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Alkylphosphine oligomer and synthesis method thereof

A synthesis method and oligomer technology are applied in the field of alkyl phosphine oligomers and their synthesis, which can solve the problems of low thermal stability, easy hydrolysis, poor acid and alkali resistance and solvent resistance, and achieve good carbon-forming ability. , Short reaction time, good solvent resistance

Active Publication Date: 2015-05-13
SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEM +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
  • Alkylphosphine oligomer and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 40.4 g of thiophene and 600 mL of solvent n-hexane into the four-neck flask. Cool the four-neck flask to -10°C and maintain it for 30min. At this temperature, n-butyl lithium in n-hexane (2.5M, 384mL) and 4.5g of tetramethylethylenediamine were slowly added dropwise from a constant pressure dropping funnel To the reaction flask, the dropwise addition time is 1.5h. 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 40° C. and the reaction was stirred at this temperature for 2 h.

[0030] 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°C during the dropping...

Embodiment 2

[0036] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 40.4 g of thiophene and 600 mL of solvent diethyl ether into the four-neck flask. Cool the four-neck flask to -20°C and maintain it for 30min. At this temperature, a cyclohexane solution of n-butyllithium (2.5M, 384mL) and 4.5g of tetramethylethylenediamine were slowly mixed through a constant pressure dropping funnel. Add it dropwise to the reaction flask, and the dropping time is 2.5h. 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 30° C. and stirred at this temperature for 3 h.

[0037] 2) Re-cool the four-neck flask to lower the system temperature to -10°C. Slowly drop 52.4 g of ethyl phosphine dichloride into the reaction flask through a constant pressure dropping funnel, and keep the temperature of the system not exceeding 20° C. during th...

Embodiment 3

[0043] 1) Connect a 2000mL four-neck flask to a mechanical stirrer and a constant pressure dropping funnel. Add 40.4 g of thiophene and 600 mL of petroleum ether into the four-neck flask. Cool the four-neck flask to -10°C and maintain it for 30 minutes. At this temperature, diethyl ether solution (2.5M, 384mL) of n-butyllithium and 4.5g of N,N'-dimethylethylenediamine were mixed by constant pressure The dropping funnel was slowly added dropwise to the reaction flask, and the dropping time was 1.5h. 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 40° C. and stirred at this temperature for 2 h.

[0044] 2) Re-cool the four-neck flask to lower the system temperature to -5°C. Slowly drop 58.0 g of n-propylphosphine dichloride into the reaction flask through a constant pressure dropping funnel, and keep the temperature of the system not exceeding 20°C during th...

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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 thiophene, adding a dehydrogenation 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): C07F9/6553C08K5/50C08L69/00C08L67/02C08L55/02
Inventor 赵巍王晓霖
Owner SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEM
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