JPH07227502A - Method for extracting soluble matter from natural solid raw material - Google Patents

Abstract

PURPOSE:To selectively extract and separate a specific component from a natural solid raw material and also to easily and properly control the content of the specific component and water in the natural solid raw material after treatment. CONSTITUTION:High pressure carbon dioxide is brought into contact with a tobacco raw material housed in a extractor 11 to dissolve and extract nicotine contained in the tobacco raw material into the high pressure carbon dioxide. Next, the high pressure carbon dioxide contg. the extracted nicotine is brought into contact with absorbing water 18 housed in an absorber 17 to absorb the nicotine. Then, the high pressure carbon dioxide from which the nicotine has been absorbed is again returned to the extractor 11 and circulated. Here, the inside of the extractor 11 is set in a pressure range of 200 to 300kg/cm<2> and in a temperature range of 50 to 80 deg.C, and the inside temperature of the absorber 17 is set in a range of 40-60 deg.C. The relative ratio of the water content to the high pressure carbon dioxide at extraction is set in the range of 55-80%.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention relates to, for example, a cigarette and a cigarette.
The present invention relates to a soluble matter extraction method for extracting components such as nicotine and caffeine from natural solid raw materials such as tea, black tea and green tea.

[0002]

2. Description of the Related Art Conventionally, as a method for extracting specific components such as nicotine and caffeine from natural solid raw materials such as tobacco, coffee, black tea and green tea, for example, high pressure fluid such as carbon dioxide in a supercritical state. There is known a method in which a natural solid raw material is brought into contact with a raw material to dissolve a specific component and then extracted.

In the extraction method using such a high-pressure fluid, the specific component is separated from the high-pressure fluid containing the specific component,
As a method for recovering, for example, a pressure change separation method is known. In this pressure separation method, for example, carbon dioxide as a high-pressure fluid is heated to a predetermined temperature of, for example, 70 ° C. in a heat exchanger, and then introduced into an extractor containing a natural solid material using a supply pump. The inside of this extractor is maintained at a predetermined pressure, for example, 250 kg / cm ² . Under such pressure and temperature conditions, the specific component contained in the natural solid raw material is dissolved in carbon dioxide and extracted. Then, carbon dioxide containing the extracted specific component is introduced into the separator. Since the inside of this separator is set to a pressure lower than that of the extractor, for example, 50 kg / cm ² , the specific component dissolved in carbon dioxide is separated due to the difference in the dissolving power.

On the other hand, it is known that when water is added to such a high-pressure fluid as a so-called entrainer, a specific component of the natural solid raw material is efficiently dissolved in the high-pressure fluid and the extraction rate can be increased. As a method of adding water, conventionally, a method of adding water to the natural solid raw material itself for humidification, a method of containing water in a high-pressure fluid, or a method of using both of them together has been carried out.

[0005]

However, in the above-mentioned pressure change separation method, components soluble in the high pressure fluid other than the required specific components are also extracted into the high pressure fluid and removed outside the system in the separator. . For example, when carbon dioxide is used as a high-pressure fluid to extract nicotine from tobacco, tobacco components other than nicotine, in particular, the fats and oils (wax) that make up the scent and taste of tobacco are also dissolved in carbon dioxide and extracted. And will be separated by the separator. As a result, the flavor and aroma of the cigarette is significantly deteriorated, and the quality is remarkably deteriorated. In addition, when caffeine is extracted from black tea, green tea, or coffee, components other than caffeine, particularly aromatic components such as essential oil components, are simultaneously extracted and separated and removed by a separator. As a result, the flavor is significantly reduced and the quality is reduced.

Further, in the above-mentioned pressure change separation method, since a new high pressure fluid is constantly supplied to extract a specific component, if the extraction time is lengthened, all the specific components in the natural solid raw material will be contained in the high pressure fluid. It will be extracted and lost. Therefore, for example, when producing a product in which the content of a specific component in a natural solid raw material such as low nicotine tobacco and low caffeine coffee is reduced to a desired level, the conventional pressure change separation method is used. , The extraction time must be adjusted appropriately after investigating the change over time of specific components. As a result, the operation of the extraction process becomes extremely complicated, and it is very difficult to manufacture a product containing a specific component with a desired concentration without variation.

On the other hand, when water is added to a high-pressure fluid as an entrainer, the conventional method of adding water often contains more water than necessary in the treated natural solid raw material. This not only makes it difficult to handle the treated natural solid raw material, but also causes the problem of deterioration due to the propagation of microorganisms. Therefore, a drying step of drying the treated raw material until the water content becomes appropriate is required, and the manufacturing cost becomes expensive as the number of manufacturing steps increases.

The present invention has been made in view of the above points, and it is possible to selectively extract and separate a specific component of a natural solid raw material, and at the same time, to treat the aroma component and water in the natural solid raw material. Provided is a method for extracting a soluble matter from a natural solid raw material, in which the content of is easily and appropriately adjusted.

[0009]

According to the present invention, high-pressure carbon dioxide is brought into contact with a natural solid raw material contained in an extractor so that a plurality of different kinds of components contained in the natural solid raw material are mixed with the high-pressure carbon dioxide. A step of dissolving and extracting the high-pressure carbon dioxide containing the plurality of different types of extracted components, among the plurality of different types of components by contacting with a predetermined amount of water contained in the absorber A method for extracting a soluble matter comprising a step of absorbing a water-soluble component in the water, and a step of returning the high-pressure carbon dioxide after the water-soluble component is absorbed to the extractor and circulating the extract, There is provided a method for extracting a soluble matter from a natural solid raw material, wherein a temperature difference is provided so that the temperature inside the vessel is higher than the temperature inside the absorber.

Here, preferably, the temperature inside the extractor and the temperature inside the absorber are adjusted so that the relative water content of the high-pressure carbon dioxide during extraction is in the range of 55 to 80%. Also, preferably, the temperature in the extractor is 50-80.
The temperature in the absorber is in the range of 40 ° C to 60 ° C.
Is the range.

[0011]

According to the method for extracting a soluble matter from a natural solid raw material of the present invention, the natural solid raw material contained in the extractor is contacted with high-pressure carbon dioxide, so that a plurality of different kinds of components contained in the natural solid raw material are contained. Are dissolved and extracted. High-pressure carbon dioxide containing these components, the water-soluble components of the components are dissolved and absorbed in water by contact with a predetermined amount of water contained in the absorber, the high-pressure carbon dioxide holds a part of the components While being discharged from the absorber.

More specifically, the natural solid raw material contained in the extractor is contacted with high-pressure carbon dioxide to dissolve and extract components including a water-soluble component and a hydrophobic component. High-pressure carbon dioxide containing this component is absorbed by dissolving only a water-soluble component in the component by contact with a predetermined amount of water contained in the absorber, high-pressure carbon dioxide is a hydrophobic component in the component It is discharged from the absorber while holding only.

The high-pressure carbon dioxide holding only the hydrophobic component is introduced into the extractor again and acts as an extracting solvent. The high pressure carbon dioxide thus circulates in a closed cycle constructed between the extractor and the absorber. As a result, the concentration of the hydrophobic component in the high-pressure carbon dioxide increases, and eventually the hydrophobic component in the natural solid raw material dissolves in the high-pressure carbon dioxide and the hydrophobic component in the high-pressure carbon dioxide re-adsorbs to the natural solid raw material. The equilibrium state is reached and apparently no dissolution of the hydrophobic component in the natural solid raw material into the high pressure carbon dioxide occurs. Therefore, it is possible to minimize the extraction of the hydrophobic component in the natural solid raw material.

On the other hand, the water-soluble component in the natural solid raw material is extracted by the high-pressure carbon dioxide circulating in the closed cycle, and is absorbed by the predetermined amount of water stored in the absorber. As a result, the water-soluble component concentration of water in the absorber increases, and eventually the water-soluble component concentration between water and high-pressure carbon dioxide reaches an equilibrium state, apparently absorbing the water-soluble component in high-pressure carbon dioxide to water. Will not happen. Furthermore, the movement of the water-soluble component between the natural solid raw material and the high-pressure carbon dioxide reaches an equilibrium state, and apparently the water-soluble component in the natural solid raw material is not dissolved in the high-pressure carbon dioxide. That is, a part of the components of the natural solid raw material is absorbed in water, and the remaining components remain in the natural solid raw material. Therefore, the content of the water-soluble component in the natural solid raw material after the extraction treatment can be adjusted by changing the amount of water inside the water absorber per natural solid raw material.

Further, the water contained in the absorber absorbs the water-soluble components in the high-pressure carbon dioxide and is dissolved in the high-pressure carbon dioxide to act as an entrainer, increasing the extraction efficiency in the extractor.

Further, since the amount of water dissolved in the high-pressure carbon dioxide when passing through this absorber becomes a saturation amount specified by the temperature of the absorber, the high-pressure carbon dioxide can be adjusted by adjusting the temperature of the absorber. The amount of water in carbon can be adjusted. On the other hand, since the temperature of the extractor is set higher than the temperature of the absorber, the relative moisture content of the high-pressure carbon dioxide containing a saturated amount of water at the absorber temperature is reduced in the extractor.
Here, the relative water content φ is expressed as follows.

Φ = (y / ys) × 100 [%] y: weight of water contained in a constant weight of high-pressure carbon dioxide [k
_{g-H 2 O / kg-} CO 2] ys: the weight of water contained in the high-pressure carbon dioxide when in a saturated state at the temperature _{[kg-H 2 O / kg} -C
O ₂ ] Therefore, by adjusting the temperature of the extractor and the temperature of the absorber, it becomes possible to bring high-pressure carbon dioxide having an appropriate relative water content into contact with the natural solid raw material at the time of extraction. The water content of the raw material is adjusted appropriately.

Furthermore, by setting the relative water content of the high-pressure carbon dioxide at the time of extraction to 55-80%, the temperature in the extractor is preferably in the range of 50-80 ° C, and the temperature in the absorber is preferably set. By setting the temperature in the extractor to a range of 40 to 60 ° C. and setting the temperature in the extractor higher than the temperature in the absorber to adjust the relative water content of the high-pressure carbon dioxide within the range, the extraction process is efficiently performed. In addition, the flavor quality of the natural solid raw material after treatment can be maintained.

[0019]

Embodiments of the present invention will be described below with reference to the drawings.

Example 1 In this example, the case where nicotine is extracted as a specific component from a tobacco raw material will be described as an example.

FIG. 1 is a schematic diagram showing an example of an extraction apparatus 10 used in the method for extracting soluble matter from a natural solid material of the present invention.

Reference numeral 11 in the drawing denotes an extractor (internal volume 9 liters, internal container for filling tobacco raw material 4 liters in volume) filled with a tobacco raw material. A jacket 12 for temperature adjustment is provided on the outer peripheral portion of the extractor 11. At the inlet side of the extractor 11, a supply pump (not shown) for supplying carbon dioxide (CO ₂ ) and a first heat exchanger 14 are provided.
A system path A is provided to reach the extractor 11 via. A flow meter 15 is provided between the extractor 11 and the first heat exchanger 14.

On the other hand, on the outlet side of the extractor 11, a system path B is provided which leads to the absorber (internal volume 6 liters) 17 via the second heat exchanger 16. A predetermined amount of absorbed water 18 is stored inside the absorber 17. A jacket 19 for temperature control is provided on the outer peripheral portion of the absorber 17.

Further, the outlet side of the absorber 17 is passed through the circulation pump 20 to the above-mentioned supply pump 13 to the extractor 11
A system path C that joins the system path A leading to is provided. A discharge valve 21 for discharging carbon dioxide is provided in a branched manner between the absorber 17 and the circulation pump 20 of the system C. A check valve 22 is provided between the supply pump 13 and the confluence of the system paths A and C to prevent the circulating carbon dioxide from flowing back to the supply pump 13.

Extraction of nicotine in the tobacco raw material is performed as follows using the extraction device 10 having the above-mentioned structure.

First, the tobacco container is filled with the tobacco raw material. On the other hand, the absorber 17 is filled with a predetermined amount of absorbed water 18.

The temperature inside the extractor 11 is set to the jacket 12
Is set to an arbitrary temperature within the range of 60 to 70 ° C. (hereinafter referred to as extraction temperature). Also, the absorber 17
The temperature inside the container (hereinafter referred to as absorption temperature) is jacket 1
9, the temperature is set to an arbitrary temperature within the range of 40 ° C to 60 ° C.

On the other hand, with the discharge valve 21 closed, carbon dioxide is supplied from the supply source by the supply pump 13.
The first heat exchanger 14 heats to the extraction temperature. Line A ~
Since C has a closed cycle, carbon dioxide is not discharged outside the system, and the pressure of carbon dioxide increases. The carbon dioxide pressure is 100 to 300 kg / cm ² , preferably 200.
When an arbitrary pressure within the range of 300 kg / cm ² (hereinafter referred to as extraction pressure) is reached, the supply pump 13 is stopped.

Next, the circulation pump 20 is operated and the system line A-
Carbon dioxide is circulated in a closed cycle consisting of BC. Confirm the circulation flow rate of carbon dioxide with the flow meter 15,
Adjust to 200 kg / h.

By circulating carbon dioxide as described above, nicotine is extracted from the tobacco raw material. That is, when high-pressure carbon dioxide comes into contact with the tobacco raw material with which the inside of the extractor 11 is filled, water-soluble components such as nicotine and hydrophobic components such as fats and oils contained in the tobacco raw material are dissolved in carbon dioxide and extracted. . Next, the carbon dioxide after the extraction process flows out of the extractor 11, and then passes through the system B,
It is cooled to the absorption temperature by the second heat exchanger 16 and introduced into the absorber 17. In the absorber 17, the carbon dioxide after the extraction treatment comes into contact with the absorbed water 18, and only the water-soluble component such as nicotine contained in the carbon dioxide is dissolved and absorbed in the absorbed water 18. Carbon dioxide containing a hydrophobic component such as oil or fat from which nicotine or the like has been separated is returned to the system A through the system C and used for the above-mentioned extraction treatment.

While repeating such a cycle, only the water-soluble component such as nicotine is gradually separated and recovered in the absorbed water 18 contained in the absorber 17. After circulating the carbon dioxide for a predetermined time, stop the circulation pump 20,
The discharge valve 21 is opened to discharge the carbon dioxide in the paths A to C and open it to the atmosphere. In this way, the processed tobacco raw material in which nicotine has been extracted is obtained inside the extractor 11.

Tests conducted in the above-mentioned method for extracting nicotine from a tobacco raw material by changing various operating conditions will be described below.

Test Example 1 In order to investigate the relationship between the extraction pressure and the nicotine removal rate, water content and taste quality of the tobacco material after treatment, the extraction pressure was set between 150 and 300 kg / cm ² as shown in Table 1. Extraction was performed according to the procedure described above under the following operating conditions except that the above procedure was changed. In this test, the tobacco raw material was a blended product, and the nicotine content on a dry weight basis was 1.9.
A chopped tobacco raw material having a water content of 9% and a dry weight-based water content of 12.5% was used.

Operating conditions Extraction temperature: 70 ° C. Absorption temperature: 53 ° C. Relative water content of carbon dioxide: 70% Amount of absorbed water: 1000 g Circulating flow rate of carbon dioxide: 200 kg / h Extraction time: 2 hours The relative water content is defined as Wes, which is the saturated dissolution amount of carbon dioxide water at the extraction pressure P and the extraction temperature Te of the extractor 11, and Wts which is the saturated dissolution amount of carbon dioxide water at the pressure P and the absorption temperature Tt. When the relative water ratio [(actual water content ÷ saturated water content) x 100] at the extraction pressure P and the extraction temperature Te of the vessel 11 is R [%], the water content We of carbon dioxide passed through the absorber 17 Is
The value is adjusted to the value shown by the following equation (1).

We = Wts = (Wes × R) / 100 (1) Wes in the above equation is the extraction pressure P and the extraction temperature that are set in advance.
Since it depends on Te, the relative water content R is
Saturated dissolution amount of carbon dioxide in water Wts, that is,
It can be adjusted by the absorption temperature Tt.

After the extraction treatment, the nicotine content and water content of the tobacco raw material were measured. Then, after smoking in a room at 22 ° C. and 60% RH for 24 hours, a smoking test was conducted to evaluate the taste quality. The results are also shown in Table 1.

[0037]

[Table 1]

* Nicotine removal rate: {1- (nicotine content of tobacco raw material after treatment ÷ nicotine content of tobacco raw material before treatment)} x 100 (%) The taste quality was evaluated using untreated tobacco raw material. As a control, the degree of flavor, dislike and irritation due to the treatment was evaluated by a ± 5 point method, and the larger the number, the better the quality. The suitability for use as a raw material for low nicotine tobacco products was evaluated according to the following 4 ranks.

X: Unusable to use Δ: Unusable to use, but with a limited blending ratio ○: Almost all can be used ◎: Unconditionally usable As shown in Table 1, The higher the extraction pressure, the higher the nicotine removal rate of the tobacco raw material after treatment, and the nicotine tended to be easily removed. Especially 200 kg / cm ²
It was found that the nicotine removal rate was significantly increased when the ratio exceeded.

The water content of the tobacco raw material after treatment is
No significant difference was observed due to changes in extraction pressure. All the test results were within the range of 18 to 20%, and almost corresponded to the value corresponding to the water content of the tobacco raw material at the relative humidity of 70% under atmospheric pressure. No problems such as crushing, handling in post-treatment, or deterioration during storage were observed.

Regarding the taste quality, the extraction pressure is 1
The processed tobacco raw material in the case of 50 kg / cm ² is
It was confirmed that the extraction treatment significantly deteriorated the taste and that it could not be used as a raw material for low nicotine tobacco products. On the other hand, the extraction pressure is 200 to 300 kg /
It was confirmed that, when the content was within the range of cm ² , the treated tobacco raw material hardly caused deterioration of taste and could be used as a raw material for low nicotine tobacco products. Of these, especially the extraction pressure is 250 kg
The optimum value was / cm ² .

Test Example 2 Extraction pressure was 250 kg / cm ² , extraction temperature was changed within the range of 50 to 90 ° C. as shown in Table 2, and absorption temperature was changed as shown in Table 2. The nicotine removal rate and the water content of the tobacco material after the treatment were measured according to the same procedure as in Test Example 1 except that the relative water content of carbon dioxide was adjusted to 70%, and the taste quality was evaluated. The results are also shown in Table 2.

[0043]

[Table 2]

As is clear from Table 2, the higher the extraction temperature, the higher the nicotine removal rate of the tobacco material after treatment, and the more easily nicotine was removed. Especially 60 ℃
It was found that the nicotine removal rate was significantly increased when the ratio exceeded.

The water content of the tobacco raw material after treatment is
No significant difference was observed due to changes in extraction temperature. All the test results were within the range of 18 to 20%, and almost corresponded to the value corresponding to the water content of the tobacco raw material at the relative humidity of 70% under atmospheric pressure. No problems such as crushing, handling in post-treatment, or deterioration during storage were observed.

Regarding the taste quality, the extraction temperature is 9
It was confirmed that the tobacco material after the treatment at 0 ° C. had a significantly deteriorated taste due to the extraction treatment and could not be used as a raw material for low nicotine tobacco products. On the other hand, when the extraction temperature is in the range of 50 to 80 ° C., the treated tobacco raw material causes little deterioration in taste and is used as a raw material for low nicotine tobacco products. It was confirmed that it was possible. Of these, the optimum extraction temperature was 70 ° C. Such a result is because only nicotine in the tobacco raw material is reduced, and the fats and oils constituting the scent and taste of the tobacco remain in the tobacco raw material.

Test Example 3 Extraction pressure was 250 kg / cm ² and extraction temperature was 70 ° C.
As a result, after the treatment, the absorption temperature was changed as shown in Table 3 and the relative water content of carbon dioxide at the time of extraction was changed within the range of 60 to 80%. The nicotine removal rate and water content of the tobacco raw material were measured to evaluate the taste quality. The results are also shown in Table 3.

[0048]

[Table 3]

As is clear from Table 3, the higher the relative moisture content of carbon dioxide, the higher the nicotine removal rate of the tobacco material after treatment, and the nicotine tended to be easily removed. The removal rate did not change much.

The water content of the tobacco raw material after treatment is
It is closely related to changes in the relative moisture content, and if the relative moisture content is less than 55%, the moisture content of the tobacco raw material will be low, and the raw material will be crushed during the removal of the tobacco raw material after the treatment or the post-treatment. It was easy. In addition, the taste quality became poor with smoke and became difficult to smoke.

On the other hand, the relative water content of carbon dioxide is 80%.
If it exceeds, the moisture content of the tobacco raw material after the treatment will rapidly increase, the tobacco raw material becomes sticky and the handleability in the post-process deteriorates, and there is a high possibility that spoilage occurs during storage, etc.
It is inevitable that some kind of drying treatment is required, and further deterioration of quality occurs at this time.

On the other hand, when the relative water content of carbon dioxide is 60 to 70%, the water content of the tobacco raw material after treatment is almost the same as the water content when stored at room temperature and atmospheric pressure. No problems such as taking out the tobacco raw material after the treatment, crushing the raw material, handleability in the post-treatment, or deterioration during storage were observed. Regarding the taste quality, it was confirmed that deterioration of the taste was not a problem and that it could be used as a raw material for low nicotine tobacco products without any worry.

From the results of the above Test Examples 1 to 3, in the extraction and separation of nicotine from the tobacco raw material by the circulation absorption type separation as shown in FIG. 1, the extraction pressure is 200 to 300 k.
g / cm ² (especially 250 kg / cm ² ), extraction temperature 6
0-80 ° C (particularly 70 ° C), and absorption temperature of 40-
It was confirmed that the temperature was 60 ° C. (particularly 48 ° C. to 54 ° C.), and it was preferable to set the relative moisture content of carbon dioxide during extraction to be 60 to 70%.

Test Example 4 In order to investigate the relationship between the extraction time and the nicotine concentration of the tobacco raw material after the treatment, the following experiment was conducted.

The filling amount of the tobacco raw material is 300 g and 60
In the case of 0 g, when the nicotine was extracted according to the above-mentioned procedure under the following conditions, the nicotine concentration in the tobacco raw material after the treatment at various extraction times of 0.5 to 3 hours was measured.

Operating conditions Extraction pressure: 250 kg / cm ² Extraction temperature: 70 ° C. Absorption temperature: 53 ° C. Relative water content of carbon dioxide: 70% Absorbed water amount: 1000 g Circulation flow rate of carbon dioxide: 200 kg / h 2 shows the characteristic diagram.

As is clear from FIG. 2, the nicotine concentration in the tobacco raw material after the treatment almost reached equilibrium in about 1 hour. It is obvious that the time required to reach equilibrium depends on the circulation flow rate of carbon dioxide (capacity of the circulation pump), and needless to say it is not necessarily one hour.

Test Example 5 Further, the extraction time was set to 2 hours, and the filling amount of the absorbed water was set to 500.
After the tobacco raw material was extracted by the same procedure as in Test Example 4 except that the amount was changed to 2,000 g, the nicotine concentration in the treated tobacco raw material was measured. The results are shown in the characteristic diagram of FIG.

As is clear from FIG. 3, it was confirmed that the nicotine concentration in the tobacco raw material after the treatment reached the equilibrium state becomes lower as the filling amount of absorbed water increases. This is a tobacco raw material when the nicotine concentration in the tobacco raw material after the treatment as shown in FIG.
Due to the distribution equilibrium of nicotine in absorbed water and carbon dioxide. Therefore, the nicotine concentration in the finally obtained tobacco raw material can be adjusted to an arbitrary value by changing only the filling amount of absorbed water. For example, in order to reduce the nicotine concentration, the filling amount of absorbed water is increased.

Example 2 In this example, the case of extracting caffeine from green tea (Japanese tea) will be described. In addition, in the following test examples, unless otherwise specified, the operation procedure was performed according to the above-described operation procedure for extracting nicotine from the tobacco raw material.

Test Example 6 200 g of green tea (water content before treatment; 2.7%, caffeine content; 3.8%) was filled in the inner container of the extractor 11 of the extraction device 10 shown in FIG. 250 kg / cm ²
Then, the amount of absorbed water, the extraction temperature and the absorption temperature were changed as shown in Table 4, decaffeination from green tea was performed, and the removal rate of caffeine was measured. The results are also shown in Table 4.

[0062]

[Table 4]

From the results of Samples 6-1 and 6-2, it was found that the higher the relative water content (absorption temperature), the higher the removal rate of caffeine at the same extraction temperature. From the results of Samples 6-2 and 6-3, it was found that the higher the extraction temperature, the higher the removal rate of caffeine. In addition, sample 6-3
From the results of 6 and 4-4, it was found that the greater the amount of absorbed water, the higher the removal rate of caffeine. As a result, decaffeination from green tea was also satisfactorily processed throughout, as in the case of the nicotine treatment from tobacco materials described above. Therefore, the flavor of tea obtained by extracting the treated product with hot water was less astringent and easier to drink than the untreated product.

Test Example 7 Next, according to the same procedure as the above-mentioned samples 6-1 to 6-4, black tea 200 having different water contents and caffeine contents was prepared.
g (water content before treatment; 7.6%, caffeine content; 2.
1%) was treated. Referring to Test Example 1 described above, the extraction temperature was 70 ° C., the amount of absorbed water was 3000 g, and the absorption temperature was 54
℃ (relative water content; 70%) and absorption temperature 59 ℃
(Relative water content: 80%). The water content after treatment and the caffeine removal rate in this case are shown in Table 5.

[0065]

[Table 5]

As is clear from Table 5, the higher the relative water content, the slightly higher the caffeine removal rate. However, when the relative water content was as high as 80%, the water content after the treatment was high and the deterioration of the flavor was remarkable, similar to the result of Test Example 3 for tobacco described above.

[0067]

As described above, according to the method for extracting a solubilized product of a natural solid raw material of the present invention, high-pressure carbon dioxide is circulated in a closed cycle including an extractor and an absorber to obtain a natural solid raw material. The water-soluble component of the plurality of different components extracted from is dissolved and absorbed in the absorbed water in the absorber and can be separated into this component and high-pressure carbon dioxide, thus deteriorating the quality of the natural solid raw material. The extraction process can be performed without any need.

Further, when the content of the component in the treated solid raw material reached the equilibrium, the component was distributed and equilibrated in the tobacco raw material, the absorbed water and the carbon dioxide, so that it was housed in the absorber. By changing the amount of water, the content of the component in the natural solid raw material after the treatment can be adjusted easily and accurately.

Further, the extraction pressure and the extraction temperature, and
By setting the internal temperature of the absorber to an appropriate value and setting the relative water content of high-pressure carbon dioxide during extraction to an appropriate range, the natural solid raw material after treatment can be processed without separate drying treatment. The water content of the can be adjusted to the desired value.

[Brief description of drawings]

FIG. 1 is a schematic view showing an example of an extraction apparatus used in the method for extracting a soluble matter from a natural solid material of the present invention.

FIG. 2 is a characteristic diagram showing the relationship between the extraction time and the nicotine content of the tobacco raw material after the treatment.

FIG. 3 is a characteristic diagram showing a relationship between a filling amount of absorbed water and a nicotine content of a tobacco raw material after treatment.

[Explanation of symbols]

10 ... Extractor, 11 ... Extractor, 13 ... Supply pump, 1
4 ... 1st heat exchanger, 16 ... 2nd heat exchanger, 17 ... Absorber, 18 ... Absorbed water, 20 ... Circulation pump, 21 ... Exhaust valve, 22 ... Check valve.

Front page continuation (72) Inventor Yoshio Yonei 6-2 Umegaoka, Aoba-ku, Yokohama-shi, Kanagawa Tobacco Central Research Institute, Tobacco Inc.

Claims (3)

[Claims] 1. A step of contacting high-pressure carbon dioxide with a natural solid raw material contained in an extractor to dissolve a plurality of different kinds of components contained in the natural solid raw material into the high-pressure carbon dioxide and extracting the same. , Contacting the extracted high-pressure carbon dioxide containing the plurality of different types of components with a predetermined amount of water contained in an absorber to absorb the water-soluble component of the plurality of different types of components into the water A method of extracting a soluble matter, comprising: a step of causing the high-pressure carbon dioxide after the water-soluble component is absorbed to be returned to the extractor for circulation, wherein the temperature inside the extractor is the absorber. A method for extracting a soluble matter from a natural solid raw material, which comprises providing a temperature difference so as to be higher than an internal temperature. 2. The temperature inside the extractor and the temperature inside the absorber are controlled so that the relative water content of the high-pressure carbon dioxide during extraction is in the range of 55 to 80%. 1. The method for extracting a soluble matter from a natural solid raw material according to 1. 3. The soluble solid raw material according to claim 1, wherein the temperature in the extractor is in the range of 50 to 80 ° C. and the temperature in the absorber is in the range of 40 to 60 ° C. Thing extraction method.