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Method for preparing caprolactam through gas phase Beckmann rearrangement of cyclohexanone-oxime gas

A technology of Beckmann rearrangement and cyclohexanone oxime, which is applied to the preparation of lactams, chemical instruments and methods, molecular sieve catalysts, etc., can solve the problem that the crushing strength is not high enough, the conversion rate of cyclohexanone oxime is not high enough and the selectivity of caprolactam is not high enough. problem, to achieve the effect of high conversion rate and continuous production

Active Publication Date: 2014-07-02
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0010] The purpose of the present invention is to overcome the insufficient crushing strength of the molecular sieve catalyst containing the MFI structure in the prior art, the conversion rate of cyclohexanone oxime and the selection of caprolactam when it is used for the gas phase Beckmann rearrangement of cyclohexanone oxime to prepare caprolactam In order to solve the disadvantages of not being high enough, it provides a method for preparing caprolactam by gas-phase Beckmann rearrangement of cyclohexanone oxime with high catalyst crushing strength, high conversion rate and high selectivity of caprolactam

Method used

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  • Method for preparing caprolactam through gas phase Beckmann rearrangement of cyclohexanone-oxime gas

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example 1

[0038] The preparation process of all-silicon-1 molecular sieve: Pour ethyl orthosilicate (abbreviated as TEOS) into a beaker at room temperature, stir for 30 minutes, and use 22.5% tetrapropylammonium hydroxide (abbreviated as TPAOH) solution Add it to tetraethyl orthosilicate, stir and hydrolyze for 3 to 5 hours at room temperature, add water to form a sol, stir evenly, and obtain a molar concentration of TPAOH / SiO 2 =0.2,EtOH / SiO 2 =4,H 2 O / SiO 2 =20 mixture, move the above mixture into a stainless steel reactor lined with polytetrafluoroethylene, crystallize at 100°C for 3 days, filter, wash, and dry at 120°C for 24 hours to obtain a full silicon- 1 molecular sieve (referred to as RBS-1).

[0039] (1) Put 2kg of 200-500 mesh RBS-1 in the turntable molding machine. The diameter of the turntable used in the turntable molding machine is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 50°, and the speed of the turntable ...

example 2

[0044] (1) Crush 2kg of HTS-1 (aluminum-free TS-1 molecular sieve with MFI structure, produced by Hunan Jianchang Petrochemical Co., Ltd., a commercial brand, with a molecular sieve solid content of about 85%) into 200-500 meshes, and place in In the turntable forming machine, the turntable diameter of the turntable rotary forming machine used is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 46°, and the rotation speed of the turntable is set at 28rpm. Spray about 1.5 kg of deionized water therein to obtain spherical particles with a diameter of about 0.2 to 0.6 mm.

[0045] (2) Separately crush the HTS-1 molecular sieve into 200-600 mesh, mix it with 30% alkaline silica sol (pH value 9-10) at a weight ratio of 2.0:1 and re-pulverize it, and take the particles smaller than 20 mesh Add 120kg to the turntable molding machine at a constant speed, finish adding within 180min, and sieve through 13 mesh and 10 mesh sieves to ob...

example 3

[0051] (1) 2kg 200-500 mesh RS-1 (manufactured by Hunan Jianchang Petrochemical Co., Ltd., commercial brand, molecular sieve solid content 85%). Place it in a turntable forming machine, wherein the turntable diameter of the turntable rotary forming machine used is 1.2m, the depth of the turntable is 450mm, the inclination angle of the turntable is determined to be 50°, and the rotation speed of the turntable is set at 30rpm. Spray about 1.5 kg of deionized water therein to obtain spherical particles with a diameter of about 0.2-0.8 mm.

[0052] (2) In addition, crush RS-1 molecular sieve into 200-800 mesh, mix it with 30% alkaline silica sol at a weight ratio of 2.2:1 and crush it again, take particles smaller than 30 mesh and add 120kg to the turntable molding machine at a constant speed, Finish adding within 240min. Sieve through 12-mesh and 9-mesh sieves to obtain spherical catalysts with a diameter of 1.7 to 2.2 mm and about 90 kg of wet balls. The remaining wet balls wit...

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Abstract

The invention provides a method for preparing caprolactam through gas phase Beckmann rearrangement of cyclohexanone-oxime gas. According to the method, under the condition of rearrangement reaction, cyclohexanone-oxime is in contact with a catalyst, and the catalyst is obtained by the steps of forming a molecular screen with an aluminum-free MFI (Melt Flow Index) structure, and enabling the molecular screen to be in contact with an alkaline buffer solution of a nitrogen-containing compound. The method is high in cyclohexanone-oxime conversion rate, and is capable of realizing long-period and continuous production; the selectivity of caprolactam is capable of reaching 95.8 percent.

Description

technical field [0001] The invention relates to a method for preparing caprolactam by gas-phase Beckmann rearrangement of cyclohexanone oxime. Background technique [0002] Caprolactam is the main raw material for the production of three series of products including nylon, industrial cord and nylon engineering plastics, and its demand has been relatively strong. The caprolactam is generally obtained by Beckmann rearrangement of cyclohexanone oxime. At present, the liquid phase rearrangement process using concentrated sulfuric acid or oleum as a catalyst is usually used in industry. The caprolactam produced by this process accounts for about 90% of the total production of caprolactam in the world, but this process needs to consume a large amount of sulfuric acid and ammonia water. Generally, 1.3-1.8 tons of ammonium sulfate will be produced as a by-product for every ton of caprolactam produced, and the production cost is relatively high. In addition, the use of sulfuric aci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/10C07D201/04B01J29/035
CPCC07D201/04C07D223/10B01J29/035B01J29/89B01J2229/38B01J35/51Y02P20/52
Inventor 程时标张树忠谢丽慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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