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Method for preparing cis-pinane by alpha-pinene hydrogenation

A hydrogen preparation and cis technology, applied in the field of α-pinene hydrogenation to prepare cis pinane, can solve the problems of difficult separation and high cost of precious metal catalysts

Active Publication Date: 2020-11-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of high cost and difficult separation of noble metal catalysts in the prior art, the present invention provides a method for preparing cis-pinane by hydrogenating α-pinene

Method used

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  • Method for preparing cis-pinane by alpha-pinene hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Catalyst Ni / CxNy@mSiO 2 preparation of

[0021] S 1 , Preparation of hollow Juans amphiphilic nano-mesoporous materials (CxNy@mSiO 2 ): Weigh 0.16g CTAB (cetyltrimethylammonium bromide) and 5mL EDA (ethylenediamine) respectively and disperse them in a mixed solution of 50mL of ethanol and water (ethanol: water = 3:7) , then add 0.12g resorcinol, ultrasonically disperse for 30min, add dropwise 0.24mL formaldehyde, stir for 2h, then add 50mg CTAB, dropwise add 0.8mL TEOS (tetraethyl orthosilicate), continue to stir for 12h, then let stand After 48h, centrifugal separation, and finally high-temperature carbonization under argon atmosphere to obtain the amphiphilic nano-mesoporous material CxNy@mSiO 2 ;

[0022] S 2 , Preparation of hollow Juans amphiphilic nanocatalysts (Ni / CxNy@mSiO 2 ): Weigh 50mg CxNy@mSiO 2 Add it to a 100mL one-necked flask, ultrasonically disperse in ethanol solution at room temperature, and then add 30mg NiCl 2 , continue to disper...

Embodiment 2

[0024] Example 2 α-pinene hydrogenation to prepare cis-pinane

[0025] Weigh 1g of α-pinene and add it to a stainless steel mechanically stirred kettle, then add 4mL of water, weigh 20mg of amphiphilic catalyst and mix evenly, replace the gas in the kettle with 1MPa hydrogen gas for 4 times, then flush into 3MPa hydrogen gas, at 60°C Mechanical stirring reaction 2h, after reaction finishes, leave standstill catalyst and product separation, after extracting with n-heptane, collect upper layer product phase and adopt chromatography to carry out quantitative analysis, α-pinene conversion rate is 95.6%, cis-pinane The selectivity was 96.5%.

Embodiment 3

[0026] Example 3 Preparation of cis-pinane by hydrogenation of α-pinene

[0027] Weigh 1g of α-pinene and add it to a stainless steel mechanically stirred kettle, then add 4mL of water, weigh 20mg of amphiphilic catalyst and mix evenly, replace the gas in the kettle with 1MPa hydrogen gas for 4 times, then flush into 3MPa hydrogen gas, at 70°C Mechanical stirring reaction 2h, after the reaction finishes, leave standstill to separate the catalyst and the product, after extracting with toluene, collect the upper product phase and carry out quantitative analysis by chromatography, the conversion rate of α-pinene is 97.1%, and the selectivity of cis-pinane 98.5%.

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PUM

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Abstract

The invention belongs to the technical field of cis-pinane preparation, and discloses a method for preparing cis-pinane through alpha-pinene hydrogenation. The method comprises the following steps: inan aqueous solution, filling H2 into alpha-pinene under the catalytic action of an amphiphilic nano mesoporous material loaded nickel active particle catalyst Ni / CxNy@mSiO2, and carrying out catalytic hydrogenation reaction to obtain cis-pinane. The catalyst Ni / CxNy@mSiO2 provided by the invention shows excellent catalytic activity and product selectivity on alpha-pinene hydrogenation catalytic reaction.

Description

technical field [0001] The invention relates to a method for preparing cis-pinane by hydrogenating alpha-pinene. Background technique [0002] my country is rich in turpentine resources, its main component α-pinene can be hydrogenated to obtain cis-pinane, and cis-pinane is a chemical compound with important applications in the fields of biopharmaceuticals, material synthesis, industrial flavors, and pesticide synthesis. Chemical intermediates. Therefore, the process of preparing cis-pinane by hydrogenation of α-pinene occupies an important position in the fields of chemical engineering, biomedicine, materials, etc.; Most of the catalysts used are Pd / C, Ru / C or Raney nickel catalysts, but the reaction conditions of these catalysts are too harsh, and the cis-trans ratio of cis-pinane and trans-pinane is low. [0003] In recent years, Hou Shengli et al. have adopted RuCl 3 ·3H 2 O is the metal precursor, polymers P123, F127 and TPGS-1000 are used as stabilizers, and H 2 Ru...

Claims

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Application Information

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IPC IPC(8): C07C5/03C07C13/40B01J27/24B01J35/00B01J35/02
CPCC07C5/03B01J27/24C07C2602/42B01J35/393B01J35/50C07C13/40
Inventor 解从霞于凤丽吴方柱李雯袁冰于世涛
Owner QINGDAO UNIV OF SCI & TECH
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