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Method of preparing bromine-containing polyphosphate fire retardant with double-spiral structure

A technology of polyphosphate ester and flame retardant, which is applied in the field of phosphorus-bromine synergistic flame retardant and its preparation, can solve the problems of material mechanical properties and mechanical properties degradation, poor use performance, low thermal stability, etc., and achieve easy Narrow control and decomposition range, good thermal stability

Inactive Publication Date: 2007-09-12
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the currently commercialized bromophosphate flame retardants are viscous liquids with high volatility and low thermal stability.
In the application process, there are many defects such as migration, frosting, mechanical properties and mechanical properties of materials, deterioration of performance, etc.

Method used

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  • Method of preparing bromine-containing polyphosphate fire retardant with double-spiral structure
  • Method of preparing bromine-containing polyphosphate fire retardant with double-spiral structure
  • Method of preparing bromine-containing polyphosphate fire retardant with double-spiral structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 500ml of anhydrous acetonitrile, 35.64g (0.12mol) of raw material 1 into a 100ml three-necked flask equipped with a spherical condenser and a stirrer, then add 65.26g (0.12mol) of tetrabromobisphenol A, and add dropwise under stirring 27.6g (0.26mol) of triethylamine, after continuing to stir for 0.5 hours, heated to reflux, reacted for 6 hours, cooled, filtered, washed three times with warm water, and dried to obtain a white solid powder with a yield of 98%.

Embodiment 2

[0024] Add 0.1mol of anhydrous potassium carbonate and 0.1mol of one of the raw materials 2 into a three-necked flask, add the solvent DMAc, reflux with toluene and bring water to form a salt, then cool to 30-35°C, add 0.1mol of raw material 1, and keep at 50-100 The reaction was stirred at °C for 10 hours. Pour into water, wash and dry. A white solid was obtained in 92% yield.

Embodiment 3

[0026] Add 0.09mol of anhydrous potassium carbonate and 0.09mol of one of the raw materials 2 into a three-necked flask, add the solvent DMAc, reflux with toluene with water to form a salt, cool to 30-35°C, add 0.1mol of raw material 1, and keep at 50-100 The reaction was stirred at °C for 8 hours. 0.02 mol of potassium salt of tribromophenol was added, and the reaction was continued for 4 hours. Pour into water, wash and dry. A white solid was obtained in 90% yield.

[0027] [η] a

thermal decomposition temperature b

0.12

0.21

0.33

302℃ c ，330-340℃ d

308℃ c ，340-350℃ d

325℃ c ，365-370℃ d

[0028] Note: a: according to the formula [ η ] = ln t t o c Determination with Ubbelohde viscometer;

[0029] b: TGA / SDTA851 from Mellert, Swede...

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Abstract

The invention relates to phosphorus - bromine flame retardant and its preparation. Its character is that it prepares a polyphosphate containing bromine with a repeating unit structure. The flame retardant obviously has phosphorus - bromine synergy-funciton, See detail on the right. It has a good thermal stability, a high decomposition temperature, a narrow ranged decomposition, as well as characteristics of carbon. It can be used for polyester, polyamide with a high processing temperature.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-bromine synergistic flame retardant and its preparation method. The invention relates to a bromine-containing polyphosphate with a double spiro ring structure and a preparation method thereof. Background technique [0002] With the rapid development of synthetic materials, synthetic plastics, rubber, and fibers are more and more used in various sectors of the national economy and people's production and life, but at the same time, fires caused by ignition of high polymers are also is greatly increasing. Therefore, people have higher and higher requirements for the flame retardancy of synthetic materials. The flame retardant function of synthetic materials is mainly realized by adding flame retardants. Among them, the decomposition temperature of bromine-containing phosphate flame retardants is mostly 200-300 ° C, which matches the decomposition temperature of various polymer materials, so it...

Claims

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Application Information

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IPC IPC(8): C09K21/12C07F9/6571C08K5/521
Inventor 郑玉斌闫莉薛英楠
Owner DALIAN UNIV OF TECH