Method for preparing 3-cyan-3,5,5-trimethyl cyclohexanone

A technology of isophorone nitrile and isophorone, applied in hydrogen cyanide addition preparation, organic chemistry and other directions, can solve the problems of reduced rectification yield, impact on economic benefits, and high requirements for production equipment

Inactive Publication Date: 2010-10-06
四川省天然气化工研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] According to the prior art, for example: in the preparation of isophorone nitrile described in published patents such as US5091554, Te Zhao 2004-155785, US6822110B2, EP-A-394967, EP-A-042119, US6022988, US5254711, all adopt high Products are purified by vacuum rectification. These methods are mainly used in industrial production, and have the following disadvantages: on the one hand, the vacuum degree required for rectification products is 1 to 3 bar, and a high-vacuum rectification tower is required, which requires high production equipment; On the one hand, during the rectification process, some raw materials or products are polymerized, and the sediment generated during the neutralization process continues to accumulate in the tower, resulting in a decrease in the rectification yield; third, the increase in aggregates will inevitably lead to parking and cleaning, and a large number The parking time increases the production cycle and affects economic benefits

Method used

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  • Method for preparing 3-cyan-3,5,5-trimethyl cyclohexanone

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 276.4g (2.0mol) of isophorone to a four-neck flask equipped with a stirring, thermometer, and reflux condenser, raise the temperature to 100°C, add 2.0g of lithium hydroxide, and dropwise add 27.0g (1.0mol) of hydrocyanic acid , the dropping time is about 50 minutes, keep the temperature at 170° C., keep the temperature for 30 minutes after dropping, cool down to 100° C., add 10 g of p-toluenesulfonic acid, and sample and analyze the yield of isophorone nitrile is 99% (calculated as HCN ), after recovering 137.1 g of isophorone by distillation, 150 g of methanol and 3.5 g of activated carbon were added, refluxed for decolorization, filtered, cooled to -5°C for crystallization. Filter and dry to obtain 150.2 g of light yellow crystalline isophorone nitrile product with a content of 99.3% and a yield of 90.3% (calculated as HCN).

Embodiment 2

[0023] The operation was the same as in Example 1. After recovering 137.4 g of isophorone by distillation, 150 g of industrial ethanol and 3.5 g of activated carbon were added, refluxed for decolorization, filtered, cooled to -5°C for crystallization. filtered, dried to obtain light yellow).

Embodiment 3

[0025] The operation was the same as in Example 1. After recovering 137.4 g of isophorone by distillation, 150 g of dichloroethane and 3.5 g of activated carbon were added, refluxed for decolorization, filtered, and cooled to -5°C for crystallization. After filtering and drying, 150.0 g of a yellow crystal isophorone nitrile product was obtained, with a content of 99.0% and a yield of 89.9% (calculated as HCN).

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Abstract

The invention discloses a method for preparing 3-cyan-3,5,5-trimethyl cyclohexanone. The method comprises the following steps of: taking isophorone as a raw material and adding hydrocyanic acid into the isophorone to perform addition reaction at the high temperature of between 100 and 200 DEG C under the action of an alkali catalyst to produce a crude product of the 3-cyan-3,5,5-trimethyl cyclohexanone; reducing the temperature to 80 to 120 DEG C, adding at least one organic acid serving as a neutralizer and a stabilizer into the reaction mixture and adding an organic solvent or a mixed solvent of the organic solvent and water into the reaction mixture; performing crystallization by cooling and filtering the mixture so as to obtain the finished 3-cyan-3,5,5-trimethyl cyclohexanone. The method can greatly reduce the production cost and has simple industrialized process and easy operation.

Description

Technical field: [0001] The present invention relates to a kind of preparation method of isophorone nitrile. Background technique: [0002] 3-cyano-3,5,5-trimethylcyclohexanone, commonly known as isophorone nitrile, is an important intermediate in industry, amination hydrogenation converts isophorone nitrile into 1-amino -3-Amino-3,5,5-trimethylcyclohexane (isophorone diamine IPDA), this compound can be used as curing agent and crosslinking agent for epoxy resin coatings; corresponding diisocyanate can also be prepared ——Isophorone diisocyanate (IPDI), used as crosslinking agent, coupling agent, hydroxyl stabilizer and special monomer in polyurethane production. [0003] Generally, isophorone nitrile is prepared by the following method: isophorone and hydrocyanic acid are added in the presence of a basic catalyst to form isophorone nitrile, then neutralized by adding acid, and then enter the distillation tower Carry out rectification and purification. Its main reaction eq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/46C07C253/10
Inventor 王锋彭琼杨漫波马毅
Owner 四川省天然气化工研究院
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