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Regeneration method of triphenyl phosphine oxide

A technology of triphenylphosphine oxide and triphenylphosphine, which is applied in the field of chemical production and resource recycling, can solve the problems of no industrial value, complex process, high cost, etc., and achieve cheap and easy mass production, simple process operation, and high yield. rate-enhancing effect

Inactive Publication Date: 2010-06-23
北京金源化学集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] These studies and methods have important reference value in the regeneration of triphenylphosphine oxide, but considering the yield, regeneration process conditions, production cost, secondary pollution, etc., or the process is complex, or the yield is low, or the cost is high, Or regeneration by-product pollution, currently has no industrial value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 56Kg of triphenylphosphine oxide into the reactor, start stirring, and raise the temperature to 250°C, and at this temperature, HCL gas is fed in at a constant rate. In addition, 12Kg of 60-mesh silicon powder and 1Kg of cuprous chloride were mixed, and ball milled in a hydrogen atmosphere for 2 hours. The powder samples after ball milling were slowly added to the reactor in batches, and after about 5 hours, the reaction of the raw materials was controlled by TLC until the raw materials were completely reacted. Cool down to about 120°C and add toluene, stir for 0.5 hours and cool down to room temperature, filter with suction, the solid residue can be used for the synthesis of white carbon black, the filtrate is decolorized with activated carbon, precipitated from the solvent, and recrystallized with methanol to obtain 48Kg of the product triphenylphosphine.

Embodiment 2

[0018] Put 56Kg TPPO and 2Kg adipic acid into the reactor, start stirring, and raise the temperature to 270°C. In addition, 6Kg of 200-mesh silicon powder, 0.5Kg of cuprous oxide, and 0.5Kg of anhydrous copper sulfate were taken, mixed, and ultrasonically treated for 10 minutes in a hydrogen atmosphere. The silicon powder mixed sample was slowly added to the reactor in batches, and after about 3 hours, the reaction of the raw materials was controlled by TLC until the raw materials were completely reacted. Cool down to about 90°C and add ethanol, stir for 0.5 hours and lower to 70°C, filter with suction, add activated carbon to the filtrate for decolorization. Suction filtration while it was hot, and triphenylphosphine crystallized when the temperature was lowered to obtain 45Kg of the product triphenylphosphine.

Embodiment 3

[0020] Put 56Kg of TPPO into the reactor, start stirring, and raise the temperature to 260°C. In addition, take 6Kg of 300-mesh silicon powder, 0.1Kg of nano-cuprous oxide, and 0.3Kg of anhydrous ferric chloride, and mix them with high temperature and strong stirring at 300°C for 30 minutes. The silicon powder mixed sample was slowly added to the reactor in batches, and hydrofluoric acid was added dropwise at the same time. After about 4 hours, the reaction of the raw materials was controlled by TLC until the raw materials were completely reacted. Cool down to about 90°C and add ethanol, stir for 0.5 hours and lower to 70°C, filter with suction, add activated carbon to the filtrate for decolorization. Suction filtration while it was hot, and triphenylphosphine crystallized when the temperature was lowered to obtain 46Kg of the product triphenylphosphine.

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PUM

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Abstract

The invention relates to the resource recovery technology for reducing and regenerating triphenyl phosphine oxide into triphenyl phosphine. In the invention, silicon powder is taken as a regenerative reagent to reduce and regenerate the triphenyl phosphine oxide, and raw materials are cheap, are easy to obtain and have simple reaction, simple operation, high yield and less byproduct, wherein the yield can reach above 85 percent. A process is particularly suitable for large-scale and middle-scale industrial production and not only effectively solves the problem of cycle use of the triphenyl phosphine oxide during the production, but also has practical meaning to other production taking the triphenyl phosphine oxide as basic raw materials.

Description

technical field [0001] The invention relates to a technology for reducing and regenerating triphenylphosphine oxide into triphenylphosphine, and belongs to the technical field of chemical production and resource recycling. Background technique [0002] Triphenylphosphine is a widely used raw material for organic synthesis, such as reagents for the preparation of Witting and Rydon reactions, ligands for homogeneous catalysts, accelerators, heat stabilizers, light stabilizers, anti- Oxygen agents, corrosion inhibitors, flame retardants, antistatic agents and processing aids, etc., play an important role in industrial production (Edited by Xu Kexun, "Fine Organic Chemical Raw Materials 6 Intermediates Manual", 5-10). However, a large amount of triphenylphosphine oxide, a by-product produced during use, is highly toxic, seriously polluting, and cumbersome to deal with, and the general treatment methods such as burning and landfilling will also bring serious secondary pollution. ...

Claims

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Application Information

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IPC IPC(8): C07F9/50
CPCY02P20/584
Inventor 张和平陈朝晖邱明建张雅丽李海滨于淑利赵磊于冰何琼
Owner 北京金源化学集团有限公司
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