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Method for preparing pinane by catalytic hydrogenation of turpentine

A technology of catalytic hydrogenation and turpentine, which is applied in the chemical industry, can solve the problems of harsh reaction conditions, low selectivity, and high price, and achieve the effects of good thermal stability, simple process, and mild process conditions

Inactive Publication Date: 2014-08-27
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used turpentine hydrogenation catalysts are noble metal catalysts and Raney Ni catalysts. The noble metal catalysts catalyzed turpentine hydrogenation has excellent catalytic activity, but the price is expensive and the selectivity is low.
The price of Raney Ni catalyst is relatively low, but the reaction conditions are relatively harsh, and the catalytic activity is lower than that of noble metal catalysts

Method used

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  • Method for preparing pinane by catalytic hydrogenation of turpentine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Catalytic hydrogenation of turpentine described in the present embodiment prepares pinane method, specifically comprises the following steps:

[0032] (1) Take turpentine and put it in the reaction kettle, then add the supported Ni-P / SiO according to the mass of the catalyst as 2% of the mass of the raw material 2 Amorphous catalyst, sealed reactor;

[0033] (2) Use N at 0.3MPa 2 Replace the air in the reactor 3 times, and then use H 2 Replace 3 times under 0.1MPa, and check the airtightness;

[0034] (3) Open H 2 Inlet valve, adjust the pressure in the reactor to 1MPa, start to heat up, control the temperature at 150°C, and react for 180min at a speed of 1000r / min;

[0035] (4) After the reaction is over, stop heating and stirring, open the kettle after pressure relief, and filter and separate the catalyst and the reaction product.

[0036] The reaction product was detected and analyzed by gas chromatography, the conversion rate of pinene was 83.41%, and the selec...

Embodiment 2

[0042] Catalytic hydrogenation of turpentine described in the present embodiment prepares pinane method, specifically comprises the following steps:

[0043] (1) Take turpentine and put it in the reaction kettle, then add the supported Ni-P / SiO according to the mass of the catalyst as 3% of the mass of the raw material 2 Amorphous catalyst, sealed reactor;

[0044] (2) Use N at 0.3MPa 2 Replace the air in the reactor 3 times, and then use H 2 Replace 3 times under 0.2MPa, and check the airtightness;

[0045] (3) Open H 2 Intake valve, adjust the pressure in the reactor to 5MPa, start to heat up, and react for 60min under the conditions of temperature control at 100°C and rotation speed of 800r / min;

[0046](4) After the reaction is over, stop heating and stirring, open the kettle after pressure relief, and filter and separate the catalyst and the reaction product.

[0047] The reaction product was detected and analyzed by gas chromatography, the conversion rate of pinene ...

Embodiment 3

[0053] Catalytic hydrogenation of turpentine described in the present embodiment prepares pinane method, specifically comprises the following steps:

[0054] (1) Take turpentine and place it in the reaction kettle, and then add the prepared supported Ni-P / SiO by 1% of the mass of the raw material as the mass of the catalyst 2 Amorphous catalyst, sealed reactor;

[0055] (2) Use N at 0.3MPa 2 Replace the air in the reactor 3 times, and then use H 2 Replace 3 times under 0.3MPa, and check the airtightness;

[0056] (3) Open H 2 Inlet valve, adjust the pressure inside the reactor to 4MPa, start to heat up, and react for 30min under the condition of temperature control at 150°C and rotation speed of 500r / min;

[0057] (4) After the reaction is over, stop heating and stirring, open the kettle after pressure relief, and filter and separate the catalyst and the reaction product.

[0058] The reaction product was detected and analyzed by gas chromatography, the conversion rate of...

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Abstract

The invention discloses a method for preparing pinane by catalytic hydrogenation of turpentine, and belongs to the chemical engineering field. The method comprises the steps: adopting ultrasound assistance to prepare a load type Ni-P / SiO2 amorphous catalyst used for preparing pinane through selective catalytic hydrogenation of turpentine, adding a carrier SiO2 into a soluble nickel salt aqueous solution with a certain concentration, then adding CH3COONa, dipping for 1-4 h under an ultrasonic assisted condition, and adjusting the pH value; then placing the above mixture in a water bath, adding NaH2PO2.H2O after constant temperature, stirring until no bubbles are produced, carrying out suction filtration on the mixture, then washing the filter cake with ammonia water, next washing with distilled water, washing with anhydrous ethyl alcohol, and then carrying out alcohol sealing; and adding the prepared load type Ni-P / SiO2 amorphous catalyst with the amount of 1-10% of the turpentine mass into a high-pressure reaction vessel, adjusting the pressure in the reaction vessel to 1-5 MPa, and carrying out a reaction for 30-180 min under conditions of the temperature of 100-150 DEG C and the rotation speed of 500-1000 r / min. The method has the advantages of simple process flow, mild reaction conditions, energy consumption saving, high yield of pinane, and good selection.

Description

technical field [0001] The invention relates to a method for preparing pinane by catalytic hydrogenation of turpentine, belonging to the field of chemical industry. Background technique [0002] my country's turpentine output ranks second in the world, and it is the main exporter of turpentine in the world. As a renewable resource, turpentine has high utilization value. Its main component, pinane, is the hydrogenation product of α-pinene, which is used for the synthesis of linalool, Dihydromyrcenol, citronellol and other spices and raw materials for industrial vitamin E. The pinane used in industrial production is required to be mainly in the cis form, because the reactivity of cis pinane is much higher than that of trans pinane. In the process of catalytic hydrogenation of turpentine, to increase the content and selectivity of cis-pinane is not only related to the type of catalyst selected, but also closely related to the selected process conditions, such as reaction temper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/40C07C5/03B01J27/185
Inventor 蒋丽红王亚明刘坤陕绍云贾庆明李丹丹杨晨蔡琴
Owner KUNMING UNIV OF SCI & TECH