monomer weight Vinyl)-N-(2-hydroxyethyl)-1,2,3,4-tetrahydroquinoline, add 0.1 part of 2-[[4-(2,2-dicyanovinyl)-3- Methylphenyl]ethylamino]ethyl-1,4-phthalic acid methyl ester as comonomer, add 0.05 part of 2,4-diphenyl-4-methyl-1-pentene as chain transfer agent , the polymerized white balls are formed through the polymerization reaction, and after drying, the porogen is extracted and dried for use. The solid catalyst can be obtained by carrying out sulfonation reaction according to the known sulfonation process of D001 macroporous cation exchange resin.

[0030] (2) transesterification reaction

[0031] According to parts by weight, add 100 parts of triphenyl phosphate and 60 parts of resorcinol into the re...

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PUM

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Abstract

The invention provides a preparation method of tetraphenyl resorcinol bis(diphenylphosphate); a solid catalyst with the framework containing heterocyclic groups, such as dicyano and quinoline is used for the preparation of tetraphenyl resorcinol bis(diphenylphosphate), anti-inactivation property of the catalyst is enhanced, the catalyst is reusable, and transesterification yield is increased.

Description

technical field [0001] The invention relates to a preparation method of phosphoric acid ester, in particular to a preparation method of resorcinol tetraphenyl diphosphate. Background technique [0002] With the improvement of people's awareness of environmental protection, halogen-free and low-toxic flame retardants have attracted much attention. At the same time, the scope of use of traditional halogenated flame retardants has become smaller and smaller. Therefore, the development of environmentally friendly, healthy and harmless flame retardants has become an inevitable trend in the development of flame retardants in today's society. Resorcinol-type phosphate oligomer (RDP) flame retardant is a kind of halogen-free additive flame retardant, because of its unique chemical structure and mechanical properties, it shows excellent thermal stability in polymers It has been widely used because of its excellent performance and super flame retardancy. [0003] CN100427494C provid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/12B01J31/10
CPCB01J31/10B01J2231/49C07F9/12
Inventor 王荣军吴健泳
Owner 山东瑞兴阻燃科技有限公司
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