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

A technology of polymers and flame retardants, applied in the field of flame retardants and their preparation, can solve the problems of limited application of washing resistance and stability, and achieve the effects of improving the resistance to washing, simple preparation methods, and environmental protection

Inactive Publication Date: 2013-02-06
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, organoboron flame retardants have problems such as water resistance and stability, which lead to extremely limited applications.

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

[0026] 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.

[0027] In a 250ml three-necked flask equipped with magnetic stirring, dropping funnel and thermometer, add 32.7g of diethanolamine borate and 150ml of dichloromethane, add 29.5g of phenylphosphoryl dichloride in the dropping funnel, and add 20ml of dichloromethane Dilution. After the diethanolamine borate is completely dissolved, start to add phenylphospho...

Embodiment 2

[0030] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0031] In a 250ml four-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add 21.8g of diethanolamine borate and 100ml of acetonitrile, add 19.7g of phenylphosphoryl dichloride in the dropping funnel, dilute it with 10ml of acetonitrile , after the diethanolamine borate is completely dissolved, start to add phenylphosphoryl dichloride dropwise. At this time, the temperature rises, and a white solid is formed. After the dropwise addition, continue to react for 1 hour; then raise the temperature to 100°C and keep it at 100°C After 5 hours, cool to room temperature, filter, wash with 100ml of dichloromethane, filter, and dry at 50°C to obtain a white powder product.

[0032] Add 3.8g of diethanolamine borate and phenylphosphoryl dichloride cocondensate, 1.2g of melamine, 35ml of DMF, and 5ml of pyridine into a three-necked flask with a temperature agent and a r...

Embodiment 3

[0034] Wherein the synthetic method of intermediate diethanolamine borate is with example 1.

[0035] 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 39.4g of phenylphosphoryl dichloride in the dropping funnel, dilute it with 20ml of acetonitrile , after the diethanolamine borate is completely dissolved, start to add phenylphosphoryl dichloride dropwise. At this time, the temperature rises, and a white solid is formed. After the dropwise addition, continue to react for 2 hours; then slowly raise the temperature to 85°C, and keep °C for 10 hours, filtered, washed with 100ml of dichloromethane, filtered, and dried at 50 °C to obtain a white powder product.

[0036] Add 11.4g of diethanolamine borate and phenylphosphoryl dichloride cocondensation product, 2.82g of phenol, 80ml of DMF, and 4.250g of triethylamine into a three-necked flask with a temperature agent and a...

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Abstract

The invention discloses a polymer type phosphorus, nitrogen and boron containing flame retardant and a preparation method thereof, and relates to a flame retardant and a preparation method thereof. The preparation method includes steps of dissolving boronic acid diethanolamine cyclic ester with a solvent and then adding into a reactor, diluting a proportion of phenylphosphonic dichloride with a corresponding solvent and the dripping into the reactor for reacting for 1-3 hours at the temperature of 0-20 DEG C, heating the solution to a reflux temperature, continuing to react for 5-24 hours, removing the solvents, washing and drying to obtain the flame retardant. The prepared phosphorus, nitrogen and boron containing flame retardant is halogen-free, and is good in charring and remarkable in flame retarding effect. As the boron element contained in the flame retardant is capable of suppressing smoke and reducing toxicity of the flame retardant, the flame retardant has the advantages of wide application scope and the like. In addition, the flame retardant can be used for flame retarding for polyethylene and epoxy resin materials; and the preparation method is simple and easy to control. The structural formula of the polymer type phosphorus, nitrogen and boron containing flame retardant is shown as follows.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a polymer-type phosphorus, nitrogen and boron-containing flame retardant and a preparation method thereof. Background technique [0002] my country is one of the countries rich in boron resources in the world. Boron and borides are important chemical raw materials, widely used in industry, agriculture, national defense, medicine and other fields. The application of boron in the field of flame retardant can be traced back to 1735. Obaveasghae in the United Kingdom used aqueous solutions such as borax, alum, and ferric sulfate as textile flame retardant finishing agents. This flame retardant method can greatly reduce the ignition performance and combustibility of fabrics. In addition, sodium calcium borate mixture has also been used as a flame retardant for fighting forest fires for a long time. As one of the earliest flame retardants used, boron-containing fl...

Claims

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Application Information

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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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