Method for continuously separating alpha-pinene and beta-pinene from turpentine

A technology of turpentine oil and tower kettle, applied in the direction of distillation purification/separation, organic chemistry, etc., can solve the problems of increasing raw material loss, prone to side reactions, and difficult control of the reaction process, etc., to prolong the collection time, increase the reflux ratio, and save energy effect

Active Publication Date: 2014-11-05
GUANGXI FORESTRY RES INST
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AI Technical Summary

Problems solved by technology

The above two inventions improve the purity of β-pinene by reaction plus rectification, but the reaction process is not easy to control and side reactions are prone to occur, which increases the loss of raw materials, reduces the flexibility of production, and cannot obtain high-purity α-pinene at the same time. -pinene and β-pinene

Method used

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  • Method for continuously separating alpha-pinene and beta-pinene from turpentine

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Experimental program
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Effect test

Embodiment 1

[0026] Masson pine turpentine, the main components are: 80.5% α-pinene, 2.0% pinene, 8.2% β-pinene, 1.0% myrcene, 1.8% limonene, 3% longifolene, 0.5% β-caryophyllene. The air in the rectification tower is exhausted with a sliding valve vacuum pump, and the vacuum degree in the rectification tower reaches -0.09MPa. The raw material is sucked into the rectification tower tower through the negative pressure of the rectification tower tank and the raw material storage tank. Open the inlet valve of the column pipe heated by steam in the bottom of the rectification column to heat the raw materials in the bottom of the column, and at the same time open the water inlet valves of the condenser and cooler at the top of the tower. The temperature of the tower bottom is controlled at 100-110°C, the temperature of the top of the tower is controlled at 80-95°C, and the total reflux is 0.5-1h, then the product discharge valve is opened, the reflux ratio is controlled at 8:1-10:1, and the frac...

Embodiment 2

[0028] The main components of slash pine turpentine are: α-pinene 59.2%, pinene 1.5%, β-pinene 28.2%, myrcene 1.1%, limonene 8.5%. The air in the rectification tower is exhausted with a sliding valve vacuum pump, and the vacuum degree in the rectification tower reaches -0.09MPa. The raw material is sucked into the rectification tower tower through the negative pressure of the rectification tower tank and the raw material storage tank. Open the inlet valve of the column pipe heated by steam in the bottom of the rectification column to heat the raw materials in the bottom of the column, and at the same time open the water inlet valves of the condenser and cooler at the top of the tower. The temperature of the tower bottom is controlled at 100-110°C, the temperature of the top of the tower is controlled at 80-95°C, and the total reflux is 0.5-1h, then the product discharge valve is opened, the reflux ratio is controlled at 8:1-10:1, and the fractionated product is Perform specifi...

Embodiment 3

[0030]Simao pine turpentine oil (β-pinene type), the main components are: 49.5% α-pinene, 1.2% β-pinene, 39.4% β-pinene, 3.7% 3-carene, 0.86% limonene, and 3.0% longifolene %, β-caryophyllene 0.5%. The air in the rectification tower is exhausted with a sliding valve vacuum pump, and the vacuum degree in the rectification tower reaches -0.09MPa. The raw material is sucked into the rectification tower tower through the negative pressure of the rectification tower tank and the raw material storage tank. Open the inlet valve of the column pipe heated by steam in the bottom of the rectification column to heat the raw materials in the bottom of the column, and at the same time open the water inlet valves of the condenser and cooler at the top of the tower. The temperature of the tower bottom is controlled at 100-110°C, the temperature of the top of the tower is controlled at 80-95°C, and the total reflux is 0.5-1h, then the product discharge valve is opened, the reflux ratio is cont...

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Abstract

The invention relates to a method for continuously separating alpha-pinene and beta-pinene from turpentine. The method comprises the following steps: raw materials are subjected to a preheating treatment; a packed tower vacuum rectification process is carried out; alpha-pinene is collected with a reflux ratio of 8:1-10:1; a middle fraction is slowly collected with a reflux ratio of 20:1-30:1; beta-pinene is collected with a reflux ratio of 8:1-15:1; and when distillation is finished, while the rectification tower is not cooled and the vacuum state is not relieved, discharge is realized through the pressure difference between a tower kettle and a residual liquid tank. Therefore, intermittent distillation continuous operation is realized. With the method provided by the invention, the content of obtained alpha-pinene can be 98%, and the content of obtained beta-pinene can be 95%.

Description

technical field [0001] The invention relates to the field of separation and purification of natural flavors and fragrances, in particular to a method and equipment for continuously separating high-purity α-pinene and β-pinene from turpentine. Background technique [0002] The annual output of turpentine in my country is about 70,000 tons, which mainly contains α-pinene, β-pinene, limonene, longifolene, caryophyllene, cedrene, α-santalene, etc. The content of each component varies with tree species. The content of α-pinene is about 65-86%, the content of β-pinene is 13.9-67.4%, and the others are mainly longifolene and caryophyllene. Many precious spices can be synthesized with high-purity α-pinene and β-pinene. For example, using α-pinene as a starting material, pinone acid or pinone aldehyde can be obtained by oxidation, and further reaction can obtain four Member ring spices; Myrcene can be obtained by pyrolysis of β-pinene, and further spices such as ionone and ambroxone ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/04C07C13/42C07C13/40
Inventor 陆顺忠孟中磊李秋庭关继华黎贵卿邱米时胜德杨漓杨素华江燕唐宾曾辉梁剑恭苏骊华党中广
Owner GUANGXI FORESTRY RES INST
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