CN106867673A - The apparatus and method that essential oil of tobaccos is extracted in a kind of superheated vapour distillation - Google Patents

Abstract

The invention discloses a device for extracting tobacco essential oil by superheated steam distillation, comprising: a distillation tank (9), the outer layer of which has a heating device (10), the upper port of which is connected to a condensation pipe (1) through a distillation gas outlet (8) The lower part, its lower port is connected to the upper port of the hot water steam generating device (12) through the water vapor outlet (11); the oil-water separator (5), its upper port is connected to the condensation pipe (1) through the condensate outlet (3) The lower port, wherein the upper part communicates with the upper part of the superheated steam generator (12) through the moisture outlet (4), and the lower part has an oil outlet (6). The invention also discloses a method for extracting tobacco essential oil with a superheated steam distillation device.

Description

A device and method for extracting tobacco essential oil by superheated steam distillation

technical field

The invention belongs to the technical field of tobacco chemistry, and in particular relates to a device and method for extracting tobacco essential oil by superheated steam distillation.

Background technique

There are many methods to extract the active ingredients of the volatile components of plants, such as solvent extraction, supercritical fluid extraction, subcritical extraction, steam distillation and so on. Among these methods, supercritical and subcritical extraction methods can be carried out at low temperature without destroying volatile components. However, the equipment of this method is complex and the extraction cost is relatively high. Among many methods, steam distillation is simple, effective, low cost and safe to operate. It is the most commonly used method for plant essential oil extraction.

However, the steam distillation method also has defects in some aspects: on the one hand, the water vapor will be partially condensed in the distillation tank during the distillation process, which reduces the amount of water vapor and the distillation effect; on the other hand, the temperature of saturated water vapor is 100 ℃, if the distillation temperature is too low, some semi-volatile components cannot be evaporated completely, resulting in a low yield of essential oil. Superheated steam distillation is a new steam distillation method newly developed in recent years. When the steam is in a superheated state, the enthalpy value of the steam is much higher than that in the saturated state. Using superheated steam distillation can effectively avoid the steam in the distillation tank. Medium condensation, the distillation temperature can be increased to above 100°C, no longer limited by the boiling point of water; for samples with relatively stable heat, superheated steam distillation can greatly increase the yield of essential oil.

Contents of the invention

The invention discloses a device and method for extracting tobacco essential oil by superheated steam distillation. Compared with the conventional method, the yield rate of the essential oil in the method of the invention is obviously improved.

On the one hand, the object of the present invention is to provide a device for extracting tobacco essential oil by superheated steam distillation; on the other hand, it is to provide a method for extracting tobacco essential oil using the steam extraction device.

A first aspect of the present invention relates to a superheated steam extraction device, which includes:

Distillation tank 9 has heating device 10 on its outer layer, its upper port communicates with the bottom of condensation pipe 1 through distillation gas outlet 8, and its lower port is connected to the upper port of hot water steam generating device 12 through water vapor outlet 11;

The oil-water separator 5, its upper port communicates with the lower port of the condensation pipe 1 through the condensate outlet 3, wherein the upper part communicates with the upper part of the steam generator 12 through the water outlet 4, and the lower part has an oil outlet 6.

Preferably, the outer heating device 10 of the extraction tank 9 is a heating jacket.

Preferably, the outer layer of the condensation pipe 1 is a condensed water interlayer, the condensed water inlet 2 is provided at the lower part of the condensed water interlayer, and the condensed water outlet 7 is provided at the upper part.

Preferably, the extraction tank 9 has a volume of 50-100L.

The second aspect of the present invention relates to the method of using the superheated steam distillation device for preparing tobacco essential oil, comprising the following steps: soaking the smoke sample with citric acid, heating the distillation tank (9), passing through the superheated steam distillation, and distilling Part condensation, oil-water separation, and the steps of collecting tobacco essential oil.

Preferably, the concentration of the citric acid is 5wt%.

The experimental steps of the extraction device of the present invention are as follows: take 20 kg of tobacco samples and infiltrate them with 5% citric acid solution, put the samples into the retort, first pass superheated steam at a temperature of 150°C into the heating jacket, and let the tank body The temperature rises above 100°C, and then the superheated steam enters the distillation tank, and the steam flow rate is 10-25kg/h. The superheated steam entrained with tobacco essential oil is exported from the steam outlet, condensed through the condenser, and the condensate enters the oil-water separator, and after being separated by the oil-water separator (the upper layer is essential oil, the lower layer is water), the water phase re-enters the water vapor through the water phase outlet The generating device is re-gasified to allow the water to be recycled, and at the same time to avoid the loss of a small amount of essential oil in the water phase; the distillation time is 1 to 3 hours. After the distillation is completed, the oily component is released from the oil outlet at the lower part of the oil-water separator, which is tobacco essential oil.

The tobacco essential oil extracted by the present invention is made into a 0.5-3% solution with glycerol triacetate, and the solution is added to the cigarette filter rod according to 7-8% of the weight of the tow; Made into cigarettes. The cigarette samples added with the essential oil of the present invention were subjected to sensory evaluation. Compared with the control, the aroma quality and aroma quantity of the cigarette smoke were improved, the miscellaneous gas and irritation were significantly reduced, and the original aroma style characteristics of tobacco were more prominent.

Compared with the prior art, the present invention has the beneficial effects of:

(1) The present invention uses superheated steam distillation. When the steam is in a superheated state, the enthalpy value of the steam is much higher than that in the saturated state, which can effectively avoid condensation of the steam in the distillation tank, and the distillation temperature can be increased to above 100°C. It is no longer limited by the boiling point of water; for tobacco samples with relatively stable heat, superheated steam distillation can greatly increase the yield of tobacco essential oil.

(2) In the preferred experimental scheme of the present invention, the distilled smoke sample is infiltrated with 5% citric acid solution, which can avoid tobacco alkaloids from steaming out in large quantities with water vapor, and saves the use of acid when conventional steam distillation is used to prepare tobacco essential oil. The step of back extraction to remove tobacco alkaloids.

(3) Tobacco essential oil of the present invention is added by triacetin, considering that triacetin is the most commonly used plasticizer in cigarette filter molding, in the cigarette filter molding process, the compound of the present invention is added by triacetin Adding the ester to the filter is easy to implement in the process, and does not add additional steps in the production process.

(4) Carry out sensory evaluation and smoking to the cigarette sample that added essential oil of the present invention, compare with contrast, the aroma quality and the aroma quality of cigarette smoke are improved, miscellaneous gas, pungency are obviously reduced, and the characteristic of original fragrance style of tobacco is more prominent .

Description of drawings

Fig. 1 is a schematic diagram of a device for extracting tobacco essential oil by superheated steam distillation of the present invention.

Reference signs are: 1-condensation pipe, 2-condensate water inlet, 3-condensate outflow outlet, 4-water phase outlet, 5-oil-water separator, 6-oil phase outlet, 7-condensate water outlet, 8 -distillation gas outlet, 9-distillation tank, 10-jacket heating device, 11-water vapor outlet, 12-superheated steam generating device.

detailed description

The present invention will be further described below in conjunction with the accompanying drawings and embodiments, but the present invention is not limited in any way. Any transformation or replacement based on the teaching of the present invention belongs to the protection scope of the present invention.

Example 1

The device for extracting tobacco essential oil by superheated steam distillation as shown in Figure 1, it comprises extracting tank 9, and its outer layer has heating device 10, and its upper port communicates with the bottom of condensing tube 1 through distillation gas outlet 8, and its lower port passes through The steam outlet 11 is connected to the upper port of the hot water steam generating device 12;

The oil-water separator 5, its upper port communicates with the lower port of the condensation pipe 1 through the condensate outlet 3, wherein the upper part communicates with the upper part of the superheated steam generator 12 through the water outlet 4, and the lower part has an oil outlet 6.

The outer layer heating device 10 of the extraction tank 9 is a water vapor heating interlayer.

The outer layer of the condensation pipe 1 is a condensed water interlayer, the condensed water inlet 2 is arranged at the lower part of the condensed water interlayer, and the condensed water outlet 7 is arranged at the upper part.

The volume of the extraction tank 9 is 50-100L.

The working principle of the water vapor extraction device is as follows: put the extract to be extracted into the extraction tank, use the water vapor in the superheated steam generator to extract, the condensed water inlet of the condensation pipe is passed into cold water, and the water vapor in the extraction tank is heated The interlayer is fed with water vapor. After the volatile components extracted by water vapor are condensed by the condenser pipe, the water vapor becomes liquid water, and enters the oil-water separator together with the volatile components. After being separated by the oil-water separator, the water re-enters the steam generating device through the water outlet, and It is recycled; the extraction time is 1 to 3 hours. After the extraction is completed, the oily component is released from the oil outlet at the lower part of the oil-water separator, which is the volatile component extract with high purity.

Example 2

Using the superheated steam generating device in Example 1 to extract the volatile components in the tobacco, the specific steps are as follows:

10kg of tobacco leaves are ground into tobacco powder with a pulverizer, put into a 100L extraction tank, add 1L of 5wt% citric acid aqueous solution (effect: the tobacco leaves contain a large amount of volatile nicotine and other alkaline substances, if extracted, Will affect the quality of volatility, citric acid is combined with alkaline substances to become ionic compounds, less volatile, and denser than water), and then extracted with water vapor in a superheated steam generating device. The condensed water inlet of the condenser pipe is fed with cold water, and the water vapor heating interlayer of the extraction tank is fed with water vapor. After the volatile components extracted by the water vapor are condensed by the condenser pipe, the water vapor becomes liquid water and enters the oil and water together with the volatile components. Separator, after being separated by the oil-water separator, the water re-enters the superheated steam generator through the water outlet, and the water is recycled; the extraction time is 1 to 3 hours. After the extraction is completed, the volatile components are released from the oil outlet at the lower part of the oil-water separator It is the volatile extract of tobacco with higher purity.

Example 3

Use the superheated steam generating device among the embodiment 1 to extract the volatile components in the Radix Glycyrrhizae, concrete steps are as follows:

Put 5 kg of licorice powder into a 50L extraction tank, then extract it with the water vapor in the superheated steam generating device, the condensed water inlet of the condensation pipe is fed with cold water, and the water vapor heating interlayer of the extraction tank is passed into water vapor, and the water vapor After the extracted volatile components are condensed by the condenser tube, the water vapor turns into liquid water and enters the oil-water separator together with the volatile components. After being separated by the oil-water separator, the water re-enters the superheated steam generator through the water outlet, and the water is obtained. Recycling; the extraction time is 1 to 3 hours. After the extraction is completed, the oily component released from the oil outlet at the lower part of the oil-water separator is the volatile extract of licorice with higher purity.

Claims (4)

1. A superheated steam distillation device, characterized in that, comprising: The distillation tank (9) has a heating device (10) on its outer layer, its upper port is connected to the lower part of the condensation pipe (1) through the distillation gas outlet (8), and its lower port is connected to the hot water through the hot water steam outlet (11). The upper port of the steam generating device (12); The oil-water separator (5), its upper port communicates with the lower port of the condensation pipe (1) through the condensate outlet (3), wherein the upper part communicates with the upper part of the superheated steam generator (12) through the moisture outlet (4), The lower part has an oil outlet (6). 2. The superheated steam distillation device according to claim 1, characterized in that the temperature of the superheated steam is 120-200°C. 3. a method for preparing tobacco essential oil by a superheated steam distillation device according to claim 1, is characterized in that, comprises the following steps: the smoke sample is infiltrated with citric acid, the retort (9) is heated, and passed through Hot water steam distillation, distillate condensation, oil-water separation, and the steps of collecting tobacco essential oil. 4. The method according to claim 3, characterized in that the concentration of the citric acid is 5 wt%.