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Method for preparing cis-pinane by adopting selective hydrogenation of alpha-pinene

A technology for hydrogen preparation and selectivity, which is applied in the fields of hydrogenation to hydrocarbon production, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. problems such as poor stability, to achieve the effects of high catalytic activity and selectivity, less by-products, and simple treatment

Inactive Publication Date: 2015-12-30
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These catalysts generally have low selectivity to cis-pinane, poor catalyst stability, and difficulties in repeated use.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: 3.0g α-pinene and 0.1gFe 3 o 4 -SiO 2 -APTES-Ru (the mass fraction of Ru is 8%) was added to the stainless steel autoclave, the air in the autoclave was replaced by hydrogen, then filled with 5.0MPa hydrogen, heated and stirred at 150°C for 5h, and allowed to stand and cooled 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. The conversion rate of α-pinene was 98.2%, and the selectivity of cis-pinane was 96.4%.

Embodiment 2

[0017] Embodiment 2: with 3.0g α-pinene and 0.1gFe 3 o 4 -SiO 2 -APTES-Ru (the mass fraction of Ru is 8%) was added to the stainless steel autoclave, the air in the autoclave was replaced by hydrogen, then filled with 5.0MPa hydrogen, heated and stirred at 160°C for 5h, and allowed to stand and cooled 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-pinane was 96.3%.

Embodiment 3

[0018] Embodiment 3: with 3.0g α-pinene and 0.1gFe 3 o 4 -SiO 2 -APTES-Ru (the mass fraction of Ru is 8%) was added to the stainless steel autoclave, the air in the autoclave was replaced by hydrogen, then filled with 6.0MPa hydrogen, heated and stirred at 160°C for 5h, and allowed to stand and cooled 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 99.5%, and the selectivity of cis-pinane was 96.2%.

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PUM

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Abstract

The invention provides a method for preparing cis-pinane by adopting selective hydrogenation of alpha-pinene. According to the method, alpha-pinene and a magnetic catalyst react in a mass ratio being 50:(1-2.7) for 4.0-6.0 h at the reaction temperature of 140-180 DEG C and under hydrogen pressure of 4.0-6.0 MPa; cis-pinane is prepared, and after reaction, a catalyst phase and a product phase are recovered respectively through an external magnetic field. The catalyst phase does not require aftertreatment and is recycled directly. Under the process conditions, the conversion rate of alpha-pinene is higher than 99%, and the selectivity of cis-pinane is higher than 96%.

Description

technical field [0001] The invention relates to a method for preparing cis-pinane by selective hydrogenation of alpha-pinene, in particular to a method for preparing cis-pinane by selective hydrogenation of alpha-pinene catalyzed by a magnetic catalyst. technical background [0002] Pinane is mainly produced by catalytic hydrogenation of α-pinene, and it is an important intermediate in the synthesis of aromatic alcohols and other fragrances. Among pinanes, cis-pinane has higher reactivity, so the purity and selectivity of cis-pinane in the process of preparing pinane by catalytic hydrogenation of α-pinene is very important. At present, the catalysts that are used to catalyze the hydrogenation of α-pinene to synthesize cis-pinane mainly include skeleton nickel (CN1191857, CN1262263), Pd / C (Wang Biyu, etc., palladium carbon catalyst is used for the preparation of α-pinene atmospheric pressure hydrogenation Research on pinane [J]. Fujian Chemical Industry, 1997, 4:14-15), Ru / A...

Claims

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Application Information

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IPC IPC(8): C07C13/40C07C5/03B01J31/28B01J31/32
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
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