Method for preparation of ketoxime compound and method for preparation of alkoxy-mine hydrochloride

A ketone compound and compound technology are applied in the field of preparation of ketoxime compounds, which can solve the problems of low conversion rate of ketoxime compounds, short service life of catalysts, low conversion rate of ketone compounds, etc. The effect of production costs

Active Publication Date: 2013-09-04
宁波四明化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] The first purpose of the present invention is in order to overcome existing operation risk in the preparation method of acetone oxime or butanone oxime, the service life of catalyst is shorter, the conversion

Method used

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  • Method for preparation of ketoxime compound and method for preparation of alkoxy-mine hydrochloride
  • Method for preparation of ketoxime compound and method for preparation of alkoxy-mine hydrochloride
  • Method for preparation of ketoxime compound and method for preparation of alkoxy-mine hydrochloride

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preparation example Construction

[0027] According to the first aspect of the present invention, the present invention provides a method for preparing a ketoxime compound, the method comprising: under the conditions of a ketoammoxime reaction, in the presence of a titanium-silicon molecular sieve catalyst, the ketone compound, peroxidized Hydrogen, water and ammonia are fed into the reactor for contact reaction, and the molar ratio of hydrogen peroxide to the ketone compound is 0.1 to less than 1.

[0028] According to the preparation method of the ketoxime compound provided by the present invention, the method preferably further includes: separating the titanium-silicon molecular sieve catalyst through the contact reaction and the catalyst containing ketoxime compound, ketone compound and A mixed liquid A of water, and separate the ketoxime compound and the mixed liquid B containing ketone compound and water from the mixed liquid A, and then return the mixed liquid B as part of the feed to the reactor to the ...

Embodiment approach

[0077] It can be seen from the above reaction formula (3) that another product of step (3) is the same substance as the ketone compound described in step (1), and in the catalytic rectification process, the ketone compound is obtained from the second rectification process. The top of the tower is discharged. In addition, since there is no additional organic solvent in the step (3), the ketone compound in the overhead distillate can be directly recycled in the step (1) after being concentrated or not, and the overhead distillate The presence of a small amount of HCl in the effluent is also conducive to stabilizing hydrogen peroxide in step (1). Therefore, according to another preferred embodiment of the present invention, the method further includes: recycling the overhead distillate of the second rectification tower with or without concentration as at least part of the distillate in step (1). ketone compounds. In this preferred embodiment, the ketone compound produced by the ...

Embodiment 1

[0086] This example is used to illustrate the preparation method of the ketoxime compound provided by the present invention.

[0087] Acetone, 27.5% by weight of hydrogen peroxide, ammonia, water and TS-1 molecular sieve catalyst (prepared according to the method of Example 1 in CN1301599A) are continuously injected into a 5L slurry bed reactor provided with a ceramic membrane separator, acetone, water The weight ratio of TS-1 molecular sieve catalyst (prepared according to the method of Example 1 in patent application CN1301599A) is 1:2:0.05, and the molar ratio of ammonia to acetone is 1.6:1. The molar ratio of hydrogen peroxide to acetone was 0.9:1, and then by controlling the feed flow and discharge flow of the slurry bed reactor, the reaction raw materials were kept at 50°C for 1 hour. At the same time, the reacted material discharged from the slurry bed reactor is separated into reacted TS-1 molecular sieve catalyst and reaction liquid through the ceramic membrane separa...

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Abstract

The present invention relates a method for preparation of ketoxime compound, comprising: feeding a ketone compound, hydrogen peroxide, water, and ammonia into a reactor for contact reaction under the conditions of oximation reaction of ketone and ammonia, in the presence of a titanium-silicon molecular sieve catalyst, wherein, the molar ratio of the hydrogen peroxide to the ketone compound is 0.1 or more and less than 1. The present invention also relates to method for preparation of alkoxy-amine hydrochloride, comprising the following steps: preparing ketoxime compound by using the method for preparation of ketoxime compound described above, preparing ketoxime ether compound from the ketoxime compound, and then feeding the ketoxime ether compound and hydrochloric acid solution respectively into a rectification tower continuously for catalytic distillation, and separating alkoxy-amine hydrochloride from the liquid of the tower bottom of the rectification tower. In the method for preparation of ketoxime compound provided in the present invention, the titanium-silicon molecular sieve catalyst has a long useful life; using the method for preparation of alkoxy-amine hydrochloride provided in the present invention, the target product can be obtained at high purity and high yield.

Description

technical field [0001] The invention relates to a preparation method of a ketoxime compound and a preparation method of alkoxyamine hydrochloride. Background technique [0002] Acetone oxime and butanone oxime have the advantages of low toxicity, environmental friendliness and high reducing performance, and are excellent reducing agents, which can replace the highly toxic N 2 h 4 It can be used as an oxygen scavenger and corrosion inhibitor for boilers, as an organic synthesis intermediate, a polyurethane sealant, and as a raw material for the synthesis of medicines, pesticides, dyes, and silicone coupling agents. [0003] For this reason, some patent applications have reported about the preparation method of acetone oxime and butanone oxime, for example, CN1556096A discloses a kind of technique that acetone or butanone oxidation produces acetone oxime or butanone oxime, and this technological process uses acetone or butanone, Ammonia and hydrogen peroxide are raw material...

Claims

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Application Information

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IPC IPC(8): C07C249/04C07C239/20
CPCC07C239/20C07C249/04C07C249/12Y02P20/10C07C251/38
Inventor 张胜建林勇
Owner 宁波四明化工有限公司
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