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Method for preparing ocimene from thermo isomeric alpha-pinene in liquid phase

A technology for thermal isomerization and basilene, which is applied in the fields of isomerization to produce hydrocarbons, distillation purification/separation, etc., can solve the problems of poor basilene selectivity, high cost of instruments and equipment, harsh reaction conditions, etc., and achieves a small difference in boiling point. , The effect of low equipment cost and high selectivity

Inactive Publication Date: 2015-06-03
江西嘉源香料有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0007] In order to solve the problems of relatively harsh reaction conditions, high cost of equipment, poor selectivity of ocimene, and high energy consumption in the existing method of cracking α-pinene to prepare ocimene, the present invention provides a method for thermal isomerization of α-pinene in liquid phase. The method for preparing ocimene from pinene has the advantages of simple operation, low equipment cost, high ocimene selectivity, high yield, good quality, continuous batch production, environmental friendliness and pollution-free, low energy consumption, economic benefit and market great prospects

Method used

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  • Method for preparing ocimene from thermo isomeric alpha-pinene in liquid phase
  • Method for preparing ocimene from thermo isomeric alpha-pinene in liquid phase
  • Method for preparing ocimene from thermo isomeric alpha-pinene in liquid phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Install the experimental setup, and then check the airtightness of the entire system. The air in the system was replaced with pure nitrogen. Inject 200ml of α-pinene into the reaction flask, add 0.80g of inhibitor BHT, and start magnetic stirring. Add pure α-pinene to the reaction chamber so that the cracking coil is submerged in the liquid, about 70ml. Turn on the vacuum pump to draw a vacuum, and turn on the condensate at the same time. After normalization, start heating the reaction flask with an oil bath. After the liquid boils, turn on the rectification tower to keep warm with voltage, and reflux for 1-2 hours. When the equilibrium is reached, the temperature at the top of the tower should be between 55-59°C. Adjust the ratio of the reflux flow rate to the production flow rate, that is, the reflux ratio is 1:1, so that α-pinene can be effectively separated. After the system runs smoothly (about 1-2h), the cracking reaction starts. The cracking voltage of the n...

Embodiment 2-5

[0031] The experimental operation method of Example 2-5 is the same as that of Example 1, except that the cracking voltage is different in Example 2-5, and the experimental results are shown in Table 2.

Embodiment 6-7

[0033] The experimental operation method of Embodiment 6-7 is the same as that of Embodiment 1, except that the liquid flow rate is different in Embodiment 6-7, and the experimental results are shown in Table 2.

[0034] Table 2 Experimental results of liquid phase cracking of α-pinene under different conditions.

[0035]

[0036] a. 1. α-pinene; 2. Dipentene; 3. Ocimene; 4. Allo-ocimene. The cycle time is 20h; Y represents the percentage content of each component in the cracked product (the peak of the corresponding peak in the gas chromatography Area); X represents the conversion rate of raw materials; S represents the selectivity of each component; b. Theoretical calculation value.

[0037] Examples 2-5 show that the thermal isomerization of α-pinene increases with the increase of reaction temperature, the conversion rate of α-pinene increases but the selectivity of ocimene decreases. From Examples 5-7, it can be concluded that with the increase of the liquid flow rate,...

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Abstract

The invention discloses a method for preparing ocimene from thermo isomeric alpha-pinene in a liquid phase, and belongs to a method for preparing ocimene. According to the method, no organic solvent or catalyst is needed; nitrogen carrier gas is not needed; only a pure alpha-pinene liquid needs to flow through the surface of an electrical heating nickel chrome wire at a proper speed, and is subjected to thermal isomerization reaction; and a reaction temperature of 300-800 DEG C is estimated while the temperature of the alpha-pinene in a liquid environment in a decompressed state is kept at 50-100 DEG C, so that the product after thermal cracking is rapidly cooled to below 100 DEG C by the surrounding liquid; and the transformation process from ocimene to alloocimene is effectively inhibited. The alpha-pinene thermal isomerization reaction is combined with operations of rectifying and separating the alpha-pinene, so that the transformation rate of raw materials and the yield of the ocimene are improved; a good effect is reached; the method is simple to operate; the equipment cost is low; and the ocimene is high in selectivity, high in yield, good in quality, free of pollution and large in economic benefits.

Description

technical field [0001] The patent of the present invention relates to a method for preparing ocimene by thermal isomerization of α-pinene in liquid phase, especially in this method neither any organic solvent and catalyst nor nitrogen as carrier gas is needed, only pure α-pinene The pinene liquid flows through the surface of the electrically heated nickel-chromium wire at a suitable speed to undergo a thermal isomerization reaction. Background technique [0002] Turpentine is one of the most important natural resources. α-pinene is the main component of turpentine, accounting for about 50-90%, and β-pinene accounts for about 5-20%. In foreign countries, especially developed countries in the United States and Western Europe, they are used as the most important chemical raw materials, with a comprehensive utilization rate of 97%, and a wide variety of products have been developed. Our country is rich in turpentine resources, but a large amount of turpentine is used as a c...

Claims

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Application Information

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IPC IPC(8): C07C11/21C07C5/31C07C7/04
Inventor 齐欣何金洞唐向阳赵温涛
Owner 江西嘉源香料有限公司
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