Joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime

A technology of cyclohexanone oxime and production process, which is applied in the field of organic chemical raw material production, can solve the problems of high production cost, unfriendly environment, complicated process, etc., so as to reduce production cost and energy consumption, reduce the deketone process, and improve the selection sexual effect

Active Publication Date: 2017-08-25
河北美邦工程科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In order to solve the problems of complex traditional process, low conversion rate, high by-product, high production cost, and unfriendly environment, the present invention adopts the combined process of cyclohexanone ammoximation and cyclohexanone hydroxaminization to produce cyclohexanone oxime, Then the generated cyclohexanone oxime is partially hydrolyzed to obtain an aqueous hydroxylamine solution. On the one hand, the aqueous hydroxylamine solution is sent to the cyclohexanone hydroxylamine oximation reactor to participate in the reaction; Hydroxylamine salt

Method used

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  • Joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime
  • Joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime
  • Joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] process such as figure 1 shown.

[0050] (1) Ammoximation reaction of cyclohexanone

[0051] Raw material cyclohexanone (mass purity 96%), ammonia, hydrogen peroxide molar ratio of 1:0.92:0.90, TS-1 catalyst concentration of 2.0% (wt) were added to the ammoximation reactor, at 80°C, 0.4MPa (G ), a heterogeneous ammoximation reaction takes place under the condition of 60rpm, the stirring speed is 60rpm, and the reaction mixture is obtained after 30 min of reaction, and then the catalyst is separated to obtain the reaction solution B;

[0052] (2) Cyclohexanone hydroxylamine oximation reaction

[0053] Add the reaction solution B obtained in step (1) and an appropriate amount of hydroxylamine into the hydroxylamine oximation reactor. Under the conditions of 20°C, 0.1MPa(G), and a stirring speed of 60rpm, the unconverted cyclohexanone and hydroxylamine in the reaction solution B are generated. Reaction, after reacting for 30min, reaction solution C was obtained; the con...

Embodiment 2

[0063] process such as figure 2 shown.

[0064] (1) Ammoximation reaction of cyclohexanone

[0065] Raw material cyclohexanone (mass purity 97%), ammonia, hydrogen peroxide molar ratio of 1:0.93:0.91, TS-2 catalyst concentration of 3.0% (wt) were added to the ammoximation reactor, at 85°C, 0.5MPa (G ), a heterogeneous ammoximation reaction takes place under the condition of 70rpm, the stirring speed is 70rpm, and the reaction mixture is obtained after reacting for 50 min, and then the catalyst is separated to obtain the reaction solution B;

[0066] (2) Cyclohexanone hydroxylamine oximation reaction

[0067] Add the reaction liquid B obtained in step (1) and an appropriate amount of hydroxylamine into the hydroxylamine oximation reactor. Under the conditions of 25°C, 0.2MPa(G), and a stirring speed of 70rpm, the unconverted cyclohexanone and hydroxylamine in the reaction liquid B are generated. Reaction, after reacting for 50min, reaction solution C was obtained; the conve...

Embodiment 3

[0077] process such as image 3 shown.

[0078] (1) Ammoximation reaction of cyclohexanone

[0079] Raw materials cyclohexanone (mass purity 98%), ammonia, hydrogen peroxide in a molar ratio of 1:0.94:0.92, TiO 2 The catalyst concentration is 4.0% (wt) and it is added into the ammoximation reactor, and the heterogeneous ammoximation reaction occurs at 90°C, 0.6 MPa(G), and the stirring speed is 90 rpm, and the reaction mixture is obtained after 80 minutes of reaction , and then the catalyst is separated to obtain the reaction solution B;

[0080] (2) Cyclohexanone hydroxylamine oximation reaction

[0081] Add the reaction solution B obtained in step (1) and an appropriate amount of hydroxylamine into the hydroxylamine oximation reactor, and unconverted cyclohexanone and hydroxylamine in the reaction solution B under the conditions of 40°C, 0.3MPa(G), and a stirring speed of 90 rpm Reaction occurs, and reaction solution C is obtained after reacting for 80 min; the conversio...

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Abstract

The invention discloses a joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime. The material comprises the steps that reaction liquid obtained by raw materials through an ammoximation reaction and a hydrooximation reaction is extracted and separated to obtain an organic phase, the organic phase is prepared into product cyclohexanone-oxime, or part of the organic phase and part of product cyclohexanone-oxime are adopted as raw materials for an oxime hydrolysis reaction to be hydrolyzed, the organic phase in hydrolysis liquid is circulated to return to a oximation reactor, part of an inorganic phase in the hydrolysis liquid is adopted as a raw material to be circulated to return to a hydroxylamine oximation reactor, and the other part of the inorganic phase is prepared into a hydroxylamine aqueous solution and hydroxylammonium salt. The joint production technology of hydroxylamine, hydroxylammonium salt and cyclohexanone-oxime is simple in procedure, the requirement of the ammoximation reaction for the purity of the raw material cyclohexanone and the catalyst performance is lowered, a high quality cyclohexanone-oxime product without cyclohexanone is obtained, the simplification of the downstream caprolactam technology and the improvement of the product quality are benefited, and the hydroxylamine and hydroxylammonium salt product which have high additional value are obtained simultaneously.

Description

technical field [0001] The invention relates to a production process of an organic intermediate, in particular to a production process of cyclohexanone oxime for co-producing hydroxylamine and hydroxylamine salt, and belongs to the technical field of organic chemical raw material production. Background technique [0002] Cyclohexanone oxime is an important organic fine chemical, a key intermediate for the synthesis of caprolactam, and a monomer for the synthesis of nylon-6 and engineering plastics. In recent years, with the continuous expansion of caprolactam demand and production capacity, its production scale has expanded rapidly, and cyclohexanone oxime has a huge market space. The prior art industrial methods for producing cyclohexanone oxime mainly include cyclohexanone direct hydroxylamine salt oximation method and cyclohexanone ammoximation method catalyzed by TS-1 molecular sieve. The direct hydroxylamine salt oximation method of cyclohexanone refers to the non-cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C249/08C07C249/14C07C251/44C01B21/14
CPCC01B21/1454C07C249/04C07C249/08C07C249/14C07C251/44
Inventor 宛捍东高文杲王延吉张东升张玉新王晓曼
Owner 河北美邦工程科技股份有限公司
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