CN104815630A - Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol - Google Patents
Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol Download PDFInfo
- Publication number
- CN104815630A CN104815630A CN201510193006.XA CN201510193006A CN104815630A CN 104815630 A CN104815630 A CN 104815630A CN 201510193006 A CN201510193006 A CN 201510193006A CN 104815630 A CN104815630 A CN 104815630A
- Authority
- CN
- China
- Prior art keywords
- graphene
- fiber
- graphene oxide
- add
- filter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol. The preparation method comprises the steps of firstly, performing oxidation treatment on graphite to obtain graphene oxide, performing ultrasonic treatment on the graphene oxide to prepare an aqueous solution or preparing a mixed aqueous solution from the graphene oxide with chitosan, next, dipping the fibers into the aqueous solution of the graphene oxide or in the mixed solution of the graphene oxide and the aqueous solution of the chitosan, drying in vacuum for 6 hours at 80 DEG C, and finally, obtaining the filter tip fibers. According to the preparation method, the chitosan is evenly attached on the surface of the fibers and a remarkable effect of reducing phenol harmful substances can be achieved. Meanwhile, due to strong Pi-Pi interaction between the graphene and the benzopyrene, the graphene modified filter tip is capable of effectively retaining the strong carcinogenic substance benzopyrene in the smoke of cigarette. The preparation method is simple, relatively high in efficiency and low in environmental pollution; meanwhile, the fibers can be modified after the graphene and the chitosan are compounded, and the synergistic effect of the graphene and the chitosan in removing arene harmful substances can be developed; as a result, the preparation method has favorable application prospect.
Description
Technical field
The present invention relates to the preparation method of composite, more particularly the preparation method of the filter fiber of a kind of selective absorption BaP and phenol.
Background technology
At present, exploration new material, the application of new technology in cigarette filter get more and more, and the low tar Less harmful cigarette preparing high-quality and safety is the general trend of international cigarette product development.General filter tip can filter out the total particulate in flue gas, reduces the intake of coke tar in cigarette.Research shows, the adsorbents such as a certain amount of active carbon, sepiolite, zeolite, activated alumina, clay, silica gel are added in filter tip, can optionally filter part gas gas-phase objects and low-boiling volatile harmful material, then can not selective filtering to non-volatile and that boiling point is higher volatile materials (as strong carcinogen BaP).
Shitosan is a kind of natural polymers, China all uses the shitosan of tens tons every year in production of cigarettes, but mainly as the adhesive of reconstituted tobacoo processing and fabricating, also there are some researchers shitosan to be used for filter tip to investigate the filtration result to nicotine in cigarette smoke and tar.Due to cationic amino being with by shitosan side chain, can the optionally harmful substance such as tar adsorption, carbon monoxide, heavy metal, but nicotine can not synchronously reduce, therefore side-stream smoke oxious component can be reduced, reduce excitant, thus effectively reduce the pollution of smoking to environment and the harm to smoker.
At present, in fact, shitosan is used for the phenol type substances removed in Sewage Environment and has been reported, the adsorbance of the composite aquogel Pyrogentisinic Acid prepared by polyvinyl alcohol/shitosan/gelatin can reach 40.1mg/g.Because shitosan is containing the functional group such as pyranoid ring of activated hydroxyl, amino, electron rich, physical absorption and chemisorbed can be formed to the chemical composition in flue gas, especially to reduction phenol nuisance Be very effective.
Graphene as a kind of nano material with unique texture and characteristic, for the reducing tar and reducing harm very advantageous of tobacco.Nano material is a kind of new material, and development in recent years is rapid, and when being used on cigarette, the amplitude of its reducing tar and reducing harm is also comparatively large, has great development potentiality, achieves phasic results at present.Graphene is that one passes through sp by carbon atom
2hybridized orbit Cheng Jian forms, and has the two-dimensional atomic crystal material of hexagonal honeycomb shape lattice structure, and it is unique and perfect structure makes it have excellent absorption and catalytic degradation characteristic.
Up-to-date research shows, CNT and Graphene have the function of scavenging free radicals, and this exists very large pi-conjugated structure owing in this type of nano-carbon material molecule, can provide electronics for free radical.Found by theoretical modeling, Graphene has scavenging action for oxygen radical, alkyl radical, hydroxyl radical free radical, nitrence free radical etc., plays the function of antioxidant, and this harmful free radicals be used in cigaratte filter removing flue gas for Graphene provides possibility.
Both at home and abroad for the research of cigarette filter, in existing technology, Chinese patent mandate publication number CN2872872Y, authorize publication date 2007.2.28, denomination of invention is " expanded graphite composite cigarette filter tip ", and this application scheme adopts in cigarette filter, adds one section of fillter section containing expanded graphite, obtained expanded graphite composite filter mouth, can the harmful substance such as nicotine gas, kerosene and nicotine effectively in filter cigarette, but can not BaP be adsorbed.Chinese patent mandate publication number CN201349521Y, authorize publication date 2009.11.25, denomination of invention is " high-efficiency cigarette filter tip containing nano-carbon material ", this application scheme nanometer is adopted material load on fiber, make filtration core, the obtained high-efficiency cigarette filter tip containing nano-carbon material, effectively can adsorb the noxious material in flue gas, cheap.Chinese patent mandate publication number CN201813833U, authorize publication date 2011.05.04, denomination of invention is " cigarette with activated carbon filter tip ", the filter tip of the smoke that this application scheme adopts is uniform-distribution with active carbon, obtained cigarette with activated carbon filter tip, active carbon can the harmful substance such as sorbing carbon monoxide, nicotine, nitrogen oxide and amine.Chinese patent mandate publication number CN201797987U, authorize publication date 2011.04.20, denomination of invention is " cigarette filter with activated carbon granule ", this application scheme adopts filter tip to be combined by two sections of filter sticks, it comprises the filter stick near pipe tobacco end, and the filter stick of close cigarette end, active carbon is sprayed with in the filter stick of cigarette end, thus the obtained cigarette filter with activated carbon granule, in the cigarette that this filter tip is, the content of harmful substance is reduced, advantages of good adsorption effect.Chinese patent mandate publication number CN201393643Y, authorize publication date 2010.02.03, denomination of invention is " cigarette filter that activated alumina ball and cocoanut active charcoal filter ", this application scheme activated alumina ball and cocoanut active charcoal is filtered to be compounded in filter tip, the cigarette filter that obtained activated alumina ball and cocoanut active charcoal filter, the activated alumina ball stronger by adsorption cleaning and high-quality cocoanut active charcoal carry out second interception, are effective and filter the harmful substance such as nicotine and tar.These cigarette filters all cannot selective absorption BaP in a word.
A kind of filter fiber prepared by the present invention, adopt the technology of spraying that Graphene or Graphene and shitosan substep are sprayed on the surface of fiber successively, the obtained fiber through Graphene/chitosan-modified after vacuum drying, fiber after modification contains a certain amount of shitosan, because shitosan is containing the functional group such as pyranoid ring of activated hydroxyl, amino, electron rich, physical absorption and chemisorbed can be formed, especially to reduction phenol nuisance Be very effective to the chemical composition in flue gas.Simultaneously owing to containing Graphene in fiber, Graphene not only has scavenging action to oxygen radical, alkyl radical, hydroxyl radical free radical, nitrence free radical etc. in cigarette smoke, and the BaP content that can effectively reduce in flue gas, but little on the content impact of nicotine.Because graphene sheet layer structure distribution is on the surface of filter fiber, BaP and the strong pi-pi bond of Graphene interact, and make BaP selective absorption at graphenic surface, and the composition such as nicotine in flue gas can not effectively adsorb.Therefore research and develop performance more carefully, low, the oligosaprobic high-quality cigarette filter of cost is imperative.
Summary of the invention
For the deficiencies in the prior art, overcome original cigarette fiber filter material Problems existing, the object of the present invention is to provide the preparation method of the filter fiber of a kind of selective absorption BaP and phenol, filter fiber surface is effectively evenly distributed in by Graphene or Graphene and shitosan, thus modification filter fiber, obtained a kind of Graphene or Graphene and chitosan-modified fiber, finally be made into cigaratte filter, the deficiency of original filter tip can be made up better, make because shitosan is containing activated hydroxyl, amino, the functional groups such as the pyranoid ring of electron rich, physical absorption and chemisorbed can be formed to the chemical composition in flue gas, especially to reduction phenol nuisance Be very effective, simultaneous oxidation Graphene is not only to oxygen radical in cigarette smoke, alkyl radical, hydroxyl radical free radical, nitrence free radical etc. has scavenging action, and the BaP content that can effectively reduce in flue gas, but it is little on the content impact of nicotine, to achieve these goals, technical solution of the present invention is:
A preparation method for the filter fiber of selective absorption BaP and phenol, described preparation method comprises the following steps:
A compound concentration is the decorating liquid of 1 ~ 10mg/ml, and ultrasonic disperse time 1 ~ 2h, obtains uniform decorating liquid, and wherein, ultrasonic device power is 100 ~ 200W;
B adopts and to spray fiber through the obtained decorating liquid of a step or brush or dip-coating or extrusion coated process, processing time 5 ~ 20 min, treatment temperature 25 ~ 50 DEG C, under being then placed in 80 DEG C of vacuum conditions by the fiber after process, dry 6h, the fiber after obtained modified liquid process.
Described fiber is the one of acetate fiber or polypropylene fibre or acid fiber by polylactic or viscose fiber or Lyocell fiber.
Described decorating liquid is the one of the mixed solution of graphene oxide water solution or graphene oxide and chitosan aqueous solution.
Described graphene oxide and the mixed solution of chitosan aqueous solution, in mixed solution, the mass concentration ratio of graphene oxide and shitosan is 0.1 ~ 1:1.
The mass content of the graphene oxide in the fiber after described modified liquid process is 0.01 ~ 0.06%.
Graphene oxide in fiber after described modified liquid process and the mass content of shitosan are 0.01 ~ 0.08%.
Owing to have employed above technical scheme, the preparation method of the filter fiber of selective absorption BaP of the present invention and phenol has the following advantages:
The preparation method of the filter fiber of 1 selective absorption BaP of the present invention and phenol, because Graphene is that one passes through sp by carbon atom
2hybridized orbit Cheng Jian forms, and has the two-dimensional atomic crystal material of hexagonal honeycomb shape lattice structure, and therefore by the fiber filter tip of Graphene modification, the perfect structure because Graphene is unique, makes filter tip have excellent absorption and catalytic degradation characteristic.Simultaneously due to cationic amino being with by shitosan side chain, can the optionally harmful substance such as tar adsorption, carbon monoxide, heavy metal, but nicotine can not synchronously reduce, therefore side-stream smoke oxious component can be reduced, reduce excitant, thus effectively reduce the pollution of smoking to environment and the harm to smoker.
The preparation method of the filter fiber of 2 selective absorption BaPs of the present invention and phenol, because Graphene has the function of scavenging free radicals, very large pi-conjugated structure is there is in this owing in this type of nano-carbon material molecule, therefore Graphene has scavenging action for oxygen radical, alkyl radical, hydroxyl radical free radical, nitrence free radical etc., play the function of antioxidant, this harmful free radicals be used in cigaratte filter removing flue gas for Graphene provides possibility.Simultaneously because graphene sheet layer structure distribution is on the surface of filter fiber, the π-π strong due to BaP and Graphene interacts, and makes Selective graphene absorption BaP, and the compositions such as nicotine in flue gas can not effectively adsorb.Simultaneously because shitosan is containing the functional group such as pyranoid ring of activated hydroxyl, amino, electron rich, physical absorption and chemisorbed can be formed to the chemical composition in flue gas, especially to reduction phenol nuisance Be very effective.
The preparation method of the filter fiber of 3 selective absorption BaPs of the present invention and phenol, preparation technology of the present invention is simple, and each component material material price is inexpensive, low cost, low stain.Selective absorption BaP prepared by this technique and the filter fiber of phenol, filter effect is better.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
A preparation method for the filter fiber of selective absorption BaP and phenol, described preparation method comprises the following steps:
A graphite pre-oxidation: the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing and causes through inspection sulfate radical-free ion, and then dry 3h in the vacuum drying chamber of 80 DEG C, obtain pre-oxidation Graphene.The secondary oxidation of pre-oxidation Graphene: the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, and then slowly add the potassium permanganate of 30g, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then adding reactant liquor transfers in the beaker of 1000ml, add the deionized water of 600ml again, add 6ml30% hydrogen peroxide again, then filter, use the hydrochloric acid of 10% successively, deionized water washing is to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C, obtain graphene oxide,
B is by graphene oxide dispersion deionized water in a step, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, the power of ultrasonic device is 100 ~ 200W, obtain graphene oxide water solution or by the graphene oxide water solution in a step and chitosan aqueous solution, ultrasonic disperse 1 ~ 2h, the power of ultrasonic device is 100 ~ 200W, is mixed with mixed solution;
C adopts and to spray fiber through the obtained graphene oxide of b step or graphene oxide and chitosan aqueous solution or brush or dip-coating or extrusion coated process, processing time 5 ~ 20 min, treatment temperature 25 ~ 50 DEG C, then under the fiber after process being placed in 80 DEG C of vacuum conditions, dry 6h, the fiber after obtained modified liquid process;
Described fiber is the one of acetate fiber or polypropylene fibre or acid fiber by polylactic or viscose fiber or Lyocell fiber.
Described decorating liquid is the one of the mixed solution of graphene oxide water solution or graphene oxide and chitosan aqueous solution.
Described graphene oxide and the mixed solution of chitosan aqueous solution, in mixed solution, the mass concentration ratio of graphene oxide and shitosan is 0.1 ~ 1:1.
The mass content of the graphene oxide in the fiber after described modified liquid process is 0.01 ~ 0.06%.
Graphene oxide in fiber after described modified liquid process and the mass content of shitosan are 0.01 ~ 0.08%.
Specific embodiment
embodiment 1
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.01% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.01% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 10%, makes phenol content reduce 5%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 2
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.015% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.015% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 12%, makes phenol content reduce 7%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 3
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.02% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.02% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 15%, makes phenol content reduce 9.5%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 4
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.025% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.03% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 18%, makes phenol content reduce 13.2%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 5
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.03% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.035% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 20%, makes phenol content reduce 15.5%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 6
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.035% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.04% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 22%, makes phenol content reduce 16.2%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 7
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.04% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.05% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 27.2%, makes phenol content reduce 16.5%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 8
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.045% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.06% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 27%, makes phenol content reduce 15%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 9
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.05% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.065% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 26.7%, makes phenol content reduce 14.8%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 10
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.055% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.07% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 26%, makes phenol content reduce 14.5%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 11
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.06% of fiber quality
4th step: the fiber dip-coating of the graphene modified three steps obtained is in obtained chitosan aqueous solution, and then dry 6h under 80 DEG C of vacuum conditions, finally makes cigaratte filter by fiber composite modified for Graphene/shitosan again.Wherein, chitosan aqueous solution accounts for 0.08% of fiber quality.After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 25.6%, makes phenol content reduce 13.6%.This modified filter tip makes BaP can only BaP in selective absorption flue gas and phenol, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 12
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.01% of fiber quality
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 10%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 13
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.015% of fiber quality.
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 12%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 14
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.02% of fiber quality.
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 15%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 15
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.025% of fiber quality.
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 18%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 16
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.03% of fiber quality.
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 20%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 17
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.04% of fiber quality.
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 27.2%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 18
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by fiber dip-coating in graphene aqueous solution, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.045% of fiber quality
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 26%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 19
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by graphene aqueous solution spraying in the fibre, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.045% of fiber quality
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 25%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 20
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: graphene aqueous solution is brushed in the fibre, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.045% of fiber quality
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 24%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
embodiment 21
The first step: pre-oxidation, the concentrated sulfuric acid getting 30ml joins in the there-necked flask of 500ml, then take 5g potassium peroxydisulfate slowly to join in the concentrated sulfuric acid, add the phosphorus pentoxide of 5g again, be warming up to 80 DEG C, then add the graphite powder of 3g, reaction 6h, reaction terminates filtration washing, and then dries 3h in the vacuum drying chamber of 80 DEG C, obtains the Graphene of pre-oxidation; Secondary oxidation, the concentrated sulfuric acid measuring 200ml joins in the there-necked flask of 500ml, be placed in the ice bath of 0 DEG C, slowly add the Graphene of pre-oxidation, then the potassium permanganate of 30g is added, be warming up to 35 DEG C and maintain 3h, then 95 DEG C are warming up at stirring 15min, then add reactant liquor to transfer in the beaker of 1000ml, then add the deionized water of 600ml, then add 6ml30% hydrogen peroxide, then filter, to neutral, and then dry 3h in the vacuum drying chamber of 80 DEG C with 10% hydrochloric acid, deionized water washing successively, obtain graphene oxide.Second step: graphene oxide is disperseed in deionized water, compound concentration is the graphene oxide dispersion of 1 ~ 10mg/ml, ultrasonic disperse 1 ~ 2h, and the power of ultrasonic device is 100 ~ 200W, obtains homogeneous, stable graphene oxide water solution; 3rd step: by graphene aqueous solution extrusion coated in the fibre, then at 80 DEG C of dry 6h, the fiber of obtained graphene modified; Wherein, Graphene accounts for 0.045% of fiber quality
After testing, the absorption of filter tip to BaP of obtained shitosan/graphene modified improves 23%.This modified filter tip makes BaP can only BaP in selective absorption flue gas, and the composition such as nicotine in flue gas can not effectively adsorb.
Claims (6)
1. a preparation method for the filter fiber of selective absorption BaP and phenol, is characterized in that: described preparation method carries out according to the following steps:
A compound concentration is the decorating liquid of 1 ~ 10mg/ml, and ultrasonic disperse time 1 ~ 2h, obtains uniform decorating liquid, and wherein, ultrasonic device power is 100 ~ 200W;
B adopts and to spray fiber through the obtained decorating liquid of a step or brush or dip-coating or extrusion coated process, processing time 5 ~ 20 min, treatment temperature 25 ~ 50 DEG C, under being then placed in 80 DEG C of vacuum conditions by the fiber after process, dry 6h, the fiber after obtained modified liquid process.
2. the preparation method of the filter fiber of a kind of selective absorption BaP according to claim 1 and phenol, is characterized in that: described fiber is the one of acetate fiber or polypropylene fibre or acid fiber by polylactic or viscose fiber or Lyocell fiber.
3. the preparation method of the filter fiber of a kind of selective absorption BaP according to claim 1 and phenol, is characterized in that: described decorating liquid is the one of the mixed solution of graphene oxide water solution or graphene oxide and chitosan aqueous solution.
4. the preparation method of the filter fiber of a kind of selective absorption BaP according to claim 3 and phenol, in described mixed solution, the mass concentration ratio of graphene oxide and shitosan is 0.1 ~ 1:1.
5. the preparation method of a kind of selective absorption BaP according to claim 1 or 3 and the filter fiber of phenol, is characterized in that: the mass content of the graphene oxide in the fiber after described modified liquid process is 0.01 ~ 0.06%.
6. the preparation method of a kind of selective absorption BaP according to claim 1 or 3 and the filter fiber of phenol, is characterized in that: the graphene oxide in the fiber after described modified liquid process and the mass content of shitosan are 0.01 ~ 0.08%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510193006.XA CN104815630A (en) | 2015-04-22 | 2015-04-22 | Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510193006.XA CN104815630A (en) | 2015-04-22 | 2015-04-22 | Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104815630A true CN104815630A (en) | 2015-08-05 |
Family
ID=53726251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510193006.XA Pending CN104815630A (en) | 2015-04-22 | 2015-04-22 | Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104815630A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105361241A (en) * | 2015-11-20 | 2016-03-02 | 东南大学 | Cigarette binary composite filter tip filled with graphene oxide and preparation method of cigarette binary composite filter tip |
| CN106268637A (en) * | 2016-08-12 | 2017-01-04 | 东华大学 | A kind of viscose rayon adsorbing material modified based on graphene oxide and preparation thereof and application |
| WO2017024933A1 (en) * | 2015-08-09 | 2017-02-16 | 济南圣泉集团股份有限公司 | Graphene adsorbing material, preparation method therefor and application thereof, and cigarette filter tip and cigarette |
| CN106820261A (en) * | 2017-04-10 | 2017-06-13 | 滁州卷烟材料厂 | A kind of filter tip for selecting to adsorb BaP and phenol in cigarette smoke |
| CN107373753A (en) * | 2017-08-29 | 2017-11-24 | 武汉纺织大学 | A kind of graphene polyose modification cigaratte filter of selective retention phenyl ring class harmful substance and preparation method thereof |
| CN107537439A (en) * | 2016-07-25 | 2018-01-05 | 济南圣泉集团股份有限公司 | A kind of graphene sorbing material, its preparation method and its application and cigarette filter |
| CN110179155A (en) * | 2019-05-30 | 2019-08-30 | 华侨大学 | A kind of application of polyamino chitosan material in cigarette filter |
| CN110860134A (en) * | 2019-11-27 | 2020-03-06 | 郑州轻工业大学 | Micro-nano fiber filter disc with adsorption and catalytic harm reduction mechanisms and preparation method and application thereof |
| CN110973700A (en) * | 2019-11-27 | 2020-04-10 | 郑州轻工业大学 | Preparation method and application of multifunctional cigarette core line with perfuming and harm-reducing effects |
| CN111203182A (en) * | 2020-01-17 | 2020-05-29 | 中国科学院宁波材料技术与工程研究所 | Modified activated carbon for adsorbing phenol and preparation method and application thereof |
| CN111821774A (en) * | 2020-08-07 | 2020-10-27 | 丛春华 | Preparation method of graphene cigarette smoke filter screen and obtained filter screen |
| CN112044398A (en) * | 2020-09-07 | 2020-12-08 | 昆明理工大学 | Application of graphene adsorption material in phenol wastewater treatment |
| CN113019322A (en) * | 2021-03-09 | 2021-06-25 | 云南中烟工业有限责任公司 | Graphene smoke adsorbing material for reducing harmful ingredients in cigarette smoke and preparation method and application thereof |
| CN115717324A (en) * | 2022-12-24 | 2023-02-28 | 广东鑫球新材料科技有限公司 | Preparation method and application of PP (polypropylene) material traditional Chinese medicine filter element |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201349521Y (en) * | 2008-08-04 | 2009-11-25 | 许以华 | Efficient nano-carbon material-containing cigarette filter tip |
| CN104389234A (en) * | 2014-09-12 | 2015-03-04 | 河南中烟工业有限责任公司 | Cigarette filter tip added with chitosan-graphene oxide composite material |
-
2015
- 2015-04-22 CN CN201510193006.XA patent/CN104815630A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201349521Y (en) * | 2008-08-04 | 2009-11-25 | 许以华 | Efficient nano-carbon material-containing cigarette filter tip |
| CN104389234A (en) * | 2014-09-12 | 2015-03-04 | 河南中烟工业有限责任公司 | Cigarette filter tip added with chitosan-graphene oxide composite material |
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102177137B1 (en) * | 2015-08-09 | 2020-11-11 | 지난 셩취엔 그룹 쉐어 홀딩 코., 엘티디. | Graphene adsorbent, its manufacturing method and use, and cigarette filter tips and tobacco |
| WO2017024933A1 (en) * | 2015-08-09 | 2017-02-16 | 济南圣泉集团股份有限公司 | Graphene adsorbing material, preparation method therefor and application thereof, and cigarette filter tip and cigarette |
| KR20180044311A (en) * | 2015-08-09 | 2018-05-02 | 지난 셩취엔 그룹 쉐어 홀딩 코., 엘티디. | Graphene sorbent, its preparation methods and uses, and cigarette filter tips and cigarettes |
| US11006664B2 (en) | 2015-08-09 | 2021-05-18 | Jinan Shengquan Group Share Holding Co., Ltd. | Graphene adsorbing material, preparation method therefor and application thereof, and cigarette filter tip and cigarette |
| 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 |
| CN105361241A (en) * | 2015-11-20 | 2016-03-02 | 东南大学 | Cigarette binary composite filter tip filled with graphene oxide and preparation method of cigarette binary composite filter tip |
| CN107537439A (en) * | 2016-07-25 | 2018-01-05 | 济南圣泉集团股份有限公司 | A kind of graphene sorbing material, its preparation method and its application and cigarette filter |
| CN107537439B (en) * | 2016-07-25 | 2019-11-22 | 济南圣泉集团股份有限公司 | A kind of graphene adsorbent material, preparation method and its application and cigarette filter |
| CN106268637A (en) * | 2016-08-12 | 2017-01-04 | 东华大学 | A kind of viscose rayon adsorbing material modified based on graphene oxide and preparation thereof and application |
| CN106820261A (en) * | 2017-04-10 | 2017-06-13 | 滁州卷烟材料厂 | A kind of filter tip for selecting to adsorb BaP and phenol in cigarette smoke |
| CN107373753A (en) * | 2017-08-29 | 2017-11-24 | 武汉纺织大学 | A kind of graphene polyose modification cigaratte filter of selective retention phenyl ring class harmful substance and preparation method thereof |
| CN110179155A (en) * | 2019-05-30 | 2019-08-30 | 华侨大学 | A kind of application of polyamino chitosan material in cigarette filter |
| CN110860134A (en) * | 2019-11-27 | 2020-03-06 | 郑州轻工业大学 | Micro-nano fiber filter disc with adsorption and catalytic harm reduction mechanisms and preparation method and application thereof |
| CN110973700A (en) * | 2019-11-27 | 2020-04-10 | 郑州轻工业大学 | Preparation method and application of multifunctional cigarette core line with perfuming and harm-reducing effects |
| CN110860134B (en) * | 2019-11-27 | 2021-09-24 | 郑州轻工业大学 | Micro-nano fiber filter disc with adsorption and catalytic harm reduction mechanisms and preparation method and application thereof |
| CN111203182A (en) * | 2020-01-17 | 2020-05-29 | 中国科学院宁波材料技术与工程研究所 | Modified activated carbon for adsorbing phenol and preparation method and application thereof |
| CN111821774A (en) * | 2020-08-07 | 2020-10-27 | 丛春华 | Preparation method of graphene cigarette smoke filter screen and obtained filter screen |
| CN112044398A (en) * | 2020-09-07 | 2020-12-08 | 昆明理工大学 | Application of graphene adsorption material in phenol wastewater treatment |
| CN113019322A (en) * | 2021-03-09 | 2021-06-25 | 云南中烟工业有限责任公司 | Graphene smoke adsorbing material for reducing harmful ingredients in cigarette smoke and preparation method and application thereof |
| CN113019322B (en) * | 2021-03-09 | 2022-11-11 | 云南中烟工业有限责任公司 | Graphene smoke adsorbing material for reducing harmful ingredients in cigarette smoke and preparation method and application thereof |
| CN115717324A (en) * | 2022-12-24 | 2023-02-28 | 广东鑫球新材料科技有限公司 | Preparation method and application of PP (polypropylene) material traditional Chinese medicine filter element |
| CN115717324B (en) * | 2022-12-24 | 2023-07-21 | 广东鑫球新材料科技有限公司 | Preparation method and application of PP material traditional Chinese medicine filter element |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104815630A (en) | Preparation method of filter tip fibers for selectively adsorbing benzopyrene and phenol | |
| KR102177137B1 (en) | Graphene adsorbent, its manufacturing method and use, and cigarette filter tips and tobacco | |
| CN101885485B (en) | Method for preparing carbon material with high specific surface area by using metallic organic framework material as template | |
| JP5771274B2 (en) | Multi-aperture carbon particle air purifier and method for producing the same | |
| JP6513401B2 (en) | Active carbon fiber having high active surface area | |
| CN103005712A (en) | Grapheme type fiber cigarette filter and preparation method thereof | |
| CN110935280B (en) | Nitrogen-doped mesoporous bamboo-based biochar and application thereof | |
| CN102008125B (en) | Metal complexing material and preparation method thereof, and application of metal complexing material in cigarettes | |
| CN105597675A (en) | Graphene adsorbing material, preparation method and application thereof and cigarette filter tip | |
| CN107537439B (en) | A kind of graphene adsorbent material, preparation method and its application and cigarette filter | |
| CN101642287A (en) | High-efficiency cigarette filter tip containing nano-carbon material | |
| CN107713007B (en) | Sepiolite antibacterial cigarette filter tip paper and preparation method thereof | |
| CN102517981B (en) | Cellulose paper capable of reducing content of hydrocyanic acid or volatile carbonyl compound in cigarette smoke and preparation and application thereof | |
| CN106820261A (en) | A kind of filter tip for selecting to adsorb BaP and phenol in cigarette smoke | |
| CN101439281A (en) | Method for preparing aminoglutaric acid modified expanded graphite and use in methyl aldehyde gas adsorption | |
| CN107199015A (en) | A kind of preparation method of sepiolite base volume cigarette filter tip adsorbent | |
| CN101406844A (en) | Method for preparing molecular sieve supported nano zinc sulphide | |
| CN101239304A (en) | Method for preparing modified expanded graphite and application in treating to formaldehyde gas | |
| CN112645324B (en) | Porous carbon composite material with core-shell structure and preparation method and application thereof | |
| CN112645328B (en) | Preparation method and application of nitrogen-containing porous carbon material | |
| CN102002888B (en) | Cellulose paper capable of reducing benzo(a)pyrene content of smoke of cigarettes, preparation method thereof and use thereof | |
| CN101439282B (en) | Method for preparing modified expanded graphite and use in benzene gas processing | |
| CN101949106B (en) | Cellulose paper for reducing formonitrile content of cigarette smoke, preparation method and application thereof | |
| CN103539743A (en) | Ionic liquid functionalized graphite oxide surface grafted Schiff base compound as well as preparation method and application thereof | |
| CN107051390A (en) | A kind of preparation method of chitosan charcoal titania nanotube composite adsorbing material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150805 |