Ethyl triphenyl phosphonium chloride preparation method

A technology of ethyl triphenyl phosphine chloride and triphenyl phosphine, applied in the field of preparation of ethyl triphenyl phosphine chloride, can solve the problem of low purity, low yield of ethyl triphenyl phosphine chloride, etc. question

Inactive Publication Date: 2017-02-15
KENTE CATALYSTS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems of low yield and low purity of the existing ethyltriphenylphosphine chloride, the present invention proposes a preparation method of ethyltriphenylphosphine chloride, the yield of the method is as high as 94%, and the purity is as high as More than 99%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of ethyltriphenylphosphine chloride:

[0019] Weigh 1mol of triphenylphosphine and 8.5mol of acetonitrile, put them into a 2000L pressure reactor, then add 1.0mol of ethyl chloride dropwise, seal the reactor after the dropwise addition; open the steam inlet valve for heating , the temperature in the pressure reactor is controlled to be 120°C, and the pressure in the kettle is 10kg / cm 2 , and keep warm for 35 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 50°C, vent the pressure reactor, keep warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.5%, and keep the supernatant for later use; the precipitate after centrifugation After drying at 100°C for 10 hours, 0....

Embodiment 2

[0021] Weigh 1mol of triphenylphosphine and 5mol of acetonitrile, put them into a 2000L pressure reactor, add 1.2mol of ethyl chloride dropwise, seal the reactor after the addition is complete; open the steam inlet valve for heating, Control the temperature in the pressure reactor to 140°C, and the pressure in the kettle to 11kg / cm 2 , and keep it warm for 32 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 55°C, vent the pressure reactor, keep it warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.8%, and keep the supernatant for later use; the precipitate after centrifugation After drying at 105°C for 18 hours, 0.9498 mol of triphenylphosphine was obtained with a yield of 94.98%. The puri...

Embodiment 3

[0023] Weigh 1mol of triphenylphosphine and 10mol of acetone, put them into a 2000L pressure reactor, then add 1.5mol of ethyl chloride dropwise, seal the reactor after the addition; open the steam inlet valve for heating, Control the temperature in the pressure reactor to 150°C, and the pressure in the kettle to 12kg / cm 2 , and keep it warm for 40 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 60°C, vent the pressure reactor, keep it warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.8%, and keep the supernatant for later use; the precipitate after centrifugation Dry at 105°C for 18 hours, then mix with acetonitrile, heat and reflux, cool and crystallize, and centrifuge for 48 hours, th...

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Abstract

The invention provides an ethyl triphenyl phosphonium chloride preparation method, which comprises: (1) adding triphenyl phosphine to an organic solvent, adding ethyl chloride in a dropwise manner, heating to a temperature of 120-160 DEG C after the adding, adjusting the reaction pressure to 8-12 kg/cm<2>, and carrying out a thermal insulation reaction for 30-40 h; (2) after completing the thermal insulation reaction, cooling to a room temperature, reducing the pressure to a normal pressure, and carrying out centrifugation on the material obtained after the reaction; and (3) drying the centrifugal precipitate so as to obtain the ethyl triphenyl phosphonium chloride. According to the present invention, with the method, the yield is up to more than 94%, and the purity is up to more than 99%.

Description

technical field [0001] The invention relates to the technical field of preparation of quaternary phosphonium salts, in particular to a preparation method of ethyltriphenylphosphine chloride. Background technique [0002] Ethyltriphenylphosphine chloride is a surfactant, powdery solid, with a melting point of 240-244°C, belonging to a quaternary phosphonium salt. The hydrogen on the ethyl group can be removed in an alkaline medium to form a phosphorus ylide. In phosphorus ylides, due to the coexistence of opposite charges in the covalently bonded molecule, it exhibits several unique properties. The electrons of the carbanion part enter the 3d empty orbital of the phosphorus atom to form a feedback bond, which makes the phosphorus ylide have considerable stability. Carbanion is prone to a series of nucleophilic reactions and is an important method for the preparation of alkenes, such as the synthesis of insect pheromones, vitamins, and plant pigments. At present, the prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/54
Inventor 项飞勇
Owner KENTE CATALYSTS INC
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