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Method for preparing 2,3-epoxypinane by epoxidizing alpha-pinene

A technology of epoxy pinane and epoxidation, applied in the direction of organic chemistry, can solve the problems of low hydrogen peroxide oxidation activity, lower reaction conversion rate, slow reaction speed, etc., and achieve effective utilization rate, fast reaction rate, and utilization rate high effect

Inactive Publication Date: 2019-05-14
ZHEJIANG XINHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the traditional H 2 o 2 The process uses prepared hydrogen peroxide as raw material. The storage and transportation of high-concentration hydrogen peroxide has great safety hazards, while low-concentration hydrogen peroxide itself contains a large amount of water. After the reaction, a large amount of waste water will be generated, causing pollution. The oxidation activity is relatively low, which will reduce the conversion rate of the reaction
In addition, because hydrogen peroxide is a water phase, and pinene is an oil phase, the two are incompatible with each other, resulting in a very slow reaction rate, often requiring the use of a large amount of solvents and phase transfer catalysts to promote the reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 5.0g Al 2 o 3 , 30g pinene, 1.5g NaHCO 3 , start stirring, control the temperature at 50 ° C, add 1050 g of anthraquinone working solution with hydrogen peroxide within 3 hours through the dropping funnel, and recover Al by filtration after the reaction is completed 2 o 3 , standing to separate the water generated by the reaction, the oil phase was washed with sodium hydroxide and sodium sulfate solution to neutrality, and the heavy aromatics were recovered by rectification under reduced pressure, and 2,3-epoxy pinane was obtained after rectification under reduced pressure. According to gas chromatography analysis, the conversion rate of α-pinene was 96%, and the yield rate of epoxy pinane was 92%. The still liquid after rectification is a mixed solution of trioctyl phosphate and anthraquinone, which is mixed with recovered heavy aromatics and returned to the hydrogenation tower of the hydrogen peroxide process as a working liquid for recycling.

Embodiment 2

[0026] Add 5.0g SiO2 to a 2000ml four-necked flask with condenser, stirrer, thermometer and dropping funnel 2 , 30g pinene, 1.4g NaHCO 3 , start stirring, control the temperature at 45 ° C, add 1050 g of anthraquinone working solution with hydrogen peroxide within 2.5 hours through the dropping funnel, and recover SiO by filtration after the reaction is completed. 2 , standing to separate the water generated by the reaction, the oil phase was washed with sodium hydroxide and sodium sulfate solution to neutrality, and the heavy aromatics were recovered by rectification under reduced pressure, and 2,3-epoxy pinane was obtained after rectification under reduced pressure. According to gas chromatography analysis, the conversion rate of α-pinene was 99.4%, and the yield rate of epoxy pinane was 95%. The still liquid after rectification is a mixed solution of trioctyl phosphate and anthraquinone, which is mixed with recovered heavy aromatics and returned to the hydrogenation tower ...

Embodiment 3

[0028] Add 5.0g of SnO to a 2000ml four-necked flask with condenser, stirrer, thermometer and dropping funnel 2 , 30g pinene, 1.5g NaHCO 3 , start stirring, control the temperature at 55 ° C, add 1100 g of anthraquinone working solution carrying hydrogen peroxide within 3.5 hours through the dropping funnel, and recover SnO by filtration after the reaction is completed. 2 , standing to separate the water generated by the reaction, the oil phase was washed with sodium hydroxide and sodium sulfate solution to neutrality, and the heavy aromatics were recovered by rectification under reduced pressure, and 2,3-epoxy pinane was obtained after rectification under reduced pressure. The conversion of α-pinene was analyzed by gas chromatography to be 100%, and the yield of pinane epoxy was 96%. The still liquid after rectification is a mixed solution of trioctyl phosphate and anthraquinone, which is mixed with recovered heavy aromatics and returned to the hydrogenation tower of the hyd...

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Abstract

The invention relates to a synthesis method for preparing 2,3-epoxypinane by epoxidizing alpha-pinene, and belongs to the field of chemical synthesis. The invention provides a method for preparing the2,3-epoxypinane by epoxidizing the alpha-pinene. The method includes the following steps: directly taking an anthraquinone working solution carrying hydrogen peroxide after catalytic hydrogenation and oxidation as an oxidant; adding the anthraquinone working solution into a reactor mixed with the alpha-pinene, bicarbonate and a catalyst for reaction; and filtering, layering, cleaning and decompressing rectification after the reaction is finished to obtain the 2,3-epoxypinane. The method has the characteristics of low cost, mild reaction conditions, convenient operation, fast reaction speed, high conversion rate, good selectivity and the like, and the process is safe and reliable and pollution-free.

Description

technical field [0001] The invention relates to a synthesis method for preparing 2,3-epoxy pinane by epoxidation of α-pinene, which belongs to the field of chemical synthesis, in particular to the field of fragrance chemistry. technical background [0002] my country is rich in turpentine resources, and its main component, pinene, has very active chemical properties and is an important raw material in the perfume industry. Among them, 2,3-epoxy pinane, which is produced by epoxidation of α-pinene, is the preparation An important intermediate of sandalwood spices. The epoxidation reaction of α-pinene can be realized in a variety of ways. At present, there are mainly hydrogen peroxide epoxidation, inorganic peroxide epoxidation, organic peroxide epoxidation, and sodium hypochlorite epoxidation. The peroxide epoxidation process has great safety hazards due to the instability of the peroxide itself; the sodium hypochlorite oxidation process needs to use expensive quaternary ammo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/12
Inventor 刘承伟应思斌朱玉成黄小朋黄菊王凤州诸葛成夏雅平孙小林方胜军杨秀峰
Owner ZHEJIANG XINHUA CHEM
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