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Production method of triphenylphosphine

A technology of triphenylphosphine and production method, which is applied in the production field of triphenylphosphine, can solve the problems of high requirements, high viscosity of reactants, side reactions, etc., achieves safe production process, overcomes low yield and avoids pollution. Effect

Active Publication Date: 2015-07-22
山东九龙石化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are two main methods for producing triphenylene sand, the magnesium method and the sodium method, but the production and preparation of sodium sand by the sodium method is highly demanding, and the reaction between sodium and chlorobenzene is violent, which is likely to cause safety accidents such as explosions and fires; and The magnesium rule is relatively safe due to mild reaction conditions. However, in the titration process of phosphine trichloride, due to the high viscosity of the reactant and slow heat transfer, it is easy to cause side reactions, resulting in low product purity and low yield. Therefore, it is necessary to provide a solution. A new method to solve the problems of the magnesium method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] (1) Mix 26 parts of tetrahydrofuran and 80 parts of toluene in the reaction kettle evenly, drop 6 parts of magnesium chips from the manhole, seal the manhole, add 10 parts of phenylmagnesium chloride trigger solution, fill with nitrogen and exhaust oxygen, and repeat replacement twice; Heat to keep the temperature in the kettle at 80±5°C, add 220 parts of chlorobenzene dropwise at a constant speed under stirring, when the dropwise addition reaches one-third of the chlorobenzene, raise the temperature to 100°C and keep it for about 30 minutes, then cool down to 80°C ±5°C, continue to drop the remaining two-thirds of the chlorobenzene, maintain the temperature of the material at 80±5°C during the dropwise addition, slowly raise the temperature to 100°C until a slight reflux occurs, and keep the temperature for 4 hours, Cool it to 50°C and pump it into another reactor;

[0017] (2) Open enough cooling water, when the kettle is cooled to 50°C, add dropwise a mixture of 10 p...

Embodiment 2

[0027] (1) Mix 30 parts of tetrahydrofuran and 100 parts of toluene in the reactor, drop 7 parts of magnesium chips from the manhole, seal the manhole, add 10 parts of phenylmagnesium chloride trigger solution, fill with nitrogen and exhaust oxygen, and repeat replacement 3 times; Heat to keep the temperature in the kettle at 80±5°C, add 240 parts of chlorobenzene dropwise at a constant speed under stirring, when about 1 / 4 of chlorobenzene is added dropwise, raise the temperature to 105°C and keep it for about 30 minutes, then cool down to 80±5°C 5°C, continue to add the remaining 3 / 4 of the chlorobenzene dropwise, maintain the temperature of the material at 80±5°C during the dropwise addition, and slowly raise the temperature to 105°C until a slight reflux occurs, keep the temperature for 4 hours, and put it Cool to 70°C and pump into another reactor;

[0028] (2) Open enough cooling water, when the kettle is cooled to 50°C, add dropwise a mixture of 11 parts of phosphorus tr...

Embodiment 3

[0038] (1) Mix 35 parts of tetrahydrofuran and 120 parts of toluene uniformly in the reactor, drop 8.5 parts of magnesium chips from the manhole, seal the manhole, add 10 parts of phenylmagnesium chloride trigger solution, fill with nitrogen and exhaust oxygen, and repeat replacement 3 times; Heat to keep the temperature in the kettle at 80±5°C, add 260 parts of chlorobenzene dropwise at a constant speed under stirring, when about 1 / 3 of chlorobenzene is added dropwise, raise the temperature to 103°C and keep it for about 30 minutes, then cool down to 80±5°C 5°C, continue to add the remaining 2 / 3 of the chlorobenzene dropwise, maintain the material temperature at 80±5°C during the dropwise addition, slowly raise the temperature to 103°C until a slight reflux occurs, keep the temperature for 4 hours, Cool to 80°C and pump into another reactor;

[0039] (2) Open enough cooling water, when the kettle is cooled to 50°C, add dropwise a mixture of 12 parts of phosphorus trichloride ...

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PUM

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Abstract

The invention discloses a production method of triphenylphosphine, which belongs to the chemical field and is characterized by comprising the following steps of: evenly mixing tetrahydrofuran and toluene uniform, putting magnesium chips, adding initiating liquid, filling nitrogen and discharging oxygen; heating up to enable the temperature of the kettle maintain to be within a range of 80+ / -5 DEG C, dropwise adding chlorobenzen at a constant speed with stirring, heating and cooling, dropwise adding chlorobenzene continously, pumping into another reaction kettle; cooling the kettle, dropwise adding phosphorus trichloride, toluene and mixture of phosphorus trichloride and toluene; cooling and dropwise adding hydrochloric acid, standing and washing with water; heating and distilling tetrahydrofuran and toluene, ending vacuum distillation; cooling materials and separating triphenylphosphine out; adding toluene and triphenylphosphine, distilling toluene, filter-pressing the concentrated liquid into another vessel, adding methyl alcohol into the kettle, separating triphenylphosphine by crystallization, centrifugally separating and drying. The product obtained by the method has the advantages of high yield, high purity and low pollution, and overcomes the problem of low yield, high production cost and large pollution in the traditional magnesium method. At the same time, the production process of the method is safe.

Description

technical field [0001] The invention relates to a production method of triphenylphosphine, which belongs to the field of chemical industry. Background technique [0002] The purpose of the present invention is to invent a production method of triphenylphosphine with stable reaction, safety and environmental protection. At present, there are two main methods for producing triphenylene sand, the magnesium method and the sodium method, but the production and preparation of sodium sand by the sodium method is highly demanding, and the reaction between sodium and chlorobenzene is violent, which is likely to cause safety accidents such as explosions and fires; and The magnesium rule is relatively safe due to mild reaction conditions. However, in the titration process of phosphine trichloride, due to the high viscosity of the reactant and slow heat transfer, it is easy to cause side reactions, resulting in low product purity and low yield. Therefore, it is necessary to provide a so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/50
Inventor 于波王红军
Owner 山东九龙石化有限公司