Carboxyethyl phenyl phosphinic acid piperazine polymer and preparation method thereof

A technology based on phosphinic acid and carboxyethylbenzene, which is applied in the field of carboxyethylphenylphosphinic acid piperazine polymer and its preparation, can solve the problems of high cost, complex synthesis process and high price, and achieve cost Inexpensive, good compatibility, good for environmental protection

Inactive Publication Date: 2010-07-14
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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

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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Example Embodiment

[0035] Example 1 In a 250ml three-necked flask equipped with a stirrer and a water separator, nitrogen protection was introduced, 0.1 mol carboxyethyl phenyl phosphinic acid and 0.1 mol anhydrous piperazine were added, and about 40 g of water was added, stirring, slowly Raise the temperature until the water evaporates and then rise to 135℃. After maintaining the temperature for 3 hours, slowly increase from 135℃ to 160℃ and react for 3h, then vacuum and react for 0.5h, cool and solidify, and wash the solid with acetone. The mixture is suction filtered, and the filter cake is vacuum-dried into a white powdery carboxyethyl phenyl phosphinic acid piperazine polymer. The yield is 95%, the melting temperature is 130±5°C, and the decomposition temperature is 200±5 ℃.

Example Embodiment

[0036] Example 2 In a 250ml three-necked flask equipped with a stirrer and a water separator, nitrogen protection was introduced, 0.1 mol carboxyethyl phenyl phosphinic acid and 0.095 mol anhydrous piperazine were added, and about 40 g of water was added, stirring, slowly Raise the temperature until the water evaporates and rise to 140°C. After maintaining the temperature for 2 hours, slowly increase from 140°C to 155°C and react for 2 hours, then vacuum and react for 0.5 hours. Cool and solidify. After the solid is dissolved in methanol, add Approximately 8 to 10 times the volume of ether, a milky liquid appears, keep stirring until solid particles appear, then separate liquids and suction filtration. After the filter residue is vacuum-dried, the white powdery carboxyethylphenylphosphinate piperazine is obtained. The polymer has a yield of 86%, a melting temperature of 130±5°C, and a decomposition temperature of 200±5°C.

Example Embodiment

[0037] Example 3 In a 250ml three-necked flask equipped with a stirrer and a water separator, nitrogen protection was introduced, 0.1 mol of carboxyethyl phenyl phosphinic acid and 0.105 mol of anhydrous piperazine were added, and about 40 g of water was added, stirring, slowly Raise the temperature until the water evaporates and then rise to 135℃. After maintaining the temperature for 4h, slowly increase from 135℃ to 160℃ for 4h, then vacuum and react for 0.5h, cool and solidify, and wash the solid with acetone. The mixture is suction filtered, and the filter cake is vacuum-dried into a white powdery carboxyethyl phenyl phosphinic acid piperazine polymer. The yield is 95%, the melting temperature is 130±5°C, and the decomposition temperature is 200±5 ℃.

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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 or equal to 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 t...

Claims

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Application Information

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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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