Device and method for preparing acetoxime

A technology of acetone oxime and heating device, which is applied in oxime preparation, chemical instruments and methods, chemical recovery, etc., can solve the problems of difficult separation and recovery of catalysts, achieve good application value, reduce wear and loss, and shorten the process flow

Inactive Publication Date: 2012-06-20
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
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  • Claims
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Problems solved by technology

[0005] The present invention provides a device and method for preparing acetone oxime, aiming at the problem that the catalyst is difficult to separate and recycle in the current research on powder TS-1 molecular sieve catalyzed acetone ammoxidation to synthesize acetone oxime. It has short process flow, simple structure, easy installation and practicality. Strong and other characteristics

Method used

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  • Device and method for preparing acetoxime
  • Device and method for preparing acetoxime
  • Device and method for preparing acetoxime

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] in such as figure 1 Acetone oxime is prepared in the device, and three monolithic TS-1 catalysts are vertically stacked in the reaction section 8 of the monolithic reactor 10; the characteristic of the cordierite carrier is that the upper bottom radius r: the lower bottom radius R: the height H is 1.5:1 : 2.5; the coating amount of its active component TS-1 molecular sieve of each monolithic TS-1 catalyst is 12% of the carrier mass; the molar ratio of acetone, tert-butanol, water, ammonia and hydrogen peroxide is 1: 1.5 :5:2:1.2; liquid space velocity is 0.5h -1 ; The reaction temperature is 70 ° C; the reaction time is 2h. The conversion of acetone was 89%, and the selectivity of acetone oxime was 79%.

Embodiment 2

[0042] in such as figure 1 Acetone oxime is prepared in the device, and four monolithic TS-1 catalysts are vertically stacked in the reaction section 8 of the monolithic reactor 10; the characteristic of the cordierite carrier is that the upper bottom radius r: the lower bottom radius R: the height H is 1.5:1 : 2.0; the coating amount of its active component TS-1 molecular sieve of each monolithic TS-1 catalyst is 12% of the carrier mass; the molar ratio of acetone, tert-butanol, water, ammonia and hydrogen peroxide is 1: 1.5 :5:2:1.2; liquid space velocity is 0.5h -1 ; The reaction temperature is 70 ° C; the reaction time is 2h. The conversion of acetone was 92%, and the selectivity of acetone oxime was 85%.

Embodiment 3

[0044] in such as figure 1 Acetone oxime is prepared in the device, and four monolithic TS-1 catalysts are vertically stacked in the reaction section 8 of the monolithic reactor 10; the characteristic of the cordierite carrier is that the upper bottom radius r: the lower bottom radius R: the height H is 1.5:1 : 2.0; the coating amount of its active component TS-1 molecular sieve of each monolithic TS-1 catalyst is 10% of the carrier mass; the molar ratio of acetone, tert-butanol, water, ammonia and hydrogen peroxide is 1:2 : 3: 2.4: 1.5; liquid space velocity is 0.5h -1 ; The reaction temperature is 70 ° C; the reaction time is 2h. The conversion of acetone is 90%, and the selectivity of acetone oxime is 82%.

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Abstract

The invention belongs to the technical field of chemical industry and relates to a device and a method for preparing acetoxime. The acetoxime is prepared from acetone, tertiary butanol, water, ammonia water and hydrogen peroxide by using an integrated TS-1 molecular sieve as a catalyst (an integrated titanium silicalite molecular sieve serves as a catalyst) and through liquid solid phase acetone ammoxidation. The device comprises a condenser, an integrated reactor and an external circulation pump. The integrated TS-1 catalyst (the integrated titanium silicalite molecular sieve serves as the catalyst) synthesized by using frustum-shaped cordierite as a carrier is loaded in the integrated reactor and is applied to preparation of the acetoxime. By adoption of the frustum-shaped cordierite carrier in the device, the wall flow phenomenon can be effectively avoided, so that activity of the catalyst and catalytic efficiency of the reactor are greatly improved. By the device and the method, the problem that the traditional powdered catalyst is difficult to recycle is solved. The device and the method have a wide market application prospect.

Description

technical field [0001] The invention relates to a device and method for preparing acetone oxime, belonging to the technical field of chemical industry. Background technique [0002] Acetone oxime, also known as dimethyl ketone oxime, is an antioxidant with excellent performance, has the characteristics of low toxicity, environmental friendliness and high reducibility, and can be used as an important additive in the passivation solution after pickling of boilers in thermal power plants. and operating water, can replace highly toxic N 2 h 4 It can be used as an oxygen scavenger and corrosion inhibitor for boilers, and can also be used as an intermediate in organic synthesis. It is an important chemical raw material. [0003] Its traditional production process generally uses hydroxylamine (hydroxylamine sulfate or hydroxylamine hydrochloride), acetone and ammonia water to react to synthesize acetone oxime. These processes generally use a slurry bed reactor. This method has co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J8/00C07C251/38C07C249/08
CPCY02P20/584
Inventor 马瑞平王媛媛张云郝丛张向京
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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