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Boron, nitrogen and phosphorus flame retardant and preparation method thereof

A phosphorus flame retardant and flame retardant technology, applied in the field of flame retardants and their preparation, to achieve the effects of environmental protection, good smoke suppression effect, and excellent durability

Inactive Publication Date: 2017-05-10
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This year, as many foreign countries have formulated a series of flame retardant specifications for the flame retardancy of materials, my country has paid more and more attention to this, but the synthesis and application of borate flame retardants in my country are still in the development stage.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 12.366g of boric acid, 46.26g of diethanolamine and 70ml of toluene into a three-necked flask equipped with magnetic stirring, thermometer, oil-water separator and reflux condenser, stir and heat to 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 80°C gave a colorless transparent viscous liquid with a yield of 86.8%. Its purity is 98.98% by titration with 0.1mol / L hydrochloric acid solution.

[0024] In a 250ml three-neck flask equipped with magnetic stirring, thermometer, and reflux condensing device, add 21.8g diethanolamine borate, 13.75g phosphorus trichloride and 100ml acetonitrile, first completely dissolve diethanolamine borate with acetonitrile and put it into the reactor In this method, add phosphorus trichloride dropwise at 10°C and react for 1 ho...

Embodiment 2

[0026] Wherein the synthetic method of intermediate boric acid diethanolamine ester is with example 1.

[0027] In a 250ml three-necked flask equipped with magnetic stirring, a thermometer, and a reflux condensing device, add 43.6g of boric acid diethanolamine ester, 28.88g of phosphorus trichloride and 120ml of acetonitrile, first completely dissolve the boric acid diethanolamine ester with acetonitrile and then put it into the reactor In 15°C, phosphorus trichloride was added dropwise and reacted for 1 hour, heated to the reflux temperature of acetonitrile, reacted for 10 hours, finished the reaction and cooled to room temperature, evaporated to remove acetonitrile under normal pressure, and obtained a white powdery solid after washing with dichloromethane, namely For flame retardants.

Embodiment 3

[0029] Wherein the synthetic method of intermediate boric acid diethanolamine ester is with example 1.

[0030] In a 250ml three-necked flask equipped with magnetic stirring, a thermometer, and a reflux condensing device, add 43.6g of boric acid diethanolamine ester, 27.5g of phosphorus trichloride and 120ml of dichloromethane, first completely dissolve the boric acid diethanolamine ester with dichloromethane Put it into the reactor, add phosphorus trichloride dropwise at 15°C, react for 3 hours, heat to the reflux temperature of dichloromethane, react for 12 hours, finish the reaction and cool to room temperature, remove dichloromethane by atmospheric pressure evaporation, wash with dichloromethane Finally, a white powdery solid is obtained, which is a flame retardant.

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PUM

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Abstract

The invention discloses a boron, nitrogen and phosphorus flame retardant and a preparation method thereof, and relates to a chemical synthesis agent and a preparation method thereof. The preparation method comprises the following steps: completely dissolving diethanolamine borate with a solvent, putting the dissolved diethanolamine borate into a reactor, dropwise adding phosphorus trichloride at the temperature of 0 to 20 DEG C for reaction for 1 to 3 hours, heating to solvent reflux temperature, carrying out reaction for 8 to 15 hours, cooling to room temperature after the reaction is ended, carrying out evaporation at normal pressure to remove the solvent, and washing with a reagent to obtain a white powdered solid which is the flame retardant. The boron, nitrogen and phosphorus flame retardant is high in char forming property, halogen-free and outstanding in flame retarding effect; particularly contains three elements, namely boron, nitrogen and phosphorus, the flame retardant is better in the flame retarding effect; furthermore, the boron element also has the advantages of inhibiting smoke, reducing toxicity of the flame retardant and the like, so that the flame retardant has a wide application value. The flame retardant can be used for flame retarding of a polyolefins material. The molecular structure of the novel boron, nitrogen and phosphorus flame retardant is as shown in the specification.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a boron nitrogen phosphorus flame retardant and a preparation method thereof. Background technique [0002] Boron-based flame retardants are also one of the flame retardants that have been used in the early days, and there are many varieties of inorganic flame retardants. Boron-based flame retardants can be divided into two types: organic boron-based and inorganic boron-based. It has the advantages of good thermal stability, low toxicity and smoke suppression, and has a good compounding effect with other flame retardants. It has a very good development prospect. In recent years, with the continuous introduction of new environmental protection requirements and regulations, boron-based flame retardants are attracting more and more attention due to their excellent characteristics, and have become one of the most active research hotspots in the field of flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/02C08K5/55C07F9/06
CPCC08G79/02C07F9/06C08K5/55
Inventor 梁兵巴明伟
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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