CN101234327A - Filter material additive and its preparation - Google Patents
Filter material additive and its preparation Download PDFInfo
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- CN101234327A CN101234327A CNA2008100080725A CN200810008072A CN101234327A CN 101234327 A CN101234327 A CN 101234327A CN A2008100080725 A CNA2008100080725 A CN A2008100080725A CN 200810008072 A CN200810008072 A CN 200810008072A CN 101234327 A CN101234327 A CN 101234327A
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- oleic acid
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Abstract
The invention relates to a filtration material promoter, a manufacturing method and the application thereof; the filtration material promoter comprises triacetin and a nanometer material of the following substances: an oleic acid modified silicon dioxide nanometer material, an oleic acid modified titanium dioxide nanometer material, an oleic acid modified aluminum trioxide nanometer material and an oleic acid modified calcium carbonate nanometer material.
Description
Invention field
The present invention relates to a kind of filter material additive, application and method for making; More specifically, the present invention relates to a kind of filter material additive, application and method for making that is used for absorbing the gas harmful components.
Background technology
In daily life, people contact gas medium usually, for example breathe air etc.But gas often comprises various impurity, and therefore for example various harmful components, help these impurity filterings to human health.For this reason, need to use filtration article, for example filter or breathing mask etc.
One concrete aspect, people find already, smoking brings adverse effect to health: epidemiology survey and experimental study show, smoking can cause the multiple disease incidence rate and the death rate to increase, as acute and chronic tracheae/bronchitis, pneumonia, miocardial infarction, headstroke, comprise many cancers of lung cancer etc.The toxicity that the past people produce when thinking smoking always is from nicotine, but in fact it is not unique toxicant.Cigarette burning is the combustion process of a complexity, there is a large amount of harmful substances in flue gas that is produced and the tar therebetween, as the special nitrosamine of tobacco, condensed-nuclei aromatics and free radical etc., these harmful substances can be directly and attack cells indirectly, be the major reason that gives rise to diseases, smoker's health is brought adverse effect.On the other hand, evidence suggests that passive smoking (flue gas that is produced when being the non-smoker because of the contact smoker smoking) health to the involuntary smoker equally causes adverse effect.Therefore, reduce the harmful components in the tobacco smoke, can alleviate the health hazard that smoking causes.For this purpose, in tobacco products such as cigarette, add filter tip etc.
In the prior art, adopted various filtering materials to make filtration article, be used for the purification of gas medium, for example filtered, its effect and effect are different.But, be used for the filtration article of poisonous substance that filtering tobacco aspiration procedure produces etc., still have further improved necessity, so that absorb this class poisonous substance more fully, be beneficial to human beings'health; Simultaneously, if such filtration article can be made with raw material cheap and easy to get, then can be applied to industrial circle more easily.
On the other hand, along with the development of nanosecond science and technology, it has been found that nano material can realize adsorption function.Yet, because nano-grain is trickle, when being used for the impurity of adsorbed gas, exist to be difficult for defectives such as fixing, fly upward everywhere especially easily, cause pollution, even directly jeopardize operator's health environment.Therefore, how by adopting nano particle to realize gas purification, there are many obstacles.
Summary of the invention
The inventor is surprised to find that, utilizes filter material additive of the present invention, can realize nano material is used for filtering material, is used for gas cleaning, and reaches beyond thought effect.
Therefore, the invention provides a kind of filter material additive, comprise glyceryl triacetate and be selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
The application that the present invention also provides a kind of filter material additive to be used to prepare filtering material, described auxiliary agent comprise glyceryl triacetate and are selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
The present invention also provides a kind of method for preparing filter material additive, comprise with glyceryl triacetate be selected from following a kind of nano material and mix: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
The present invention also provides a kind of method for preparing filtering material, comprises
(1) with glyceryl triacetate be selected from following a kind of nano material and mix: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification;
(2) will mix with a kind of fibrous material by the mixture that (1) obtains.
The specific embodiment
The invention provides a kind of filter material additive, comprise glyceryl triacetate and be selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
In the present invention, glyceryl triacetate is a known product, can buy.
In the present invention, the alundum (Al nano material of the titanium dioxide nano material of the silica nano material of oleic acid modification, oleic acid modification, oleic acid modification and the calcium carbonate nano material of oleic acid modification can adopt known method or similar method to make, for example can make: " oleic acid is to the surface modification of nano SiO 2 particle " (Zongwei Li according to the method for following document, Yongfa Zhu, Surface-modification of SiO
2Nanoparticles with oleic acid, Applied SurfaceScience, 211 (1-4): 215-320,2003) and " surface modification of titania nanoparticles " (Li Zongwei, Zhu Yongfa, Study on the Surface-modification of TiO
2Nanoparticles, ACTA CHIMICA SINICA, 61 (9): 1484-1487,2003).The specific area of nano material is higher than 150m
2/ g preferably is higher than 200m
2/ g more preferably is higher than 250m
2/ g further preferably is higher than 280m
2/ g.
In a preferred embodiment of the invention, in the filter material additive, the content of glyceryl triacetate is 0.05-25 weight % (percentage by weight based on filter material additive (nano material and glyceryl triacetate) total amount, down together), more preferably 0.10-20 weight %, further preferred 0.5-15 weight %, preferred especially 1.0-12 weight %.Preferably, glyceryl triacetate evenly mixes with nano material.
Description for each composition, content and state in the filter material additive, no matter be for the description of their wide sense or for the description of their various preferred meaning, be applicable to that all filtering material of the present invention, filter material additive are used to prepare the application of filtering material, prepare the method for filter material additive and prepare the method for filtering material, wherein the description of preferred meaning is corresponding to corresponding optimal technical scheme separately.
The present invention also provides a kind of filtering material, a kind of filter material additive that comprises a kind of fiber and mix with fiber, described auxiliary agent comprise glyceryl triacetate and are selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
In filtering material of the present invention, fiber can be the fiber that is usually used in this purpose, is preferably the acetate fiber tow.
In a kind of preferred embodiment of filtering material of the present invention, the content of filter material additive is 6-10 weight % based on the total amount of fiber and filter material additive.Preferably, fiber and filter material additive evenly mix.
The present invention also provides a kind of filter material additive to be used to prepare the application of filtering material, described filtering material comprises fiber and filter material additive, and described auxiliary agent comprises glyceryl triacetate and is selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
The present invention also provides a kind of method for preparing filter material additive, comprise with glyceryl triacetate be selected from following a kind of nano material and mix: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
The present invention also provides a kind of method for preparing filtering material, comprises
(1) with glyceryl triacetate be selected from following a kind of nano material and mix: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification makes filter material additive;
(2) will mix with a kind of fibrous material by the filter material additive that (1) obtains.
In the present invention, when nano material is mixed with glyceryl triacetate, can assist in stirring, for example agitator is with rotating speed 100-3,000 rev/min was stirred 10-100 minute, nano particle and glyceryl triacetate is evenly disperseed.
Filtering material of the present invention can be directly used in tobacco product, filter, breathing mask etc. (can be cylindricality, cylindrical shape, cast, particle shape, hollow type, multi-layer planar type or sphere etc.), to remove toxic component and the impurity in flue gas and the gas.Filtering material of the present invention can directly use separately, also can with common filtering material produced with combination composite filter material.
Compare with the contrast cigarette that the filtering material that only uses glyceryl triacetate is made, in the cigarette smoke that makes with filtering material of the present invention NNN, NAT, NAB, NNK four grow tobacco peculiar N-nitrosamine total amount obviously selectivity reduce, the total amount of benzo [a] pyrene, benzo [a] anthracene, three kinds of condensed-nuclei aromatics of also can obviously reduce.
Those skilled in the art can understand, and filtering material of the present invention is cheap and easy to get, and cost that can be lower is realized the filtering of harmful ingredients in flue gas.
Further specify the present invention by the following examples, but they do not constitute limitation of the scope of the invention.
Embodiment
Embodiment 1
With reference to " oleic acid is to the surface modification of nano SiO 2 particle " (Zongwei Li, YongfaZhu, Surface-modification of SiO
2Nanoparticles with oleic acid, Applied SurfaceScience, 211 (1-4): 215-320,2003) (specific area is 180m for the calcium carbonate nano material of the oleic acid modification that makes
2/ g) join in the glyceryl triacetate with 2 weight %, stir with 1,000 rev/min of rotating speed with agitator and made that this nano material is even must to be scattered in the glyceryl triacetate in 30 minutes, obtain filter material additive.
Above-mentioned filter material additive is evenly joined in the acetate fiber tow with 8 weight %, make cigarette acetate fiber filter stick.
With this filter stick and the common acetate fiber filter stick ratio produced with combination combined filtration rod (diameter 7.5mm, length is 25mm) with 15: 10, a section of nano material that contains the oleic acid modified calcium carbonate is near pipe tobacco.
Cigarette is the Zhongnanhai board 8mg cigarette of commercially available BJ Tobacco Factory, remove filter tip, be hinged with the cigarette filter of above-mentioned preparation, cigarette and cigarette smoke are carried out routine (cigarette weight, dilution factor, resistance to suction, puff number, TPM, moisture, releasing content of coke tar, nicotine amount) and special index (4 grow tobacco peculiar N-nitrosamine NNN, NAT, NAB, NNK, 3 kinds of condensed-nuclei aromatics benzos [a] pyrene, benzo [a] anthracene and (Chrysene)) test, the results are shown in Table 2.
(commercially available BJ Tobacco Factory produces Zhongnanhai 8mg cigarette with the contrast cigarette that is labeled as contrast, (auxiliary agent of interpolation only is a glyceryl triacetate with the acetate fiber filter stick with common cigarette, ratio be glyceryl triacetate and acetate fiber tow total amount 8%), filter stick diameter 7.5mm, length is 25mm, down with) relatively, NNN, NAT, NAB, NNK selectivity reduce that percentage is respectively 20.0%, 38.4%, 15.6%, 22.9%, 4 kind of TSNA total amount selectivity reduces by 27.7%; Benzo [a] pyrene, benzo [a] anthracene and selectivity reduce that percentage is respectively 24.4%, 14.6%, 14.8%, 3 kind of PAHs total amount selectivity reduces by 16.5%.
Embodiment 2
Will be by " surface modification of titania nanoparticles " (Li Zongwei, Zhu Yongfa, Studyon the Surface-modification of TiO
2Nanoparticles, ACTA CHIMICA SINICA, 61 (9): 1484-1487,2003) (specific area is 150m for the titanium dioxide nano material of the oleic acid modification that makes
2/ g) join in the glyceryl triacetate with 6 weight %, this nano material was dispersed in glyceryl triacetate in 30 minutes with agitator with 1,000 rev/min of stirring of rotating speed, obtain filter material additive.
Above-mentioned filter material additive is evenly joined in the acetate fiber tow with 8 weight %, make cigarette acetate fiber filter stick.
With this filter stick and common acetate fiber filter stick with 15: 10 length than produced with combination combined filtration rod (diameter 7.5mm, length is 25mm), a section of titanium dioxide nano material that contains the oleic acid modification is near pipe tobacco.
Cigarette is the Zhongnanhai board 8mg cigarette of commercially available BJ Tobacco Factory, remove filter tip, be hinged with the cigarette filter of above-mentioned preparation, cigarette and cigarette smoke are carried out routine (cigarette weight, dilution factor, resistance to suction, puff number, TPM, moisture, releasing content of coke tar, nicotine amount) and special index (4 grow tobacco peculiar N-nitrosamine NNN, NAT, NAB, NNK, 3 kinds of condensed-nuclei aromatics benzos [a] pyrene, benzo [a] anthracene and ) test, the results are shown in Table 2.
With the contrast cigarette relatively, NNN, NAT, NAB, NNK selectivity reduce that percentage is respectively 34.5%, 45.5%, 23.8%, 29.2%, 4 kind of TSNA total amount selectivity reduces by 37.4%; Benzo [a] pyrene, benzo [a] anthracene and selectivity reduce that percentage is respectively 41.9%, 40.5%, 31.5%, 3 kind of PAHs total amount selectivity reduces by 36.2%.
Embodiment 3
With reference to " oleic acid is to the surface modification of nano SiO 2 particle " (Zongwei Li, YongfaZhu, Surface-modification of SiO2 nanoparticles with oleic acid, AppliedSurface Science, 211 (1-4): 215-320,2003) (specific area is 360m to the alundum (Al nano material of the oleic acid modification that makes
2/ g) join in the glyceryl triacetate with 12 weight %, this nano material was dispersed in glyceryl triacetate in 30 minutes with agitator with 1,000 rev/min of stirring of rotating speed, obtain filter material additive.
Above-mentioned filter material additive is evenly joined in the acetate fiber tow with 8 weight %, make cigarette acetate fiber filter stick.
With this filter stick and common acetate fiber filter stick with 15: 10 length than produced with combination combined filtration rod (diameter 7.5mm, length is 25mm), a section of alundum (Al nano material that contains the oleic acid modification is near pipe tobacco.
Cigarette is that the Zhongnanhai board 8mg cigarette of commercially available BJ Tobacco Factory is removed filter tip, be hinged with the cigarette filter of above-mentioned preparation, cigarette and cigarette smoke are carried out routine (cigarette weight, dilution factor, resistance to suction, puff number, TPM, moisture, releasing content of coke tar, nicotine amount) and special index (4 grow tobacco peculiar N-nitrosamine NNN, NAT, NAB, NNK, 3 kinds of condensed-nuclei aromatics benzos [a] pyrene, benzo [a] anthracene and ) test, the results are shown in Table 2.
The results are shown in Table 2.With the contrast cigarette relatively, NNN, NAT, NAB, NNK selectivity reduce percentage be respectively 39.2%, 46.4%, 25.4%, 38.6%,, 4 kinds of TSNAs total amount selectivity reduce by 41.5%; Benzo [a] pyrene, benzo [a] anthracene and selectivity reduce that percentage is respectively 48.9%, 42.6%, 32.2%, 3 kind of PAHs total amount selectivity reduces by 38.5%.
Embodiment 4
Will be by " oleic acid is to the surface modification of nano SiO 2 particle " (Zongwei Li, YongfaZhu, Surface-modification of SiO
2Nanoparticles with oleic acid, Applied SurfaceScience, 211 (1-4): 215-320,2003) (specific area is 287m for the silica nano material of the oleic acid modification that makes
2/ g) with 8.0 weight % (based on the total amount of glyceryl triacetate and nano particle, down together), join in the glyceryl triacetate, use agitator with rotating speed 1,000 rev/min of stirring was dispersed in the glyceryl triacetate this nano material in 30 minutes, obtained filter material additive.
Above-mentioned filter material additive is evenly added the acetate fiber tow with 8 weight % (based on filter material additive and acetate fiber tow total amount, down together), make cigarette acetate fiber filter stick.
(auxiliary agent of interpolation only is a glyceryl triacetate with the acetate fiber filter stick with this plug of filtration material and common cigarette, ratio be glyceryl triacetate and acetate fiber tow total amount 8%) with 15: 10 length than produced with combination combined filtration rod (diameter 7.5mm, length is 25mm), one section of silica nano material that contains the oleic acid modification near pipe tobacco.
Cigarette is the Zhongnanhai board 8mg cigarette of commercially available BJ Tobacco Factory, removes filter tip, is hinged with the cigarette filter of above-mentioned preparation.
Cigarette and cigarette smoke are carried out routine (cigarette weight, dilution factor, resistance to suction, puff number, TPM, moisture, releasing content of coke tar, nicotine amount) and special index (4 grow tobacco peculiar N-nitrosamine NNN, NAT, NAB, NNK, 3 kinds of condensed-nuclei aromatics (PAHs) benzos [a] pyrene, benzo [a] anthracene and ) test, the results are shown in Table 2.
As shown in table 2, (commercially available BJ Tobacco Factory produces Zhongnanhai 8mg cigarette with the contrast cigarette that is labeled as contrast, (auxiliary agent of interpolation only is a glyceryl triacetate with the acetate fiber filter stick with common cigarette, ratio be glyceryl triacetate and acetate fiber tow total amount 8%) filter diameter 7.5mm, length is 25mm) relatively, when adopting filtering material of the present invention to make filter tip, in the cigarette smoke, NNN, NAT, NAB, NNK selectivity reduce percentage be respectively 43.7%, 50.3%, 30.5%, 38.1%,, 4 kinds of TSNAs total amount selectivity reduce by 44.7%; Benzo [a] pyrene, benzo [a] anthracene and selectivity reduce that percentage is respectively 52.1%, 46.2%, 35.4%, 3 kind of PAHs total amount selectivity reduces by 41.9%.
The composition of table 1 filter material additive of the present invention
| Form | Embodiment | |||
| 1 | 2 | 3 | 4 | |
| Glyceryl triacetate | 98％ | 94％ | 88％ | 92％ |
| The nano SiO 2 particle of oleic acid modification | 0 | 0 | 0 | 8％ |
| The alundum (Al nano particle of oleic acid modification | 0 | 0 | 12％ | 0 |
| The titania nanoparticles of oleic acid modification | 0 | 6％ | 0 | 0 |
| The calcium carbonate nano particle of oleic acid modification | 2％ | 0 | 0 | |
Experimental technique
One, (Polycyclic AromaticHydrocarbons, PAHs) assay method of (benzo [a] pyrene (being called for short " B[a] P "), benzo [a] anthracene (being called for short " B[a] A ") and (hereinafter to be referred as " CH ")) of 3 kinds of condensed-nuclei aromatics in the cigarette smoke
1. reagent and instrument
Cyclohexane, n-hexane, absolute ether (being chromatographically pure); Benzo [a] pyrene, benzo [a] anthracene, standard specimen (Fluka company, the U.S.); 9-phenylanthracene standard specimen (Fluka); Tool plug conical flask concentrates bottle; The silica gel solid-phase extraction column; Rotary Evaporators; Varian 3900/Saturn2100T gas chromatograph-mass spectrometer (GC-MS); Elastic quartz capillary tube chromatographic column VF-5MS, 30m * 0.25mm * 0.25 μ m, SM450 type smoking machine (Cerulean company, Britain).
2. the collection of flue gas TPM and preliminary treatment
Before the experiment of used cigarette under (22 ± 1) ℃, relative humidity (60 ± 2) % condition balance 48h, then through weight and resistance to suction sorting, the test cigarette of choosing uniformity props up.
With cigarette sample and cambridge filter in climatic chamber (temperature: 22 ℃ ± 2 ℃, humidity: 60% ± 5) balance after 48 hours according to I SO 4387 smoking cigarettes.Every cambridge filter is collected the flue gas granule phase substance of 5 cigarette.4 filter discs are put into the 100mL conical flask; accurately add 40mL cyclohexane (analyzing pure); mark (9-phenylanthracene in accurately adding; concentration is 200ng/mL) 2mL; ultrasonic extraction 40min; left standstill several minutes; accurately shifting out the 10mL extract is added on the silica gel solid-phase extraction column; make liquid all flow through pillar; and then gradation adds 30mL cyclohexane wash-out; collect all eluents, eluent is concentrated into 0.5mL under nitrogen protection on the Rotary Evaporators, analyze with GC3900/SATURN 2100T gas chromatograph-mass spectrometer (GC-MS).With the cyclohexane is solvent, preparation benzo (a) pyrene, benzo (a) anthracene, , standard serial solution, concentration is 20ng/mL-500ng/mL, and interior mark (9-phenylanthracene) concentration is 200ng/mL, is ordinate with standard specimen and interior target peak area ratio, its concentration ratio is an abscissa, the production standard working curve is obtained equation of linear regression, with the content of 3 kinds of condensed-nuclei aromatics in this experiment with computing sample.
3. look-mass spectral analysis
Instrument condition: chromatographic column: VF-5MS, 30m * 0.25mm * 0.25 μ m; Carrier gas: helium (99.999%), carrier gas constant current: 1.0mL/min, injector temperature: 280 ℃, split sampling: 5: 1, sampling volume; 1.0 150 ℃ of μ L initial temperatures keep 2min to rise to 250 ℃ with 8 ℃/min then and keep 14.5min to rise to 280 ℃ of maintenance 5min with 30 ℃/min then.Trap temperature: 220 ℃ of transmission line temperature: 270 ℃ are adopted the SIS scan mode.
4. the qualitative, quantitative of 3 kinds of condensed-nuclei aromatics in the cigarette smoke TPM
In order to determine the peak position of 3 kinds of condensed-nuclei aromatics, adopt: (1) compares the relative retention time of the chromatographic peak of 3 kinds of condensed-nuclei aromatics standard specimens and sample; (2) 3 kinds of condensed-nuclei aromatics standard specimens are joined in the sample, chromatographic peak is increased; (3) select two ions, calculate and compare in 3 kinds of condensed-nuclei aromatics standard specimens and the abundance ratio of two ions in the sample, carry out qualitative 3 kinds of condensed-nuclei aromatics in the sample.Adopt internal standard method to carry out quantitative analysis.
Two, 4 grow tobacco distinctive nitrosamine (Tobacco SpecificNitrosamines, TSNAs) assay methods of (N-amyl group-(2-pyrrole radicals)-nitrosamine (be called for short NNN), N-nitrosonornicotine (being called for short NNK), N-nitroso anabasine (being called for short NAT), N-nitroso anabasine (being called for short NAB) in the cigarette smoke
1. material, reagent and instrument
Carrene chromatographically pure (or analyzing pure through heavily steaming) methyl alcohol chromatographically pure (or analyzing pure through heavily steaming) anhydrous sodium sulfate is analyzed pure ascorbic acid and is analyzed soda ash aluminium oxide 100-300 order; N-amyl group-(2-pyrrole radicals)-nitrosamine, N-nitrosonornicotine, N-nitroso anabasine, N-nitroso anabasine, 4-(methyl nitrosamino group)-1-(3-pyridine radicals)-1-butanone are the import standard specimen, and purity is greater than 97%.The Varian3900 gas chromatograph; 510 type thermal energy analyzer; SM450 type smoking machine (Cerulean company, Britain); The automatic concentrating instrument of TURBO VAPOR.Glass chromatography column (500mm is long for tool plug, 20mm internal diameter); Assay balance: sensibility reciprocal 0.1mg; Supersonic generator
2. gas-chromatography-thermal energy analyzer (GC-TEA) method is measured the pre-treatment of TSNAs
(1) suction of cigarette
Handle the glass fibre filter disc with ascorbic acid/methanol solution, the 44mm filter disc uses 2mL ascorbic acid/methanol solution (5mg/mL), press YC/T29-1996 (standard name: cigarette, measure TPM and tar with smoking machine) standard conditions behind the filter disc balance 48h and collect the granule phase substance of 20 cigarette with conventional analysis.
(2) sample extraction and concentrated
Filter disc is put into the 250mL conical flask, place in the supersonic generator, divide 3 ultrasonic extractions, for the first time in conical flask, add the 100mL carrene, respectively add 80mL, each ultrasonic extraction 10min all the other twice with carrene.All extracts are filtered behind anhydrous sodium sulfate drying, be transferred in the 500mL ground round-bottomed flask.The round-bottomed flask that fills extract is connected Rotary Evaporators, logical high pure nitrogen rotary evaporation, it is stand-by to be concentrated into about 5mL under 40 ℃.
(3) chromatographic column is prepared
Activation 2h is stand-by down at 110 ℃ for alkali alumina.Chromatographic column keeps clean dried, adds the 30mL carrene earlier, with wet method the 15g alkali alumina is added in the chromatographic column again, stirs aluminium oxide with glass rod and drives all bubbles away.With 50mL carrene elution chromatography post.When dropping to alumina layer, liquid level closes the chromatographic column piston.
(4) column chromatography
Concentrating sample is once added chromatographic column, and with 5mL * 3 washed with dichloromethane flask inwalls.Cleaning solution adds chromatographic column.With 30mL carrene elution chromatography post, do not collect eluent.Use 100mL 8% ethanol/methylene (v/v) eluant solution chromatographic column at last, collect whole eluents.
(5) eluent concentrates
Accurately add the 1mL inner mark solution in eluent, logical high pure nitrogen is concentrated into it about 1mL under 40 ℃, transfers in the 2mL chromatogram bottle stand-by.
3. the GC-TEA qualitative analysis of TSNAs in the cigarette smoke TPM
Through the analytic sample that pre-treatment prepares, adopt capillary gas chromatography-heat energy to analyze combined instrument and carry out Analysis and Identification.Standard sample is mixed with mixed solution, carries out gas chromatographic analysis, determine the relative retention time of each reference material mass peak, the relative retention time with the determinand mass peak of tested flue gas sample compares qualitative then.
4. the GC-TEA quantitative analysis of TSNAs in the cigarette smoke TPM
With the ratio mapping of TSNAs peak area and internal standard area in the comparison chromatogram of the content of four kinds of TSNAs in the standard serial solution and interior scalar, obtain a value (slope) and the b value (intercept) of working curve.The content of 4 kinds of TSNAs in the sample calculates by following formula, gets the test result of the arithmetic mean of instantaneous value of two parallel sample as sample.Content is represented with the nanogram number of the TSNA that contains in every cigarette.
Three, the tar assay method adopts YC/T29-1996 (cigarette standard: cigarette, measure TPM and tar with smoking machine with conventional analysis).
Table 2. contains filtering material cigarette smoke test result
| Embodiment | 1# | 2# | 3# | 4# | Contrast |
| Average weight (g) | 0.867 | 0.874 | 0.876 | 0.880 | 0.878 |
| Puff number | 7.2 | 7.2 | 6.9 | 7.0 | 6.9 |
| TPM (mg/ props up) | 9.03 | 9.74 | 9.47 | 9.70 | 9.31 |
| Moisture (mg/ props up) | 0.50 | 0.58 | 0.27 | 0.41 | 0.66 |
| Tar content (mg/ props up) | 7.75 | 8.32 | 8.37 | 8.47 | 7.79 |
| Tar content rate of change (%) | -0.5 | 6.8 | 7.4 | 8.7 | - |
| Nicotine amount (mg/ props up) | 0.78 | 0.84 | 0.83 | 0.82 | 0.86 |
| Nicotine amount rate of change (%) | -9.3 | -2.3 | -3.5 | -4.7 | - |
| Resistance to suction (Pa) | 1189 | 1216 | 1201 | 1224 | 1221 |
| Resistance to suction rate of change (%) | -2.6 | -0.4 | -1.6 | 0.2 | - |
| Dilution factor (%) | 28.02 | 25.23 | 26.01 | 25.21 | 26.89 |
| Change of initial dilution rate (%) | 4.2 | -6.2 | -3.3 | -6.2 | - |
| NNN content (ng/ props up) | 104.20 | 94.80 | 89.48 | 85.28 | 131.14 |
| NNN reduced rate (%) | 20.5 | 27.7 | 31.8 | 35.0 | - |
| NNN selectivity reduced rate (%) | 20.0 | 34.5 | 39.2 | 43.7 | - |
| NAT content (ng/ props up) | 84.96 | 85.20 | 84.92 | 81.24 | 139.10 |
| NAT reduced rate (%) | 38.9 | 38.7 | 39.0 | 41.6 | - |
| NAT selectivity reduced rate (%) | 38.4 | 45.5 | 46.4 | 50.3 | - |
| NAB content (ng/ props up) | 7.00 | 6.92 | 6.84 | 6.52 | 8.34 |
| NAB reduced rate (%) | 16.1 | 17.0 | 18.0 | 21.8 | - |
| NAB selectivity reduced rate (%) | 15.6 | 23.8 | 25.4 | 30.5 | - |
| NNK content (ng/ props up) | 59.32 | 60.08 | 53.28 | 54.68 | 77.42 |
| NNK reduced rate (%) | 23.4 | 22.4 | 31.2 | 29.4 | - |
| NNK selectivity reduced rate (%) | 22.9 | 29.2 | 38.6 | 38.1 | - |
| Nitrosamine total content (ng/ props up) | 255.4 8 | 247.0 0 | 234.5 2 | 227.7 2 | 356.0 0 |
| Nitrosamine reduced rate (%) | 28.2 | 30.6 | 34.1 | 36.0 | - |
| Nitrosamine selectivity reduced rate (%) | 27.7 | 37.4 | 41.5 | 44.7 | - |
| Benzo [a] anthracene content (ng/ props up) | 14.25 | 11.12 | 10.88 | 10.48 | 16.78 |
| Benzo [a] anthracene reduced rate (%) | 15.1 | 33.7 | 35.2 | 37.5 | - |
| Benzo [a] anthracene selectivity reduced rate (%) | 14.6 | 40.5 | 42.6 | 46.2 | - |
| content (ng/ props up) | 24.16 | 21.48 | 21.45 | 20.89 | 28.51 |
| reduced rate (%) | 15.3 | 24.7 | 24.8 | 26.7 | - |
| selectivity reduced rate (%) | 14.8 | 31.5 | 32.2 | 35.4 | - |
| Benzo [a] pyrene content (ng/ props up) | 8.02 | 6.93 | 6.25 | 6.04 | 10.68 |
| Benzo [a] pyrene reduced rate (%) | 24.9 | 35.1 | 41.5 | 43.4 | - |
| Benzo [a] pyrene selectivity reduced rate (%) | 24.4 | 41.9 | 48.9 | 52.1 | - |
| Condensed-nuclei aromatics total content (ng/ props up) | 46.43 | 39.53 | 38.58 | 37.41 | 55.97 |
| Condensed-nuclei aromatics reduced rate (%) | 17.0 | 29.4 | 31.1 | 33.2 | - |
| Condensed-nuclei aromatics selectivity reduced rate (%) | 16.5 | 36.2 | 38.5 | 41.9 | - |
Claims (6)
1. a filter material additive comprises glyceryl triacetate and is selected from following a kind of nano material: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
2. the filter material additive of claim 1, wherein the specific area of nano material is higher than 150m
2/ g preferably is higher than 200m
2/ g more preferably is higher than 250m
2/ g further preferably is higher than 280m
2/ g.
3. claim 1 or 2 filter material additive, wherein the content of glyceryl triacetate is 0.05-25 weight % based on the total amount of nano material and glyceryl triacetate, more preferably 0.10-20 weight %, further preferred 0.5-15 weight %, preferred especially 1.0-12 weight %.
4. method for preparing filter material additive, comprise with glyceryl triacetate be selected from following a kind of nano material and mix: the calcium carbonate nano material of the titanium dioxide nano material of a kind of silica nano material of oleic acid modification, a kind of oleic acid modification, a kind of alundum (Al nano material of oleic acid modification and a kind of oleic acid modification.
5. the method for claim 4, wherein the specific area of nano material is higher than 150m
2/ g preferably is higher than 200m
2/ g more preferably is higher than 250m
2/ g further preferably is higher than 280m
2/ g.
6. claim 4 or 5 method, wherein the content of glyceryl triacetate is 0.05-25 weight % based on the total amount of nano material and glyceryl triacetate, more preferably 0.10-20 weight %, further preferred 0.5-15 weight %, preferred especially 1.0-12 weight %.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102715655A (en) * | 2011-10-20 | 2012-10-10 | 广西中烟工业有限责任公司 | Cigarette filter stick capable of reducing phenol and crotonaldehyde ingredients in cigarette smoke |
-
2008
- 2008-03-06 CN CN2008100080725A patent/CN101234327B/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102715655A (en) * | 2011-10-20 | 2012-10-10 | 广西中烟工业有限责任公司 | Cigarette filter stick capable of reducing phenol and crotonaldehyde ingredients in cigarette smoke |
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