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Preparation method of triphenylphosphine

A technology of triphenylphosphine and triphenylphosphine dichloride, applied in the field of triphenylphosphine preparation, can solve the problems of high process risk, high market price, excess active aluminum powder and the like, and achieves high process safety, The effect of sufficient market supply and low cost

Active Publication Date: 2022-01-11
HUNAN JINGSHI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

After triphenylphosphine is used in the wittig reaction, it becomes triphenylphosphine oxide as a by-product; if triphenylphosphine oxide is treated as waste residue, not only the treatment cost is high, but also it is difficult to treat the phosphorus content in the three wastes to environmental protection standards below standard
The disadvantage is that the market price of 1,1,3,3-tetramethyldisiloxane is relatively high, a large amount of polydimethylsiloxane needs to be properly disposed of after the reaction, and the environmental protection cost is high
The disadvantage is: if lithium aluminum hydride is used for reduction in the second step, the cost of raw materials is high; if aluminum powder (sheet) is used for reduction, although the cost is low, the aluminum powder (sheet) needs to be more than 3 times in excess to have a higher production cost. The conversion rate of active aluminum powder (sheet) is relatively large and it is difficult to recycle and apply it, so it can only be disposed of by adding acid; the waste of active aluminum powder (sheet) is more, and hydrogen gas is generated during post-treatment after adding acid, which increases the risk of process during production. Larger, and produce a huge amount of aluminum salts, not environmentally friendly

Method used

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  • Preparation method of triphenylphosphine
  • Preparation method of triphenylphosphine
  • Preparation method of triphenylphosphine

Examples

Experimental program
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preparation example Construction

[0059] The embodiment of the present invention provides the present invention provides a kind of preparation method of triphenylphosphine, comprises the following steps:

[0060] Sodium trimethoxy borohydride is prepared by reacting trimethoxy borohydride sodium with triphenylphosphine dichloride to obtain triphenylphosphine.

[0061] It also includes: reacting sodium hydride and trimethyl borate to obtain a reaction solution of sodium trimethoxy borohydride; adding the obtained reaction solution of sodium trimethoxy borohydride dropwise to solution 1 to react to obtain triphenyl base phosphine. Described solution one is the triphenylphosphine dichloride solution containing catalytic amount of aluminum trichloride or stannous chloride.

[0062] It also includes: adding sodium hydride and solvent A to the reaction bottle 1; then cooling down to -50-10°C under the protection of nitrogen, and stirring evenly at -50-10°C under the condition of heat preservation, and then adding s...

experiment example 1

[0105] 1.1. Add 20 g (0.5 mol) of 60% sodium hydride and 80 g of anhydrous tetrahydrofuran into a 250 ml reaction bottle one. Under nitrogen protection, stir and cool down to 0-10°C. Then maintain nitrogen protection, stirring and liquid temperature 0-10°C, dropwise add 57.2g (0.55mol) of trimethyl borate; after the dropwise addition, continue to keep warm at 0-10°C and stir for 1 hour.

[0106] 1.2. Add 74.9g (0.225mol) of triphenylphosphine dichloride and 300g of tetrahydrofuran to another 1000ml reaction flask II, and control the temperature at 0-10°C under nitrogen protection and stirring. Then first add 0.375g of stannous chloride; then stir at 0-10°C under temperature control, and dropwise add the reaction mixture obtained in 4.1.1. After the dropwise addition, continue to keep warm at 0-10°C for 15 hours. Then, it was filtered at room temperature to remove the insoluble matter (sodium chloride) produced by the reaction.

[0107] 1.3, the filtrate gained in 1.2 is con...

experiment example 2

[0109] 2.1. Add 20 g (0.5 mol) of 60% sodium hydride and 120 g of anhydrous 2-methyltetrahydrofuran into 1000 ml reaction flask one. Under the protection of nitrogen, stir and cool down to -50~-40°C. Then maintain nitrogen protection, stirring and liquid temperature -50~-40°C, dropwise add a mixture of 208g (2mol) of trimethyl borate and 200g of 2-methyltetrahydrofuran; continue to keep warm at -50~-40°C after the dropwise addition Stir for 5 hours.

[0110] 2.2. Add 66.6g (0.2mol) of triphenylphosphine dichloride and 533g of 2-methyltetrahydrofuran / trimethyl borate mixture to another 2000ml reaction flask II, and control under nitrogen protection and stirring. Temperature -20~-10℃. Then add 3.33g of anhydrous aluminum trichloride first; then stir at -20 to -10°C under temperature control, and dropwise add the reaction mixture obtained in 4.2.1. After the dropwise addition, continue to keep warm at -20~-10°C for 3 hours. Then filter at -20 to -10°C to remove the insoluble ...

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Abstract

The invention provides a preparation method of triphenylphosphine. The preparation method comprises the following steps of: preparing trimethoxy sodium borohydride, and making the trimethoxy sodium borohydride react with triphenylphosphine dichloride to obtain the triphenylphosphine; performing a reaction on sodium hydride and trimethyl borate so as to obtain a trimethoxy sodium borohydride reaction solution; and dropwise adding the obtained trimethoxy sodium borohydride reaction solution into a solution I, and performing reaction to obtain triphenylphosphine. The method provided by the invention has the advantages of high triphenylphosphine acquisition rate, high purity and environmental protection.

Description

technical field [0001] The invention relates to the technical field of triphenylphosphine preparation, in particular to a preparation method of triphenylphosphine. Background technique [0002] Triphenylphosphine is a chemical raw material with a wide range of uses, and is widely used in the wittig reaction process in industries such as medicine and chemical industry, and catalyst ligands and the like. After triphenylphosphine is used in the wittig reaction, it becomes triphenylphosphine oxide as a by-product; if triphenylphosphine oxide is treated as waste residue, not only the treatment cost is high, but also it is difficult to treat the phosphorus content in the three wastes to environmental protection standards below standard. Therefore, the technology of reducing triphenylphosphine oxide to obtain triphenylphosphine has also been extensively studied and applied. [0003] 1.2. At present, there are mainly two kinds of industrial methods for reducing and preparing triph...

Claims

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Application Information

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IPC IPC(8): C07F9/50
CPCC07F9/5022
Inventor 宋斌龚秦丽邓伟强
Owner HUNAN JINGSHI NEW MATERIAL CO LTD
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