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Novel process for preparing alpha-terpineol by catalyzing turpentine oil with MoO3/ZnO2

A technology for the production of turpentine and terpineol, applied in the direction of hydroxyl addition preparation, etc., can solve the problems of long production cycle, environmental pollution, high energy consumption, etc., and achieve the effects of increasing conversion rate, reducing energy consumption, and shortening reaction time

Inactive Publication Date: 2008-12-03
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The invention can solve the above-mentioned problems of long production cycle, high energy consumption, environmental pollution and equipment corrosion

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In WF-4000C microwave reactor, press turpentine: dehydrated alcohol: water=1: 1: 1-3 (mol), catalyst consumption 2%-10% (wt), microwave power 300-500W, reaction temperature 50- 90°C, reaction time 2h. Sampling for GC analysis.

[0034] The components of the product are as follows: (GC%)

[0035] 1. α-pinene 2.44%; 2. Camphene 3.77%; 3. β-pinene 0.51%, 4. δ-3-carene 2.64%; 5. Limonene 16.11%; 6.1.8-Cineole 1.62% ; 7. γ-Terpinene 16.94%; 8. Terpinene 0.69%; 9. Feminyl Alcohol 0.85%; 10. α-Terpineol 51.00%; 1.65%.

[0036] The calculated conversion rate of turpentine (α-pinene) is 96.94%, and the yield of α-terpineol is 52.98%.

Embodiment 2

[0038] In WF-4000C microwave reactor, press turpentine: dehydrated alcohol: water=1: 1: 1-3 (mol), catalyst consumption 2%-10% (wt), microwave power 300-500W, reaction temperature 50- 90°C, reaction time 2h. Sampling for GC analysis.

[0039] The components of the product are as follows: (GC%)

[0040] 1. α-pinene 3.95%; 2. Camphene 3.50%; 3. β-pinene 0.58%; 4. δ-3-carene 2.61%; 5. Limonene 16.59%; 6.1.8-Cineole 1.40% ; 7. γ-Terpinene 16.32%; 8. Terpinene 0.76%; 9. Feminyl Alcohol 0.87%; 10. α-Terpineol 49.50%; 2.32%.

[0041] The calculated conversion rate of turpentine (α-pinene) is 95.29%, and the yield of α-terpineol is 51.42%.

Embodiment 3

[0043] In WF-4000C microwave reactor, press turpentine: dehydrated alcohol: water=1: 1: 1-3 (mol), catalyst consumption 2%-10% (wt), microwave power 300-500W, reaction temperature 50- 90°C, reaction time 1h. Sampling for GC analysis.

[0044] The components of the product are as follows: (GC%)

[0045] 1. α-pinene 3.34%; 2. Camphene 3.89%; 3. β-pinene 0.36%, 4. δ-3-carene 2.46%; 5. Limonene 18.45%; 6.1.8-Cineole 1.32% ; 7. γ-Terpinene 17.20%; 8. Terpinene 0.22%; 9. Feminyl Alcohol 0.11%; 10. α-Terpineol 52.08%; 0.35%.

[0046] The calculated conversion rate of turpentine (α-pinene) is 96.16%, and the yield of α-terpineol is 54.10%.

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PUM

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Abstract

The invention discloses a method for preparing alpha-terpineol by MnO3 / ZrO2 solid super acid prepared by the impregnation method to catalyze turpentine through hydration reaction in a WF-4000C microwave quick-reaction system. The technological conditions for preparing MnO3 / ZrO2 are as follows: the concentration of an ammonium molybdate solution is between 0.2 and 2 mol / L; the impregnation temperature is between 50 and 80 DEG C, the impregnation time is between 2 and 5 hours, the calcination temperature is between 400 and 650 DEG C, and the calcination time is between 2 and 5 hours. The technological conditions for preparing the alpha-terpineol through the hydration reaction of the turpentine in a microwave field are as follows: the ratio of the turpentine to the absolute ethyl alcohol to water is 1 to 1 to 1-3 (mols); the amount of catalyst is between 2 and 10 percent (weight percent); the microwave power is between 300 and 500 watts; and the reaction temperature is between 50 and 90 DEG C, and the reaction time is between 1 and 3 hours. The conversion rate of the turpentine is between 90 and 97 percent, and the yield of the alpha-terpineol is between 51 and 53 percent; the reaction time is greatly shortened; and the advantages of promotion of the organic chemical reaction speed by microwaves, reduction of the production cost and energy conservation are fully revealed. Because the method has the advantages of low-price and easily obtained raw materials, low production cost, simple synthetic technology, superior performance, suitability for industrialized production, etc., the method has strong market competitive strength and promotion and application value.

Description

technical field [0001] The present invention relates to the fine chemical catalyst technology of natural product deep processing, especially relates to the microwave-promoted MoO 3 / ZnO 2 A method for catalyzing turpentine to produce α-terpineol. Background technique [0002] Microwave is an electromagnetic wave with a frequency of 300MHz-300GHz, its wavelength is between 100cm-1mm, and its energy is about several Jmol -1 . Microwaves are a form of energy that can be converted into energy in a medium. [0003] The convening of the World Conference on Microwave Chemistry in 1992 marked the birth of a new interdisciplinary subject that applied microwave technology to chemical processes. For more than ten years, researchers have achieved rich research results in the study of promoting organic chemical reactions with microwave radiation. The principle of using microwave radiation technology to promote the chemical reaction process has two aspects: one is the heating effect ...

Claims

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Application Information

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IPC IPC(8): C07C33/14C07C29/04B01J23/28B01J23/06
Inventor 王亚明陈秋玲蒋丽红刘天成曹振恒张思华
Owner KUNMING UNIV OF SCI & TECH
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