JPS6161790B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention extracts leaf tobacco using carbon dioxide in the liquid range at an extraction temperature of -5 to 15°C, preferably 0 to 5°C, thereby containing no or almost no ethanol-insoluble matter and having a large effect of enhancing flavor and aroma. The present invention relates to a method for producing tobacco extract. It is an undeniable fact that the characteristics of recent cigarette products are that they tend to be low in nicotine and low in tar, and as a result, the tobacco-like flavor is becoming weaker. On the other hand, the flavor quality of raw tobacco leaf has been deteriorating due to changes in soil quality and cultivation methods.
Furthermore, with the use of recycled tobacco and the introduction of synthetic tobacco, it has become difficult to produce products with excellent aroma and taste using traditional processing methods in the cigarette manufacturing process. Therefore, when manufacturing tobacco products using these raw materials, there is an urgent need for technology to enhance the tobacco-like aroma and taste and suppress the bad habits of the raw materials. One of the effective means for solving this problem is a method of flavoring low-quality tobacco raw materials by adding tobacco extract, which has a large flavor-enhancing effect. The method of adding and flavoring this tobacco extract to tobacco raw materials during the tobacco manufacturing process is generally the same as the method of adding flavoring materials for tobacco. That is, in the case of a water-insoluble flavoring agent, it is diluted with ethanol, and the ethanol solution is atomized and uniformly added to tobacco raw materials using a spray nozzle or the like. Therefore, if solids such as ethanol-insoluble substances are mixed into this additive solution, the spray nozzle for flavoring will not only become clogged and cause trouble in the process, but also cause problems when using the ethanol solution. Undissolved substances float or settle in a given additive solution, making the concentration and composition of the additive solution non-uniform, and when these are added to add flavor, this can lead to the production of defective products. The purpose of the present invention is to have a large aroma and taste enhancing effect,
To produce a tobacco extract that is free of solid matter, homogeneous, and has good workability by a simple method. That is, the present invention extracts leaf tobacco using carbon dioxide in the liquid range at an extraction temperature of -5 to 15°C, thereby producing flavorful tobacco that does not contain any or almost no ethanol-insoluble materials such as resin and wax in leaf tobacco. This is a method for producing tobacco extract with a large enhancing effect. The technology to obtain tobacco extract by extracting various types of leaf tobacco with carbon dioxide has been known for a long time, and the method of extracting tobacco waste with carbon dioxide in the liquid range (LUGANSKAJA, LN et al., Tabak 1 , 30;
1967, SSSR) has been reported. However, in this method, the extraction operation is performed at an extraction temperature of 20 to 30°C, and according to the tests conducted by the present inventors, in this temperature range, the amount of ethanol-insoluble substances extracted increases, and the obtained tobacco extract becomes This was also a region where the aroma and taste enhancing effect was also small. In addition, a patent (unexamined patent application) for separating and removing resins, wax, and other ethanol-insoluble substances and nicotine by mixing the extract obtained by primary extraction of leaf tobacco with an organic solvent etc. with an adsorbent and performing secondary extraction with carbon dioxide. 1982-107165) has been filed. However, this method involves mixing the ethanol-insoluble substances such as resin and wax in the extract with an adsorbent for secondary extraction, and then over-separating the secondary extract in a step. Although it is separated and removed, it requires many steps, which makes the operation complicated, and also requires a two-step concentration process in the primary and secondary extraction, so the aroma and flavor components with low boiling points disappear by volatilization. there is a possibility. This tendency is considered to be particularly pronounced when an organic solvent is used for the primary extraction. According to the present invention, using carbon dioxide in the liquid range (hereinafter referred to as liquid carbon dioxide), leaf tobacco is grown from -5 to 15
By performing the extraction operation at an extraction temperature of .degree. C., a homogeneous tobacco extract containing no or almost no ethanol-insoluble materials such as resin and wax can be obtained. Moreover, the extraction operation only needs to be carried out once, and there is no need for addition of an adsorbent or additional steps, so the number of manufacturing steps is reduced and the operation is simplified. Furthermore, since the concentration process only needs to be carried out once, there is less volatilization and loss of flavor components with low boiling points, and this combined with the good recovery of low boiling point components, which is a feature of the carbon dioxide extraction method, results in a high quality product that has a large effect of enhancing aroma and flavor. You can obtain tobacco extract. Further, according to the present invention, it is possible to lower the extraction rate of nicotine from leaf tobacco, and therefore, it is possible to obtain a tobacco extract with a low nicotine content, which can be said to be one of the characteristics of the present production method. Next, the method for producing tobacco extract according to the present invention will be explained in detail according to the flow of the extraction device. FIG. 1 shows an example of an extraction device for carrying out the method of the present invention. First, leaf tobacco is shredded, coarsely crushed, or crushed by a commonly used method and placed in the extractor 1, which is a high-pressure container, and extracted with liquid carbon dioxide at an extraction temperature of -5 to 15°C. To obtain a tobacco extract, that is, a tobacco extract that does not contain any insoluble substances and has a large aroma and taste enhancing effect. As for the types of leaf tobacco used as the extraction raw material, one or more types of blended or manufactured tobacco such as yellow variety, burley variety, Japanese native variety, orient leaf, or fermented leaf are used. Leaf tobacco containing these varieties or having a unique aroma and taste due to fermentation treatment, etc., is shredded, coarsely crushed, or crushed into pieces of about 0.5 to 3 mm in width or 0.2 to 3 mm in diameter using a shredder, coarse crusher, or crusher. The leaf tobacco used as the raw material for this extraction is preferably of good quality with excellent aroma and taste even when smoked as is, and has a moisture content of 5 to 18% (based on dry matter), especially 10 to 14%.
It is more preferable to use it as % (based on dry matter). In the extraction operation, the raw tobacco leaves are put into the extractor 1, the system is sealed, and then liquid carbon dioxide is injected from the storage tank 5 using the pump 6 to maintain the temperature at -5 to 15°C.
Extraction is carried out at a temperature range of The extraction method may be either a batch method or a once-through method. In the case of batch method,
Liquid carbon dioxide, which is an extraction agent, is filled into the extractor 1 containing leaf tobacco, which is an extraction raw material, at a predetermined extraction ratio, and a batch extraction operation is performed at a predetermined extraction temperature. The extract is transferred from extractor 1 to separator 2. In the separator 2, the extract is separated into extract and carbon dioxide. That is, separator 2
The carbon dioxide vaporized therein exits from the separator 2 and is compressed by the compressor 3, further cooled by the heat exchanger 4, liquefied again, and recovered in the storage tank 5. Therefore, only the leaf tobacco extract remains in the separator 2, and it is taken out from the bottom of the separator 2 as appropriate. Furthermore, since the extract obtained by the method of the present invention dissolves well in ethanol, it is possible to dissolve the extract in ethanol and take it out from the bottom of the separator 2 in addition to cleaning the extract that has adhered to the inner wall of the separator 2 after the extraction operation is completed. I don't mind. The extracting agent ratio, that is, the injection ratio of liquid carbon dioxide, which is an extracting agent, to leaf tobacco, which is an extraction raw material, is preferably 3 to 60, particularly 15 to 35, in terms of weight ratio. The pressure inside the extractor 1 during extraction indicates the value of the pressure on the saturated liquid line at each extraction temperature. For example, at an extraction temperature of -5 to 15°C, the pressure inside the extractor 1 is 30 to 51 kg/cm ² , respectively. Lowering the extraction temperature in this way also lowers the extraction pressure, which is generally advantageous in terms of production costs and operation of the extraction device.
The extraction temperature is in the negative range, and if it is too low, it will be disadvantageous in terms of operating costs. The extraction temperature is adjusted by circulating constant-temperature water or brine through a jacket attached to the extractor 1, but the liquid carbon dioxide to be injected into the extractor 1 is made to reach near the extraction temperature in advance using the heat exchanger 8. and more effective. The extraction time varies depending on the form of the extraction raw material, but it takes 15 minutes to 8 hours after filling the extractor 1 with liquid carbon dioxide.
In particular, it is more preferable to complete the extraction operation in 1 to 4 hours. When the extraction is completed, the extract is retained in the extractor 1 and only the extract is transferred to the separator 2. In this case, the temperature of the separator 2 should be the same as or lower than the extraction temperature to improve transfer efficiency. It is preferable from this point of view. When using the once-through method for extraction,
Liquid carbon dioxide is passed by a pump 6 from a storage tank 5 into an extractor 1 containing leaf tobacco, which is an extraction raw material, and is preheated by a heat exchanger 8 before entering the extractor 1. The amount of liquid passed is 0.5 to 60 kg/hour, especially 10 to 30 kg of liquid carbon dioxide per 1 kg of leaf tobacco.
Preferably it is carried out in Kg/hour. When liquid carbon dioxide flows through the extractor 1, the average residence time is 0.5
It is preferable to carry out the reaction for 8 hours, particularly 1 to 4 hours. Extraction pressure is 27-100Kg/ ^cm2 , especially 30-60Kg/cm2.
It is preferable to work in cm ² . Liquid carbon dioxide in which an extract containing flavor components of leaf tobacco is dissolved in the extractor 1, that is, an extract liquid, is continuously transferred from the extractor 1 to the separator 2. In the separator 2, liquid carbon dioxide is vaporized and separated from leaf tobacco extract. The gaseous carbon dioxide discharged from the separator 2 is liquefied again in the heat exchanger 4 and collected in the storage tank 5, and is again sent to the extractor 1 by the pump 6 and recycled as an extractant. The temperature of the separator 2 in this case is the storage tank 5
By operating with a temperature difference of 2° C. or more higher than the internal temperature, carbon dioxide can be vaporized in the separator 2 and liquefied in the heat exchanger 4 in sequence. The leaf tobacco extract remaining in the separator 2 is taken out of the system by opening and closing a valve in the lower piping of the separator 2. The present invention will be explained below by way of examples. Example 1 200g of American Burley leaf tobacco (moisture content 11.3
% vs. dry matter) was cut into 0.8 mm width using a rotary cutting machine.
It was placed in extractor 1, 6.0 kg of liquid carbon dioxide was injected, and extraction was performed for 1.5 hours at an extraction temperature of 2°C. At this time, the pressure inside the extractor 1 was 37 Kg/cm ² . After the extraction time had elapsed, the extract was transferred to separator 2 maintained at 0°C. Carbon dioxide was vaporized and separated and removed from the extract in the separator 2 to obtain 2.0 g of leaf tobacco extract. 99% ethanol to this extract
After adding 50 ml, most of the extract was dissolved. Regarding this ethanol solution, the amount of ethanol insoluble matter was measured by passing it through a glass filter [Note 1]. As a result, the amount of ethanol insoluble matter was 0.02 g, and the proportion to the extract, that is, the content of ethanol insoluble matter was only 1%. This extract was sprayed at 5 ppm into chopped pieces of domestic Burley variety, which has a light flavor and a unique taste, and was then rolled up into cigarettes using a conventional method.
As a result of tasting the product by a specially trained expert panel of people by comparing it with a control product without additives, all 10 people found that the flavor typical of Burley increased compared to the control product.
It was determined that the bitterness of the raw materials was suppressed, and it became clear that the effect of improving the aroma and flavor was significant. Example 2 American yellow seed leaf tobacco (moisture content 11.6% vs. dry matter)
60 g and 40 g of Orient leaf tobacco (moisture content: 12.5% dry matter) were ground into an average particle size of 0.06 mm using a ball mill and placed in extractor 1. followed by liquid carbon dioxide 3.0
Kg was injected and extraction was carried out for 2 hours at an extraction temperature of 0°C. At this time, the pressure inside extractor 1 is 35Kg/cm ²
It was hot. After the extraction time had elapsed, the extract was transferred to separator 2 maintained at 0°C. Carbon dioxide was removed from separator 2 to obtain 0.8 g of extract. As a result of adding 30 ml of 99% ethanol to this extract, the extract was completely dissolved in ethanol and no undissolved matter was observed. Example 3 100g of American yellow leaf tobacco (moisture content
10.6% vs. dry matter) screen milled to an average particle size of 0.7
coarsely crushed to mm and put into extractor 1, then pump 6
Then, 5.0 kg of liquid carbon dioxide was injected and a batch extraction operation was performed for 3 hours at an extraction temperature of 2°C. After the extraction time has elapsed, the extract is transferred to separator 2 at 0°C to vaporize and remove carbon dioxide, and 30 ml of 99% ethanol is added to the extract remaining in separator 2 to form an ethanol solution. Recovered. On the other hand, after putting 100g of the same coarsely crushed leaf tobacco into the extractor, liquid carbon dioxide was passed through the extractor at a flow rate of 1.5Kg/hour using the pump 6, and the temperature was raised to 40℃ using the heat exchanger 8 to reach a supercritical state. A flow-through extraction operation was performed for 3 hours at an extraction pressure of 250 kg/cm ² . After the extraction time had elapsed, carbon dioxide in the separator 2 was separated and removed, and the remaining extract was recovered as an ethanol solution by adding 60 ml of 99% ethanol. As shown in Table 1, the extract using liquid carbon dioxide at an extraction temperature of 2°C was very well soluble in ethanol and did not contain any ethanol-insoluble matter. Furthermore, the extraction rate of nicotine from the extraction raw material was much lower when extracted at 2°C than when extracted at 40°C, and therefore the nicotine content in the extract was lowered. Next, each extract was added by spraying at 5 ppm to chopped domestic yellow seeds, which have a light flavor and a unique taste, and then rolled up into cigarettes using a conventional method.
A specially trained expert panel of 10 people tested the product using a method [Note 2] that compared the aroma and taste with a control product without additives. Table 1 shows the average value of the aroma and taste evaluation scores in this tasting, and it was recognized that the effect of enhancing the aroma and taste of the extract by liquid carbon dioxide at 2°C was very large.

[Table] Example 4 200g of American yellow medium leaf tobacco (moisture content
12.1% dry matter) was shredded into 0.8 mm width with a rotary shredder and placed in the extractor 1, and liquid carbon dioxide was passed through it at a flow rate of 3.2 kg/hour using the pump 6, and the extraction temperature was 1°C. A once-through extraction operation was performed for 2 hours at an extraction pressure of 40 kg/cm ² . After the extraction time had elapsed, carbon dioxide in the separator 2 was separated and removed to obtain 2.0 g of extract. When 50 ml of 99% ethanol was added to this extract, most of the extract was dissolved. The ethanol insoluble matter content of this ethanol solution was determined according to Example 1 and was found to be 1%. The nicotine content of the extract was 3%. Next, this extract was sprayed at 5 ppm on minced domestically produced medium-leaved yellow seeds that have a light flavor and a unique taste, and the aroma and taste were evaluated in accordance with Example 1. Compared to the control product, it was judged that the flavor characteristic of yellow varieties was increased and the characteristic bitterness was suppressed, and it was found that the effect of improving the aroma and taste was large. Example 5 200g of American yellow true leaf tobacco (moisture content
11.6% dry matter) was shredded into 0.8 mm width using a cutting machine, placed in extractor 1, and 6.0 kg of liquid carbon dioxide was injected to adjust the extraction temperature to -5, 2, 15 and 15, respectively.
A batch extraction operation was performed at 30°C for 4 hours. Thereafter, extracts at each extraction temperature were obtained in the same manner as in Example 1 (Table 2). 50 ml of 99% ethanol was added to each extract, and the insoluble matter was measured, and the ethanol insoluble matter content is shown in Table 2.
Ethanol-insoluble matter is extracted at extraction temperatures of -5 and 2.
At 30°C, it was not present at all, but as the extraction temperature rose, it increased to 7% at 30°C. Furthermore, the lower the extraction temperature, the lower the nicotine content in the extract (Table 2). Next, each extract was added by spraying at 5 ppm to chopped domestic yellow seeds, and the aroma and taste were evaluated in the same manner as in Example 3.
As shown in Table 2, the average aroma and flavor evaluation score for extracts produced at an extraction temperature of 15°C or lower is 2 or more, which clearly shows that the effect of enhancing flavor and aroma is much greater than that for extracts produced at 30°C. Summer.

[Table] Example 6 220 g of minced product brand "Peace" was placed in extractor 1, 2.2 kg of liquid carbon dioxide was injected, and a batch extraction operation was performed for 1.5 hours at an extraction temperature of 15°C. Transfer the extract to separator 2 maintained at 10°C,
Carbon dioxide was separated and removed to obtain 1.0 g of extract.
30 ml of 99% ethanol was added to this extract, and the content of ethanol insoluble matter was determined in the same manner as in Example 1, and was found to be 2.4%. This extract was further diluted with ethanol to make an ethanol solution with a concentration of 0.1%, and placed in a commercially available portable atomizer. 1 cigarette of "Peace", a product whose flavor has faded more than a year after manufacture. One puff was added to the book by spraying. This spray-added cigarette was tasted by a specially trained panel of 10 people, comparing it to a non-additive product. All 10 people found that the cigarette had an increased peace-like aroma compared to the control product, and was well-balanced as a peace-like product. It was evaluated that the flavor became more aromatic, and it became clear that the aroma and flavor had improved. The measurement and evaluation methods for each note shown in the text of Examples 1 and 3 and Tables 1 and 2 are as follows. [Note-1] Method for measuring ethanol insoluble substances Add 99% ethanol so that the sample concentration falls within the range of 3 to 5%, and let stand at 20°C for at least 20 hours. Subsequently, the sample solution was passed through a 1G4 glass filter, and the solid matter separated on the glass filter was dried under reduced pressure in a desiccator for 2 hours to determine the dry weight, and it was considered as an ethanol-insoluble matter. [Note-2] Evaluation of aroma and taste: 2-point comparison method The 2-point comparison method means 0 points if there is no difference compared to the control, 1 point if there is a slight difference, and 3 points if there is a significant difference. In this method, the flavor is scored as (+) if the flavor is good and (-) if it is bad compared to the control. (Seiji Yoshikawa, Food Quality Measuring Method, 44
Page, Korin Shoin, published in 1963)

[Brief explanation of the drawing]

FIG. 1 shows an example of a layout of an apparatus for carrying out the method of the present invention. 1: extractor, 2: separator, 3: compressor, 4: heat exchanger, 5: storage tank, 6: pump, 7: flow meter, 8: heat exchanger.

Claims (1)

[Scope of Claims] 1. In a method for obtaining tobacco extract by extracting leaf tobacco with carbon dioxide, leaf tobacco is extracted using carbon dioxide in the liquid range at an extraction temperature of -5 to 15°C, thereby making it insoluble in ethanol. A method for producing a tobacco extract, which is characterized by producing a tobacco extract that contains no or almost no substances and has a large aroma and taste enhancing effect. 2. One or two types of leaf tobacco, such as yellow variety, burley variety, Japanese native variety, orient leaf, or fermented leaf, as the starting material for extraction.
The method according to claim 1, which uses more than one type of blended product and manufactured tobacco.