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Polymer type phosphorus, nitrogen and boron containing flame retardant and preparation method thereof

A technology for polymers and flame retardants, applied in the field of chemical synthesis agents and their preparation, can solve the problems of poor polymer compatibility, great influence on flame retardant efficiency, influence on mechanical properties of materials, etc. Washable, environmentally friendly effect

Inactive Publication Date: 2014-07-02
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the boron-containing compounds reported above all have hydrolytic instability, which has a greater impact on the flame retardant efficiency, and secondly, poor compatibility with polymers, which also has a greater impact on the mechanical properties of the material.

Method used

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  • Polymer type phosphorus, nitrogen and boron containing flame retardant and preparation method thereof
  • Polymer type phosphorus, nitrogen and boron containing flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 12.366g (0.2mol) of boric acid, 46.26g (0.44mol) of diethanolamine and 70ml of toluene into a three-necked flask equipped with magnetic stirring, thermometer, and oil-water separator, heat, stir and reflux until the separated water reaches 10.6ml to end the reaction. The toluene was distilled off under reduced pressure to obtain a light yellow transparent viscous liquid. Excess diethanolamine was removed by washing with tetrahydrofuran. Vacuum drying at 50°C gave 37.20 g of a colorless transparent viscous liquid with a yield of 85.30%. Its purity is 98.83% by titration with 0.1mol / L hydrochloric acid solution.

[0028] In the 250ml four-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, add diethanolamine borate 32.7g and 150ml methylene chloride, add 26.9g phenyl phosphorus dichloride in the dropping funnel, use it Dilute with 20ml of dichloromethane. After the diethanolamine borate is completely dissolved, start to add phenylphosphor...

Embodiment 2

[0031] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0032] In a 250ml four-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, add 21.8g of diethanolamine borate and 100ml of acetonitrile, add 17.9g of phenylphosphorous dichloride in the dropping funnel, and dissolve it with 10ml of acetonitrile Dilute, after the diethanolamine borate is completely dissolved, start to add phenylphosphorous dichloride dropwise, at this time, the temperature rises, and a white solid is formed, continue to react for 1 hour after the dropwise addition; then slowly raise the temperature to 100°C, Keep the reaction at 100°C for 5 hours, cool to room temperature, filter, wash with 100ml of dichloromethane, filter, and dry at 50°C to obtain a white powder product.

[0033] Add 3.6g of diethanolamine borate and phenylphosphorus dichloride co-condensation polymer, 1.2g of melamine, 35ml of DMF, and 5ml of pyridine into a three-necked...

Embodiment 3

[0035] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0036] In a 500ml four-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, add 43.6g of diethanolamine borate and 200ml of acetonitrile, add 35.8g of phenylphosphine dichloride in the dropping funnel, and dissolve it with 20ml of acetonitrile Dilute, after the diethanolamine borate is completely dissolved, start to add phenylphosphorous dichloride dropwise, at this time, the temperature rises, and a white solid is formed, continue to react for 2 hours after the addition; then slowly raise the temperature to 85°C, Keep the reaction at 85°C for 12 hours, filter, take out the solid, wash with 100ml of dichloromethane, filter, and dry at 50°C to obtain a white powder product.

[0037] Add 10.8g of diethanolamine borate and phenylphosphorus dichloride co-condensation polymer, 2.82g of phenol, 80ml of DMF, and 4.250g of triethylamine into a three-necked flask wi...

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Abstract

The polymer-type phosphorus-, nitrogen- and boron-containing flame retardant and its preparation method relate to a chemical synthesis agent and its preparation method. First, the boric acid diethanolamine ester is dissolved in a solvent and added to a reactor, and a certain proportion of phenyl Phosphorus dichloride was diluted with corresponding solvent and added dropwise to the reactor, after reacting at 0~20°C for 1~3h, heated to reflux temperature and continued to react for 3~24h, the solvent was removed, washed and dried, and the obtained The product is end-capped to remove the halogen in the end group. The prepared flame retardant containing phosphorus, nitrogen, and boron is halogen-free, has good char formation, and has a remarkable flame-retardant effect. The boron element contained not only has a smoke-suppressing effect but also The toxicity of the flame retardant is reduced, and it has wide application value. It can be used for flame retardant of polyolefin and epoxy resin materials. Molecular structure of polymeric phosphorus, nitrogen and boron flame retardants:.

Description

technical field [0001] The invention relates to a chemical synthesis agent and a preparation method thereof, in particular to a polymer type flame retardant containing phosphorus, nitrogen and boron and a preparation method thereof. Background technique [0002] In recent decades, with the vigorous development of polymer materials and their products, they are gradually replacing natural polymers such as traditional steel, metal, cement and wood wool. It is widely used in various sectors of the national economy such as industry, agriculture, military affairs, and transportation. However, it is well known that most polymer materials are flammable and flammable, and when burned, more polymers or difficult-to-decompose substances will be decomposed to produce more combustibles, causing fires and endangering people's lives and property. In order to solve the problem of heat resistance of polymer materials, flame retardants have become a hot research topic in the scientific and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L85/02C08G79/02C08K5/55C07F9/6596
Inventor 梁兵朱明曹俊王长松宁志高
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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