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A method for preparing cis-pinane by hydrogenation of α-pinene

A technology for the preparation of hydrogen and pinene, which is applied in the field of selective hydrogenation of α-pinene by magnetic catalysts to prepare cis-pinane, which can solve the problems of poor catalyst stability, difficult separation and recovery, poor reusability, etc. Less, simple product post-processing, good recycling effect

Inactive Publication Date: 2017-12-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these catalysts have improved the productive rate of cis-pinane to a certain extent, they still have poor catalyst stability, difficulty in separation and recovery, and poor reusability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Combine 2.5g α-pinene and 0.06g Fe 3 O 4 @C / Ru (wherein the mass fraction of Ru is 6.0%) was added to a stainless steel autoclave, replaced the air in the autoclave with hydrogen 5 times and then filled with 4.0MPa hydrogen, heated and stirred at 120°C for 4h, and allowed to stand and cool to room temperature. Under the action of an external magnetic field, the product phase and the catalyst phase are directly separated in the kettle, and the separated catalyst can be directly recycled without post-treatment. The α-pinene conversion rate was 99.1%, and the cis-pinene selectivity was 96.7%.

Embodiment 2

[0017] Example 2: Combine 2.5g α-pinene and 0.05g Fe 3 O 4 @C / Ru (wherein the mass fraction of Ru is 6.0%) was added to a stainless steel autoclave, replaced the air in the autoclave with hydrogen 5 times and then filled with 4.0MPa hydrogen, heated and stirred at 120°C for 4h, and allowed to stand and cool to room temperature. Under the action of an external magnetic field, the product phase and the catalyst phase are directly separated in the kettle, and the separated catalyst can be directly used for the next reaction without post-treatment. The α-pinene conversion rate was 98.6%, and the cis-pinene selectivity was 96.2%.

Embodiment 3

[0018] Example 3: Combine 2.5g α-pinene and 0.06g Fe 3 O 4 @C / Ru (wherein the mass fraction of Ru is 6.0%) was added to the stainless steel autoclave, replaced the air in the autoclave with hydrogen 5 times and then filled with 5.0MPa hydrogen, heated and stirred at 120°C for 4h, and allowed to stand and cool to room temperature. Under the action of an external magnetic field, the product phase and the catalyst phase are directly separated in the kettle, and the separated catalyst can be directly used for the next reaction. The conversion rate of α-pinene was 99.4%, and the selectivity of cis-pinene was 96.1%.

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PUM

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Abstract

A method for preparing cis-pinane by hydrogenating α-pinene, the reaction is carried out under the conditions that the mass ratio of α-pinene to a magnetic catalyst is 50:1.2-2, the reaction temperature is 100-130°C, and the hydrogen pressure is 3.0-5.0 MPa 3.0 to 5.0 hours to prepare cis-pinane. After the reaction, use an external magnetic field to recover the catalyst phase and the product phase respectively. The catalyst phase does not need to be post-treated and can be directly recycled, which has good reusability. Under the process conditions, the conversion rate of α-pinene is greater than 98%, and the selectivity of cis-pinane is greater than 96%.

Description

Technical field [0001] The invention relates to a method for preparing cis-pinene by hydrogenation of alpha-pinene, that is, to a method for preparing cis-pinene through selective hydrogenation of alpha-pinene through a magnetic catalyst. technical background [0002] Cis-pinene is mainly produced by the catalytic hydrogenation of α-pinene, and the main products in the hydrogenation reaction of α-pinene are cis-pinene and trans-pinene. Cis-pinene is a synthetic adhesive, coating, and flavor It is an important intermediate of chemical products such as perfumes and cosmetics. Therefore, it is particularly important to improve the selectivity of cis-pinane. At present, Pd / C (Wang Biyu, etc., palladium-carbon catalyst is used in the atmospheric hydrogenation of α-pinene to produce pinane in the industry [J].Fujian Chemical Industry, 1997,4:14-15) to catalyze α-pine The olefin hydrogenation reaction, but the process has the disadvantages of low yield, long reaction time, high price, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/40C07C5/03
CPCY02P20/584
Inventor 于世涛刘悦解从霞李露刘仕伟刘福胜
Owner QINGDAO UNIV OF SCI & TECH