CN104389234B - Cigarette filter tip added with chitosan-graphene oxide composite material - Google Patents

Cigarette filter tip added with chitosan-graphene oxide composite material Download PDF

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Publication number
CN104389234B
CN104389234B CN201410464317.0A CN201410464317A CN104389234B CN 104389234 B CN104389234 B CN 104389234B CN 201410464317 A CN201410464317 A CN 201410464317A CN 104389234 B CN104389234 B CN 104389234B
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graphene oxide
filter tip
shitosan
prepared
composite
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CN201410464317.0A
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Chinese (zh)
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CN104389234A (en
Inventor
高明奇
冯晓民
张展
李明哲
聂聪
鲁平
纪朋
董艳娟
杨金初
王墨染
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河南中烟工业有限责任公司
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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

A kind of cigarette filter adding shitosan-graphene oxide composite material

Technical field

The invention belongs to cigarette filter production technical field, it is related to one kind, for cigarette mainstream flue gas, there is feature absorption The added material of effect, gathers more particularly to a kind of shell to cigarette mainstream flue gas harmful components with efficient absorption ability Sugar-graphene oxide composite material and the cigarette filter using the preparation of this material.

Background technology

Existing cigarette filter adsorbing material species various it has been reported that or application additives of filter tip mainly active charcoal Class, natural material class, mineral material class, biomaterial class, polymerization species etc., but mostly there is addition in above additives of filter tip Greatly, the problems such as adsorption efficiency is low, impact cigarette flavor, service life are short, interpolation form is single and uneven, therefore, filter tip adds Plus the species of agent and addition manner await increasing and develop.

Graphene be a kind of by carbon atom with sp2The two dimensional surface knot in cellular regular hexagon lattice for the hybrid orbital composition The material of structure, its thickness is only the thickness of a carbon atomic layer.Graphene is a kind of preferable atresia adsorbent, adsorption master Occur on its surface, due to its special structure, Graphene has larger specific surface area, there is adsorption capacity greatly simultaneously, Absorption is rapidly it is easy to reclaim with the features such as secondary use, a lot of reports are used as novel absorption material at present.

Graphene oxide is a kind of modified graphene after electrochemistry or acid treatment, except possessing the above-mentioned of common graphite alkene Outside characteristic, abundant hydroxyl, carboxyl and carbon and oxygen functional group are also contained in its surface, easy and hydroxyl, amino, carboxyl isopolarity group shape Become hydrogen bond action, therefore, graphene oxide has good selectivity and makees to conjugated molecule, base, porphyrin and aldehyde ketone molecule etc. With being widely used in sample pre-treatments absorption.

Graphene is also studied in Nicotiana tabacum L. harm reduction technology and is applied, but number of applications and form are all less.Contain Gold etc.(Graphene oxide modified active carbon fiber filters the releaser of cigarette mainstream flue gas, analyzes and tests journal, and 2013,32 (7):851~855)Composite is made graphene oxide-loaded on NACF and is added in cigarette filter, be combined The characterization result of material shows, Load Balanced, and the surface activity site of composite is increased, and adds the Medicated cigarette of this composite Pyrogentisinic Acid, Blausure (German) and aldoketoneses have good selective absorption.Patent CN2013100015888 reports graphite alkenes This carrier, on Carbon fibe or acetate fiber carrier, is added by material load using industry existing dual filter production method To in filter tip, make composite filter tip.

Graphene oxide functionalization is exactly using its defect that surface produces in preparation process and group, it is carried out altogether Valence link or the modification of non-covalent bond, regulate and control it physically or chemically.Xu etc.(Flexible graphene films via The filtration of water-soluble noncovalent functionalized graphene sheets, J Am Chem Soc, 2008,130(18), 5856 ~ 5857)Sulfonated polyaniline and Graphene are carried out non-covalent compound, prepare There is the graphene nanocomposite material of preferable water dispersible, this material mainly utilizes substantial amounts of benzene ring structure and stone on polyaniline Black alkene sp2There is stronger π-π and interact and electrostatic force in structure.Xu etc.(A Graphene Hybrid Material Covalently Functionalized with Porphyrin: Synthesis and Optical Limiting Property, Advanced Materials, 2009,21(12):1275~1279)With graphene oxide as precursor, by covalent Compound, it is combined with graphene oxide using the porphyrin with active amine and realizes functionalization and reduced, successfully prepare porphin Quinoline-graphene complex.Zhao etc.(Morphology and Mechanical Properties of Chitosan/ Graphene Oxide Nanocomposites, 2011,69(10): 1259~1263)It is prepared for shell by solution blended process to gather Sugar-stannic oxide/graphene nano composite, and pass through AFM, the method such as TEM, XRD and tension test is to its form and mechanical property Can be studied, result shows stannic oxide/graphene nano particle good dispersion in chitosan basal body.

At present, although graphene oxide composite material is applied in multiple fields, so far, aoxidize stone Black olefinic functionality composite in field of harm and tar reduction of cigarettes there is not yet Patents and document report, the introduction not yet arrived and should With.

Content of the invention

Present invention aim at providing a kind of cigarette filter shitosan-graphene oxide composite material, should using load The binary combined filter tip that the cellulose embossed paper of composite is prepared with vinegar fiber material can be to being harmful in cigarette mainstream flue gas Point carrying out high-efficient filter removes.

The technical solution used in the present invention is as follows:

A kind of cigarette filter shitosan-graphene oxide composite material is it is characterised in that this composite adopts solution Miscible method preparation, specifically includes following steps:

(1)Prepare the graphene oxide aqueous dispersion that mass concentration is 0.2 mg/mL with ultra-pure water;

(2)Add chitosan into 3%(v/v)Acetic acid aqueous solution in be configured to shell that mass concentration is 2.0 mg/mL and gather Sugar-acetic acid solution;

(3)In the case of constantly stirring, by step(2)In 360 ~ 980 mL shitosans-acetic acid solution be added dropwise over Step(1)In 200 ~ 400 mL graphene oxide aqueous dispersions of middle preparation, and continue to stir 1 h, form shitosan-oxygen Graphite alkene compound suspension.This suspension is further dried and can obtain the shitosan-oxidation stone being easy to preserve for a long time Black alkene composite materials finished product.

Above-mentioned steps(3)In, the mass ratio of graphene oxide in prepared shitosan-graphene oxide composite materials Example is between 2% ~ 10%.

Using the cigarette paper matter filter unit of described shitosan graphene oxide composite material preparation, using following step Suddenly it is prepared from:

(1)The shitosan of preparation-graphene oxide compound suspension is uniformly coated in the way of two-sided brushing The surface of cellulose embossed paper;

(2)By step(1)In be coated with the cellulose embossed paper of shitosan-graphene oxide complex in 40 DEG C of temperature strip Dry under part;The cellulose embossed paper dried can be prepared into cigarette filter paper filter tip unit.

Repeat the above steps(1)、(2), the negative of shitosan in paper filter tip unit-graphene oxide complex can be increased Carrying capacity it is however generally that, in paper filter tip unit in every cigarette filter load shitosan-graphene oxide composite material quality Between 0.5 ~ 6mg, preferably consumption is 5mg.

Cellulose embossed paper be by be purification after cellulose be prepared from, its not only the same with acetate tow to flue gas grain Phase thing has mechanical retention effect, and filter efficiency is far above vinegar fibre, and meanwhile, there is abundant oxy radical on its surface, is suitable to In its area load composite.

Using the binary combined filter tip prepared by described cigarette paper matter filter unit, including cellulose acetate filter unit, papery Filter unit and be wrapped in the outer forming paper outside two sections of filter unit and tipping paper successively.

In described binary combined filter tip it is however generally that, in every convention filter paper filter tip unit weight be 80 ~ 85mg, It is preferably 80mg.

Cigarette filter provided by the present invention shitosan-graphene oxide composite material, in combination with shitosan and The excellent properties of two kinds of adsorbing materials of graphene oxide, using the hydroxyl in surface of graphene oxide, carboxyl, carbonyl and epoxy Between the hydroxyl on group and shitosan surface, the composite with special nature is formed by hydrogen bond action, thus improving Graphene Biocompatibility and the dispersibility in polymeric matrix;The active group simultaneously utilizing two kinds of material surfaces passes through hydrogen The modes such as key, conjugation realize the selective absorption retention to harmful components in cigarette mainstream flue gas.

Cigarette filter provided by the present invention shitosan-graphene oxide composite material addition in filter tip is few In the case of, you can efficient absorption is carried out to volatile aldehyde ketone rush cancer molecule, phenol, HCN, and this composite green ring Protect, no additional murder by poisoning;Its preparation method is simple simultaneously, and raw material is easy to get it is easy to large-scale production and low production cost, thus Field of harm and tar reduction of cigarettes has broad application prospects.

Specific embodiment

With reference to embodiment, the present invention will be further described.

Embodiment 1

Cigarette filter prepared by the present embodiment shitosan-graphene oxide composite material, specifically includes following steps:

(1)Configure the graphene oxide aqueous dispersion of 0.2 mg/mL with ultra-pure water;

(2)Add chitosan into 3%(v/v)Acetic acid aqueous solution in be configured to 2.0 mg/mL shitosan-acetic acid molten Liquid;

(3)In the case of constantly stirring, by step(2)In 980 mL shitosans-acetic acid solution be added dropwise over step (1)In 200 mL graphene oxide aqueous dispersions of middle preparation, and continue to stir 1 h, form shitosan-graphene oxide Compound suspension, this suspension is further dried and can obtain the shitosan-graphene oxide being easy to preserve for a long time and be combined Thing finished material.

Above-mentioned steps(3)The mass ratio of graphene oxide in prepared shitosan-graphene oxide composite materials For 2%.

Using the cigarette paper matter filter unit of above-mentioned shitosan-graphene oxide composite material preparation, using following step Suddenly it is prepared from:

(1)The shitosan of preparation-graphene oxide complex aaerosol solution is uniformly coated with the way of two-sided brushing Surface in cellulose embossed paper;

(2)By step(1)In be coated with the cellulose embossed paper of shitosan-graphene oxide complex in 40 DEG C of temperature strip Dry under part;Routinely step is prepared into paper filter tip unit to the cellulose embossed paper dried.

Repeat the above steps(1)、(2), the load capacity of material in paper filter tip unit can be adjusted.

Using the binary combined filter tip prepared by above-mentioned cigarette paper matter filter unit, including cellulose acetate filter unit, papery Filter unit and be wrapped in the outer forming paper outside two sections of filter unit and tipping paper successively.

In binary combined filter tip described in the present embodiment, in every filter tip, paper filter tip unit weight is 80mg, every filter tip The shitosan being loaded in middle paper filter tip unit-graphene oxide composite materials quality is 5 mg.

Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result See testing result contrast table.

Embodiment 2

The same embodiment of preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material 1, only adjustment 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%.

Using the preparation of described shitosan-graphene oxide composite material cigarette filter preparation process with embodiment 1, often Propping up paper filter tip unit weight in filter tip is 80mg, the shitosan being loaded in paper filter tip unit in every filter tip-oxidation stone Black alkene composite materials quality is similarly 5 mg.

Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result See testing result contrast table.

Embodiment 3

The same embodiment of preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material 1, only adjustment 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%.

Using the preparation of described shitosan-graphene oxide composite material cigarette filter preparation process with embodiment 1, often Propping up paper filter tip unit weight in filter tip is 80mg, the shitosan being loaded in paper filter tip unit in every filter tip-oxidation stone Black alkene composite materials quality is similarly 5 mg.

Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result See testing result contrast table.

Embodiment 4

The same embodiment of preparation method of the shitosan of the cigarette filter prepared by the present embodiment-graphene oxide composite material 1, only adjustment 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%.

Using the preparation of described shitosan-graphene oxide composite material cigarette filter preparation process with embodiment 1, often Propping up paper filter tip unit weight in filter tip is 80mg, the shitosan being loaded in paper filter tip unit in every filter tip-oxidation stone Black alkene composite materials quality is similarly 5 mg.

Prepare finished cigarettes with above-mentioned binary combined filter tip, and do further flue gas inspection analysis.Concrete testing result See testing result contrast table.

The graphene oxide Chitosan Composites that there is provided to illustrate the invention and multiple using its prepared binary Close the harm reduction effect to cigarette mainstream flue gas composition for the filter tip, inventor has done further blank and controlled trial.Concrete condition It is described as follows.

Blank assay:It is provided without any added material, only paper vinegar binary is prepared into fiber embossed paper and acetate tow multiple Close filter tip.And done further flue gas inspection analysis.

Controlled trial 1 preparation cellulose embossed paper used by binary combined filter tip be:0.2 mg/mL graphene oxide is divided Aproll solution is uniformly coated on the surface of cellulose embossed paper, 40 DEG C of drying, other same embodiments in the way of two-sided brushing 1.In every filter tip, paper filter tip unit weight is 80mg, the graphene oxide being loaded in paper filter tip unit in every filter tip Quality of materials is 5 mg.And done further flue gas inspection analysis.

Controlled trial 2 preparation cellulose embossed paper used by binary combined filter tip be:By 2.0 mg/mL shitosans-acetic acid Solution is uniformly coated on the surface of cellulose embossed paper, 40 DEG C of drying in the way of two-sided brushing, and other are with embodiment 1.Often Propping up paper filter tip unit weight in filter tip is 80mg, the chitosan material quality being loaded in paper filter tip unit in every filter tip For 5 mg.And done further flue gas inspection analysis.

Concrete testing result contrast table is as follows.

Data analysiss in table be can be seen that with graphene oxide and shitosan reduction effect to main flume harmful components Really, the former amplitude is relatively large, but after the two is prepared into complex, to the reducing effect of main flume harmful components more Substantially, there is preferable adsorption effect especially for aldoketoneses, little polar molecule compound.Meanwhile, can be seen by data in table Go out, with the increase of graphene oxide mass ratio in shitosan-graphene oxide composite material(Embodiment 1 is to embodiment 4 In composite, the ratio of graphene oxide is continuing to increase), composite improves to harmful components adsorption efficiency, but is directed to not Same harmful components, after the mass ratio of graphene oxide reaches certain value, change is no longer obvious.

In general, graphene oxide has the characteristics such as specific surface area is big, avtive spot is many, and shitosan has preferably Biocompatibility, surface has abundant hydroxyl and amino.Cigarette filter provided by the present invention shitosan-graphene oxide Composite preferably achieves the mutual supplement with each other's advantages of bi-material, when preparing cigarette filter, due to graphene oxide and fiber Plain embossed paper can firmly can be combined by noncovalent interaction, thus composite is difficult for drop-off in filter tip.

Using the binary combined filter tip prepared by shitosan-graphene oxide composite material provided by the present invention, one The problems such as determine to overcome that the adsorption efficiency that traditional filter tip adsorption material exists is low in degree, weaken cigarette flavor, shitosan-oxidation Only graphene oxide solution need to be combined through simply non-covalent with shitosan during graphene composite material preparation, in preparation volume During cigarette filter tip, only composite need to be carried on cellulose embossed paper by way of coating, then routine operation, because And preparation method environmental protection, simple, particularly big with the contact area of flue gas, contact uniformly, thus have preferable Application value.

Claims (2)

1. application in Medicated cigarette for the shitosan-graphene oxide composite material is it is characterised in that by shitosan-graphene oxide After composite is carried on cellulose embossed paper, it is prepared into filter tip application;
Described shitosan-graphene oxide composite material, using the preparation of solution therewith method, specifically includes following steps:
(1)Prepare the graphene oxide aqueous dispersion that mass concentration is 0.2 mg/mL;
(2)Add chitosan into 3%(v/v)Acetic acid aqueous solution in be configured to shitosan that mass concentration is 2.0 mg/mL- Acetic acid solution;
(3)In the case of constantly stirring, by step(2)Middle shitosan-acetic acid solution is added dropwise over step(1)Middle preparation In graphene oxide aqueous dispersion, and continue to stir 1 h, form shitosan-graphene oxide compound suspension;
Step(3)In, in prepared shitosan-graphene oxide composite materials the mass ratio of graphene oxide be 2% ~ 10%.
2. application in Medicated cigarette for the shitosan-graphene oxide composite material as claimed in claim 1 is it is characterised in that this filter Mouth unit is prepared from using following steps:
(1)Prepared shitosan-graphene oxide compound suspension is uniformly coated on fibre in the way of two-sided brushing The surface of the plain embossed paper of dimension;
(2)By step(1)In be coated with the cellulose embossed paper of shitosan-graphene oxide complex under 40 DEG C of temperature conditionss Dry, the cellulose embossed paper after drying is prepared into filter unit.
CN201410464317.0A 2014-09-12 2014-09-12 Cigarette filter tip added with chitosan-graphene oxide composite material CN104389234B (en)

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CN106690404B (en) * 2015-11-18 2018-07-27 中国烟草总公司郑州烟草研究院 Tobacco shred additive and its preparation method and application based on graphene nanocomposite material
CN105361241B (en) * 2015-11-20 2019-07-12 东南大学 A kind of cigarette binary combined filter tip and preparation method thereof filled with graphene oxide
CN106833893A (en) * 2017-02-27 2017-06-13 河南中烟工业有限责任公司 Milk fragrance additive of phenol and its preparation method and application in a kind of reduction cigarette smoke
CN108755268A (en) * 2018-05-29 2018-11-06 宁波亚洲浆纸业有限公司 A kind of moisture-proof coating of paper grade (stock), asphalt board and preparation method thereof
CN109700072B (en) * 2018-12-24 2020-08-28 中国科学技术大学 Biodegradable composite filter tip material capable of regulating and controlling temperature of cigarette filter tip and preparation method thereof

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