CN107080287A - A kind of activated carbon dipping method of modifying and application - Google Patents

A kind of activated carbon dipping method of modifying and application Download PDF

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Publication number
CN107080287A
CN107080287A CN201610086109.0A CN201610086109A CN107080287A CN 107080287 A CN107080287 A CN 107080287A CN 201610086109 A CN201610086109 A CN 201610086109A CN 107080287 A CN107080287 A CN 107080287A
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CN
China
Prior art keywords
activated carbon
modified
cigarette
modifying
acid
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
Application number
CN201610086109.0A
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Chinese (zh)
Inventor
李钢
吴达
刘百战
蔡振波
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Shanghai Tobacco Group Co Ltd
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Shanghai Tobacco Group Co Ltd
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Filing date
Publication date
Application filed by Shanghai Tobacco Group Co Ltd filed Critical Shanghai Tobacco Group Co Ltd
Priority to CN201610086109.0A priority Critical patent/CN107080287A/en
Publication of CN107080287A publication Critical patent/CN107080287A/en
Pending legal-status Critical Current

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Classifications

    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/16Use of materials for tobacco smoke filters of inorganic materials
    • A24D3/163Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/32Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/102Carbon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2258/00Sources of waste gases
    • B01D2258/02Other waste gases
    • B01D2258/0283Flue gases

Abstract

The present invention is provided in a kind of activated carbon dipping method of modifying, the aqueous solution that activated carbon is added to acid, through being drying to obtain modified activated carbon after dipping is modified.The activated carbon dipping method of modifying is directed to the deficiency of the activated carbon modified technology of existing cigarette, the sour method of modifying of activated carbon simple and easy to apply is provided, both it need not pre-process, without by high-temperature high-pressure or the method such as being heated to reflux to activated carbon processing, the specific surface area and micro- mesoporous pore volume of modified activated carbon have significant change.Modified activated carbon prepared by the present invention is applied in cigarette filter, compared with the unmodified activated carbon of commercialization, is obviously improved the aroma quality in flue gas, perfume quantity, flue gas concentration and the flue gas property sent out, and alleviate the dry sensation and excitement of cigarette smoke thoroughly, so as to improve the suction taste of cigarette on the whole.

Description

A kind of activated carbon dipping method of modifying and application
Technical field
The present invention relates to the applied technical field of modified activated carbon, impregnate method of modifying more particularly, to a kind of activated carbon and answer With.
Background technology
First active carbon filter cigarette is released in the fifties by American Tobacco industry, and major tobacco companies have carried out largely afterwards Research work by activated carbon application in cigarette filter.At present, the application of Active carbon composite filter abroad in blended type cigarette has been Through comparative maturity, there are Japan, South Korea, Hungary, Russia and Venezuela etc. in staple market.Japan, South Korea, Europe and Active carbon filter cigarette portion is larger in part South American nations cigarette market, wherein in the cigarette market of two countries of Japan and Korea S, making 95% and 90% or so is more up to the cigarette market occupation rate of Active carbon composite filter.
The domestic research on Active carbon composite filter cigarette is started late, and is started from the end of the eighties, is mainly used in blended type cigarette, Application in Virginian-type cigarette is less.In recent years, although the domestic Virginian-type cigarette product for also occurring in that some active carbon filters, But consumer generally reflects that active carbon filter has harmful effect to the suction taste of Virginian-type cigarette, there is certain dry sensation and excitant, because This active carbon filter not yet large-scale application is in Virginian-type cigarette product.
Filtering of the activated carbon to cigarette smoke is mainly realized by suction-operated:Absorption of the activated carbon to flue gas is mainly thing Reason absorption, is as caused by the surface condensation on activated carbon capillary.In addition to physical absorption, chemisorbed also plays certain Effect.The adsorptivity of activated carbon is mainly what is determined by surface texture properties and surface chemistry, and wherein surface texture properties are determined Determine the physical absorption of activated carbon, surface chemistry influences the chemisorbed of activated carbon.Therefore, the method for modifying of activated carbon is passed through Research, changes its specific surface area and micro- mesoporous ratio, can change absorption property of the activated carbon to flue gas material, and then improve fire-cured tobacco type The suction taste of cigarette.
The content of the invention
The shortcoming of prior art, a kind of activated carbon dipping method of modifying of present invention offer, acid is added by activated carbon in view of the above The aqueous solution in, through being drying to obtain modified activated carbon after dipping is modified.The activated carbon dipping method of modifying is lived for existing cigarette Property charcoal modification technology deficiency there is provided the sour method of modifying of activated carbon simple and easy to apply, need not both pre-process, without passing through High-temperature high-pressure the method such as is heated to reflux to activated carbon processing, and the specific surface area and micro- mesoporous pore volume of modified activated carbon have notable change Change.Modified activated carbon prepared by the present invention is applied in cigarette filter, compared with the unmodified activated carbon of commercialization, is obviously improved cigarette Aroma quality in gas, perfume quantity, flue gas concentration and the flue gas property sent out, and alleviate the dry sensation and excitement of cigarette smoke thoroughly, from And improve the suction taste of cigarette on the whole.
In order to solve the above technical problems, the present invention is achieved by the following technical solutions:
First aspect present invention is provided in a kind of activated carbon dipping method of modifying, the aqueous solution that activated carbon is added to acid, and dipping is modified By being drying to obtain modified activated carbon.
It is preferred that, the acid is citric acid, malic acid, tartaric acid, hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid or acetic acid.More preferably , the acid is citric acid.
It is preferred that, the mass concentration of the sour aqueous solution is 0.1-40%.It is furthermore preferred that the quality of the sour aqueous solution is dense Spend for 5-10%.Even more preferably, the mass concentration of the sour aqueous solution is 5%.
It is preferred that, the mass ratio of the sour aqueous acid medium and the activated carbon is 0.15-60:50.
It is preferred that, dipping modification time is 6-48h.
It is preferred that, dry temperature is 105-150 DEG C, and the dry time is 6-48h.
It is preferred that, the activated carbon is cocoanut active charcoal.Cocoanut active charcoal is using cocoanut shell as raw material, through produced in series technique finishing Work is formed.
The activated carbon dipping method of modifying can be used for the preparation of activated carbon.
Second aspect of the present invention provides modified activated carbon made from any of the above-described described activated carbon dipping method of modifying.
Third aspect present invention provides the application that above-mentioned modified activated carbon is applied in cigarette filter, specifically, is inhaled improving cigarette The application of taste.
Fourth aspect present invention provides the application that above-mentioned modified activated carbon is applied in cigarette filter, specifically, has in reduction cigarette The application of evil composition.
Fifth aspect present invention provides the application that above-mentioned modified activated carbon is applied in cigarette filter, specifically, fragrant improving cigarette The application of gas composition.
Beneficial effects of the present invention:The activated carbon dipping method of modifying of the present invention is directed to the deficiency of the activated carbon modified technology of existing cigarette, The sour method of modifying of activated carbon simple and easy to apply is provided, need not both be pre-processed, without by high-temperature high-pressure or being heated to reflux waiting just Method has significant change to activated carbon processing, the specific surface area and micro- mesoporous pore volume of modified activated carbon.Modification prepared by the present invention Activated carbon application is in cigarette filter, compared with the unmodified activated carbon of commercialization, is obviously improved the aroma quality in flue gas, perfume quantity, Flue gas concentration and the flue gas property sent out, and alleviate the dry sensation and excitement of cigarette smoke thoroughly, so as to improve the suction of cigarette on the whole Taste.
Brief description of the drawings
Fig. 1 is activated carbon scanning electron microscope diagram piece before modified;
Fig. 2 is modified activated carbon scanning electron microscope diagram piece;
Fig. 3 is sensory evaluation figure of the modified activated carbon in cigarette filter.
Embodiment
Illustrate embodiments of the present invention below by way of specific instantiation, those skilled in the art can be as disclosed by this specification Content understand easily the present invention other advantages and effect.The present invention can also add by way of a different and different embodiment To implement or apply, the various details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention God is lower to carry out various modifications or alterations.
Technical scheme is described in detail in conjunction with drawings and examples.
Main method of testing is as follows:
1st, modified activated carbon is tested than surface and pore structure
By full-automatic surface analysis instrument, 120 DEG C of pretreatments, using static volume absorption method and according to langmuir equations, BET equations, BJH models, calculate material BET specific surface area, total pore volume, the parameter such as micropore specific area.
2nd, cigarette is smoked panel test marking
Evaluation table is dissected according to following sense organ to be smoked panel test, to cigarette flavor matter, perfume quantity, flue gas concentration, the flue gas property sent out thoroughly, Harmony, fine and smooth soft degree, miscellaneous gas, comfort level, pleasant impression clean level, strength marking.
Cigarette is smoked panel test 1 2 3 4 5 6
Aroma quality Difference It is poor It is fair Preferably It is good Very well
Perfume quantity Difference It is poor It is fair Preferably It is good Very well
Flue gas concentration Difference It is poor It is fair Preferably It is good Very well
The flue gas property sent out thoroughly Difference It is poor It is fair Preferably It is good Very well
Harmony Difference It is poor It is fair Preferably It is good Very well
Fine and smooth soft degree Difference It is poor It is fair Preferably It is good Very well
Miscellaneous gas Difference It is poor It is fair Preferably It is good Very well
Comfort level Difference It is poor It is fair Preferably It is good Very well
Pleasant impression is clean Difference It is poor It is fair Preferably It is good Very well
Strength It is relatively low It is relatively low It is moderate - - -
Embodiment 1
Taking 50g activated carbons, (French pick up company, BCCplus model cocoanut active charcoals are separately added into different sour of 0.1mol/L After aqueous solution 150mL, the modified 24h of dipping, 24h is dried under the conditions of 120 DEG C, modified activated carbon is made.
Modified activated carbon is tested than surface, test result is shown in Table 1, handled through the different sour aqueous solution of 0.1mol/L Activated carbon afterwards, is changed with being not impregnated with sour activated carbon compared to specific surface area, but change is not notable.
The specific surface area of activated carbon of the table 1 after sour aqueous solution processing different 0.1mol/L
Embodiment 2
By taking citric acid as an example, implementation process is described.
50g activated carbons (French pick up company, BCCplus models activated carbon) are taken to be separately added into the citric acid of different quality concentration Aqueous solution 150mL, after the modified 24h of dipping, 24h is dried under the conditions of 120 DEG C, modified activated carbon is made.
Modified activated carbon is tested than surface and pore structure, test result is shown in Table 2, and modified activated carbon is with citric acid matter Its specific surface area of the change of amount concentration has significant change with total pore volume.
The different quality concentration citric acid-modified active carbon pore structure parameter of table 2
Smoked panel test by cigarette, show that the modified activated carbon effect of the citric acid progress dipping of 5% mass concentration is best.
As Fig. 1 and Fig. 2 (in table 2 mass concentration be activated carbon after 5% citric acid-modified SEM) shown in, the present invention relies on lemon Lemon aqueous acid Immesion active carbon, activity is can be seen that by the activated carbon scanning electron microscope diagram piece before and after citric acid-modified The specific surface area of charcoal and micro- mesoporous pore volume change.
As shown in figure 3, by mass concentration in table 2 be 5% citric acid-modified after activated carbon application in cigarette filter, according to cigarette Sensory evaluation requirement, in aroma quality, perfume quantity, flue gas concentration, the flue gas property sent out thoroughly, harmony, fine and smooth soft degree, miscellaneous gas, Flue gas sense organ is evaluated in terms of comfort level, pleasant impression clean level, strength.Evaluation result shows, the activity with commercialization Charcoal is compared, and the quality of flue gas can be improved using modified certain preferably gone out the activated carbon of the present invention.
According to national standard GB/T 12496.20-1990《Wood activated charcoal method of inspection pH value》To preferred activated carbon and unmodified Activated carbon pH value tested.As a result show, the pH value of unmodified activated carbon is 10.31, and modified certain preferred money is lived Property charcoal pH value be 2.65.It is modified by this method, the pH value significant changes of activated carbon.
Embodiment 3
In order to investigate the actual harm reduction effect of modified activated carbon, 10wt% aqueous citric acid solutions dipping made from embodiment 2 is modified Modified activated carbon afterwards is applied to filter tip cigarette, analysis and overall harmfulness index assessment by 7 kinds of harmful components of cigarette smoke, Check analysis is carried out with unmodified active carbon filter cigarette, 3 are the results are shown in Table, it is seen then that although modified activated carbon specific surface area ratio is not Modified activated carbon is small, but it modified can still obtain preferable harm reduction effect by impregnating;During applied to same brand cigarette, Modified activated carbon is compared with unmodified activated carbon, NH3, NNK, BaP, the content of phenol has decline, meanwhile, overall harm Sex index has declined.
The analysis method of seven kinds of harmful components:CO is analyzed according to GB/T 23356-2009 standards;HCN analysis according to YC/T253-2008 standards;NNK analyses use triplex tandem quadrupole rod gas chromatography mass spectrometry method;NH3Analysis according to YC/T377-2010 standards;BaP is analyzed according to GB/T 2130-2007 standards;Phenol is analyzed according to YC/T255-2008 standards; Crotonaldehyde is analyzed according to YC/T254-2008 standards.
Overall harmfulness index assessment:Quote certainly《Cigarette Evaluation of Harmfulness principle and method》, Beijing, Chemical Industry Press, 2009.09。
The modified activated carbon Harm reduction techniques effect assessment of table 3
Embodiment 4
Further to verify the influence of the property activated carbon to Main Fragrance in cigarette smoke, following experimental program is taken:
In order to ensure practical application, to adding modified activated carbon in filter tip (after mass concentration is 5% citric acid-modified in table 2 30-35mg modified activated carbons are added in activated carbon, every cigarette) and without the cigarette of the same race progress physical testing of activated carbon, It the results are shown in Table 4, it is seen then that total ventilation rate, filter ventilation rates and open resistance to suction are smaller with control sample difference, add this method Modified activated carbon has substantially no effect on the physical property of cigarette.
The cigarette physical testing of table 4
(1) rotating disc type smoking machine smoking cigarette
Before rotating disc type smoking machine smoking cigarette, need first to be balanced cigarette, equilibrium condition is:22 ± 1 DEG C, humidity is 60 ± 2%. Need to hunt leak to smoking machine afterwards, and the projects such as wind speed, pumping volume are debugged.Carried out according to iso standard.Wind Velocity modulation is whole to 20 ± 2cm/s, and pumping volume is adjusted to 35mL, and regulation carries out cigarette smoking after finishing.
(2) it is prepared by Virginian-type cigarette Smoke Particulate sample trapping
The granule phase substance of 20 cigarette is trapped with cambridge filter by rotating disc type smoking machine, filter disc is placed in conical flask, 20mL is added Methyl tert-butyl ether solvent, the full flue gas inner mark solutions of 400 μ L, shake 45 minutes, extract is got in chromatogram bottle, remain into Sample is analyzed.
(3) heartcut two-dimensional gas chromatography/mass spectrography detection Smoke Particulate
Gc/ms Analyser is cut using two-dimensional center, identification and internal standard method have been carried out to flavor component in Smoke Particulate Relative quantification, the results are shown in Table 5.
The flavor component of table 5
As a result show:The activated carbon being modified using this method detects that fragrance component is significantly improved compared with unmodified activated carbon, Meet preferably with smoking result.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any to be familiar with this skill The personage of art all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Therefore, such as Those of ordinary skill in the art without departing from disclosed spirit with completed under technological thought all etc. Modifications and changes are imitated, should be covered by the claim of the present invention.

Claims (10)

1. a kind of activated carbon impregnates method of modifying, it is characterised in that in the aqueous solution that activated carbon is added to acid, through drying after dipping is modified Produce modified activated carbon.
2. activated carbon according to claim 1 impregnates method of modifying, it is characterised in that the acid is citric acid, malic acid, wine Stone acid, hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid or acetic acid.
3. activated carbon according to claim 1 impregnates method of modifying, it is characterised in that the mass concentration of the sour aqueous solution is 0.1-40%.
4. activated carbon according to claim 1 impregnates method of modifying, it is characterised in that the sour aqueous acid medium and the work Property charcoal mass ratio be 0.15-60:50.
5. activated carbon according to claim 1 impregnates method of modifying, it is characterised in that dipping modification time is 6-48h.
6. activated carbon according to claim 1 impregnates method of modifying, it is characterised in that dry temperature is 105-150 DEG C, is done The dry time is 6-48h.
7. modified activated carbon made from the activated carbon dipping method of modifying described in any one of claim 1 to 6.
8. the modified activated carbon described in claim 7 is improving the application of cigarette odor-absorbing.
9. the modified activated carbon described in claim 7 is reducing the application of cigarette harmful components.
10. the modified activated carbon described in claim 7 is improving the application of cigarette flavor composition.
CN201610086109.0A 2016-02-15 2016-02-15 A kind of activated carbon dipping method of modifying and application Pending CN107080287A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108479706A (en) * 2018-04-25 2018-09-04 浙江省林业科学研究院 A kind of modification bamboo charcoal and its preparation method and application
CN109499543A (en) * 2018-10-31 2019-03-22 榆林学院 A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion

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CN104549151A (en) * 2014-12-30 2015-04-29 广东中烟工业有限责任公司 Modification method and application of activated carbon for cigarettes
US20150329364A1 (en) * 2014-05-13 2015-11-19 Georgia-Pacific Chemicals Llc Activated carbon products and methods for making and using same

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US20150329364A1 (en) * 2014-05-13 2015-11-19 Georgia-Pacific Chemicals Llc Activated carbon products and methods for making and using same
CN104549151A (en) * 2014-12-30 2015-04-29 广东中烟工业有限责任公司 Modification method and application of activated carbon for cigarettes

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108479706A (en) * 2018-04-25 2018-09-04 浙江省林业科学研究院 A kind of modification bamboo charcoal and its preparation method and application
CN108479706B (en) * 2018-04-25 2021-04-02 浙江省林业科学研究院 Modified bamboo charcoal and preparation method and application thereof
CN109499543A (en) * 2018-10-31 2019-03-22 榆林学院 A kind of preparation method for the modified activated carbon handling Pb In Exhausted Water ion

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Application publication date: 20170822