CN107946082A - A kind of preparation method and its usage of cigarette filter/graphene composite material - Google Patents

A kind of preparation method and its usage of cigarette filter/graphene composite material Download PDF

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Publication number
CN107946082A
CN107946082A CN201711020223.4A CN201711020223A CN107946082A CN 107946082 A CN107946082 A CN 107946082A CN 201711020223 A CN201711020223 A CN 201711020223A CN 107946082 A CN107946082 A CN 107946082A
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China
Prior art keywords
cigarette filter
composite material
graphene
graphene composite
preparation
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CN201711020223.4A
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Chinese (zh)
Inventor
程有亮
张庆玲
方长青
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Xian University of Technology
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Xian University of Technology
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Priority to CN201711020223.4A priority Critical patent/CN107946082A/en
Publication of CN107946082A publication Critical patent/CN107946082A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/44Raw materials therefor, e.g. resins or coal
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of cigarette filter/graphene composite material, the cigarette filter of recycling is soaked several times in graphene oxide alcohol dispersion liquid, drying, is then carbonized, that is, obtains cigarette filter/graphene composite material.The invention also discloses the purposes of material prepared.The present invention makes graphene oxide doped into the filter tip of useless cigarette butt by controlling dispersion concentration of the graphene oxide in ethanol solution.Carbonization rear oxidation graphene is heat-treated as graphene and adulterated wherein, and contains the trace elements such as nitrogen.Obtained composite material is porous, and has high ratio surface, excellent electric conductivity and ion transporting.Therefore it can be used as the electrode material of ultracapacitor.The present invention also has the advantages that technique is simple, cost is low, fireballing, can directly recycle discarded cigarette butt, have good environmental benefit and economic benefit.

Description

A kind of preparation method and its usage of cigarette filter/graphene composite material
Technical field
The invention belongs to technical field of composite materials, is related to a kind of preparation side of cigarette filter/graphene composite material Method, the invention further relates to the purposes of cigarette filter/graphene composite material made from the above method.
Background technology
Predicted according to the World Health Organization, the number of global smoker in 2025 will rise to 1,700,000,000 people.China is in the world most Big cigarette production country and maximum cigarette consumption country, according to statistics, Chinese smoking number nearly 400,000,000 or so, Annual number is all constantly rising.These discarded cigarette butts cause environment very big negative effect, therefore to discarding cigarette butt Recycling has important application value.
The recycling of useless cigarette butt is primarily referred to as the materials such as nicotine, the Salanesol adsorbed to filter tip and the inside Recycling.The main raw material(s) of filter tip is acetate fiber, is chiefly used in the manufacture of textile, plate, sheet material etc..Nicotine is also known as cigarette Alkali, is the main component of tobacco, its chemical formula is C10H14N2, water-soluble, ethanol, chloroform, ether, oils, are mainly used in Medicine and the insect-pest of crops etc..Salanesol molecular formula is C45H74O, it is not soluble in water, methanol, ethanol are slightly soluble in, is dissolved in Acetone, chloroform, hexane, its application are mainly the fields such as medicine, antibacterial.At present, recycling of the China to cigarette butt and immature, Do not accomplish really also to recycle.In general, useless cigarette butt is exactly to recyclable materials in the first step of recycling Extraction and separation, i.e., to discarding in cigarette butt the recycling of nicotine and Salanesol contained, it is necessary to by multiple times of filtration, though technique is simple The list but rate of recovery is not high.
Porous material is a research hotspot of current electrode material for super capacitor, its porosity is conducive to the biography of ion It is defeated.Graphene has high-specific surface area, excellent electric conductivity, its composite material is chiefly used in electrode material.Due to useless cigarette butt filtering Mouth is loose structure, and the inside remains the trace elements such as nitrogen, and remaining nitrogen has raising electrochemistry in its carbonized product The effect of performance.Therefore, by useless cigarette butt filter tip with graphene is compound not only can directly recycle useless cigarette butt, applied and stored up Energy field also has extensive prospect.
The content of the invention
The object of the present invention is to provide a kind of preparation method of cigarette filter/graphene composite material, is cigarette filter The recycling of mouth provides a kind of new method.
It is a further object of the present invention to provide the purposes of cigarette filter/graphene composite material made from the above method.
The technical solution adopted in the present invention is a kind of preparation method of cigarette filter/graphene composite material, will be returned The cigarette filter of receipts soaks several times in graphene oxide-alcohol dispersion liquid, and drying, is then carbonized, that is, obtains cigarette mistake Filter tip/graphene composite material.
The features of the present invention also resides in,
The cigarette filter of recycling is used filter tip, wherein after burning containing pipe tobacco, by the material of absorption generation.
The concentration of graphene oxide-alcohol dispersion liquid is 0.2g/L~1g/L.
Immersion process is:First the cigarette filter of recycling is soaked in graphene oxide-alcohol dispersion liquid, is stood, so Soak again afterwards, this process repeats 10~20 times, and each soaking time is 20~60s.
Cigarette filter and the mass volume ratio of graphene oxide-alcohol dispersion liquid are 0.01~0.15g/ml.
Drying temperature is 70~100 DEG C, and drying time is 1~2h.
Carbonization is specially:After the cigarette filter of drying is put into tube furnace, nitrogen is passed through, furnace temperature is warming up to 800 DEG C 120~180min is kept the temperature after~900 DEG C, treats that stove is cooled to room temperature and closes nitrogen.
10~20 DEG C/min of heating rate.
Nitrogen flow is 40~100sccm.
Another technical solution of the present invention is, using a kind of preparation of cigarette filter/graphene composite material The purposes of cigarette filter/graphene composite material made from method, the electrode material as ultracapacitor.
The invention has the advantages that the present invention chooses useless cigarette butt filter tip, since the material of cigarette butt filter tip is acetic acid Fiber, becomes carbon material after its high temperature cabonization.And there is loose structure, beneficial to the transmission of ion.Contain in useless cigarette butt filter tip The materials such as nicotine, that is, contain nitrogen, there is good effect for adion.Graphene and discarded cigarette butt are filtered After mouth is compound, the high ratio surface of the loose structure of useless cigarette butt filter tip and graphene is effectively combined, obtained composite material It is porous, and there is high ratio surface, excellent electric conductivity and ion transporting.Therefore it can be used as the electrode material of ultracapacitor Material.In addition the present invention also has the advantages that technique is simple, cost is low, fireballing, can directly recycle discarded cigarette butt, have Good environmental benefit and economic benefit.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of cigarette filter/graphene composite material prepared by embodiment 1;
Fig. 2 is the scanning electron microscope diagram of cigarette filter/graphene composite material prepared by embodiment 2;
Fig. 3 is the scanning electron microscope diagram of cigarette filter/graphene composite material prepared by embodiment 3.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of cigarette filter/graphene composite material of the present invention, first by graphene oxide in ethanol Ultrasonic disperse in solution, the alcohol solution dipping that the cigarette filter of recycling then is added graphene several times, dry in an oven It is dry.Finally the cigarette filter of drying is put into tube furnace and is carbonized, that is, obtains cigarette filter/graphene composite material.
Specifically implement according to following steps:
Step 1, graphene oxide is disperseed in ethanol, to obtain graphene oxide-second that concentration is 0.2g/L~1g/L Alcohol dispersion liquid;
Step 2, it is 0.01~0.15g/ml according to the mass volume ratio of cigarette filter and dispersion liquid, by cigarette filter 20~60s is soaked in the dispersion liquid that step 1 obtains, is then placed within 1~3min of standing on culture dish, then be immersed in oxidation stone In the alcohol dispersion liquid of black alkene.This process repeats 10~20 times.Then 1~2h is dried in an oven, and drying temperature is 70~100 ℃。
Step 3, after the cigarette filter after step 2 is dried is put into tube furnace, be passed through nitrogen, flow for 40~ 100sccm, furnace temperature keep the temperature 120~180min after being warming up to 800 DEG C~900 DEG C, and 10~20 DEG C/min of heating rate, treats that stove is cold But arrive room temperature and close nitrogen, obtain cigarette filter/graphene composite material.
The present invention chooses useless cigarette filter, since the material of cigarette filter is acetate fiber, after its high temperature cabonization into For carbon material.And there is loose structure, beneficial to the transmission of ion.Containing materials such as nicotines in useless cigarette filter, that is, Containing nitrogen, there is good effect for adion.At present, graphene-based composite material is chiefly used in electrode material, because It is with high ratio surface and good electric conductivity.By graphene and cigarette filter it is compound after, by the porous of cigarette filter Structure and the high ratio surface of graphene are effectively combined, and obtained material is conducive to the transmission of ion.
The present invention soaks graphene oxide ultrasonic disperse in ethanol, then cigarette filter for several times in dispersion liquid, By controlling concentration of the graphene oxide in ethanol solution, make graphene oxide doped into the filter tip of useless cigarette butt.Carbonization After to show as the composite material porous, graphene oxide is heat-treated as graphene and doping wherein, and micro containing nitrogen etc. Element.Obtained material is porous, and has high ratio surface, excellent electric conductivity and ion transporting.Therefore can be used as surpassing The electrode material of level capacitor.
The present invention also has the advantage that technique is simple, cost is low, and speed is fast, can directly recycle discarded cigarette butt, With good environmental benefit and economic benefit.
Embodiment 1
By 8mg graphene dispersions in the ethanol of 40ml, ultrasonic disperse 30min.According to cigarette filter and dispersion liquid Mass volume ratio is 0.01g/ml, and useless cigarette filter is soaked 20s in the alcohol dispersion liquid of graphene, then pulls placement out 3min is shelved on culture dish.Then it is immersed in again in dispersion liquid, this process is repeated 10 times.Cigarette filter after immersion is existed Dried in baking oven, temperature is 70 DEG C, time 2h.Cigarette filter after drying is placed in crucible, is carbonized in tube furnace. Nitrogen, flow 40sccm are passed first into, furnace temperature keeps the temperature 180min, heating rate 10~20 after being warming up to 800 DEG C~820 DEG C DEG C/min, treat that stove is cooled to room temperature and closes nitrogen.Obtained cigarette filter/graphene composite material SEM pictures such as Fig. 1 institutes Show, here it is apparent that the loose structure of composite material, since graphene concentration is low, graphene cannot be substantially found on its surface Doping is wherein.
Embodiment 2
By 20mg graphene dispersions in the ethanol of 40ml, ultrasonic disperse 30min.According to cigarette filter and dispersion liquid Mass volume ratio is 0.15g/ml, and useless cigarette filter is soaked 60s in the alcohol dispersion liquid of graphene, then pulls placement out 3min is shelved on culture dish.Then it is immersed in again in the dispersion liquid of ethanol, this process is repeated 15 times.By the cigarette mistake after immersion Filter tip is dried in an oven, and temperature is 100 DEG C, time 1h.Cigarette filter after drying is placed in crucible, in tube furnace Middle carbonization.Nitrogen, flow 70sccm are passed first into, furnace temperature keeps the temperature 160min, heating rate after being warming up to 840 DEG C~860 DEG C 10~20 DEG C/min, treat that stove is cooled to room temperature and closes nitrogen.Obtain cigarette filter/graphene composite material SEM pictures such as Shown in Fig. 2, being clear that in composite material has graphene sheet layer doping, illustrates that cigarette butt filters mouth/graphene composite material It is successfully prepared.
Embodiment 3
By 40mg graphene dispersions in the ethanol of 40ml, ultrasonic disperse 30min.According to cigarette filter and dispersion liquid Mass volume ratio is 0.05g/ml, and useless cigarette filter is soaked 30s in the alcohol dispersion liquid of graphene, then pulls placement out 2min is shelved on culture dish.Then it is immersed in again in the dispersion liquid of ethanol, this process is repeated 20 times.By the cigarette mistake after immersion Filter tip is dried in an oven, and temperature is 85 DEG C, time 1.5h.Cigarette filter after drying is placed in crucible, in tubular type It is carbonized in stove.Nitrogen, flow 100sccm are passed first into, furnace temperature keeps the temperature 120min, heating speed after being warming up to 880 DEG C~900 DEG C 10~20 DEG C/min of rate, treats that stove is cooled to room temperature and closes nitrogen.Obtain cigarette filter/graphene composite material SEM pictures As shown in Figure 3, it can be seen that the graphene sheet layer of doping is very much, the stacking of graphene sheet layer locally occurs.
Embodiment 4
By 10mg graphene dispersions in the ethanol of 40ml, ultrasonic disperse 30min.According to cigarette filter and dispersion liquid Mass volume ratio is 0.08g/ml, and useless cigarette filter is soaked 40s in the alcohol dispersion liquid of graphene, then pulls placement out 2min is shelved on culture dish.Then it is immersed in again in the dispersion liquid of ethanol, this process is repeated 13 times.By the cigarette mistake after immersion Filter tip is dried in an oven, and temperature is 75 DEG C, time 2h.Cigarette filter after drying is placed in crucible, in tube furnace Middle carbonization.Nitrogen, flow 55sccm are passed first into, furnace temperature keeps the temperature 170min, heating rate after being warming up to 820 DEG C~840 DEG C 10~20 DEG C/min, treat that stove is cooled to room temperature and closes nitrogen.
Embodiment 5
By 32mg graphene dispersions in the ethanol of 40ml, ultrasonic disperse 30min.According to cigarette filter and dispersion liquid Mass volume ratio is 0.12g/ml, and useless cigarette filter is soaked 50s in the alcohol dispersion liquid of graphene, then pulls placement out 1min is shelved on culture dish.Then it is immersed in again in the dispersion liquid of ethanol, this process is repeated 18 times.By the cigarette mistake after immersion Filter tip is dried in an oven, and temperature is 90 DEG C, time 1h.Cigarette filter after drying is placed in crucible, in tube furnace Middle carbonization.Nitrogen, flow 85sccm are passed first into, furnace temperature keeps the temperature 140min, heating rate after being warming up to 860 DEG C~880 DEG C 10~20 DEG C/min, treat that stove is cooled to room temperature and closes nitrogen.

Claims (10)

1. a kind of preparation method of cigarette filter/graphene composite material, it is characterised in that the cigarette filter of recycling exists Soaked in graphene oxide-alcohol dispersion liquid several times, drying, is then carbonized, that is, obtains cigarette filter/graphene composite wood Material.
A kind of 2. preparation method of cigarette filter/graphene composite material according to claim 1, it is characterised in that The cigarette filter of the recycling is used filter tip, wherein after burning containing pipe tobacco, by the material of absorption generation.
A kind of 3. preparation method of cigarette filter/graphene composite material according to claim 1, it is characterised in that The concentration of the graphene oxide-alcohol dispersion liquid is 0.2g/L~1g/L.
A kind of 4. preparation method of cigarette filter/graphene composite material according to claim 1, it is characterised in that The immersion process is:First the cigarette filter of recycling is soaked in graphene oxide-alcohol dispersion liquid, is stood, Ran Houzai Secondary immersion, this process repeat 10~20 times, and each soaking time is 20~60s.
5. according to a kind of preparation method of cigarette filter/graphene composite material of claim 1-4 any one of them, it is special Sign is that the cigarette filter and the mass volume ratio of graphene oxide-alcohol dispersion liquid are 0.01~0.15g/ml.
6. according to a kind of preparation method of cigarette filter/graphene composite material of claim 1-4 any one of them, it is special Sign is that the drying temperature is 70~100 DEG C, and drying time is 1~2h.
7. according to a kind of preparation method of cigarette filter/graphene composite material of claim 1-4 any one of them, it is special Sign is that the carbonization is specially:After the cigarette filter of drying is put into tube furnace, nitrogen is passed through, furnace temperature is warming up to 800 DEG C~900 DEG C after keep the temperature 120~180min, treat stove be cooled to room temperature close nitrogen.
A kind of 8. preparation method of cigarette filter/graphene composite material according to claim 7, it is characterised in that 10~20 DEG C/min of heating rate.
A kind of 9. preparation method of cigarette filter/graphene composite material according to claim 7, it is characterised in that The nitrogen flow is 40~100sccm.
10. it is made using a kind of preparation method of cigarette filter/graphene composite material of claim 1-9 any one of them Cigarette filter/graphene composite material purposes, it is characterised in that the electrode material as ultracapacitor.
CN201711020223.4A 2017-10-27 2017-10-27 A kind of preparation method and its usage of cigarette filter/graphene composite material Pending CN107946082A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110449165A (en) * 2019-07-11 2019-11-15 广东工业大学 A kind of carbon fiber and its preparation method and application using load cadmium sulfide particle made of discarded cigarette butt
WO2020231362A1 (en) * 2019-05-10 2020-11-19 Kalabak Fevzi Recycling method of cigarette butts
CN113082205A (en) * 2021-04-08 2021-07-09 华南师范大学 Nano titanium dioxide photocatalytic antibacterial material, preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN104362340A (en) * 2014-09-18 2015-02-18 秦皇岛中科远达电池材料有限公司 High-performance lithium iron phosphate cathode material and preparation method thereof
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CN104362340A (en) * 2014-09-18 2015-02-18 秦皇岛中科远达电池材料有限公司 High-performance lithium iron phosphate cathode material and preparation method thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020231362A1 (en) * 2019-05-10 2020-11-19 Kalabak Fevzi Recycling method of cigarette butts
CN110449165A (en) * 2019-07-11 2019-11-15 广东工业大学 A kind of carbon fiber and its preparation method and application using load cadmium sulfide particle made of discarded cigarette butt
CN113082205A (en) * 2021-04-08 2021-07-09 华南师范大学 Nano titanium dioxide photocatalytic antibacterial material, preparation method and application thereof

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