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Preparation method of phosphonium salt

A technique of quaternary phosphonium salt and Grignard method is applied in the field of improvement of the preparation process of quaternary phosphonium salt, which can solve the problems of consuming manpower and material resources, tedious operation, affecting yield and the like, and achieves saving manpower and material resources, simplifying synthesis process and yield. improved effect

Inactive Publication Date: 2014-05-21
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the operation is relatively cumbersome, especially after the trialkylphosphine is synthesized by the Grignard method, cooling, hydrolysis, and liquid separation are required. On the one hand, this process is complicated to operate and consumes manpower and material resources. The increase of air-sensitive operation links will inevitably cause some side reactions and affect the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Under nitrogen protection, 9 grams of magnesium, 5.9 grams of chlorobutane and 100 mL of ether were added to a 1000 mL four-neck flask equipped with electric stirring, a thermometer, a constant pressure dropping funnel and a condenser tube, and then 28.8 grams of chlorobutane Add n-butane and 150mL xylene to the dropping funnel. Add a grain of iodine into the four-neck bottle, heat it to initiate and stabilize, and gradually drop the mixed solution of n-chlorobutane and xylene from the dropping funnel, heat and keep the reaction going on smoothly. After about two hours of reaction, the magnesium chips are basically The response is complete. Cool down to below 0°C, start dropwise adding a mixture of 15.5 g of phosphorus trichloride and 100 mL of xylene and keep the reaction temperature below 0°C. After dripping, start to heat up and distill out the ether at the same time. After most of the ether is evaporated, the temperature gradually rises to about 120°C. At this time...

Embodiment 2

[0017] Under nitrogen protection, 9 grams of magnesium, 5.9 grams of chlorobutane and 100 mL of ether were added to a 1000 mL four-neck flask equipped with electric stirring, a thermometer, a constant pressure dropping funnel and a condenser tube, and then 28.8 grams of chlorobutane Add n-butane and 150mL xylene to the dropping funnel. Add a grain of iodine into the four-neck bottle, heat it to initiate and stabilize, and gradually drop the mixed solution of n-chlorobutane and xylene from the dropping funnel, heat and keep the reaction going on smoothly. After about two hours of reaction, the magnesium chips are basically The response is complete. Cool down to below 0°C, start dropwise adding a mixture of 15.5 g of phosphorus trichloride and 100 mL of xylene and keep the reaction temperature below 0°C. After dripping, start to heat up and distill out the ether at the same time. After most of the ether is evaporated, the temperature gradually rises to about 120°C. At this time...

Embodiment 3

[0019] Under nitrogen protection, 9 grams of magnesium, 5.9 grams of chlorobutane and 100 mL of tetrahydrofuran were respectively added to a 1000 mL four-neck flask equipped with electric stirring, a thermometer, a constant pressure dropping funnel and a condenser tube, and then 28.8 grams of chlorinated Add n-butane and 150mL xylene to the dropping funnel. Add a grain of iodine into the four-neck bottle, heat it to initiate and stabilize, and gradually drop the mixed solution of n-chlorobutane and xylene from the dropping funnel, heat and keep the reaction going on smoothly. After about two hours of reaction, the magnesium chips are basically The response is complete. Cool down to below 0°C, start dropwise adding a mixture of 15.5 g of phosphorus trichloride and 100 mL of xylene and keep the reaction temperature below 0°C. After dripping, start to heat up the temperature and distill the tetrahydrofuran out at the same time. After most of the tetrahydrofuran is evaporated, th...

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Abstract

The invention relates to a preparation method of a phosphonium salt, in particular relates to improvement of a preparation process of a phosphonium salt. The preparation method is characterized by comprising the following steps: carrying out a reaction on an alkane Grignard reagent and phosphorous trichloride so as to generate trialkyl phosphine; directly adding alkyl halide in the reaction in the former step without hydrolysis and separation so as to synthesize the phosphonium salt; and finally, separating and purifying by utilizing a principle that the phosphonium salt can be transferred in an organic phase and a water phase under a certain condition. Compared with the existing technology that the phosphonium salt is synthesized by a Grignard method, the hydrolysis step after trialkyl phosphine is synthesized is omitted in the preparation method provided by the invention, thereby simplifying the synthesis process, saving labor power and material resources and avoiding the side reaction and loss which are possibly brought by a middle operation so that the yield is improved; and the final yield is up to about 80%.

Description

technical field [0001] The invention relates to the improvement of the preparation process of the quaternary phosphonium salt, and more particularly relates to a method for further reducing the production cost and improving the yield by simplifying the Grignard method for synthesizing the quaternary phosphonium salt process. Background technique [0002] Quaternary phosphonium salts can be used in solvents, bactericides, surfactants, catalysts and antistatic agents. [0003] The current method for synthesizing quaternary phosphonium salts is mainly prepared by direct heating reaction of trialkylphosphine and alkyl halide (Journal of Moleculer Catalysis A: Chemical, 256(1-2), 295-300; 2006). The preparation of trialkylphosphine can have different methods, there is preparation by addition reaction of olefin and phosphine (CN1069029), and preparation by Grignard reaction. Patent CN200310100174 discloses a method for synthesizing trialkylphosphine and further synthesizing quate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/54
Inventor 常卫星李靖
Owner NANKAI UNIV
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