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Novel process for synthesizing oxime through in-situ generated ammonia

An in-situ generation, ammonia synthesis technology, applied in the preparation of oxime, organic chemistry and other directions, can solve the problems of affecting the recycling of catalysts, catalyst destruction, unavoidable side reactions, etc., to achieve high product yield, strong operability, The effect of simple post-processing process

Active Publication Date: 2017-06-27
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, for the ammoximation process of the ammoxidation method, there are currently the following problems: (1) the utilization rate of the raw material ammonia is low, and side reactions are difficult to avoid; (2) the concentrated ammonia solution of the ammoximation reaction has damage to the catalyst effect, affecting the continuous and stable circulation of the catalyst

Method used

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  • Novel process for synthesizing oxime through in-situ generated ammonia
  • Novel process for synthesizing oxime through in-situ generated ammonia
  • Novel process for synthesizing oxime through in-situ generated ammonia

Examples

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Effect test

Embodiment 1

[0031] Add 36g butanone (0.5mol), 535g mass concentration of 5% ammonium chloride aqueous solution (0.5mol), 2% catalyst TS-1 into the flask, start the stirrer, adjust to a suitable stirring rate. The temperature gradually rose to 60°C, and at the same time, 145.75g of 20% sodium carbonate (0.275mol) aqueous solution and 27.3% of hydrogen peroxide 65.4g (0.525mol) were added dropwise, and the dropwise addition time was 3h; after the dropwise addition, the reaction was continued for 2h, and the reaction ended After cooling to room temperature, the catalyst was filtered out, and 43.4 g of butanone oxime was obtained by gas chromatography analysis with a yield of 99.7%.

Embodiment 2～3

[0033] Butanone is replaced by acetone or cyclohexanone, and all the other are with embodiment 1. The yields of the products acetone oxime and cyclohexanone were determined by gas phase to be 99.6% and 99.9% respectively.

Embodiment 4～8

[0035] The operating steps and operating conditions for synthesizing butanone oxime in Example 1 are the same, except that the strong base and weak acid salt and the ammonium salt are different. Determined by gas phase analysis, the yield of butanone oxime is shown in Table 1.

[0036] The butanone oxime yield of table 1. embodiment 4~8

[0037] Ammonium salt with a mass fraction of 5% 20% mass fraction of strong base and weak acid salt Yield / % Example 4 ammonium chloride potassium carbonate 99.4 Example 5 ammonium sulfate Sodium carbonate 99.8 Example 6 ammonium sulfate potassium carbonate 99.5 Example 7 Ammonium acetate Sodium carbonate 99.6 Example 8 Ammonium acetate potassium carbonate 99.5

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Abstract

The invention discloses a novel process for synthesizing oxime through in-situ generated ammonia. The novel process is characterized in that ammonium salt and strong alkali and weak acid salt generate ammonia in situ, and then the ammonia reacts with ketone and hydrogen peroxide under catalysis of a titanium silicalite molecular sieve. The synthetic process has the advantages of simple oximation reaction, mild reaction conditions, few by-products, high product yield and environmentally friendliness. The synthesizing method is simple, an aftertreatment process is simple and convenient and has very strong operability and repeatability, and industrial production is promoted.

Description

technical field [0001] The invention relates to a synthesis process of oxime, in particular to a new process for synthesizing oxime by generating ammonia in situ. It belongs to the technical field of organic synthesis. Background technique [0002] Oxime is an organic compound formed by the action of carbonyl-containing aldehydes and ketones and hydroxylamine, and the general formula has a C=NOH group. Oximes formed from aldehydes are called aldoximes, and oximes formed from ketones are called ketoximes. Oxime can be hydrolyzed to obtain the original aldehyde or ketone. [0003] Oxime can undergo a rearrangement reaction to generate amides. Caprolactam, the raw material for industrial production of nylon, is obtained by rearrangement reaction of oxime generated from cyclohexanone. Some oximes can be used as analytical reagents, antioxidants, passivators, etc. [0004] At present, there are two main synthetic routes of oxime: (1) hydroxylamine method, the method of prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/04C07C251/44C07C251/38
CPCC07C249/04C07C251/44C07C251/38
Inventor 岳涛邢文国陈贵军杨旭王瑞菲卢福军冯维春翟云鸽
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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