CN106381682B - A kind of nano-titanium dioxide/active carbon fiber felt three-dimensional porous material of high absorption-photocatalysis performance and preparation method thereof - Google Patents
A kind of nano-titanium dioxide/active carbon fiber felt three-dimensional porous material of high absorption-photocatalysis performance and preparation method thereof Download PDFInfo
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- CN106381682B CN106381682B CN201610737919.8A CN201610737919A CN106381682B CN 106381682 B CN106381682 B CN 106381682B CN 201610737919 A CN201610737919 A CN 201610737919A CN 106381682 B CN106381682 B CN 106381682B
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- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic System; Titanates; Zirconates; Stannates; Plumbates
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Abstract
The present invention relates to Material Field, a kind of high absorption-photocatalysis performance nano-titanium dioxide/active carbon fiber felt three-dimensional porous material and preparation method thereof is disclosed.The material has three-dimensional porous structure using active carbon fiber felt as substrate, and nano-titanium dioxide is attached in active carbon fiber felt.Nano-titanium dioxide is mainly anatase, and partial size is 50nm~1 μm.Preparation method comprises the steps of：(1) active carbon fiber felt is immersed in zinc oxide crystal layer solution, Best-Effort request method, obtains the active carbon fiber felt of surface depositing zinc oxide crystal layer；(2) active carbon fiber felt of depositing zinc oxide crystal layer is immersed in titania growth liquid, by hydro-thermal method in zinc oxide crystal layer surface in situ growth of nano titanium dioxide.The method of the present invention is simple, easy to operate, economic and practical, environmentally friendly, and preparation gained composite material is had broad application prospects with stronger absorption property, higher photocatalysis performance and excellent filter effect in air purification field.
Description
Technical field
The present invention relates to weaving material field, field of inorganic nonmetallic material, indoor volatile organic gases (VOC) to handle
Field, specially a kind of high absorption-photocatalysis performance nano-titanium dioxide/active carbon fiber felt three-dimensional porous material and its preparation
Method.
Technical background
It is continuously improved with the development of economy with the civilization degree of social progress and human lives, the transition of life makes
People to rest on the indoor time increasingly longer.The all one's life of people, there are about 70%~92% times to be spent indoors, therefore good
Good indoor air environment is most important to human health.However, on the one hand since the airtightness of energy problem and building mentions
Height, fresh air volume is reduced in building；On the other hand it is the extensive application of new decorative material for building, gives off some harmful gas
Body.A series of stiff reactions are often shown so as to cause long-term work and the people lived in modern architecture.Its symptom is head
Bitterly, sleepy, nauseous, runny nose, several diseases of respiratory tract, alimentary canal, Neurology etc. ten, heavy then skin allergy, leukaemia and blood
Cancer.It is domestic for many years studies have shown that room air pollution degree is often more seriously polluted than outdoor environment, be easy to cause containing more
The harmful substance of human body diseases；The statistics of Environmental Protection Agency (EPA) shows that room air pollution degree often exceeds outdoor 2~5
Times, even exceed 100 times sometimes；Environmental Protection in America scientist has found that interior has 11 kinds of toxic chemical substance concentration to be higher than outdoor,
In 6 kinds be carcinogen.The investigation result of Canadian health organization show in current people's illnesses 68% all with Interior Space
Gas pollution is related.The World Health Organization announces：The whole world has 100,000 people to die of asthma because of room air pollution every year.It is indoor
Pollutants in air type is more, can be divided into physical contamination, chemical contamination, biological pollution by property.The wherein organic dirt of volatility
Dye object (Volatile Organic compounds, VOCs) is a kind of important indoor air pollutants.VOCs is by its chemistry
Structure can be divided into：Alkane, aromatic hydrocarbon, alkene, halohydrocarbon, aldehydes, ketone and other.
Currently, having absorption, biological treatment, chemical treatment, heat treatment, catalysis for the processing method that this pollutant uses
The methods of oxidation, phase transfer and photocatalytic degradation.Wherein, absorption and photocatalytic degradation are considered as eliminating these pollutants most to have
One of method of effect.Pollutant can be quickly removed by absorption, but is easy to reach saturation absorption and inactivate, while passing through desorption
Reproducing adsorbent may cause secondary pollution.Photocatalysis technology is a kind of environmental-friendly green technology.In the excitation lower half of light
Conductor material generates the very strong active specy of oxidisability, and with most organic pollutants molecule redox can occur for these species
Reaction, being allowed to thorough mineralising is carbon dioxide, water, mineral acid or salt etc..Compared with traditional method of contaminants disposal, photocatalysis skill
Art has (1) except cleanliness height, without secondary pollution；(2) it does not need to introduce other chemical species in the reaction；(3) using cheap
Solar energy degrade to organic matter.In photocatalysis technology, TiO2Light urges agent good, nontoxic, cheap with its chemical stability
The features such as being easy to get is known as ideal environmental improvement photochemical catalyst, this process does not need other chemical assistants, reacts item
Part is mild, is the research field for having very much development potentiality.However, TiO2The specific surface area of photochemical catalyst is limited, to pollution
The absorption property of object is poor, and pollutant is difficult to be enriched in catalyst surface, causes contaminant molecule and catalyst TiO2Molecular collision
It reduces, when degrading low-concentration organic, catalytic efficiency is very low.In addition, nanometer powder shape catalyst is solid in photocatalytic process
Fixed and separation is all more difficult, to strongly limit its application in actually pollution purification, it is therefore necessary to design
It is a kind of integrate absorption with photocatalysis and be easy to fix and isolated novel composite nano material.
In order to overcome these disadvantages, light is urged being combined together with adsorption technology in recent years by domestic and foreign scholars, is made full use of
Their own advantage improves air purification effect.It is useless containing phenol that 105129903 A of patent CN reports a kind of photocatalysis treatment
The preparation method of the titanium dioxide strainer of water is being made although the strainer of the method synthesis integrates absorption and photocatalysis
By activated carbon fibre and nano-titanium dioxide mechanical mixture during standby, the conjugation of composite material is low, the dust particles to fall off
Easily cause secondary pollution.104772133 A of patent CN reports a kind of indoor cleaning photoactivation agent and preparation method thereof, leads to
It crosses on the compound complex carries that nano-titanium dioxide is carried on to the formation of active carbon fibre peacekeeping mesoporous silicon oxide, improves nano-silica
Change the photocatalysis performance of titanium.But the technique patent has the following defects：(1) long preparation period, and three are used in preparation process
The reagents such as toluene, potassium bichromate can cause secondary pollution to environment.(2) preparation gained nano-titanium dioxide/activated carbon fibre-
Without any adhesive between nano-titanium dioxide and carrier in silica, conjugation is poor.(3) process conditions are more severe
It carves, needs control accurate pH, material need to be calcined to obtain under nitrogen protection.102658115 A of patent CN reports a kind of for sky
Cerium nano-titanium dioxide/activated carbon fibre composite photo-catalyst preparation method is mixed in gas purification, by by nano-titanium dioxide
It is added in cerous nitrate solution with activated carbon fibre, high temperature hydro-thermal (200-220 DEG C) mixes cerium two in activated carbon fibre surface deposition
Titanium oxide, hydrothermal temperature is excessively high in the technique, has security risk, and mix between cerium titanium dioxide and activated carbon fibre without any glue
Glutinous agent, so that most cerium nano-titanium dioxide of mixing not depends on active carbon fiber felt growth but reunites in fiber crossovers institute
In the duct of formation, reduces the absorption property of active carbon fiber felt itself and particle is easy to fall off, will cause secondary pollution.
Therefore, it is necessary to be improved the prior art, a kind of composite material with high absorption and photocatalysis performance is obtained.
Summary of the invention
The present invention is intended to provide a kind of high absorption-photocatalysis performance nano-titanium dioxide/active carbon fiber felt is three-dimensional porous
Material.
The present invention also provides the preparation methods of above-mentioned material.
Technical solution is a kind of high absorption-photocatalysis performance nano-titanium dioxide/three-dimensional porous material of active carbon fiber felt
Material, using active carbon fiber felt as substrate, and nano-titanium dioxide is attached in active carbon fiber felt；The material has three-dimensional more
Pore structure, aperture are 1~100 μm；Specific surface area is 200~3000m2/g；Nano-titanium dioxide partial size is 50nm~1 μm.
In the zinc oxide crystal layer that active carbon fiber felt surface deposition thickness is 500nm~1 μm, nano-titanium dioxide is attached
On zinc oxide crystal layer surface, and nano-titanium dioxide is mainly anatase.
Preferably, aperture is mainly distributed as 20~70 μm, more preferably 30~50 μm.
Preferably, nano-titanium dioxide partial size is 500nm~1 μm.
The preparation method of above-mentioned composite material includes：
(1) active carbon fiber felt of activating pretreatment is immersed in zinc oxide crystal layer solution, using Best-Effort request method, is obtained
Obtain the active carbon fiber felt of surface depositing zinc oxide crystal layer；
The Best-Effort request method is：(a) active carbon fiber felt of activating pretreatment is immersed in zinc oxide crystal layer solution,
2~10min is impregnated, then slowly lifting is taken out upwards with the speed of 1~5mm/s；Products therefrom is done under the conditions of 30~80 DEG C
Dry 20min~1hr；(b) above-mentioned Best-Effort request and drying process 1~8 time are repeated；(c) by the active carbon fiber felt of drying in 60
0.5~6hr is dried at~180 DEG C again；Obtain the active carbon fiber felt of surface depositing zinc oxide crystal layer；
The zinc oxide crystal layer solution preparation method includes the following steps：Soluble zinc salt is dissolved in alcohol；Then plus
Enter triethylamine, 10min~1hr is stirred under the conditions of 30~100 DEG C, and be aged 1~5hr in room temperature condition, obtain zinc oxide crystalline substance
Layer solution；
Wherein zinc ion content is 0.02~0.3mol/L, and zinc ion and triethylamine molar ratio are 1：0.2~3；Preferably,
Zinc ion content is 0.04~0.25mol/L, and zinc ion and triethylamine molar ratio are 1：0.4~2.5；
The soluble zinc salt is acetic acid dihydrate zinc or zinc nitrate hexahydrate；The alcohol is selected from methanol, ethyl alcohol, third
Alcohol, n-butanol, isobutanol or the tert-butyl alcohol.
(2) it is raw to immerse nano-titanium dioxide for the active carbon fiber felt of surface depositing zinc oxide crystal layer prepared by step (1)
In long liquid, the r of hydro-thermal reaction 2 at 100~200 DEG C~for 24 hours；
The nano-titanium dioxide growth-promoting media contains 0.05~0.25mol/L TiO 2 precursor, 0.3~1mol/L
Sulfuric acid and 0.5~5mol/L hydrochloric acid；The molar ratio of TiO 2 precursor and sulfuric acid is 1:1~8, the molar ratio of sulfuric acid and hydrochloric acid
It is 1：0.2~8；Preferably, TiO 2 precursor content is 0.08~0.15mol/L, and sulfuric acid content is 0.5~1mol/L,
Content of hydrochloric acid is 0.5~5mol/L, and the molar ratio of TiO 2 precursor and sulfuric acid is 1:6~8, the molar ratio of sulfuric acid and hydrochloric acid
It is 1：0.5~6.
In step (1), 200~3000m of specific surface area of the active carbon fiber felt2/ g, with a thickness of 1~20mm.It is described
The preprocess method of active carbon fiber felt be that active carbon fiber felt is cut into required shape, is then placed it in containing surface
Activating agent, acid, alkaline matter pretreatment fluid in, under the conditions of 50~120 DEG C stir 1~2h, respectively through deionized water and second
It is dry under the conditions of 30~80 DEG C after alcohol cleaning；In the pretreatment fluid, the concentration of surfactant is 1~10mmol/L,
The concentration of acid is 1~10mmol/L, and the concentration of alkaline matter is 100~500mmol/L.The surfactant is selected from
Triton-X100, beta-cyclodextrin or cetyl trimethylammonium bromide；The acid is monohydrate potassium, glycine or borax；
The alkaline matter is sodium hydroxide, potassium hydroxide or sodium citrate.
The present invention for substrate, prepares nanometer titanium dioxide by hydro-thermal method with weaving material active carbon fiber felt (ACFF)
Titanium/active carbon fiber felt three-dimensional porous material.One layer of oxidation is deposited on active carbon fiber felt surface by dip-coating method first
Zinc crystal layer, the zinc oxide crystal layer serve as the adhesive between nano-titanium dioxide and active carbon fiber felt, effectively prevent existing
In technology, the caducous problem of active carbon fiber felt surfacing.Zinc oxide crystal layer with a thickness of 500nm~1 μm, if crystal layer is thick
Degree is more than the range, and micro-sphere structure made of active carbon fiber felt surface nano-titanium dioxide particle packing is destroyed, direct shadow
Ring the Photocatalytic Degradation Property of composite material.Then by hydro-thermal method, the active carbon fiber felt for loading zinc oxide crystal layer is immersed
In the precursor solution of titanium dioxide, anatase nano-titanium dioxide is grown in zinc oxide crystal layer surface in situ.
Nano-titanium dioxide obtained depends on active carbon fiber felt growth, will not block the duct of carbon fiber felt itself.
Composite material has three-dimensional porous structure, large specific surface area；Conjugation between material and active carbon fiber felt is high and in absorption-
Stronger activity is shown in Photocatalytic Degradation of Toluene experiment, adsorption rate is up to after 95%, 35h to high concentration toluene after 1.5h
Degradation rate be up to 80%.Preparing raw material used in the composite material is common analytical pure reagent, safely and will not be to ring
Cause secondary pollution in border.
The beneficial effects of the present invention are：
(1) nano-titanium dioxide prepared by the present invention/active carbon fiber felt three-dimensional porous material, with activity cheap and easy to get
Carbon fibe felt is substrate, deposits the zinc oxide crystal layer that a layer thickness is 500nm~1 μm on its surface by dip-coating method；Benefit
The adhesive between nano-titanium dioxide and active carbon fiber felt is served as with the crystal layer, effectively prevent active carbon fiber felt surface
Then the active carbon fiber felt for loading zinc oxide crystal layer is immersed in the precursor liquid of nano-titanium dioxide, is passed through by material falls back
Hydro-thermal method grows anatase-phase nano titanium dioxide in zinc oxide crystal layer surface in situ, and preparation gained nano-titanium dioxide depends on work
Property Carbon fibe growth, the duct of active carbon fiber felt itself will not be blocked.It is method safety, simple to operation, economical and to environment
It is friendly.
(2) nano-titanium dioxide prepared by the present invention/active carbon fiber felt three-dimensional porous material, there is biggish specific surface
Product, and the nano-titanium dioxide of active carbon fiber felt substrate surface is partial size between 50nm to 1 μm of microballoon, has porous knot
Structure.The microspheric superstructure can provide more active sites in Photocatalytic Degradation Process.Work with stronger absorption property
Property Carbon fibe felt is mutually cooperateed with the nanometer titanium dioxide micro-sphere of superstructure, substantially increases photocatalysis efficiency.
(3) nano-titanium dioxide prepared by the present invention/active carbon fiber felt three-dimensional porous material has mechanicalness appropriate
Can there are stronger absorption property, higher photocatalysis performance and excellent filter effect with good processability, handle
When volatile organic gases, secondary pollution not will cause to environment, be fully utilized convenient for it in photocatalysis field, it is net in air
Change field has broad application prospects.
Detailed description of the invention
Nano-titanium dioxide/active carbon fiber felt three-dimensional porous material SEM image that Fig. 1 is prepared for embodiment 1, a, b,
C is zinc oxide crystal layer/active carbon fiber felt of different multiples.
SEM photograph, d, e, f are nano-titanium dioxide/active carbon fiber felt SEM photograph of different multiples.
Fig. 2 is the graph of pore diameter distribution of active carbon fiber felt used in embodiment 1.
Fig. 3 is nano-titanium dioxide/active carbon fiber felt three-dimensional porous material pore-size distribution prepared by embodiment 1
Figure.
Fig. 4 is nano-titanium dioxide/active carbon fiber felt three-dimensional porous material nano surface titanium dioxide prepared by embodiment 1
The TEM photo of titanium, wherein a, b are high low power TEM photo, and c is electronic diffraction ring piece.
Fig. 5 is nano-titanium dioxide/active carbon fiber felt three-dimensional porous material XRD spectrum prepared by embodiment 1, and a is
The XRD spectra of active carbon fiber felt, b are nano-titanium dioxide/active carbon fiber felt XRD spectra.
Fig. 6 is that nano-titanium dioxide/active carbon fiber felt three-dimensional porous material absorption various concentration prepared by embodiment 1 is waved
Toluene adsorption curve after hair property organic gas toluene experiment, the dosage of curve (a) toluene are 2 μ L, concentration 1734mg/m3
(460ppm)；The dosage of curve (b) toluene is 3.5 μ L, concentration 3305mg/m3(877ppm)；The dosage of curve (c) toluene is
5 μ L, concentration 4335mg/m3(1150ppm)。
Fig. 7 is that nano-titanium dioxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation prepared by embodiment 1 is different
CO after intensity volatile organic gas toluene experiment2The dosage of generating rate curve, curve (a) toluene is 2 μ L, and concentration is
1734mg/m3(460ppm)；The dosage of curve (b) toluene is 3.5 μ L, concentration 3305mg/m3(877ppm)；Curve (c) toluene
Dosage be 5 μ L, concentration 4335mg/m3(1150ppm)。
Fig. 8 is that nano-titanium dioxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation prepared by embodiment 1 is different
The dosage of CO generating rate curve after intensity volatile organic gas toluene experiment, curve (a) toluene is 2 μ L, and concentration is
1734mg/m3(460ppm)；The dosage of curve (b) toluene is 3.5 μ L, concentration 3305mg/m3(877ppm)；Curve (c) toluene
Dosage be 5 μ L, concentration 4335mg/m3(1150ppm)。
Fig. 9 is that nano-titanium dioxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation prepared by embodiment 1 is different
Degradation rate curve after intensity volatile organic gas toluene experiment.The dosage of curve (a) toluene is 2 μ L, concentration 1734mg/
m3(460ppm)；The dosage of curve (b) toluene is 3.5 μ L, concentration 3305mg/m3(877ppm)；The dosage of curve (c) toluene
For 5 μ L, concentration 4335mg/m3(1150ppm)。
Specific example mode
Below in conjunction with specific embodiment, the present invention is further explained.
Embodiment 1
(1) 1.10g acetic acid dihydrate zinc (5mmol) is accurately weighed to be added in 50mL (0.65mol) isopropanol (AR),
15min is stirred under the conditions of 85 DEG C, and 0.7mL (5mmol) triethylamine (AR) is then added, stirs 5min under the conditions of 85 DEG C, and in
It is aged 3h under room temperature to get zinc oxide crystal layer solution.
(2) by active carbon fiber felt (thickness：1mm, specific surface area 1100m2/ g) it is cut into the bulk of 2cm*2cm*1mm, it sets
In the pretreatment fluid containing 5mmol/L Triton-X100,5mmol/L monohydrate potassium and 300mmol/L sodium hydroxide,
1.5h is stirred under the conditions of 100 DEG C；Respectively after deionized water and ethyl alcohol cleaning, dry 1hr under the conditions of 60 DEG C.
(3) step (2) are pre-processed and dry active carbon fiber felt immerse in the zinc oxide crystal layer solution of step (1),
5min is impregnated, active carbon fiber felt is then lifted vertically upwards with the speed of 1mm/s, products therefrom is dried under the conditions of 60 DEG C
30min, then repeats above-mentioned Best-Effort request process 4 times, the activated fibre substrate of drying is again placed in baking oven, at 120 DEG C
1h is dried again, it can be in the zinc oxide crystal layer of active carbon fiber felt surface deposition compact.
(4) by 0.5mL (0.00142mol) butyl titanate (AR), 2mL (0.02347mol) concentrated hydrochloric acid (AR), 0.5mL
(0.00936mol) concentrated sulfuric acid (AR) is mixed with 10mL secondary distilled water, stirs 30min under room temperature, is then aged 1h, i.e.,
Obtain nano-titanium dioxide growth-promoting media.
(5) the nano-titanium dioxide growth-promoting media of 10mL is added into water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
It ties up felt to immerse in growth-promoting media, water heating kettle is sealed, hydro-thermal 4h, is cooled to room temperature to water heating kettle under the conditions of 180 DEG C, takes out and produces
Object rinses 2~5 times with ethyl alcohol and secondary distilled water to get nano-titanium dioxide/active carbon fiber felt three-dimensional porous material.
The active carbon fiber felt and nano-titanium dioxide/active carbon fibre of load zinc oxide crystal layer resulting to embodiment 1
The pattern of dimension felt three-dimensional porous material is mutually characterized with object, gained scanning electron microscope image (SEM), pore-size distribution map, transmission
Sem image (TEM) and wide-angle x ray diffraction map (XRD) are respectively as shown in Fig. 1,2,3,4,5.
By the SEM picture of Fig. 1 (a, d) it is found that preparing resulting material with three-dimensional porous structure, wherein a figure is blank
The low-powered microscope photo of active carbon fiber felt, d figure are nano-titanium dioxide/active carbon fiber felt three-dimensional porous material low power
Microscope photo.By the SEM picture of Fig. 1 (b, c) it is found that the surface active carbon fiber felt (ACFF) deposited one layer of fine and close oxidation
Zinc crystal layer (thickness 500nm~1 μm), and the crystal layer is accumulated by nano particle.By the SEM of Fig. 1 (e, f) it is found that after hydro-thermal
The nano particle of some spherical shapes is grown in zinc oxide crystal layer surface in situ, diameter is about 900nm, is demonstrate,proved through XRD spectra (Fig. 2)
Bright, which is the nano-titanium dioxide of Anatase.The TEM photo (a) of Fig. 4 further proves activated carbon fibre
The titanium dioxide on felt surface be micro-sphere structure, electronic diffraction ring piece (c) show the microballoon be polycrystalline structure, if illustrate it be by
Dry titanium dioxide nanoparticle is accumulated, and several irregular stacking holes are scattered with inside microballoon.SEM picture (e, f)
Display titanium dioxide nanoparticle is grown on active carbon fiber felt surface, rather than reunites in the duct of fibrofelt, does not influence
The absorption property of active carbon fiber felt.Moreover, compared with the Titanium dioxide/active carbon fibrofelt that prior art mixing method obtains,
The nano-titanium dioxide obtained of embodiment 1/active carbon fiber felt three-dimensional porous material is after touching, the titanium dioxide of attachment
Nano particle is not easy to fall off.Fig. 2,3 are respectively blank active carbon fiber felt and nano-titanium dioxide/active carbon fiber felt three
The graph of pore diameter distribution of porous material is tieed up, the graph of pore diameter distribution spectrum of Fig. 2 shows that active carbon fiber felt has porous structure, and aperture is main
It is distributed in 25~40 μm；The graph of pore diameter distribution of Fig. 3, which is composed, to be shown after its area load nano-titanium dioxide, active carbon fiber felt
The three-dimensional porous structure of itself is not destroyed, and with the attachment of material, aperture increases are mainly distributed on 35~50 μm.Three
Tie up the specific surface area about 1100m of porous material2/g。
The low power TEM photo and electronic diffraction ring piece of Fig. 4 three-dimensional porous material surface nano-titanium dioxide show,
The titanium dioxide of active carbon fiber felt surface growth is porous microsphere structure made of nano particle accumulation.
Embodiment 2
The organic gas of volatility is carried out to the resulting nano-titanium dioxide of embodiment 1/active carbon fiber felt three-dimensional porous material
The absorption of body toluene and photocatalytic degradation experiment：
(1) 4 nano-titanium dioxides/active carbon fiber felt three-dimensional porous material (quality about 0.2g) is taken, reactor tank is placed in
Bottom.Then, 2 μ L, 3.5 μ L, 5 μ L toluene are injected separately into reactor tank with microsyringe.It is carried out under room temperature no light condition
Half-light adsorbs 1.5h, and every 1min acquires a gaseous sample, carries out online content with INNOVA-1412i infrared photo acoustic chromatograph
Analysis.
(2) after adsorption equilibrium, opening ultraviolet source (high-pressure sodium lamp, 32W) progress photocatalytic degradation experiment, illumination 35h, often
1min acquires a gaseous sample, carries out content analysis by INNOVA-1412i infrared photo acoustic chromatograph.According to the dense of toluene
Degree variation and CO2, CO generating rate, it is three-dimensional more to compare nano-titanium dioxide under various concentration gradient/active carbon fiber felt
The adsorption-photocatalytic degradation activity of Porous materials.
Absorption-photocatalysis experiment the data obtained of above-mentioned volatile organic gases toluene draw and analyzed, no
Adsorption curve with concentration toluene is as shown in fig. 6, CO during various concentration Photocatalytic Degradation of Toluene2, CO generating rate curve
As shown in Figure 7,8.The experimental results showed that first of the nano-titanium dioxide/active carbon fiber felt three-dimensional porous material to various concentration
Benzene shows stronger absorption property, and adsorption efficiency is up to 95%~98% within 1.5h.To degradation various concentration toluene
CO in the process2, CO generating rate curve carry out linear fit, fitting result shows after turning on light three-dimensional porous material in 500min
Material is very fast to the degradation rate of toluene, can be attributed to absorption and light-catalysed mutual synergistic effect；After 500min, CO, CO2Life
At good linear relationship is kept between rate and the concentration of toluene, illustrate that nano-titanium dioxide/active carbon fiber felt is three-dimensional more
Porous materials stability in entire Photocatalytic Degradation Process is stronger.Compare CO and CO2Production quantity, due to entire photocatalytic degradation
The production quantity of CO is less than CO in the process2The 1% of production quantity, therefore CO can be ignored during Photocatalytic Degradation of Toluene.
The degradation rate curve of various concentration toluene is as shown in Figure 9.As the concentration of toluene increases, toluene in same time
Degradation rate is respectively 81.5%, 61.6%, 57.0%, illustrates nano-titanium dioxide/active carbon fiber felt three-dimensional porous material pair
Preferable Photocatalytic Degradation Property is still remain in the degradation of high concentration toluene, which is that the reality of composite material is answered
With providing strong theoretical foundation.
Embodiment 3
(1) 1.10g acetic acid dihydrate zinc (5mmol) is accurately weighed to be added in 100mL (1.31mol) isopropanol (AR),
15min is stirred under the conditions of 85 DEG C, 1.4mL (10mmol) triethylamine (AR) is then added, stirs 5min under the conditions of 85 DEG C, and
In ageing 3h under room temperature to get zinc oxide crystal layer solution.
(2) active carbon fiber felt is cut into 2cm*2cm*1mm (thickness：1mm, specific surface area 1100m2/ g) bulk, in advance
It is dry after processing, with 1 step of embodiment (2).
(3) step (2) are pre-processed and dry active carbon fiber felt immerse in the zinc oxide crystal layer solution of step (1),
2min is impregnated, active carbon fiber felt is then lifted vertically upwards with the speed of 5mm/s, products therefrom is dried under the conditions of 80 DEG C
1h, then repeats above-mentioned Best-Effort request process 8 times, and the activated fibre substrate of drying is again placed in baking oven, and 180 DEG C are done again
Dry, dry 4h can be in active carbon fiber felt surface depositing zinc oxide crystal layer.
(4) with 1 step of embodiment (4).
(5) with 1 step of embodiment (5).
Obtained three-dimensional porous material electron microscope, XRD spectra result have good light with embodiment 1, and to toluene
Catalytic degradation performance.
Embodiment 4
(1) (2) are the same as 1 step of embodiment (1) (2).
(3) it will be immersed in zinc oxide crystal layer solution by pretreatment and dry active carbon fiber felt, impregnate 20min, so
Active carbon fiber felt is lifted vertically upwards with the speed of 5mm/s afterwards, products therefrom dries 1h under the conditions of 30 DEG C, then repeats
It states Best-Effort request process 5 times, the activated fibre substrate of drying is again placed in baking oven, 180 DEG C are dried again, dry 1h, i.e.,
It can be in active carbon fiber felt surface depositing zinc oxide crystal layer.
(4) by 0.5mL butyl titanate (0.00142mol), 4mL (0.04695mol) concentrated hydrochloric acid (AR), 0.5mL
(0.93622mol) concentrated sulfuric acid (AR) is mixed with 10mL secondary distilled water, stirs 1h under room temperature, is aged 3h then to get receiving
Rice titania growth liquid.
(5) the nano-titanium dioxide growth-promoting media of 10mL is added into water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
It ties up felt to immerse in growth-promoting media, water heating kettle is sealed, hydro-thermal for 24 hours, is cooled to room temperature to water heating kettle under the conditions of 100 DEG C, is taken out and is produced
Object is rinsed with ethyl alcohol and secondary distilled water for several times to get nano-titanium dioxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result have good light with embodiment 1, and to toluene
Catalytic degradation performance.
Embodiment 5
(1) with 3 step of embodiment (1).
(2) active carbon fiber felt is cut into 2cm*2cm*1mm (thickness：1mm, specific surface area 1100m2/ g) bulk, in advance
It is dry after processing, with 1 step of embodiment (2).
(3) it will be immersed in zinc oxide crystal layer solution by pretreatment and dry active carbon fiber felt, impregnate 10min, so
Active carbon fiber felt is lifted vertically upwards with the speed of 1mm/s afterwards, products therefrom is dried 1h under the conditions of 80 DEG C, then repeated
It states Best-Effort request process 5 times, the activated fibre substrate of drying is dried under the conditions of 30 DEG C, dry 4h, it can be in active carbon fibre
Tie up felt surface depositing zinc oxide crystal layer.
(4) with 4 step of embodiment (4).
(5) the nano-titanium dioxide growth-promoting media of 10mL is added into water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
It ties up felt to immerse in growth-promoting media, water heating kettle is sealed, hydro-thermal 14h, is cooled to room temperature to water heating kettle under the conditions of 180 DEG C, takes out and produces
Object is rinsed with ethyl alcohol and secondary distilled water for several times to get nano-titanium dioxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result have good light with embodiment 1, and to toluene
Catalytic degradation performance.
Embodiment 6
(1) 1.10g acetic acid dihydrate zinc (5mmol) is accurately weighed to be added in 25mL (0.33mol) isopropanol (AR),
1h is stirred under the conditions of 30 DEG C, and 0.35mL (2.5mmol) triethylamine (AR) is then added, stirs 1h under the conditions of 30 DEG C, and in room
5h is aged under the conditions of temperature to get zinc oxide crystal layer solution.
(2) with 5 step of embodiment (2).
(3) dry active carbon fiber felt is immersed in zinc oxide crystal layer solution, 10min is impregnated, then with the speed of 2mm/s
Degree upwards dry 1h under the conditions of 30 DEG C, then repeat above-mentioned Best-Effort request mistake by vertical lifting active carbon fiber felt, products therefrom
Journey 5 times, the activated fibre substrate of drying is dried under the conditions of 60 DEG C, dries 4h, can be deposited on active carbon fiber felt surface
Zinc oxide crystal layer.
(4) by 0.5mL (0.00142mol) butyl titanate (AR), 0.5mL (0.00587mol) concentrated hydrochloric acid (AR),
0.5mL (0.93622mol) concentrated sulfuric acid (AR) is mixed with 10mL secondary distilled water, is stirred 1h under room temperature, is then aged 3h,
Up to nano-titanium dioxide growth-promoting media.
(5) the nano-titanium dioxide growth-promoting media of 10mL is added into water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
It ties up felt to immerse in growth-promoting media, water heating kettle is sealed, hydro-thermal 2h, is cooled to room temperature to water heating kettle under the conditions of 200 DEG C, takes out and produces
Object is rinsed with ethyl alcohol and secondary distilled water for several times to get nano-titanium dioxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result have good light with embodiment 1, and to toluene
Catalytic degradation performance.
Embodiment 7
(1)~(3) are the same as 6 step of embodiment (1)~(3).
(4) it will be immersed in zinc oxide crystal layer solution by pretreatment and dry active carbon fiber felt, impregnate 5min, then
Active carbon fiber felt is vertically lifted upwards with the speed of 2mm/s, and products therefrom is dried 30min under the conditions of 60 DEG C, then repeated
Above-mentioned Best-Effort request process 4 times dries the activated fibre substrate of drying under the conditions of 100 DEG C, dries 2h, can be in active carbon
Fibrofelt surface depositing zinc oxide crystal layer.
(4) with 5 step of embodiment (4).
(5) the nano-titanium dioxide growth-promoting media of 10mL is added into water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
It ties up felt to immerse in growth-promoting media, water heating kettle is sealed, hydro-thermal 14h, is cooled to room temperature to water heating kettle under the conditions of 150 DEG C, takes out and produces
Object is rinsed with ethyl alcohol and secondary distilled water for several times to get nano-titanium dioxide/active carbon fiber felt three-dimensional porous material.
The obtained nano-titanium dioxide of embodiment 3~7/active carbon fiber felt three-dimensional porous material, electron microscope, XRD
Spectrogram result has good Photocatalytic Degradation Property with embodiment 1, and to toluene, and titanium dioxide nanoparticle is not easy
It falls off.
The above embodiment is a preferred embodiment of the present invention, but protection scope of the present invention is not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.The term occurred in the present invention is used for this
The elaboration and understanding of inventive technique scheme, are not construed as limiting the invention.
Claims (8)
1. a kind of nano-titanium dioxide/active carbon fiber felt three-dimensional porous material of high absorption-photocatalysis performance, feature exist
In using active carbon fiber felt as substrate, and nano-titanium dioxide is attached in active carbon fiber felt；
The material has three-dimensional porous structure, and aperture is 1~100 μm；Specific surface area is 200~3000m2/g；
The nano-titanium dioxide partial size is 50nm~1 μm；
In the zinc oxide crystal layer that active carbon fiber felt surface deposition thickness is 500nm~1 μm, nano-titanium dioxide is attached to
Zinc oxide crystal layer surface, and the nano-titanium dioxide is mainly anatase.
2. the nano-titanium dioxide of high absorption-photocatalysis performance/active carbon fiber felt three-dimensional porous material described in claim 1,
It is characterized in that, the nano-titanium dioxide partial size is 500nm~1 μm.
3. the three-dimensional porous material of nano-titanium dioxide/active carbon fiber felt of high absorption-photocatalysis performance as claimed in claim 1 or 2
The preparation method of material, which is characterized in that step includes：
(1) active carbon fiber felt of activating pretreatment is immersed in zinc oxide crystal layer solution, using Best-Effort request method, obtains table
The active carbon fiber felt of face depositing zinc oxide crystal layer；
The zinc oxide crystal layer solution is the alcoholic solution containing soluble zinc salt, triethylamine；Wherein zinc ion content is 0.02
The molar ratio of~0.3mol/L, zinc ion and triethylamine is 1：0.2~3；
(2) active carbon fiber felt of surface depositing zinc oxide crystal layer prepared by step (1) immerses nano-titanium dioxide growth-promoting media
In, hydro-thermal reaction 2~r, washing for 24 hours is dried to obtain nano-titanium dioxide/work of high absorption-photocatalysis performance at 100~200 DEG C
Property Carbon fibe felt three-dimensional porous material；
In the nano-titanium dioxide growth-promoting media, TiO 2 precursor content is 0.05~0.25mol/L, also contains 0.3
~1mol/L sulfuric acid and 0.5~5mol/L hydrochloric acid；The molar ratio of TiO 2 precursor and sulfuric acid is 1:1~8, sulfuric acid and hydrochloric acid
Molar ratio be 1：0.2~8；
The TiO 2 precursor is butyl titanate, isopropyl titanate or titanium tetrachloride.
4. the three-dimensional porous material of nano-titanium dioxide/active carbon fiber felt of high absorption-photocatalysis performance according to claim 3
The preparation method of material, which is characterized in that in step (1) the zinc oxide crystal layer solution；Soluble zinc salt is acetic acid dihydrate zinc
Or zinc nitrate hexahydrate；The alcohol is selected from methanol, ethyl alcohol, propyl alcohol, n-butanol, isobutanol or the tert-butyl alcohol；Wherein zinc ion contains
Measuring is 0.04~0.25mol/L, and the molar ratio of zinc ion and triethylamine is 1：0.4~2.5.
5. the nano-titanium dioxide of high absorption-photocatalysis performance according to claim 3 or 4/active carbon fiber felt is three-dimensional
The preparation method of porous material, which is characterized in that the zinc oxide crystal layer solution preparation method includes the following steps：It will be solvable
Property zinc salt is dissolved in alcohol；Then triethylamine is added, 10min~1hr is stirred under the conditions of 30~100 DEG C, and old in 10~40 DEG C
Change 1~5hr, obtains zinc oxide crystal layer solution.
6. a kind of nano-titanium dioxide of high absorption-photocatalysis performance according to claim 3/active carbon fiber felt is three-dimensional
The preparation method of porous material, which is characterized in that in nano-titanium dioxide growth-promoting media described in step (2), titanium dioxide forerunner
Body content is 0.08~0.15mol/L, and sulfuric acid content is 0.5~1mol/L, and content of hydrochloric acid is 0.5~5mol/L, titanium dioxide
The molar ratio of presoma and sulfuric acid is 1:6~8, the molar ratio of sulfuric acid and hydrochloric acid is 1：0.5~6.
7. nano-titanium dioxide/active carbon fiber felt of high absorption-photocatalysis performance according to claim 3 is three-dimensional porous
The preparation method of material, which is characterized in that the 200~3000m of specific surface area of step (1) described active carbon fiber felt2/ g, it is described
The preprocess method of active carbon fiber felt be that active carbon fiber felt is cut into required shape, then place it in containing
In the pretreatment fluid of Triton-X100, citric acid and sodium hydroxide, 1~2h is stirred under the conditions of 50~120 DEG C, is passed through respectively
It is dry under the conditions of 30~80 DEG C after deionized water and ethyl alcohol cleaning；
In the pretreatment fluid, the concentration of Triton-X100 is 1~10mmol/L, and the concentration of citric acid is 1~10mmol/L,
The concentration of sodium hydroxide is 100~500mmol/L.
8. nano-titanium dioxide/active carbon fiber felt of high absorption-photocatalysis performance according to claim 3 is three-dimensional porous
The preparation method of material, which is characterized in that Best-Effort request method is in step (1)：
(a) active carbon fiber felt of activating pretreatment is immersed in zinc oxide crystal layer solution, impregnates 2~10min, then with 1~
The speed of 5mm/s upwards slowly take out by lifting, products therefrom dry 20min~1hr under the conditions of 30~80 DEG C；
(b) above-mentioned Best-Effort request and drying process 1~8 time are repeated；
(c) active carbon fiber felt of drying is dried to 0.5~6hr again at 60~180 DEG C.
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| CN106964330B (en) * | 2017-04-07 | 2019-04-12 | 武夷学院 | Activated carbon fiber film loads TiO2The preparation method of/ZnO photocatalyst |
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| CN110270312B (en) * | 2019-06-21 | 2022-07-15 | 四川农业大学 | Metal organic framework material-activated carbon composite fiber membrane and preparation method thereof |
| CN110538629A (en) * | 2019-08-06 | 2019-12-06 | 广东工业大学 | Method for preparing adsorption material by using mobile phone protective film adhesive, prepared adsorption material and application |
| CN112323480A (en) * | 2020-11-25 | 2021-02-05 | 重庆纤维研究设计院股份有限公司 | Method for preparing rod-shaped zinc oxide photocatalytic particle composite fiber felt for air purification |
| CN112619411B (en) * | 2020-12-14 | 2023-08-25 | 山东飞薄新材料科技有限公司 | Preparation method and application of air purification material with fiber bundles as base material |
| 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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