A tobacco dry distillation refined product, a preparation method and application thereof

Abstract

This invention discloses a tobacco pyrolysis refined product, its preparation method, and its application. The pyrolysis refined product is obtained by pyrolysis of tobacco raw materials to obtain pyrolyzed tobacco material; the pyrolyzed tobacco material is mixed evenly with a solvent and homogenized, then separated into solid and liquid components, and the supernatant is collected to obtain a pyrolyzed tobacco material extract; the extract is then subjected to molecular distillation, and the light component fraction is collected to obtain the final product. Based on the synergistic effect between its components, this refined product significantly increases the content and variety of aroma compounds, especially pyrazines, pyridines, and nicotines. When used as a flavoring agent in heated cigarettes, it effectively improves the sensory quality of heated cigarettes. Heated cigarettes using this refined product have a rich and mellow aroma, high richness, significantly increased smoke concentration, a more comfortable strength, a more delicate and mellow smoke, a significantly improved aftertaste, and a greatly improved consistency in aroma and smoke.

Description

Technical Field

[0001] This invention relates to a tobacco dry distillation refined product, specifically to a tobacco dry distillation refined product and its preparation method and application, belonging to the field of flavor and fragrance technology. Background Technology

[0002] Heated cigarettes primarily work by heating tobacco leaves at a low temperature. The tobacco leaf is precisely heated using temperature control technology to achieve the ideal temperature for releasing the aromatic compounds and nicotine, thus producing smoke. This method heats the tobacco leaves to a level sufficient to release their flavor without igniting them. Its taste is closest to traditional cigarettes and is expected to be the first to be accepted by smokers. Comparative analysis of heated cigarettes and traditional cigarettes reveals that the fundamental sensory difference lies in their different heating temperatures. Traditional cigarettes involve combustion, with aroma compounds arising from the transfer of these compounds within the tobacco itself and the complex thermal decomposition reactions during combustion. Whether through the transfer of aroma compounds or thermal decomposition, the aroma compounds primarily originate from the pyrolysis / distillation zone of the cigarette during combustion, at temperatures ranging from approximately 250 to 600°C. Heated cigarettes, on the other hand, involve heating, not combustion, with heating temperatures generally not exceeding 300°C. The internal temperature of the cigarette is even lower. Therefore, compared to traditional cigarettes, heated cigarettes, due to their lower temperature, do not reach the aroma-producing temperature of traditional cigarettes, resulting in significantly less aroma richness. Consequently, external extracts are needed to enhance the smoke quality.

[0003] In existing technologies, common extraction methods for preparing tobacco extracts include solvent extraction, steam distillation, and supercritical fluid extraction. CN102349698B describes extracting tobacco leaves or stems by heating and reflux with water, ethanol, or ether, followed by sedimentation and filtration to obtain the tobacco extract. CN104761538A describes simultaneously adding tobacco and alkaline materials to a steam distillation vessel to extract a nicotine-containing tobacco extract. CN109275947B describes placing tobacco raw materials in a supercritical fluid extraction device, adding a certain amount of entrainer at a specific extraction pressure and temperature, and obtaining the tobacco extract from the separation vessel.

[0004] However, the tobacco extracts obtained by traditional methods currently have a weak aroma, especially lacking the base aroma of tobacco, which cannot meet the requirements of flavoring for heated cigarettes. Summary of the Invention

[0005] To address the problems existing in the prior art, the first objective of this invention is to provide a tobacco dry distillation refined product. Based on the synergistic effect between the components, this refined product significantly increases the content and types of aroma substances, especially pyrazines, pyridines, and nicotines. While ensuring that heated cigarettes have a significant tobacco aroma, it imparts a variety of aroma profiles such as roasted, nutty, caramelized, sweet, and hay-like aromas.

[0006] The second objective of this invention is to provide a method for preparing tobacco dry distillation refined products. This method first alters the internal structure of tobacco raw materials through heating and dry distillation, causing some macromolecular substances in the tobacco leaves to decompose into small-molecule aroma compounds, including alkaloids such as nicotine, which are broken down into mesmin, cotinine, dienicotinic acid, 2,3'-bipyridine, and other major and minor alkaloids in tobacco. These compounds are then subjected to homogenization and molecular distillation to further extract phenolic compounds from the tobacco raw materials. This preparation method has the advantages of simple process and wide availability of raw materials. While significantly improving the flavor characteristics of the refined products, it also effectively realizes the resource utilization of tobacco scraps.

[0007] The third objective of this invention is to provide an application of tobacco dry distillation refined product as a flavoring agent for heated tobacco products. Based on the superior technical effects of the aforementioned multi-component composite refined product, its application as a flavoring agent in heated tobacco products can effectively improve the sensory quality of heated tobacco products. GC-MS testing shows that the total amount of aroma compounds in this refined product includes more than 30 substances in 5 major categories. Sensory analysis shows that heated tobacco products using the refined product of this invention have a rich and mellow aroma with high richness, significantly increased smoke concentration, a more comfortable strength, a more delicate and mellow smoke, a significantly improved aftertaste, and a substantial improvement in the consistency of aroma and smoke.

[0008] To achieve the above-mentioned technical objectives, the present invention provides a method for preparing tobacco dry distillation refined product, wherein tobacco raw materials are subjected to dry distillation reaction to obtain dry distilled tobacco material; the dry distilled tobacco material is mixed evenly with a solvent and homogenized, and then the supernatant is collected after solid-liquid separation to obtain dry distilled tobacco material extract; the dry distilled tobacco material extract is subjected to molecular distillation, and the light component fraction is collected to obtain the final product.

[0009] The tobacco dry distillation refined product for heated cigarettes provided by this invention is obtained by heating tobacco powder or shredded tobacco in a sealed environment at 80℃-300℃ to obtain dry distilled tobacco powder. The dry distilled tobacco powder and propylene glycol are then homogenized under high pressure to obtain a homogenized dry distilled tobacco powder extract. The extract is then subjected to molecular distillation to obtain the tobacco dry distillation refined product. Chromatographic analysis shows a significant increase in the types and quantities of volatile products in the tobacco dry distillation refined product. At a dry distillation temperature of 100-150℃, the aroma components mainly include megastigmatrienone, hydroxydamaconone, 7-hydroxyfarnesene, and acetyldamaconone, with a certain increase in content. At a dry distillation temperature of 200℃, the aroma components mainly include pyrazines, pyridines, nicotine, and the types and contents of aroma substances are significantly increased. At a dry distillation temperature of 300℃, the aroma components mainly include nitrogenous substances such as pyrazines, pyridines, and nicotine, with a certain increase in content, and phenolic substances also increase. It imparts to heated cigarettes the aromas of flue-cured tobacco, roasted tobacco, nuts, caramel, sweet, and hay.

[0010] As a preferred embodiment, the tobacco raw material is at least one of tobacco, burley tobacco and cigar tobacco, and its morphology is tobacco shreds and / or tobacco powder.

[0011] As a preferred embodiment, the process of the dry distillation reaction is as follows: tobacco raw materials are placed in a high-temperature dry distillation reactor and heated in a sealed manner at 80-300°C for 0.5-2 hours.

[0012] The dry distillation reaction employed in this invention effectively expands the internal structure of tobacco leaves, significantly increasing the bulkiness of the raw material. Simultaneously, it damages special tissues such as vascular bundles and fiber bundles to varying degrees, ensuring the complete release of aroma compounds from all parts of the tobacco. At heating temperatures of 100–200°C, aroma compounds such as megastigmatrienone and hydroxydamascone are easily released from tobacco leaves. At heating temperatures of 200–300°C, alkaloids such as alkaloids can decompose into mesmin, cotinine, dienicotinic acid, 2,3'-bipyridine, and other major and minor alkaloids in tobacco, resulting in a certain increase in alkaloid content in the tobacco leaves. During the heating process, carbonyl compounds (reducing sugars, fructose, glucose) and amino compounds (proteins, free amino acids, and proline) naturally present in tobacco undergo pyrolysis and Maillard reaction product transfer under high-temperature conditions, generating various special aroma and olfactory substances, such as pyrazines and pyridines, which significantly influence the flavor characteristics of tobacco leaves. Therefore, tobacco leaves heated to 200-300℃ contain a high concentration of pyridine and pyrazine compounds. Phenolic compounds have complex precursors; small-molecule sugars, cellulose, hemicellulose, lignin, and pectin are the main precursors of phenolic compounds in tobacco smoke. As the heating temperature gradually approaches 300℃, these substances partially decompose, producing certain phenolic compounds. After extraction and refining of heated tobacco, the content of corresponding aroma components such as pyrazines, pyridines, alkaloids, ketones, alcohols, and esters in the refined heated tobacco product increases significantly. This results in a richer and more flavorful product, greatly improving the sensory quality of heated cigarettes. When used in heated cigarettes, it can impart aromas of flue-cured tobacco, roasted tobacco, nuts, caramel, sweet, and hay, effectively enhancing the intrinsic quality of heated cigarette products, with excellent application results.

[0013] As a preferred embodiment, the solvent is at least one of deionized water, ethanol, and propylene glycol; the mass ratio of the dry distillation fume to the solvent is 1:6 to 10.

[0014] As a preferred embodiment, the homogenization method is high-pressure homogenization, the conditions of which are: after the dry distillation fume and solvent are mixed evenly, homogenization is carried out at a pressure of 100-150 bar for 40-60 min.

[0015] As a preferred embodiment, the solid-liquid separation method is centrifugal separation, with the following conditions: centrifugation at 3000-500 rpm for 5-10 minutes at room temperature.

[0016] As a preferred embodiment, the molecular distillation conditions are: vacuum degree of 1.0 to 3.0 mbar, temperature of 60 to 100°C, feeding rate of 2 to 6 mL / min, and film scraping rate of 200 to 300 r / min.

[0017] The present invention also provides a tobacco dry distillation refined product, characterized in that it is prepared by the method described in any one of the above-mentioned methods.

[0018] As a preferred embodiment, the main aroma compounds in the dry distillation product include pyrazines, pyridines, and alkaloids.

[0019] The present invention also provides an application of tobacco dry distillation refined product as a flavoring agent for heated non-combustible cigarettes.

[0020] Compared with the prior art, the beneficial technical solution of the present invention is as follows:

[0021] 1) The tobacco refined product provided by the present invention significantly increases the content and types of aroma substances based on the synergistic effect between the components, especially pyrazine, pyridine and nicotine substances. While ensuring that the heated cigarette has a significant tobacco aroma, it endows it with a variety of aromas such as roasted aroma, nutty aroma, caramel sweet aroma, fresh sweet aroma and hay aroma.

[0022] 2) The preparation method provided by this invention first changes the internal structure of tobacco raw materials through heating and dry distillation, causing some macromolecular substances in tobacco leaves to decompose into small molecule aroma substances, including alkaloids such as nicotine, which are broken down into mesmin, cotinine, dienicotinic acid, 2,3'-bipyridine, and the main and minor alkaloids in tobacco. Then, after homogenization and molecular distillation, phenolic compounds in tobacco raw materials are further extracted. This preparation method has the advantages of simple process and wide availability of raw materials. While greatly improving the flavor characteristics of refined products, it also effectively realizes the resource utilization of tobacco scraps.

[0023] 3) Based on the excellent technical effects of the above-mentioned multi-component composite refined product, the application of it as a flavoring agent in heated cigarettes can effectively improve the sensory quality of heated cigarettes. According to GC-MS testing, the total amount of aroma substances in the refined product includes more than 30 kinds in 5 categories. According to sensory test analysis, the heated cigarettes using the refined product of this invention have a rich and mellow aroma, high richness, significantly increased smoke concentration, more comfortable strength, more delicate and mellow smoke, significantly improved aftertaste, and greatly improved consistency of aroma and smoke. Attached Figure Description

[0024] Figure 1 SPME / GC-MS analysis chromatograms of tobacco pyrolysis products obtained at different pyrolysis temperatures provided in the embodiments of the present invention;

[0025] Wherein, 1- is unheated tobacco powder extract, 2- is tobacco powder purified by dry distillation at 150℃, 3- is tobacco powder purified by dry distillation at 200℃, 4- is tobacco powder purified by dry distillation at 230℃, and 5- is tobacco powder purified by dry distillation at 250℃. Detailed Implementation

[0026] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without making inventive steps are within the scope of protection of the present invention.

[0027] Example 1

[0028] 1 kg of tobacco powder was placed in a high-temperature dry distillation reactor and heated at 80°C in a sealed container for 1 hour. After cooling to room temperature, 0.7 kg of dry distilled tobacco powder was obtained. The dry distilled tobacco powder and propylene glycol were mixed evenly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 minutes. The homogenized mixture of dry distilled tobacco powder and propylene glycol was then placed in a centrifuge bottle for solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 4.2 kg of homogenized dry distilled tobacco powder extract. Molecular distillation was then carried out under conditions of vacuum of 1.0–3.0 mbar, evaporation temperature of 60–100°C, feeding rate of 2 mL / min, and scraping film speed of 300 r / min, yielding 0.6 kg of refined tobacco dry distillate. When used in heated cigarettes, it can impart a flue-cured tobacco aroma, a sweet aroma, and a hay aroma to the heated cigarettes.

[0029] Example 2

[0030] 1 kg of tobacco powder was placed in a high-temperature dry distillation reactor and heated at 150°C in a sealed container for 0.5 h. After cooling to room temperature, 0.6 kg of dry distilled tobacco powder was obtained. The dry distilled tobacco powder and propylene glycol were mixed evenly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 min. The homogenized mixture of dry distilled tobacco powder and propylene glycol was then placed in a centrifuge bottle for solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 3.5 kg of homogenized dry distilled tobacco powder extract. Molecular distillation was then carried out under conditions of vacuum of 1.0–3.0 mbar, evaporation temperature of 60–100°C, feeding rate of 2 mL / min, and scraping film speed of 300 r / min to obtain 0.5 kg of refined tobacco dry distillate. This refined tobacco product can be used in heated cigarettes to impart a flue-cured and roasted tobacco aroma.

[0031] Example 3

[0032] This embodiment is exactly the same as Embodiment 2, except that the high-temperature dry distillation heating temperature is 200℃.

[0033] Example 4

[0034] This embodiment is exactly the same as Embodiment 2, except that the high-temperature dry distillation heating temperature is 230°C.

[0035] Example 5

[0036] 1 kg of tobacco powder was placed in a high-temperature dry distillation reactor and heated at 250℃ in a sealed environment for 0.5 h. After cooling to room temperature, 0.5 kg of dry distilled tobacco powder was obtained. The dry distilled tobacco powder and propylene glycol were mixed evenly at a mass ratio of 1:10 and homogenized under high pressure at 150 bar for 60 min. The homogenized mixture of dry distilled tobacco powder and propylene glycol was then placed in a centrifuge bottle for solid-liquid separation at room temperature. After centrifugation, the supernatant was collected, yielding 2.8 kg of homogenized dry distilled tobacco powder extract. Molecular distillation was then carried out under conditions of vacuum of 1.0–3.0 mbar, evaporation temperature of 60–100℃, feeding rate of 2 mL / min, and scraping film speed of 300 r / min, yielding 0.35 kg of refined tobacco dry distillate. When used in heated cigarettes, it can impart flue-cured, roasted, nutty, and caramel-sweet aromas to the cigarettes.

[0037] Comparative Example 1

[0038] This comparative example is exactly the same as Example 1, except that no high-temperature dry distillation reaction is performed.

[0039] The present invention also performed SPME / GC-MS analysis on the purified distillates obtained in Comparative Example 1 and Examples 2-5, and the results are as follows: Figure 1 As shown in Table 1.

[0040] Table 1

[0041]

[0042] Acids

[0043]

[0044] esters

[0045]

[0046] Pyrazines

[0047]

[0048] Pyridines

[0049]

[0050] Alkaloids

[0051]

[0052] Ketones

[0053]

[0054] lactones

[0055]

[0056] alcohols

[0057]

[0058] alkenes

[0059]

[0060] Phenols

[0061]

[0062] The table shows that the types and quantities of volatile products in refined tobacco products changed significantly with increasing temperature. The highest contents of pyrazines, pyridines, and alkaloids were found in refined tobacco products from 230℃ and 250℃, approximately three times the contents of pyrazines and pyridines in refined tobacco products from 200℃, and 50-200 times the contents of untreated refined tobacco products. This indicates that heat treatment of tobacco is an effective method to increase the content of pyrazines and pyridines in refined products. The highest contents of alkaloids were found in refined tobacco products from 230℃ and 250℃, with diene nicotine, mesmin, and orthonicotine contents increasing approximately tenfold, cotinine contents increasing approximately fourfold, and nicotine contents remaining relatively similar.

[0063] The content of aroma compounds such as ketones, alcohols, and esters in the refined tobacco products processed at 200℃, 230℃, and 250℃ were all relatively high. Compared with the untreated tobacco products, the content of ketones, alcohols, and esters in the refined tobacco products increased by about 20 times, the content of dihydroactinol increased by about 4 times, and the content of 4-hydroxy-β-dihydrodamascone and limonene increased by about 1 time. Treating tobacco products at a certain temperature has a certain impact on increasing the content of aroma compounds such as ketones, alcohols, and esters in the refined tobacco products.

[0064] The content of phenolic substances in the refined tobacco products processed at 230℃ and 250℃ showed a significant increase, approximately 20 times higher than that in untreated refined tobacco products. This indicates that increased temperature has a substantial impact on the production of harmful substances such as phenols.

[0065] As the distillation temperature increases, the types and quantities of aroma components in the extract significantly increase. Distillation treatment has a positive impact on the content of organic acids, pyrazines, and pyridines in the extract. Distillation treatment can significantly increase the content of geraniol, farnesylacetone, dihydroactinol, 4-hydroxy-β-dihydrodamascone, and limonene in refined tobacco products.

[0066] This is likely because heat treatment alters the internal structure of tobacco leaves, making it easier to release aroma compounds. Simultaneously, heating allows the tobacco's own aroma compounds to undergo a non-enzymatic browning reaction, generating new aromas and enriching the effective aroma components in the tobacco leaves. The richness of aroma components in heated tobacco dust is significantly increased. After extraction and refining of the heated tobacco dust, the corresponding aroma components in the refined heated tobacco product, such as pyrazines, pyridines, alkaloids, ketones, alcohols, and esters, show a significant increase. The richness and flavor of the refined product are greatly altered, resulting in a substantial improvement in the sensory quality of heated cigarettes.

[0067] In addition, the present invention also conducted sensory evaluation tests on blank samples and Examples 1, 2 and 5, and the results are shown in Table 2.

[0068] Table 2

[0069]

[0070] 0# blank sample; 1# sheet with 2% of the dry distillation product of Example 1 added; 2# sheet with 2‰ of the dry distillation product of Example 2 added; 3# sheet with 2% of the 250 dry distillation product added.

[0071] Compared to the control, the addition of dry distilled refined products significantly increased the richness and fullness of the aroma. The smoke concentration was significantly increased, the strength was more comfortable, the smoke was more delicate and mellow, the aftertaste was significantly improved, and the consistency of aroma and smoke was improved.

[0072] Heated cigarettes, operating at temperatures between 200-300℃, have fewer characteristic aroma components. Adding refined heated tobacco products effectively improves the lack of aroma and thin base of the cigarette sheet itself, resulting in a base sheet with better aroma and different styles. Adding tobacco refined products at different heating temperature ranges during the flavoring process further enhances the roasting, caramelizing, and smoky aromas of heated cigarettes, significantly improving the sensory quality of the product. This is related to the higher mass fractions of pyridines, pyrazines, ketones, and alcohols in heated cigarettes.

Claims

1. A method for preparing tobacco dry distillation refined product, characterized in that: The tobacco raw material is subjected to dry distillation to obtain dry distilled tobacco. The dry distilled tobacco is mixed with a solvent and homogenized. After solid-liquid separation, the supernatant is collected to obtain the dry distilled tobacco extract. The dry distilled tobacco extract is subjected to molecular distillation, and the light component fraction is collected to obtain the final product.

2. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The tobacco raw material is at least one of tobacco, burley tobacco and cigar tobacco, and its morphology is tobacco shreds and / or tobacco powder.

3. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The process of the dry distillation reaction is as follows: tobacco raw materials are placed in a high-temperature dry distillation reactor and heated in a sealed environment at 80-300°C for 0.5-2 hours.

4. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The solvent is at least one of deionized water, ethanol, and propylene glycol; the mass ratio of the dry distillation fume to the solvent is 1:6 to 10.

5. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The homogenization method is high-pressure homogenization, and the conditions are: after the dry distillation fume and solvent are mixed evenly, homogenize at a pressure of 100-150 bar for 40-60 min.

6. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The solid-liquid separation method is centrifugal separation, and the conditions are: centrifugation at 3000-500 rpm for 5-10 minutes at room temperature.

7. The method for preparing tobacco dry distillation refined product according to claim 1, characterized in that: The conditions for molecular distillation are: vacuum degree of 1.0 to 3.0 mbar, temperature of 60 to 100 °C, feeding rate of 2 to 6 mL / min, and scraping rate of 200 to 300 r / min.

8. A tobacco dry distillation refined product, characterized in that: Prepared by the method described in any one of claims 1 to 7.

9. A tobacco dry distillation refined product according to claim 8, characterized in that: The main aroma compounds in the dry distillation product include pyrazines, pyridines, and alkaloids.

10. The application of the tobacco dry distillation refined product according to claim 8, characterized in that: As a flavoring agent for heated tobacco products.

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