Novel method for synthesizing chlorodiphenylphosphine by one-step process

A new technology of diphenylphosphine chloride, which is applied in the field of synthesis of diphenylphosphine chloride, can solve the problems of heavy pollution, complicated process steps, high-temperature disproportionation environment, etc., and achieve the effect of realizing recovery, increasing income and reducing pollution

Pending Publication Date: 2019-07-02
上海振品化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] In the prior art, when producing diphenylphosphine chloride, the process steps are complicated, and there are many deficiencies such as high-temperature disproportionation and heavy environmental pollution. Based on the

Method used

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  • Novel method for synthesizing chlorodiphenylphosphine by one-step process

Examples

Experimental program
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Effect test

specific Embodiment 1

[0033] Add 1.86mol PH and 0.9mol anhydrous AlCl3 into a dry four-necked flask with a stirrer, immediately install the reflux condenser and tail gas receiver, replace the air in the system with nitrogen, and add PCl3 dropwise within 45min while stirring 0.9mol, after dropping, slowly raise the temperature to the reflux of the reaction mixture, after the AlCl3 is completely dissolved, raise the temperature to 140~150°C within 2h. Continue to react in this temperature range for 6h, cool to 35°C, dropwise add 1.8mol Dilute it with phosphorus chloride, then add 0.96 mol of pyridine dropwise at 25 to 40 to obtain a light yellow viscous substance, which is extracted with 500ml of phosphorus trichloride each time, and continuously extracted several times. The low boiling point was removed to obtain 127.5g of crude product. The 140-142°C fraction was collected at 0.4kPa to obtain 90.2g of colorless viscous liquid with a yield of 45.40%. The infrared spectrum of the product Ph2PCl was co...

specific Embodiment 2

[0035] Add 1.86mol phH and 0.9mol anhydrous AlCl3 into a dry four-necked flask with a stirrer, immediately install a reflux condenser and a tail gas receiver, replace the air in the system with nitrogen, and add PCl3 dropwise within 45 minutes while stirring 0.9mol, after dropping, slowly raise the temperature to the reflux of the reaction mixture, after the AlCl3 is completely dissolved, raise the temperature to 140~150°C within 2h. Continue to react in this temperature range for 6h, cool to 35°C, dropwise add 1.8mol Dilute it with phosphorus chloride, then add 0.96 mol of 2-methylpyridine dropwise at 25-40 to obtain a light yellow viscous substance, extract it with 500ml phosphorus trichloride each time, and extract it several times continuously. The solvent was removed under reduced pressure to obtain 127.5 g of the crude product. The 140-142 ° C fraction was collected at 0.4 kPa to obtain 102 g of a colorless viscous liquid with a yield of 510%. The infrared spectrum of the...

specific Embodiment 3

[0037] Add 1.86mol phH and 0.9mol anhydrous AlCl3 into a dry four-necked flask with a stirrer, immediately install a reflux condenser and a tail gas receiver, replace the air in the system with nitrogen, and add PCl3 dropwise within 45 minutes while stirring 0.9mol, after dropping, slowly raise the temperature to the reflux of the reaction mixture, after the AlCl3 is completely dissolved, raise the temperature to 140~150°C within 2h. Continue to react in this temperature range for 6h, cool to 35°C, dropwise add 1.8mol Dilute it with phosphorus chloride, then add 0.96 mol of lutidine dropwise at 25-40 to obtain a light yellow viscous substance, extract with 500ml phosphorus trichloride each time, and extract continuously several times, and evaporate the solvent at normal pressure , the low boiling point was removed under reduced pressure to obtain 127.5g of crude product. The 140-142°C fraction was collected at 0.4kPa to obtain 103.5g of colorless viscous liquid with a yield of ...

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Abstract

The invention relates to a novel method for synthesizing chlorodiphenylphosphine by a one-step process. The method comprises the following steps: respectively adding phosphorus trichloride, benzene and aluminum trichloride into a three-necked bottle, performing programmed heating to 140-150 DEG C while stirring under the protection of nitrogen, carrying out a heat insulation reaction at the temperature of 140-150 DEG C until no reflux state, and cooling the obtained reaction solution to room temperature; adding an organic solvent to the reaction solution, performing stirring for several hours,dropwise adding a decomplexing agent, stirring the obtained solution for several hours after the drop-by-drop addition of the decomplexing agent is finished, standing the solution to layer the solution, separating out the obtained decomplexing agent layer, carrying out reduced pressure distillation on the obtained organic solvent layer to obtain crude chlorodiphenylphosphine, and distilling the crude chlorodiphenylphosphine under a high vacuum to obtain pure chlorodiphenylphosphine. The method reduces the environmental pollution by recovering the aluminum trichloride, increases the yield of abyproduct, increases the income, and also has the advantages of high yield, low cost and short reaction time.

Description

technical field [0001] The invention relates to the technical field of diphenylphosphine chloride synthesis, in particular to a novel method for synthesizing diphenylphosphine chloride in one step. Background technique [0002] In the prior art, when producing diphenylphosphine chloride, the process steps are complicated, and there are many deficiencies such as high-temperature disproportionation and heavy environmental pollution. Based on the shortcomings of the prior art, the invention provides a synthetic process route that is simple, easy to operate, and low in production cost. A production method of diphenylphosphine chloride with low environmental pollution. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a novel method for synthesizing diphenylphosphine chloride in one step, so as to solve the defects in the prior art. [0004] The technical scheme that the present invention solves the problems of the tec...

Claims

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Application Information

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IPC IPC(8): C07F9/52C01B25/10C01F7/04
CPCC07F9/52C01B25/10C01F7/04
Inventor 王志军蔡珍珍
Owner 上海振品化工有限公司
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