CN111418874A - Coating preparation method of cigar-flavor cigarette paper - Google Patents
Coating preparation method of cigar-flavor cigarette paper Download PDFInfo
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- CN111418874A CN111418874A CN202010390964.7A CN202010390964A CN111418874A CN 111418874 A CN111418874 A CN 111418874A CN 202010390964 A CN202010390964 A CN 202010390964A CN 111418874 A CN111418874 A CN 111418874A
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- tobacco
- coating
- cigarette paper
- flavor
- cigar
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Tobacco Products (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
The invention discloses a coating preparation method of cigar flavor cigarette paper, which comprises the following steps: preparing a tobacco concentrate; subjecting the tobacco concentrate to molecular distillation, and collecting light components to obtain a first tobacco extract; adding the mixture of amino acid and sugar into the tobacco leaf extract, and filtering, diluting, performing membrane separation and concentrating under reduced pressure after the reaction is finished to obtain a second tobacco extract; preparing a tobacco regrind; preparing a cigar flavor tobacco flavor; preparing a cigar flavor coating liquid; coating the cigarette paper for the first time by adopting a roller coating method; and (3) coating the cigarette paper for the second time by adopting a spray coating method to obtain the cigar flavor cigarette paper. The coating preparation method of the cigar flavor cigarette paper can effectively enhance the cigar flavor of cigarettes, can increase the concentration and the thickness of smoke, enables the prepared cigar flavor cigarette paper to show a dyeing effect without adding extra pigment, and is beneficial to optimizing the sensory experience of cigar flavor cigarettes.
Description
Technical Field
The invention relates to the field of cigarette manufacturing, in particular to a coating preparation method of cigar flavor cigarette paper.
Background
The cigar-type cigarette integrates the advantages and characteristics of cigar and flue-cured tobacco, and has the flavor characteristics of rich and rich cigar and pure and comfortable flue-cured tobacco. In actual production, the cigar flavor of cigar-type cigarettes is usually achieved by adopting a mode of flavoring cigarette paper and/or tobacco.
However, the existing cigar flavor cigarette paper has turbid fragrance, and cigar type cigarettes prepared from the cigar flavor cigarette paper have low smoking quality, so that the sensory experience of consumers is seriously influenced.
Therefore, how to provide the cigar flavor cigarette paper which can effectively enhance the cigar flavor and improve the smoking quality becomes a technical problem which needs to be solved urgently in the field.
Disclosure of Invention
The invention aims to provide a novel technical scheme of a coating preparation method of cigar flavor cigarette paper, which can effectively enhance cigar flavor and improve smoking quality.
According to the first aspect of the invention, a coating preparation method of the cigar flavor cigarette paper is provided.
The coating preparation method of the cigar flavor cigarette paper comprises the following steps:
(1) carrying out reduced pressure concentration treatment on the supernatant after the tobacco extract is dissolved to obtain a tobacco concentrate;
(2) subjecting the obtained tobacco concentrate to molecular distillation, and collecting light components to obtain a first tobacco extract;
(3) adding the mixture of amino acid and sugar into the tobacco leaf extract, reacting for a period of time, and filtering, diluting, membrane separating and concentrating under reduced pressure after the reaction is finished to obtain a second tobacco extract;
(4) mixing the first tobacco extract and the second tobacco extract to obtain a tobacco recombinant;
(5) preparing a spice for cigar flavor cigarettes, wherein the spice for cigar flavor cigarettes comprises 1-10 parts of tobacco heavy component, 1-5 parts of cocoa extract, 0.01-0.05 part of sandalwood oil, 0.05-0.1 part of 2-methylvaleric acid and 0.001-0.005 part of isovaleric acid in parts by weight;
(6) diluting the cigar flavor tobacco flavor to the required concentration to obtain cigar flavor coating liquid;
(7) coating the cigarette paper for the first time by adopting a roller coating method, and drying the cigarette paper coated for the first time at a low temperature;
(8) and (3) coating the cigarette paper for the second time by adopting a spray coating method, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper.
Optionally, the step (1) is specifically as follows:
(1-1) carrying out first extraction treatment on tobacco leaves, and then carrying out reduced pressure evaporation treatment on an extract liquor obtained by the first extraction to obtain a tobacco extract;
and (1-2) separating supernatant at low temperature after dissolving the prepared tobacco extract, and carrying out reduced pressure concentration treatment on the supernatant to obtain the tobacco concentrate.
Optionally, the first extraction in the step (1-1) adopts a subcritical extraction method, the extraction condition is that the extraction is carried out for 0.5h-2h at the temperature of 25-50 ℃, and the material-liquid ratio is 1 (8-20).
Optionally, the step (3) is specifically as follows:
(3-1) carrying out second extraction treatment on the tobacco leaves after the first extraction, and carrying out reduced pressure concentration on the extract liquor after the second extraction until the mass percentage content of dry matters is 30-50% to obtain a tobacco leaf extract;
(3-2) adding a mixture with the molar ratio of the amino acid to the sugar being (0.5-1):1 into the tobacco extract according to the mass ratio of the mixture of the amino acid and the sugar to the tobacco extract being (1-3):10, reacting at 80-110 ℃ for 1-3 h, filtering a reaction product after the reaction is finished, diluting the obtained filtrate, filtering the diluted liquid through an ultrafiltration membrane of 10-50kD, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
Optionally, in the step (3-1), a leaching extraction method is adopted for the second extraction, the extraction condition is that the extraction is carried out for 0.5h-3h at the temperature of 60-80 ℃, and the material-liquid ratio is 1 (6-12).
Optionally, the step (2) is specifically as follows:
and carrying out secondary molecular distillation treatment on the obtained tobacco concentrate, wherein the temperature of the primary molecular distillation is 40-80 ℃, the distillation pressure is 0.001-0.01 mbar, the heavy component obtained after the primary molecular distillation is subjected to secondary molecular distillation, the temperature of the secondary molecular distillation is 100-120 ℃, the distillation pressure is 0.001-0.01 mbar, and the light component obtained after the secondary molecular distillation is collected to obtain the first tobacco extract.
Optionally, the step (4) is specifically as follows:
mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1 (10-20) to obtain the tobacco recombinant.
Optionally, the step (6) is specifically as follows:
(6-1) mixing the cigar flavor tobacco flavor and the combustion improver according to the mass ratio of (96-99) to (1-4) to prepare cigar flavor stock solution;
(6-2) mixing the cigar flavor stock solution with an organic solvent to prepare cigar flavor coating liquids with different concentrations.
Optionally, the step (8) is specifically as follows:
and (3) coating the cigarette paper for the second time by adopting a spray coating method, arranging a plurality of spray heads in the running direction of the cigarette paper, wherein the concentrations of the cigar flavor coating liquids in the spray heads are different, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper.
Optionally, the concentration of the cigar flavor coating liquid used in the first coating in the step (7) is the same as the concentration of the lowest cigar flavor coating liquid used in the spraying in the step (8).
The cigar flavor cigarette paper prepared by the coating preparation method of the cigar flavor cigarette paper can effectively enhance the cigar flavor of cigarettes, can increase the concentration and the thickness of smoke, can make the prepared cigar flavor cigarette paper show a dyeing effect without adding extra pigment, and is beneficial to optimizing the sensory experience of cigar flavor cigarettes.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The invention provides a coating preparation method of cigar flavor cigarette paper, which comprises the following steps:
step (1): and (4) carrying out reduced pressure concentration treatment on the supernatant after the tobacco extract is dissolved to obtain the tobacco concentrate. The tobacco extract can be prepared by concentrating the extractive solution of tobacco leaf.
Step (2): subjecting the obtained tobacco concentrate to molecular distillation, and collecting light components to obtain a first tobacco extract. The molecular distillation treatment is beneficial to reducing the content of low-carbon alkane and high-carbon fatty acid in the tobacco concentrate.
And (3): adding the mixture of amino acid and sugar into the tobacco leaf extract, reacting for a period of time, filtering, diluting, performing membrane separation, and concentrating under reduced pressure to obtain a second tobacco extract.
The above-mentioned tobacco leaf extract is generally a product obtained by concentrating an extract obtained by extracting raw materials such as tobacco leaves, tobacco shreds, tobacco stems, or tobacco shreds. The extractant can be water or ethanol, and the concentration of the ethanol can be flexibly selected according to actual requirements, for example, ethanol with the volume percentage content of 50% is selected as the extractant.
In practice, the amino acid in step (3) may be glutamic acid and/or aspartic acid, and the sugar may be glucose.
And (4): mixing the first tobacco extract and the second tobacco extract to obtain the tobacco recombinant. The obtained tobacco recombinant is beneficial to increasing the concentration and the thickness of smoke and can also play a role in dyeing.
And (5): preparing a spice for cigar flavor cigarettes, wherein the spice for cigar flavor cigarettes comprises 1-10 parts of tobacco heavy component, 1-5 parts of cocoa extract, 0.01-0.05 part of sandalwood oil, 0.05-0.1 part of 2-methylvaleric acid and 0.001-0.005 part of isovaleric acid in parts by weight. The cigar flavor tobacco flavor disclosed by the disclosure takes the tobacco recombinant as a basic aroma source, can provide cigar characteristic aromas such as hay aroma, sweet aroma, sour aroma and the like, and is outstanding in cigar flavor.
And (6): and (3) diluting the cigar flavor cigarette flavor to the required concentration to obtain the cigar flavor coating liquid. The cigar flavor cigarette flavor obtained in the step (5) can be diluted by those skilled in the art according to actual needs, so as to prepare a cigar flavor coating liquid which can be used for coating operation.
And (7): and (3) coating the cigarette paper for the first time by adopting a roll coating method, and drying the cigarette paper coated for the first time at a low temperature. The roller speed of the first coating is usually constant, and the uniform coating can be carried out on the cigarette paper. The cigarette paper after the first coating can be dried at a low temperature of 60-80 ℃.
And (8): and (3) coating the cigarette paper for the second time by adopting a spray coating method, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper. The concentrations of the cigar flavor coating liquids at different positions on the cigarette paper at the time of spraying in the second coating may be the same or different. The cigarette paper after the second coating can be dried at a low temperature of 60-80 ℃.
The cigarette coating process has the advantages that the concentration and the thickness of smoke are increased by the aid of the secondary coating process, so that the cigar flavor of the cigarette is changed more abundantly, and smoking experience of consumers is improved.
The cigar flavor cigarette paper prepared by the coating preparation method of the cigar flavor cigarette paper can effectively enhance the cigar flavor of cigarettes, can increase the concentration and the thickness of smoke, can make the prepared cigar flavor cigarette paper show a dyeing effect without adding extra pigment, and is beneficial to optimizing the sensory experience of cigar flavor cigarettes.
In one embodiment of the coating preparation method of the cigar flavor cigarette paper disclosed by the invention, the step (1) is specifically as follows:
step (1-1): after the tobacco leaves are subjected to primary extraction treatment, the extract liquor obtained by the primary extraction is subjected to reduced pressure evaporation treatment, and the tobacco extract is prepared. In order to improve the extraction efficiency, the particle size of the tobacco leaf raw material to be extracted may be 10-100 mesh.
Step (1-2): and (3) separating supernatant at low temperature after the prepared tobacco extract is dissolved, and carrying out reduced pressure concentration treatment on the supernatant to obtain the tobacco concentrate. Step (1-2) facilitates further removal of impurities.
In specific implementation, a certain amount of 95% ethanol or absolute ethanol is added into the tobacco extract, the tobacco extract is fully dissolved after being heated to 30-50 ℃ and kept for 20-60 min, then the dissolved solution is cooled to room temperature, and the tobacco extract is frozen for 8-24 h under the conditions of-20 ℃ to-5 ℃. And then carrying out suction filtration on the frozen dissolved solution at low temperature or centrifuging at the rotating speed of 4000rpm for 10-30 min, and carrying out reduced pressure concentration on the filtrate or the centrifuged supernatant to remove ethanol, thus obtaining the tobacco concentrate.
Further, the first extraction in the step (1-1) adopts a subcritical extraction method, the extraction condition is that the extraction is carried out for 0.5h-2h at the temperature of 25-50 ℃, and the material-liquid ratio is 1 (8-20). In particular, the extraction pressure can be selected as the saturation vapor pressure of the extractant used at the corresponding temperature.
Further, the step (3) is specifically as follows:
step (3-1): and carrying out secondary extraction treatment on the tobacco leaves subjected to the primary extraction, and concentrating the extract liquor subjected to the secondary extraction under reduced pressure until the mass percentage content of dry matters is 30-50% to obtain the tobacco leaf extract. In specific implementation, the second extraction can be repeated twice to more fully and effectively extract the effective components in the tobacco leaves.
Step (3-2): adding a mixture with the molar ratio of amino acid to sugar of (0.5-1):1 into the tobacco extract according to the mass ratio of the mixture of amino acid and sugar to the tobacco extract of (1-3):10, reacting at 80-110 ℃ for 1-3 h, filtering a reaction product after the reaction is finished, diluting the obtained filtrate, filtering the diluted liquid through an ultrafiltration membrane of 10-50kD, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
And (3) after the reaction in the step (3-2) is finished, filtering, diluting, performing membrane separation and concentrating under reduced pressure are favorable for reducing the content of impurities in the second tobacco extract. In specific implementation, the reaction product can be filtered firstly after the reaction is finished, the obtained filtrate is diluted by adding water until the mass percentage of the stock solution is 10% -30%, then the diluted liquid is filtered by an ultrafiltration membrane of 10-50kD, and then the permeate is concentrated under reduced pressure to finally obtain the second tobacco extract.
The implementation mode of the coating preparation method of the cigar flavor cigarette paper is used for carrying out grading extraction on chemical components with different polarities in tobacco leaves, so that the tobacco leaf resources can be utilized to the maximum extent, and the purposes of cost reduction and efficiency improvement are achieved.
Further, in the step (3-1), the extraction method is adopted for the second extraction, and the extraction condition is that the extraction is carried out for 0.5h-3h at the temperature of 60-80 ℃, and the material-liquid ratio is 1 (6-12). The extractant can be water or ethanol, and the concentration of the ethanol can be flexibly selected according to actual requirements, for example, ethanol with the volume percentage content of 50% is selected as the extractant.
In one embodiment of the coating preparation method of the cigar flavor cigarette paper, the step (2) is as follows:
and carrying out secondary molecular distillation treatment on the obtained tobacco concentrate, wherein the temperature of the primary molecular distillation is 40-80 ℃, the distillation pressure is 0.001-0.01 mbar, the heavy component obtained after the primary molecular distillation is subjected to secondary molecular distillation, the temperature of the secondary molecular distillation is 100-120 ℃, the distillation pressure is 0.001-0.01 mbar, and the light component obtained after the secondary molecular distillation is collected to obtain the first tobacco extract. The secondary molecular distillation treatment is beneficial to further reducing the content of low-carbon alkane and high-carbon fatty acid in the tobacco concentrate.
The first tobacco extract obtained by molecular distillation effectively reduces the content of low-carbon alkane and high-carbon fatty acid in the finally obtained tobacco recombinant, so that the sweet aroma, the sour aroma, the baking aroma and other aroma of the tobacco recombinant are more prominent, meanwhile, the offensive odor and the irritation are reduced, and the smoking experience is improved.
In one embodiment of the coating preparation method of the cigar flavor cigarette paper, in order to obtain a tobacco recombinant with better flavor, the step (4) is specifically as follows:
mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1 (10-20) to obtain the tobacco recombinant.
In one embodiment of the coating preparation method of the cigar flavor cigarette paper, in order to improve the use feeling of the cigarette paper, the step (6) is specifically as follows:
step (6-1): mixing the cigar flavor tobacco flavor and the combustion improver according to the mass ratio of (96-99) to (1-4) to prepare the cigar flavor stock solution. The combustion improver can be a combustion improver commonly used in the field, and the combustion improver is not further limited by the disclosure.
Step (6-2): mixing the cigar flavor stock solution and an organic solvent to prepare cigar flavor coating liquids with different concentrations. The organic solvent may be, for example, ethanol, propylene glycol or a mixture of ethanol and propylene glycol. When a mixture of ethanol and propylene glycol is used as the solvent, the volume ratio of ethanol to propylene glycol may be 3: 1.
For the selection of the concentration of the cigar flavour coating liquid, in order to maintain a good smoking experience, the concentration of the cigar flavour coating liquid can be controlled to be 1-5 per mill of the mass of the dry matter of the cut tobacco of a single cigarette.
In one embodiment of the coating preparation method of the cigar flavor cigarette paper disclosed by the invention, the step (8) is specifically as follows:
and (3) coating the cigarette paper for the second time by adopting a spray coating method, arranging a plurality of spray heads in the running direction of the cigarette paper, wherein the concentrations of the cigar flavor coating liquids in the spray heads are different, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper. The concentration of the cigar flavor coating liquid in each spray head is controlled to be different, so that concentration change can be formed on the cigarette paper, a consumer can feel the cigar flavor which changes continuously in the smoking process, and the sensory enjoyment is improved.
In specific implementation, three spray heads can be arranged, and the concentration of the cigar flavor coating liquid in each spray head is respectively 1 per mill, 2 per mill and 5 per mill of the mass of the dry matter of the tobacco shred of a single cigarette.
Further, in order to maintain a good pumping experience, the concentration of the cigar flavor coating liquid used for the first coating in step (7) is the same as the concentration of the lowest cigar flavor coating liquid used for spraying in step (8). For example, when the minimum concentration of the cigar flavor coating liquid in the spray head in the spray coating method is 1% by mass of the cut tobacco of a single cigarette, the concentration of the cigar flavor coating liquid used in the roll coating method is controlled so that the mass of the dry matter is 1% by mass of the cut tobacco of a single cigarette.
The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.
Example 1
The tobacco leaves are crushed to 100 meshes, transferred to a subcritical extraction kettle, and then added with dimethyl ether, the material-liquid ratio is 1:8, the entrainer is 95% ethanol (the amount is 5% of the dimethyl ether), and the mixture is extracted for 2 hours at 25 ℃, and the extraction pressure is the saturated vapor pressure of the dimethyl ether at the temperature. And (4) after extraction, decompressing and evaporating to obtain tobacco extract.
Adding 5 times of 95% ethanol into tobacco extract, heating to 30 deg.C, and maintaining for 60min to dissolve completely. Then cooled to room temperature and transferred to a-20 ℃ freezer for freezing for 8 h. Filtering at low temperature to obtain filtrate, and concentrating the filtrate under reduced pressure until no ethanol is present to obtain tobacco concentrate.
The tobacco concentrate was transferred to a molecular distillation feed tank and distilled at 60 ℃ under 0.001mbar and the heavy fractions were collected. Distilling the heavy component at 120 deg.C under 0.001mbar for a second time, and collecting the light component to obtain first tobacco extract. The first tobacco extract was subjected to composition analysis by GC-MS, and the content of low-carbon alkane was only 0.4393mg/g, and the contents of linolenic acid and linoleic acid were 4.2163 mg/g and 9.4097mg/g, respectively.
Collecting the tobacco leaves after subcritical extraction, transferring the tobacco leaves to a round-bottom flask, then adding water, controlling the material-liquid ratio to be 1:12, heating to 60 ℃, extracting for 3 hours, and extracting twice. And combining the extraction liquid obtained in the two extraction steps after the extraction is finished, and concentrating under reduced pressure until the dry matter content is 30% to obtain the tobacco leaf extract.
Adding glutamic acid and glucose into the tobacco leaf extract at a molar ratio of 1:1, and heating to 80 ℃ for reaction for 3 h. After the reaction is finished, adding water to dilute the mixture until the mass fraction is 10%, then filtering the mixture by a 10kD ultrafiltration membrane, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
Mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1:10 to obtain the tobacco recombinant. Preparing cigar flavor stock solution according to 1 weight percent of combustion improver and 99 weight percent of cigar flavor cigarette flavor. The flavor for cigar flavor cigarettes comprises 1 percent of tobacco heavy component, 1 percent of cocoa extract, 0.01 percent of sandalwood oil, 0.1 percent of 2-methylvaleric acid, 0.001 percent of isovaleric acid and the balance of ethanol. Mixing the cigar flavor stock solution with an ethanol/propylene glycol mixed solvent with the volume ratio of 3:1 to prepare cigar flavor coating liquids with different concentrations.
Example 2
Crushing tobacco leaves to 100 meshes, transferring the crushed tobacco leaves to a subcritical extraction kettle, adding dimethyl ether into the subcritical extraction kettle at a material-liquid ratio of 1:10, extracting the crushed tobacco leaves for 0.5h at 40 ℃ by using absolute ethyl alcohol (the dosage of the dimethyl ether is 10%) as an entrainer, and the extraction pressure is the saturated vapor pressure of the dimethyl ether at the temperature. And (4) after extraction, decompressing and evaporating to obtain tobacco extract.
Adding 10 times of anhydrous ethanol into tobacco extract, heating to 50 deg.C, and maintaining for 20min for dissolving completely. Subsequently cooled to room temperature and transferred to a refrigerator at-5 ℃ for freezing for 24 h. Centrifuging at 4000rpm for 10min at low temperature, collecting supernatant, and concentrating under reduced pressure until no ethanol is contained to obtain tobacco concentrate.
The tobacco concentrate was transferred to a molecular distillation feed tank and distilled at 80 ℃ under 0.01mbar, and the heavy fractions were collected separately. Distilling the heavy component at 100 deg.C under 0.01mbar for a second time, and collecting the light component to obtain first tobacco extract. The characteristic aroma components of the first tobacco extract are analyzed by GC-MS, the content of the characteristic aroma components is greatly improved compared with that before distillation, the total content of ketone substances is 49.1827mg/g, wherein the content of megastigmatrienone is improved by 7.73 times, geranylacetone is 2 times of that before separation, and farnesylacetone is 6.36 times of that before separation.
Collecting the tobacco leaves after subcritical extraction, transferring the tobacco leaves to a round-bottom flask, then adding 50% ethanol with the material-liquid ratio of 1:6, heating to 80 ℃, extracting for 0.5h, and extracting twice. And combining the extraction liquid obtained in the two extraction steps after the extraction is finished, and concentrating under reduced pressure until the dry matter content is 50% to obtain the tobacco leaf extract.
Adding aspartic acid and glucose into the tobacco leaf extract at a molar ratio of 1:2, and heating to 110 ℃ for reacting for 1 h. And after the reaction is finished, adding water to dilute the mixture until the mass fraction is 30%, then filtering the mixture by a 50kD ultrafiltration membrane, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
Mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1:20 to obtain the tobacco recombinant. Preparing cigar flavor stock solution according to 4 wt% of combustion improver and 96 wt% of cigar flavor cigarette flavor. The spice for cigar flavor cigarettes comprises 5 percent of tobacco heavy component, 5 percent of cocoa extract, 0.05 percent of sandalwood oil, 0.08 percent of 2-methylvaleric acid, 0.005 percent of isovaleric acid and the balance of ethanol in percentage by weight. Mixing the cigar flavor stock solution with an ethanol/propylene glycol mixed solvent with the volume ratio of 3:1 to prepare cigar flavor coating liquids with different concentrations.
Example 3
Pulverizing tobacco leaf to 50 mesh, transferring to subcritical extraction kettle, adding butane at material-liquid ratio of 1:20, and extracting at 50 deg.C under saturated vapor pressure of butane at the temperature for 1 hr. And (4) after extraction, decompressing and evaporating to obtain tobacco extract.
Adding 8 times of anhydrous ethanol into tobacco extract, heating to 40 deg.C, and maintaining for 40min to dissolve completely. Subsequently cooled to room temperature and transferred to a-15 ℃ freezer for freezing for 12 h. Centrifuging at 4000rpm for 10min at low temperature, collecting supernatant, and concentrating under reduced pressure until no ethanol is contained to obtain tobacco concentrate.
The tobacco concentrate was transferred to a molecular distillation feed tank and distilled at 40 ℃ under 0.001mbar, collecting the heavy components. Performing secondary distillation on the heavy component at 120 deg.C and 0.01mbar, and collecting light component to obtain first tobacco extract.
Collecting the tobacco leaves after subcritical extraction, transferring the tobacco leaves to a round-bottom flask, then adding 30% ethanol with the material-liquid ratio of 1:10, heating to 70 ℃, extracting for 1h, and extracting twice. And combining the extraction liquid obtained in the two extraction steps after the extraction is finished, and concentrating under reduced pressure until the dry matter content is 40% to obtain the tobacco leaf extract.
Adding glutamic acid, aspartic acid and glucose into the tobacco leaf extract, wherein the molar ratio of the acid to the sugar is 1:1, and heating to 80 ℃ for reaction for 3 h. And after the reaction is finished, adding water to dilute the mixture until the mass fraction is 20%, then filtering the mixture by a 30kD ultrafiltration membrane, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
Mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1:15 to obtain the tobacco recombinant. Preparing cigar flavor stock solution according to 2 weight percent of combustion improver and 98 weight percent of cigar flavor cigarette flavor. The flavor for cigar flavor cigarettes comprises 10 percent of tobacco heavy component, 3 percent of cocoa extract, 0.02 percent of sandalwood oil, 0.05 percent of 2-methylvaleric acid, 0.002 percent of isovaleric acid and the balance of ethanol. Mixing the cigar flavor stock solution with an ethanol/propylene glycol mixed solvent with the volume ratio of 3:1 to prepare cigar flavor coating liquids with different concentrations.
The prepared cigar flavor coating liquid is used for preparing primary coating cigarette paper and secondary spraying cigarette paper through primary coating and secondary spraying respectively, and the primary coating cigarette paper and the secondary spraying cigarette paper are used for making cigarettes.
The results of comparing the cigarette samples using the primary coated cigarette paper, the cigarette samples using the secondary coated cigarette paper and the blank cigarette (the cigarette samples without the coating liquid) by suction evaluation are shown in table 1.
TABLE 1 comparison of assessment results
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (10)
1. A coating preparation method of cigar flavor cigarette paper is characterized by comprising the following steps:
(1) carrying out reduced pressure concentration treatment on the supernatant after the tobacco extract is dissolved to obtain a tobacco concentrate;
(2) subjecting the obtained tobacco concentrate to molecular distillation, and collecting light components to obtain a first tobacco extract;
(3) adding the mixture of amino acid and sugar into the tobacco leaf extract, reacting for a period of time, and filtering, diluting, membrane separating and concentrating under reduced pressure after the reaction is finished to obtain a second tobacco extract;
(4) mixing the first tobacco extract and the second tobacco extract to obtain a tobacco recombinant;
(5) preparing a spice for cigar flavor cigarettes, wherein the spice for cigar flavor cigarettes comprises 1-10 parts of tobacco heavy component, 1-5 parts of cocoa extract, 0.01-0.05 part of sandalwood oil, 0.05-0.1 part of 2-methylvaleric acid and 0.001-0.005 part of isovaleric acid in parts by weight;
(6) diluting the cigar flavor tobacco flavor to the required concentration to obtain cigar flavor coating liquid;
(7) coating the cigarette paper for the first time by adopting a roller coating method, and drying the cigarette paper coated for the first time at a low temperature;
(8) and (3) coating the cigarette paper for the second time by adopting a spray coating method, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper.
2. The coating preparation method according to claim 1, wherein the step (1) is specifically as follows:
(1-1) carrying out first extraction treatment on tobacco leaves, and then carrying out reduced pressure evaporation treatment on an extract liquor obtained by the first extraction to obtain a tobacco extract;
and (1-2) separating supernatant at low temperature after dissolving the prepared tobacco extract, and carrying out reduced pressure concentration treatment on the supernatant to obtain the tobacco concentrate.
3. The coating preparation method of claim 2, wherein the first extraction in the step (1-1) is performed by a subcritical extraction method, and the extraction conditions are that the extraction is performed at 25-50 ℃ for 0.5-2 h, and the material-liquid ratio is 1 (8-20).
4. The coating preparation method according to claim 2, wherein the step (3) is specifically as follows:
(3-1) carrying out second extraction treatment on the tobacco leaves after the first extraction, and carrying out reduced pressure concentration on the extract liquor after the second extraction until the mass percentage content of dry matters is 30-50% to obtain a tobacco leaf extract;
(3-2) adding a mixture with the molar ratio of the amino acid to the sugar being (0.5-1):1 into the tobacco extract according to the mass ratio of the mixture of the amino acid and the sugar to the tobacco extract being (1-3):10, reacting at 80-110 ℃ for 1-3 h, filtering a reaction product after the reaction is finished, diluting the obtained filtrate, filtering the diluted liquid through an ultrafiltration membrane of 10-50kD, and concentrating the permeate under reduced pressure to obtain a second tobacco extract.
5. The coating preparation method of claim 4, wherein the second extraction in the step (3-1) is a leaching extraction method, and the extraction conditions are 60-80 ℃ for 0.5-3 h, and the ratio of materials to liquids is 1 (6-12).
6. The coating preparation method according to claim 1, wherein the step (2) is specifically as follows:
and carrying out secondary molecular distillation treatment on the obtained tobacco concentrate, wherein the temperature of the primary molecular distillation is 40-80 ℃, the distillation pressure is 0.001-0.01 mbar, the heavy component obtained after the primary molecular distillation is subjected to secondary molecular distillation, the temperature of the secondary molecular distillation is 100-120 ℃, the distillation pressure is 0.001-0.01 mbar, and the light component obtained after the secondary molecular distillation is collected to obtain the first tobacco extract.
7. The coating preparation method according to claim 1, wherein the step (4) is specifically as follows:
mixing the first tobacco extract and the second tobacco extract according to the mass ratio of 1 (10-20) to obtain the tobacco recombinant.
8. The coating preparation method according to claim 1, wherein the step (6) is specifically as follows:
(6-1) mixing the cigar flavor tobacco flavor and the combustion improver according to the mass ratio of (96-99) to (1-4) to prepare cigar flavor stock solution;
(6-2) mixing the cigar flavor stock solution with an organic solvent to prepare cigar flavor coating liquids with different concentrations.
9. The coating preparation method according to any one of claims 1 to 8, characterized in that said step (8) is in particular as follows:
and (3) coating the cigarette paper for the second time by adopting a spray coating method, arranging a plurality of spray heads in the running direction of the cigarette paper, wherein the concentrations of the cigar flavor coating liquids in the spray heads are different, and drying the cigarette paper coated for the second time at a low temperature to obtain the cigar flavor cigarette paper.
10. The coating preparation method according to claim 9, wherein the concentration of the cigar flavor coating liquid used in the first coating in the step (7) is the same as the concentration of the lowest cigar flavor coating liquid used in the spraying in the step (8).
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