Alkylphosphine oligomer and synthesis method thereof

A synthesis method and oligomer technology, which are applied in the field of alkylphosphine oligomers and their synthesis, can solve the problems of easy hydrolysis, poor acid and alkali resistance, poor solvent resistance, low thermal stability, etc., and achieve short reaction time, durability The effect of good solvent performance and good char formation ability

Active Publication Date: 2015-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of alkylphosphine oligomer flame retardant and its synthesis method aiming at the shortcomings of existing phosphate flame retardants such as low thermal stability, easy hydrolysis, poor acid and alkali resistance and solvent resistance

Method used

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  • Alkylphosphine oligomer and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 149.8 g of 4,4'-dibromobiphenyl and 600 mL of solvent tetrahydrofuran into the four-neck flask. Place the four-necked bottle in a cold well, cool it to -70°C and maintain it for 30 minutes, at this temperature, add a solution of n-butyllithium in n-hexane (2.5M, 384mL) and 3.32g of tetramethylethylenediamine by constant pressure dropwise The liquid funnel was added slowly, and the dropping time was 2h. With the addition of n-butyllithium, the temperature of the system rises spontaneously. After the dropwise addition, the temperature of the system was slowly raised to 25° C. and stirred at this temperature for 1 h.

[0029] 2) Re-cool the four-neck flask to lower the system temperature to -5°C. Slowly drop 46.8 g of methylphosphine dichloride into the reaction flask through a constant pressure dropping funnel, and keep the temperature of the system not exceeding 20...

Embodiment 2

[0035] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 149.8 g of 4,4'-dibromobiphenyl and 600 mL of solvent n-butyl ether into the four-neck flask. Place the four-necked bottle in a cold well, cool it to -70°C and maintain it for 30 minutes, at this temperature, add a solution of n-butyllithium in n-hexane (2.5M, 384mL) and 3.32g of tetramethylethylenediamine by constant pressure dropwise The liquid funnel was added slowly, and the dropping time was 2h. With the addition of n-butyllithium, the temperature of the system rises spontaneously. After the dropwise addition, the temperature of the system was slowly raised to 25° C. and stirred at this temperature for 1 h.

[0036] 2) Re-cool the four-neck flask to lower the system temperature to -5°C. Slowly drop 70.0 g of n-butylphosphine dichloride into the reaction flask through a constant pressure dropping funnel, and keep the temperature of the system not exceeding 20°...

Embodiment 3

[0042] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 149.8 g of 4,4'-dibromobiphenyl and 600 mL of solvent anisole into the four-neck flask. Place the four-neck bottle in a cold well, cool to -70°C and maintain it for 30 minutes, at this temperature, add n-butyllithium in n-hexane (2.5M, 384mL) and N,N-dimethylethylenediamine 3.32g Add slowly from the constant pressure dropping funnel, and the dropping time is 2h. With the addition of n-butyllithium, the temperature of the system rises spontaneously. After the dropwise addition, the temperature of the system was slowly raised to 25° C. and stirred at this temperature for 1 h.

[0043] 2) Re-cool the four-neck flask to lower the system temperature to -5°C. Slowly drop 63.6 g of tert-butylphosphine dichloride into the reaction flask through a constant pressure dropping funnel, and keep the temperature of the system not exceeding 20°C during the dropping process. Afte...

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Abstract

The present invention discloses an alkylphosphine oligomer and a synthesis method thereof, wherein the structure general formula of the alkylphosphine oligomer is represented by the figure. The synthesis method comprises: adding a solvent and a stabilizer to p-dibromobiphenyl, adding a dehalogenating agent to a reactor under a cooling condition, increasing the reaction temperature to produce a dilithium salt, cooling the reaction system, adding alkyl phosphine dichloride in a dropwise manner, increasing the reaction temperature, adding a reagent, carrying out a quenching reaction, completing the reaction, and carrying out solvent removing, alcohol washing, water washing and drying to obtain the alkylphosphine oligomer. The product of the present invention has advantages of strong char formation ability and good stability. The synthesis method has advantages of continuous reaction process, short reaction time, simple synthesis process, and efficient reaction.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to an alkylphosphine oligomer and a synthesis method thereof. Background technique [0002] Since the 1980s, flame retardants have become one of the most important additives for polymer materials, and their usage is increasing day by day. Among many flame retardants, organophosphorus flame retardants are recognized as important varieties that can replace halogenated flame retardants because of their environmental friendliness and high efficiency. While endowing materials with good flame retardancy, compared with halogen flame retardants, it has the characteristics of less smoke generation and less formation of toxic and corrosive gases. In recent years, research on organophosphorus flame retardants has become a hot topic in the field of flame retardants. [0003] The combustion process of polymers can be divided into five stages: heating, decomposition, ignition, combu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/50C08K5/50C08L55/02C08L69/00
Inventor 赵巍王晓霖李明刘名瑞薛倩
Owner CHINA PETROLEUM & CHEM CORP
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