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Catalytic Hydrotreating Process of Rectification Raffinate of Chloropivaloyl Chloride

A technology of chloropivaloyl chloride and catalytic hydrogenation, which is applied in the field of chemical technology, can solve the problems of high cost, low utilization rate of raw materials, environmental pollution, etc., and achieve the goal of reducing the generation of three wastes, saving production costs, and huge economic benefits Effect

Active Publication Date: 2022-03-25
山东民基新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, alkali neutralization requires a large amount of lye, and the biochemical treatment is difficult and costly. The incineration treatment requires high requirements and directly causes environmental pollution. The separation of products and impurities in the production of downstream products is the main problem, and the utilization rate of raw materials is also low.
[0004] Chinese patent CN 107721841 A discloses a method for recovering pivalic acid from pivaloyl chloride rectification raffinate, and directly converts pivaloyl chloride and pivalic anhydride in pivaloyl chloride rectification raffinate into pivalic acid, But there is no treatment process for the rectification raffinate of chlorpivaloyl chloride in the prior art, because the existence of chloride ion in the chlorpivaloyl chloride has an impact on hydrolysis, adopting existing hydrolysis condition hydrolysis effect is not good
[0005] At this stage, there is no relevant patent report on the recycling method of chlorpivaloyl chloride rectification raffinate. Based on the above problems, in order to improve production efficiency and waste construction, it is urgent to develop a chlorpivaloyl chloride rectification raffinate recycling method

Method used

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  • Catalytic Hydrotreating Process of Rectification Raffinate of Chloropivaloyl Chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of catalytic hydrotreating process of rectification raffinate of chlorpivaloyl chloride:

[0024] Add 1500kg of rectification residue of chlorpivaloyl chloride into the hydrolysis kettle, turn on the mechanical stirring, heat to 50°C under normal pressure, then add 285kg of water, add 5.7kg of manganese chloride tetrahydrate, and dissolve the manganese chloride tetrahydrate with water in advance. Control the temperature of the hydrolysis tank to react at 65°C for 1.5 hours, and let the layers stand for 0.5 hours. The black water-containing impurities are first separated from the lower layer, and then the crude chloropivalic acid is separated from the upper layer; the crude chloropivalic acid is sent to the composite catalyst The hydrogenation tower of Sn-Pd / C carries out catalytic hydrodechlorination reaction, the weight content of Sn in the composite catalyst Sn-Pd / C is 0.3%, the weight content of Pd is 0.5%, the temperature of catalytic hydrogenation reaction is...

Embodiment 2

[0030] A kind of catalytic hydrotreating process of rectification raffinate of chlorpivaloyl chloride:

[0031] Add 1500kg of chlorpivaloyl chloride rectification residue into the hydrolysis kettle, turn on the mechanical stirring, heat to 50°C under normal pressure, then add 285kg of water, add 5.4kg of manganese chloride tetrahydrate, and dissolve the manganese chloride tetrahydrate with water in advance. Control the temperature of the hydrolysis tank at 70°C for 1.5 hours, let stand and separate the layers for 0.5 hours, the lower layer first separates black water-containing impurities, and then separates the upper layer of crude chloropivalic acid; send the crude chloropivalic acid to the composite catalyst The hydrogenation tower of Sn-Pd / C carries out catalytic hydrodechlorination reaction, the weight content of Sn in the composite catalyst Sn-Pd / C is 0.3%, the weight content of Pd is 0.5%, the temperature of catalytic hydrogenation reaction is 130 ±10°C, pressure 0.22Mp...

Embodiment 3

[0036] A kind of catalytic hydrotreating process of rectification raffinate of chlorpivaloyl chloride:

[0037] Add 1500kg of rectification residue of chlorpivaloyl chloride into the hydrolysis kettle, start the mechanical stirring, heat to 50°C under normal pressure, then add 300kg of water, add 5.7kg of manganese chloride tetrahydrate, and dissolve the manganese chloride tetrahydrate with water in advance, Control the temperature of the hydrolysis tank to react at 65°C for 1.5 hours, and let the layers stand for 0.5 hours. The black water-containing impurities are first separated from the lower layer, and then the crude chloropivalic acid is separated from the upper layer; the crude chloropivalic acid is sent to the composite catalyst The hydrogenation tower of Sn-Pd / C carries out catalytic hydrodechlorination reaction, the weight content of Sn in the composite catalyst Sn-Pd / C is 0.3%, the weight content of Pd is 0.5%, the temperature of catalytic hydrogenation reaction is 1...

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Abstract

The invention belongs to the technical field of chemical technology, and in particular relates to a catalytic hydrogenation treatment process for rectification raffinate of chlorpivaloyl chloride. Add water and a hydrolysis aid to the rectification raffinate of chlorpivaloyl chloride for hydrolysis. The hydrolysis aid uses one or two of manganese chloride tetrahydrate or nickel chloride hexahydrate. After the hydrolysis is completed, the layers are separated, and the upper layer The crude product of chloropivalic acid is transferred to a hydrogenation tower for catalytic hydrogenation reaction to obtain the crude product of pivalic acid, and the crude product of pivalic acid is rectified to obtain the finished product of pivalic acid. The hydrolysis aids are manganese chloride tetrahydrate and nickel chloride hexahydrate. In the present invention, high-purity pivalic acid is prepared by converting the rectification raffinate of chlorpivaloyl chloride, and the rectification raffinate of chlorpivaloyl chloride is no longer treated as hazardous waste, fully realizing the resource utilization of waste; It reduces waste discharge, reduces the generation of three wastes, reduces the environmental protection pressure of enterprises, and reduces the production cost of products at the same time, resulting in huge economic benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical technology, and in particular relates to a catalytic hydrogenation treatment process for rectification raffinate of chlorpivaloyl chloride. Background technique [0002] Chloropivaloyl chloride, also known as 3-chloro-2,2-dimethylpropionyl chloride (CPC), is a colorless, transparent and irritating liquid, used as a pharmaceutical and pesticide intermediate, and can be used to synthesize the pesticide oxadiazon . [0003] There are three main treatment methods for the distillation raffinate of acidic chlorpivaloyl chloride: incineration treatment, high-temperature alkaline neutralization post-biological treatment, and the use of the main components contained in it to produce downstream products. Among them, alkali neutralization requires a large amount of lye, and the biochemical treatment is difficult and costly. The incineration treatment requires high requirements and directly causes environme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/377C07C53/124C07C51/42
CPCC07C51/04C07C51/377C07C51/42C07C53/19C07C53/124
Inventor 韦兵张海朋李建军杨中原李萍林苗苗王建芹祝新涛张瑞扈世琳陈凯黄超鹏
Owner 山东民基新材料科技有限公司
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