Regenerating method of waste thionyl chloride

A technology of thionyl chloride and polyacrylamide, which is applied in the field of purification of thionyl chloride and regeneration of waste thionyl chloride, can solve the problem of complex thionyl chloride composition, high investment in rectification equipment, and energy consumption of rectification process High-level problems, to achieve the effect of fast adsorption speed, low investment and low consumption

Active Publication Date: 2018-08-24
LUDONG UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The impurity contained in the newly produced thionyl chloride is mainly sulfur monochloride, and the impurity content is very low. The purpose of product purification is achieved by rectification. The rectification process has high energy consumption and high design cost. Due to the Strong corrosiveness, high investment in rectification equipment
Thionyl chloride recovered after acid chlorination has complex components, including impurities in reactants, unreacted organic acids, by-produ

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: a kind of regeneration method of waste sulfur oxychloride, it comprises the steps:

[0020] Weigh 5g of anionic polyacrylamide and 5g of mordenite in the presence of 0.3g of silane coupling agent KH550 to prepare polyacrylamide / zeolite cross-linked composite adsorption material; The waste thionyl chloride produced by the acyl chloride production process was placed in a 100mL agitator, mixed evenly, and adsorbed for 60 minutes; vacuum distillation was carried out at 78°C to obtain 99.6% of the first-grade product thionyl chloride, with a recovery rate of 90% %.

Embodiment 2

[0021] Embodiment 2: a kind of regeneration method of waste sulfur oxychloride, it comprises the steps:

[0022] Weigh 150g of cationic polyacrylamide and 300g of beta zeolite in the presence of 4.5g of silane coupling agent KH570 to prepare cationic polyacrylamide / zeolite cross-linked composite adsorbent material. The waste thionyl chloride was placed in a 50L stirrer, mixed evenly, adsorbed for 90 minutes, and subjected to vacuum distillation at 78°C to obtain 99.7% first-grade thionyl chloride with a recovery rate of 98%.

Embodiment 3

[0023] Embodiment 3: a kind of regeneration method of waste sulfur oxychloride, it comprises the steps:

[0024] Weigh 5kg of cationic polyacrylamide and 10kg of beta zeolite in the presence of 150g of silane coupling agent KH550 to prepare cationic polyacrylamide / zeolite cross-linked composite adsorbent material. The waste thionyl chloride produced by chemical production process was placed in a 10 cubic meter agitator to make it evenly mixed, adsorbed for 120 minutes, and carried out vacuum distillation at 78°C to obtain 99.8% first-grade product thionyl chloride, the recovery rate 99%.

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Abstract

The invention discloses a regenerating method of waste thionyl chloride. A polyacrylamide/zeolite crosslinking compound adsorption material is prepared from polyacrylamide and zeolite in the absence of a coupling agent, the polyacrylamide/zeolite crosslinking compound adsorption material and waste thionyl chloride are placed in a mixer at normal temperature to be evenly mixed, adsorption is conducted for 60-120 min, depressurized distilling is conducted at 78 DEG C, and the first-grade thionyl chloride with the concentrationof 99.5% is obtained. The problems that waste thionyl chloride is highin recovery energy consumptiom, the process is complex and the environment is polluted are solved; the waste thionyl chloride recovery method which is low in cost, simple in production process, beneficial for industrialization and free of pollution is provided and can be used for recovering the waste thionyl chloride generated in different acylating chlorination production processes.

Description

Technical field: [0001] The invention relates to a regeneration method of waste thionyl chloride, in particular to a purification technology of thionyl chloride which is selectively adsorbed by a polyacrylamide / zeolite cross-linked composite adsorption material and then distilled, and belongs to the technical field of environmental protection. Background technique: [0002] Thionyl chloride is an important fine chemical raw material, widely used in medicine, pesticide, dye industry and organic synthesis industry. The production of acid chloride products is generally to reflux the acid with excess thionyl chloride, and then evaporate the excess thionyl chloride to obtain acid chloride. In the production process, the excess thionyl chloride will be recovered, but the recycled Because sulfoxide contains impurities, its quality is seriously reduced, and it cannot be used in the production of acid chlorides. It can only be disposed of as waste liquid, causing a lot of pollution, ...

Claims

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Application Information

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IPC IPC(8): C01B17/45B01J20/26B01J20/30
CPCB01J20/267C01B17/4584C01P2006/80
Inventor 邢国秀刘诗丽杨正龙
Owner LUDONG UNIVERSITY
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