CN101015394A - Filter tip capable of eliminating nitrite amine and phenols in cigarette fume and its making process - Google Patents
Filter tip capable of eliminating nitrite amine and phenols in cigarette fume and its making process Download PDFInfo
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- CN101015394A CN101015394A CN 200710034453 CN200710034453A CN101015394A CN 101015394 A CN101015394 A CN 101015394A CN 200710034453 CN200710034453 CN 200710034453 CN 200710034453 A CN200710034453 A CN 200710034453A CN 101015394 A CN101015394 A CN 101015394A
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- nacf
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Abstract
The invention discloses a making method of filter mouth to reduce harmful material of amine nitrite and phenol in the flue gas of cigarette, which comprises the following steps: adopting common active charcoal fiber as carrier; expanding hole; immersing; dispersing Al(NO3)3) or Fe(NO3)3 or their composition on the carrier; sintering; making modified active charcoal fiber with different-content Al2O3, Fe2O3 and Al2O3-Fe2O3; using the 5-30mg modified active charcoal fiber to make composite filter mouth; fitting for removing tar, NNN, NNK, NAR, NAB, phenol, pyrocatechol, hydroquinone, resorcinol, p-cresol and (p+m)-cresol by 7%, 32%, 63%, 43%, 28%, 25%, 21%, 25%, 36%, 25% and 25%.
Description
Technical field
The present invention relates to a kind of cigarette filter that reduces nitrosamine and aldehydes matter in the cigarette smoke and preparation method thereof.
Background technology
Since the beginning of the sixties, the cigarette manufacturer of the various countries of tobacco business has dropped into great amount of manpower and material resources and a huge sum of money in succession, and extensive and deep research has been carried out in the aspects such as technology, theoretical method and application in practice that reduce harmful substance in the cigarette smoke.Because filter tip can be held back the TPM in the cigarette mainstream flue gas effectively, thereby cigarette filter just becomes the reduction tar content in cigarette of generally employing and a kind of method of other harmful substance.In world wide, development of new filter material and sorbing material improve its absorption property to some harmful smoke compositions, keep the smoking quality of cigarette to be still the main research topic of tobacco circle from now on as far as possible.Granular active carbon is the absorption additive that is generally adopted in filter tip, compare with granular active carbon, NACF has many characteristics: 1, bigger external surface area, adsorption capacity is big, adsorption efficiency is high, adsorption rate is fast. for the 10-100 of granular active carbon doubly; 2, the surface exists more active function groups to be easy to be configured to other reactive groups of harmful components in the selectivity reducing cigarette fume; 3, particularly outstanding to the absorption property of low concentration material; 4, the characteristic that has catalytic gas phase oxidation-reduction reaction.Because it is above that NACF has, and obtained very big application in the environmental protection field.Therefore, utilize the above characteristic of NACF, and carry out suitable modification and can develop a kind of new cigarette harm reduction material.Utilize modified active carbon fiber can effectively reduce tar in the flue gas as the patent CN 03124627.3 before us as the pipe tobacco substitute.It is the cigarette filter of filter material that CN01234329.3 has described with the polyethylene nitrile based active carbon fiber, can effectively reduce tar.CN 200420054775.9 presses close to an end of pipe tobacco or the viscose-based active carbon fiber filter post of one section loaded with nano TiO2 is set at filter-tip middle part at filter tip, can efficiently remove tar, nicotine, benzene, formaldehyde, acetaldehyde and NO in the cigarette smoke
xEtc. harmful substance.CN200510040612.4 is with TiO
2-Pd-Cu based active carbon fiber and acetate fiber or polypropylene fiber are made the cigarette composite filter-tip by certain segmentation scales, and the content of tar, nicotine, carbon monoxide, benzo [a] pyrene and fatty aldehyde material in the cigarette smoke is reduced.
Except that tar, nicotine, carbon monoxide, benzo [a] pyrene and fatty aldehyde material, nitrosamine and aldehydes matter also are harmful substances important in the cigarette smoke.How reducing nitrosamine and aldehydes matter effectively also is the required problem of facing of scientific research personnel of tobacco business.
Summary of the invention
We discover, add in the cigarette filter with the NACF of aluminium oxide, iron oxide or the modification of alumina-ferric oxide composite oxides, make composite filter tip, can significantly remove nitrosamine and phenols harmful substance in the cigarette smoke.
This composite filter tip preferably can reach 17%, 32%, 63%, 43%, 28%, 25%, 21%, 25%, 36%, 25% and 25% respectively to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), phenol, catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
What the purpose of this invention is to provide nitrosamine and aldehydes matter in a kind of selectivity reducing cigarette fume contains cigarette filter of modified active carbon fiber and preparation method thereof.
The objective of the invention is to realize in the following manner:
A kind of filter tip that reduces nitrosamine and phenols harmful substance in the cigarette smoke, contain modified active carbon fiber, modified active carbon fiber is made up of reaming NACF and the composite oxides that load on active component aluminium oxide, iron oxide or alumina-ferric oxide on the reaming NACF, and described reaming NACF is distributed with the mesopore duct of the 2-3 nanometer of 15-25%.
The weight ratio of described active component and reaming NACF is 1～30% for good.
Filter tip is the binary composite filter tip, contains modified active carbon fiber 5-30mg in every filter tip.
The preparation method of modified active carbon fiber wherein is: have the reaming catalyst activity charcoal fiber of ferric nitrate to put into activation furnace load; described ferric nitrate accounts for NACF weight ratio 5-10%; heating rate with 4-6 ℃/minute under nitrogen protection is raised to 850-900 ℃; feeding steam after constant temperature 5-15 minute activates; nitrogen protection was cooled to room temperature, the sample 2N-HNO after coming out of the stove after activation finished
3Washing obtains being distributed with the reaming NACF in mesopore duct of the 2-3 nanometer of 15-25%; With aluminum nitrate or ferric nitrate or both mixed solutions dipping reaming NACF 10-30 hour, after the 100-150 ℃ of oven dry,, obtain modified active carbon fiber at 250～450 ℃ of roasting 4-6 hours.
Filter tip preparation method of the present invention is: prepared modified active carbon fiber is added in the acetate fiber filter tip, make the binary composite filter tip, contain modified active carbon fiber 5-30 milligram in every cigarette filter, the composite filter tip cigarette is become cigarette.
The present invention has the performance of nitrosamine and phenols harmful substance in the selective removal cigarette smoke well, also can reduce tar content in cigarette simultaneously.
Preparation method of the present invention compares with existing technology has following advantage:
Contained modified active carbon fiber has the mesopore duct of the 2-3 nanometer of 15-25% in the filter tip of the present invention, and load has the aluminium oxide of active component, iron oxide and their composite oxides, nitrosamine and aldehydes matter in the filter tip of the preparing energy selective removal cigarette smoke.And preparation technology is simple.
The specific embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further, and the present invention can be the described any embodiment of summary of the invention.
Embodiment 1
With load 5% ferric nitrate (with the NACF benchmark, weight ratio) common NACF is put into activation furnace, heating rate with 5 ℃/minute under the nitrogen protection is raised to 870 ℃, behind the constant temperature 10 minutes, feeding steam activates, time is 100 minutes, and the activation sample that the back nitrogen protection is cooled to after room temperature is come out of the stove that finishes washs with the nitric acid of 2 equivalents, obtains having the reaming NACF of part central hole structure; The reaming NACF has the mesopore duct of 15% 2-3 nanometer.
Embodiment 2
With load 10% ferric nitrate (with the NACF benchmark, weight ratio) common NACF is put into activation furnace, heating rate with 5 ℃/minute under the nitrogen protection is raised to 870 ℃, behind the constant temperature 10 minutes, feeding steam activates, time is 100 minutes, and the activation sample that the back nitrogen protection is cooled to after room temperature is come out of the stove that finishes washs with the nitric acid of 2 equivalents, obtains having the reaming NACF of part central hole structure; The reaming NACF has the mesopore duct of 25% 2-3 nanometer.
Embodiment 3
Under the room temperature, mass concentration 18%Al (NO
3)
3Impregnating volume embodiment 1 gained reaming NACF 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 15% aluminium oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 15 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip falls salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol clearance to tar, N-nitroso and is respectively 15%, 18%, 23%, 35%, 21%, 6%, 10%, 11%.
Embodiment 4
Under the room temperature, mass concentration 18%Al (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 15% aluminium oxide.Prepared modified active carbon fiber is added in the acetate fiber filter tip, make the binary composite filter tip, contain 15 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 15%, 32%, 40%, 43%, 28%, 12%, 14%, 12% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol fall in tar, N-nitroso.
Embodiment 5
Under the room temperature, mass concentration 18%Fe (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 20% iron oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 15 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 17%, 11%, 41%, 21%, 13%, 25%, 11%, 25%, 36%, 21% and 25% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), phenol, catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 6
Under the room temperature, mass concentration 5%Al (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 3% aluminium oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 30 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 9%, 18%, 38%, 27%, 14%, 21%, 17%, 12%, 13% and 8% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 7
Under the room temperature, mass concentration 5%Fe (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 gram 24 hours, 120 ℃ are dried by the fire in the back 450 ℃ of roastings 5 hours, obtain modified active carbon fiber, and this modified active carbon fiber contains 7% iron oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 30 milligrams of NACFs in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 10%, 20%, 44%, 33%, 28%, 21%, 16%, 9%, 9% and 20% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 8
Under the room temperature, mass concentration 30%Al (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 25% aluminium oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 10 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip falls salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol clearance to tar, N-nitroso and is respectively 13%, 7%, 49%, 19%, 9%, 16%, 17%, 14%.
Embodiment 9
Under the room temperature, mass concentration 30%Fe (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 450 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 29% iron oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 10 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 6%, 12%, 63%, 36%, 20%, 19%, 18%, 14%, 25% and 21% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 10
Under the room temperature, mass concentration 18%Al (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 250 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 15% aluminium oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 30 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 7%, 18%, 19%, 23%, 16%, 4%, 15%, 6%, 9%, 4% and 7% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), phenol, catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 11
Under the room temperature, mass concentration 18%Fe (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 250 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 20% iron oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 30 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 11%, 13%, 33%, 15%, 17%, 19%, 12%, 17%, 23%, 19% and 14% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), phenol, catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Embodiment 12
Under the room temperature mass concentration is respectively 10%Al (NO
3)
3And 10%Fe (NO
3)
3Impregnating volume embodiment 2 gained reaming NACFs 5 grams 24 hours 250 ℃ of roastings 5 hours, obtain modified active carbon fiber after 120 ℃ of oven dry, and this modified active carbon fiber contains 8% aluminium oxide and 12% iron oxide.Prepared NACF is added in the acetate fiber filter tip, make the binary composite filter tip, contain 30 milligrams of modified active carbon fibers in every cigarette filter, the composite filter tip cigarette is become cigarette.This composite filter tip is respectively 15%, 30%, 60%, 24%, 25%, 16%, 21%, 20%, 30%, 20% and 24% to the clearance that salt nicotine (NNN), 4-(methyl nitrosamine)-1-(3-pyridine radicals)-1-butanone (NNK), N-nitroso anabasine (NAT), N-nitroso anatabine (NAB), phenol, catechol, hydroquinones, resorcinol, p-Cresol and (adjacent+)-cresols fall in tar, N-nitroso.
Claims (5)
1, a kind of filter tip that reduces nitrosamine and phenols harmful substance in the cigarette smoke, it is characterized in that: contain modified active carbon fiber in the filter tip, modified active carbon fiber is made up of reaming NACF and the composite oxides that load on active component aluminium oxide, iron oxide or alumina-ferric oxide on the reaming NACF, and described reaming NACF is distributed with the mesopore duct of the 2-3 nanometer of 15-25%.
2, reduce the cigarette filter of nitrosamine and aldehydes matter in the cigarette smoke according to one kind of claim 1, it is characterized in that: the weight ratio of active component and reaming NACF is 1～30%.
3, reduce the cigarette filter of nitrosamine and aldehydes matter in the cigarette smoke according to one kind of claim 1, it is characterized in that: filter tip is the binary composite filter tip, contains modified active carbon fiber 5-30mg in every filter tip.
4, a kind of preparation method of modified active carbon fiber: it is characterized in that: have the reaming catalyst activity charcoal fiber of ferric nitrate to put into activation furnace load; described ferric nitrate accounts for NACF weight ratio 5-10%; heating rate with 4-6 ℃/minute under nitrogen protection is raised to 850-900 ℃; feeding steam after constant temperature 5-15 minute activates; nitrogen protection was cooled to room temperature, the sample 2N-HNO after coming out of the stove after activation finished
3Washing obtains the reaming NACF; With aluminum nitrate or ferric nitrate or both mixed solutions dipping reaming NACF 10-30 hour, after the 100-150 ℃ of oven dry,, obtain modified active carbon fiber at 250～450 ℃ of roasting 4-6 hours.
5, a kind ofly reduce that the cigarette filter preparation method of nitrosamine and aldehydes matter is in the cigarette smoke:
There is the reaming catalyst activity charcoal fiber of ferric nitrate to put into activation furnace load; described ferric nitrate accounts for NACF weight ratio 5-10%; heating rate with 4-6 ℃/minute under nitrogen protection is raised to 850-900 ℃; feeding steam after constant temperature 5-15 minute activates; nitrogen protection was cooled to room temperature, the sample 2N-HNO after coming out of the stove after activation finished
3Washing obtains the reaming NACF; With aluminum nitrate or ferric nitrate or both mixed solutions dipping reaming NACF 10-30 hour, after the 100-150 ℃ of oven dry,, obtain modified active carbon fiber at 250～450 ℃ of roasting 4-6 hours; Prepared modified active carbon fiber is added in the acetate fiber filter tip, make the binary composite filter tip, contain modified active carbon fiber 5-30 milligram in every cigarette filter.
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Cited By (6)
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| CN101297715B (en) * | 2008-06-26 | 2011-01-26 | 湖南中烟工业有限责任公司 | Additive agent for reducing aldehydes matter content in cigarette flue gas, production method and application thereof |
| CN102058159A (en) * | 2010-11-30 | 2011-05-18 | 湖南中烟工业有限责任公司 | Cigarette filter additive for selectively reducing main carbonyl compounds in cigarette mainstream smoke as well as preparation and application thereof |
| CN104275157A (en) * | 2014-09-10 | 2015-01-14 | 江苏金聚合金材料有限公司 | Adsorbent for purifying coal ethylene glycol and preparation method of adsorbent for purifying coal ethylene glycol |
| CN106263015A (en) * | 2016-08-30 | 2017-01-04 | 云南中烟工业有限责任公司 | A kind of reduce cigarette smoke phenol the method highlighting its delicate fragrance type main body note |
| CN112841708A (en) * | 2019-12-26 | 2021-05-28 | 深圳市环球绿地新材料有限公司 | Application of spherical carbon in smoke adsorption generated by combustion of tobacco products |
| CN113957740A (en) * | 2020-07-20 | 2022-01-21 | 福建中烟工业有限责任公司 | Method for preparing activated carbon fiber composite paper, obtained paper and application thereof |
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| CN105077577A (en) * | 2015-07-10 | 2015-11-25 | 湖北中烟工业有限责任公司 | Cigarette filter tip additive and manufacturing method thereof |
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| CN101297715B (en) * | 2008-06-26 | 2011-01-26 | 湖南中烟工业有限责任公司 | Additive agent for reducing aldehydes matter content in cigarette flue gas, production method and application thereof |
| CN102058159A (en) * | 2010-11-30 | 2011-05-18 | 湖南中烟工业有限责任公司 | Cigarette filter additive for selectively reducing main carbonyl compounds in cigarette mainstream smoke as well as preparation and application thereof |
| CN104275157A (en) * | 2014-09-10 | 2015-01-14 | 江苏金聚合金材料有限公司 | Adsorbent for purifying coal ethylene glycol and preparation method of adsorbent for purifying coal ethylene glycol |
| CN106263015A (en) * | 2016-08-30 | 2017-01-04 | 云南中烟工业有限责任公司 | A kind of reduce cigarette smoke phenol the method highlighting its delicate fragrance type main body note |
| CN112841708A (en) * | 2019-12-26 | 2021-05-28 | 深圳市环球绿地新材料有限公司 | Application of spherical carbon in smoke adsorption generated by combustion of tobacco products |
| CN113957740A (en) * | 2020-07-20 | 2022-01-21 | 福建中烟工业有限责任公司 | Method for preparing activated carbon fiber composite paper, obtained paper and application thereof |
| CN113957740B (en) * | 2020-07-20 | 2023-06-09 | 福建中烟工业有限责任公司 | Method for preparing activated carbon fiber composite paper, obtained paper and application thereof |
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