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Method for isomerizing alpha-pinene

A technology of isomerization and pinene, applied in the direction of isomerization hydrocarbon production, organic chemistry, etc., can solve the problems of complicated product post-processing, environmental pollution, etc., and achieve the effects of short time consumption, high reactivity and mild reaction conditions

Inactive Publication Date: 2013-07-17
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of liquid acid as a catalyst has the problems of environmental pollution and complicated post-processing of products.

Method used

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  • Method for isomerizing alpha-pinene
  • Method for isomerizing alpha-pinene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 10 ml granular (diameter ≤ 2 mm) high-purity γ-Al 2 o 3 Put it into the glass material fixed bed reaction tube I, in the high-purity N 2 (purity ≥ 99.99%, flow rate 20 -100ml / min) in the atmosphere at 500 o C pretreatment for 2 hours, after that, feed CCl simultaneously at a flow rate of 0.8-2.00 ml / h 4 (pre-dried to remove water), in-situ generation of AlCl 3 ; 5ml of 40-60 mesh mesoporous SiO2 was loaded into the fixed bed reaction tube II 2 , at high purity N 2 300 in airflow (40 ml / min) o After C pretreatment for 2 h, the reaction tube I was connected to the reaction tube II, and the 2 In situ generation of AlCl under gas flow 3 with SiO 2 Reaction of surface hydroxyl groups with AlCl 3 fixed load. After 2-3h, stop feeding CCl 4 , at 300 o Continue to use N under C 2 Purge for 1 h, under N 2 Cool to room temperature under protection for later use. The catalyst is denoted as AlCl 3 / SiO 2 .

[0016] Add magnetite, 2ml α-pinene, 0.2ml n-decane...

Embodiment 2

[0020] According to the AlCl prepared in Example 1 3 / SiO 2 Catalyst, at 40 oC At the reaction temperature of α-pinene, the isomerization reaction was carried out for 60 min and 120 min respectively. Other conditions are with embodiment 1. The results are shown in Table 2: AlCl 3 / SiO 2 Catalyzed α-pinene isomerization results (reaction times vary).

[0021]

[0022] Table 2

Embodiment 3

[0024] According to the preparation method of the catalyst in Example 1, the support is changed to double-hole γ-Al 2 o 3 . Carrier in high purity N 2 400 in airflow o After C pretreatment for 2 h, in N 2 Cool down to 300 in airflow o C, with in situ generated AlCl 3 Reaction 3 h, N 2 Warm up to 400 in airflow o C was purged for 1 h, cooled to room temperature for later use, and the obtained catalyst was denoted as AlCl 3 / γ-Al 2 o 3 .

[0025] Use this catalyst to catalyze the isomerization of α-pinene: add magneton, 2 ml α-pinene, 0.2 ml n-decane (internal standard) and 0.1 g AlCl in a dry reaction tube 3 / γ-Al 2 o 3 catalyst. The results at different reaction temperatures and reaction times are shown in Table 3: AlCl 3 / γ-Al 2 o 3 Catalyzed α-pinene isomerization reaction results.

[0026]

[0027] table 3

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Abstract

The invention relates to a method for isomerizing alpha-pinene. The method comprises the following steps of: immobilizing active components such as halide, chloride and bromide on the surface of alumina, silicon oxide, SiO2-Al2O3 or silicon-aluminium molecular sieve by virtue of surface grafting reaction, and catalyzing isomerisation reaction of the alpha-pinene with solid acid, wherein halide can be aluminium, stibium, zinc, iron, titanium, tin and zirconium, and the reaction is performed for 10-240 minutes at the temperature of 5-80 DEG C in the manner of constant-pressure liquid-solid multiphase stirring reaction or fixed bed reaction. The new method for isomerizing the alpha-pinene, provided by the invention, has the advantages that the reaction condition is mild, the selectivity of main products (camphene, limonene and terpinolene) is high, and the catalyst produces no pollution to the equipment and environment, thus the catalysis process is environmentally friendly.

Description

technical field [0001] The present invention relates to a new method for isomerization of α-pinene. Specifically, it is a method for isomerizing α-pinene by adopting a liquid-solid heterogeneous stirring reaction mode or a fixed bed reaction mode on a solid-supported halide catalyst. Background technique [0002] α-pinene is the main component of turpentine, which is the most produced and cheapest essential oil in the world. α-pinene is particularly sensitive to acids, and can undergo reactions such as isomerization, oxidation, hydrogenation, addition, esterification, and polymerization, especially the isomerization products under the action of acids, which are ideal for the preparation of spices, medicines, and fine chemicals. important intermediates, such as the synthesis of camphor from camphene. There are many catalysts for isomerization of α-pinene, but the reaction products are complicated. Therefore, under relatively mild reaction conditions, improving the conversi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C5/29C07C5/31C07C13/23C07C13/21C07C13/47
Inventor 田福平吴义辉蔡天锡贺民
Owner DALIAN UNIV OF TECH
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