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Phosphorus-nitrogen containing flame retardant modified silane coupler and preparation method thereof

A silane coupling agent and modification technology, which is applied in the field of flame retardant modified silane coupling agent and its preparation, to achieve the effect of solving the problem of flammability

Inactive Publication Date: 2009-12-30
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to propose a phosphorus-nitrogen-containing flame-retardant modified silane coupling agent and its preparation method, to solve the flammability problem existing in the existing silane coupling agent and to further expand its scope of use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours; the system was heated until the temperature rose to 83°C, kept at this temperature for reflux reaction for 2 hours, and dichloromethane was removed by decompression precipitation to obtain a white solid ;

[0014] Take 9.224 g of the white solid obtained above, put it in a 150 ml three-necked flask, add 50 ml of tetrahydrofuran to dissolve it, then add 5.060 g of triethylamine, pass nitrogen gas for 10 minutes, heat up to 50 ° C, and drop 10.32 g of N-(β- Aminoethyl)-γ-aminopropylmethyldimethoxysilane, kept at 50°C to continue the reaction for 5 hours after the dropwise addition. After the reaction is completed, filter, and...

Embodiment 2

[0023] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours. The temperature of the system was kept rising to 83° C. for reflux reaction for 2 hours, and the methylene chloride was removed under reduced pressure to obtain a white solid.

[0024] In a 150ml three-neck flask, take 9.224g of the above solid, dissolve it in 50ml of tetrahydrofuran, add 5.060g of triethylamine, blow nitrogen for 10 minutes, heat up to 80°C, add dropwise 9.567g of γ-aminopropylmethyldiethoxy Silane, after the dropwise addition was completed, the reaction was continued at 80° C. for 7 hours. After the reaction is completed, filter, and remove the solvent from the filtrate under reduced pressure to obtain a v...

Embodiment 3

[0034] Add 10.4g of neopentyl glycol and 100mL of dichloromethane into a 250mL three-necked flask equipped with a reflux condenser with a dryer and a constant pressure dropping funnel, raise the temperature to 50°C, and fill 9.6mL of Phosphorus oxychloride was slowly added dropwise while stirring, and the dropwise addition was completed in about 1.5 hours. The temperature of the system was kept rising to 83° C. for reflux reaction for 2 hours, and the methylene chloride was removed under reduced pressure to obtain a white solid.

[0035] In a 150ml three-necked flask, take 9.224g of the above solid, dissolve it in 50ml of tetrahydrofuran, add 5.060g of triethylamine, blow nitrogen for 10 minutes, heat up to 60°C, add 11.34g of aminopropyltriethoxysilane dropwise, add dropwise After completion, the reaction was continued at 60° C. for 5 hours. After the reaction is completed, filter, and remove the solvent from the filtrate under reduced pressure to obtain a viscous liquid, whi...

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PUM

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Abstract

The invention discloses a phosphorus-nitrogen containing flame retardant modified silane coupler and a preparation method thereof. The preparation method is characterized by comprising the following steps: taking methylene chloride as a solvent and part of polyhydric alcohol or polyatomic phenol as a reaction matrix, adding a phosphorous compound with active reaction groups dropwise based on the reaction mol ratio, agitating an obtained mixture at room temperature for 2-5h, filtering the obtained mixture to remove the solvent, thus obtaining white solid power; and then taking tetrahydrofuran as a solvent and triethylamine as an acid adding agent, adding siloxane with active functional groups dropwise based on the reaction mol ratio under the protection of inert gas, agitating and reacting at 50-80 DEG C for 5-8h, and filtering and depressurizing the mixture to remove the solvent, thus obtaining the phosphorus-nitrogen containing flame retardant modified silane coupler. As flame retardant elements of phosphorus and nitrogen are introduced in molecules, the phosphorus-nitrogen containing flame retardant modified silane coupler has good flame retardant property.

Description

technical field [0001] The invention belongs to the technical field of silane coupling agent modification, and in particular relates to a phosphorus-nitrogen-containing flame-retardant modified silane coupling agent and a preparation method thereof. Background technique [0002] Silane coupling agent is a type of silane with organic functional groups, which contains reactive groups that can chemically bond with inorganic materials (such as glass, silica sand, metal) and chemically bond with organic materials (synthetic resins). The reactive group can adopt the general formula Y(CH 2 ) nSiX 3 In the formula, n=0~3; X is a hydrolyzable group; Y is an organic functional group. In the prior art, by changing the organic functional group, the silane coupling agent can have unique properties, and its application field is expanding day by day. For example, Chinese Patent Application Publication No. CN 101104622A reports that a diphenylsulfone-based aminosilane coupling agent can ...

Claims

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Application Information

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IPC IPC(8): C07F9/24C07F7/18C08K9/04C08K5/544
Inventor 胡源胡爽宋磊
Owner UNIV OF SCI & TECH OF CHINA
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