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Preparation method of organic silicon-phosphorus synergistic flame retardant

A synergistic flame retardant and silicone technology, applied in the field of flame retardants, can solve problems such as inability to effectively exert the flame retardant effect, excessive addition of flame retardants, poor compatibility between flame retardants and substrates, and achieve The effect of improving synthesis efficiency, improving affinity, and enhancing flame retardant effect

Active Publication Date: 2018-12-21
德清顾舒家华高分子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the fact that the flame retardant contains halogen elements in the prior art, which is harmful to the environment and the human body. At the same time, the compatibility between the flame retardant and the base material is poor, and the flame retardant effect cannot be effectively exerted. As well as the problem of excessive addition of flame retardants, an organosilicon-phosphorus synergistic flame retardant that does not contain halogen elements, has good compatibility between flame retardants and substrates, and can effectively reduce the amount of additions is provided. The preparation method of the agent

Method used

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  • Preparation method of organic silicon-phosphorus synergistic flame retardant

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Embodiment 1

[0031] A preparation method of an organosilicon-phosphorus synergistic flame retardant, said preparation method comprising the following steps:

[0032] (1) Preparation of polyhydrogen silsesquioxane: trichlorosilane is hydrolyzed in an aqueous solution under the action of a catalyst to obtain polyhydrogen silsesquioxane. The specific steps are as follows:

[0033] (1.1) Preliminary condensation: Add 100 parts of chloroform, 1 part of catalyst and 15 parts of distilled water into the reaction kettle, then stir the solution at high speed to form an emulsion, then lower the temperature to -20°C, and slowly add trichlorosilane dropwise 20 parts, after the dropwise addition, the temperature was raised to room temperature, and the stirring reaction was continued for 8 hours;

[0034] (1.2) Hydrochloric acid removal: then add 15 parts of triethylamine therein, continue to react for 2 hours, stop reaction then, filter and remove the triethylamine hydrochloride salt that reaction gene...

Embodiment 2

[0040] A preparation method of an organosilicon-phosphorus synergistic flame retardant, said preparation method comprising the following steps:

[0041] (1) Preparation of polyhydrogen silsesquioxane: trichlorosilane is hydrolyzed in an aqueous solution under the action of a catalyst to obtain polyhydrogen silsesquioxane. The specific steps are as follows:

[0042] (1.1) Preliminary condensation: Add 100 parts of chloroform, 5 parts of catalyst and 15 parts of distilled water into the reaction kettle, then stir the solution at high speed to form an emulsion, then lower the temperature to -20°C, and slowly add trichlorosilane dropwise 35 parts, after the dropwise addition, the temperature was raised to room temperature, and the stirring reaction was continued for 12 hours;

[0043] (1.2) Hydrochloric acid removal: then add 15 parts of triethylamine therein, continue to react for 5 hours, stop reaction then, filter and remove the triethylamine hydrochloride salt that reaction ge...

Embodiment 3

[0049] A preparation method of an organosilicon-phosphorus synergistic flame retardant, said preparation method comprising the following steps:

[0050] (1) Preparation of polyhydrogen silsesquioxane: trichlorosilane is hydrolyzed in an aqueous solution under the action of a catalyst to obtain polyhydrogen silsesquioxane. The specific steps are as follows:

[0051] (1.1) Preliminary condensation: Add 100 parts of chloroform, 3 parts of catalyst and 15 parts of distilled water into the reaction kettle, then stir the solution at high speed to form an emulsion, then lower the temperature to -20°C, and slowly add trichlorosilane dropwise 30 parts, after the dropwise addition, the temperature was raised to room temperature, and the stirring reaction was continued for 10 hours;

[0052] (1.2) Hydrochloric acid removal: then add 15 parts of triethylamine therein, continue to react for 3 hours, stop reaction then, filter and remove the triethylamine hydrochloride salt that reaction ge...

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Abstract

The invention relates to the field of flame retardants, in particular to a preparation method of an organic silicon-phosphorus synergistic flame retardant. The preparation method comprises the following steps: (1) preparing polyhydroxy silsesquioxane: performing hydrolytic reaction on trichlorosilane in an aqueous solution in the presence of a catalyst to obtain the polyhydroxy silsesquioxane; (2)performing phosphate esterification: enabling the polyhydroxy silsesquioxane and phosphate to have condensation reaction under the catalysis of pentafluorophenyl borane to obtain phosphate esterifiedpolyhydroxy silsesquioxane; (3) performing grafting reaction: mixing the phosphate esterified polyhydroxy silsesquioxane and a silane coupling agent, and performing hydrolysis to obtain the organic silicon-phosphorus synergistic flame retardant. The preparation method has the following advantages: (1) the silicon and phosphorus are synergistic to resist the flame, so that the flame-retardant effect of the flame retardant can be effectively improved; (2) the flame retardant contains no halogen element, so that no harm is caused to the environment; and (3) while the high flame-retardant efficiency is ensured, the synthetic cost of the flame retardant can be effectively reduced.

Description

technical field [0001] The invention relates to the field of flame retardants, in particular to a method for preparing an organosilicon-phosphorus synergistic flame retardant. Background technique [0002] Polyurethane foam is made of isocyanate and hydroxyl compound through polymerization and foaming. According to its hardness, it can be divided into two types: soft and hard, of which soft is the main variety. Generally speaking, it has excellent elasticity, softness, elongation and compressive strength; good chemical stability, resistance to many solvents and oils; excellent abrasion resistance, 20 times larger than natural sponge; and excellent processing It is a kind of cushioning material with excellent performance, but the price is relatively high. [0003] Polyurethane foam generally improves the flame retardancy of the foam by adding flame retardants to delay burning, block smoke and even self-extinguish the burning part. Polyols containing flame retardant elements...

Claims

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Application Information

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IPC IPC(8): C08G77/398C08G77/395C08G77/04C08L75/04C08L83/08
CPCC08G77/045C08G77/395C08G77/398C08L75/04C08L2201/02C08L2203/14C08L83/08
Inventor 卢伟蔡盼盼
Owner 德清顾舒家华高分子材料有限公司
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