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Cyclododecanol preparation method

A technology of cyclododecanol and cyclododecene, applied in the field of preparation of cyclododecanol, can solve problems such as difficulty in taking into account the utilization rate and selectivity of hydrogen peroxide in oxidation reaction, adverse effects of separation and purification, and explosion of peroxide, and the like. Conducive to safe operation, green reaction process, and the effect of promoting complete conversion

Inactive Publication Date: 2020-01-14
CHINA TIANCHEN ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In US6043383, cyclododecene and hydrogen peroxide can achieve epoxidation reaction under specific weak acid conditions. This oxidation system is difficult to take into account the utilization rate and selectivity of hydrogen peroxide in the oxidation reaction, and there is also a risk of peroxide explosion.
And the by-products of bis-epoxidation and other high-boiling products have adverse effects on separation and purification

Method used

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  • Cyclododecanol preparation method
  • Cyclododecanol preparation method
  • Cyclododecanol preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 3L autoclave, add 1.0Kg of cyclododecene, 100g of tert-butanol, 100g of water, 10g of H-ZSM-5, blow nitrogen gas at 0.01MPa, raise the temperature to 100°C, and monitor the reaction for 6 hours. The oil and water were separated, and then the unreacted cyclododecene and the crude product were removed under reduced pressure, and the rectification separation obtained cyclododecanol with a conversion rate of 45% (GC content of 99.5%) and a yield of 84%.

Embodiment 2

[0031] In a 50L high-pressure reactor, add 1.0Kg of cyclododecene, 10Kg of tert-amyl alcohol, 2Kg of water, 10Kg of H-β molecular sieves, feed argon gas at 10.0MPa, raise the temperature to 250°C, and monitor the reaction for 4 hours. Oil and water were separated, and then the unreacted cyclododecene and the crude product were decompressed to obtain cyclododecanol with a conversion rate of 75% (GC content of 99.5%) and a yield of 86%.

Embodiment 3

[0033] In a 5L high-pressure reactor, add 1.0Kg of cyclododecene, 1Kg of polyethylene glycol dimethyl ether, 500g of water, 100g of macroporous sulfonic acid resin, feed carbon monoxide at 1MPa, raise the temperature to 120°C, and maintain the reaction for 3 hours. After the reaction, the oil and water were separated, and then the unreacted cyclododecene and the crude product were removed under reduced pressure, and the rectification and separation obtained cyclododecanol with a conversion rate of 70% (GC content of 99.5%) and a yield of 89%.

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Abstract

The invention provides a cyclododecanol preparation method, which comprises: 1) stirring and mixing cyclododecene, an organic solvent, water and a catalyst, wherein the catalyst is a solid acid, and aweight ratio of the cyclododecene to the organic solvent to the water to the catalyst is 1:(0.1-10):(0.1-2):(0.01-10); and 2) introducing gas to achieve a certain pressure, and gradually raising thetemperature to a certain temperature in a gas atmosphere, wherein the gas pressure is maintained at 0.01-10 MPa, and the reaction temperature is maintained at 100-250 DEG C. According to the method ofthe invention, the cyclododecanol can be prepared through hydration at a high yield, the yield reaches 64-91%, and the catalyst has no obvious change after being recycled 50 times.

Description

technical field [0001] The invention belongs to the technical field of chemical materials, and in particular relates to a preparation method of cyclododecanol. Background technique [0002] Cyclododecanol is a key intermediate for the preparation of macrocyclic muskone and long carbon chain special nylon, specific products such as 3-methylcyclopentadecone, racemic muskone, cyclopentadecanone lactone, 5-cyclohexadecanone Enone, cyclopentadecanone, 12-methyl-14-carbonylbicyclo[9,3,1]pentadecane, dodecanedioic acid, dodecanediamine, nylon 12, nylon 1212, nylon 612, nylon 12T, Nylon 1012. [0003] The first industrialization route of cyclododecanol uses cyclododecene to react with an oxidant to prepare epoxycyclododecane, followed by a hydrogenation process. In the US4469880 patent report, it is mentioned that a metal borate is used as a catalyst and oxygen is used as an oxygen source to carry out an epoxidation reaction process of cyclododecane. The conversion rate of raw mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/04C07C35/205
CPCC07C29/04C07C2601/20C07C35/205
Inventor 冯传密史文涛吴昊吕金昆王聪刘新伟杨克俭
Owner CHINA TIANCHEN ENG
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