Method for production of triphenylphosphine by reduction process
A technology of triphenylphosphine and reduction method, which is applied in the field of production of triphenylphosphine by reduction method, can solve the problems of harsh production process, high control requirements, high risk, etc., and achieve safe and stable production, advanced technology and low cost Effect
Inactive Publication Date: 2019-10-18
闫福全
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Problems solved by technology
[0003] At present, some domestic manufacturers use metal magnesium, chlorobenzene and phosphorus trichloride to produce triphenylphosphine. The production process is harsh, the control requirements are high, the risk is high, and the yield is not high.
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[0022] A method for producing triphenylphosphine by reduction method, is characterized in that, comprises the following steps:
[0023] Step 1: Add triphenylphosphine oxide to the reduction kettle, cool the jacket of the reduction kettle to below 30 degrees with circulating water, open the hydrochloric acid falling film absorption device, add trichlorosilane dropwise through the high-level tank under normal pressure, and generate hydrochloric acid gas for the reaction Falling film absorption, stirring and refluxing for a certain period of time. After the reaction of triphenylphosphine is complete for sampling and analysis, a certain amount of trichlorosilane is recovered by steaming and heating. The trichlorosilane evaporated during the recovery process is added to the next batch of trichlorosilane The chlorosilane high level tank is applied, and then the jacket is passed through cooling water to cool down to 30 degrees, and the above-mentioned generated materials are started t...
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Relating to the field of triphenylphosphine production, the invention discloses a method for production of triphenylphosphine by reduction process. The steps include: dehydrating triphenylphosphine oxide and a solvent toluene, then adding trichlorosilane dropwise, reducing triphenylphosphine oxide into triphenylphosphine, adding the product into a hydrolysis kettle dropwise, using the emitted tailgas HCL by chloromethyl ether, and then performing recovery by a falling film absorption device to obtain by-product hydrochloric acid, separating aqueous phase and filtering out silicon dioxide, subjecting an organic phase to washing layering, then putting the organic phase into a distillation kettle to recover toluene, subjecting the toluene to recycling, removing solution from the material andperforming dissolving with methanol, stirring the substances evenly, conducting cooling crystallization, applying methanol several times, then performing distillation for reuse, centrifuging the crystallized material, and then conducting vacuum drying packaging, thus obtaining the product triphenylphosphine. The method for production of triphenylphosphine by reduction process has the beneficial effects of environmental protection, no generation of three wastes and cost saving.
Description
technical field [0001] The invention relates to the field of triphenylphosphine production, in particular to a reduction method for producing triphenylphosphine. Background technique [0002] Triphenylphosphine is a white crystalline solid with molecular formula: (C6H5)3P. It is an important organic intermediate raw material for medicines, pesticides, dyes, spices, photosensitive chemicals, polymer catalysts and other products. Triphenylphosphine is widely used in many fields such as medicine, pesticides, dyes, spices, photosensitive chemicals, polymer catalysts, etc. With the advancement of science and technology, the use of triphenylphosphine continues to expand, and many downstream products are currently very developed in China. Prospect of fine chemical intermediates or chemicals, it is necessary to speed up the development and production of triphenylphosphine. [0003] At present, some domestic manufacturers use metal magnesium, chlorobenzene and phosphorus trichloride...
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CPCC07F9/5022C07F9/505
Inventor 闫福全
Owner 闫福全