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Method for preparing phosphorus-containing organic silicon flame retardant agent

A flame retardant and silicone technology, which is applied in the field of preparation of phosphorus-containing silicone flame retardants, can solve the problems of poor heat resistance, high volatility, and unsatisfactory polymer compatibility, and achieves increased flexibility and The effect of high temperature resistance

Inactive Publication Date: 2012-03-07
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most phosphorus-based flame retardants are liquid, have poor heat resistance, high volatility, and poor compatibility with polymers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Install a stirrer, thermometer, and spherical condenser in a 500ml three-necked bottle, add 100ml toluene and 20.2g triethylamine, and weigh 75.8g (0.1 mol) of hydroxyl-terminated polydimethylsiloxane (HO(SiMe 2 O) 10H) Stir and mix with 20.0g (0.103mol) of phenylphosphoryl dichloride, react at 80°C for 4h, filter off the precipitate, and distill off toluene to obtain 88.5g of phosphorus-containing polysiloxane (P-Cl mole is 0.06).

[0034] 2) Install a stirrer, a thermometer, and a spherical condenser on a 500ml three-necked bottle, and add 100ml of chloroform and 4.75g of pyridine. 88.5g of phosphorus-containing polysiloxane and 20.8g of amino-containing polysiloxane (structural formula Me 3 SiO(Me 2 SiO) 100 (MeNH 2 C 3 h 6 SiO) 50 (MeSiO 3 / 2 ) 20 (PhSiO 3 / 2 ) 20 SiMe 3 , the molar number of amino groups is 0.06), reacted at 20°C for 17h, filtered, and evaporated the solvent to obtain 107.1g of phosphorus-containing silicone flame retardant.

[00...

Embodiment 2

[0037] 1) Install a stirrer, thermometer, and spherical condenser in a 500ml three-necked bottle, add 150ml petroleum ether and 10g sodium bicarbonate, and weigh 37.1g (0.05 mol) of aminopropyl-terminated polysiloxane (NH 2 C 3 h 6 Me 2 SiO(Me 2 SiO) 3 (SiMePhO) 2 SiMe 2 C 3 h 6 NH 2 ) and 15.3g (0.1mol) of phosphorus oxychloride were stirred and mixed, reacted at 20°C for 20h, filtered off the precipitate, and evaporated petroleum ether to obtain 48.8g of phosphorus-containing polysiloxane (P-Cl molar number is 0.2 ).

[0038] 2) Install a stirrer, a thermometer, and a spherical condenser on a 500ml three-necked bottle, and add 120ml tetrahydrofuran and 8.0 g sodium hydroxide. 48.8g of phosphorus-containing polysiloxane and 168.5g of hydroxyl-containing polysiloxane (structural formula Me 3 SiO(Me 2 SiO) 30 (MeHOSiO) 80 (PhHOSiO) 50 (MeSiO 3 / 2 ) 40 (PhSiO 3 / 2 ) 30 SiMe 3 , the molar number of hydroxyl groups is 1.0), reacted at 80°C for 4 hours, filtered...

Embodiment 3

[0041] 1) Install a stirrer, a thermometer, and a spherical condenser in a 500ml three-necked bottle, add 150ml xylene and 12g potassium carbonate, and weigh 21.6g (0.1 mol) of diphenylsilanediol (Ph 2 Si(OH) 2 ) and 20.0g (0.13mol) of phosphorus oxychloride were stirred and mixed, reacted at 60°C for 12h, filtered off the precipitate, and distilled off the xylene to obtain 34.3g of phosphorus-containing polysiloxane (the molar number of P-Cl was 0.19 ).

[0042] 2) Install a stirrer, a thermometer, and a spherical condenser on the 500ml three-necked bottle, and add 100ml acetone and 8.0 g sodium hydroxide. 34.3g of phosphorus-containing polysiloxane and 92.9g of methylaminopropyl dimethoxysilane (structural formula MeNH 2 C 3 h 6 Si(OMe) 2 ), the molar number of amino groups is 0.57), reacted at 50°C for 12 hours, filtered, and evaporated the solvent to obtain 120.3g of phosphorus-containing silicone flame retardant.

[0043] Flame retardant application performance: Aft...

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Abstract

The invention relates to a method for preparing phosphorus-containing organic silicon flame retardant agent, and aims at solving the technical problem of ensuring a simple, mild and controllable preparation method, the hydrolysis stability of products and the great improvement of high temperature resistance. The method comprises the following steps: 1) in the presence of organic solvent and acid binding agent, uniformly mixing functionality terminated organic silicon compound and P-Cl bond-containing phosphorous compound in the molar ratio of 1 to 2, and reacting for 4 to 20 hours at the temperature of between 20 and 80 DEG C; filtering the precipitate after reaction, evaporating to remove organic solvent and preparing phosphorous-containing polysiloxane; and 2) in the presence of the organic solvent and the acid binding agent, leading the phosphorous-containing polysiloxane to react with the functional group containing organic silicon compound for 4 to 20 hours at the temperature of between 20 and 80 DEG C; and filtering the precipitate after reaction, evaporating to remove organic solvent to prepare the product.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis, in particular to a method for preparing a phosphorus-containing organosilicon flame retardant. Background technique [0002] With the development of my country's synthetic material industry and the continuous expansion of application fields, flame retardants have broad market prospects in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, and basic necessities of life. [0003] Organophosphorus flame retardant is a kind of flame retardant with good flame retardant performance. It has dual functions of flame retardant and plasticizing. It can replace halogenated flame retardants and is an environmentally friendly flame retardant. However, most phosphorus-based flame retardants are liquid, have poor heat resistance, high volatility, and poor compatibility with polymers. [0004] Silicone flam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/30C08G77/395C08G81/00C09K21/14C08L55/02C08L23/12C08L69/00C08L77/00C08L87/00C08L83/08
Inventor 来国桥李美江蒋剑雄倪勇吕素芳
Owner HANGZHOU NORMAL UNIVERSITY