CN104223356A - Method for improving quality of tobacco extract by using amphoteric ion exchange membrane - Google Patents
Method for improving quality of tobacco extract by using amphoteric ion exchange membrane Download PDFInfo
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- CN104223356A CN104223356A CN201410445963.2A CN201410445963A CN104223356A CN 104223356 A CN104223356 A CN 104223356A CN 201410445963 A CN201410445963 A CN 201410445963A CN 104223356 A CN104223356 A CN 104223356A
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- ion exchange
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Abstract
The invention discloses a method for improving the quality of a tobacco extract by using an amphoteric ion exchange membrane. The method comprises the following steps: placing a self-made chitosan/carboxymethyl cellulose/polyether polyol amphoteric ion exchange membrane in tobacco extract aqueous solution with a pH (potential of Hydrogen) value of 3.5-5.0, soaking and stirring for 4-10 hours, and adsorbing protein macromolecules in the tobacco extract to improve the quality of the tobacco extract; then placing the amphoteric ion exchange membrane having adsorbed the protein macromolecules in buffer solution with a pH value of 8-10, soaking and stirring for 3-10 hours, and performing desorption regeneration to realize recycling of the amphoteric ion exchange membrane. The amphoteric ion exchange membrane and the application method are simple, and the quality of the tobacco extract can be improved better.
Description
Technical field
The invention belongs to tobacco extract processing technology field, be specifically related to a kind of method utilizing amphoteric ion exchange membrane to improve tobacco extract quality.
Background technology
In beating and double roasting and sheet cigarette technology for making tobacco threds process, the reasons such as broken and tobacco leaf efflorescence are made due to machinery, cause a large amount of waste tobacco leafs such as short stalk, stalk label, broken cigarette, offal and cigarette ash rod to produce, even also have part due to store improper and in process the outer tobacco leaf of disallowable grade out as gone mouldy tobacco leaf or obstruct head.These waste tobacco leaf resources are difficult to again be applied to production of cigarettes, add the loss of tobacco leaf resource.
A large amount of results of study confirms, adopt the endogenous components of waste tobacco leaf Resource Access to carry out flavouring to cigarette product, to mend perfume (or spice) very effective, and flavouring additive derives from tobacco itself, have good harmony with cigarette product, its security simultaneously have also been obtained good guarantee.But, traditional tobacco extract extracting method, because of extraction process simple coarse, the tobacco extract complicated component obtained, is difficult to be formed the cigarette additive with specific function; Containing a large amount of protein and other macromolecular substances in tobacco extract, also exist while enriching flue gas and flavouring and increase excitant and the defect such as residual, have impact on the effect that tobacco endogenous components is reinforced to perfuming cigarette.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of method utilizing amphoteric ion exchange membrane to improve tobacco extract quality is provided.
* except as otherwise noted, percentage of the present invention is mass percent.
Object of the present invention is achieved by the following technical programs.
Utilize amphoteric ion exchange membrane to improve a method for tobacco extract quality, it is characterized in that: comprise the following steps:
(1) be the tobacco extract aqueous solution of dry matter content 5% by deionized water by tobacco extract dilution, then with sour, the pH value of the tobacco extract aqueous solution be adjusted to 3.5-5.0, for subsequent use;
Wherein, described acid is one in hydrochloric acid, acetic acid, oxalic acid, malic acid, citric acid or its mixture;
(2) amphoteric ion exchange membrane is placed in the tobacco extract aqueous solution that step (1) resulting ph is 3.5 ~ 5.0, soak and stir 4-10 hour, protein macromolecule in tobacco extract is adsorbed, improves the quality of tobacco extract;
(3) amphoteric ion exchange membrane adsorbing protein macromolecule is placed in the cushioning liquid that pH value is 8 ~ 10, soak and stir 3-10 hour, carrying out desorption and regeneration, film is taken out, repeatedly rinse to neutrality by deionized water, realize the regeneration of amphoteric ion exchange membrane.
Wherein, described cushioning liquid is the one in sodium hydrogen phosphate-potassium phosphate buffer, boric acid-borate buffer solution, Glycine-NaOH buffer solution, borax-NaOH, sodium carbonate-bicarbonate buffer solution.
Wherein, the preparation method of described amphoteric ion exchange membrane, is characterized in that: comprise the following steps:
(1) be that the shitosan of 50 ~ 80 parts is dissolved in the acetum of 2% completely by weight portion, be mixed with the chitosan-acetic acid solution of 2%; Be that the carboxymethyl cellulose of 20 ~ 50 parts is dissolved in deionized water completely by weight portion, be mixed with the carboxymethyl cellulose aqueous solution of 2%, for subsequent use;
Wherein, the viscosity of described shitosan is 100-400mPa.s, and deacetylation is greater than 90%; Described carboxymethyl cellulose viscosity is 300-1400mPa.s;
(2) by the chitosan-acetic acid solution of 2%, the carboxymethyl cellulose aqueous solution of 2% and PPG are that the ratio of 5 ~ 8:2 ~ 5:1 ~ 3 is placed in mixing in beaker by weight, the concentrated hydrochloric acid of instillation 36% regulates solution ph to 3.0, it is transparent and homogeneous system that stirring 30min makes it miscible, add the glutaraldehyde water solution that concentration is 1g/L again, beaker is placed in the stirred in water bath 30min that temperature is 60 DEG C, according to silica gel: (shitosan/carboxymethyl cellulose/PPG) weight ratio is that the ratio of 10:1 adds silica gel pore-foaming agent, being stirred to silica gel is dispersed in mixed solution, for subsequent use,
Wherein, the weight ratio sum of the chitosan-acetic acid solution of described 2%, the carboxymethyl cellulose aqueous solution of 2% and PPG is 10.
Wherein, described PPG is one in polyethylene glycol, polypropylene glycol, polyoxypropyleneglycol, polytetrahydrofuran diol or its mixture, and the molecular weight of described PPG is 1000 ~ 10000;
Wherein, the particle diameter of described silica gel pore-foaming agent is 100 ~ 400 orders;
(3) mixed solution obtained in step (2) is cast in the level and smooth Teflon mould in bottom surface, after natural air drying film forming, taking out diaphragm and being placed on temperature is leave standstill in the NaOH solution of 80 DEG C to remove silica gel pore-foaming agent in diaphragm and remaining acid, add epichlorohydrin reaction 3h, take out diaphragm and spend deionized water to neutral, for subsequent use;
(4) diaphragm is placed in constant temperature roaster, regulates the temperature inside the box to 60 DEG C, after oven dry, namely obtain described amphoteric ion exchange membrane.
Compared with prior art, the present invention has following beneficial effect:
1, shitosan/carboxymethyl cellulose/PPG amphoteric ion exchange membrane of the present invention, membrane aperture can be controlled by silica gel pore-foaming agent size, preferably resolves the problem that tight, the large molecule of conventional ion exchanger resin cross-linked structure is difficult to enter.
2, shitosan and carboxymethyl cellulose are natural macromolecular substances, strand skeleton has a large amount of hydrophilic radicals, make it have good hydrophily, avoid the Irreversible Adsorption that common synthesizing cross-linked resin hydrophobic skeleton may bring in aqueous phase absorption.
3, shitosan/carboxymethyl cellulose/PPG amphoteric ion exchange membrane, preparation technology is simple, and raw material is easy to get and low price, and this amphoteric ion exchange membrane has good regeneration function, its cost processing tobacco extract is reduced greatly, and treatment effect is better.
Detailed description of the invention
Below in conjunction with embodiment, invention is specifically described; what deserves to be explained is, embodiment, only for being further elaborated to the present invention, is not limiting the scope of the invention; according to the teachings of the present invention done any change or replacement, all belong to protection scope of the present invention.
Preparation embodiment 1
3.5g shitosan (deacetylation >=95) is dissolved in the acetum of 175g 2%, is configured to the chitosan-acetic acid solution of 2%, and for subsequent use after filtering out insoluble matter; Get 1g carboxymethyl cellulose to be again dissolved in 49g deionized water, be configured to 2% carboxymethyl cellulose aqueous solution for subsequent use.By above-mentioned shitosan, cmc soln mixes according to 7:2:1 mass ratio with polyethylene glycol (molecular weight is 2000), and the pH value to 3.0 of mixed solution is regulated with concentrated hydrochloric acid, continued mechanical stirs 30min and makes its miscible one-tenth transparent and homogeneous system, then the glutaraldehyde water solution of 20.65ml 1g/L is added, and system is placed in the water-bath of 60 DEG C, after continuing stirring reaction 30min, add silica gel: (shitosan/carboxymethyl cellulose/polyethylene glycol) weight ratio is the silica gel pore-foaming agent (particle diameter is 100 ~ 400 orders) of 10:1, mixture continues mechanical agitation 3h and is dispersed in mixed solution to silica gel, then mixture is watered and cast from the level and smooth Teflon mould in bottom surface, natural air drying film forming.After film is air-dry, diaphragm is placed in the 5%NaOH solution of 80 DEG C, remove the silica gel pore-foaming agent in diaphragm and remaining acid, add the epichlorohydrin reaction 3h of 1.91g simultaneously, the degree of cross linking of further raising blend film, after silica gel pore-foaming agent fully dissolves, film is taken out, after being washed till neutrality by a large amount of deionized waters, film being placed in 60 DEG C of constant temperature ovens and drying stand-by.
Preparation embodiment 2
3g shitosan (deacetylation >=95) is dissolved in the acetum of 150g 2%, is configured to the chitosan-acetic acid solution of 2%, and for subsequent use after filtering out insoluble matter; Get 1.5g carboxymethyl cellulose to be again dissolved in 73.5g deionized water, be configured to 2% carboxymethyl cellulose aqueous solution for subsequent use.By above-mentioned shitosan, cmc soln mixes according to 6:3:1 mass ratio with polyethylene glycol (molecular weight 2000), and the pH value to 3.0 of mixed solution is regulated with concentrated hydrochloric acid, continued mechanical stirs 30min and makes its miscible one-tenth transparent and homogeneous system, then the glutaraldehyde water solution of 17.7g 1g/L is added, and system is placed in the water-bath of 60 DEG C, after continuing stirring reaction 30min, add silica gel: (shitosan/carboxymethyl cellulose/polyethylene glycol) mass ratio is the silica gel pore-foaming agent (particle diameter is 100-400 order) of 10:1, mixture continues mechanical agitation 3h, silica gel is made to be dispersed in mixed solution, then mixture is watered and cast from the level and smooth Teflon mould in bottom surface, natural air drying film forming.After film is air-dry, diaphragm is placed in the 5%NaOH solution of 80 DEG C, progressively remove the silica gel pore-foaming agent in diaphragm and remaining acid, add 1.64g epichlorohydrin reaction 3h simultaneously, the degree of cross linking of further raising blend film, after silica gel pore-foaming agent fully dissolves, film is taken out, after being washed till neutrality by a large amount of deionized waters, film being placed in 60 DEG C of constant temperature ovens and drying stand-by.
Application Example 1
First dry stand-by shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane 0.1g deionized water soaked overnight by preparation embodiment 1, for subsequent use; It is the 5% tobacco extract aqueous solution that red large kind tobacco extract (dry matter content 48.50%) is diluted to dry matter content by deionized water, and regulates pH value of solution to 4.5 with acetic acid, for subsequent use; Then shitosan/carboxymethyl cellulose/polyethylene glycol the amphoteric ion exchange membrane after above-mentioned immersion is all placed in the red large kind leaf tobacco extract of 50ml dry matter content 5%, stir after 6 hours, taken out by film, it is stand-by after 1.250 ± 0.008g/ml that tobacco extract is concentrated into density.It is in the borax-sodium hydroxide buffer solution of 8.9 that the shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane taken out is immersed in pH value, stir 8 hours namely renewable, the step then repeated above can carry out upgrading process to new red large kind tobacco extract.
Before and after the process of red large kind tobacco extract, the change of protein content sees the following form:
Evaluation procedure:
Get cloud and mist (purple) unprinted leaf group pipe tobacco at relative humidity (60 ± 2) %, in the climatic chamber of temperature (22 ± 1) DEG C, balance 48h.Take the unprinted leaf group pipe tobacco 50g balanced respectively, respectively the red large kind tobacco extract before and after amphoteric ion exchange membrane process in Application Example 1 is evenly added in unprinted leaf group pipe tobacco with 1% of pipe tobacco weight, after material is by pipe tobacco uniform pickup, each sample is placed in relative humidity (60 ± 2) % again, balance 48h in the climatic chamber of temperature (22 ± 1) DEG C, each processing sample does 3 parallel tests.The sample pipe tobacco handled well is made cigarette with the auxiliary material of cloud and mist (purple) and is used for sensory evaluation, and sensory evaluation index is got average compare.
Analyses Methods for Sensory Evaluation Results sees the following form:
Organoleptic indicator | Contrast | Film process |
Oral stimulation/tongue calcination | 6.5 | 6.5 |
Oral cavity remains/dry sensation | 6.5 | 6.5 |
Convergence | 7.0 | 7.0 |
Throat stimulates | 6.5 | 7.0 |
Throat is dry | 6.5 | 6.5 |
Nasal cavity stimulates | 6.5 | 6.5 |
Fragrance | 7.0 | 7.5 |
Rich | 7.0 | 7.5 |
Fine and smooth soft/mellow and full | 6.5 | 7.0 |
Assorted gas | 6.5 | 6.5 |
Flue gas concentration | 7.5 | 7.5 |
Strength | 5.5 | 5.5 |
Total score | 79.5 | 81.5 |
Result shows: red large kind tobacco extract is after the amphoteric ion exchange membrane process in preparation embodiment 1, and compared with control sample, can reduce throat stimulates, and improves fragrance texture, rich simultaneously, makes flue gas more fine and smooth soft.
Application Example 2
First dry stand-by shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane 0.1g deionized water soaked overnight by preparation embodiment 2, stand-by.It is the 5% tobacco extract aqueous solution that red large kind tobacco extract (dry matter content 48.50%) is diluted to dry matter content by deionized water, and regulates pH value of solution to 3.5 with acetic acid, stand-by.Then shitosan/carboxymethyl cellulose/polyethylene glycol the amphoteric ion exchange membrane after above-mentioned immersion is all placed in the red large kind leaf tobacco extract of 50ml dry matter content 5%, stir after 4 hours, taken out by film, it is stand-by after 1.250 ± 0.008g/ml that tobacco extract is concentrated into density.It is in the borax-sodium hydroxide buffer solution of 8 that the shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane taken out is immersed in pH value, stir 3 hours namely renewable, the step then repeated above can carry out upgrading process to new red large kind tobacco extract.
Before and after the process of red large kind tobacco extract, the change of protein content sees the following form:
Evaluation procedure:
Get cloud and mist (purple) unprinted leaf group pipe tobacco at relative humidity (60 ± 2) %, in the climatic chamber of temperature (22 ± 1) DEG C, balance 48h.Take the unprinted leaf group pipe tobacco 50g balanced respectively, respectively the red large kind tobacco extract before and after amphoteric ion exchange membrane process in Application Example 2 is evenly added in unprinted leaf group pipe tobacco with 1% of pipe tobacco weight, after material is by pipe tobacco uniform pickup, each sample is placed in relative humidity (60 ± 2) % again, balance 48h in the climatic chamber of temperature (22 ± 1) DEG C, each processing sample does 3 parallel tests.The sample pipe tobacco handled well is made cigarette with the auxiliary material of cloud and mist (purple) and is used for sensory evaluation, and sensory evaluation index is got average compare.
Analyses Methods for Sensory Evaluation Results sees the following form:
Organoleptic indicator | Contrast | Film process |
Oral stimulation/tongue calcination | 6.5 | 6.5 |
Oral cavity remains/dry sensation | 6.5 | 6.5 |
Convergence | 7.0 | 7.0 |
Throat stimulates | 6.5 | 7.0 |
Throat is dry | 6.5 | 6.5 |
Nasal cavity stimulates | 6.5 | 6.5 |
Fragrance | 7.0 | 7.5 |
Rich | 7.0 | 7.0 |
Fine and smooth soft/mellow and full | 6.5 | 7.0 |
Assorted gas | 6.5 | 6.5 |
Flue gas concentration | 7.5 | 7.5 |
Strength | 5.5 | 5.5 |
Total score | 79.5 | 81.0 |
Result shows: red large kind tobacco extract is after the amphoteric ion exchange membrane process in preparation embodiment 2, and compared with control sample, can reduce throat stimulates, and improves fragrance texture simultaneously, makes flue gas more fine and smooth soft.
Application Example 3
First dry stand-by shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane 0.1g deionized water soaked overnight by preparation embodiment 1, stand-by.It is the 5% tobacco extract aqueous solution that red large kind tobacco extract (dry matter content 48.50%) is diluted to dry matter content by deionized water, and regulates pH value of solution to 5.0 with acetic acid, stand-by.Then shitosan/carboxymethyl cellulose/polyethylene glycol the amphoteric ion exchange membrane after above-mentioned immersion is all placed in the red large kind leaf tobacco extract of 50ml dry matter content 5%, stir after 10 hours, taken out by film, it is stand-by after 1.250 ± 0.008g/ml that tobacco extract is concentrated into density.It is in the borax-sodium hydroxide buffer solution of 10 that the shitosan/carboxymethyl cellulose/polyethylene glycol amphoteric ion exchange membrane taken out is immersed in pH value, stir 10 hours namely renewable, the step then repeated above can carry out upgrading process to new red large kind tobacco extract.
Before and after the process of red large kind tobacco extract, the change of protein content sees the following form:
Evaluation procedure:
Get cloud and mist (purple) unprinted leaf group pipe tobacco at relative humidity (60 ± 2) %, in the climatic chamber of temperature (22 ± 1) DEG C, balance 48h.Take the unprinted leaf group pipe tobacco 50g balanced respectively, respectively the red large kind tobacco extract before and after amphoteric ion exchange membrane process in Application Example 3 is evenly added in unprinted leaf group pipe tobacco with 1% of pipe tobacco weight, after material is by pipe tobacco uniform pickup, each sample is placed in relative humidity (60 ± 2) % again, balance 48h in the climatic chamber of temperature (22 ± 1) DEG C, each processing sample does 3 parallel tests.The sample pipe tobacco handled well is made cigarette with the auxiliary material of cloud and mist (purple) and is used for sensory evaluation, and sensory evaluation index is got average compare.
Analyses Methods for Sensory Evaluation Results sees the following form:
Organoleptic indicator | Contrast | Film process |
Oral stimulation/tongue calcination | 6.5 | 6.5 |
Oral cavity remains/dry sensation | 6.5 | 6.5 |
Convergence | 7.0 | 7.0 |
Throat stimulates | 6.5 | 7.0 |
Throat is dry | 6.5 | 7.0 |
Nasal cavity stimulates | 6.5 | 6.5 |
Fragrance | 7.0 | 7.5 |
Rich | 7.0 | 7.5 |
Fine and smooth soft/mellow and full | 6.5 | 7.0 |
Assorted gas | 6.5 | 6.5 |
Flue gas concentration | 7.5 | 7.5 |
Strength | 5.5 | 5.5 |
Total score | 79.5 | 82.0 |
Result shows: red large kind tobacco extract is after the amphoteric ion exchange membrane process in preparation embodiment 1, and compared with control sample, can reduce throat stimulates and dry sensation, improves fragrance texture, rich simultaneously, makes flue gas more fine and smooth soft.
Claims (8)
1. utilize amphoteric ion exchange membrane to improve a method for tobacco extract quality, it is characterized in that: comprise the following steps:
(1) be the tobacco extract aqueous solution of dry matter content 5% by deionized water by tobacco extract dilution, then with sour, the pH value of the tobacco extract aqueous solution be adjusted to 3.5-5.0, for subsequent use;
(2) amphoteric ion exchange membrane is placed in the tobacco extract aqueous solution that step (1) resulting ph is 3.5 ~ 5.0, soaks and stir 4-10 hour, the protein macromolecule in tobacco extract is adsorbed;
(3) amphoteric ion exchange membrane adsorbing protein macromolecule is placed in the cushioning liquid that pH value is 8 ~ 10, soak and stir 3-10 hour, carrying out desorption and regeneration, film is taken out, repeatedly rinse to neutrality by deionized water, make the regeneration of amphoteric ion exchange membrane.
2. the method utilizing amphoteric ion exchange membrane to improve tobacco extract quality according to claim 1, is characterized in that: sour described in step (1) is the one in hydrochloric acid, acetic acid, oxalic acid, malic acid, citric acid or its mixture.
3. the method utilizing amphoteric ion exchange membrane to improve tobacco extract quality according to claim 1, is characterized in that: the cushioning liquid described in step (3) is the one in sodium hydrogen phosphate-potassium phosphate buffer, boric acid-borate buffer solution, Glycine-NaOH buffer solution, borax-NaOH, sodium carbonate-bicarbonate buffer solution.
4. a preparation method for amphoteric ion exchange membrane, is characterized in that: comprise the following steps:
(1) be that the shitosan of 50 ~ 80 parts is dissolved in the acetum of 2% completely by weight portion, be mixed with the chitosan-acetic acid solution of 2%; Be that the carboxymethyl cellulose of 20 ~ 50 parts is dissolved in deionized water completely by weight portion, be mixed with the carboxymethyl cellulose aqueous solution of 2%, for subsequent use;
(2) by the chitosan-acetic acid solution of 2%, the carboxymethyl cellulose aqueous solution of 2% and PPG are that the ratio of 5 ~ 8:2 ~ 5:1 ~ 3 is placed in mixing in beaker by weight, the concentrated hydrochloric acid of instillation 36% regulates solution ph to 3.0, it is transparent and homogeneous system that stirring 30min makes it miscible, add the glutaraldehyde water solution that concentration is 1g/L again, beaker is placed in the stirred in water bath 30min that temperature is 60 DEG C, according to silica gel: (shitosan/carboxymethyl cellulose/PPG) weight ratio is that the ratio of 10:1 adds silica gel pore-foaming agent, being stirred to silica gel is dispersed in mixed solution, for subsequent use,
(3) mixed solution obtained in step (2) is cast in the level and smooth Teflon mould in bottom surface, after natural air drying film forming, taking out diaphragm and being placed on temperature is leave standstill in the NaOH solution of 80 DEG C to remove silica gel pore-foaming agent in diaphragm and remaining acid, add epichlorohydrin reaction 3h, take out diaphragm and spend deionized water to neutral, for subsequent use;
(4) diaphragm is placed in constant temperature roaster, regulates the temperature inside the box to 60 DEG C, after oven dry, namely obtain described amphoteric ion exchange membrane.
5. the preparation method of amphoteric ion exchange membrane according to claim 4, is characterized in that: described in step (1), the viscosity of shitosan is 100-400mPa.s, and deacetylation is greater than 90%; Described carboxymethyl cellulose viscosity is 300-1400mPa.s.
6. the preparation method of amphoteric ion exchange membrane according to claim 4, is characterized in that: described in step (2), the weight ratio sum of the chitosan-acetic acid solution of 2%, the carboxymethyl cellulose aqueous solution of 2% and PPG is 10.
7. the preparation method of amphoteric ion exchange membrane according to claim 4, it is characterized in that: PPG described in step (2) is one in polyethylene glycol, polypropylene glycol, polyoxypropyleneglycol, polytetrahydrofuran diol or its mixture, and the molecular weight of described PPG is 1000 ~ 10000.
8. the preparation method of amphoteric ion exchange membrane according to claim 4, is characterized in that: described in step (2), the particle diameter of silica gel pore-foaming agent is 100 ~ 400 orders.
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CN103082394A (en) * | 2013-01-25 | 2013-05-08 | 安徽中烟工业有限责任公司 | Regulation and control method for paper-making method reproducing tobacco leaf extract liquor negative ion components |
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EP0035052B1 (en) * | 1980-03-05 | 1984-12-27 | Philip Morris Incorporated | Method of treating tobacco extracts employing electrodialysis |
CN101204249A (en) * | 2007-12-11 | 2008-06-25 | 广东中烟工业公司 | Preparation method for tobacco extracting |
CN101606748A (en) * | 2008-06-19 | 2009-12-23 | 湖北中烟工业有限责任公司 | Handle the slice production method of tobacco waste extract with membrane separation technique |
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