CN102423138B - Nano porous fiber filter tip additive material for reducing amount of released formonitrile in cigarette smoke, preparation method and application - Google Patents
Nano porous fiber filter tip additive material for reducing amount of released formonitrile in cigarette smoke, preparation method and application Download PDFInfo
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- CN102423138B CN102423138B CN201110209715.4A CN201110209715A CN102423138B CN 102423138 B CN102423138 B CN 102423138B CN 201110209715 A CN201110209715 A CN 201110209715A CN 102423138 B CN102423138 B CN 102423138B
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Abstract
The invention relates to a nano porous fiber filter tip additive material for selectively reducing the amount of released formonitrile in cigarette smoke, a preparation method and application, and the material, the method and the application belong to the field of cigarette harm and tar reduction. The invention is characterized in that the nano fiber material is a porous TiO2 nano fiber with a large special surface and a high length-to-diameter ratio obtained by the electrospinning technology. The nano fiber material can adsorb the formonitrile under the normal temperature, and when being added into a cigarette filter stick, the material can reduce the content of the formonitrile in the mainstream smoke of a cigarette by more than 40 percent, and does not affect the smoking quality of the cigarette. The preparation technique is simple, and the material can be used for selectively reducing the harm of cigarettes.
Description
Technical field
The nanofiber filter tip that the present invention relates to hydrogen cyanide burst size in a kind of selectivity reducing cigarette fume adds material, preparation method and application, belongs to the burnt field of Harm reduction techniques battle array.
Background technology
Hydrogen cyanide is a kind of high volatile volatile extremely toxic substance, to human body threshold value 10ppm only, the activity of inhibitory enzyme after suction human body, be combined with ferricytochrome oxidase, generate cyanocytochromeoxidase, lose the effect of transmitting oxygen, cause the poisoning of histanoxia, health is had to very big harm.The nitrogen-containing compound burning cracking that hydrogen cyanide in cigarette mainly comes from tobacco generates, content is about 30～300 μ g/cig, hydrogen cyanide in flue gas has very big harm to human body after sucking, therefore, how research reduces the hydrogen cyanide in cigarette mainstream flue gas, and the security of raising smoking property of cigarette is significant to health.
At present, the method for abroad for reducing cigarette mainstream flue gas hydrogen cyanide burst size mainly contains: dilution method, absorption method, direct oxidation method and catalytic oxidation.Dilution method makes the loss of cigarette flavor amount larger, affects suction quality.The catalytic temperature higher (as patent CN1416950A and CN1462652A, catalytic temperature requires 250～450 ℃) of catalytic oxidation, is unfavorable for operation.Absorption method removes in the research of hydrogen cyanide, more deep to active carbon research, but active carbon is effectively reducing cigarette smoking quality in absorption flue gas gaseous component, has larger limitation.Therefore, be necessary that development of new material effectively reduces the harmful components in cigarette smoke, do not affect cigarette smoking quality, improve smoking property of cigarette security.
Summary of the invention:
The present invention is directed to above-mentioned prior art not enough, invent and a kind ofly prepare nano-porous fiber material, and be applied to the selective absorption of determination of hydrogen cyanide in mainstream cigarette smoke, guarantee that cigarette smoking quality is unaffected simultaneously.
Another object of the present invention is that invention nano-fiber material is to obtain TiO2 nanofiber by Electrospinning.This Material Addition, in cigarette filter rod, can be reduced to the content of determination of hydrogen cyanide in mainstream cigarette smoke more than 30%, simultaneously on cigarette smoking quality without impact.
The object of the invention is to be achieved through the following technical solutions:
In a kind of selectivity reducing cigarette main flume, the nano-porous fiber filter tip of hydrogen cyanide burst size adds material, it is characterized in that: it is nano titania porous fibrous material that described filter tip adds material, this material be can absorbing acid gases Electrospun porous nano TiO
2fibrous material.
Described nano-porous fiber material is to obtain by Electrospinning the porous TiO having compared with high-ratio surface and draw ratio
2nanofiber, titanium dioxide nanofiber material has loose structure, and its specific area is 65～118m
2/ g.
The diameter of described poriferous titanium dioxide nano-fiber material is 50～500 nanometers, and length is 100～1000 microns.
In selectivity reducing cigarette main flume, the nano-porous fiber filter tip of hydrogen cyanide burst size adds a material preparation method, it is characterized in that: filter tip adds material to be prepared by Electrospinning, and concrete steps are as follows:
(1), 0.8～2.0g tetraisopropyl titanate presoma is joined in 2.0～4.0mL absolute ethyl alcohol, and add isopyknic acetic acid, drying condition lower magnetic force stirs it is mixed, and preferred tetraisopropyl titanate quality is 1.5g, and the volume of absolute ethyl alcohol and acetic acid is 3mL;
(2), by 0.30～0.60g polyvinylpyrrolidone (PVP) solution, join in 2.0～4.0mL ethanol, the quality of preferably polyethylene pyrrolidones is 0.45g, ethanol volume is 3mL, under drying condition, stir and obtain homogeneous phase solution, and the macromolecule homogeneous phase solution obtaining is joined in TiO 2 precursor solution prepared by step (1) fast, under drying condition, stir 30～90min, optimize mixing time 60min;
(3), the solution of preparation in above-mentioned steps (2) is joined in syringe, between control work receiving pole and syringe needle, voltage is 8.0～14KV, optimization voltage is 10KV, regulating receiver and spinning syringe needle distance is 8～12cm, the rate of outflow of solution is 0.2～0.8mL/h, the optimization rate of outflow is 0.5mL/h, take aluminium cover as anode, aluminium foil is that negative electrode receives product, then by minus plate, obtain containing the nano fibrous membrane of PVP template at 400～700 ℃ of sintering 2～5h to remove macromolecule template, obtain poriferous titanium dioxide nano-fiber material.
In step (2), its optimization calcining heat of nano fibrous membrane and time are respectively 450 ℃ and 3h.
Application choice reduces the Electrospun porous nano TiO of determination of hydrogen cyanide in mainstream cigarette smoke burst size
2fibrous material adds material as filter tip, it is characterized in that Electrospun porous nano titania fiber Material Addition in filter tip, for reducing the burst size of the hydrogen cyanide in cigarette mainstream flue gas.
The application of the Electrospun porous nano titania fiber material of the hydrogen cyanide burst size in selectivity reducing cigarette main flume, it is characterized in that by this Electrospun porous nano titania fiber add to cigarette filter rod in, composite filter cigarette is become to cigarette.
The application of the Electrospun porous nano titania fiber material of the hydrogen cyanide burst size in selectivity reducing cigarette main flume, its feature with every cigarette filter in the amount of the porous nano titania fiber that adds be 5～30mg.
The invention provides filter tip interpolation material has the following advantages:
1. this poriferous titanium dioxide nanofiber surface has abundant basic sites, and has stronger hydrogen bond action with hydrogen cyanide, therefore can effectively remove the hydrogen cyanide in flue gas.
2. the TiO 2 porous nano material that the present invention is prepared by Electrospinning makes to adsorb substrate specific area and enlarges markedly, and promotes sorbing material fully to contact with hydrogen cyanide, improves adsorption efficiency;
3. this patent contrivance effectively adsorbs the hydrogen cyanide in main flume, reduces and reaches more than 40%;
4. because titanium dioxide nanofiber length is at 100～1000 microns, there is very large draw ratio, add that filter tip sucks the stopping of conventional cellulose acetate filter rod of end, so this nanofiber is combined stablely with acetate silk, can not be inhaled into human body.
5. this patent contrivance has no adverse effects to cigarette smoking quality.
6. technology of preparing of the present invention is simple, and this material can be used for cigarette selective harm reduction, and this Material Addition, in cigarette filter, can effectively be adsorbed to the hydrogen cyanide in main flume, does not affect cigarette smoking quality simultaneously.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of institute's operative installations in step (3); Wherein: 1, syringe, 2, syringe needle, 3, high voltage source, 4, receive aluminium foil.
Fig. 2 is the electron scanning micrograph of the nano-porous fiber material prepared of the method for embodiment 1.
The specific embodiment:
In a kind of selectivity reducing cigarette main flume of the present invention, the nano-porous fiber filter tip of hydrogen cyanide burst size adds material, it is characterized in that: it is nano titania porous fibrous material that described filter tip adds material, this material be can absorbing acid gases Electrospun porous nano TiO
2fibrous material.
Described nano-porous fiber material is to obtain by Electrospinning the porous TiO having compared with high-ratio surface and draw ratio
2nanofiber, titanium dioxide nanofiber material has loose structure, and its specific area is 65～118m
2/ g.
The diameter of described poriferous titanium dioxide nano-fiber material is 50～500 nanometers, and length is 100～1000 microns.
Preparation method's concrete steps of the present invention are as follows:
1,0.8～2.0g tetraisopropyl titanate presoma is joined in 2.0～4.0mL absolute ethyl alcohol, and add isopyknic acetic acid, drying condition lower magnetic force stirs it is mixed.Preferred tetraisopropyl titanate quality is 1.5g, and the volume of absolute ethyl alcohol and acetic acid is 3mL;
2, by 0.30～0.60g polyvinylpyrrolidone (PVP) solution, join in 2.0～4.0mL ethanol, the quality of preferably polyethylene pyrrolidones is 0.45g, ethanol volume is 3mL, under drying condition, stir and obtain homogeneous phase solution, and the macromolecule homogeneous phase solution obtaining is joined in TiO 2 precursor solution prepared by step (1) fast, under drying condition, stir 30～90min, optimize mixing time 60min;
3, the solution of preparation in above-mentioned steps (2) is joined in syringe, between control work receiving pole and syringe needle, voltage is 8.0～14KV, optimization voltage is 10KV, regulating receiver and spinning syringe needle distance is 8～12cm, the rate of outflow of solution is 0.2～0.8mL/h, and the optimization rate of outflow is 0.5mL/h.Take aluminium cover as anode, aluminium foil is that negative electrode receives product, then by minus plate, obtain containing the nano fibrous membrane of PVP template at 400～700 ℃ of sintering 2～5h to remove macromolecule template, obtain poriferous titanium dioxide nano-fiber material, it optimizes calcining heat and the time is respectively 450 ℃ and 3h;
Application choice reduces the Electrospun porous nano TiO of determination of hydrogen cyanide in mainstream cigarette smoke burst size
2fibrous material adds material as filter tip, it is characterized in that Electrospun porous nano titania fiber Material Addition in filter tip, for reducing the burst size of the hydrogen cyanide in cigarette mainstream flue gas.
By this Electrospun porous nano titania fiber add to cigarette filter rod in, composite filter cigarette is become to cigarette.With the amount of the porous nano titania fiber adding in every cigarette filter be 5～30mg.
Embodiment 1:
Material preparation:
1.1.5g tetraisopropyl titanate, 3mL ethanol and 3mL acetic acid magnetic agitation 10min;
2. in above-mentioned homogeneous phase solution, add PVP solution (0.45g PVP is dissolved in 3mL ethanol), continue to stir 1h.
3. above-mentioned precursor solution is joined in syringe, controlling voltage between work receiving pole and syringe needle is 10KV, and regulating receiver and spinning syringe needle distance is 10cm, and the rate of outflow of solution is 0.5mL/h.
4. the titania fiber preparing is placed in Muffle furnace in 450 ℃ of calcining 3h, after calcining, obtains Electrospun nano titania porous fibrous material.The specific surface of the nanofiber finally obtaining characterizes by nitrogen adsorption (Sorptomatic1990 Full-automatic physical and chemical adsorption instrument), and its specific area is 98m
2/ g, its pattern, length and diameter characterize (as shown in Figure 2) by SEM (JSM-7401 field emission scanning electron microscope, Japan).
Electrospun nano titania porous fibrous material is used as composite filter tip addition material, addition is 8mg/cig, the cigarette that does not add any filter tip adsorption material of take is control sample, according to standard aspiration condition, on smoking machine, carry out cigarette smoking test, and according to standard YCT253-2008, carry out the detection of hydrogen cyanide burst size.Three of each sample Duplicate Samples, result is as shown in table 1.
Table 1 Electrospun titanium dioxide nano material addition 8mg/cig
Application process of the present invention is: the acetate fibres that this Electrospun porous nano titania fiber is scattered in to cigarette filter rod is intrafascicular, makes cigarette binary combined filter tip, in every cigarette filter, adds 5～30mg, and composite filter cigarette is become to cigarette.
Filter tip of the present invention adds material take diameter as 50～500 nanometers, and length is that the form of the nanofiber of 100～1000 microns is made cigarette binary combined filter tip, in every cigarette filter, adds 5～30mg, can effectively reduce hydrogen cyanide content in main flume.
Embodiment 2: material preparation method is with embodiment 1, Electrospun nano titania porous fibrous material is used as composite filter tip addition material, addition is 30mg/cig, the cigarette that does not add any filter tip adsorption material of take is control sample, according to standard aspiration condition, on smoking machine, carry out cigarette smoking test, and carry out the detection of hydrogen cyanide burst size according to standard YCT253-2008.Three of each sample Duplicate Samples, shown in result table 2.
Table 2 Electrospun titanium dioxide nano material addition 30mg/cig
The above results shows, material of the present invention can be used for the production of composite filter tip cigarette, can reduce cigarette mainstream flue gas hydrogen cyanide burst size more than 40%, do not affect cigarette smoking quality simultaneously, and material is prepared simple and easy, can be used for suitability for industrialized production.
Claims (5)
1. the Electrospun porous nano TiO of hydrogen cyanide burst size in a selectivity reducing cigarette main flume
2fibrous material adds the application of material as filter tip, it is characterized in that Electrospun porous nano titania fiber Material Addition in filter tip, for reducing the burst size of the hydrogen cyanide in cigarette mainstream flue gas;
Described porous nano titania fiber material be can absorbing acid gases Electrospun porous nano TiO
2fibrous material;
Described nano-porous fiber material is to obtain by Electrospinning the porous TiO having compared with high-ratio surface and draw ratio
2nanofiber, titanium dioxide nanofiber material has loose structure, and its specific area is 65～118 m
2/ g;
The diameter of described poriferous titanium dioxide nano-fiber material is 50～500 nanometers, and length is 100～1000 microns.
2. the application of the Electrospun porous nano titania fiber material of the hydrogen cyanide burst size in selectivity reducing cigarette main flume according to claim 1, it is characterized in that this Electrospun porous nano titania fiber to add in cigarette filter rod, cigarette filter rod cigarette is become to cigarette.
3. according to the application of the Electrospun porous nano titania fiber material of the hydrogen cyanide burst size in selectivity reducing cigarette main flume described in claim 1 or 2, it is characterized in that the amount of the porous nano titania fiber that adds in every cigarette filter is 5～30 mg.
4. in selectivity reducing cigarette main flume, the nano-porous fiber filter tip of hydrogen cyanide burst size adds a material preparation method, it is characterized in that: filter tip adds material to be prepared by Electrospinning, and concrete steps are as follows:
(1), 0.8～2.0 g tetraisopropyl titanate presoma is joined in 2.0～4.0 mL absolute ethyl alcohols, and add isopyknic acetic acid, drying condition lower magnetic force stirs it is mixed,
(2), by 0.30～0.60 g polyvinylpyrrolidone PVP solution, join in 2.0～4.0 mL ethanol, under drying condition, stir and obtain homogeneous phase solution, and the macromolecule homogeneous phase solution obtaining is joined in TiO 2 precursor solution prepared by step (1) fast, under drying condition, stir 30～90 min;
(3), the solution of preparation in above-mentioned steps (2) is joined in syringe, between control work receiver and spinning syringe needle, voltage is 8.0～14 KV, regulating receiver and spinning syringe needle distance is 8～12 cm, the rate of outflow of solution is 0.2～0.8 mL/h, take aluminium cover as anode, aluminium foil is that negative electrode receives product, then by minus plate, obtain containing the nano fibrous membrane of PVP template at 400～700 ℃ of sintering 2～5 h to remove macromolecule template, obtain poriferous titanium dioxide nano-fiber material.
5. in selectivity reducing cigarette main flume according to claim 4, the nano-porous fiber filter tip of hydrogen cyanide burst size adds material preparation method, it is characterized in that:
In step (1), tetraisopropyl titanate quality is 1.5 g, and the volume of absolute ethyl alcohol and acetic acid is 3 mL;
In step (2), the quality of polyvinylpyrrolidone is 0.45g, and ethanol volume is 3mL, mixing time 60 min,
In step (3), its calcining heat of nano fibrous membrane and time are respectively 450 ℃ and 3 h,
In step (3), voltage is 10 KV, and the rate of outflow is 0.5 mL/h.
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| TWI511929B (en) * | 2012-06-29 | 2015-12-11 | Univ Nat Yunlin Sci & Tech | Method of fabricating titanium dioxide fibers and photocatalystic purification installation |
| CN103693681A (en) * | 2013-12-11 | 2014-04-02 | 贵州中烟工业有限责任公司 | Method for preparing super-long titanate micro/nanotubes |
| CN105155350B (en) * | 2015-08-04 | 2017-03-29 | 浙江中烟工业有限责任公司 | Nanofiber extrusion coating paper of crotonic aldehyde and its preparation method and application in a kind of reduction flue gas |
| CN107227502A (en) * | 2016-03-23 | 2017-10-03 | 张国勇 | A kind of electrostatic spinning formula of liquid of composite air filtering material |
| CN106418689B (en) * | 2016-09-28 | 2022-07-05 | 北京科技大学 | Cigarette holder and preparation method thereof |
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| CN101239737A (en) * | 2008-02-29 | 2008-08-13 | 中国科学院理化技术研究所 | Titanium dioxide thin film material with hierarchical structure and preparation method thereof |
| CN101428852A (en) * | 2008-12-05 | 2009-05-13 | 中国科学院化学研究所 | Method for producing ultra-dewatering titanium dioxide film with electrostatic spinning |
| CN101649502A (en) * | 2009-09-16 | 2010-02-17 | 清华大学 | Method for preparing mesoporous microsphere compound polymer fiber by electrospinning |
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| CN101239737A (en) * | 2008-02-29 | 2008-08-13 | 中国科学院理化技术研究所 | Titanium dioxide thin film material with hierarchical structure and preparation method thereof |
| CN101428852A (en) * | 2008-12-05 | 2009-05-13 | 中国科学院化学研究所 | Method for producing ultra-dewatering titanium dioxide film with electrostatic spinning |
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