CN117326731A - Enrichment and separation method for flavor components in reconstituted tobacco production wastewater - Google Patents
Enrichment and separation method for flavor components in reconstituted tobacco production wastewater Download PDFInfo
- Publication number
- CN117326731A CN117326731A CN202311271678.9A CN202311271678A CN117326731A CN 117326731 A CN117326731 A CN 117326731A CN 202311271678 A CN202311271678 A CN 202311271678A CN 117326731 A CN117326731 A CN 117326731A
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- Prior art keywords
- concentration
- wastewater
- reconstituted tobacco
- liquid
- trapped fluid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 241000208125 Nicotiana Species 0.000 title claims abstract description 73
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 73
- 239000002351 wastewater Substances 0.000 title claims abstract description 73
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000000926 separation method Methods 0.000 title claims abstract description 32
- 239000000796 flavoring agent Substances 0.000 title claims abstract description 23
- 235000019634 flavors Nutrition 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 239000012530 fluid Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 41
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 28
- 238000011084 recovery Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 20
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 19
- 229960002715 nicotine Drugs 0.000 claims abstract description 18
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010257 thawing Methods 0.000 claims abstract description 10
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 235000019504 cigarettes Nutrition 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 16
- 230000008014 freezing Effects 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 11
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 10
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- 238000001704 evaporation Methods 0.000 claims description 8
- 230000008020 evaporation Effects 0.000 claims description 8
- 238000011085 pressure filtration Methods 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
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- -1 2-isopropyl-8-hydroxy-8-methyl-6-nonene Chemical compound 0.000 description 4
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- IKDIJXDZEYHZSD-UHFFFAOYSA-N 2-phenylethyl formate Chemical compound O=COCCC1=CC=CC=C1 IKDIJXDZEYHZSD-UHFFFAOYSA-N 0.000 description 4
- ROWKJAVDOGWPAT-UHFFFAOYSA-N Acetoin Chemical compound CC(O)C(C)=O ROWKJAVDOGWPAT-UHFFFAOYSA-N 0.000 description 4
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 4
- CUBICSJJYOPOIA-UHFFFAOYSA-N Ethylmethylmaleimide Chemical compound CCC1=C(C)C(=O)NC1=O CUBICSJJYOPOIA-UHFFFAOYSA-N 0.000 description 4
- FLIACVVOZYBSBS-UHFFFAOYSA-N Methyl palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC FLIACVVOZYBSBS-UHFFFAOYSA-N 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
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- XLSMFKSTNGKWQX-UHFFFAOYSA-N hydroxyacetone Chemical compound CC(=O)CO XLSMFKSTNGKWQX-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 4
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- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 3
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- POYYYXPQBFPUKS-UHFFFAOYSA-N 2-butylcyclohexan-1-one Chemical compound CCCCC1CCCCC1=O POYYYXPQBFPUKS-UHFFFAOYSA-N 0.000 description 2
- ISTJMQSHILQAEC-UHFFFAOYSA-N 2-methyl-3-pentanol Chemical compound CCC(O)C(C)C ISTJMQSHILQAEC-UHFFFAOYSA-N 0.000 description 2
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- 238000005189 flocculation Methods 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- NMRPBPVERJPACX-UHFFFAOYSA-N octan-3-ol Chemical compound CCCCCC(O)CC NMRPBPVERJPACX-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/22—Treatment of water, waste water, or sewage by freezing
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the technical field of reconstituted tobacco production and processing, and particularly relates to an enrichment and separation method for flavor components in reconstituted tobacco production wastewater. The method comprises the steps of carrying out multistage purification treatment on concentrated wastewater in reconstituted tobacco and carrying out primary purification treatment on low-concentration wastewater, adopting a reverse osmosis membrane to concentrate two purifying solutions respectively to obtain high nicotine trapped fluid and high fragrance trapped fluid, compounding the high nicotine trapped fluid and the high fragrance trapped fluid, and carrying out freeze thawing and centrifugation to obtain enriched separating liquid of high tobacco fragrance components. The enriched components comprise most of tobacco fragrance components in the wastewater, and the enriched separation liquid has high stability and long storage time. The method can improve the recovery rate of the tobacco fragrance components, greatly reduce the discharge amount of wastewater, and has good process adaptability and popularization significance.
Description
Technical Field
The invention belongs to the technical field of reconstituted tobacco production, and particularly relates to an enrichment and separation method of flavor components in reconstituted tobacco production wastewater.
Background
The paper-making reconstituted tobacco is a sheet-like reconstituted product prepared by using tobacco materials such as tobacco dust, tobacco stems, crushed tobacco sheets and the like as raw materials and adopting a paper-making method. As the papermaking forming technology similar to the traditional papermaking industry is adopted, more than 50 tons of wastewater is discharged per 1 ton of reconstituted tobacco produced, and the wastewater discharged in the production process of the reconstituted tobacco can be classified into high-concentration wastewater, medium-concentration wastewater and low-concentration wastewater according to the characteristics and the discharge characteristics of the wastewater. The medium-concentration wastewater mainly comes from pulp washing water in the pulping process and white water generated in the sheet-based papermaking process, and has the characteristics of continuous discharge, large discharge water quantity, low COD (chemical oxygen demand), high suspended solids content, high chromaticity, high nicotine and the like; the low-concentration waste water mainly contains condensed water during concentration and evaporation, has more tobacco aroma components and Maillard reactants generated during high-temperature concentration of extracting solution, such as benzyl alcohol, 3-oxo-alpha-ionol, butyrolactone, megastigmatrienone and other tobacco aroma components, is of great importance to the smoking sensory quality of cigarettes, and mainly influences aroma quality and aroma concentration of sensory quality, and the medium-concentration waste water and the low-concentration waste water are main sources of waste water discharge. The wastewater discharge not only causes the loss of tobacco flavor components, but also increases the sewage treatment load. Therefore, the recovery of the tobacco flavor components in the reconstituted tobacco production wastewater not only can realize the efficient utilization of resources, but also can reduce the sewage treatment load.
The invention patent with the publication number of CN113498875B discloses a method for recovering aroma substances in concentrated white water of reconstituted tobacco and application thereof, which adopts ceramic microfiltration membranes to purify the white water, utilizes macroporous resins with two different polarities in series to recover aroma substances in the purified white water, and directly adopts membrane purification equipment to remove impurities due to more impurities in the white water, so that the membrane flux in the running process can be reduced more rapidly, the membrane flux can recover the initial level after the membrane flux is subjected to drug washing, but frequent washing can directly influence the continuity and stability of the use of the membrane flux, in addition, the resin has the characteristic of selective adsorption, the method can not completely recover the aroma substances in the waste water, and the resin with less concentrated components per unit mass has lower treated white water amount and higher input cost.
The invention patent with the authority of publication number CN112499807B discloses a recovery method of aroma components in papermaking wastewater, interception concentrated solution formed by the recovery method and application of the aroma components, which is to purify the papermaking wastewater by utilizing the processes of filtration, flocculation sedimentation, microfiltration and ultrafiltration, and then enrich the aroma components by using a reverse osmosis membrane, wherein the papermaking white water contains more calcium carbonate. In addition, the concentration of the trapped concentrated solution obtained by reverse osmosis concentration is lower, so that the storage and transportation are affected, the use amount is more during use, and the production energy consumption is increased.
The invention patent with the publication number of CN113455694B discloses a recycling system of concentrated evaporation condensate water of reconstituted tobacco by a papermaking method, which is characterized in that the concentrated evaporation condensate water is recycled for dilution and concentration adjustment of dry materials after extraction and squeezing, although the sensory quality of products can be improved to a certain extent, when the concentrated evaporation condensate water is directly recycled for the processes, the produced products still need to undergo the processes of pulping, net-surfing, coating and drying, only a small part of fragrance components remain in the products, and the purpose of improving the customized quality of the products cannot be achieved by recycling the concentrated evaporation condensate water for online slurry.
Therefore, there is a need for an improved and optimized recovery method of tobacco flavor components in reconstituted tobacco production wastewater to increase the recovery rate of the flavor components.
Disclosure of Invention
In view of the technical problems, the invention provides the enrichment and separation method for the aroma components in the reconstituted tobacco production wastewater, which has the advantages of simple process and low cost, can obtain enrichment and separation liquid containing high nicotine and high tobacco aroma components, and can specifically improve the strength and aroma quality of cigarette products. The enriched components comprise most of tobacco fragrance components in the wastewater, and the enriched separation liquid has high stability and long storage time.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the enrichment and separation method of the flavor components in the reconstituted tobacco production wastewater comprises the steps of carrying out multistage purification treatment on the concentrated wastewater in the reconstituted tobacco, carrying out primary purification treatment on the low-concentration wastewater, adopting a reverse osmosis membrane to concentrate the two purification solutions respectively to obtain high-nicotine trapped fluid and high-flavor trapped fluid, compounding the high-nicotine trapped fluid and the high-flavor trapped fluid, and carrying out freeze thawing and centrifugation to obtain the enrichment and separation liquid of the flavor components of the high tobacco.
The method specifically comprises the following steps:
1) Purifying medium-concentration wastewater: sequentially carrying out normal pressure filtration, centrifugal filtration, pressure filtration and acidification treatment on the medium-concentration wastewater of the reconstituted tobacco production wastewater to obtain medium-concentration purified liquid;
2) Purifying low-concentration waste water: filtering or centrifugally filtering the low-concentration wastewater of the reconstituted tobacco production wastewater by filter paper to obtain a low-concentration purifying liquid;
3) Reverse osmosis: respectively carrying out reverse osmosis concentration treatment on the medium-concentration purifying liquid obtained in the step 1) and the low-concentration purifying liquid obtained in the step 2) to obtain medium-concentration trapped liquid and low-concentration trapped liquid respectively, wherein the concentration multiple is 20-200 times;
4) Freezing and thawing: mixing the medium-concentration trapped fluid and the low-concentration trapped fluid according to a certain proportion to obtain mixed trapped fluid, freezing the mixed trapped fluid at the temperature of-20 ℃ to-10 ℃, taking out the mixed trapped fluid after the trapped fluid is completely frozen, melting the mixed trapped fluid at room temperature (25+/-5 ℃), and collecting the mixed trapped fluid to obtain high-concentration recovered fluid;
5) Enrichment and separation: and centrifuging or filtering to remove precipitate in the high-concentration recovery liquid, wherein the obtained supernatant is the enrichment and separation liquid of the high-tobacco aroma components.
Specifically, in the step 1), the medium-concentration wastewater of the reconstituted tobacco production wastewater is derived from pulp washing wastewater of a pulping process or white water of a papermaking process.
Specifically, in the step 1), one or a combination of two modes of an arc screen and a fine mesh filter is selected for normal pressure filtration, so that large suspended matters such as long fibers can be removed.
Specifically, in the step 1), centrifugal filtration is performed by using a decanter centrifuge or a disk centrifuge, so that suspended matters and impurities such as solid calcium carbonate, fine fibers and the like in the wastewater can be removed.
Specifically, in the step 1), the pressure filtration selects one or two modes of a pressure filter or a membrane purification filtration device, wherein the filtration medium of the pressure filter is one of natural quartz sand and manganese sand; the membrane purification can be one or two of ultrafiltration and nanofiltration; pressure filtration is used to remove larger particle suspensions and colloids such as solid calcium carbonate in wastewater.
Specifically, in the step 1), 0.4-2 per mill (relative to the mass of the filtrate) of organic acid is added to adjust the pH of the filtrate to 5.1-6.0, the organic acid can be one or more of oxalic acid, succinic acid, malic acid, citric acid and benzoic acid, the purpose of acidification is to decompose water-soluble calcium carbonate, and the purpose of acidification is to improve the sensory evaluation quality of the final enriched separation solution, improve the stability of nicotine at the same time, avoid the conversion of nicotine into reduced nicotine or other components in the subsequent storage process, and prolong the storage time of the enriched separation solution.
Specifically, in the step 2), the low-concentration wastewater of the reconstituted tobacco production wastewater is derived from concentrated evaporation condensate water in a concentration process.
Specifically, in the step 3), the trapped fluid and the penetrating fluid are obtained through reverse osmosis treatment, wherein the trapped fluid keeps most of tobacco fragrance components in the wastewater, and the penetrating fluid is cleaner clear liquid which can replace clear water to be used in the tobacco leaf reconstruction process; in the step 3), the pressure is 0.6-1.2 Mpa during reverse osmosis concentration.
Specifically, in the step 4), the mixing ratio of the medium-concentration trapped fluid to the low-concentration trapped fluid is 0.5:1-1:20 (volume ratio); collecting the liquid before freezing in the volume of 15-20% after thawing; the concentration of nicotine and other tobacco aroma components contained in the collected high-concentration recovery liquid is improved by 3-4 times relative to the concentration of the reverse osmosis trapped liquid;
further, other tobacco flavor components include acetoin, phenethyl alcohol, 2-acetylpyrrole, benzyl alcohol, dihydroactinolide, furfural, solanone, butyrolactone, phenylacetaldehyde, 3-oxo- α -ionol, 3- (4, 8, 12-trimethyltridecyl) furan, hydroxyacetone, 4-cyclopentene-1, 3-dione, 2 (3H) -furanone, 4-oxoisophorone, benzaldehyde, methyl palmitate, palmitic acid, 3-hydroxy- β -damascenone, 2-methyl-3-pentanol, benzoic acid, (E) -5-isopropyl-8-hydroxy-8-methyl-6-nonen-2-one, ethyl maltol, 1-pentene-3-one, 3-ethyl-4-methyl-pyrrole-2, 5-dione, 3-oxo- α -ionone, γ -octanol, γ -caprolactone, 2-hydroxy-3-pentanone, megalin, 2-butylcyclohexanone, phenethyl formate, benzofuranone, 2-isopropyl-8-hydroxy-8-methyl-6-nonene, ethyl maltol, 3-methyl-2-butanone, 2, 5-methyl-butanone, 2-methyl-6-butanone, maleic anhydride, and the like. Specifically, in the step 5), the centrifugal speed is 3000-10000 r/min, and the centrifugal time is 3-20 min.
Specifically, the precipitate in step 5) is mainly formed by water-soluble substances such as proteins and the like dissolved in the production wastewater and substances such as calcium salts and the like formed by organic acid regulation, and the substances such as water-soluble proteins, calcium salts and the like can be precipitated by freezing.
Furthermore, based on a general inventive concept, the invention also provides application of the enrichment and separation liquid in cigarettes.
The enrichment and separation liquid is applied to reconstituted tobacco coating liquid, traditional cigarette flavoring or slurry preparation for producing the heated non-combustible cigarettes by a thick slurry method, so that the aroma quality and strength of the sensory quality of the product can be improved.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides the enrichment and separation method for the aroma components in the reconstituted tobacco production wastewater, which is simple and convenient to operate and high in operation efficiency. The method can enrich most of tobacco fragrance components in the reconstituted tobacco production wastewater, improve the recovery rate of the tobacco fragrance components, and the recovered substances can be applied to products such as reconstituted tobacco, traditional cigarettes and heated non-combustible cigarettes, so that the fragrance quality and strength improvement of the sensory quality of the products can be realized; meanwhile, the wastewater discharge amount is greatly reduced, and the method has good process adaptability and popularization significance.
Drawings
FIG. 1 is a chart of GC chromatography detection of the major volatile tobacco flavor components in concentrated evaporative condensate and white water;
FIG. 2 is a flow chart of color change of a product obtained by the method for enriching and separating aroma components in reconstituted tobacco production wastewater.
Detailed Description
For an understanding of the present invention, reference will now be made in detail to the present invention, examples of which are illustrated in the accompanying drawings and described in the preferred embodiments, but the scope of the invention is not limited to the specific embodiments.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
The enrichment and separation method of the flavor components in the reconstituted tobacco production wastewater comprises the following specific steps:
1) Purifying medium-concentration wastewater: filtering white water in the papermaking section through an arc screen at normal pressure to remove large suspended matters such as long fibers in the wastewater, so as to obtain filtrate, wherein the content (mass percent) of the suspended matters is reduced from 0.32% to 0.20%;
removing suspended matters and impurities such as fine fibers, calcium carbonate with larger particle size and the like in the filtrate through a horizontal decanter centrifuge, wherein the content of the suspended matters is reduced to 0.06%;
purifying and filtering the filtrate treated by the horizontal decanter centrifuge by using an ultrafiltration membrane (specifically a SiC ultrafiltration membrane with a membrane aperture of 70 nm), wherein suspended matters are not contained, and the content of calcium ions in the treated filtrate is 310mg/L;
the main volatile aroma components in the filtrate after multistage filtration are nicotine, and at the same time, the filtrate also contains a small amount of tobacco volatile aroma components such as dihydroactinolide, megastigmatrienone, 3-hydroxy-beta-damascenone, 3-oxo-alpha-ionone and the like, at the moment, 0.6 per mill (relative to the mass of the filtrate) oxalic acid is added for acidizing treatment, the pH value after the treatment is 5.07, acidified white water is obtained, nicotine salt in the acidified white water is mainly oxalic acid nicotine salt, the concentration of the oxalic acid nicotine salt is detected to be 64.8mg/L by high performance liquid chromatography, and the proportion of the nicotine in the total volatile aroma components reaches 94%;
2) Purifying low-concentration waste water: filtering the concentrated evaporated condensate water by filter paper to remove solid such as scrap iron, scaling matters on the wall of a pipeline and the like in the condensate water, thereby obtaining purified condensate water;
the purified condensate water has main volatile flavor components such as acetoin, phenethyl alcohol, 2-acetylpyrrole, benzyl alcohol, dihydroactinolide, furfural, solanone, butyrolactone, phenylacetaldehyde, 3-oxo-alpha-ionol, 3- (4, 8, 12-trimethyltridecyl) furan, hydroxyacetone, 4-cyclopentene-1, 3-dione, 2 (3H) -furanone, 4-oxoisophorone, benzaldehyde, methyl palmitate, palmitic acid, 3-hydroxy-beta-damascenone, 2-methyl-3-pentanol, benzoic acid, (E) -5-isopropyl-8-hydroxy-8-methyl-6-nonene-2-one, ethyl maltol, 1-pentene-3-one, 3-ethyl-4-methyl-pyrrole-2, 5-dione, 3-oxo-alpha-ionone, gamma-octanol, gamma-caprolactone, 2-hydroxy-3-pentanone, soybean trienone, 2-butylcyclohexanone, phenethyl formate, baker, 2-isopropyl-8-hydroxy-8-methyl-6-nonene, 2-methyl-6-nonene, ethyl maltol, 3-methyl-2-methyl-3-butanone, 2-methyl-6-butanone, 2-methyl-butanone, 3-methyl-6-butanone, 3-methyl-butanone, 3-butanone, the concentration is in the range of 36mg/L to 730 mg/L;
3) Reverse osmosis: respectively carrying out reverse osmosis concentration on the acidified white water and purified condensate water under the operation pressure of 0.8Mpa to obtain acidified white water trapped fluid (namely white water reverse osmosis concentrated fluid), purified condensate water trapped fluid (namely condensate water reverse osmosis concentrated fluid) and permeate fluid, wherein the concentration multiple of the white water reverse osmosis concentrated fluid is 40 times, (meanwhile, the white water which is not acidified by oxalic acid is directly subjected to reverse osmosis treatment as a control group, and compared with purified white water without oxalic acid, the concentration multiple can be increased by 21 percent when the reverse osmosis is carried out in the embodiment), and the concentration of nicotine in the trapped fluid reaches 1539.6mg/L; the concentration multiple of the condensed water reverse osmosis concentrated solution is 50 times, the aperture of the reverse osmosis membrane is 0.1nm, wherein the trapped liquid retains most of tobacco fragrance components in the wastewater, and the permeate liquid is cleaner supernatant liquid which can replace clear water for the tobacco leaf reconstruction process; FIG. 1 is a schematic illustration of the concentrated evaporative condensate and the major volatile tobacco flavor components in the white water, it being seen that the concentrated evaporative condensate has a greater tobacco flavor component than the white water, the tobacco flavor component in the former contributing to the aroma and concentration of the cigarette product, the major component of the white water being nicotine, which is critical to the cigarette stiffness;
4) Freezing and thawing: the white water reverse osmosis concentrated solution and the condensed water reverse osmosis concentrated solution are mixed according to the volume ratio of 0.5:1, recording the volume of the mixed reverse osmosis concentrated solution as V 1 Freezing the mixed reverse osmosis concentrated solution at the temperature of minus 16 ℃, taking out the mixed solution after the liquid is totally frozen and naturally thawing the mixed solution at room temperature (25+/-5 ℃), collecting thawing solution just after thawing, and calculating the final collection volume to be 20% of the volume before freezing, wherein the part of the liquid is called high-concentration recovery solution;
5) Enrichment and separation: centrifuging the high-concentration recovery liquid at 8000r/min for 10min for enrichment, removing sediment in the high-concentration recovery liquid, and obtaining supernatant which is enrichment separation liquid with high tobacco aroma components, wherein the concentration and recovery rate of main tobacco aroma components in the enrichment separation liquid are shown in the following table 1;
TABLE 1
Note that: the recovery rate is the recovery quality of each aroma component relative to the quality of each aroma component of the purified liquid before reverse osmosis.
The main nicotine salt in the enriched separating liquid is oxalic acid nicotine salt, the concentration of the main nicotine salt reaches 5542.7mg/L, the recovery rate of nicotine can reach 64.8%, and the content of calcium ions is 291mg/L. Fig. 2 is a flow chart of the method of the invention, and the percentage amounts in fig. 2 refer to the volume ratio of the collected volume to the liquid before freezing concentration, and as can be seen from fig. 2, the process can realize high concentration of the production wastewater after the implementation of the process, and the activity of original flavor components of tobacco can be maintained to the greatest extent by adopting reverse osmosis concentration and freezing concentration, and meanwhile, the loss of low boiling components and side reactions during evaporation concentration are avoided.
Application example 1
The invention also provides application of the enrichment and separation liquid in cigarettes, which comprises the following specific steps:
the enriched separating liquid is used as a test group, white water recovery solution without organic acid is used as a control group, the two are respectively added into the heating non-burning cigarettes, the addition amount is 2 percent (relative to the mass of the heating non-burning cigarette core material), and smoking (sensory evaluation) is carried out according to the Chinese style cigarette style sensory evaluation method of YC/T497-2014 cigarettes.
The result shows that the enrichment and separation liquid obtained by the application contains various important flavor components of tobacco and nicotine with obvious effect of improving the strength, the organic acid is mainly oxalic acid added, and also contains a small amount of organic acids such as 2-ethylbutyric acid, benzoic acid, phenylacetic acid, palmitic acid and the like contained in the tobacco, after the enrichment and separation liquid is applied to cigarette products, natural tobacco fragrance is increased, smoke concentration is increased, strength is increased, oral cavity irritation is reduced, aftertaste is slightly improved, sensory evaluation total score is increased by 1.5 minutes compared with that of a control group (white water recovery solution without organic acid is applied to cigarette products), and aroma and oral cavity irritation of the products can be obviously improved compared with that of the control group (white water recovery solution without organic acid is applied to cigarette products).
In addition, after the enrichment and separation liquid is stored for 6 months at room temperature, the concentration of nicotine in the enrichment and separation liquid is still maintained above 5250mg/L through detection, and the enrichment and separation liquid has better stability.
Finally, what should be said is: the foregoing description is only of the preferred embodiments of the invention and the application of the principles of the invention. It will be understood by those skilled in the art that the present invention is not limited to the particular embodiments described herein, but is capable of various obvious changes, rearrangements and substitutions as will now become apparent to those skilled in the art without departing from the scope of the invention. Therefore, while the present invention has been described in connection with the above embodiments, it is to be understood that the invention is not limited to the specific embodiments disclosed and that many other and equally effective embodiments may be devised without departing from the spirit of the invention, and the scope thereof is determined by the scope of the appended claims.
Claims (8)
1. The enrichment and separation method of the flavor components in the reconstituted tobacco production wastewater is characterized by comprising the following steps of:
1) Purifying medium-concentration wastewater: sequentially carrying out normal pressure filtration, centrifugal filtration, pressure filtration and acidification treatment on the medium-concentration wastewater of the reconstituted tobacco production wastewater to obtain medium-concentration purified liquid;
2) Purifying low-concentration waste water: filtering or centrifugally filtering the low-concentration wastewater of the reconstituted tobacco production wastewater by filter paper to obtain a low-concentration purifying liquid;
3) Reverse osmosis: respectively carrying out reverse osmosis concentration treatment on the medium-concentration purifying liquid obtained in the step 1) and the low-concentration purifying liquid obtained in the step 2) to obtain medium-concentration trapped liquid and low-concentration trapped liquid respectively, wherein the concentration multiple is 20-200 times;
4) Freezing and thawing: mixing the medium-concentration trapped fluid and the low-concentration trapped fluid according to a certain proportion to obtain mixed trapped fluid, freezing the mixed trapped fluid at the temperature of-20 ℃ to-10 ℃, taking out the mixed trapped fluid after the trapped fluid is completely frozen, melting the mixed trapped fluid at room temperature, and collecting the mixed trapped fluid to obtain high-concentration recovered fluid;
5) Enrichment and separation: and centrifuging or filtering to remove precipitate in the high-concentration recovery liquid, wherein the obtained supernatant is the enrichment and separation liquid of the high-tobacco aroma components.
2. The method for enriching and separating aroma components in reconstituted tobacco production wastewater according to claim 1, wherein in step 1), the medium-concentrated wastewater of the reconstituted tobacco production wastewater is derived from pulp washing wastewater of a pulping process or white water of a papermaking process.
3. The method for enriching and separating aroma components in reconstituted tobacco production wastewater according to claim 1, wherein in the step 1), the acidification treatment is to add 0.4-2 per mill of organic acid relative to the mass of the filtrate to adjust the pH of the filtrate to 5.1-6.0, and the organic acid is one or more of oxalic acid, succinic acid, malic acid, citric acid and benzoic acid.
4. The method for enriching and separating aroma components from reconstituted tobacco production wastewater according to claim 1, wherein in step 2), the low-concentration wastewater of the reconstituted tobacco production wastewater is derived from concentrated evaporation condensate water of a concentration process.
5. The method for enriching and separating aroma components in reconstituted tobacco production wastewater according to claim 1, wherein in the step 3), the pressure is 0.6-1.2 mpa during reverse osmosis concentration.
6. The method for enriching and separating aroma components in reconstituted tobacco production wastewater according to claim 1, wherein in the step 4), the mixing volume ratio of medium-concentration trapped fluid and low-concentration trapped fluid is 0.5:1-1:20; collecting the liquid before thawing, wherein the collecting amount is 15% -20% of the liquid before freezing; the concentration of nicotine and other tobacco aroma components contained in the collected high-concentration recovery liquid is improved by 3-4 times relative to the concentration of the reverse osmosis trapped liquid.
7. The enrichment and separation method of flavor components in reconstituted tobacco production wastewater according to claim 1, wherein in the step 5), the centrifugal speed is 3000 r/min-10000 r/min, and the centrifugal time is 3 min-20 min.
8. Use of the enriched separation solution obtained by the method of any one of claims 1-7 in cigarettes.
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