Environment-friendly synthesis method for diphenyl phosphine chloride

A technology of diphenylphosphine chloride and a synthesis method, which is applied in chemical instruments and methods, aluminum compounds, compounds of Group 5/15 elements of the periodic table, etc., can solve problems such as pollution of the environment, and reduce pollution and production time short, yield-enhancing effect

Inactive Publication Date: 2012-04-04
GANSU RES INSTION OF CHEM IND GRICI +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] The purpose of the present invention is to provide an environmentally friendly synthesis method of diphenylphosphine ch...

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  • Environment-friendly synthesis method for diphenyl phosphine chloride

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Embodiment 1

[0029] 1. Add 137.7g (1.0mol) of phosphorus trichloride, 78g (1.0mol) of benzene and 160.2g (1.2mol) of aluminum trichloride into the three-necked flask respectively, pass in nitrogen protection, stir vigorously, and heat up to 140- 150°C, keep reflux (a large amount of white smoke is released at this time). When the white smoke disappears, start to cool down to room temperature.

[0030] 2. Post-processing operations:

[0031] After adding heptane to the above reaction solution and stirring for 0.5 h, β-triethyl chlorophosphate was added dropwise, and the addition was completed after 0.5 h. Stir for 1.0h and let stand for 1.0h. Separate the lower β-triethyl chlorophosphate layer, and distill the heptane layer under reduced pressure. The crude diphenylphosphine chloride (CDPP) was obtained with a content of about 98% and a small amount of complexes, and the yield was 92.5-95.5%. The crude product was distilled under high vacuum to obtain pure diphenylphosphine chloride (CD...

Embodiment 2

[0036] 1. Add 137.7g (1.0mol) of phosphorus trichloride, 78g (1.0mol) of benzene and 173.3g (1.3mol) of aluminum trichloride into a three-necked flask respectively, pass in nitrogen protection, stir vigorously, and heat up to 140- 150°C, keep reflux (a large amount of white smoke is released at this time). When the white smoke disappears, start to cool down to room temperature.

[0037] 2. Post-processing operations:

[0038] After adding heptane to the above reaction solution and stirring for 0.5 h, β-triethyl chlorophosphate was added dropwise, and the addition was completed after 0.5 h. Stir for 1.0h and let stand for 1.0h. Separate the lower β-triethyl chlorophosphate layer, and distill the heptane layer under reduced pressure. The crude diphenylphosphine chloride (CDPP) was obtained with a content of about 98% and a small amount of complexes, and the yield was 92.5-95.5%. The crude product was distilled under high vacuum to obtain pure diphenylphosphine chloride (CDPP...

Embodiment 3

[0042] 1. Add 137.7g (1.0mol) of phosphorus trichloride, 78g (1.0mol) of benzene and 133.3g (1.0mol) of aluminum trichloride into the three-necked flask respectively, pass in nitrogen protection, stir vigorously, and heat up to 140- 150°C, keep reflux (a large amount of white smoke is released at this time). When the white smoke disappears, start to cool down to room temperature.

[0043] 2. Post-processing operations:

[0044] After adding heptane to the above reaction solution and stirring for 0.5 h, β-triethyl chlorophosphate was added dropwise, and the addition was completed after 0.5 h. Stir for 1.0h and let stand for 1.0h. Separate the lower β-triethyl chlorophosphate layer, and distill the heptane layer under reduced pressure. The crude diphenylphosphine chloride (CDPP) was obtained, with a content of about 98%, and a small amount of complexes, with a yield of 85.5-91.5%. The crude product was distilled under high vacuum to obtain pure diphenylphosphine chloride (CD...

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Abstract

The invention discloses an environment-friendly synthesis method for diphenyl phosphine chloride and aims to solve the problem of environmental pollution in the conventional process. The method comprises the following steps of: adding phosphorus trichloride, benzene and aluminium trichloride into a three-mouth bottle respectively; introducing nitrogen for protection; stirring intensely; heating to 140 to 150 DEG C; maintaining reflux; discharging a large amount of white smoke until the white smoke disappears; cooling to room temperature; and performing aftertreatment operation comprising the steps of adding an organic solvent into reaction liquid in the step A, stirring for 0.5 hour, adding a decomplexing agent beta-chlorophosphate triethyl ester dropwise for 0.5 hour, stirring for 1.0 hour, standing for 1.0 hour, removing the lower layer of the decomlexing agent layer, distilling the organic solvent layer under reduced pressure to obtain a crude product diphenyl phosphine chloride, and distilling the crude product diphenyl phosphine chloride under high vacuum to obtain the pure product diphenyl phosphine chloride. By the method, the aluminium trichloride is recovered through an environment-friendly idea, so environmental pollution is reduced, a byproduct is increased, and yield is increased. The method is high in yield, low in cost and short in reaction time.

Description

technical field [0001] The invention relates to an environment-friendly synthesis method of diphenylphosphine chloride. Background technique [0002] Chlorodiphenylphosphine, Ph 2 PCl) is an important diphenylphosphine reagent, which can be combined with active hydrogen-containing compounds (such as HNRR 1 , HOR) reaction, and can also react with lithium metal to prepare Ph 2 P － , to synthesize various Ph-containing 2 P — Group compounds. Contains Ph 2 P group compounds can be used as ligands of transition metals and metal carbonyls, and are often used in catalytic hydrogenation, asymmetric hydrogenation, carbonylation, oligomerization and other reactions. But the preparation of Ph 2 The operation of PCl is cumbersome and the conditions are harsh. At present, there is no large-scale production in China, and most of them rely on imports, which are expensive. [0003] Prepare Ph 2 PCl is usually prepared in a two-step process: [0004] Dichlorophenylphosphine (Ph ...

Claims

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Application Information

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IPC IPC(8): C07F9/52C01F7/26
Inventor 韩庆荣张鹏云王琴赵坤李春新
Owner GANSU RES INSTION OF CHEM IND GRICI
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