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Method and device for preparing caprolactam through Beckmann rearrangement of cyclohexanone oxime under catalysis of TFA (trifluoroacetic acid)

A technology for the rearrangement of cyclohexanone oxime and Beckmann catalyzed by trifluoroacetic acid, which is applied in the direction of organic chemistry, can solve the problem of by-product large ammonium sulfate, and achieve the effect of high concentration

Inactive Publication Date: 2018-01-09
沧州旭阳化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at the problem that a large amount of ammonium sulfate is by-produced in the process of producing a large amount of ammonium sulfate by neutralizing and crystallizing the rearrangement liquid obtained from the rearrangement reaction existing in the existing technology of cyclohexanone oxime to produce caprolactam to obtain 70 wt% crude caprolactam oil. Method and device for preparing caprolactam through Beckmann rearrangement of cyclohexanone oxime catalyzed by trifluoroacetic acid

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  • Method and device for preparing caprolactam through Beckmann rearrangement of cyclohexanone oxime under catalysis of TFA (trifluoroacetic acid)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] use as figure 1 The process shown in the experiment was carried out.

[0055] Acetonitrile and trifluoroacetic acid from trifluoroacetic acid and low-boiling aprotic substance storage tank were pressurized by a feed pump (not shown) at acetonitrile concentration of 0.3 wt%, and cyclohexanone oxime from cyclohexanone oxime storage tank was pressurized. Ketoxime (concentration after mixing with acetonitrile and trifluoroacetic acid is 1.9mol / L) is fully mixed in the static mixer, enters the ring distribution pipe at the bottom of the rearrangement reactor, is further fully mixed by the agitator, and Under the action of acid catalysis, the Beckmann rearrangement reaction is carried out; since the rearrangement reaction is an exothermic reaction, a cooling coil is installed inside the reactor, and cooling water is supplied to the inner coil through the cooling desalted water pump of the heat removal system, and the amount of cooling water is controlled The reaction tempera...

Embodiment 2

[0059] use as figure 1 The process shown in the experiment was carried out.

[0060] Acetonitrile and trifluoroacetic acid from trifluoroacetic acid and low-boiling aprotic substances storage tank were pressurized by a feed pump (not shown) at acetonitrile concentration of 5 wt%, and cyclohexanone from cyclohexanone oxime storage tank Oxime (concentration after mixing with acetonitrile and trifluoroacetic acid is 1.9mol / L) is fully mixed in the static mixer, and then enters the annular distribution pipe at the bottom of the rearrangement reactor, and is further fully mixed by the agitator, and in the acid Under the action of catalysis, the Beckmann rearrangement reaction is carried out; since the rearrangement reaction is an exothermic reaction, a cooling coil is installed inside the reactor, and cooling water is supplied to the inner coil through the cooling desalted water pump of the heat removal system, and the reaction is controlled by the amount of cooling water The temp...

Embodiment 3

[0064] use as figure 1 The process shown in the experiment was carried out.

[0065] Acetonitrile and trifluoroacetic acid from trifluoroacetic acid and low-boiling aprotic substances storage tank were pressurized by a feed pump (not shown) at acetonitrile concentration of 0.1 wt%, and cyclohexanone oxime from cyclohexanone oxime storage tank was pressurized. Ketoxime (concentration after mixing with trifluoroacetic acid and acetonitrile is 3mol / L) is fully mixed in the static mixer, enters the annular distribution pipe at the bottom of the rearrangement reactor, and is further fully mixed by the agitator, and in the acid Under the action of catalysis, the Beckmann rearrangement reaction is carried out; since the rearrangement reaction is an exothermic reaction, a cooling coil is installed inside the reactor, and cooling water is supplied to the inner coil through the cooling desalted water pump of the heat removal system, and the reaction is controlled by the amount of coolin...

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Abstract

The invention relates to a method and a device for preparing caprolactam through Beckmann rearrangement of cyclohexanone oxime under catalysis of TFA (trifluoroacetic acid). According to the method, alow-boiling-point non-protic substance is taken as a proton transfer agent, TFA is taken as a catalyst, cyclohexanone oxime is catalyzed at the temperature of 35-120 DEG C to be subjected to a Beckmann rearrangement reaction, caprolactam is prepared, a reactant is subjected to distillation separation, caprolactam, TFA and the low-boiling-point non-protic substance are obtained, and TFA and the low-boiling-point non-protic substance are returned to a reaction procedure for cyclic utilization. The process procedure is short, the reaction condition is mild, energy consumption is low, no ammoniumsulfate byproducts are produced, and the method and device are green and environmentally friendly; compared with conventional processes, an ammonium sulfate device is omitted, the caprolactam production cost can be effectively reduced, and a great significance is produced for production of caprolactam.

Description

technical field [0001] The invention relates to a method and a device for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime, in particular to a method and a device for preparing caprolactam by catalyzing the Beckmann rearrangement of cyclohexanone oxime with trifluoroacetic acid. Background technique [0002] Caprolactam is an important chemical monomer, which can be used in the synthesis of polymer products such as fibers, engineering plastics, and biaxially oriented nylon, and has high application value. The industrial production process of caprolactam includes the liquid phase rearrangement process catalyzed by oleum and the gas phase rearrangement process catalyzed by S-1. The two caprolactam production processes have their own advantages and disadvantages. [0003] Liquid-phase rearrangement process catalyzed by oleum: use oleum as a catalyst to catalyze the Beckmann rearrangement reaction of liquid cyclohexanone oxime at a temperature of about 110°...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10
Inventor 刘怡宏邢亚峰赵朋伟刘冬然霍增辉石峰
Owner 沧州旭阳化工有限公司
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