Polymer type boron-containing flame retardant and preparation method thereof

A technology of flame retardants and polymers, applied in the field of flame retardants and their preparation, can solve the problems of poor washing resistance and achieve the effects of not easy migration, excellent durability, and easy control

Inactive Publication Date: 2014-04-09
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, organoboron compounds have poor washing resistance due to hydrolytic instability, which limits their application to a certain extent.

Method used

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  • Polymer type boron-containing flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 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.

[0026] In a 250ml three-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add 32.7g of diethanolamine borate and 150ml of dichloromethane, add 22.9g of phosphorus oxychloride in the dropping funnel, dilute with 20ml of dichloromethane After the diethanolamine borate is completely dissolved, the phosphorus oxychloride is added dro...

Embodiment 2

[0029] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0030] In the 250ml four-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, add diethanolamine borate 21.8g and 100ml acetonitrile, add 15.3g phosphorus oxychloride in the dropping funnel, it is diluted with 10ml acetonitrile, After the diethanolamine borate is completely dissolved, start to add phosphorus oxychloride dropwise. At this time, the temperature rises and a white solid is formed. After the addition, continue to react for 1 hour; then raise the temperature to 100°C and keep it at 100°C for 5 hours. , cooled to room temperature, filtered, washed with 100ml of dichloromethane, filtered, and dried at 50°C to obtain a white powder product.

[0031] Add 3.3g of diethanolamine borate and phosphorous oxychloride cocondensate, 1.2g of melamine, 35ml of DMF, and 5ml of pyridine into a three-neck flask with a temperature agent and a reflux condenser, hea...

Embodiment 3

[0033] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0034] In the 500ml four-necked bottle equipped with magnetic stirring, dropping funnel and thermometer, add diethanolamine borate 43.6g and 200ml acetonitrile, add 30.6g phosphorus oxychloride in the dropping funnel, it is diluted with 20ml acetonitrile, After the diethanolamine borate is completely dissolved, start to add phosphorus oxychloride dropwise. At this time, the temperature rises, and a white solid is formed. After the addition, continue to react for 2 hours; then slowly raise the temperature to 85°C, and keep 85°C for reaction After 10 hours, filter, wash with 100ml of dichloromethane, filter, and dry at 50°C to obtain a white powder product.

[0035] Add 10.0g of diethanolamine borate and phosphorus oxychloride cocondensation polymer, 2.82g of phenol, 80ml of DMF, and 4.250g of triethylamine into a three-necked flask with a temperature agent and a reflux condenser, and ...

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Abstract

The invention relates to a flame retardant and a preparation method thereof, in particular to a polymer type boron-containing flame retardant and a preparation method thereof; the method comprises the steps of: firstly, dissolving diethanolamine borate by solvent and then adding the solution into a reactor; diluting phosphorus oxychloride with a certain ratio by corresponding solvent and dripping the diluent into the reactor, and carrying out a reaction at the lower temperature for 1-3 hours; after that, heating up to the reflux temperature, and continuously reacting for 3-18 hours; and removing the solvent, washing and drying to obtain the flame retardant. The flame retardant contains P, N and B, and is good in charring property and remarkable in inflaming retarding effect; the flame retardant contains the B element, thus inhibiting smoke and reducing the toxicity of the flame retardant; and the flame retardant has the characteristics of being wide in application scope and the like. The flame retardant can be used for inflaming retarding polyolefins and epoxy resin material. The preparation method provided by the invention is simple and easy to contain. The flame retardant containing P, N and B has the following structure shown in the specification.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a polymer type boron-containing flame retardant and a preparation method thereof. Background technique [0002] In recent years, due to the frequent occurrence of fire accidents, especially in public places, once a fire breaks out, it will not only cause heavy casualties, but also cause property losses, which will have a serious impact on society. According to the statistical analysis of fire data in major countries in the world in recent years, the incidence of fire and the losses caused by fire are still on the rise. The direct economic loss of fire in industrialized countries is 0.1% to 0.2% of the gross national product. The indirect economic loss can sometimes reach the national level. 1% of GDP. Therefore, the prevention of fire has become an important issue of concern at present, and people have begun to study various flame-retardant and fire-resistant...

Claims

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Application Information

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