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Technological method for synthesizing ketoxime

A process method and a technology for synthesizing ketoxime, applied in oxime preparation, organic chemistry, etc., can solve problems such as dissolution and loss of catalyst active elements, impact on catalyst recycling, unreasonable raw material reaction ratio, etc., to avoid pollution and separation problems, The effect of improving material utilization and improving stability

Active Publication Date: 2017-06-13
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, for the continuous operation of the ammoximation process, there are currently the following problems: (1) the raw material reaction ratio is unreasonable, the waste of raw materials is serious, and the conversion rate is low; (2) the concentrated ammonia solution of the ammoximation reaction is easily Lead to the dissolution and loss of active elements in the catalyst, affecting the continuous and stable recycling of the catalyst

Method used

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  • Technological method for synthesizing ketoxime
  • Technological method for synthesizing ketoxime
  • Technological method for synthesizing ketoxime

Examples

Experimental program
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Effect test

Embodiment 1

[0032] First configure NaHCO with pH=10 3 Add 50g of aqueous solution into the three-necked flask, then add 2g of TS-1 catalyst, 80g of cyclohexanone in sequence, and the temperature of the water bath is 50°C. Insert the pH meter detection electrode, start stirring, and feed ammonia and hydrogen peroxide at the same time. 10g, the feeding time is 1 hour, the rate of passing hydrogen peroxide is kept at 1.2:1 with the molar ratio of ammonia water, until the pH value is restored from 12 during the reaction to the initial pH value = 10, continue to keep warm for 5 hours, and stop the reaction. After cooling to room temperature, the upper light phase is taken out to obtain the product oxime, part of the lower water phase is released, and 70% of the water is removed by rotary evaporation, and then returned to the reactor to continue recycling. The gas chromatogram of its product is shown in figure 1 .

Embodiment 2

[0034] First configure NaHCO with pH=9 3 Add 50g of aqueous solution into the three-necked flask, then add 2g of TS-1 catalyst, 87g of acetone in sequence, the temperature of the water bath is 70°C, insert the detection electrode of the pH meter, start stirring, and feed ammonia gas and hydrogen peroxide at the same time, the amount of ammonia gas feeding is 10g , the feeding time is 1 hour, the rate of passing hydrogen peroxide is kept at 1.2:1 with the molar amount of ammonia water, until the pH value is restored from 12 in the reaction process to the initial pH value = 9, continue to keep warm for 5 hours, and stop the reaction. After cooling to room temperature, the upper light phase is taken out to obtain the product oxime, part of the lower water phase is released, and 70% of the water is removed by rotary evaporation, and then returned to the reactor to continue recycling.

Embodiment 3

[0036] First configure Na with pH=12 2 CO 3 Add 50g of aqueous solution into the three-necked flask, then add 2g of TS-1 catalyst, 90g of methyl ethyl ketone in sequence, the temperature of the water bath is 50°C, insert the pH meter detection electrode, start stirring, and feed ammonia and hydrogen peroxide at the same time, the amount of ammonia gas is 10g, the feeding time is 1 hour, the rate of passing hydrogen peroxide is kept at 1.2:1 with the molar amount of ammonia water, until the pH value returns from 13 during the reaction to the initial pH value = 12, continue to keep warm for 5 hours, and stop the reaction. After cooling to room temperature, the upper light phase is taken out to obtain the product oxime, part of the lower water phase is released, and 70% of the water is removed by rotary evaporation, and then returned to the reactor to continue recycling.

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Abstract

The invention discloses a technological method for synthesizing ketoxime. In a system of a carbonate water solution, a titanium silicalite molecular sieve is adopted as a catalyst, and ketone, ammonia and hydrogen peroxide react to generate ketoxime; the pH value of the reaction system is monitored in real time in the reaction process to judge the reaction process and determine the optimal reaction ratio. The pH value in the reaction system is monitored to judge the reaction process and determine the optimal reaction ratio, and then the pH value of the system is adjusted through a carbonate water solution in order to increase the reaction rate and the conversion rate of ammonia.

Description

technical field [0001] The invention relates to a synthesis method, in particular to a process for synthesizing ketoxime, and belongs to the technical field of organic synthesis. Background technique [0002] Since the existing ammoximation reaction process needs to add water-miscible low-carbon alcohols, such as tert-butanol as a solvent, but the selected solvent cannot stably exist in the oleum system, and must undergo multiple distillations before the rearrangement reaction In separation processes such as extraction and extraction, there are generally disadvantages such as complex process, high energy consumption, and poor stability of oxime solution. Patent CN200510032184 discloses an improved ammoximation technology, using two heterogeneous reaction integration processes, the solvent used in the Beckmann rearrangement reaction is the same as that used in the oximation reaction, and the solvent can be stable in the rearrangement system containing oleum There is no react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/08C07C251/42C07C251/38
CPCC07C249/08C07C251/42C07C251/38C07C249/04C07C249/14
Inventor 岳涛杨旭邢文国陈琦陈贵军卢福军冯维春翟云鸽
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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