CN104389234A - Cigarette filter tip added with chitosan-graphene oxide composite material - Google Patents
Cigarette filter tip added with chitosan-graphene oxide composite material Download PDFInfo
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- CN104389234A CN104389234A CN201410464317.0A CN201410464317A CN104389234A CN 104389234 A CN104389234 A CN 104389234A CN 201410464317 A CN201410464317 A CN 201410464317A CN 104389234 A CN104389234 A CN 104389234A
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Abstract
Belonging to the technical field of cigarette filter tip production, the invention relates to a chitosan-graphene oxide composite material with efficient adsorption capacity on harmful ingredients of cigarette main stream smoke and a cigarette filter tip prepared from the material. The cigarette filter tip is prepared from the chitosan-graphene oxide composite material by a solution miscibility technique. Firstly the chitosan-graphene oxide composite material is prepared into a cigarette paper filter tip unit, and then the cigarette paper filter tip unit is prepared into a binary composite filter tip. Under the circumstance of a very small adding amount into the cigarette filter tip, the chitosan-graphene oxide composite material for cigarette filter tips provided by the invention can realize efficient adsorption of volatile aldehyde and ketone promoting molecules, phenol, HCN and the like. Also, the composite material is green, environment-friendly, and free of additional toxicity. At the same time, the preparation method has the characteristics of simplicity, easily available raw materials, easy scale production and low production cost. Thus, the cigarette filter tip added with the chitosan-graphene oxide composite material has broad application prospects in the harm and tar reduction field of cigarettes.
Description
Technical field
The invention belongs to cigarette filter production technical field, relate to and a kind of for cigarette mainstream flue gas, there is functional adsorbing adding material, relate to a kind of shitosan-graphene oxide composite material that there is efficient adsorption ability to cigarette mainstream flue gas harmful components and the cigarette filter utilizing this material to prepare more specifically.
Background technology
Existing cigarette filter sorbing material is of a great variety, the additives of filter tip reported or apply mainly contains active carbon class, natural material class, mineral material class, biomaterial class, polymer class etc., but the problems such as above additives of filter tip exists mostly, and addition is large, adsorption efficiency is low, affect cigarette flavor, service life is short, interpolation form is single and uneven, therefore, the kind of additives of filter tip and addition manner await increasing and development.
Graphene be a kind of by carbon atom with sp
2the material of the two-dimension plane structure of hybridized orbit composition in cellular regular hexagon lattice, its thickness is only the thickness of a carbon atomic layer.Graphene is a kind of desirable atresia adsorbent, suction-operated mainly occurs in its surface, due to the structure that it is special, Graphene has larger specific area, there is adsorption capacity simultaneously large, absorption rapidly, is easy to the features such as recovery and secondary use, much reports used as novel absorption material at present.
Graphene oxide is a kind of modified graphene after electrochemistry or acid treatment, except the above-mentioned characteristic possessing common graphite alkene, its surface is also containing abundant hydroxyl, carboxyl and carbon and oxygen functional group, easy and hydroxyl, amino, carboxyl isopolarity group form hydrogen bond action, therefore, graphene oxide has good selectively acting to conjugated molecule, base, porphyrin and aldehyde ketone molecule etc., has been widely used in sample pre-treatments absorption.
Graphene have also been obtained investigation and application in tobacco harm reduction technology, but number of applications and form are all less.(the releaser of graphene oxide modified active carbon fiber filtering cigarette mainstream flue gas such as Sheng Jin, analytical test journal, 2013,32(7): 851 ~ 855) on activated carbon fiber, make composite by graphene oxide-loaded and add in cigarette filter, the characterization result display of composite, Load Balanced, and the surface-activity site of composite is increased, and adds the cigarette Pyrogentisinic Acid of this composite, hydrogen cyanide and aldoketones and has good selective absorption.Patent CN2013100015888 reports by Graphene class material load on Carbon fibe or acetate fiber carrier, adopts the existing dual filter production method of industry to add in filter tip by this carrier, makes composite filter tip.
Graphene oxide functionalization is exactly utilize its defect that surface produces in preparation process and group, it is carried out to the modification of covalent bond or non-covalent bond, regulates and controls its physics or chemical property.(the Flexible graphene films via the filtration of water-soluble noncovalent functionalized graphene sheets such as Xu, J Am Chem Soc, 2008,130(18), 5856 ~ 5857) sulfonated polyaniline and Graphene are carried out non-covalent compound, prepare the graphene nanocomposite material with better water dispersible, this material mainly utilizes benzene ring structures a large amount of on polyaniline and Graphene sp
2there is stronger π-π and interact and electrostatic force in structure.(the A Graphene Hybrid Material Covalently Functionalized with Porphyrin:Synthesis and Optical Limiting Property such as Xu, Advanced Materials, 2009,21(12): 1275 ~ 1279) take graphene oxide as precursor, by covalency compound, utilize the band porphyrin of active amine and graphene oxide compound practical function and reduced, successfully preparing porphyrin-graphene complex.(the Morphology and Mechanical Properties of Chitosan/Graphene Oxide Nanocomposites such as Zhao, 2011,69(10): 1259 ~ 1263) prepared shitosan-stannic oxide/graphene nano composite by solution blended process, and pass through AFM, TEM, the method such as XRD and tension test is studied its form and mechanical property, and result shows stannic oxide/graphene nano particle good dispersion in chitosan basal body.
At present, although graphene oxide composite material is applied in multiple field, so far, graphene oxide functional composite material falls burnt field at Harm reduction techniques and there is not yet Patents and bibliographical information, the introduction of not yet arriving and application.
Summary of the invention
The object of the invention is to provide a kind of cigarette filter shitosan-graphene oxide composite material, and the binary combined filter tip utilizing the cellulose embossed paper of this composite of load and vinegar fiber material to prepare can carry out high-efficient filter to the harmful components in cigarette mainstream flue gas and remove.
The technical solution used in the present invention is as follows:
A kind of cigarette filter shitosan-graphene oxide composite material, is characterized in that, this composite adopts solution therewith legal system standby, specifically comprises the following steps:
(1) prepare with ultra-pure water the graphene oxide aqueous dispersion that mass concentration is 0.2 mg/mL;
(2) shitosan is joined 3%(v/v) acetic acid aqueous solution in be mixed with shitosan-acetic acid solution that mass concentration is 2.0 mg/mL;
(3) when constantly stirring, 360 ~ 980 mL shitosan-acetic acid solutions in step (2) are dropwise added in 200 ~ 400 mL graphene oxide aqueous dispersions of preparation in step (1), and continue stirring 1 h, form shitosan-graphene oxide compound suspension.Further for this suspension drying can be obtained and be convenient to the long-term shitosan-graphene oxide composite materials finished product preserved.
In above-mentioned steps (3), in prepared shitosan-graphene oxide composite materials, the mass ratio of graphene oxide is between 2% ~ 10%.
Utilize cigarette paper matter filter unit prepared by described shitosan-graphene oxide composite material, adopt following steps to be prepared from:
(1) shitosan of preparation-graphene oxide compound suspension is coated on uniformly the surface of cellulose embossed paper in the mode of two-sided brushing;
(2) the cellulose embossed paper being coated with shitosan-graphene oxide compound in step (1) is dried under 40 DEG C of temperature conditions; The cellulose embossed paper of drying can be prepared into cigarette filter papery filter unit.
Repeat above-mentioned steps (1), (2), the load capacity of shitosan in paper filter tip unit-graphene oxide compound can be increased, generally speaking, shitosan-graphene oxide composite material the quality of often propping up load in paper filter tip unit in cigarette filter is between 0.5 ~ 6mg, and preferably consumption is 5mg.
Cellulose embossed paper be by be purify after cellulose be prepared from, it is not only the same with acetate tow has mechanical retention effect to Smoke Particulate, and filter efficiency is fine far above vinegar, simultaneously, there is abundant oxy radical on its surface, is suitable at its area load composite.
Utilize the binary combined filter tip prepared by described cigarette paper matter filter unit, comprise cellulose acetate filter unit, paper filter tip unit and the outer forming paper be wrapped in successively outside two sections of filter unit and tipping paper.
In described binary combined filter tip, generally speaking, often propping up paper filter tip unit weight in convention filter is 80 ~ 85mg, is preferably 80mg.
Cigarette filter shitosan-graphene oxide composite material provided by the present invention, combine the excellent properties of shitosan and graphene oxide two kinds of sorbing materials simultaneously, utilize between the hydroxyl on the hydroxyl in surface of graphene oxide, carboxyl, carbonyl and epoxide group and shitosan surface and form the composite with special nature by hydrogen bond action, thus improve the biocompatibility of Graphene and the dispersiveness in polymeric matrix; Utilize the active group of two kinds of material surfaces to realize retaining the selective absorption of harmful components in cigarette mainstream flue gas by the mode such as hydrogen bond, conjugation simultaneously.
Cigarette filter shitosan-graphene oxide composite material provided by the present invention is when in filter tip, addition is few, cancer molecule can be urged to volatile aldehyde ketone, phenol, HCN carry out efficient adsorption, and this composite environmental protection, poison without additional; Its preparation method is simple simultaneously, and raw material is easy to get, and is easy to large-scale production and low production cost, thus falls burnt field at Harm reduction techniques and has broad application prospects.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
embodiment 1
Cigarette filter prepared by the present embodiment shitosan-graphene oxide composite material, specifically comprises the following steps:
(1) the graphene oxide aqueous dispersion of 0.2 mg/mL is configured with ultra-pure water;
(2) shitosan is joined 3%(v/v) acetic acid aqueous solution in be mixed with the shitosan-acetic acid solution of 2.0 mg/mL;
(3) when constantly stirring, 980 mL shitosan-acetic acid solutions in step (2) are dropwise added in 200 mL graphene oxide aqueous dispersions of preparation in step (1), and continue stirring 1 h, form shitosan-graphene oxide compound suspension, further for this suspension drying can be obtained and be convenient to the long-term shitosan-graphene oxide composite materials finished product preserved.
In shitosan prepared by above-mentioned steps (3)-graphene oxide composite materials, the mass ratio of graphene oxide is 2%.
Utilize cigarette paper matter filter unit prepared by above-mentioned shitosan-graphene oxide composite material, adopt following steps to be prepared from:
(1) shitosan of preparation-graphene oxide compound aaerosol solution is coated on uniformly the surface of cellulose embossed paper in the mode of two-sided brushing;
(2) the cellulose embossed paper being coated with shitosan-graphene oxide compound in step (1) is dried under 40 DEG C of temperature conditions; The cellulose embossed paper of drying routinely step is prepared into paper filter tip unit.
Repeat above-mentioned steps (1), (2), the load capacity of material in paper filter tip unit can be adjusted.
Utilize the binary combined filter tip prepared by above-mentioned cigarette paper matter filter unit, comprise cellulose acetate filter unit, paper filter tip unit and the outer forming paper be wrapped in successively outside two sections of filter unit and tipping paper.
In binary combined filter tip described in the present embodiment, often propping up paper filter tip unit weight in filter tip is 80mg, and the shitosan-graphene oxide composite materials quality of often propping up institute's load in paper filter tip unit in filter tip is 5 mg.
Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result is shown in testing result contrast table.
embodiment 2
The preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material is with embodiment 1, and only adjusting graphene oxide aqueous dispersion volume is 300 mL, and adjustment shitosan acetic acid solution volume is 470 mL.
In prepared shitosan-graphene oxide composite materials, the mass ratio of graphene oxide is 6%.
The preparation process of the cigarette filter utilizing described shitosan-graphene oxide composite material to prepare is with embodiment 1, often propping up paper filter tip unit weight in filter tip is 80mg, and the shitosan-graphene oxide composite materials quality of often propping up institute's load in paper filter tip unit in filter tip is similarly 5 mg.
Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result is shown in testing result contrast table.
embodiment 3
The preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material is with embodiment 1, and only adjusting graphene oxide water solution volume is 400 mL, and adjustment shitosan acetic acid solution volume is 460 mL.
In prepared shitosan-graphene oxide composite materials, the mass ratio of graphene oxide is 8%.
The preparation process of the cigarette filter utilizing described shitosan-graphene oxide composite material to prepare is with embodiment 1, often propping up paper filter tip unit weight in filter tip is 80mg, and the shitosan-graphene oxide composite materials quality of often propping up institute's load in paper filter tip unit in filter tip is similarly 5 mg.
Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result is shown in testing result contrast table.
embodiment 4
The preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material is with embodiment 1, and only adjusting graphene oxide water solution volume is 400 mL, and adjustment shitosan acetic acid solution volume is 360 mL.
In prepared shitosan-graphene oxide composite materials, the mass ratio of graphene oxide is 10%.
The preparation process of the cigarette filter utilizing described shitosan-graphene oxide composite material to prepare is with embodiment 1, often propping up paper filter tip unit weight in filter tip is 80mg, and the shitosan-graphene oxide composite materials quality of often propping up institute's load in paper filter tip unit in filter tip is similarly 5 mg.
Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result is shown in testing result contrast table.
For graphene oxide-Chitosan Composites provided by the present invention being described and utilizing the binary combined filter tip prepared by it to the harm reduction effect of cigarette mainstream flue gas composition, inventor has done further blank and check experiment.Concrete condition is described as follows.
Blank test: do not adopt any adding material, is only prepared into paper vinegar binary combined filter tip with fiber embossed paper and acetate tow.And done further flue gas inspection analysis.
Binary combined filter tip cellulose used embossed paper prepared by check experiment 1 is: the surface 0.2 mg/mL graphene oxide aqueous dispersion being coated on uniformly cellulose embossed paper in the mode of two-sided brushing, 40 DEG C of oven dry, other are with embodiment 1.Often propping up paper filter tip unit weight in filter tip is 80mg, and the graphene oxide composite material quality of often propping up institute's load in paper filter tip unit in filter tip is 5 mg.And done further flue gas inspection analysis.
Binary combined filter tip cellulose used embossed paper prepared by check experiment 2 is: the surface 2.0 mg/mL shitosan-acetic acid solutions being coated on uniformly cellulose embossed paper in the mode of two-sided brushing, 40 DEG C of oven dry, other are with embodiment 1.Often propping up paper filter tip unit weight in filter tip is 80mg, and the chitosan material quality of often propping up institute's load in paper filter tip unit in filter tip is 5 mg.And done further flue gas inspection analysis.
Concrete testing result contrast table is as follows.
In his-and-hers watches, data analysis can be found out, graphene oxide and shitosan have reduction effect to main flume harmful components, the former amplitude is relatively large, but after the two is prepared into compound, more obvious to the reduction effect of main flume harmful components, particularly there is good adsorption effect for aldoketones, little polar molecule compound.Simultaneously, as can be seen from data in table, along with the increase (in embodiment 1 to embodiment 4, in composite, the ratio of graphene oxide is continuing to increase) of graphene oxide mass ratio in shitosan-graphene oxide composite material, composite improves harmful components adsorption efficiency, but for different harmful components, after the mass ratio of graphene oxide reaches certain value, change no longer obvious.
Generally speaking, graphene oxide has the characteristics such as specific area is large, avtive spot is many, and shitosan has good biocompatibility, and surface has abundant hydroxyl and amino.Cigarette filter shitosan-graphene oxide composite material provided by the present invention achieves the mutual supplement with each other's advantages of bi-material preferably, when preparing cigarette filter, because graphene oxide and cellulose embossed paper can by noncovalent interaction energy firmly compound, thus composite difficult drop-offs in filter tip.
Utilize the binary combined filter tip prepared by shitosan-graphene oxide composite material provided by the present invention, the adsorption efficiency overcoming the existence of traditional filter tip adsorption material is to a certain extent low, weaken the problems such as cigarette flavor, only need by graphene oxide solution and shitosan through simple non-covalent compound time prepared by shitosan-graphene oxide composite material, when preparing cigarette filter, only need composite be carried on cellulose embossed paper by the mode of coating, then routine operation, thus preparation method's environmental protection, simple, particularly large with the contact area of flue gas, contact evenly, thus there is good application value.
Claims (5)
1. cigarette filter shitosan-graphene oxide composite material, is characterized in that, this composite adopts solution therewith legal system standby, specifically comprises the following steps:
(1) the graphene oxide aqueous dispersion that mass concentration is 0.2 mg/mL is prepared;
(2) shitosan is joined 3%(v/v) acetic acid aqueous solution in be mixed with shitosan-acetic acid solution that mass concentration is 2.0 mg/mL;
(3) when constantly stirring, 360 ~ 980 mL shitosan-acetic acid solutions in step (2) are dropwise added in 200 ~ 400 mL graphene oxide aqueous dispersions of preparation in step (1), and continue stirring 1 h, form shitosan-graphene oxide compound suspension.
2. utilize cigarette filter papery filter unit prepared by shitosan-graphene oxide composite material described in claim 1, it is characterized in that, this paper filter tip unit adopts following steps to be prepared from:
(1) shitosan prepared by claim 1-graphene oxide compound suspension is coated on uniformly the surface of cellulose embossed paper in the mode of two-sided brushing;
(2) dried under 40 DEG C of temperature conditions by the cellulose embossed paper being coated with shitosan-graphene oxide compound in step (1), the cellulose embossed paper after oven dry is prepared into paper filter tip unit.
3. utilize the binary combined filter tip prepared by cigarette filter papery filter unit described in claim 2, it is characterized in that, this filter tip comprises cellulose acetate filter unit, paper filter tip unit and the outer forming paper be wrapped in successively outside two sections of filter unit and tipping paper.
4. binary combined filter tip as claimed in claim 3, it is characterized in that, often propping up paper filter tip unit weight in cigarette filter is 80mg.
5. binary combined filter tip as claimed in claim 4, it is characterized in that, the shitosan-graphene oxide composite material quality of often propping up institute's load in paper filter tip unit in cigarette filter is 5mg.
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