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Method for recycling triphenyl phosphine oxide and triphenylphosphine from waste slag

A technology for triphenylphosphine oxide and triphenylphosphine, which is applied in the field of recycling triphenylphosphine oxide and triphenylphosphine, can solve the problems of high equipment requirements, inability to use, and incompatibility with the basic conditions of domestic enterprises, etc. Achieve the effect of high product purity, low cost, great implementation value and potential social and economic benefits

Inactive Publication Date: 2009-07-15
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] This technical route has high requirements for equipment and strict operation, which does not meet the basic conditions of domestic enterprises, and domestic enterprises are unable to adopt related technologies

Method used

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  • Method for recycling triphenyl phosphine oxide and triphenylphosphine from waste slag
  • Method for recycling triphenyl phosphine oxide and triphenylphosphine from waste slag
  • Method for recycling triphenyl phosphine oxide and triphenylphosphine from waste slag

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take the waste residue and wash it with sulfuric acid with a mass concentration of 5%, and then dry it in an oven. Weigh 10g of waste residue and make it all dissolve with 100mL chlorobenzene, use liquid chromatography (HPLC) to measure that the mass content of triphenylphosphine is 25% and the mass content of triphenylphosphine oxide is 50%, and slowly add 1.5g of it dropwise under stirring Concentrated sulfuric acid with a mass concentration of 98%, after the dropwise addition, the reaction was continued for 1 hour. Filtration obtained a white filter residue with a melting point of 178.6-179.0°C. The filtrate was washed with 30mL saturated sodium bicarbonate solution until it was neutral, and then spin-dried to obtain a light yellow solid. The light yellow solid was recrystallized with petroleum ether to obtain 2.1g of white triphenylphosphine. The melting point of the product triphenylphosphine was 78.8- 79.4°C, HPLC purity 99.1%, recovery rate 84%. Add 45mL chloro...

Embodiment 2

[0031] Take the waste residue and wash it with sulfuric acid with a mass concentration of 1%, and then dry it in an oven. Weigh 10g of waste residue with a mixture of 10mL of chlorobenzene and 90mL of acetone to dissolve it completely, and use HPLC to determine that the mass content of triphenylphosphine is 25% and the mass content of triphenylphosphine oxide is 50%, and slowly add 1.2g of it dropwise under stirring Concentrated sulfuric acid with a mass concentration of 98%, after the dropwise addition, the reaction was continued for 1 hour. Filtration obtained a white filter residue with a melting point of 177.8-178.7°C. The filtrate was washed with 30 mL of saturated sodium bicarbonate solution to neutrality, and then spin-dried to obtain 2.3 g of white triphenylphosphine. The melting point of the product triphenylphosphine was 78.7-79.5° C., the HPLC purity was 99.1%, and the recovery rate was 92%. Add 45mL chlorobenzene and 45mL saturated sodium bicarbonate solution to t...

Embodiment 3

[0033] Take the waste residue and wash it with sulfuric acid with a mass concentration of 8%, and then dry it in an oven. Weigh 100g waste residue and make it all dissolve with 1000mL chlorobenzene, use HPLC to measure that the mass content of triphenylphosphine is 25% and the mass content of triphenylphosphine oxide is 50%, and slowly add 15g of phosphine with a mass concentration of 98% under stirring. Concentrated sulfuric acid, after the dropwise addition was completed, the reaction was continued for 1 hour. Filtration obtained a white filter residue with a melting point of 178.4-179.6°C. The filtrate was washed with 300mL saturated sodium bicarbonate solution until it was neutral, and then spin-dried to obtain a light yellow solid. Recrystallize the light yellow solid with petroleum ether to obtain 22g of white triphenylphosphine. The melting point of the product triphenylphosphine is 79.8-80.4°C , HPLC purity 99.3%, recovery rate 88%. Add 450mL chlorobenzene and 450mL ...

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Abstract

The invention relates to a method for recovering triphenylphosphine oxide and triphenylphosphine from waste residue. The method comprises the following processes: drying the waste residue washed with inorganic acid, completely dissolving the waste residue with an organic solvent, slowly adding concentrated sulfuric acid to dissolved solution dropwise, stirring and filtering to obtain filter residue and filtrate; adding sodium bicarbonate solution to the filtrate to obtain neutral solution, spin drying and recrystallizing with the organic solvent to obtain the triphenylphosphine; and adding the organic solvent and the sodium bicarbonate solution for extraction and spin drying an obtained organic layer to obtain the triphenylphosphine oxide. The method can help recover the triphenylphosphine and the triphenylphosphine oxide with the weight percentage of about 90% and about 97% respectively, has the advantages of low cost, high yield, environmental protection, simple industrialized operation, high product purity and the like, and effectively solves problems of complex operation, high energy consumption, low yield, severe environmental pollution and the like, thus having greater application value and potential social and economical benefits.

Description

technical field [0001] The invention relates to a recovery method, in particular to a method for recovering triphenylphosphine oxide and triphenylphosphine from waste residue. Background technique [0002] Triphenylphosphine oxide is a main by-product formed in the chemical production process, especially the Wilkinson catalyst for the homogeneous catalytic hydrogenation of olefins and the Wittig reaction. Triphenylphosphine oxide is highly toxic and cannot be directly discharged or buried, otherwise it will cause environmental pollution. The domestic basic method for this kind of waste treatment is to evaporate the waste liquid from the solution and store it. This method consumes a lot of energy but cannot achieve the purpose of complete separation. Triphenylphosphine is widely used in organic synthesis. It is not only an important chemical raw material, but also a ligand for homogeneous catalysts in petrochemical and fine chemical production. It can also be used as an acce...

Claims

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Application Information

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IPC IPC(8): C07F9/50C07F9/53
Inventor 杨泽慧李陵岚邵丹凤周国权王庭恭
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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