A kind of polymerized flame retardant integrated with boron, nitrogen and phosphorus and preparation method thereof

A phosphorus flame retardant and polymerized technology, applied in the field of boron-nitrogen-phosphorus-integrated polymerized flame retardant and its preparation, can solve the problems of poor polymer compatibility, great influence on flame retardant efficiency, influence on material mechanical properties, etc. , to achieve the effect of not easy migration, good smoke suppression and wide application range

Active Publication Date: 2018-06-19
LIAONING JINGHUA NEW MATERIAL CO LTD
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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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  • A kind of polymerized flame retardant integrated with boron, nitrogen and phosphorus and preparation method thereof
  • A kind of polymerized flame retardant integrated with boron, nitrogen and phosphorus and preparation method thereof
  • A kind of polymerized flame retardant integrated with boron, nitrogen and phosphorus and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] 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.

[0025] with magnetic stirring, thermometer, N 2 Add 18.15g of pentaerythritol, 33ml of phosphorus oxychloride, 0.1g of 2-methylaminopyridine and 100ml of chlorobenzene into the 250ml three-necked flask of the catheter and reflux condenser (connected with HCl tail gas absorption device), and pass N 2 protection, react at 60°C for 2h, then raise the temperature to 100°...

Embodiment 2

[0028] Wherein the synthetic method of intermediate boric acid diethanolamine ester and dipentaerythritol dichlorophosphate is with example 1.

[0029] In a 250ml three-neck flask equipped with a magnetic stirrer, a thermometer, and a vacuum decompression device, add 23.98g of diethanolamine borate, 32.67g of dipentaerythritol dichlorophosphate and 80ml of acetonitrile, react at 80°C for 1 hour, and then evaporate the solvent under reduced pressure , using the vacuum melting method to react at 160°C for 1 hour. After the reaction, keep the vacuum state to room temperature, and finally grind to obtain a bright yellow powdery solid, wash with 80ml tetrahydrofuran, filter, and dry at 80°C to obtain the flame retardant.

Embodiment 3

[0031] Wherein the synthetic method of intermediate boric acid diethanolamine ester and dipentaerythritol dichlorophosphate is with example 1.

[0032] In a 250ml three-neck flask equipped with a magnetic stirrer, a thermometer, and a vacuum decompression device, add 41.42g of boric acid diethanolamine ester, 50.49g of dipentaerythritol dichlorophosphate and 120ml of acetonitrile, react at 80°C for 2 hours, and then evaporate the solvent under reduced pressure , using the vacuum melting method to react at 180°C for 1 hour. After the reaction, keep the vacuum state to room temperature, and finally grind to obtain a bright yellow powdery solid, wash with 100ml tetrahydrofuran, filter, and dry at 80°C to obtain the flame retardant.

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PUM

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Abstract

A boron, nitrogen and phosphorus-integrated polymerized flame retardant and a preparation method thereof relate to a flame retardant and a preparation method thereof. First, dissolve diethanolamine borate and dipentaerythritol dichlorophosphate with a solvent and put them into a reactor, react at a certain temperature for 1~3 hours, heat to the boiling point of the solvent, and distill the solvent under reduced pressure. Under vacuum conditions, use the melt polymerization method to react at a certain temperature for 1~4h. After the reaction, continue to vacuum until the temperature of the reactor drops to room temperature, and grind to obtain a bright yellow powder. After washing with reagents, filtering, and vacuum drying, you can get flame retardant agent. The boron, nitrogen, and phosphorus flame retardant has good char formation, is halogen-free, and has remarkable flame retardant effect, especially containing three elements of boron, nitrogen, and phosphorus, which not only makes the flame retardant effect better, but also boron element also has smoke suppression effect and reduces flame retardancy. The flame retardant has advantages such as the toxicity of the flame retardant, which makes the flame retardant have a wide range of application values. Can be used for flame retardancy of polyolefin materials. Molecular structure of "boron nitrogen phosphorus integrated" polymeric boron nitrogen phosphorus flame retardant.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a boron, nitrogen and phosphorus-integrated polymerized flame retardant and a preparation method thereof. Background technique [0002] Since entering the 21st century, polymer materials and their products have been more and more vigorously developed and widely used in various fields, but most polymer materials have some fatal shortcomings, such as: easy to burn, and when burned The speed is fast, accompanied by the release of a large amount of toxic gas. According to the statistics of relevant departments, the real culprit that causes a large number of casualties in fire accidents is not the burning of flames, but the suffocation or poisoning caused by the smoke and toxic gases released during the burning of materials. It can be seen that the evaluation of materials is no longer limited to its use and processing performance, but also needs to pay attention t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C07F9/6574C08L63/00C08L23/00C08L85/02C08K5/55
Inventor 梁兵巴明伟
Owner LIAONING JINGHUA NEW MATERIAL CO LTD
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