Aryl phosphine chloride production waste residue treatment process

A technology for aryl phosphine chloride and treatment process, which is applied in the field of diphenyl phosphine chloride production waste residue treatment process, can solve the problems of a large amount of waste residue, cannot be reused, and is sensitive to external conditions, and achieves good economic benefits, low cost, The effect of simple operation process

Active Publication Date: 2018-06-12
CHANGSHANG NEWSUN CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Method 4) The cost of ionic liquid synthesis is high and sensitive to external conditions, it is easy to fail, not only cannot be reused, but also produces a large amount of waste residue, post-processing is more difficult than method 1)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) 100kg of arylphosphine chloride production waste residue is pulverized so that the particle size reaches below 50 mesh;

[0024] (2) Under the cooling of the jacket circulating water, put the pulverized waste residue into 200kg of n-butanol in batches and stir for 2h at room temperature, press filter to obtain 53.0kg of filter residue and 250L of n-butanol filtrate;

[0025] (3) filter residue is sent into roasting furnace, and roasting temperature is 200 ℃, obtains Potassium Chloride 49.7kg;

[0026] (4) 250L of n-butanol filtrate was slowly dropped into 500L of 10% hydrochloric acid solution for hydrolysis, the hydrolysis temperature was controlled not to exceed 50°C, and the organic phase and the aqueous phase were obtained after the hydrolysis was completed and left standing for liquid separation;

[0027] (5) Gained aqueous phase distillation concentrates and obtains product crystalline aluminum chloride 47kg, and concentrated gained hydrochloric acid solution ...

Embodiment 2

[0030] (1) 100kg of arylphosphine chloride production waste residue is pulverized so that the particle size reaches below 50 mesh;

[0031] (2) Under the cooling of the jacket circulating water, put the pulverized waste residue into 300kg of n-butanol in batches and stir for 2h at room temperature, press filter to obtain 50.8kg of filter residue and 400L of n-butanol filtrate;

[0032] (3) filter residue is sent into roasting furnace, and roasting temperature is 200 ℃, obtains potassium chloride 48.9kg;

[0033] (4) The n-butanol filtrate is slowly dripped into 800L 10% hydrochloric acid solution for hydrolysis, the hydrolysis temperature is controlled to be no more than 80° C., and the organic phase and the aqueous phase are obtained after the hydrolysis is completed and left to stand for liquid separation;

[0034] (5) Gained aqueous phase distillation concentrates and obtains product crystalline aluminum chloride 48.2kg, and concentrated gained hydrochloric acid solution is...

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Abstract

The invention discloses an aryl phosphine chloride production waste residue treatment process, and particularly a diphenyl phosphine chloride production waste residue treatment process. According to the process, aluminium chloride is separated from potassium chloride by utilizing different solubility of the aluminium chloride and the potassium chloride in n-butyl alcohol; the recycled potassium chloride can be re-utilized directly as a complexing agent; aluminum chloride crystals obtained after hydrolysis can also be sold out directly as a product; a small amount of organic distillation residue is outsourced for treating.

Description

technical field [0001] The invention relates to a process for treating the production waste residue of arylphosphine chloride, in particular to a process for treating the production waste residue of diphenylphosphine chloride. technical background [0002] Diphenylphosphine chloride is an important intermediate for the preparation of photoinitiator TPO, and its demand will increase day by day. Due to the special physical characteristics of diphenylphosphine chloride, the preparation process is cumbersome, and it is difficult to realize large-scale industrial production. , a large number need to rely on imports. At present, the main manufacturers of diphenylphosphine chloride in the country include Qingdao Fuslin Chemical Technology Co., Ltd.; Shandong Hongyu Chemical Co., Ltd., etc. The preparation of diphenylphosphine chloride mainly has the following preparation methods : [0003] 1) Conventional production method: take benzene, phosphine trichloride, anhydrous aluminum c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/04C01F7/56B09B3/00
CPCC01D3/04C01F7/56B09B3/80
Inventor 叶正培辜艳华周谭
Owner CHANGSHANG NEWSUN CHEM IND
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