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Preparation method of high-selectivity pinane

A high-selectivity, pinane technology, used in the chemical industry, can solve the problems of harsh operating conditions, poor enantioselectivity, and large safety hazards, and achieve the effects of simple preparation process, mild reaction conditions, and low equipment requirements.

Inactive Publication Date: 2016-02-17
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the catalysts used for the catalytic hydrogenation of turpentine to prepare cis-pinane are mostly nickel catalysts. Although the production cost is low, the reaction temperature and reaction pressure are high, the requirements for reaction equipment are high, the operating conditions are harsh, and there are great safety hazards. And the content of cis-pinane in the product is low, and the enantioselectivity is relatively poor

Method used

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  • Preparation method of high-selectivity pinane
  • Preparation method of high-selectivity pinane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation method of highly selective pinane described in the present embodiment specifically comprises the following steps:

[0026] (1) Take turpentine and put it in the reaction kettle, then add [Rh(COD)Cl] according to the mass of the catalyst as 1% of the mass of the raw material 2 Catalyst, sealed reactor.

[0027] (2) Use N at 0.3MPa 2 Replace 3 times, and then use H 2 Replace 3 times at 0.3MPa, adjust the hydrogen pressure in the reactor to 3MPa, maintain the pressure and check for leaks, control the rotation speed at 600r / min, and react at 40°C for 3h.

[0028] (3) After the reaction is over, stop heating and stirring, and open the reactor after pressure relief to separate the catalyst from the reaction product.

[0029] The reaction product was detected and analyzed by gas chromatography, the conversion rate of pinene was 98.13%, and the enantioselectivity of cis-pinane was 98.09%.

[0030] [Rh(COD)Cl] described in this embodiment 2 Catalyst is prepa...

Embodiment 2

[0036] (1) Take turpentine and put it in the reaction kettle, then add [Rh(COD)Cl] according to the mass of the catalyst as 5% of the mass of the raw material 2 Catalyst, sealed reactor.

[0037] (2) Use N at 0.5MPa 2 Replaced twice, then H 2 Replace twice at 0.5MPa, adjust the hydrogen pressure in the reactor to 3MPa, maintain the pressure and check for leaks, control the rotation speed at 600r / min, and react at 70°C for 3h.

[0038] (3) After the reaction is over, stop heating and stirring, and open the reactor after pressure relief to separate the catalyst from the reaction product.

[0039] The reaction product was detected and analyzed by gas chromatography, the conversion rate of pinene was 92.01%, and the enantioselectivity of cis-pinane was 96.00%.

[0040] [Rh(COD)Cl] described in this embodiment 2 Catalyst is prepared by following method, specifically comprises the following steps:

[0041] (1) Add RhCl at 0.033g / mL 3 ·3H 2 O is heated and dissolved in absolut...

Embodiment 3

[0046] (1) Take turpentine and put it in the reaction kettle, then add [Rh(COD)Cl] according to the mass of the catalyst as 3% of the mass of the raw material 2 Catalyst, sealed reactor.

[0047] (2) Use N at 0.1MPa 2 Replace 3 times, and then use H 2Replace 3 times at 0.1MPa, adjust the hydrogen pressure in the reactor to 2MPa, maintain the pressure and check for leaks, control the speed at 600r / min, and react at 40°C for 3h.

[0048] (3) After the reaction is over, stop heating and stirring, and open the reactor after pressure relief to separate the catalyst from the reaction product.

[0049] The reaction product was detected and analyzed by gas chromatography, the conversion rate of pinene was 96.98%, and the enantioselectivity of cis-pinane was 98.05%.

[0050] [Rh(COD)Cl] described in this embodiment 2 Catalyst is prepared by following method, specifically comprises the following steps:

[0051] (1) Add RhCl at 0.033g / mL 3 ·3H 2 O is heated and dissolved in absolu...

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Abstract

The invention relates to a preparation method of high-selectivity pinane, and belongs to the field of chemical industry. The method comprises the technological steps: heating RhCl3.3H2O to be dissolved in an ethanol solution, adding 1,5-cyclooctadiene (COD) according to the molar ratio of 1,5-cyclooctadiene to rhodium of 3 to 7, backflowing for a certain period of time, then carrying out suction filtration on the mixture, then washing with anhydrous ethanol, and drying to obtain a rhodium complex [Rh(COD)Cl]2; and adding the prepared rhodium complex [Rh(COD)Cl]2 in a high pressure reaction kettle with the amount 1-7% of the mass of turpentine oil, covering a lid, sealing, respectively replacing with nitrogen gas and hydrogen gas, carrying out pressure maintaining and leakage detection, adjusting the reaction kettle pressure to be 1-5 MPa, and carrying out a reaction for 1-5 h at the reaction temperature of 30-70 DEG C. The method has the advantages of mild reaction condition, simple technological process, low energy consumption, high alpha-pinene conversion rate, and high selectivity of the product cis-pinane.

Description

technical field [0001] The invention relates to a method for preparing pinane with high selectivity, belonging to the field of chemical industry. Background technique [0002] my country is rich in turpentine resources and is the main exporter of turpentine in the world. The main components of turpentine are α-pinene and β-pinene. Under the action of certain temperature, pressure, solvent and suitable catalyst, α-pinene can be catalytically hydrogenated to produce pinane. Pinane is an important Raw materials for spices and pharmaceutical industry, important intermediates for the preparation of spices such as citronellol, linalool, rose musk and dihydromyrcenol, vitamin E, and borneol. There are two isomers of pinane, cis and trans. The pinane used in industry requires cis-pinane as the main form. Because of the large steric hindrance of trans-pinane, its activity is far inferior to that of cis-pinane. High alkanes. [0003] At present, the catalysts used for the catalytic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/40C07C5/03B01J31/22
Inventor 蒋丽红王亚明王红琴杨晨张家华鞠江月李怡然晋艳琼
Owner KUNMING UNIV OF SCI & TECH
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