Carboxyethyl phenyl phosphinic acid piperazine polymer and preparation method thereof

A technology based on phosphinic acid and carboxyethyl benzene is applied in the field of carboxyethyl phenyl phosphinic acid piperazine polymer and its preparation, and achieves the effects of simple equipment, low cost and good application prospect.

Inactive Publication Date: 2012-09-05
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, the high-priced organic flame retardant produced by Klein Company is mainly used in the fields of engineering nylon, PBT, and electrical thin electronic circuit boards in my country. The synthesis process is complicated, the cost is high, and the price is high.

Method used

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  • Carboxyethyl phenyl phosphinic acid piperazine polymer and preparation method thereof
  • Carboxyethyl phenyl phosphinic acid piperazine polymer and preparation method thereof
  • Carboxyethyl phenyl phosphinic acid piperazine polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Example 1 In a 250ml three-necked flask equipped with a stirrer and a water separator, pass through nitrogen protection, add 0.1mol carboxyethylphenylphosphinic acid and 0.1mol anhydrous piperazine, add about 40g of water, stir, slowly Raise the temperature until the water evaporates, raise it to 135°C, maintain the temperature for 3 hours, then slowly raise it from 135°C to 160°C for 3 hours, then vacuumize the reaction for 0.5h, cool and solidify, wash the solid with acetone, and then The mixture was filtered with suction, and the filter cake was vacuum-dried to be a white powdery piperazine polymer with carboxyethylphenylphosphinic acid, with a yield of 95%, a melting temperature of 130±5°C, and a decomposition temperature of 200±5°C. ℃.

Embodiment 2

[0038] Example 2 In a 250ml three-necked flask equipped with a stirrer and a water separator, pass through nitrogen protection, add 0.1mol carboxyethylphenylphosphinic acid and 0.095mol anhydrous piperazine, add about 40g of water, stir, slowly Raise the temperature until the water evaporates, raise it to 140°C, maintain the temperature for 2 hours, then slowly raise it from 140°C to 155°C for 2 hours, then vacuumize for 0.5 hours, cool and solidify, dissolve the solid with methanol, add About 8 to 10 times the volume of diethyl ether, milky liquid appears, keep stirring until solid particles appear, then separate liquid and suction filter, and the filter residue is vacuum-dried to become white powder carboxyethylphenyl phosphinic acid piperazine The polymer has a yield of 86%, a melting temperature of 130±5°C, and a decomposition temperature of 200±5°C.

Embodiment 3

[0039] Example 3 In a 250ml three-neck flask equipped with a stirrer and a water separator, nitrogen protection was introduced, 0.1mol carboxyethylphenylphosphinic acid and 0.105mol anhydrous piperazine were added, about 40g of water was added, stirred, and slowly Raise the temperature until the water evaporates, raise it to 135°C, maintain the temperature for 4 hours, then slowly raise it from 135°C to 160°C for 4 hours, then vacuumize for 0.5 hours, cool and solidify, wash the solid with acetone, and then The mixture was filtered with suction, and the filter cake was vacuum-dried to be a white powdery piperazine polymer with carboxyethylphenylphosphinic acid, with a yield of 95%, a melting temperature of 130±5°C, and a decomposition temperature of 200±5°C. ℃.

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Abstract

The invention relates to a carboxyethyl phenyl phosphinic acid piperazine polymer and a preparation method thereof. The structure of the polymer is shown in a formula, wherein n is more than 1. The preparation method comprises the following steps: directly reacting carboxyethyl phenyl phosphinic acid with piperazine in a molar ratio of 1:0.95-1.05 in a nitrogen atmosphere at the temperature of between 135 and 160 DEG C or continuously reacting the carboxyethyl phenyl phosphinic acid with the piperazine in water or an organic solvent for 4 to 8 hours; and removing water generated in the process of reaction, then purifying and drying the reactant to obtain the carboxyethyl phenyl phosphinic acid piperazine polymer. The carboxyethyl phenyl phosphinic acid piperazine polymer has the advantages of high flame resistance, stable physicochemical property, good intermiscibility with high molecular materials, contribution to environmental protection, diversified synthetic method, simple and easily controlled process, simple needed device, low cost and suitability for scale production of different types of enterprises.

Description

technical field [0001] The invention relates to a P-N synergistic flame-retardant halogen-free compound and its preparation process, in particular to a carboxyethylphenylphosphinic acid piperazine polymer and its preparation method. The compound can be used as polyesters, polyamides, Flame retardant for epoxy resin, fiberglass resin, paint (water-soluble, oil-soluble), etc. Background technique [0002] At present, as the global call for flame retardant and halogen-free is getting higher and higher, the halogenated flame retardants that have been recognized for a long time are facing huge challenges, and the green and environmentally friendly phosphorus nitrogen intumescent flame retardants are becoming more and more popular among consumers. Those who favor it, especially organic phosphine flame retardants, because they contain C-P bonds, have high chemical stability, water resistance, solvent resistance, high flame retardancy, low smoke, and low toxicity, and are becoming ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G69/42C07F9/6509
Inventor 王彦林王冬军韩虹
Owner SUZHOU UNIV OF SCI & TECH
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