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Method for preparing dicyanomethyl phenylphosphine

A technology of cyanomethylphenylphosphine and dicyanomethylphenyl, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve environmental pollution of waste residues and low yield and other problems, to achieve the effect of less by-products, simple production process, and obvious environmental protection

Active Publication Date: 2011-02-16
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are a small number of literature reports to prepare dicyanomethylphenylphosphine by the reaction method of zinc powder catalyzed phenylphosphine dichloride and bromoacetonitrile at present, but the yield of this method is low, and a large amount of waste residues are produced in the product synthesis process, which leads to serious environmental pollution. Therefore, New synthetic methods need to be developed

Method used

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  • Method for preparing dicyanomethyl phenylphosphine

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Embodiment 1

[0021] Install a reactor, add 1 mole of zinc powder and 30 moles of tetrahydrofuran to the reactor under nitrogen protection, and then dropwise add a mixture of 1 mole of phenylphosphorus dichloride, 2.2 moles of bromoacetonitrile and 5 moles of tetrahydrofuran at room temperature , the dropwise addition time was 1 hour, and the reaction was stirred at room temperature for 2 hours after the dropwise addition was completed. After the reaction, the temperature of the solution in the reactor was raised to 50° C., and then the tetrahydrofuran and bromoacetonitrile in the solution were distilled off under a pressure of 60 mmHg. After steaming, add 10 moles of dichloromethane and 5 moles of water to the reactor, stir well, then stand for stratification, extract the upper organic layer, and then distill the organic layer at 60 mmHg and room temperature to remove the dichloride. After methane, the finished product of biscyanomethylphenylphosphine is obtained. After testing, the melti...

Embodiment 2

[0024] A reactor was installed, 1 mole of zinc powder and 30 moles of tetrahydrofuran were added to the reactor under nitrogen protection, and then a mixture of 1 mole of phenylphosphorus dichloride, 2.4 moles of bromoacetonitrile and 5 moles of tetrahydrofuran was added dropwise at a constant speed at 60 °C. The dropwise addition time was 1.5 hours. After the dropwise addition was completed, the reaction was stirred at 60° C. for 2 hours. After the reaction, the temperature of the solution in the reactor was kept at 60° C., and then the tetrahydrofuran and bromoacetonitrile in the solution were distilled off under a pressure of 60 mmHg. After steaming, add 10 moles of dichloromethane and 5 moles of water to the reactor, stir well, then stand for stratification, extract the upper organic layer, and then distill the organic layer at 60 mmHg and room temperature to remove the dichloride. After methane, the finished product of biscyanomethylphenylphosphine is obtained. After tes...

Embodiment 3

[0027] A reactor was installed, 1 mole of zinc powder and 10 moles of tetrahydrofuran were added to the reactor under nitrogen protection, and then a mixture of 1 mole of phenylphosphorus dichloride, 2 moles of bromoacetonitrile and 10 moles of tetrahydrofuran was added dropwise at a constant speed at 70 °C. The dropwise addition time was 2 hours. After the dropwise addition was completed, the reaction was stirred at 70° C. for 3 hours. After the reaction, the temperature of the solution in the reactor was kept at 70°C, and then the tetrahydrofuran and bromoacetonitrile in the solution were distilled off under a pressure of 60 mmHg. After steaming, add 10 moles of dichloromethane and 5 moles of water to the reactor, stir well, then stand for stratification, extract the upper organic layer, and then distill the organic layer at 60 mmHg and room temperature to remove the dichloride. After methane, the finished product of biscyanomethylphenylphosphine is obtained. After testing,...

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Abstract

The invention discloses a method for preparing dicyanomethyl phenylphosphine, which comprises the following steps of: adding tetrahydrofuran and zinc powder into a reactor, adding dropwise the mixed solution of dichlorophenylphosphine, bromoacetonitrile and the tetrahydrofuran, performing reaction at the constant temperature of 20 to 70 DEG C for 0.5 to 3 hours, performing primary distillation under reduced pressure to recover the tetrahydrofuran and the bromoacetonitrile after the reaction is finished, continuing to add dichloromethane and water into the distilled reactor, performing demixing under stirring to obtain an organic layer, and performing secondary distillation under reduced pressure to remove the dichloromethane to obtain the dicyanomethyl phenylphosphine finished product. The dicyanomethyl phenylphosphine product prepared by the method has the purity of over 98 percent; and the production process is simple, the production is easy to control and the method is favorable for large-scale production.

Description

technical field [0001] The present invention relates to a preparation method of biscyanomethylphenylphosphine. Background technique [0002] Dicyanomethylphenylphosphine is an important organophosphorus compound, which can be used to synthesize biscarboxymethylphenylphosphine oxide and bishydroxyethylphenylphosphine oxide, and the latter two can be used in PET, PBT, PA, respectively. It is a reactive and environmentally friendly flame retardant with excellent performance and has a good market prospect. At present, there are a small amount of literature reports to use zinc powder to catalyze the reaction of phenylphosphine dichloride and bromoacetonitrile to prepare biscyanomethylphenylphosphine, but the yield of this method is low, and the product synthesis process produces a large amount of waste residue and causes serious environmental pollution. Therefore, New synthetic methods need to be developed. SUMMARY OF THE INVENTION [0003] In order to solve the above technic...

Claims

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Application Information

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IPC IPC(8): C07F9/50
Inventor 赵伟王忠卫宋思思段好东
Owner SHANDONG UNIV OF SCI & TECH
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