Supercharge Your Innovation With Domain-Expert AI Agents!

Method for preparing triphenylphosphine

A technology of triphenylphosphine and triphenylphosphine sulfide, applied in the field of preparation of triphenylphosphine, can solve the problems of difficult control of chlorobenzene and phosphorus trichloride, complicated reaction steps, multiple reactions in addition amount, etc. The effect of easy to master the amount of ingredients, easy control of the reaction process and simple process flow

Inactive Publication Date: 2013-05-01
HUBEI XINGFA CHEM GRP CO LTD
View PDF0 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the sodium method is mainly used for the preparation of triphenylphosphine, and there are two main process routes. One is a step-by-step synthesis method, which is to first react chlorobenzene with metal sodium to produce phenyl sodium at 20-30 ° C, and then Adding phosphorus trichloride and phenyl sodium to react to prepare triphenylphosphine, this method has complex reaction steps, long reaction process, many side reactions, and low product yield
Another kind of method is the disclosed method of German patent Ger.offen1618116, and it is to drip chlorobenzene and phosphorus trichloride and metal sodium to react simultaneously at 50-60 ℃ to prepare triphenylphosphine, although this method is simple, but The amount of chlorobenzene and phosphorus trichloride that initiates the reaction is difficult to control. If the amount added is small, the initiation time is too long. If the amount added makes the reaction too violent, the temperature of the system changes suddenly, which is difficult to control and sometimes causes accidents.
Above two kinds of prior art are because sodium dispersibility is not good, easily cause the degree of reaction to be little, material consumption is big, the defect that cost is high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing triphenylphosphine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 48g (0.36mol) of aluminum trichloride, 3.85g (0.12mol) of sublimed sulfur, 16.55g (0.12mol) of phosphorus trichloride and 150mL of excess benzene into a 250mL round-bottomed flask with a reflux device, and heat to The internal reactants are in a state of strong reflux, the reflux temperature is 75-80°C, and the reaction is stirred for 8 hours. After the reaction, the product was slowly poured into 400mL of ice-water mixture to dissolve and cool, stirred, left for a while, separated, and the organic phase was separated, and the aqueous phase was extracted three times with benzene to extract the organic phase. The organic phases were combined, dried with anhydrous sodium sulfate, the solvent benzene was distilled off, and then recrystallized with acetone-water to obtain white triphenylphosphine sulfide crystals. Then mix 8.4g (0.15mol) of triphenylthiophosphine and reduced iron powder and put it into a round-bottomed three-neck flask, stir and react at 350°C for 2 hou...

Embodiment 2

[0019] Add 48g (0.36mol) of aluminum trichloride, 3.85g (0.12mol) of sublimed sulfur, 16.55g (0.12mol) of phosphorus trichloride and 150mL of excess benzene into a 250mL round-bottomed flask with a reflux device, and heat to The internal reactants are in a state of strong reflux, the reflux temperature is 90-100°C, and the reaction is stirred for 9 hours. After the reaction, the product was slowly poured into 400mL of ice-water mixture to dissolve and cool, stirred, left for a while, separated, and the organic phase was separated, and the aqueous phase was extracted three times with benzene to extract the organic phase. The organic phases were combined, dried with anhydrous sodium sulfate, the solvent benzene was distilled off, and then recrystallized with acetone-water to obtain white triphenylphosphine sulfide crystals. Then mix 9.8g (0.15mol) of triphenylthiophosphine and reduced zinc powder and put it into a three-necked round-bottomed flask. Stir and react at 370°C for 3 ...

Embodiment 3

[0020] Add 48g (0.36mol) of aluminum trichloride, 3.85g (0.12mol) of sublimed sulfur, 16.55g (0.12mol) of phosphorus trichloride and 150mL of excess benzene into a 250mL round-bottomed flask with a reflux device, and heat to The internal reactants are in a state of strong reflux, the reflux temperature is 75-80°C, and the reaction is stirred for 8 hours. After the reaction, the product was slowly poured into 400mL of ice-water mixture to dissolve and cool, stirred, left for a while and then separated, and the organic phase was separated, and the aqueous phase was extracted three times with benzene to extract the organic phase. The organic phases were combined, dried with anhydrous sodium sulfate, the solvent benzene was distilled off, and then recrystallized with acetone-water to obtain white triphenylphosphine sulfide crystals. Then mix 8.8g (0.15mol) of triphenylthiophosphine and reduced nickel powder and put it into a three-necked round-bottomed flask. Stir and react at 400...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method for preparing triphenylphosphine. Phosphorus trichloride, sublimed sulfur and benzene are used as reactants to react to obtain triphenylphosphine sulfide under the condition of a catalyst, and the triphenylphosphine sulfide is reduced to obtain the triphenylphosphine under the existence of a reducing agent existing. The method for preparing the triphenylphosphine has the advantages of simple process flow and low cost and is suitable for industrial production, and reaction is easily controlled.

Description

technical field [0001] The invention belongs to the field of preparation of triphenylphosphine, and mainly relates to a preparation method of triphenylphosphine. Background technique [0002] Triphenylphosphine is the basic raw material of rhodium-phosphine complex catalyst, and has wide application in domestic petrochemical industry. At present, the sodium method is mainly used for the preparation of triphenylphosphine, and there are two main process routes. One is a step-by-step synthesis method, which is to first react chlorobenzene with metal sodium to produce phenyl sodium at 20-30 ° C, and then Add phosphorus trichloride and phenyl sodium to react to prepare triphenylphosphine. This method has complex reaction steps, long reaction process, many side reactions and low product yield. Another kind of method is the disclosed method of German patent Ger.offen1618116, and it is to drip chlorobenzene and phosphorus trichloride and metal sodium to react simultaneously at 50-6...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/50
Inventor 熊涛魏文彬李永刚陈松何西平林萌
Owner HUBEI XINGFA CHEM GRP CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com