CN113498875A - Method for recovering aroma substances in reconstituted tobacco concentrated white water and application - Google Patents
Method for recovering aroma substances in reconstituted tobacco concentrated white water and application Download PDFInfo
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- CN113498875A CN113498875A CN202110778976.1A CN202110778976A CN113498875A CN 113498875 A CN113498875 A CN 113498875A CN 202110778976 A CN202110778976 A CN 202110778976A CN 113498875 A CN113498875 A CN 113498875A
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- aroma substances
- reconstituted tobacco
- white water
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/14—Forming reconstituted tobacco products, e.g. wrapper materials, sheets, imitation leaves, rods, cakes; Forms of such products
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/12—Chemical features of tobacco products or tobacco substitutes of reconstituted tobacco
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The invention relates to a method for recovering aroma substances in thick white water of reconstituted tobacco and application thereof, wherein the thick white water generated by the reconstituted tobacco is filtered by a ceramic microfiltration membrane to obtain filtrate; a series adsorption resin column formed by connecting a weak-polarity adsorption filler and a medium-polarity adsorption filler in series is used for adsorbing the filtrate so as to realize the adsorption of the aroma substances; eluting the adsorption filler with ethanol, sequentially collecting the deep red eluent at the front section, the brown red eluent at the middle section and the light yellow eluent at the rear section, and further separating and refining the eluent at the rear section. The technical scheme mainly comprises the steps of series resin adsorption, sectional collection, separation and refining of recovered components, and the economic benefit is increased; the method is simple, the resin can be regenerated and recycled, the raw materials are saved, and the cost is low.
Description
Technical Field
The invention belongs to the technical field of reconstituted tobacco processing, and particularly relates to a method for recovering aroma substances in reconstituted tobacco concentrated white water and application thereof.
Background
The paper-making reconstituted tobacco is a reconstituted tobacco finished product prepared by using water as a main extraction solvent, carrying out solid-liquid separation on soluble components and insoluble components of tobacco raw materials (such as tobacco powder, broken tobacco pieces, tobacco flakes, tobacco stems and the like), concentrating the soluble components, pulping the insoluble components, and then carrying out papermaking, coating, drying and other processes.
In the production process of the reconstituted tobacco by the paper-making method, pulp is washed before being screened and manufactured, a large amount of concentrated white water is generated in the process, volatile components in the concentrated white water are detected, and the main components are nitrogenous heterocyclic substances and other tobacco fragrance components, particularly the nicotine content is high and is about 7 times of the reconstituted tobacco extracting solution respectively. The nicotine and other tobacco aroma substances in the reconstituted tobacco dense white water can improve the strength and the original tobacco aroma of tobacco products such as reconstituted tobacco, reconstituted tobacco shredding, heated cigarettes and the like. Through the recovery of nicotine and other fragrant substances in the concentrated white water, the added value of the reconstituted tobacco production industry can be improved, and the wastewater treatment pressure of the subsequent production can be reduced.
At present, the nicotine in tobacco wastewater is recovered by a solvent extraction method, an adsorbent adsorption method and the like, and patent number CN104387365A discloses a method for extracting nicotine in tobacco wastewater, wherein organic solvent is adopted for extraction, then sulfuric acid solution is used for back extraction, and finally reduced pressure distillation is carried out to obtain nicotine sulfate. The patent No. CN105621745A discloses a method for recovering nicotine in tobacco processing wastewater, which comprises the steps of coagulating with a Ca/Mg/Al coagulant, adsorbing with an adsorbent, desorbing with an organic solvent, distilling under reduced pressure and the like, wherein in the method, pigments, acids, alcohols, esters and other substances in tobacco are easily adsorbed by the adsorbent aiming at the tobacco processing wastewater, so that the obtained nicotine has low purity. Patent No. CN 112457917A discloses a method for recovering flavor components in reconstituted tobacco condensed water, eluent formed by the method and application, and the content also relates to the recovery of flavor substances, but the adopted reverse osmosis mode can filter out partial components which have positive effects on tobacco senses, and meanwhile, the concentration of the eluent is difficult to achieve the purpose of concentrating to a certain degree and the relative separation and refining of the components. Patent No. CN 112499807 a discloses recovery of flavor components in papermaking wastewater, a trapped concentrate formed therefrom, and uses thereof, and although the content relates to recovery of flavor substances in reconstituted tobacco papermaking wastewater, components recovered by microfiltration, ultrafiltration, or reverse osmosis include components such as chloride ions, sulfate ions, phosphate ions, etc. having a high content in papermaking wastewater, which have a side effect on tobacco, and a large amount of components having a large molecular weight are removed relatively cleanly, affecting the contribution to sensory quality in use. The concentrated liquid trapped by this method is difficult to separate according to different flavors.
Disclosure of Invention
The invention provides a method for recovering aroma substances in reconstituted tobacco concentrated white water and application thereof, concentrated solutions with different aroma characteristics are obtained by further separating and refining eluent according to different elution components, and a large amount of concentrated white water can be used as production water after being recovered, so that the wastewater treatment pressure after production is reduced, and the water consumption is reduced.
In order to realize the purpose, the invention is realized by the following technical scheme:
a method for recovering aroma substances in reconstituted tobacco concentrated white water comprises the following steps:
s1, filtering thick white water generated by the reconstituted tobacco leaves through a ceramic microfiltration membrane to obtain filtrate;
s2, adopting a series adsorption resin column formed by a series connection mode of a weak-polarity adsorption filler and a medium-polarity adsorption filler to adsorb the filtrate obtained in the step S1 so as to realize the adsorption of the aroma substances;
s3, eluting the series adsorption resin column with ethanol with volume percentage of more than 95% at the flow rate of 0.5BV/h, wherein the use amount of the eluent is 2-4BV, and collecting the first 0.1-0.12BV of dark red eluent, the middle 0.1-0.12BV of brown red eluent and the last 2.8-3.8BV of light yellow eluent in turn.
Further, in step S1, the operation pressure of the filtration is 0.1-0.2MPa, and the pore diameter of the ceramic microfiltration membrane is 10 nm.
Further, in step S2, the weak polar adsorption filler is LS169A, AB-8 or X-5 adsorption resin, and the particle size is 0.3-1.25 μm.
Further, in step S2, the medium polarity adsorption filler is LS313 or ADS-17.
Further, in step S2, the aroma substances include a low-polarity aroma substance, a medium-polarity aroma substance and a high-polarity aroma substance, wherein the medium-polarity aroma substance at least includes phenethyl alcohol, furfural or nicotine, the low-polarity aroma substance at least includes megastigmatrienone, neophytadiene, actinidiolide or damascenone, and the high-polarity aroma substance is a tobacco pigment aroma substance.
Further, in step S2, the filtrate was passed through the series-connected adsorbent resin columns at a flow rate of 6-8 BV/h.
Further, a separation and refining step S4 is included after the step S3, the light yellow eluent of last 2.8-3.8BV in the step S3 is rectified, the number of theoretical plates is 10-12, the ethanol recovery temperature is 60 ℃, the rectified solution is diluted by pure water or reverse osmosis water with the volume percentage of 50-60%, and then the diluted solution is loaded into a waterproof grafted C18 filler at the flow rate of 3-4 BV/h;
s5, eluting the grafted C18 filler in the step S4 by 25 percent, 40 percent, 85 percent and 100 percent of ethanol in percentage by volume at the speed of 0.3-0.5BV/h respectively to obtain ethanol recovery solutions with different fragrances respectively; rectifying the ethanol recovery liquid with different flavors, wherein the theoretical plate number is 10-12, the ethanol recovery temperature is 60 ℃, and obtaining the separation and refining solution with different tobacco flavor characteristics.
An application of a fragrant substance in reconstituted tobacco thick white water is characterized in that an eluent obtained by any recovery method of the fragrant substance in the reconstituted tobacco thick white water is used for reconstituted tobacco.
Further, the deep red eluent of the first 0.1-0.12BV is used for improving the tobacco fragrance of the reconstituted tobacco in the concentrated solution for producing the reconstituted tobacco; the middle 0.1-0.12BV of brownish red eluent is used for improving the smoking strength and the flavor enhancement effect of the reconstituted tobacco, the reconstituted tobacco shreds, the heated cigarettes and the like; finally, the separation and refining solution of the faint yellow eluent with 2.8-3.8BV is used for flavoring functional tobacco products and special tobacco products.
The invention has the beneficial effects that:
the technical scheme not only provides a separation and refining concentrated solution which is simple and convenient to operate and can obtain different fragrance characteristics, but also can be used for process water after a large amount of concentrated white water is recovered, thereby reducing the pressure of wastewater treatment after production and reducing water consumption.
Drawings
FIG. 1 is a GC/MS total ion flow chromatogram of concentrated white water.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for describing the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
In the following examples of the present application, the used apparatuses, instruments, reagents and the like are commercially available unless otherwise specified.
The GC/MS of the concentrated white water is shown in FIG. 1.
The application provides a method for recovering aroma substances in reconstituted tobacco concentrated white water, which comprises the following steps:
1. and (3) filtering:
the concentrated white water is filtered by a ceramic microfiltration membrane, the operation pressure of the filtration is 0.1-0.2Mp, and the aperture of the ceramic microfiltration membrane is 10 nm. Aims to remove fine fibers and partial larger molecular substances in the thick white water.
2. Adsorption of aroma substances in the concentrated white water:
the adsorption is carried out by adopting an adsorption resin column formed by connecting a weak-polarity adsorption filler and a medium-polarity adsorption filler in series, so that the adsorption of medium-polarity aroma substances such as phenethyl alcohol, furfural and nicotine and the adsorption of weak-polarity aroma substances such as megastigmatrienone, neophytadiene, actinidiolide and damascenone are ensured. The low-polarity adsorption filler can be LS169A, AB-8, X-5 and other adsorption resins, the particle size is 0.3-1.25 μm, and the medium-polarity adsorption filler can be LS313, ADS-17 and other adsorption fillers. The filtrate after passing through the ceramic membrane flows through the adsorption resin columns connected in series at the flow rate of 6-8 BV/h.
3. Elution and recovery:
eluting the adsorption resin column with ethanol with volume percentage of more than 95% at the flow rate of 0.5BV/h, wherein the dosage of the eluent is 2-4 BV. Respectively and sequentially collecting the deep red eluent of the first 0.1-0.12BV, the brown red eluent of the middle 0.1-0.12BV and the light yellow eluent of the last 2.8-3.8BV in a sectional manner.
4. Concentration and separation of recovered components:
finally rectifying 2.8-3.8BV light yellow eluent, wherein the theoretical plate number is 10-12, and the ethanol recovery temperature is 60 ℃. The rectified solution is diluted by 50-60% pure water or reverse osmosis water, and then loaded into water-resistant grafting C18 filler (the filler can be AQ-2C18, SB-AQ, etc.), and loaded at the flow rate of 3-4 BV/h.
5. Separation and purification of recovered components:
eluting with 25%, 40%, 85% and 100% ethanol at 0.3-0.5BV/h to obtain ethanol recovery solutions with different flavors. Rectifying the ethanol recovery liquid with different flavors, wherein the theoretical plate number is 10-12, the ethanol recovery temperature is 60 ℃, and obtaining the separation and refining solution with different tobacco flavor characteristics.
The application also relates to application of the aroma substances in the reconstituted tobacco concentrated white water, and the deep red eluent, the brownish red eluent, the light yellow eluent or the separation and refining solution with different tobacco aroma characteristics obtained by rectifying the light yellow eluent are applied.
Use of specific recovered components:
the deep red eluent of 0.1-0.12BV before sectional collection is tobacco pigment (aroma substance with larger polarity), the main components are carotenoid and Maillard product, the deep red eluent has positive effect on the sensory quality of the cigarette, is not easy to volatilize, and can be added into the concentrated solution for producing the reconstituted tobacco to improve the tobacco fragrance of the reconstituted tobacco; the middle 0.1-0.12BV of brownish red eluent (low-polarity aroma substances) contains higher nicotine, furfural and N heterocyclic micromolecule compounds, so that the smoking strength of reconstituted tobacco, reconstituted tobacco shredding, heated cigarettes and the like can be improved, and meanwhile, the aroma-increasing effect is also realized; and finally, separating and refining the 2.8-3.8BV light yellow eluent, and according to different aroma substances, the solution can be used for developing and enhancing aroma of functional tobacco products and special tobacco products.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (9)
1. A method for recovering aroma substances in reconstituted tobacco concentrated white water is characterized by comprising the following steps:
s1, filtering thick white water generated by the reconstituted tobacco leaves through a ceramic microfiltration membrane to obtain filtrate;
s2, adopting a series adsorption resin column formed by a series connection mode of a weak-polarity adsorption filler and a medium-polarity adsorption filler to adsorb the filtrate obtained in the step S1 so as to realize the adsorption of the aroma substances;
s3, eluting the series adsorption resin column with ethanol with volume percentage of more than 95% at the flow rate of 0.5BV/h, wherein the use amount of the eluent is 2-4BV, and collecting the first 0.1-0.12BV of dark red eluent, the middle 0.1-0.12BV of brown red eluent and the last 2.8-3.8BV of light yellow eluent in turn.
2. The method for recovering the aroma substances in the reconstituted tobacco concentrated white water according to claim 1, wherein in the step S1, the filtering operation pressure is 0.1-0.2MPa, and the pore diameter of the ceramic microfiltration membrane is 10 nm.
3. The method for recovering the aroma substances in the reconstituted tobacco concentrated white water according to claim 1, wherein in the step S2, the weakly polar adsorption filler is LS169A, AB-8 or X-5 adsorption resin, and the particle size is 0.3-1.25 μm.
4. The method for recovering the aroma substances in the reconstituted tobacco concentrated white water according to claim 1, wherein in step S2, the medium-polarity adsorption filler is LS313 or ADS-17.
5. The method for recovering the aroma substances in the reconstituted tobacco concentrated white water according to claim 1, wherein in step S2, the aroma substances comprise low-polarity aroma substances, medium-polarity aroma substances and high-polarity aroma substances, wherein the medium-polarity aroma substances at least comprise phenethyl alcohol, furfural or nicotine, the low-polarity aroma substances at least comprise megastigmatrienone, neophytadiene, actinidiolide or damascone, and the high-polarity aroma substances are tobacco pigment aroma substances.
6. The method for recovering aroma substances in reconstituted tobacco concentrated white water according to claim 1, wherein in step S2, the filtrate is passed through a series-connected adsorption resin column at a flow rate of 6-8 BV/h.
7. The method for recovering the aroma substances in the reconstituted tobacco concentrated white water according to claim 1, which is characterized by further comprising a separation and refining step S4 after the step S3, wherein the light yellow eluent of last 2.8-3.8BV in the step S3 is rectified, the number of theoretical plates is 10-12, the ethanol recovery temperature is 60 ℃, and the rectified solution is diluted by pure water or reverse osmosis water with the volume percentage of 50-60%, then loaded into a waterproof grafted C18 filler and loaded at the flow rate of 3-4 BV/h;
s5, eluting the grafted C18 filler in the step S4 by 25 percent, 40 percent, 85 percent and 100 percent of ethanol in percentage by volume at the speed of 0.3-0.5BV/h respectively to obtain ethanol recovery solutions with different fragrances respectively; rectifying the ethanol recovery liquid with different flavors, wherein the theoretical plate number is 10-12, the ethanol recovery temperature is 60 ℃, and obtaining the separation and refining solution with different tobacco flavor characteristics.
8. The application of the aroma substances in the reconstituted tobacco concentrated white water is characterized in that the eluent obtained by the recovery method of the aroma substances in the reconstituted tobacco concentrated white water according to any one of claims 1 to 7 is used for the reconstituted tobacco.
9. The application of the aroma substances in the reconstituted tobacco concentrated white water according to claim 8, wherein the deep red eluent of the first 0.1-0.12BV is used for improving the tobacco aroma of the reconstituted tobacco in the reconstituted tobacco production concentrated solution; the middle 0.1-0.12BV of brownish red eluent is used for improving the smoking strength and the flavor enhancement effect of the reconstituted tobacco, the reconstituted tobacco shreds, the heated cigarettes and the like; finally, the separation and refining solution of the faint yellow eluent with 2.8-3.8BV is used for flavoring functional tobacco products and special tobacco products.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1455349A (en) * | 1973-10-11 | 1976-11-10 | Kimberly Clark Co | Method of making reconstituted tobacco having reduced nitrates |
| CN102488313A (en) * | 2011-11-27 | 2012-06-13 | 中国海诚工程科技股份有限公司 | Recycling method of coating liquid of papermaking reconstituted tobacco |
| CN103349867A (en) * | 2013-07-15 | 2013-10-16 | 河南卷烟工业烟草薄片有限公司 | Paper-making process reconstituted tobacco papermaking white water reuse treatment method |
| CN103349351A (en) * | 2013-07-24 | 2013-10-16 | 江苏久吾高科技股份有限公司 | Method for reconstituting tobacco leaves by paper making method based on membrane separation technique |
| CN112457917A (en) * | 2020-11-04 | 2021-03-09 | 上海烟草集团有限责任公司 | Method for recovering flavor components in reconstituted tobacco condensed water, eluent formed by method and application |
-
2021
- 2021-07-09 CN CN202110778976.1A patent/CN113498875B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1455349A (en) * | 1973-10-11 | 1976-11-10 | Kimberly Clark Co | Method of making reconstituted tobacco having reduced nitrates |
| CN102488313A (en) * | 2011-11-27 | 2012-06-13 | 中国海诚工程科技股份有限公司 | Recycling method of coating liquid of papermaking reconstituted tobacco |
| CN103349867A (en) * | 2013-07-15 | 2013-10-16 | 河南卷烟工业烟草薄片有限公司 | Paper-making process reconstituted tobacco papermaking white water reuse treatment method |
| CN103349351A (en) * | 2013-07-24 | 2013-10-16 | 江苏久吾高科技股份有限公司 | Method for reconstituting tobacco leaves by paper making method based on membrane separation technique |
| CN112457917A (en) * | 2020-11-04 | 2021-03-09 | 上海烟草集团有限责任公司 | Method for recovering flavor components in reconstituted tobacco condensed water, eluent formed by method and application |
Non-Patent Citations (1)
| Title |
|---|
| 罗永明等: "《中药化学成分提取分离技术与方法》", 31 January 2016, 上海科学技术出版社 * |
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