Preparation method and application of tobacco absolute
The process of expansive tank deposits through molecular distillation technology is used to prepare high-quality tobacco clean oil, which solves the problems of low aroma components and high odors in the existing extraction methods, and achieves efficient tobacco fragrance enrichment and odor removal. Suitable for the production of tobacco products.
Patent Information
- Application Number
- CN202411382692.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-30
- Publication Date
- 2024-12-31
AI Technical Summary
The existing tobacco extraction methods have problems such as low content of aroma-causing ingredients, many odorous substances, and unstable quality. The molecular distillation technology has high requirements for material applicability, which can easily lead to contamination of the equipment and condensation surface.
Molecular distillation technology is used to process the tank deposits of the expanded silk process. The tobacco oil is prepared by ethanol dissolution, low-temperature wax analysis, vacuum suction filtration and rotary evaporation concentration, combined with the feed speed of the molecular distillation equipment and the scraper rotation speed adjustment, tobacco clean oil is prepared, avoiding complexity. The sugar removal step enriches fragrance-making ingredients and removes odorous substances.
It has achieved the preparation of high-quality tobacco clean oil, improved the fragrance-making effect, and is suitable for molecular distillation equipment, removes odor substances, and improves the aroma quality of tobacco products.
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Figure CN119214350A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of tobacco flavor extracts, and in particular to a preparation method of tobacco absolute oil and its application. Background Art
[0002] In order to reduce the tar content of cigarettes and improve the quality of tobacco, carbon dioxide expansion tobacco technology has been widely used in the tobacco industry. In the process of cold-end impregnation of tobacco with carbon dioxide expansion, the carbon dioxide liquid is pumped from the process tank to the impregnator located at a high place. After the impregnation is completed, the carbon dioxide liquid flows back to the process tank by its own gravity. Due to the repeated recycling of carbon dioxide liquid, impurities including tobacco oil and tobacco dust gradually form muddy tobacco scale, which is deposited at the bottom of the process tank, which will have an adverse effect on production. Therefore, the process tank needs to be emptied and cleaned regularly. During this process, solvent extraction of the chemical components of tobacco by liquid carbon dioxide occurs at the same time. Although the sediment in the expanded process tank is enriched with a large amount of tobacco flavor components, it is still treated as waste and is not further utilized.
[0003] Tobacco extract is an effective way to make up for the original aroma of tobacco by separating and extracting the natural aroma components in tobacco leaves and using them as additives for cigarette flavoring. However, conventional separation and extraction methods have problems such as low content of aroma components, many unpleasant odor substances, and unstable quality. Therefore, there is an urgent need for a separation and extraction method that can highly enrich the aroma components in tobacco and remove the unpleasant odor substances in the extract.
[0004] Molecular distillation technology is a liquid-liquid separation technology carried out under high vacuum conditions, with the characteristics of low distillation temperature, high vacuum, short material heating time, and high separation degree. This technology is particularly suitable for the separation of high boiling point, heat-sensitive and easily oxidizable materials, and has great advantages in the separation and purification of natural products. However, molecular distillation technology has high requirements for the applicability of materials. The tobacco extract obtained by conventional extraction methods has a high sugar content and poor fluidity under high vacuum, which can easily cause problems such as coking of molecular distillation equipment and contamination of the condensation surface. Summary of the invention
[0005] In order to solve the above technical problems, the present application provides a method for preparing tobacco oil using the sediment of a fiber expansion process tank and its application. The method provided in the present application can be applied to molecular distillation equipment without complicated sugar removal steps, and the prepared tobacco extract has a good aroma effect.
[0006] The present application provides the use of a fiber expansion process tank sediment in the preparation of tobacco clean oil or tobacco products, wherein the tobacco products include at least one of cigarettes, cigars, shredded tobacco, redried tobacco leaves or tobacco leaves.
[0007] The present application provides a method for preparing tobacco clean oil, which comprises subjecting the sediment of a fiber expansion process tank to molecular distillation separation to obtain tobacco clean oil.
[0008] The present application provides the application of the above-mentioned preparation method in the production of tobacco products.
[0009] The beneficial effects brought about by this specification include but are not limited to: (1) The method provided in this application uses a molecular distillation technology to treat the sediment of the expanded fiber process tank to prepare tobacco pure oil. It is the first time that the molecular distillation technology is used to separate the sediment of the expanded fiber process tank, turning the process waste of expanded tobacco into treasure. (2) The method provided in this application uses a molecular distillation technology to treat the sediment of the expanded fiber process tank to prepare tobacco pure oil. It does not require a complicated sugar removal step and can be applied to molecular distillation equipment. (3) The method provided in this application uses a molecular distillation technology to treat the sediment of the expanded fiber process tank to prepare tobacco pure oil. It enriches the beneficial aroma components in the crude tobacco extract, removes the unpleasant odor substances that are not conducive to the senses while ensuring high efficiency, and obtains high-quality tobacco-derived flavors. BRIEF DESCRIPTION OF THE DRAWINGS
[0010] The present application will be further described in the form of exemplary embodiments, which will be described in detail with reference to the accompanying drawings. These embodiments are not restrictive, and include:
[0011] Figure 1 The present invention is a process flow chart for preparing tobacco extract according to some embodiments of the present application. DETAILED DESCRIPTION
[0012] In order to more clearly illustrate the technical solutions of the embodiments of this specification, the following is a brief introduction to the drawings required for the description of the embodiments. Obviously, the drawings described below are only some examples or embodiments of this specification. For ordinary technicians in this field, this specification can also be applied to other similar scenarios based on these drawings without creative work. Unless it is obvious from the language environment or otherwise explained, the same reference numerals in the figures represent the same structure or operation.
[0013] As shown in this specification and claims, unless the context clearly indicates an exception, the words "a", "an", "an" and / or "the" do not refer to the singular and may also include the plural. Generally speaking, the terms "comprise" and "include" only indicate the inclusion of the steps and elements that have been clearly identified, and these steps and elements do not constitute an exclusive list. The method or device may also include other steps or elements.
[0014] Flowcharts are used in this specification to illustrate the operations performed by the system according to the embodiments of this specification. It should be understood that the preceding or following operations are not necessarily performed precisely in order. Instead, the steps may be processed in reverse order or simultaneously. At the same time, other operations may also be added to these processes, or one or more operations may be removed from these processes.
[0015] The present application provides the use of a fiber expansion process tank sediment in the preparation of tobacco clean oil or tobacco products, wherein the tobacco products include at least one of cigarettes, cigars, shredded tobacco, redried tobacco leaves or tobacco leaves.
[0016] The present application also provides a method for preparing tobacco clean oil, which is characterized in that the sediment of the fiber expansion process tank is subjected to molecular distillation separation to obtain tobacco clean oil.
[0017] In some embodiments, the method for preparing tobacco oil may specifically include the following steps:
[0018] a Pre-treatment: dissolving the sediment in the fiber expansion process tank with ethanol, performing low-temperature wax precipitation, vacuum filtration and rotary evaporation concentration to obtain crude tobacco oil;
[0019] b. Desolventization: Pour the crude tobacco oil into the molecular distillation equipment, adjust the feed rate to 50-150 mL / h, and the scraper speed to 200-300 r / min to obtain the heavy component A2;
[0020] c Distillation: pour the heavy component A2 back into the feed tank, the feed rate is 50-150 mL / h, the scraper speed is 200-300 r / min, and the tobacco oil is obtained.
[0021] In some embodiments, the pre-treatment may specifically include the following steps: mixing the sediment from the fiber expansion tank with ethanol, allowing the mixture to stand overnight, collecting the filtrate, and evaporating and concentrating the mixture to obtain a crude tobacco oil.
[0022] In certain embodiments, the ethanol concentration can be 70% to 100%. For example, the ethanol concentration can be about 70%, 72%, 74%, 76%, 78%, 80%, 82%, 84%, 86%, 88%, 90%, 92%, 94%, 96%, 98% or 100%. Also included are any ranges characterized by a combination of the above end values, which will not be repeated here. In certain embodiments, preferably, the ethanol concentration can be 100%.
[0023] In some embodiments, the mass ratio of the sediment in the fiber expansion process tank to ethanol may be 1:(2-3). In some embodiments, preferably, the mass ratio of the sediment in the fiber expansion process tank to ethanol may be 1:2.
[0024] In some embodiments, the temperature of the overnight standing can be -5 to 5°C. For example, the temperature of the overnight standing can be about -5, -4, -3, -2, -1, 0, 1, 2, 3, 4 or 5°C. Any range characterized by a combination of the above end values is also included, which will not be repeated here. In some embodiments, preferably, the temperature of the overnight standing can be 5°C.
[0025] In some embodiments, the evaporation concentration temperature may be 50 to 60° C. For example, the evaporation concentration temperature may be about 50, 52, 54, 56, 58 or 60° C. Any range characterized by a combination of the above end values is also included, which will not be repeated here. In some embodiments, preferably, the evaporation may be rotary evaporation. In some embodiments, more preferably, the rotary evaporation temperature may be 55° C.
[0026] In some embodiments, the desolvation step may include the following features:
[0027] The vacuum degree is 50-150 mbar, for example, 60-140 mbar, 70-130 mbar, 80-120 mbar, 90-110 mbar, 90-100 mbar;
[0028] and / or, the feed temperature is 20-40°C, for example, 22-38°C, 24-36°C, 26-34°C, 28-32°C, 30-32°C;
[0029] and / or, the temperature of the heavy component is 55 to 75°C, for example, 57 to 73°C, 59 to 71°C, 61 to 69°C, 63 to 67°C, 65 to 67°C;
[0030] and / or, the main evaporator temperature is 60-100° C., for example, 62-98° C., 64-96° C., 66-94° C., 68-92° C., 70-90° C., 72-88° C., 74-86° C., 76-84° C., 78-82° C., 80-82° C.;
[0031] and / or, the light component temperature is 2 to 8°C, for example, 3 to 7°C, 4 to 6°C, 5 to 6°C;
[0032] and / or, the feed rate is 50 to 150 mL / h, for example, 60 to 140 mL / h, 70 to 130 mL / h, 80 to 120 mL / h, 90 to 110 mL / h, 100 to 110 mL / h;
[0033] And / or, the scraper speed is 200-300 r / min, for example, 210-290 r / min, 220-280 r / min, 230-270 r / min, 240-260 r / min, 250-260 r / min.
[0034] In some embodiments, the desolvation step includes the following features:
[0035] The vacuum degree is 100mbar,
[0036] and / or, feed temperature 30°C;
[0037] and / or, the temperature of the heavy component is 65°C;
[0038] and / or, main evaporator temperature 80°C;
[0039] and / or, light component temperature 5°C;
[0040] and / or, the feed rate is 100 mL / h;
[0041] And / or, the scraper speed is 250r / min.
[0042] In some embodiments, the tobacco clean oil includes a first tobacco clean oil and a second tobacco clean oil.
[0043] In some embodiments, the distillation includes a first distillation and a second distillation.
[0044] In some embodiments, preferably, the first distillation step includes the following features:
[0045] Vacuum degree 0.001~0.004mbar, for example, 0.002~0.003mbar;
[0046] and / or, the feed temperature is 30-70°C, for example, 32-68°C, 34-66°C, 36-64°C, 38-62°C, 40-60°C, 42-58°C, 44-56°C, 46-54°C, 48-52°C, 50-52°C;
[0047] and / or, the recombinant temperature is 50-90°C, for example, 52-88°C, 54-86°C, 56-84°C, 60-82°C, 62-80°C, 64-78°C, 66-76°C, 68-74°C, 70-72°C;
[0048] and / or, the main evaporator temperature is 80-100° C., for example, 82-98° C., 84-96° C., 86-94° C., 88-92° C., 90-92° C.;
[0049] and / or, the light component temperature is 12 to 20°C, for example, 14 to 18°C, 16 to 18°C;
[0050] and / or, the feed rate is 50 to 150 mL / h, for example, 55 to 145 mL / h, 60 to 140 mL / h, 65 to 135 mL / h, 70 to 130 mL / h, 75 to 125 mL / h, 80 to 120 mL / h, 85 to 115 mL / h, 90 to 110 mL / h, 95 to 105 mL / h, 100 to 105 mL / h;
[0051] and / or, the scraper speed is 200-300 r / min, for example, 210-290 r / min, 220-280 r / min, 230-270 r / min, 240-260 r / min, 250-260 r / min;
[0052] And / or, the heavy component A2 is poured back into the feed tank to obtain the heavy component H2 and the light component D2, wherein the light component D2 is the first tobacco clean oil.
[0053] In some embodiments, preferably, the second distillation step includes the following features:
[0054] Vacuum degree 0.001~0.004mbar, for example, 0.002~0.003mbar;
[0055] and / or, the feed temperature is 50-80°C, for example, 52-78°C, 54-76°C, 56-74°C, 58-72°C, 60-70°C, 62-68°C, 64-66°C;
[0056] and / or, the recombinant temperature is 50-90°C, for example, 52-88°C, 54-86°C, 56-84°C, 58-82°C, 60-80°C, 62-78°C, 64-76°C, 66-74°C, 68-72°C, 70-72°C;
[0057] and / or, the main evaporator temperature is 100-110° C., for example, 102-108° C., 104-106° C.;
[0058] and / or, the light component temperature is 10-30°C, for example, 12-28°C, 14-26°C, 16-24°C, 18-22°C, 20-22°C;
[0059] and / or, the feed rate is 50 to 150 mL / h, for example, 55 to 145 mL / h, 60 to 140 mL / h, 65 to 135 mL / h, 70 to 130 mL / h, 75 to 125 mL / h, 80 to 120 mL / h, 85 to 115 mL / h, 90 to 110 mL / h, 95 to 105 mL / h, 100 to 105 mL / h;
[0060] and / or, the scraper speed is 200-300 r / min, for example, 210-290 r / min, 220-280 r / min, 230-270 r / min, 240-260 r / min, 250-260 r / min;
[0061] And / or, the heavy component H2 is poured back into the feed tank to obtain the light component D3, and the light component D3 is the second tobacco clean oil.
[0062] In some embodiments, more preferably, the first distillation step comprises the following features:
[0063] Vacuum degree 0.002mbar,
[0064] and / or, feed temperature 50°C;
[0065] and / or, the temperature of the heavy component is 70°C;
[0066] and / or, main evaporator temperature 90°C;
[0067] and / or, light component temperature 16°C;
[0068] and / or, the feed rate is 100 mL / h;
[0069] and / or, the scraper speed is 250r / min;
[0070] And / or, the heavy component A2 is poured back into the feed tank to obtain the heavy component H2 and the light component D2, wherein the light component D2 is the first tobacco clean oil.
[0071] In some embodiments, more preferably, the second distillation step comprises the following features:
[0072] Vacuum degree 0.002mbar,
[0073] and / or, feed temperature 65°C,
[0074] and / or, the temperature of the heavy component is 70°C,
[0075] and / or, main evaporator temperature 105°C,
[0076] and / or, light component temperature 20°C,
[0077] and / or, the feed rate is 100 mL / h,
[0078] and / or, the scraper speed is 250r / min,
[0079] And / or, the heavy component H2 is poured back into the feed tank to obtain the light component D3, and the light component D3 is the second tobacco clean oil.
[0080] The present application also provides the application of the above-mentioned preparation method in the production of tobacco products.
[0081] The experimental methods in the following examples are conventional methods unless otherwise specified. The experimental materials used in the following examples are purchased from conventional biochemical reagent companies unless otherwise specified. The quantitative tests in the following examples are repeated three times, and the results are averaged.
[0082] Example 1
[0083] 1 Experimental Materials and Methods
[0084] Materials and instruments
[0085] Sediment from the fiber expansion tank (Shanghai Cigarette Factory fiber expansion workshop); anhydrous ethanol (J&K); α-ionone internal standard working solution (11.2 μg / mL, cyclohexane solution), BSTFA-TMCS (99:1) derivatization reagent (Sigma Aldrich), DMF solution containing n-heptadecane internal standard (0.3 mg / mL), n-hexane (J&K), methyl tert-butyl ether (J&K)
[0086] Molecular distillation instrument (Germany VTA, VKL70-5FDRR); rotary evaporator (Germany ); GC / MS (Agilent, USA); Large volume injection-GC / MS (Agilent, USA)
[0087] Test methods
[0088] 1.2.1 Analysis of carbohydrate components (silylation-GC / FID)
[0089] Accurately weigh 10.0 mg of common tobacco pure oil sample or expanded fiber process tank sediment sample, add 0.5 mL of internal standard extraction solution and 0.5 mL of derivatization reagent, vortex and oscillate for extraction. Heat in a 70°C oven for 30 minutes, place in a drying dish for more than 6 hours, centrifuge and take the supernatant for GC / FID analysis.
[0090] Chromatographic column: Restek Rtx-1 capillary column (30m×0.25mm×0.5um); injection volume 1uL, split ratio 20:1; inlet temperature: 280℃; carrier gas He gas, constant flow rate 1.5mL / min; temperature program: 125℃, hold for 5min; 2.5℃ / min to 210℃, 10℃ / min to 300℃, hold for 15min; FID temperature 300℃; H2 constant flow: 40mL / min; air constant flow: 400mL / min; carrier gas N2: 45ml / min; signal acquisition: 50Hz / 0.004min, save mode.
[0091] After measurement, the mass fractions of glucose, fructose and sucrose in ordinary tobacco pure oil samples were 7.6%, 3.1% and 0.1% respectively, while the mass fractions of glucose, fructose and sucrose in the sediment sample of the expanded silk process tank were 0.03%, 0.11% and 0.16% respectively. This is because carbon dioxide is a non-polar solvent and sugar substances are difficult to dissolve in carbon dioxide. Molecular distillation usually requires that the mass fraction of sugar substances in the raw materials be below 2.5%. Therefore, after the sediment of the expanded silk process tank is purified and impurities are removed, it can be applied to molecular distillation technology for further refining.
[0092] Example 2 - Preparation of D2 Absolute Oil by One Molecular Distillation Process
[0093] Take 1.0 kg of the sediment from the fiber expansion process tank, slowly add 2.0 kg of anhydrous ethanol to dissolve it, stir it evenly to obtain a sediment solution, put it in a 5°C refrigerator for low-temperature wax precipitation and let it stand overnight, filter it using vacuum filtration and collect the filtrate, and use a rotary evaporator to remove the solvent ethanol at a temperature of 55°C to obtain a concentrate A0, about 300 mL, with a yield of 30.6% (calculated based on the mass of the sediment from the fiber expansion process tank).
[0094] Using concentrate A0 as raw material, molecular distillation refining is carried out. The specific process steps and parameters are as follows:
[0095] Desolventization: Adjust the instrument vacuum to 100.0 mbar, feed temperature to 30.0°C, heavy component temperature to 65.0°C, main evaporator temperature to 80.0°C, and light component temperature to 5.0°C. Pour the concentrate A0 into the feed tank, adjust the feed rate to 100 mL / h, and the scraper speed to 250 r / min to obtain the light component (solvent) and heavy component A2.
[0096] Primary distillation: adjust the instrument vacuum degree to 0.002mbar, feed temperature to 50.0℃, heavy component temperature to 70.0℃, main evaporator temperature to 90.0℃, light component temperature to 16.0℃. Pour the heavy component A2 back into the feed tank, adjust the feed rate to 100mL / h, and the scraper speed to 250r / min, to obtain the primary heavy component H2 and the primary light component D2, and record the primary light component D2 as D2 net oil, with a yield of 1.6% (calculated based on the mass of the concentrate A0)
[0097] Table 1 Main process parameters of primary molecular distillation
[0098]
[0099] Example 3 - Preparation of D3 Absolute Oil by Secondary Molecular Distillation Process
[0100] Take 1.0 kg of the sediment from the fiber expansion tank, slowly add 2.0 kg of anhydrous ethanol to dissolve it, stir it evenly to obtain a sediment solution, put it in a 5°C refrigerator and let it stand overnight, filter it using vacuum filtration and collect the filtrate, and remove the solvent using a rotary evaporator to obtain a concentrate A0, about 300 mL, with a yield of 30.6% (calculated based on the mass of the sediment from the fiber expansion tank).
[0101] Using concentrate A0 as raw material, molecular distillation refining is carried out. The specific process steps and parameters are as follows:
[0102] Desolventization: Adjust the instrument vacuum to 100.0 mbar, feed temperature to 30.0°C, heavy component temperature to 65.0°C, main evaporator temperature to 80.0°C, and light component temperature to 5.0°C. Pour the concentrate A0 into the feed tank, adjust the feed rate to 100 mL / h, and the scraper speed to 250 r / min to obtain the light component (solvent) and heavy component A2.
[0103] Primary distillation: adjust the instrument vacuum degree to 0.002mbar, feed temperature to 50.0℃, heavy component temperature to 70.0℃, main evaporator temperature to 90.0℃, light component temperature to 16.0℃. Pour the heavy component A2 back into the feed tank, adjust the feed rate to 100mL / h, and the scraper speed to 250r / min to obtain the primary heavy component H2 and the primary light component D2.
[0104] Secondary distillation: adjust the instrument vacuum degree to 0.002mbar, feed temperature to 65.0℃, heavy component temperature to 70.0℃, main evaporator temperature to 105.0℃, light component temperature to 20.0℃. Pour the heavy component H2 back into the feed tank, adjust the feed rate to 100mL / h, and the scraper speed to 250r / min, to obtain secondary heavy component H3 and secondary light component D3, and record the secondary light component D3 as D3 net oil, with a yield of 8.3% (calculated based on the mass of concentrate A0).
[0105] Table 2 Main process parameters of secondary molecular distillation
[0106]
[0107] Example 4
[0108] Volatile and semi-volatile component analysis (GC / MS):
[0109] Take 500 mg of each sample of concentrate A0, D2 light component, H2 heavy component, D3 light component H3 heavy component, add 5 ml of anhydrous ethanol to dissolve, then add 200 μL of positioning internal standard solution, filter and perform GC / MS detection, use library retrieval method combined with relevant literature for qualitative analysis, and use chromatographic peak area normalization method to quantitatively calculate the relative percentage content of each aroma component. Chromatographic column: DB-5MS capillary column (30m×0.25mm×0.25μm); carrier gas: helium (≥99.999%); constant flow mode flow rate: 1.5mL / min; injection volume 2μL, temperature program: keep at 40℃ for 5min, increase to 250℃ at a rate of 3.5℃ / min, increase to 280℃ at a rate of 40℃ / min and keep for 10min. Mass spectrometer transmission line temperature: 280°C; electron energy: 70 eV; EI source temperature: 230°C; quadrupole temperature: 150°C; mass scanning range: 33-400 amu.
[0110] Neutral aroma component analysis (large volume injection GC / MS):
[0111] Take 50 mg of each sample of concentrate A0, D2 light component, H2 heavy component, D3 light component and H3 heavy component, add 5 ml of extraction solvent (a mixture of n-hexane and methyl tert-butyl ether in a volume ratio of 1:1) to dissolve, then add 200 μL of 11.2 μg / mL α-ionone internal standard solution, vortex and let stand overnight, centrifuge and take the supernatant for large volume injection-GC / MS analysis.
[0112] The method for neutral aroma components is to use the Nist library search method for qualitative analysis and the internal standard method for quantitative analysis. Large volume injection-GC / MS injection volume is 10uL, with EPC backflush device. Chromatographic column: DB-5MS capillary column (30m×0.25mm×0.25μm); carrier gas: helium (≥99.999%); constant flow mode flow rate: 2mL / min; injection port: keep at 50℃ for 0.1min, increase to 250℃ at a rate of 500℃ / min for 60min, increase to 350℃ at a rate of 500℃ / min for 20min; temperature program: keep at 40℃ for 3min, increase to 100℃ at a rate of 10℃ / min, increase to 250℃ at a rate of 3℃ / min for 1min, and then increase to 300℃ at a rate of 20℃ / min for 20min. Mass spectrometer interface temperature: 230°C; electron energy: 70 eV; EI source temperature: 230°C; quadrupole temperature: 150°C; mass scanning range: 33-500 amu.
[0113] Table 3 GC / MS component analysis results of neutral aroma components in sediments before and after molecular distillation
[0114]
[0115] A total of 67 components were detected from the sediment of the tobacco expansion process tank by GC / MS method, and 17 important aroma components in tobacco were analyzed in detail. In addition to the highest content of neophytadiene, it also contains damascenone methylcyclopentenolone, geranyl acetone, benzyl alcohol, phenylethyl alcohol, norsolanadione, megastigmatrienol, 2,3'-bipyridine, 3-hydroxy-β-dihydrodamascenone, cephariol, dihydroactin, farnesyl acetone and other common aroma components in tobacco. After molecular distillation enrichment, the enrichment multiples in the D2 and D3 light component fractions can reach dozens of times.
[0116] Sensory quality evaluation:
[0117] The concentrates A0, D2 pure oil and D3 pure oil were diluted with 75% ethanol respectively and injected into blank cigarettes at an addition amount of 10 mg / kg to obtain test cigarette samples. The cigarettes injected with the same amount of 75% ethanol were used as control cigarette samples. The sensory quality evaluation was carried out by the comparative method, and the evaluation team was composed of personnel with smoking evaluation qualifications in the flavoring room of the technical center.
[0118] Table 4 Evaluation of flavoring of different fractions of molecular distillation
[0119]
[0120] Concentrate A0 has the effects of enhancing aroma quality, increasing aroma volume, masking impurities, increasing smoke concentration, reducing irritation, reducing residue and increasing oral sweetness.
[0121] D2 absolute oil has an elegant, sweet aroma, which can significantly improve the aroma quality of cigarette smoke, cover up impurities, slightly increase the concentration and strength, and significantly increase the sweetness in the mouth.
[0122] D3 absolute oil has a good sweet aroma and tobacco flavor, and the aroma volume and smoke concentration of cigarettes are significantly increased, but its contribution to the sweetness in the mouth is slightly less than that of the D2 fraction, and the irritation is slightly increased.
[0123] In summary, the D2 fraction has the best smoking effect, and the D3 fraction also has a good smoking effect, both of which are significantly better than A0. The reason is that the aroma components related to the fragrance are usually relatively volatile, so they are mainly enriched in the D2 and D3 fractions. And with the increase in the intensity of molecular distillation, the fragrance in the smoke gradually decreases. The comprehensive yields of D2 and D3 absolute oils are 1.6% and 8.3% respectively. Considering comprehensively, the D3 fraction has the best smoking effect as a tobacco flavor.
[0124] The basic concepts have been described above. Obviously, for those skilled in the art, the above detailed disclosure is only for example and does not constitute a limitation of this specification. Although not explicitly stated here, those skilled in the art may make various modifications, improvements and corrections to this specification. Such modifications, improvements and corrections are suggested in this specification, so such modifications, improvements and corrections still belong to the spirit and scope of the exemplary embodiments of this specification.
[0125] At the same time, this specification uses specific words to describe the embodiments of this specification. For example, "one embodiment", "an embodiment", and / or "some embodiments" refer to a certain feature, structure or characteristic related to at least one embodiment of this specification. Therefore, it should be emphasized and noted that "one embodiment" or "an embodiment" or "an alternative embodiment" mentioned twice or more in different positions in this specification does not necessarily refer to the same embodiment. In addition, certain features, structures or characteristics in one or more embodiments of this specification can be appropriately combined.
[0126] In some embodiments, numbers describing the number of components and attributes are used. It should be understood that such numbers used in the description of the embodiments are modified by the modifiers "about", "approximately" or "substantially" in some examples. Unless otherwise specified, "about", "approximately" or "substantially" indicate that the numbers are allowed to vary by ±20%. Accordingly, in some embodiments, the numerical parameters used in the specification and claims are approximate values, which may change according to the required features of individual embodiments. In some embodiments, the numerical parameters should take into account the specified significant digits and adopt the general method of retaining digits. Although the numerical domains and parameters used to confirm the breadth of their range in some embodiments of this specification are approximate values, in specific embodiments, the setting of such numerical values is as accurate as possible within the feasible range.
[0127] Finally, it should be understood that the embodiments described in this specification are only used to illustrate the principles of the embodiments of this specification. Other variations may also fall within the scope of this specification. Therefore, as an example and not a limitation, alternative configurations of the embodiments of this specification may be considered consistent with the teachings of this specification. Accordingly, the embodiments of this specification are not limited to the embodiments explicitly introduced and described in this specification.
Claims
1. Application of the sediment of the tobacco expansion process tank in the preparation of tobacco clean oil or tobacco products, wherein the tobacco products include at least one of cigarettes, cigars, shredded tobacco, redried tobacco leaves or tobacco leaves.
2. A method for preparing tobacco oil, characterized in that: The sediment from the tobacco expansion process tank is separated by molecular distillation to obtain tobacco clean oil.
3. The preparation method according to claim 2, characterized in that: The specific steps include: a Pre-treatment: dissolving the sediment in the fiber expansion process tank with ethanol, performing low-temperature wax precipitation, vacuum filtration and rotary evaporation concentration to obtain crude tobacco oil; b. Desolventization: Pour the crude tobacco oil into the molecular distillation equipment, adjust the feed rate to 50-150 mL / h, and the scraper speed to 200-300 r / min to obtain the heavy component A2; c Distillation: pour the heavy component A2 back into the feed tank, the feed rate is 50-150 mL / h, the scraper speed is 200-300 r / min, and the tobacco oil is obtained.
4. The preparation method according to claim 1, characterized in that: The pretreatment specifically comprises the following steps: mixing the sediment from the fiber expansion process tank with ethanol, leaving it to stand overnight, collecting the filtrate, and evaporating and concentrating it to obtain a crude tobacco oil.
5. The preparation method according to claim 4, characterized in that: The ethanol concentration is 70% to 100%, preferably, the ethanol concentration is 100%; The mass ratio of the sediment in the fiber expansion process tank to ethanol is 1:(2-3), preferably, the mass ratio of the sediment in the fiber expansion process tank to ethanol is 1:2; The temperature of the overnight standing is -5 to 5°C, preferably, the temperature of the overnight standing is 5°C; The evaporation concentration temperature is 50-60°C. Preferably, the evaporation is rotary evaporation. More preferably, the rotary evaporation temperature is 55°C.
6. The preparation method according to claim 3, characterized in that: The desolventizing step includes the following features: Vacuum degree is 50~150mbar; and / or, the feed temperature is 20 to 40°C; and / or, the temperature of the heavy component is 55 to 75°C; and / or, the main evaporator temperature is 60-100°C; and / or, the light component temperature is 2 to 8°C; and / or, the feed rate is 50 to 150 mL / h; And / or, the scraper speed is 200-300 r / min.
7. The preparation method according to claim 3, characterized in that: The desolventizing step includes the following features: The vacuum degree is 100mbar, and / or, feed temperature 30°C; and / or, the temperature of the heavy component is 65°C; and / or, main evaporator temperature 80°C; and / or, light component temperature 5°C; and / or, the feed rate is 100 mL / h; And / or, the scraper speed is 250r / min.
8. The preparation method according to claim 3, characterized in that: The tobacco clean oil includes a first tobacco clean oil and a second tobacco clean oil; The distillation comprises a first distillation and a second distillation; Preferably, the first distillation step comprises the following features: Vacuum degree 0.001~0.004mbar; and / or, the feed temperature is 30 to 70° C.; and / or, the temperature of the heavy component is 50 to 90°C; and / or, the main evaporator temperature is 80-100°C; and / or, the light component temperature is 12-20°C; and / or, the feed rate is 50 to 150 mL / h; and / or, the scraper speed is 200-300 r / min; and / or, pouring the heavy component A2 back into the feed tank to obtain the heavy component H2 and the light component D2, wherein the light component D2 is the first tobacco clean oil; Preferably, the second distillation step comprises the following features: Vacuum degree 0.001~0.004mbar; and / or, the feed temperature is 50 to 80°C; and / or, the temperature of the heavy component is 50 to 90°C; and / or, the main evaporator temperature is 100-110°C; and / or, the light component temperature is 10 to 30°C; and / or, the feed rate is 50 to 150 mL / h; and / or, the scraper speed is 200-300 r / min; And / or, the heavy component H2 is poured back into the feed tank to obtain the light component D3, and the light component D3 is the second tobacco clean oil.
9. The preparation method according to claim 8, characterized in that: The first distillation step includes the following features: Vacuum degree 0.002mbar, and / or, feed temperature 50°C; and / or, the temperature of the heavy component is 70°C; and / or, main evaporator temperature 90°C; and / or, light component temperature 16°C; and / or, the feed rate is 100 mL / h; and / or, the scraper speed is 250r / min; and / or, pouring the heavy component A2 back into the feed tank to obtain the heavy component H2 and the light component D2, wherein the light component D2 is the first tobacco clean oil; The second distillation step includes the following features: Vacuum degree 0.002mbar, and / or, feed temperature 65°C, and / or, the temperature of the heavy component is 70°C, and / or, main evaporator temperature 105°C, and / or, light component temperature 20°C, and / or, the feed rate is 100 mL / h, and / or, the scraper speed is 250r / min, And / or, the heavy component H2 is poured back into the feed tank to obtain the light component D3, and the light component D3 is the second tobacco clean oil.
10. Use of the preparation method according to any one of claims 2 to 9 in the production of tobacco products.
Citation Information
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