CN117859944A

CN117859944A - Low-temperature heating non-combustible tobacco particles and preparation method and application thereof

Info

Publication number: CN117859944A
Application number: CN202410169876.2A
Authority: CN
Inventors: 杜赫; 陈晨; 乔月梅; 常正兴; 王歆远
Original assignee: Inner Mongolia Kunming Cigarettes Co ltd
Current assignee: Inner Mongolia Kunming Cigarettes Co ltd
Priority date: 2024-02-06
Filing date: 2024-02-06
Publication date: 2024-04-12

Abstract

The application discloses tobacco particles for low-temperature heating non-combustion and a preparation method and application thereof, and belongs to the technical field of tobacco product manufacturing processes. The preparation method comprises the following steps: performing biological fermentation on the tobacco powder raw material, and then performing low-temperature drying, crushing and sieving; adding a thickening agent, granulating, and performing microwave drying to obtain tobacco powder particles with micropore structures; spraying the biological fermentation extract, the pyrolysis oil and the fuming agent on the tobacco powder particles to obtain the low-temperature heating non-burning tobacco particles. The tobacco particles which are not burnt by low-temperature heating are obtained through biological fermentation, low-temperature drying, granulation and microwave drying of the tobacco powder raw materials, and spraying of biological fermentation extract, pyrolysis oil and a smoke agent, the preparation method is simple, the industrial popularization is easy, and the quality and the sensory quality of smoke are effectively improved.

Description

Low-temperature heating non-combustible tobacco particles and preparation method and application thereof

Technical Field

The application relates to low-temperature heating non-combustible tobacco particles and a preparation method and application thereof, and belongs to the technical field of tobacco product manufacturing processes.

Background

Along with the continuous improvement of the demands of consumers on the taste and quality of cigarettes, the traditional cigarettes are gradually replaced by novel cigarette products due to the defects of impure fragrance, higher content of harmful substances and the like. The heating non-burning cigarette is a novel product combining a heating appliance and a cigarette bullet, is a low-temperature cigarette designed by taking 'only heating and non-burning' as thought, and utilizes a special heating device to heat the treated tobacco shreds and the cigarette bullet to a certain temperature, so that the cigarette bullet is heated to a degree sufficient to emit smoke for people to inhale, aroma components in the tobacco can be effectively released, and meanwhile, the generation of harmful substances is reduced.

The carrier of flavour substances, nicotine and smoking agents is important for heating non-combustible cigarettes. The currently developed smoke releasing materials mainly comprise cut tobacco, tobacco dust, tobacco sheets, conventional tobacco particles and the like. The materials can release smoke with the characteristic aroma of tobacco under different heating environments, but the tobacco shreds, the tobacco dust and the tobacco sheets have the defects of uneven heating, easy carbonization, inconvenient operation and the like. The problems of small smoke amount, uneven smoke generation, easy coking and the like exist in the tobacco shreds and the tobacco dust because the atomizing agent is difficult to add; while the tobacco sheet used by the iQOS solves the problem of smoke generation, the manufacturing process is complex, the equipment cost is high, the adjustability is not strong, and the smoke has heavy burnt paper taste, so that the taste is affected. The conventional tobacco particles have the characteristics of unobvious flavor, inconsistent front and rear smoke quantity, uneven heating, small smoke quantity, easy generation of burnt smell, and incapability of keeping cigarette aroma, thereby directly affecting the smoke quality and sensory quality.

Disclosure of Invention

In order to solve the problems, the low-temperature heating non-combustible tobacco particles, the preparation method and the application thereof are provided, and the low-temperature heating non-combustible tobacco particles are obtained through biological fermentation, low-temperature drying, granulation, microwave drying and spraying of biological fermentation extract, pyrolysis oil and fuming agent of tobacco powder raw materials, so that the preparation method is simple, the industrial popularization is easy, and the quality and the sensory quality of smoke are effectively improved.

According to one aspect of the present application, there is provided a method of preparing low temperature heated non-combustible tobacco particles comprising the steps of:

(1) Performing biological fermentation on the tobacco powder raw material, and then performing low-temperature drying, crushing and sieving;

(2) Adding a thickening agent, granulating, and performing microwave drying to obtain tobacco powder particles with micropore structures;

(3) Spraying the biological fermentation extract, the pyrolysis oil and the fuming agent on the tobacco powder particles obtained in the step (2) to obtain low-temperature heating non-burning tobacco particles.

Optionally, the pyrolysis oil comprises tobacco dry distillation pyrolysis oil and tobacco high-pressure pyrolysis oil, and the addition amount of the tobacco dry distillation pyrolysis oil is 0.01-0.015% of the mass of tobacco particles; the addition amount of the tobacco high-pressure pyrolysis oil is 0.1-0.15% of the mass of tobacco particles; the addition amount of the biological fermentation extract is 2% -2.7% of the mass of the tobacco particles; the addition amount of the smoke agent is 27% -33% of the mass of the tobacco particles.

Optionally, the fuming agent is glycerin and propylene glycol, and the ratio of glycerin to propylene glycol is 7:3.

optionally, the biological fermentation comprises adding the tobacco powder raw material and the compound fermentation enzyme preparation into a biological static fermentation box, adding water to ensure that the moisture of the tobacco powder is 30-40%, and fermenting for 70-75 h at the fermentation environment temperature of 40-50 ℃ and the fermentation environment humidity of 75-85%.

Optionally, the complex fermentation enzyme preparation comprises laccase, medium temperature amylase, neutral protease, plant hydrolase and pectinase; the mass ratio of laccase, medium-temperature amylase, neutral protease, plant hydrolase and pectase in the composite fermentation enzyme preparation is 2-3: 2 to 2.5: 2-3: 2 to 2.6:1 to 1.5 percent, and the addition amount of the composite fermentation enzyme preparation is 1 to 1.5 percent of the mass of the tobacco powder.

Optionally, the low-temperature drying is to put the tobacco powder into a blast drying box and dry for 3-4 hours at 50-60 ℃ until the moisture content of the tobacco powder is not higher than 8%; the number of the screen meshes of the crushing and sieving is 110-130 meshes.

Optionally, the microwave power of the microwave drying is 5.6-6 kw, the microwave time is 2.5-3 min, the thickening agent is obtained by dissolving sodium carboxymethyl cellulose in water, and the mass of the sodium carboxymethyl cellulose is 1.5-2% of the mass of the water; the addition amount of the sticky agent is 10-15% of the mass of the tobacco powder raw material.

Optionally, the preparation method of the tobacco high-pressure pyrolysis oil comprises the following steps: adding tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced to the pressure of 1MPa, adding 70% ethanol, reacting for 50min at the temperature of 280 ℃ and the feed-liquid ratio of 1: under the condition of 6g/ml, the pressure is controlled below 10MPa, and the tobacco high-pressure cracking oil is extracted.

According to another aspect of the application, the application also provides the low-temperature heating non-combustible tobacco particles prepared by the preparation method.

According to a further aspect of the application, the application further provides the application of the low-temperature heating non-combustible tobacco particles in the field of tobacco products.

Benefits of the present application include, but are not limited to:

1. according to the preparation method of the low-temperature heating non-combustible tobacco particles, the tobacco particles are obtained through biological fermentation, low-temperature drying, granulation, microwave drying, spraying and spraying of biological fermentation extract, pyrolysis oil and a fuming agent of the tobacco powder raw materials, the preparation method is simple, industrial popularization is easy, and the quality and sensory quality of smoke are effectively improved.

2. According to the preparation method of the low-temperature heating non-combustible tobacco particles, the chemical components in the tobacco powder are interfered through biological fermentation, so that the bad smell caused by heating of macromolecular substances is reduced, and meanwhile, the volatile aroma components of small molecules are increased, and the tobacco powder raw materials are improved from the source; after microwave drying treatment, the tobacco particles are provided with a micropore structure to bear biological fermentation extract, pyrolysis oil and fuming agent, and the aroma release is stable.

3. According to the preparation method of the low-temperature heating non-combustible tobacco particles, the biological fermentation effect is improved and the sensory quality of tobacco powder is improved by limiting the technological parameters of biological fermentation, the compound fermentation enzyme preparation and the proportion of the compound fermentation enzyme preparation; the extraction process parameters of the tobacco high-pressure pyrolysis oil are limited, so that the yield of the tobacco high-pressure pyrolysis oil and the flavor component content of the pyrolysis product are improved, and the sensory quality of tobacco particles is further improved.

Drawings

The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:

fig. 1 is a schematic diagram of the effect of oxygen on the tobacco high pressure pyrolysis oil yield according to an embodiment of the present application.

FIG. 2 is a graph showing the effect of ethanol concentration on tobacco high pressure pyrolysis oil yield according to the examples of the present application.

Fig. 3 is a schematic diagram showing the effect of extraction time on tobacco high pressure pyrolysis oil yield according to the embodiment of the present application.

Fig. 4 is a schematic diagram showing the effect of extraction temperature on tobacco high-pressure pyrolysis oil yield according to the embodiment of the present application.

Fig. 5 is a schematic diagram of the effect of feed liquid comparison on the yield of tobacco high-pressure pyrolysis oil according to the embodiment of the application.

Fig. 6 is an effect of the amount of addition of a smoking agent on sensory quality in accordance with an embodiment of the present application.

Fig. 7 is a schematic diagram showing the effect of the added amount of the biofermentation extract on the sensory quality.

Fig. 8 is a schematic diagram showing the effect of the addition amount of tobacco high-pressure pyrolysis oil on sensory quality according to the embodiment of the present application.

Detailed Description

The present application is described in detail below with reference to examples, but the present application is not limited to these examples.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described in this patent are illustrative only.

Example 1

The preparation method of the tobacco high-pressure pyrolysis oil comprises the following steps: adding tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced to the pressure of 1MPa, adding 70% ethanol, reacting for 50min at the temperature of 280 ℃ and the feed-liquid ratio of 1: under the condition of 6g/ml, the pressure is controlled below 10MPa, and the tobacco high-pressure cracking oil is extracted;

preparing biological fermentation extract: adding tobacco powder and water into a fermentation barrel, and adding a biological enzyme composite preparation, wherein the mass ratio of the tobacco powder to the water to the biological enzyme composite preparation is 1:10:0.01; the biological enzyme composite preparation comprises medium-temperature amylase, laccase, cellulase and plant hydrolase, wherein the mass ratio of the medium-temperature amylase to the laccase to the cellulase to the plant hydrolase is 1.5:1.5:3:2; and (3) putting the fermentation barrel into a fermentation cabinet for fermentation, wherein the fermentation temperature is 45 ℃, the fermentation time is 24 hours, the fermentation environment humidity is 75%, centrifuging the fermented product after the fermentation is finished, and concentrating the liquid part under reduced pressure to obtain the biological fermentation extract.

A preparation method of low-temperature heating non-combustible tobacco particles, which comprises the following steps:

(1) Carrying out biological fermentation on the tobacco powder raw material, wherein the biological fermentation comprises the steps of adding the tobacco powder raw material and a compound fermentation enzyme preparation into a biological static fermentation box, wherein the mass ratio of laccase, medium-temperature amylase, neutral protease, plant hydrolase and pectase in the compound fermentation enzyme preparation is 2:2:2:2:1, adding water to make the tobacco powder moisture be 30% and fermenting at 40 ℃ and 75% humidity for 70h, then drying at low temperature, pulverizing and sieving, drying at low temperature for 3h at 50 ℃ in a blast drying oven until the tobacco powder moisture content is 8%; the mesh number of the crushing and sieving screen is 110 meshes;

(2) Adding a thickening agent, wherein the thickening agent is obtained by dissolving sodium carboxymethyl cellulose in water, and the mass of the sodium carboxymethyl cellulose is 1.5% of that of the water; granulating, and performing microwave drying, wherein the microwave power of the microwave drying is 5.6kw, and the microwave time is 2.5min, so as to obtain tobacco powder particles with micropore structures;

(3) Spraying biological fermentation extract, pyrolysis oil and a fuming agent on the tobacco powder particles obtained in the step (2), wherein the pyrolysis oil comprises tobacco dry distillation pyrolysis oil and tobacco high-pressure pyrolysis oil, the addition amount of the tobacco dry distillation pyrolysis oil is 0.01% of the mass of the tobacco particles, and the addition amount of the tobacco high-pressure pyrolysis oil is 0.1% of the mass of the tobacco particles; the addition amount of the biological fermentation extract is 2% of the mass of the tobacco particles; the addition amount of the smoke agent is 27% of the mass of the tobacco particles, the smoke agent is glycerin and propylene glycol, and the ratio of the glycerin to the propylene glycol is 7: and 3, obtaining low-temperature heating non-combustible tobacco particles.

Example 2

(1) Carrying out biological fermentation on the tobacco powder raw material, wherein the biological fermentation comprises the steps of adding the tobacco powder raw material and a compound fermentation enzyme preparation into a biological static fermentation box, wherein the mass ratio of laccase, medium-temperature amylase, neutral protease, plant hydrolase and pectase in the compound fermentation enzyme preparation is 3:2.5:3:2.6:1.5, adding water to ensure that the water content of the tobacco powder is 40 percent, fermenting for 75 hours at the fermentation environment temperature of 50 ℃ and the fermentation environment humidity of 85 percent, then drying at low temperature, crushing and sieving, and drying at low temperature to ensure that the tobacco powder is dried for 4 hours at 60 ℃ in a blast drying box until the water content of the tobacco powder is 8 percent; the mesh number of the crushing and sieving is 130 meshes;

(2) Adding a thickening agent, wherein the thickening agent is obtained by dissolving sodium carboxymethyl cellulose in water, and the mass of the sodium carboxymethyl cellulose is 2% of that of the water; granulating, and performing microwave drying, wherein the microwave power of the microwave drying is 6kw, and the microwave time is 3min, so as to obtain tobacco powder particles with micropore structures;

(3) Spraying biological fermentation extract, pyrolysis oil and a fuming agent on the tobacco powder particles obtained in the step (2), wherein the pyrolysis oil comprises tobacco dry distillation pyrolysis oil and tobacco high-pressure pyrolysis oil, the addition amount of the tobacco dry distillation pyrolysis oil is 0.015% of the mass of the tobacco particles, and the addition amount of the tobacco high-pressure pyrolysis oil is 0.15% of the mass of the tobacco particles; the addition amount of the biological fermentation extract is 2.7% of the mass of the tobacco particles; the addition amount of the smoke agent is 33% of the mass of the tobacco particles, the smoke agent is glycerin and propylene glycol, and the ratio of the glycerin to the propylene glycol is 7: and 3, obtaining low-temperature heating non-combustible tobacco particles.

Example 3

(1) Carrying out biological fermentation on the tobacco powder raw material, wherein the biological fermentation comprises the steps of adding the tobacco powder raw material and a compound fermentation enzyme preparation into a biological static fermentation box, wherein the mass ratio of laccase, medium-temperature amylase, neutral protease, plant hydrolase and pectase in the compound fermentation enzyme preparation is 3:2.5:3:2:1, adding water to ensure that the water content of the tobacco powder is 35%, fermenting for 72 hours at the fermentation environment temperature of 45 ℃ and the fermentation environment humidity of 80%, drying at low temperature, crushing and sieving, and drying at low temperature to ensure that the tobacco powder is dried for 4 hours at 60 ℃ in a blast drying box until the water content of the tobacco powder is 8%; the mesh number of the crushed and sieved sieve is 120 meshes;

(2) Adding a thickening agent, wherein the thickening agent is obtained by dissolving sodium carboxymethyl cellulose in water, and the mass of the sodium carboxymethyl cellulose is 1.7% of that of the water; granulating, and performing microwave drying, wherein the microwave power of the microwave drying is 5.6kw, and the microwave time is 2.7min, so as to obtain tobacco powder particles with micropore structures;

(3) Spraying biological fermentation extract, pyrolysis oil and a fuming agent on the tobacco powder particles obtained in the step (2), wherein the pyrolysis oil comprises tobacco dry distillation pyrolysis oil and tobacco high-pressure pyrolysis oil, the addition amount of the tobacco dry distillation pyrolysis oil is 0.01% of the mass of the tobacco particles, and the addition amount of the tobacco high-pressure pyrolysis oil is 0.1% of the mass of the tobacco particles; the addition amount of the biological fermentation extract is 2.5% of the mass of the tobacco particles; the addition amount of the smoke agent is 30% of the mass of the tobacco particles, the smoke agent is glycerin and propylene glycol, and the ratio of the glycerin to the propylene glycol is 7: and 3, obtaining low-temperature heating non-combustible tobacco particles.

Comparative example 1

Comparative example 1 differs from example 3 in that no tobacco high pressure pyrolysis oil was sprayed, the remainder being the same.

Comparative example 2

Comparative example 2 differs from example 3 in that the amount of smoke agent added was 15%, 20%, 25% and 35% of the mass of the tobacco dust particles, respectively, and the remainder was the same.

Comparative example 3

Comparative example 3 differs from example 3 in that the amount of the biologically fermented extract added was 1.5%, 2%, 3%, 3.5% of the mass of the tobacco dust particles, respectively, and the remainder was the same.

Comparative example 4

Comparative example 4 differs from example 3 in that the amount of tobacco high-pressure pyrolysis oil added is 0.03%, 0.05%, 0.2%, 0.3% of the mass of the tobacco dust particles, respectively, and the rest is the same.

Experimental example 1 selection of conditions for preparation of tobacco pyrolysis oil

1.1 Effect of oxygen-passing amount on extraction yield of tobacco high-pressure pyrolysis oil

Accurately weighing 50g of tobacco powder, adding the tobacco powder into a high-pressure reaction kettle, respectively reacting under the conditions of introducing compressed air and different compressed air, adding 70% ethanol, reacting for 30min at 250 ℃, and mixing the materials with a feed liquid ratio of l: under the condition of 10, the pressure is controlled below 10MPa, and the tobacco powder pyrolysis oil is extracted. The extract was concentrated under reduced pressure by filtration, and then weighed. The results are shown in figure 1, the yield of the high-pressure pyrolysis oil fed with no air is lower, and the sensory evaluation has gasoline smell, and the high-pressure pyrolysis reaction needs enough oxygen to participate in the comprehensive consideration.

1.2 selection of ethanol concentration

Accurately weighing 50g of tobacco powder, adding the tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced until the pressure is 1MP a, respectively adding 0%, 30%, 50%, 70% and 100% ethanol, reacting for 30min at the temperature of 250 ℃ and the feed-liquid ratio of l: under the condition of 10, the pressure is controlled below 10MPa, and the tobacco powder pyrolysis oil is extracted. The extract is weighed after being concentrated under reduced pressure by filtration, the yield of the aroma substances is calculated, and the optimal ethanol concentration is selected. As a result, as shown in fig. 2, the extraction effect of the high-pressure pyrolysis oil was deteriorated from good as the concentration of ethanol was increased, and 70% ethanol was selected as the extractant in consideration of energy consumption and economic efficiency.

1.3 selection of extraction time

Accurately weighing 50g of tobacco powder, adding the tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced until the pressure is 1MP a, adding 70% ethanol, and setting the reaction time to be 10min, 20min, 30min,50min and 60min respectively, wherein the reaction temperature is 250 ℃, and the feed liquid ratio is l: under the condition of 10, the pressure is controlled below 10MPa, and the tobacco powder pyrolysis oil is extracted. Filtering, concentrating under reduced pressure, weighing the extractive solution, calculating the yield of aroma substances, and selecting the optimal extraction time. As a result, as shown in fig. 3, the tobacco high-pressure pyrolysis oil extraction rate showed a tendency to increase and decrease with the increase of the extraction time, and reached the maximum at 30 min. The energy consumption and the economic benefit are comprehensively considered, and the extraction time is properly selected to be 30 minutes.

1.4 selection of extraction temperature

Accurately weighing 50g of tobacco powder, adding the tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced until the pressure is 1MP a, adding 70% ethanol, and reacting for 30min at 150 ℃, 200 ℃, 250 ℃ and 300 ℃ respectively, wherein the feed-liquid ratio is l: under the condition of 10, the pressure is controlled below 10MPa, and the tobacco powder pyrolysis oil is extracted. The extract is weighed after being concentrated under reduced pressure by filtration, the yield of the aromatic substances is calculated, and the optimal extraction temperature is selected. As a result, as shown in FIG. 4, the extraction rate of the high-pressure pyrolysis oil of tobacco tended to increase with increasing extraction temperature, and remained substantially stable at 250 ℃. Therefore 250℃is chosen as the optimum extraction temperature.

1.5 selection of feed to liquid ratio

Accurately weighing 50g of tobacco powder, adding the tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced until the pressure is 1MP a, adding 70% ethanol, reacting for 30min at the temperature of 250 ℃ respectively, and the feed liquid ratio of 1:2, 1:5, 1:8 and l: under the condition of 10, the pressure is controlled below 10MPa, and the tobacco powder pyrolysis oil is extracted. Filtering, concentrating under reduced pressure, weighing the extract, calculating the yield of the aromatic substances, and selecting the optimal feed-liquid ratio. As shown in FIG. 5, the extraction rate of the tobacco high-pressure pyrolysis oil is in an upward trend along with the increase of the extracting solution, and the extraction rate is basically kept stable at 1:5. Economic factors are comprehensively considered, so that 1:5 is selected as the optimal extraction liquid-to-liquid ratio.

2.1 orthogonal test

Based on the single factor test result, the reaction is carried out under the condition that the pressure in a high-pressure reaction kettle is 1MPa, the reaction pressure is controlled below 10MPa, the ethanol concentration (A), the extraction time (B), the extraction temperature (C) and the feed liquid ratio (D) are selected, 4 factors are taken as indexes, and the extraction rate of the tobacco high-pressure pyrolysis oil is taken as an index, and an L9 (34) orthogonal table is adopted to design an orthogonal test (as shown in table 1) so as to screen the optimal extraction process parameters.

TABLE 1 L9 (34) orthogonal test factor level Table

2.2 repeatability test

And (3) carrying out repeated verification tests for 3 times under the optimal test conditions determined by the orthogonal test, and calculating the high-pressure cracking oil-decomposing yield of the tobacco.

The results are shown in Table 2,

TABLE 2 L9 (34) results of orthogonal experiments

As shown in table 2, comparing R values, four factors affect the tobacco pyrolysis oil yield in the following order: extraction temperature > ethanol concentration > extraction time > feed-liquid ratio. As can be seen from the comparison of K values, A2B3C2D3 is the optimal extraction condition, namely, the ethanol concentration is 70%, the extraction time is 50min, the extraction temperature is 280 ℃, and the feed-liquid ratio is 1:6g/mL. The extraction rates of the 3 parallel verification tests under the condition are 31.88%, 31.95% and 31.45%, and the average value of the extraction rates is 31.76% of tobacco pyrolysis oil under the optimal condition.

2.3 analysis of tobacco high pressure pyrolysis oil composition

Taking 0.1g of concentrated high-pressure pyrolysis oil, putting the concentrated high-pressure pyrolysis oil into a 50mL triangular flask, adding 20mL of dichloromethane into the triangular flask, performing ultrasonic extraction for 30min, standing, putting the extract into a concentration bottle through an organic film, adding 1mL of phenethyl acetate internal standard solution (the concentration is 0.3416 mg/mL), concentrating the extract to 1mL at 60 ℃, and performing GC-MS analysis. The volatile aroma component content was calculated.

Gas chromatography conditions: chromatographic column: HP-5MS (60 m. Times.250. Mu. m x 0.25 μm); sample inlet temperature: 280 ℃; sample injection amount: 1 μl; split ratio: 5:1; heating program: 50 ℃ (hold 2 min), then raise to 280 ℃ (hold 20 min) at 4 ℃/min; mass spectrometry conditions: temperature of the transmission line: 280 ℃; EI source electron energy: 70eV; electron multiplier voltage: 1650v; mass scan range: 35-550amu; ion source temperature: 230 ℃; four-stage bar temperature: 150 ℃; and (3) utilizing a Nist11 database to collect a mass spectrum particle flow diagram of volatile components of the tobacco extract for analysis and identification.

Calculation method for yield of tobacco high-pressure pyrolysis oil

Yield of tobacco-producing high pressure pyrolysis oil = weight of pyrolysis oil with moisture removed/amount of tobacco fines charged ×100

Calculation method of flavor component content of cracked product

Lysates were characterized using a Nist11 standard library, and the relative correction factor (relative to the internal standard) was assumed to be 1, and the amounts of the respective aroma substances were quantitatively calculated according to the following formula.

The results are shown in tables 3 and 4.

TABLE 3 analysis of major flavor components of high pressure pyrolysis oil for tobacco

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As can be seen from Table 3, the main chemical components of the tobacco pyrolysis oil comprise furfural, 2-cyclopentenone, furfuryl alcohol, methylcyclopentenolone, 2-acetyl furan, 2 (5H) -furanone, 5-methyl-2 (5H) -furanone, pinacolone, 5-methylfuran aldehyde, benzyl alcohol, ethyl maltol, cinnamaldehyde, 5-hydroxymethylfurfural, eggplant ketone, citronellal, 2, 6-dimethyl pyrazine, 2,3, 5-trimethyl pyrazine, ethyl vanillin, ethyl palmitate, 5-methyl-2- (1-methylethyl) -2-cyclohexene-1-one, vanillin, geranylacetone, neophytadiene, nicotine, megastigmatrienone, dihydro kiwi lactone and the like.

TABLE 4 ranges for the content of various compounds in high pressure pyrolysis oil

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Analysis and classification research are carried out on chemical components in the tobacco high-pressure pyrolysis oil by using GC-MS, so that the content of various chemical components such as alkaloids, hydrocarbons, phenols, aldehydes, ketones, heterocycles, phenols and the like is clarified, and is shown in table 4. The tobacco high-pressure pyrolysis oil contains ketone, aldehyde, ester, hydrocarbon, alcohol, phenol, alkaloid, heterocycle, and organic acids in the content ranges of 129.98mg/g, 69.96mg/g, 61.33mg/g, 15.106mg/g, 32.94mg/g, 40.7mg/g, 38.23mg/g, 0.7068mg/g, and 8.246mg/g.

Experimental example 2

The sensory quality evaluation of the tobacco particles prepared in examples 1 to 3 and comparative example 1 was performed, and seven indexes of concentration, aroma, flavor, strength, harmony, miscellaneous gases, irritation and taste were selected as sensory evaluation indexes of the heated non-combustible cigarettes, with reference to the sensory quality evaluation method of the conventional cigarettes. Wherein concentration refers to the size or shade (plumpness) of the smoke; aroma refers to the pleasant aroma and taste perceived during pumping; the stiffness refers to physiological satisfaction brought by smoke nicotine; the harmony means that the fragrance is harmonious and consistent, and the characteristics of a certain monomer, such as flavoring, charging and smoke fragrance, are not felt, and the formula of the leaf group is harmonious; irritation refers to the slight and noticeable discomfort perceived by the smoke. Such as punching the nasal cavity, oral cavity and throat, singing Mao Jihuo, etc.; miscellaneous gases refer to unpleasant gases contained in the smoke, such as sweet greasy feeling or other chemical gases caused by heating glycerin and propylene glycol in the non-combustible cigarettes; mouthfeel refers to the overall taste sensation imparted to the oral cavity during the aspiration process, including comfort, cleanliness, sweetness, dryness, etc., and is generally described as comfortable, more comfortable, still comfortable, etc.

Before or during the evaluation of the test specimens, 9 panelists were organized to perform sensory evaluation corresponding to the standard sample (IQOS) in order to calibrate the calibre. Adopting a percentage system, and dividing the maximum part into 100 parts; each index is divided into score units of 0.5; when seven indexes of concentration, aroma, fragrance, strength, harmony, irritation, miscellaneous gas and taste are evaluated and recorded, the quality of each index meets the requirements of the corresponding index, and the corresponding score is obtained; the result statistical weighted average calculates single average score to be accurate to 0.01; the sensory quality score was expressed as the sum of the average scores of the individual items, to the nearest 0.1. The evaluation criteria are shown in Table 5, and the evaluation results are shown in Table 6.

TABLE 5 sensory quality criteria

TABLE 6 sensory quality evaluation results

Experimental example 3

The sensory quality and evaluation of comparative example 2 and example 3 were carried out by referring to the evaluation method of experimental example 2, and the effect of the addition amount of the smoke agent on the sensory quality was obtained, and the results are shown in fig. 6.

Experimental example 4

The sensory quality and evaluation of comparative example 3 and example 3 were carried out with reference to the evaluation method of experimental example 2, and the effect of the added amount of the biofermentation extract on the sensory quality was obtained, and the result is shown in fig. 7.

Experimental example 5

With reference to the evaluation method of experimental example 2, the sensory quality and evaluation of comparative example 3 and example 3 were carried out to obtain the influence of the addition amount of the tobacco high-pressure pyrolysis oil on the sensory quality, and the results are shown in fig. 8.

As shown in fig. 6, as the addition amount of the smoke agent increases, the sensory quality increases and decreases, and an inflection point exists at 30%, and as the addition amount of the smoke agent is lower than 30%, the sensory quality also increases continuously and reaches the highest point at 30% with the addition amount of the smoke agent increasing; when the addition amount of the smoke agent is higher than 30%, the sensory quality is reduced along with the increase of the addition amount of the smoke agent, the application limits the addition amount of the smoke agent to achieve better sensory quality, and analysis is because the addition amount of the smoke agent is increased along with the increase of the addition amount of the smoke agent, but the excessive addition amount of the smoke agent can cause the mouth to feel sweet and greasy, and the sensory quality is reduced.

As shown in fig. 7, as the addition amount of the biofermentation extract increases, the sensory quality increases and decreases, and an inflection point exists at 2.5%, when the addition amount of the biofermentation extract is lower than 2.5%, as the addition amount of the biofermentation extract increases, the sensory quality also increases continuously, and when the addition amount of the biofermentation extract reaches 2.5%, the highest point is reached; when the addition amount of the biological fermentation extract is higher than 2.5%, the sensory quality is reduced along with the increase of the addition amount of the biological fermentation extract, so that the addition amount of the biological fermentation extract is limited to achieve better sensory quality.

As shown in fig. 8, as the amount of tobacco high-pressure pyrolysis oil added increases, the sensory quality score of the heated nonflammable cigarette tends to increase and then decrease, and the sensory quality score is highest when the amount of tobacco high-pressure pyrolysis oil added is 0.1%. The increase of the proportion of the tobacco high-pressure pyrolysis oil is beneficial to the promotion of aroma and strength, the excessive addition can cause bitter taste, and the addition of the tobacco high-pressure pyrolysis oil is 0.1 percent and is more suitable.

The foregoing is merely exemplary of the present application, and the scope of the present application is not limited to the specific embodiments, but is defined by the claims of the present application. Various modifications and changes may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical ideas and principles of the present application should be included in the protection scope of the present application.

Claims

1. A method for preparing low-temperature heated non-combustible tobacco particles, comprising the steps of:

2. The preparation method of claim 1, wherein the pyrolysis oil comprises tobacco dry distillation pyrolysis oil and tobacco high-pressure pyrolysis oil, and the addition amount of the tobacco dry distillation pyrolysis oil is 0.01% -0.015% of the mass of tobacco particles; the addition amount of the tobacco high-pressure pyrolysis oil is 0.1-0.15% of the mass of tobacco particles; the addition amount of the biological fermentation extract is 2% -2.7% of the mass of the tobacco particles; the addition amount of the smoke agent is 27% -33% of the mass of the tobacco particles.

3. The method of claim 2 wherein the smoking agent is glycerin and propylene glycol in a ratio of 7:3.

4. the preparation method according to claim 1, wherein the biological fermentation comprises adding tobacco powder raw materials and a composite fermentation enzyme preparation into a biological static fermentation box, adding water to make the moisture of the tobacco powder 30% -40%, and fermenting at the fermentation environment temperature of 40-50 ℃ and the fermentation environment humidity of 75% -85% for 70-75 h.

5. The method of claim 4, wherein the complex fermentation enzyme preparation comprises laccase, mesophilic amylase, neutral protease, plant hydrolase and pectinase; the mass ratio of laccase, medium-temperature amylase, neutral protease, plant hydrolase and pectase in the composite fermentation enzyme preparation is 2-3: 2 to 2.5: 2-3: 2 to 2.6:1 to 1.5 percent, and the addition amount of the composite fermentation enzyme preparation is 1 to 1.5 percent of the mass of the tobacco powder.

6. The preparation method of claim 1, wherein the low-temperature drying is to dry the tobacco powder in a forced air drying oven at 50-60 ℃ for 3-4 hours until the moisture content of the tobacco powder is not higher than 8%; the number of the screen meshes of the crushing and sieving is 110-130 meshes.

7. The preparation method according to claim 1, wherein the microwave power of the microwave drying is 5.6-6 kw, the microwave time is 2.5-3 min, the thickening agent is obtained by dissolving sodium carboxymethyl cellulose in water, and the mass of the sodium carboxymethyl cellulose is 1.5-2% of the mass of the water; the addition amount of the sticky agent is 10-15% of the mass of the tobacco powder raw material.

8. The method of claim 1, wherein the method of preparing the tobacco high pressure pyrolysis oil comprises the steps of: adding tobacco powder into a high-pressure reaction kettle, reacting under the condition that compressed air is introduced to the pressure of 1MPa, adding 70% ethanol, reacting for 50min at the temperature of 280 ℃ and the feed-liquid ratio of 1: under the condition of 6g/ml, the pressure is controlled below 10MPa, and the tobacco high-pressure cracking oil is extracted.

9. The low-temperature heating non-combustible tobacco particles prepared by the preparation method of any one of claims 1 to 8.

10. Use of the low temperature heated non-combustible tobacco particles of claim 9 in the field of tobacco products.