JP3264515B2 - Method and apparatus for extracting soluble matter from natural solid raw material - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION This invention, in a supercritical state dioxide
The present invention relates to a soluble matter extraction method and a soluble matter extraction apparatus for extracting a soluble matter from a tobacco raw material using carbon .

[0002]

2. Description of the Related Art Conventionally, as a method for removing soluble substances such as nicotine and caffeine from natural solid raw materials such as tobacco, tea and coffee, an inert extractant in a supercritical state is passed through the raw materials to remove the soluble substances. There is known a method of extracting a soluble substance by dissolving it in an extractant. As an inert extractant,
For example, when carbon dioxide is pressurized, the density increases and the liquid or supercritical (31.1 ° C. or higher, 75.3 kg / cm
2 or more) state, and the ability to dissolve the substance is improved.
And such supercritical carbon dioxide (CO2)
Is contacted with, for example, a tobacco raw material, whereby nicotine in the raw material is dissolved in CO2. Thereafter, the CO2 containing nicotine expands under reduced pressure or heating to reduce its density and its dissolving power, thereby precipitating nicotine.

On the other hand, it is known that a soluble substance can be efficiently extracted from a raw material by using water in combination with an inert extractant. For this reason, conventionally, for example, when nicotine is extracted from tobacco, a method of humidifying the tobacco raw material or performing extraction using CO2 containing water, or a method of using both together is adopted. . As an example, Japanese Patent Publication No. 51-9838 discloses a method of adding water to CO2 by flowing CO2 through a water tank in which water is stored.

[0004]

However, when humidifying the raw material, equipment for performing the humidification step is required, so that the entire extraction equipment becomes large and the processing time becomes long. Further, the raw material whose moisture has been increased to, for example, about 20% by humidification tends to be deteriorated, and the storage place and the storage period are limited. Further, the raw material containing a large amount of water is easily fixed when filled in the extractor, and when the raw material contains a large amount of water, the flow of the extractant is caused to cause a non-uniform removal of the soluble matter of the raw material after the treatment. Become.

When water is added to an extractant by passing water in a water tank, it is necessary to use a pressure-resistant container capable of withstanding a pressure equivalent to the processing pressure of the raw material as the water tank, which makes the processing apparatus expensive and The capacity of the container is also large. In addition, in the case of this method, the amount of water added to the extractant cannot be adjusted, and the extractant contains water in a state close to saturation. For this reason, the raw material after the treatment contains a large amount of water, which makes it difficult to handle and requires a post-treatment step such as drying. Further, some of the inert extractants are difficult to dissolve in water such as chlorofluorocarbons and nitrous oxide, and the conventional method has a problem that sufficient water cannot be added to such an extractant. .

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a method for extracting a soluble substance, which does not require humidifying or drying the tobacco raw material, and which can efficiently extract a desired amount of soluble substance from the raw material. It is an object of the present invention to provide a solute extractor.

[0007]

To achieve the above object, according to an aspect of, according to the extraction method of the present invention, the supercritical dioxide
Supplying water to the carbon, with the addition of water to carbon dioxide and mixed by the supplied water and carbon dioxide and a line mixer, by adjusting the amount of water supplied to carbon dioxide water content of carbon dioxide to carbon dioxide Is adjusted to 50 to 70% of the saturated dissolution amount of water .

[0008] The extraction device of the present invention, an extraction vessel containing the tobacco material, and flow means for flowing the supercritical carbon dioxide through the extraction vessel, is provided on the inflow side of the extraction vessel, the carbon dioxide Water supply means for supplying water to the extraction vessel, a line mixer provided on the inflow side of the extraction vessel for mixing the supplied water and carbon dioxide, and the diacid
The water content of the carbon dioxide by adjusting the water supply to
Adjusting means for adjusting the saturated solubility of water in carbon dioxide to 50 to 70% . The line mixer is a means for mixing water and carbon dioxide in a pipe, and various types having a baffle, a mechanical stirrer, and the like are known, and a static mixer is particularly preferable.

[0009]

According to the extraction method of the present invention, the water content of carbon dioxide is considered in consideration of the state of the tobacco raw material to be treated or the water content or moisture value of the processed raw material, the nicotine content, and the like. Can be adjusted freely. Thereby,
A pre-processing step such as humidification or a post-processing step such as drying can be omitted, and prompt processing can be performed. In addition, water can be easily added to an inert extractant in which water is difficult to dissolve and mix, and the range of extractants that can be used can be expanded.

Further, according to the extraction apparatus of the present invention, the water content of carbon dioxide can be adjusted by the adjusting means, so that the soluble matter can be efficiently extracted from the raw material, and the desired moisture value and the soluble matter can be obtained. A tobacco raw material having a content can be provided. In addition, there is no need to provide a humidifying device, a drying device, and the like, and the size and cost of the device can be reduced.

[0011]

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

First, an embodiment in which the present invention is applied to a nicotine extraction apparatus for extracting nicotine from tobacco raw materials will be described.

As shown in FIG. 1, the extraction apparatus includes an extraction container 10 containing a tobacco cut as a raw material. The extraction container passes carbon dioxide (CO 2) as an inert extractant through the extraction container. It is connected in a closing circuit 12 for flowing. The closing circuit 12 includes a storage tank 14,
A predetermined amount of CO2 is supplied to this storage tank from a supply source (not shown) via a valve 15 and a first heat exchanger 17. The CO2 is cooled by the first heat exchanger 17 and stored in the storage tank 14 in a liquefied state. The storage tank 14 is connected to a suction port of a first pump 20 via a flow meter 16 and a second heat exchanger 18.
The first pump 20 is constituted by a variable displacement type liquid pump, and its discharge port is connected to the lower end of the extraction container 10 via a third heat exchanger 22 and a static mixer 24 as a line mixer. .

The upper end of the extraction vessel 10 is connected to a separator 28 via a first pressure regulating valve 26 and a fourth heat exchanger 27, and the separator is further connected to a second pressure regulating valve 30, It is connected to the storage tank 14 via a gas purifier 32 and a fifth heat exchanger 34. The above-mentioned elements constituting the closing circuit 12 are connected by a circulation pipe 36 and constitute a circulation means in the present invention.

As shown in FIG. 2, the static mixer 2
4 is a main body pipe 38 having substantially the same diameter as the distribution pipe 36,
A stirring blade 40 is provided in the main pipe along the axial direction thereof. Each end of the main body pipe 38 has a flange 38a, and is connected to the flow pipe 36 by the flange. Thereby, the body pipe 38
Constitutes a part of the distribution pipe 36 through which CO2 flows.

The stirring blades 40 are formed by twisting a rectangular plate 180 degrees in the opposite direction to the first element, similarly to the three first elements 40a formed by twisting a rectangular plate 180 degrees. Three second elements 40b, the first elements and the second elements are arranged alternately, and are mutually 90 degrees apart.
They are connected at an angle of degrees.

A second pump 44 is connected to an upstream end of the main body pipe 38 via a water supply pipe 42. The second pump 44 comprises a variable displacement fluid pump,
The amount of water supplied to the static mixer 24, that is, the amount of water added, can be freely adjusted. And the second pump 4
Reference numeral 4 designates a supply means for supplying water to CO2 and an adjusting means for adjusting the amount of supplied water.

A method for extracting nicotine from tobacco raw materials using the nicotine extraction apparatus configured as described above will be described.

First, after a predetermined amount of CO2 is supplied to the storage tank 14, the valve 15 is closed, and then the first pump 20 is operated. Then, CO2 is stored in storage tank 14
Flows into the second heat exchanger 18 through the flow meter 16 from the
Here, it is cooled again and completely liquefied. And CO
2 is compressed to a predetermined pressure by the first pump 20 and then flows into the third heat exchanger 22 where it is heated to about 70 ° C. to be in a supercritical state (31.1 ° C. or higher, 75.3 kg / cm2
Above). The supercritical CO2 flows into the static mixer 24. At the same time, water adjusted to a desired amount by the second pump 44 is supplied to the static mixer 24. Thus, CO2 and water flow together through the static mixer 24, with the stirring blades 4
The first element 40a of 0 is turned clockwise, for example, and the second element 40b is turned counterclockwise.
The water flows in the static mixer 24 while being repeatedly inverted with the CO2, and is mixed and dissolved in the CO2, and CO2 having a desired water content is discharged from the static mixer. The water content of CO2 can be set to a desired value by adjusting the amount of water supplied to the static mixer 24 by the second pump 44. The preferred moisture content is 50-70%, most preferably 60%, of the saturated solubility of water in CO2 at each extraction temperature and pressure. For example, when the extraction temperature in the extraction vessel is 60 ° C. and the extraction pressure is 300 kg / cm 2,
The addition amount of water is preferably 1.9 to 2.7 / kg-CO2.

The extraction temperature in the extraction container is preferably 50 to 80 ° C., and the extraction pressure is 150 to 300 kg.
/ Cm2.

Subsequently, supercritical CO2 containing water is used.
Flows into the extraction container 10 and flows through the tobacco cuts in the extraction container. At that time, the nicotine in the tobacco cut is dissolved in CO2 and extracted from the tobacco cut. The nicotine-containing CO2 passes through the first pressure regulating valve 26 from the extraction container 10 and is reduced in pressure here. By reducing the pressure, the dissolving power of CO2 is reduced, and nicotine is precipitated from CO2. Then, CO2 is passed through a fourth heat exchanger 27 to a separator 28.
And is heated in these heat exchangers and separators to be vaporized and separated from water and nicotine. The precipitated nicotine and water as the extracted substance are stored in the separator 28 and discharged to the outside of the extraction device via the valve 46 after the completion of the extraction process or during the extraction process.

The CO 2 from which nicotine has been separated is further decompressed by the second pressure regulating valve 30 and then subjected to a gas purifier 32.
, Where water and volatile components remaining in the CO2 are removed and purified. The purifier 32 is filled with a filler such as molecular sieve, activated alumina, silica gel, and magnesium sulfate. Purified C
O2 is cooled and liquefied in the fifth heat exchanger 34 and then returned to the storage tank 14.

By repeating the above steps for a predetermined time, nicotine is extracted from the tobacco cut in the extraction container 10, and a tobacco cut having a desired nicotine content is generated.

The inventor of the present application used three kinds of addition methods in order to examine the relationship between the method of adding water to CO2 and the nicotine removal rate and the quality characteristics of the raw material after the treatment, and used nicotine under the same conditions as the other conditions. An extraction test was performed.

In Test 1, 300 g of a tobacco cut (blend product, nicotine content 2.2% by dry weight) cut into a product was used as a raw material by using the nicotine extraction apparatus and the extraction method according to the present embodiment described above. It was stored in an extraction container having a volume of 4 liters. The moisture value of the tobacco pieces stored in the extraction container is 12.3% by weight, which is in a moisture range suitable for handling. Through this extraction container, nicotine was extracted by flowing CO2 at an extraction temperature of 70 DEG C., an extraction pressure of 300 kg / cm @ 2, and a flow rate of 320 g / min for 2.5 hours. that time,
2.86 g / kg- at the upstream end of the static mixer
Water was supplied at the ratio of CO2, mixed and dissolved in CO2, and supplied to the extraction vessel.

In Test 2, the raw material was cut into tobacco pieces (moisture value 1
2.3% by weight) and 22.7% by weight in advance by a spray method.
The extract was placed in a polypropylene bag, allowed to stand overnight, and then stored in an extraction container, through which water-free CO2 was passed.

In Test 3, a water tank (inner diameter 10 cm, height 50 c) was installed on the upstream side of the extraction container containing the tobacco cuts.
m), store water at a height of 10 cm, and set a temperature of 70 cm from the bottom of the water tank.
A predetermined amount of CO2 at a temperature of 300 DEG C. and a pressure of 300 kg / cm @ 2 was flowed to dissolve the water, and then supplied to the extraction vessel.

Table 1 below shows the nicotine removal rate and the tobacco cut water value after the treatment in each test.
As can be seen from Table 1, in the case of Test 2 in which the raw materials are pre-humidified, the nicotine removal rate is considerably lower than in the other two methods. In addition, the water value of the tobacco cut after the treatment was 3.8.
% By weight, and many cigarette crushes occurred upon removal from the extraction container. In the case of Test 3 in which CO2 was added through a water tank, the nicotine removal rate was as excellent as 99%, but the tobacco chopped after treatment had a very high moisture value of 23.3% by weight, which caused problems in handling and quality. is there.

On the other hand, in Test 1 in which water was added to CO 2 using a static mixer, the nicotine removal rate was almost the same as in Test 3, and the water value of the tobacco cut after treatment was 14.7% by weight. %, And acceptable values in terms of handling and quality were obtained.

Table 1 Test Cut to raw material cut to CO2 Cut after processing Nicotine Summary NO. How to add moisture value (%) Moisture value (%) Removal rate (%) 12.3 Stat mixer 14.7 97 2. 22.7 None 3.8 75 Humidification of raw materials 3. 12.3 Aquarium 23.3 99

Table 2 Minced after water treatment to CO2 Nicotine Summary Water content * Water content Water content Removal rate (g / kg-CO2) (%) (Weight%) (%) 1.90 40 8.6 82 * Water to CO2 2.38 50 11.0 91 Ratio of water to solubility 2.86 60 14.4 97 Amount 3.33 70 18.1 98 3.81 80 23.2 99 As can be seen from Table 2 above, as the amount of water and the ratio of water increase, the nicotine removal rate increases. The moisture value of the step after treatment also increases. Generally, the moisture value of the tobacco cut is about 12% in which there is no problem in terms of handleability and quality of the cut. From Table 2, the water content is 50 to 6
When it was set to 0%, it was found that a treated product having a moisture value after the treatment in the above range could be obtained. When the water content was 50% or more, the nicotine removal rate was 90% or more.

When the proportion of water was fixed at 60% and the relationship between the extraction temperature and the water content of the tobacco cut after the treatment and the nicotine removal rate were examined, the results shown in FIG. 3 were obtained. In this case, the other test conditions were the same as in Test 1 described above. As can be seen from FIG. 3, the moisture value of the tobacco cut was about 12% at any of the extraction temperatures, and at an extraction temperature of 70 ° C. or more, the nicotine removal rate was 95% or more.

Further, in order to investigate the occurrence of CO2 drift in the extraction vessel due to the water content of the tobacco cut before the treatment, as shown in FIG. 4, tobacco cuts having different moisture values (nicotine content 2 15 kg in a cylindrical extraction container (inner diameter 35 cm, height 170 cm), CO2 was extracted through the extraction container at an extraction temperature of 70 ° C., an extraction pressure of 250 kg / cm 2 and a flow rate of 250 g / min at 6.5.
The nicotine was extracted by flowing over time. Tobacco chopping
The extraction container was filled by hand so as to be contained as uniformly as possible, and a wire netting 48 was inserted every 5 kg, and the extraction was performed by dividing the container into three blocks 50a, 50b, and 50c from the CO2 inflow side. Then, the tobacco cut after processing was collected from the five regions A, B, C, D, and E in each block, and the nicotine content was examined. The test results are shown in Table 3 below.

Table 3 Test 1 Raw material moisture content Nicotine content at the processing step NO. (% By weight) ABCDE Average value Coefficient of variation (%) 19.8 0.16 0.25 0.45 0.40 0.51 0.35 36.6 2. 12.5 0.22 0.25 0.20 0.20 0.25 0.22 10.0 As can be seen from Table 3, test 1 in which the above-mentioned extraction treatment was performed on tobacco cuts having a high moisture value (19.8% by weight)
In the case of, the nicotine content of the cut tobacco cut from the areas A to E is lower than that of the test 2 in which the above-mentioned extraction treatment was performed on the cut tobacco having a low moisture value (12.5% by weight). Have large variations, and the average value of these nicotine contents is also high. From this fact, it is inferred that when the water content of the tobacco cut of the raw material is high, CO2 drift is likely to occur in the extraction vessel. Therefore, it was confirmed that humidifying the tobacco raw material before the treatment was not preferable for uniformly removing nicotine.

According to the nicotine extraction apparatus and the extraction method configured as described above, by adjusting the amount of water supplied to the static mixer 24, the C sent to the tobacco unit is adjusted.
The water content of O2 can be adjusted to a desired value which is equal to or lower than the saturated state, and can be set to a supersaturated state if necessary. Therefore, by adjusting the water content of CO2 so that the water content (moisture value) of the tobacco raw material after the treatment becomes a desired value, the treated product can be prevented from being excessively humidified, and the drying process after the treatment can be prevented. Can be omitted. Therefore,
Operation costs and equipment costs can be reduced. Further, since the tobacco raw material after the treatment can be set to the optimum moisture content, the handleability and quality of the treated product are greatly improved.

Further, nicotine can be efficiently extracted without humidifying the tobacco raw material before the treatment, the pretreatment step can be omitted, and the C content in the extraction container can be reduced.
Nicotine can be uniformly extracted over the entire tobacco raw material, which can prevent O2 drift. Further, even if the nicotine content of the tobacco raw material before the treatment differs depending on the type, a desired nicotine removal rate can be obtained by adjusting the water content of CO2.

Further, since the water supplied from the pump is mixed with the inert extractant by the static mixer and added to the inert extractant, the water is not limited to carbon dioxide, but is not limited to carbon dioxide. Water can be easily added to the active extractant. Therefore, various inert extractants can be used, and desired soluble substances can be extracted from various natural solid raw materials.

The present invention is not limited to the above-described embodiment, but can be variously modified within the scope of the present invention.

For example, in the above-described embodiment, the amount of water supplied to CO2 is adjusted using a variable displacement pump. However, the present invention is not limited to this. As shown in FIG. It may be used, and the supply amount may be adjusted by a flow control valve 52 as flow adjustment means provided between the pump and the static mixer. In addition, the present invention is not limited to extracting nicotine from tobacco raw materials,
It is needless to say that the present invention can be applied to the case where other soluble substances such as caffeine are extracted from other natural solid raw materials, for example, black tea, green tea, coffee and the like. Further, as the inert extractant, another extractant such as Freon, nitrous oxide, or lower halogen hydrocarbon having a low critical temperature may be used.

[0040]

As described above, according to the present invention, the carbon dioxide
Since the water content of carbon is adjusted to a desired value and supplied to the tobacco raw material, it is not necessary to perform a treatment such as humidification or drying of the raw material, and it is possible to efficiently extract a desired amount of nicotine. A method for extracting a solute and an apparatus for extracting a solute can be provided.

[Brief description of the drawings]

FIG. 1 is a diagram schematically showing a nicotine extraction device according to one embodiment of the present invention.

FIG. 2 is an enlarged sectional view showing a static mixer of the nicotine extraction device.

FIG. 3 is a characteristic diagram showing a relationship between an extraction temperature, a nicotine removal rate, and a water value of a tobacco cut after treatment.

FIG. 4 is a schematic diagram showing an extraction container used for a drift generation test.

FIG. 5 is a sectional view corresponding to FIG. 2, showing a modification of the water supply unit.

[Explanation of symbols]

10 extraction container, 12 closing circuit, 14 storage tank,
17, 18, 22, 27, 34: heat exchanger; 24: static mixer; 44: second pump.

Continued on the front page (72) Inventor Jin Shigematsu 4-12-62 Higashi Shinagawa, Shinagawa-ku, Tokyo Japan Tobacco Inc. (72) Inventor Nobuo Okabayashi 1-77, Kurobeoka, Hiratsuka-shi, Kanagawa Japan Tobacco Inside the Hiratsuka Plant of Sangyo Co., Ltd. (72) Makoto Ouchi 1-77, Kurobeoka, Hiratsuka-shi, Kanagawa Prefecture Japan Inside the Hiratsuka Plant of Tobacco Inc. (72) Inventor Heiji Nozoe 1-77, Kurobeoka, Hiratsuka-shi, Kanagawa Japan (56) References JP-A-2-103202 (JP, A) JP-A-63-83198 (JP, A) JP-A-64-67201 (JP, A) JP 4-71603 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) B01D 11/00-11/04

Claims (4)

(57) [Claims] Claims: 1. A supercritical carbon dioxide through tobacco raw material
In solubles extraction method for extracting solubles from tobacco material by passing a carbon, and supplying water to the carbon dioxide, by mixing the supplied water and carbon dioxide in the line mixer, carbon dioxide Adding water to the tobacco , flowing water-added carbon dioxide through the tobacco raw material , and dissolving a soluble substance in the tobacco raw material in the carbon dioxide, and dissolving the soluble substance dissolved from the carbon dioxide. And a step of separating, wherein the adding step adjusts a water supply amount to carbon dioxide .
Determine the water content of carbon dioxide as
A method for extracting a soluble matter, comprising a step of adjusting the concentration to 50 to 70% . 2. The method according to claim 1, wherein the dissolving step is performed at an extraction temperature of 50 to 50.
This performing 80 ° C., with extraction pressure 150~300kg / cm ²
2. The method for extracting a soluble matter according to claim 1, wherein: 3. A solubles extraction apparatus for extracting soluble matter from the tobacco material, and the extraction vessel containing the tobacco material, and flow means for flowing the supercritical carbon dioxide through the extraction vessel, the above extraction vessel A water supply means provided on the inflow side and supplying water to the carbon dioxide; and a water supply means provided on the inflow side of the extraction vessel and provided with the supplied water.
A line mixer for mixing the carbon dioxide, by adjusting the amount of water supplied to the carbon dioxide 50% to 70% of the saturated dissolved amount of the water of the water content of the carbon to carbon dioxide
And an adjusting means for adjusting the temperature of the soluble matter. 4. The system according to claim 1, wherein said distribution means is provided with a water supply port.
The carbon oxide is extracted at an extraction temperature of 50 to 80 ° C and an extraction pressure of 150 to
Means to flow through the extraction vessel at 300 kg / cm ²
4. The extractable substance according to claim 3, wherein the extractable substance is provided.
Output device.