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A kind of preparation method of intumescent flame retardant

An intumescent flame retardant and the technology of preparation steps, which are applied in the field of preparation of intumescent flame retardants, can solve problems such as poor compatibility and moisture absorption, and achieve the effects of good compatibility, good flame retardant effect, and uniform dispersion

Active Publication Date: 2018-05-08
SHAOXING GOLD SUN TEXTILE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention: for the present intumescent flame retardants due to rich -OH, -NH 2 , -NH 4 + Such as hydrophilic genes, poor compatibility with polymer matrix, and the problem of moisture absorption will also occur on the surface of flame-retardant material products. A preparation method for intumescent flame retardants is provided. The present invention first uses trihydroxyformaldehyde Ethyl ethane is esterified with tea saponin, the esterified product is esterified with phenyl trichloromethane, and finally it is esterified with ammonium polyphosphate to obtain an intumescent flame retardant. Tea saponin contains -OH and -COOH can react with -OH in carbon source trihydroxymethylethane, and can also react with -NH in ammonium polyphosphate 4 + reaction, and phenyltrichlorosilane can not only react with -OH but also with -NH 4 + Reaction, because the reaction is difficult to generate a single compound with a clear structure in one-to-one correspondence between the molecules, and it is more likely to be a cross-linked polymer that is cross-linked and polycondensed between the molecules to form a three-dimensional structure. This type of polymer flame retardant and polymer material It has good compatibility and will not produce moisture absorption on the surface of flame retardant materials, so it can be widely used in polyolefin, polyester, nylon, rubber, ABS, polyamide, epoxy resin, phenolic resin and other high As an additive flame retardant in polymers, it has the characteristics of high efficiency, low toxicity, and smoke-free. It is a new type of flame retardant that meets environmental protection requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0015] First, measure 300mL of absolute ethanol and add it to a three-necked flask equipped with a condenser tube and a thermometer, place it in an oil bath, add 10g of trihydroxymethylethane and 3g of tea saponin to the flask in sequence, and control the temperature at 95°C , adding 5mL mass concentration of 98% concentrated sulfuric acid to the flask at a speed of 2mL / min, magnetically stirred for 2h to obtain tea saponin trihydroxymethylethane ester; Add 3g of phenyltrichlorosilane, control the temperature at 95°C, stir and react for 2 hours, wet the pH test paper with water, and then penetrate into the top of the reaction solution in the flask until the pH test paper shows neutrality, stop the reaction, and obtain organosilane modified tea Saponin trihydroxymethylethane ester; add 3g ammonium polyphosphate to the above organosilane-modified tea saponin trihydroxymethylethane ester, control the temperature of the oil bath at 90°C, and pour it into the flask at a speed of 2mL...

example 2

[0018]First, measure 350mL of absolute ethanol and add it to a three-necked flask equipped with a condenser tube and a thermometer and place it in an oil bath. Then add 15g of trihydroxymethylethane and 4g of tea saponin to the flask, and control the temperature at 100°C. Add 8mL mass concentration of 98% concentrated sulfuric acid to the flask at a speed of 2mL / min, and react with magnetic stirring for 2.5h to obtain tea saponin trihydroxymethylethane ester; Add 4g of phenyltrichlorosilane, control the temperature at 100°C, stir and react for 2.5 hours, wet the pH test paper with water and penetrate into the reaction solution in the flask until the pH test paper shows neutrality, stop the reaction, and obtain organosilane modified Tea saponin trihydroxymethylethane ester; add 4g ammonium polyphosphate to the above organosilane modified tea saponin trihydroxymethylethane ester, control the oil bath temperature at 95°C, add 2mL / min to the flask Add 8 mL of concentrated sulfuric...

example 3

[0021] First, measure 400mL of absolute ethanol and add it to a three-neck flask equipped with a condenser tube and a thermometer, place it in an oil bath, add 20g of trihydroxymethylethane and 5g of tea saponin to the flask in sequence, and control the temperature at 105°C , add 10mL mass concentration of 98% concentrated sulfuric acid to the flask at a speed of 2mL / min, and react with magnetic stirring for 3h to obtain tea saponin trihydroxymethylethane ester; Add 5g of phenyltrichlorosilane, control the temperature at 60°C, stir and react for 3 hours, wet the pH test paper with water, and then penetrate into the flask above the reaction solution until the pH test paper shows neutrality, stop the reaction, and obtain organosilane modified tea Saponin trihydroxymethylethane ester; add 5g ammonium polyphosphate to the above organosilane-modified tea saponin trihydroxymethylethane ester, control the temperature of the oil bath at 100°C, and add 5g of ammonium polyphosphate to th...

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Abstract

The invention discloses a preparation method of an intumescent flame retardant, and belongs to the technical field of synthesis of flame retardants. Firstly, trihydroxy methyl-hexane and tea saponin are esterified, an esterified product is then esterified with phenyl trichloromethane, finally, the product and ammonium polyphosphate are subjected to esterification reaction to obtain the intumescent flame retardant, the tea saponin contains -OH and -COOH which can react with -OH in the trihydroxy methyl-hexane of a carbon source, and can further react with -NH4+ in the ammonium polyphosphate, the phenyl trichloromethane not only can react with -OH, but also can react with -NH4+, single compounds which have clear structures are difficultly produced among molecules by reaction in a one-to-one correspondence manner, more possibly, components are cross-linked with one another among the molecules and are condensed into cross-linked polymers which have three-dimensional structures, and the polymer flame retardant is well compatible to a high polymer material. The intumescent flame retardant has the features of high efficiency, low toxicity, zero smoke and the like, and is a novel flame retardant which meets the requirement of environmental protection.

Description

technical field [0001] The invention relates to a preparation method of an intumescent flame retardant, belonging to the technical field of flame retardant synthesis. Background technique [0002] With the development of society, polymer materials are widely used in industrial production and people's daily life. High-rise buildings, interior decoration, electrical appliances, automobiles, and conveyor belts in underground coal mines all have polymer materials. However, most polymer materials have a fatal shortcoming, that is, they are easy to decompose and burn at high temperatures. Most of their oxygen index is less than 21, so as long as they encounter a fire source, most polymer materials will ignite in the air and then burn, and their molten droplets can also ignite other combustibles, causing the fire to spread. , The poisonous gas and black smoke released by thermal decomposition of polymer materials when they are burned have caused great threats and harm to people's ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L63/00C08L87/00C08K7/14C08K5/5317C08K5/5435
CPCC08L63/00C08L2201/02C08L87/00C08K7/14C08K5/5317C08K5/5435C08K5/0066
Inventor 曹思珂
Owner SHAOXING GOLD SUN TEXTILE CO LTD
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