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A kind of method for preparing pinane by catalytic hydrogenation of β-pinene

A technology for catalytic hydrogenation and pinene, which is applied in the chemical industry to achieve the effects of easy recovery, superior performance and reduced pollution

Active Publication Date: 2018-08-10
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, β-pinene hydrogenation reaction is rarely reported [Setrak Tanielyan, et al. Top. Catal., 2014, 57(17-20): 1564-1569], therefore, the development of new catalysts for β-pinene hydrogenation reaction It is of great significance to speed up the deep processing of turpentine

Method used

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  • A kind of method for preparing pinane by catalytic hydrogenation of β-pinene
  • A kind of method for preparing pinane by catalytic hydrogenation of β-pinene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The method for preparing pinane by catalytic hydrogenation of β-pinene described in this embodiment specifically comprises the following steps:

[0031] (1) Take a certain amount of β-pinene and put it in the reaction kettle, and then add the supported [Rh(COD)Cl] according to the mass of the catalyst at 5% of the mass of β-pinene 2 / C catalyst, sealed reactor;

[0032] (2) Use N at 0.3MPa 2 Replace the gas in the kettle 3 times, and then use H 2 Replace the gas in the kettle for 3 times under 0.3MPa, and check the air tightness;

[0033] (3) Open H 2 The inlet valve was used to adjust the reaction pressure to 1MPa, and the reaction was carried out at 80°C for 5h.

[0034] (4) After the reaction is over, stop heating and stirring, open the reaction kettle after pressure relief, and filter and separate the catalyst and reactants.

[0035] The reaction product was detected and analyzed by gas chromatography, the conversion rate of β-pinene was 99.76%, and the cis-tra...

Embodiment 2

[0041] The method for preparing pinane by catalytic hydrogenation of β-pinene described in this embodiment specifically comprises the following steps:

[0042] (1) Take a certain amount of β-pinene and put it in the reaction kettle, and then add the supported [Rh(COD)Cl] according to the mass of the catalyst at 3% of the mass of β-pinene 2 / C catalyst, sealed reactor;

[0043] (2) Use N at 0.1MPa 2 Replace the gas in the kettle 3 times, and then use H 2 Replace the gas in the kettle for 3 times under 0.1MPa, and check the air tightness;

[0044] (3) Open H 2 Inlet valve, adjust the reaction pressure to 3MPa, and react at 50°C for 3h.

[0045] (4) After the reaction is over, stop heating and stirring, open the reaction kettle after pressure relief, and filter and separate the catalyst and reactants.

[0046] The reaction product was detected and analyzed by gas chromatography, the conversion rate of β-pinene was 99.81%, and the cis-trans ratio of pinane was 7.64.

[0047]...

Embodiment 3

[0052] The method for preparing pinane by catalytic hydrogenation of β-pinene described in this embodiment specifically comprises the following steps:

[0053] (1) Take a certain amount of β-pinene and put it in the reactor, and then add the supported [Rh(COD)Cl] according to the mass of the catalyst at 4% of the mass of β-pinene 2 / C catalyst, sealed reactor;

[0054] (2) Use N at 0.3MPa 2 Replace the gas in the kettle 3 times, and then use H 2 Replace the gas in the kettle for 3 times under 0.3MPa, and check the air tightness;

[0055] (3) Open H 2 Inlet valve, adjust the reaction pressure to 4MPa, and react at 40°C for 4h.

[0056] (4) After the reaction is over, stop heating and stirring, open the reaction kettle after pressure relief, and filter and separate the catalyst and reactants.

[0057] The reaction product was detected and analyzed by gas chromatography, the conversion rate of β-pinene was 100%, and the cis-trans ratio of pinane was 8.04.

[0058] Loading t...

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Abstract

The invention relates to a method for preparing pinane by beta-pinene hydrogenation and belongs to the chemical field. The method comprises the following technological steps: adding a carrier active carbon into a certain concentration of [Rh(COD)Cl]2 methanol solution in an inert atmosphere, stirring at room temperature for 2-5 h, standing, moving away a solvent by the use of a syringe, and drying in an inert atmosphere to obtain a supported [Rh(COD)Cl]2 / C catalyst; carrying out an oxidation treatment on the carrier active carbon by the use of 15-45% HNO3 before supporting; adding the prepared catalyst which accounts for 1-5% of mass of beta-pinene into a high pressure reactor, adjust pressure in the high pressure reactor to 1-5 MPa, and reacting at the temperature of 30-80 DEG C at the rotating speed of 800 r / min for 1-5h. The reaction condition of the method is mild; the technological process is simple; energy consumption is low; conversion rate of beta-pinene is high; the catalyst is easy to separate from a product; and the catalyst can be recycled.

Description

technical field [0001] The invention relates to a method for preparing pinane by catalytic hydrogenation of β-pinene, which belongs to the field of chemical industry. Background technique [0002] Turpentine oil is composed of a variety of monoterpene compounds with similar structures. It is a valuable natural product and natural intermediate, and has a wide range of application values. my country has a large output of turpentine and is the main exporter of turpentine in the world. With the continuous deepening of turpentine deep processing research and the continuous development of separation and purification technology, the research, development and application of turpentine components and their derivatives have attracted much attention. β-pinene, one of the important components of turpentine, can undergo various reactions such as hydrogenation, oxidation, and polymerization on its multi-ring, bridging ring and extracyclic double bonds, and then obtain a series of β-pinen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C5/03C07C13/40B01J31/22
CPCY02P20/584
Inventor 蒋丽红王亚明王红琴陕绍云贾庆明郑文龙刘磊徐涛
Owner KUNMING UNIV OF SCI & TECH
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