CN104351943A - Method for reducing TSNA (tobacco-specific nitrosamines) content and nitrate content of reconstituted tobacco concentrated solution according to electrodialysis method - Google Patents
Method for reducing TSNA (tobacco-specific nitrosamines) content and nitrate content of reconstituted tobacco concentrated solution according to electrodialysis method Download PDFInfo
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- CN104351943A CN104351943A CN201410456054.9A CN201410456054A CN104351943A CN 104351943 A CN104351943 A CN 104351943A CN 201410456054 A CN201410456054 A CN 201410456054A CN 104351943 A CN104351943 A CN 104351943A
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- electrodialysis desalination
- electrodialysis
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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
- A24B15/22—Treatment of tobacco products or tobacco substitutes by application of electric or wave energy or particle radiation
Abstract
The invention discloses a method for reducing the TSNA (tobacco-specific nitrosamines) content and the nitrate content of a reconstituted tobacco concentrated solution according to an electrodialysis method. The method comprises three times of electrodialysis treatment procedures: for the first time, electrodialysis desalination treatment is carried out to remove nitrate radical in the reconstituted tobacco concentrated solution, wherein the acid consumption used for adjusting a feed liquid to be acidic is reduced at the same time; for the second time, electrodialysis desalination treatment is carried out under a strong acid condition to remove TSNA in the papermaking reconstituted tobacco concentrated solution; for the third time, electrodialysis desalination treatment is carried out to recycle nicotine, wherein by-products generated in the step can be used for preparing fertilizer. The method has the advantages that the characteristics of reconstituted tobacco concentrated solution and electrodialysis are utilized comprehensively; TSNA and the precursor-nitrate of TSNA are effectively removed, while great loss of nicotine caused by the conventional electrodialysis treatment is avoided; the by-products are utilized effectively; the effects in the aspects of efficiency improvement, energy conservation, pollution reduction and the like are obvious; the method is suitable for industrialized mass production.
Description
One, technical field
The present invention relates to a kind of separation method, specifically a kind of method utilizing electroosmose process to reduce TSNA and nitrate content in reproduced tobacco concentrated liquid.
Two, background technology
Tobacco-specific nitrosamine (TSNA), as NNK, NNN, NAT and NAB etc., is one of main harmful components of cigarette smoke, produces material impact to the harmfulness index of cigarette product.Tobacco-specific nitrosamine in flue gas is mainly derived from the thermal synthesis of the heat transfer of the tobacco-specific nitrosamine contained by tobacco self and the precursor (as nitrate, nitrite etc.) of tobacco-specific nitrosamine.The tobacco-specific nitrosamine content and the tobacco-specific nitrosamine precursor that reduce tobacco self are the main method reducing tobacco-specific nitrosamine burst size in cigarette smoke.
Papermaking-method reconstituted tobaccos is the restructuring tobacco that application papermaking basic technology is produced, and it has that burn rate is fast, releasing content of coke tar is low, Filling power is high and the feature such as degrading resistance property is good, is the important composition that Modern cigarette industry is filled a prescription.The restructuring tobacco that papermaking-method reconstituted tobaccos is prepared according to the method for papermaking primarily of offal and raw tobacco material, owing to containing a large amount of tobacco-specific nitrosamine precursors such as nitrate, nitrite in offal and offal, simultaneously also containing tobacco-specific nitrosamine, tobacco-specific nitrosamine particularly in burley tobaccos raw tobacco material, this must cause the tobacco-specific nitrosamine burst size in flue gas of papermaking-method reconstituted tobaccos high.Reducing tobacco-specific nitrosamine and precursor thereof in papermaking-method reconstituted tobaccos raw material is the difficult problem urgently to be resolved hurrily promoting papermaking-method reconstituted tobaccos harm reduction quality.
The Modulatory character of reconstituted tobacco chemical constituent and physical parameter is its most outstanding advantage.The current regulation and control for reconstituted tobacco component are added effect group grading mode mainly through the selection of raw material, biochemical treatment and external source and are carried out, but these technology also exist limited in one's ability, the defect such as production operability is weak or processing cost is high of regulation and control tobacco-specific nitrosamine and precursor content thereof, and the application in papermaking-method reconstituted tobaccos is produced is subject to certain restrictions.Current membrane technology is also for the regulation and control of reconstituted tobacco nitrate and nitrite, as CN102524934A, CN101606748A all propose use pressure drive membrane, as microfiltration membranes, milipore filter and NF membrane, remove large biological molecule, nitrate and chlorion, to promote the quality of papermaking-method reconstituted tobaccos, but also there is low, the selective weak and industrialization high in cost of production defect of electrolyte removal efficiency for the removal of ionic compound in pressure drive membrane, its process of industrialization is slow.Electrodialysis is the electric drive membrane technology utilizing ion exchange principle desalination, there is efficient desalting efficiency, good effect is shown in removal NO3-N and NO2-N, as CN103082394A, CN103330277A and US4302308A, US4253929 utilizes the nitrate in electrodialysis methods removal tobacco extract or reconstituted tobacco extract, nitrite and chlorion, certain effect is shown in reduction flue gas tobacco-specific nitrosamine burst size, but the method that these patents provide only has reducing effect to the precursor nitrate of tobacco-specific nitrosamine, the tobacco-specific nitrosamine of thermal synthesis part in flue gas can be reduced, but to tobacco-specific nitrosamine in tobacco extract without reducing effect, the tobacco-specific nitrosamine of heat transfer is influenced hardly.In addition tobacco extract is faintly acid, and the nicotine in tobacco also runs off in a large number in electrodialytic process, the highlyest runs off 85%, and this will cause papermaking-method reconstituted tobaccos to suck the reduction of strength.Therefore how reduce TSNA in tobacco extract and precursor (nitrate) thereof comprehensively and ensure that cigarette sensory quality significantly reduces the problem that flue gas tobacco-specific nitrosamine burst size urgently needs to solve.
Three, summary of the invention
The present invention aims to provide a kind of method utilizing electroosmose process to reduce TSNA and nitrate content in reproduced tobacco concentrated liquid, this method can reduce TSNA in reproduced tobacco concentrated liquid and nitrate simultaneously, a large amount of losses of nicotine can be avoided again simultaneously, while effectively reducing reconstituted tobacco flue gas TSNA burst size, ensure that the sucking quality of reconstituted tobacco.
First the present invention utilizes two step electroosmose process to reduce the content of tobacco-specific nitrosamine in reproduced tobacco concentrated liquids and precursor-nitrate thereof, simultaneously based on the difference of nicotine form under condition of different pH effectively reclaim first time electrodialysis process the nicotine that removes out.
The present invention utilizes the method for TSNA and nitrate content in electroosmose process reduction reproduced tobacco concentrated liquid, and this cleans the method preparing nicotine, and detailed process is as follows:
1) first time electrodialysis desalination process
Be that the reproduced tobacco concentrated liquid of 8-20% is at 10-20A/cm by solid content
2constant current density condition under to carry out first time electrodialysis desalination process to voltage stabilization be 60V, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 1ms/cm;
Described reproduced tobacco concentrated liquid traditionally papermaking-method reconstituted tobaccos production technology prepares, and detailed process is as follows:
A, in extractor, add papermaking-method reconstituted tobaccos raw material and water according to the ratio of weight ratio 1:10, at the temperature of 50-65 DEG C, stir 1h;
B, the compound obtained by step a obtain tobacco extraction liquid through squeezing, filtration, centrifugation successively, and namely the tobacco extraction liquid of gained obtains reproduced tobacco concentrated liquid after 65 DEG C of Vacuum Concentrations, and solid content is 8-20%.
2) second time electrodialysis desalination process
The pH value of the feed liquid obtained after regulating first time electrodialysis desalination process by pH value regulator to 1-3, at 10-20A/cm
2constant current density condition under to carry out electrodialysis desalination process to voltage stabilization be 60V, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 0.5ms/cm;
3) third time electrodialysis desalination process
It is 40-50% that the salting liquid that first time electrodialysis desalination process removes is concentrated into solid content, by pH value regulator adjust ph to 11-12, at 10-20A/cm
2constant current density condition under to carry out electrodialysis desalination process to voltage stabilization be 60V, under 60V voltage stabilizing condition, electrodialysis desalination process is 0.3ms/cm to electrical conductivity, can be used as fertilizer after the salting liquid spraying dry removed;
4) concentrated
The feed liquid obtained after the feed liquid obtained after the process of second time electrodialysis desalination and third time electrodialysis desalination process merged, being concentrated into density is 1.2g/cm
3, obtain low-nitrosamine reproduced tobacco concentrated liquid.
Step 2) described in pH value regulator be one or more in citric acid solution, malic acid solution and oxalic acid solution.
Step 3) described in pH value regulator be one or more in KOH solution, NaOH solution.
Step 1 of the present invention), 2) and 3) in electrodialysis parameters arrange identical: the membrane stack of use is made up of 5 groups of homogeneous-phase anion exchange films and homogeneous phase cation exchange film; The base material of film is Kynoar; Room, pole uses the Na of 0.3mol/L
2sO
4solution.
The nitrate anion in reproduced tobacco concentrated liquid is removed in first time electrodialysis desalination process, also reduces feed liquid simultaneously and is adjusted to the acid acid amount used; The tobacco-specific nitrosamine in papermaking-method reconstituted tobaccos concentrate is removed in the process of second time electrodialysis desalination under strongly acidic conditions; Third time electrodialysis desalination process is to reclaim nicotine, and the accessory substance produced is for the preparation of fertilizer.
Science integration of the present invention make use of concentrate and electrodialytic characteristic, both TSNA and precursor-nitrate thereof had effectively been stripped of, turn avoid the nicotine that conventional electrodialysis process causes to run off in a large number, accessory substance is also utilized effectively simultaneously, synergy, energy-conservation, subtract dirty in etc. in Be very effective, be suitable for industrialized production.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, present invention utilizes the characteristic that electrodialysis desalination efficiency is high, and based on the morphological differences of nicotine under condition of different pH, utilize electroosmose process process feed liquid, both nitrate in efficient removal concentrate, effectively prevent the loss of nicotine simultaneously.
2, the present invention is based on tobacco-specific nitrosamine under the condition of pH<3 in protonated characteristic, two step electroosmose process are utilized to remove TSNA content in concentrate, the method had both effectively reduced the TSNA content in concentrate, also significantly reduced the consumption of acid simultaneously.
3, science integration of the present invention make use of concentrate and electrodialytic characteristic, both TSNA and precursor-nitrate thereof had effectively been stripped of, turn avoid the nicotine that conventional electrodialysis process causes to run off in a large number, accessory substance is also utilized effectively simultaneously, synergy, energy-conservation, subtract dirty in etc. in Be very effective, be suitable for industrialized production.
4, the present invention only increases concentrate electrodialysis process operation on existing papermaking-method reconstituted tobaccos Process ba-sis, does not change other technique, can commercial application fast.
Four, accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Five, detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail, but it is not limitation of the invention.
Embodiment 1:
Utilize electroosmose process to reduce the method for TSNA and nitrate content in reproduced tobacco concentrated liquid in the present embodiment, detailed process is as follows:
1) first time electrodialysis desalination process
Be 5.6 by initial pH value, solid content is that the reproduced tobacco concentrated liquid of 15% is at 10A/cm
2constant current density condition under carry out first time electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 1ms/cm;
Described reproduced tobacco concentrated liquid traditionally papermaking-method reconstituted tobaccos production technology prepares, and detailed process is as follows:
A, in extractor, add papermaking-method reconstituted tobaccos raw material and water according to the ratio of weight ratio 1:10, at the temperature of 50-65 DEG C, stir 1h;
B, the compound obtained by step a obtain tobacco extraction liquid through squeezing, filtration, centrifugation successively, and namely the tobacco extraction liquid obtained obtains reproduced tobacco concentrated liquid after 65 DEG C of Vacuum Concentrations, and solid content is 15%.
2) second time electrodialysis desalination process
The pH value to 2.0 of the feed liquid obtained after regulating first time electrodialysis desalination process by citric acid solution, at 10A/cm
2constant current density condition under carry out electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 0.5ms/cm;
3) third time electrodialysis desalination process
It is 45% that the salting liquid that first time electrodialysis desalination process removes is concentrated into solid content, by KOH solution adjust ph to 12, at 10A/cm
2constant current density condition under carry out electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process is 0.3ms/cm to electrical conductivity, can be used as fertilizer after the salting liquid spraying dry removed;
4) concentrated
The feed liquid obtained after the feed liquid obtained after the process of second time electrodialysis desalination and third time electrodialysis desalination process merged, being concentrated into density is 1.2g/cm
3, solid content is 40%, obtains low-nitrosamine, protonitrate reproduced tobacco concentrated liquid.In obtained low-nitrosamine, protonitrate reproduced tobacco concentrated liquid, NNK, NNN, NAT and NAB content declines 91.2%, 86.3%, 82.1%, 86.9% respectively; Nitrate content reduces by 92.7%; Nicotine only declines 8.6%.
Step 1 of the present invention), 2) and 3) in electrodialysis parameters arrange identical: the membrane stack of use is made up of 5 groups of homogeneous-phase anion exchange films and homogeneous phase cation exchange film; The base material of film is Kynoar; Room, pole uses the Na of 0.3mol/L
2sO
4solution.
Utilize this low-nitrosamine, NNK, NNN, NAT and NAB burst size declines to a great extent in reconstituted tobacco cigarette mainstream flue gas prepared by protonitrate reproduced tobacco concentrated liquid, TSNA total volume has decreased by 83.2%.
Embodiment 2:
Utilize electroosmose process to reduce the method for TSNA and nitrate content in reproduced tobacco concentrated liquid in the present embodiment, detailed process is as follows:
1) first time electrodialysis desalination process
Be 5.2 by initial pH value, solid content is that the reproduced tobacco concentrated liquid of 20% is at 20A/cm
2constant current density condition under carry out first time electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 1ms/cm;
Described reproduced tobacco concentrated liquid traditionally papermaking-method reconstituted tobaccos production technology prepares, and detailed process is as follows:
A, in extractor, add papermaking-method reconstituted tobaccos raw material and water according to the ratio of weight ratio 1:10, at the temperature of 50-65 DEG C, stir 1h;
B, the compound obtained by step a obtain tobacco extraction liquid through squeezing, filtration, centrifugation successively, and namely the tobacco extraction liquid obtained obtains reproduced tobacco concentrated liquid after 65 DEG C of Vacuum Concentrations, and solid content is 20%.
2) second time electrodialysis desalination process
The pH value to 2.5 of the feed liquid obtained after regulating first time electrodialysis desalination process by citric acid solution, at 20A/cm
2constant current density condition under carry out electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 0.5ms/cm;
3) third time electrodialysis desalination process
It is 40% that the salting liquid that first time electrodialysis desalination process removes is concentrated into solid content, by NaOH solution adjust ph to 11, at 20A/cm
2constant current density condition under carry out electrodialysis desalination process and reach stationary value 60V to membrane stack voltage drop, under 60V voltage stabilizing condition, electrodialysis desalination process is 0.3ms/cm to electrical conductivity, can be used as fertilizer after the salting liquid spraying dry removed;
4) concentrated
The feed liquid obtained after the feed liquid obtained after the process of second time electrodialysis desalination and third time electrodialysis desalination process merged, being concentrated into density is 1.2g/cm
3, solid content is 40%, obtains low-nitrosamine, protonitrate reproduced tobacco concentrated liquid.In obtained low-nitrosamine, protonitrate reproduced tobacco concentrated liquid, NNK, NNN, NAT and NAB content declines 83.4%, 76.9%, 78.5%, 77.1% respectively; Nitrate content reduces by 93.8%; Nicotine only declines 12.3%.
Step 1 of the present invention), 2) and 3) in electrodialysis parameters arrange identical: the membrane stack of use is made up of 5 groups of homogeneous-phase anion exchange films and homogeneous phase cation exchange film; The base material of film is Kynoar; Room, pole uses the Na of 0.3mol/L
2sO
4solution.
Utilize this low-nitrosamine, NNK, NNN, NAT and NAB burst size declines to a great extent in reconstituted tobacco cigarette mainstream flue gas prepared by protonitrate reproduced tobacco concentrated liquid, TSNA total volume has decreased by 78.6%.
Claims (8)
1. utilize electroosmose process to reduce a method for TSNA and nitrate content in reproduced tobacco concentrated liquid, it is characterized in that comprising the following steps:
1) first time electrodialysis desalination process
Reproduced tobacco concentrated liquid being carried out under constant current density condition first time electrodialysis desalination process to voltage stabilization is 60V, and under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 1ms/cm;
2) second time electrodialysis desalination process
The pH value of the feed liquid obtained after regulating first time electrodialysis desalination process by pH value regulator is to 1-3, under constant current density condition, carry out electrodialysis desalination process to voltage stabilization is 60V, and under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 0.5ms/cm;
3) third time electrodialysis desalination process
It is 40-50% that the salting liquid that first time electrodialysis desalination process removes is concentrated into solid content, by pH value regulator adjust ph to 11-12, under constant current density condition, carry out electrodialysis desalination process to voltage stabilization is 60V, and under 60V voltage stabilizing condition, electrodialysis desalination process to electrical conductivity is 0.3ms/cm;
4) concentrated
The feed liquid obtained after the feed liquid obtained after the process of second time electrodialysis desalination and third time electrodialysis desalination process is merged, after evaporation and concentration, namely obtains low-nitrosamine reproduced tobacco concentrated liquid.
2. method according to claim 1, is characterized in that:
Step 2) described in pH value regulator be one or more in citric acid solution, malic acid solution and oxalic acid solution.
3. method according to claim 1, is characterized in that:
Step 3) described in pH value regulator be one or more in KOH solution, NaOH solution.
4. method according to claim 1, is characterized in that:
The solid content of described reproduced tobacco concentrated liquid is 8-20%.
5. method according to claim 1, is characterized in that:
Step 1) in the current density of electrodialysis desalination process be 10-20A/cm
2.
6. method according to claim 1, is characterized in that:
Step 2) in the current density of electrodialysis desalination process be 10-20A/cm
2.
7. method according to claim 1, is characterized in that:
Step 3) in the current density of electrodialysis desalination process be 10-20A/cm
2.
8. method according to claim 1, is characterized in that:
Step 1 of the present invention), 2) and 3) in electrodialysis use membrane stack be made up of 5 groups of homogeneous-phase anion exchange films and homogeneous phase cation exchange film, the base material of film is Kynoar; Room, pole uses the Na of 0.3mol/L
2sO
4solution.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105029670A (en) * | 2015-08-28 | 2015-11-11 | 安徽中烟工业有限责任公司 | Method for selectively lowering content of Zn in reconstituted tobacco extract liquor generated through papermaking method |
| CN105077560A (en) * | 2015-08-28 | 2015-11-25 | 安徽中烟工业有限责任公司 | Method for selectively reducing Se content in paper-making process reconstituted tobacco extraction liquid |
| CN105124742A (en) * | 2015-08-28 | 2015-12-09 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Cr in paper-making reconstituted tobacco extraction liquid |
| CN105124743A (en) * | 2015-08-28 | 2015-12-09 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Cd in paper-making reconstituted tobacco extraction liquid |
| CN105146721A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Pb in paper-making method reconstituted tobacco extract liquor |
| CN105148735A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Selective regulation method of nitrate and nitrite in papermaking method reproduced tobacco leaf extract liquor |
| CN105146722A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Hg in paper-making method reconstituted tobacco extract liquor |
| CN105169949A (en) * | 2015-08-28 | 2015-12-23 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of As in papermaking technology reconstructed tobacco leaf extract liquid |
| WO2017197052A1 (en) * | 2016-05-10 | 2017-11-16 | Massachusetts Institute Of Technology | Selective reduction of tobacco-specific nitrosamines and related methods |
| WO2023112927A1 (en) * | 2021-12-14 | 2023-06-22 | 日本たばこ産業株式会社 | Plant extract production method |
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| CN105029670A (en) * | 2015-08-28 | 2015-11-11 | 安徽中烟工业有限责任公司 | Method for selectively lowering content of Zn in reconstituted tobacco extract liquor generated through papermaking method |
| CN105077560A (en) * | 2015-08-28 | 2015-11-25 | 安徽中烟工业有限责任公司 | Method for selectively reducing Se content in paper-making process reconstituted tobacco extraction liquid |
| CN105124742A (en) * | 2015-08-28 | 2015-12-09 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Cr in paper-making reconstituted tobacco extraction liquid |
| CN105124743A (en) * | 2015-08-28 | 2015-12-09 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Cd in paper-making reconstituted tobacco extraction liquid |
| CN105146721A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Pb in paper-making method reconstituted tobacco extract liquor |
| CN105148735A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Selective regulation method of nitrate and nitrite in papermaking method reproduced tobacco leaf extract liquor |
| CN105146722A (en) * | 2015-08-28 | 2015-12-16 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of Hg in paper-making method reconstituted tobacco extract liquor |
| CN105169949A (en) * | 2015-08-28 | 2015-12-23 | 安徽中烟工业有限责任公司 | Method for selectively reducing content of As in papermaking technology reconstructed tobacco leaf extract liquid |
| WO2017197052A1 (en) * | 2016-05-10 | 2017-11-16 | Massachusetts Institute Of Technology | Selective reduction of tobacco-specific nitrosamines and related methods |
| US20170325495A1 (en) * | 2016-05-10 | 2017-11-16 | Massachusetts Institute Of Technology | Selective reduction of tobacco-specific nitrosamines and related methods |
| JP2019518442A (en) * | 2016-05-10 | 2019-07-04 | マサチューセッツ インスティテュート オブ テクノロジー | Selective reduction of tobacco specific nitrosamines and related methods |
| US10383357B2 (en) | 2016-05-10 | 2019-08-20 | Massachusetts Institute Of Technology | Selective reduction of tobacco-specific nitrosamines and related methods |
| WO2023112927A1 (en) * | 2021-12-14 | 2023-06-22 | 日本たばこ産業株式会社 | Plant extract production method |
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