Method for preparing dicyanomethyl phenylphosphine

A technology of cyanomethylphenylphosphine and dicyanomethylphenyl, which is applied in the fields of 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: 2013-11-27
SHANDONG UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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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

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  • Method for preparing dicyanomethyl phenylphosphine

Examples

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Embodiment 1

[0021] Install the reactor, add 1 mole of zinc powder and 30 moles of tetrahydrofuran to the reactor under the protection of nitrogen, and then dropwise dropwise a mixture of 1 mole of phenylphosphine dichloride, 2.2 moles of bromoacetonitrile and 5 moles of tetrahydrofuran at room temperature , The dropwise addition time was 1 hour, and after the dropwise addition was completed, the reaction was stirred at room temperature for 2 hours. 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 let stand to separate layers, extract the upper organic layer, and then distill the organic layer at 60mmHg and room temperature to remove dichloromethane. After methane, the finished product of dicyanomethylphenylphosphine can be obtained. Aft...

Embodiment 2

[0024] Install the reactor, add 1 mole of zinc powder and 30 moles of tetrahydrofuran to the reactor under the protection of nitrogen, and then dropwise dropwise a mixture of 1 mole of phenylphosphine dichloride, 2.4 moles of bromoacetonitrile and 5 moles of tetrahydrofuran at 60 ° C. solution, the dropwise addition time was 1.5 hours, and the reaction was stirred at 60° C. for 2 hours after the dropwise addition was completed. 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 let stand to separate layers, extract the upper organic layer, and then distill the organic layer at 60mmHg and room temperature to remove dichloromethane. After methane, the finished product of dicyanomethylphenylphosphine can be obtained. After testing,...

Embodiment 3

[0027] Install the reactor, add 1 mole of zinc powder and 10 moles of tetrahydrofuran to the reactor under the protection of nitrogen, and then dropwise dropwise a mixture of 1 mole of phenylphosphine dichloride, 2 moles of bromoacetonitrile and 10 moles of tetrahydrofuran at 70°C solution, the dropwise addition time was 2 hours, and the reaction was stirred at 70° C. for 3 hours after the dropwise addition was completed. After the reaction, the temperature of the solution in the reactor was kept at 70° C., and then 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 let stand to separate layers, extract the upper organic layer, and then distill the organic layer at 60mmHg and room temperature to remove dichloromethane. After methane, the finished product of dicyanomethylphenylphosphine can be obtained. After testing, the melti...

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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 invention relates to a preparation method of dicyanomethylphenylphosphine. 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. 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. Contents of the invention [0003] In order to solve the above tec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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