Preparing method of phosphorus based silane flame retardant

A technology of flame retardant and silane, applied in the field of preparation of phosphorus-based silane flame retardant, can solve the problems of high cost, unfavorable personal safety of experimenters, long reaction period, etc. Effect

Inactive Publication Date: 2017-08-11
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has strict requirements, high cost, and long reaction cycle; at the same time, tetramethylammonium hydroxide is easy to decompose and produce toxic gas when heated, which is not conducive to the personal safety of experimenters.

Method used

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  • Preparing method of phosphorus based silane flame retardant
  • Preparing method of phosphorus based silane flame retardant
  • Preparing method of phosphorus based silane flame retardant

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preparation example Construction

[0022] A preparation method of a phosphorus-based silane flame retardant, using organosilicon oligomers and aminosiloxanes as raw materials, and using a mixture of reaction auxiliary agent A and reaction auxiliary agent B as a reaction auxiliary agent, and reacting to obtain phosphorus-based silane flame retardants. Combustion agent; Wherein, reaction auxiliary agent A is trimethylsilanol, trimethylsiliconate or tetrakis (trimethylsilyl) silane; Reaction auxiliary agent B is hexamethyldisilazane or bis(trimethylsilazane) Silicon base) amino salt; the molar ratio of reaction auxiliary agent A to reaction auxiliary agent B is (0.04-10):1. Wherein the trimethylsiliconate is sodium trimethylsiliconate, potassium trimethylsiliconate or lithium trimethylsiliconate. The bis(trimethylsilyl)amide salt is sodium bis(trimethylsilyl)amide, lithium bis(trimethylsilyl)amide or potassium bis(trimethylsilyl)amide.

[0023] Preferably, the reaction temperature of the silicone oligomer and ami...

Embodiment 1

[0028] Preparation of DVN

[0029] In a 500ml three-neck round bottom flask, 5mol of organosilicon oligomer (DOPO-VMDMS) and 10mol of aminosiloxane (NMDMS) were added in different proportions. First add 0.25mol trimethylsilanol, then slowly add 0.5mol bis(trimethylsilyl) lithium amide, continue to stir and react for 12 hours, carry out classification filtration to the reaction system according to molecular weight, obtain unreacted raw materials, Lithium salt, water, a small amount of lithium bis(trimethylsilyl)amide, and DVN; DVN is a slightly yellow translucent solid at room temperature, and the yield is about 96%. The reaction temperature was 35°C.

[0030] Reaction phenomenon: During the reaction process, before the addition of bis(trimethylsilyl)amide lithium, there is no change, and when bis(trimethylsilyl)amide lithium is added, heat is gradually generated, and the color of the reaction solution gradually turns yellow.

[0031] Wherein, in this embodiment, the reaction...

Embodiment 2

[0034] The difference from the example is that 0.25 mol of trimethylsilanol is replaced by 0.25 mol of trimethylsiliconate. In this embodiment, when trimethylsiliconate is used, the molar ratio of trimethylsiliconate to lithium bis(trimethylsilyl)amide is (0.1-10):1. DVN yield was 96.5%.

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Abstract

The invention belongs to the field of phosphorus based silane flame retardants, and particularly relates to a phosphorus based silane flame retardant and a preparing method thereof. According to the method, organosilicon oligomer and amino siloxane are used as raw materials, a mixed agent of a reaction auxiliary A and a reaction auxiliary B is used as a reaction auxiliary, and the phosphorus based silane flame retardant is obtained through a reaction, wherein the reaction auxiliary A is hydroxytrimethylsilane, hydroxytrimethylsilane salt or tetrakis(trimethylsilyl)silane, the reaction auxiliary B is hexamethyldisilazane or bis(trimethylsilyl)amide salt, and the molar ratio of the reaction auxiliary A to the reaction auxiliary B is (0.04-10):1. According to the phosphorus based silane flame retardant and the preparing method thereof, the synthesis cost of the phosphorus based silane flame retardant in the prior art is effectively lowered, the synthesis technology is simple, and the safety coefficient is high.

Description

technical field [0001] The invention belongs to the field of phosphorus-based silane flame retardants, and in particular relates to a preparation method of phosphorus-based silane flame retardants. Background technique [0002] Since the 1970s when Saito et al successfully synthesized the novel phosphaphenanthrene compound 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), the development of phosphaphenanthrene compounds and applications began to attract attention. Because phosphophenanthrene compounds generally have the characteristics of high phosphorus content, good heat resistance and chemical stability, no hydrolysis absorption, no volatility, good compatibility with polymers, and no precipitation, they are used as flame retardants. It can provide good flame retardancy for the polymer, and the flame retardancy effect is long-lasting, low smoke and low toxicity, and has little effect on the physical, mechanical and electrical properties of the polymer. Under the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/30C08G77/26C08G77/06
CPCC08G77/06C08G77/26C08G77/30C08G77/70C08G77/80
Inventor 李舟吴狄峰
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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