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Industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone

A technology of isophorone and isophoronenitrile, applied in the field of organic chemical synthesis, can solve problems such as difficult handling of solid cyanide-containing waste, high requirements for production equipment, and difficulty in industrialized production, and achieve low production cost and simple process , the effect of reducing production costs

Active Publication Date: 2013-11-27
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The defect of above invention is: one, the production of used raw material liquid hydrocyanic acid is very dangerous, and the requirement for the liquefaction technology of hydrogen cyanide gas and equipment safety performance is all very high, so there is very big difficulty in industrialized production
2. The basic catalyst used needs to be neutralized with an organic acid or an inorganic acid after the reaction, which will produce a large amount of salt deposits and require additional filtration equipment, which not only increases the operating procedures, but also produces difficult-to-handle solids containing Cyanide waste
3. A high-vacuum rectification tower is required for post-processing, which requires high production equipment and increases production costs

Method used

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  • Industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone
  • Industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone
  • Industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone

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Experimental program
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Effect test

Embodiment 1

[0028] Add 138g (1.0mol) of isophorone to a four-neck flask with stirring and a thermometer, raise the temperature to 100°C, add 4.3g (0.05mol) of acetone cyanohydrin, and feed hydrogen cyanide gas to control the amount of gas At 40g (1.5mol), keep the temperature at 100°C, react for 1 hour, cool down to 5°C, filter, and dry to obtain 153g of light yellow isophoronenitrile product with a content of 97.3% and a yield of 95.6%.

Embodiment 2

[0030] Add 138g (1.0mol) of isophorone to a four-necked flask with stirring and a thermometer, raise the temperature to 200°C, add 0.85g (0.01mol) of acetone cyanohydrin, and feed hydrogen cyanide gas to control the amount of gas At 33g (1.2mol), keep the temperature at 200°C, react for 0.5 hours, cool down to 0°C, filter, and dry to obtain 146.4g of light yellow isophoronenitrile product with a content of 95.3% and a yield of 93.2%.

Embodiment 3

[0032] Add 138g (1.0mol) of isophorone to a four-neck flask with stirring and a thermometer, raise the temperature to 150°C, add 1.7g (0.02mol) of acetone cyanohydrin, and feed hydrogen cyanide gas to control the amount of gas At 35g (1.3mol), keep the temperature at 150°C, react for 0.7 hours, cool down to -5°C, filter, and dry to obtain 152.8g of light yellow isophoronenitrile product with a content of 98.3% and a yield of 94.2%.

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Abstract

The invention relates to an industrial production method of 3-cyano-3,5,5-trimethylcyclohexanone, which comprises the following steps: reacting raw materials isophorone and gas hydrocyanic acid by using acetone cyanohydrin as a catalyst; and after the reaction is finished, cooling, and filtering to obtain the 3-cyano-3,5,5-trimethylcyclohexanone. The raw material hydrocyanic acid is introduced into the reaction system in a gas mode, thereby saving the step of production of liquid hydrocyanic acid; no alkaline catalyst is needed in the reaction process, so that neutralizing treatment is not needed after the reaction is finished, thereby avoiding generation of salt and reducing the operation; and thus, the method has the advantages of simpler procedure, lower production cost and higher operation safety.

Description

technical field [0001] The invention uses acetone cyanohydrin and gaseous hydrogen cyanide as raw materials to synthesize 3-cyano-3,5,5-trimethylcyclohexanone (isophorone nitrile), which belongs to the technical field of organic chemical synthesis. Background technique [0002] 3-cyano-3,5,5-trimethylcyclohexanone, commonly known as isophoronenitrile, is an important chemical intermediate. Isophorone nitrile is aminated and hydrogenated to generate isophorone diamine, and then further synthesize isophorone diisocyanate. This compound can be used in the preparation of epoxy resin, and can also be used as a crosslinking agent in polyurethane production. Coupling agent, hydroxyl stabilizer and special monomer. [0003] Usually, isophoronenitrile is prepared by the following method: isophorone and liquid hydrocyanic acid are reacted in the presence of a basic catalyst, and then enter a distillation column for rectification or purification by recrystallization, and finally obtai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/46C07C253/30
Inventor 张辰亮姚立国王学花王振宇魏利华邵爱军王少丹李娟
Owner HEBEI CHENGXIN
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