CN106381682A - Nano-TiO2/activated carbon fibrofelt three-dimensional porous material high in adsorption and photocatalytic performance, and preparation method thereof - Google Patents
Nano-TiO2/activated carbon fibrofelt three-dimensional porous material high in adsorption and photocatalytic performance, and preparation method thereof Download PDFInfo
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- CN106381682A CN106381682A CN201610737919.8A CN201610737919A CN106381682A CN 106381682 A CN106381682 A CN 106381682A CN 201610737919 A CN201610737919 A CN 201610737919A CN 106381682 A CN106381682 A CN 106381682A
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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
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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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- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- 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
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Abstract
The invention relates to the field of materials and discloses a nano-TiO2/activated carbon fibrofelt three-dimensional porous material high in adsorption and photocatalytic performance, and a preparation method thereof. The material is of a three-dimensional porous structure and an activated carbon fibrofelt is adopted as a substrate. Meanwhile, nano-TiO2 is adhered inside the activated carbon fibrofelt. The nano-TiO2 is mainly composed of anatase and the partical size of the nano-TiO2 is 50 nm-1 mum. The preparation method comprises the following steps: (1) dipping the activated carbon fibrofelt into a zinc oxide crystal layer solution, and obtaining the activated carbon fibrofelt with a zinc oxide crystal layer deposited on the surface thereof through the dip-coating method; (2) dipping the activated carbon fibrofelt with the zinc oxide crystal layer deposited on the surface thereof into a TiO2 growth-promoting solution, and growing nano-TiO2 in situ on the surface of the zinc oxide crystal layer through the hydrothermal method. The method is simple, easy to operate, economical, applicable and environmentally-friendly. The prepared composite material is strong in adsorption performance, high in photocatalytic performance and excellent in filtering effect. Therefore, the material has a wide application prospect in the field of air purification.
Description
Technical field
The present invention relates to weaving material field, field of inorganic nonmetallic material, indoor volatile organic gas (VOC) process
Field, specially a kind of height absorption-photocatalysis performance nano titanium oxide/active carbon fiber felt three-dimensional porous material and its preparation
Method.
Technical background
The civilization degree of the progress with expanding economy and society and human lives improves constantly, and the transition of life makes
Obtain people's stop time indoors more and more longer.The time that all one's life of people there are about 70%～92% is spent indoors, therefore good
Good indoor air environment is most important to health.However, on the one hand because the seal of energy problem and building carries
Height, in building, resh air requirement reduces；On the other hand it is the extensive application of new decorative material for building, give off some harmful gas
Body.Thus leading to long-term work and the people that live in modern architecture often show a series of stiff reactions.Its symptom is head
Bitterly, sleepy, nauseous, watery nasal discharge, several disease of respiratory tract, digestive tract, Neurology Department etc. ten, heavy then skin allergy, leukemia and blood
Cancer.Domestic research for many years shows, room air pollution degree is often seriously polluted than outdoor environment, containing more easily causing
The harmful substance of human body diseases；The statistics of U.S. Environmental Protection Agency (EPA) (EPA) shows, room air pollution degree often exceeds outdoor 2～5
Times, sometimes even exceed 100 times；It is higher than outdoor that Environmental Protection in America scientist finds that there are 11 kinds of toxic chemical substance concentration interior, its
In 6 kinds be carcinogen.The survey result of Canadian health organization show in current people's illnesses 68% all with Interior Space
Gas pollution is relevant.World Health Organization (WHO) announces：The whole world has 100,000 people to die from asthma because of room air pollution every year.Indoor
Pollutants in air species is more, can be divided into physical contamination, chemical contamination, biological pollution by property.The wherein organic dirt of volatility
Dye thing (Volatile Organic compounds, VOCs) is the important indoor air pollutants of a class.VOCs presses its chemistry
Structure can be divided into：Alkane, aromatic hydrocarbon, alkene, halohydrocarbon, aldehydes, ketone and other.
At present, the processing method using for this pollutant has absorption, biological treatment, chemical treatment, heat treatment, catalysis
The methods such as oxidation, phase transfer and photocatalytic degradation.Wherein, absorption and photocatalytic degradation are considered as to eliminate these pollutant to have most
One of method of effect.Pollutant quickly can be removed by absorption, but easily reach saturation absorption and inactivate, pass through desorption simultaneously
Reproducing adsorbent is likely to result in secondary pollution.Photocatalysis technology is a kind of eco-friendly green technology.Excite lower half in light
Conductor material produces the very strong active specy of oxidisability, and these species can occur oxidoreduction with most organic pollutants molecule
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) and removes cleanliness height, non-secondary pollution；(2) do not need to introduce other chemical species in the reaction；(3) can be utilized inexpensively
Solar energy Organic substance is degraded.In photocatalysis technology, TiO2Light urges agent good, nontoxic, cheap with its chemical stability
The features such as be easy to get, is described as ideal environmental improvement photocatalyst, and this process does not need other chemical assistants, reacts bar
Part is gentle, is a research field having very much development potentiality.However, TiO2The specific surface area of photocatalyst is limited, to pollution
The absorption property of thing is poor, and pollutant are difficult to be enriched with catalyst surface, causes contaminant molecule and catalyst TiO2Molecular collision
Reduce, 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, thus strongly limit its application in actual pollution purifies it is therefore necessary to design
One kind integrates absorption and with photocatalysis and is easy to fix and detached novel composite nano material.
In order to overcome these shortcomings, light is urged and being combined together with adsorption technology by Chinese scholars in recent years, makes full use of
The advantage of each of which, improves air purification effect.Patent CN 105129903 A reports a kind of photocatalysis treatment and gives up containing phenol
The preparation method of the titanium dioxide filter screen of water, although the filter screen of the method synthesis integrates absorption and photocatalysis, in system
By NACF and nano titanium oxide mechanical mixture during standby, the conjugation of composite is low, the dust granules coming off
Easily cause secondary pollution.Patent CN 104772133 A reports a kind of indoor cleaning photoactivation agent and preparation method thereof, leads to
Cross and nano titanium oxide is carried on the compound complex carries of active carbon fibre peacekeeping mesoporous silicon oxide formation, improve nano-silica
Change the photocatalysis performance of titanium.But there is following defect in this technique patent：(1) using three in long preparation period, and preparation process
The reagent such as toluene, potassium dichromate, can cause secondary pollution to environment.(2) prepare gained nano titanium oxide/NACF-
No any adhesive between nano titanium oxide and carrier in silicon dioxide, conjugation is poor.(3) this process conditions is more severe
Carve, need control accurate pH, material need to be calcined under nitrogen protection and obtain.Patent CN 102658115 A reports one kind for sky
The preparation method mixing cerium nano titanium oxide/NACF composite photo-catalyst that gas purifies, by by nano titanium oxide
It is added in cerous nitrate solution with NACF, high temperature hydro-thermal (200-220 DEG C) mixes cerium two in NACF surface deposition
Titanium oxide, in this technique, hydrothermal temperature is too high, has potential safety hazard, and mixes no any glue between cerium titanium dioxide and NACF
Glutinous agent so that most mix cerium nano titanium oxide not depend on active carbon fiber felt growth but reunite in fiber crossovers institute
In the duct being formed, reduce the absorption property of active carbon fiber felt itself and granule is easy to fall off, secondary pollution can be caused.
Accordingly, it would be desirable to be improved to prior art, obtain a kind of composite with high absorption and photocatalysis performance.
Content of the invention
The present invention is intended to provide a kind of height absorption-photocatalysis performance nano titanium oxide/active carbon fiber felt is three-dimensional porous
Material.
Present invention also offers the preparation method of above-mentioned material.
Technical scheme is, a kind of height absorption-photocatalysis performance nano titanium oxide/three-dimensional porous material of active carbon fiber felt
Material, with active carbon fiber felt as base material, and nano titanium oxide is attached in active carbon fiber felt；It is many that this material has three-dimensional
Pore structure, aperture is 1～100 μm；Specific surface area is 200～3000m2/g；Nano titanium oxide particle diameter is 50nm～1 μm.
It is the zinc oxide crystal layer of 500nm～1 μm in described active carbon fiber felt surface deposit thickness, nano titanium oxide is attached
On zinc oxide crystal layer surface, and nano titanium oxide is mainly anatase.
Preferably, aperture is mainly distributed as 20～70 μm, more preferably 30～50 μm.
Preferably, nano titanium oxide particle diameter is 500nm～1 μm.
The preparation method of above-mentioned composite includes：
(1) by the active carbon fiber felt immersion zinc oxide crystal layer solution of activating pretreatment, using Best-Effort request method, obtain
Obtain the active carbon fiber felt of surface depositing zinc oxide crystal layer；
Described Best-Effort request method is：A the active carbon fiber felt of activating pretreatment is immersed in zinc oxide crystal layer solution by (),
Dipping 2～10min, then with the slowly lifting taking-up upwards of the speed of 1～5mm/s；Products therefrom is dry under the conditions of 30～80 DEG C
Dry 20min～1hr；B () repeats above-mentioned Best-Effort request and dry run 1～8 time；C () is by the active carbon fiber felt dried in 60
After drying 0.5～6hr at～180 DEG C；Obtain the active carbon fiber felt of surface depositing zinc oxide crystal layer；
Described zinc oxide crystal layer solution compound method comprises the following steps：Soluble zinc salt is dissolved in alcohol；Then plus
Enter triethylamine, under the conditions of 30～100 DEG C, stir 10min～1hr, and be aged 1～5hr in room temperature condition, obtain zinc oxide brilliant
Layer solution；
Wherein zinc ion content is 0.02～0.3mol/L, and zinc ion and triethylamine mol ratio are 1：0.2～3；Preferably,
Zinc ion content is 0.04～0.25mol/L, and zinc ion and triethylamine mol ratio are 1：0.4～2.5；
Described soluble zinc salt is two acetate hydrate zinc or zinc nitrate hexahydrate；Described alcohol be selected from methanol, ethanol, third
Alcohol, n-butyl alcohol, isobutanol or the tert-butyl alcohol.
(2) the active carbon fiber felt immersion nano titanium oxide life of the surface depositing zinc oxide crystal layer prepared by step (1)
In long liquid, hydro-thermal reaction 2～24hr at 100～200 DEG C；
Described nano titanium oxide growth-promoting media contains 0.05～0.25mol/L TiO 2 precursor, 0.3～1mol/L
Sulphuric acid and 0.5～5mol/L hydrochloric acid；TiO 2 precursor is 1 with the mol ratio of sulphuric acid:1～8, the mol ratio of sulphuric acid and hydrochloric acid
For 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 TiO 2 precursor is 1 with the mol ratio of sulphuric acid:6～8, the mol ratio of sulphuric acid and hydrochloric acid
For 1：0.5～6.
In step (1), the specific surface area 200～3000m of described active carbon fiber felt2/ g, thickness is 1～20mm.Described
The preprocess method of active carbon fiber felt be that active carbon fiber felt is cut into required form, be then placed on containing surface
Activating agent, acid, in the pretreatment fluid of alkaline matter, stir 1～2h under the conditions of 50～120 DEG C, respectively through deionized water and second
After alcohol cleaning, it is dried under the conditions of 30～80 DEG C；In described pretreatment fluid, surfactant concentration be 1～10mmol/L,
The concentration of acid is 1～10mmol/L, and the concentration of alkaline matter is 100～500mmol/L.Described surfactant is selected from
Triton-X100, beta-schardinger dextrin-or cetyl trimethylammonium bromide；Described acid is monohydrate potassium, glycine or Borax；
Described alkaline matter is sodium hydroxide, potassium hydroxide or sodium citrate.
The present invention, with weaving material active carbon fiber felt (ACFF) as substrate, prepares nanometer titanium dioxide by hydro-thermal method
Titanium/active carbon fiber felt three-dimensional porous material.First pass through dip-coating method and deposit one layer of oxidation on active carbon fiber felt surface
Zinc crystal layer, this zinc oxide crystal layer serves as the adhesive between nano titanium oxide and active carbon fiber felt, effectively prevent existing
In technology, the caducous problem of active carbon fiber felt surfacing.The thickness of zinc oxide crystal layer is 500nm～1 μm, if crystal layer is thick
Degree exceedes this scope, and the micro-sphere structure of active carbon fiber felt surface nano-titanium dioxide particle packing is destroyed, direct shadow
Ring the Photocatalytic Degradation Property of composite.Then pass through hydro-thermal method, by the active carbon fiber felt immersion of load zinc oxide crystal layer
In the precursor solution of titanium dioxide, grow anatase nano titanium oxide in zinc oxide crystal layer surface in situ.
The nano titanium oxide being obtained depends on active carbon fiber felt growth, will not block the duct of carbon fiber felt itself.
It is big that composite has three-dimensional porous structure, specific surface area；Conjugation between material and active carbon fiber felt high and absorption-
Stronger activity is shown, after 1.5h, adsorption rate is up to after 95%, 35h to high concentration toluene in Photocatalytic Degradation of Toluene experiment
Degradation rate be up to 80%.Prepare the raw material that this composite used and be common analytical pure reagent, safety and will not be to ring
Secondary pollution is caused in border.
The beneficial effects of the present invention is：
(1) nano titanium oxide/active carbon fiber felt three-dimensional porous material of present invention preparation, with activity cheap and easy to get
Carbon fibe felt is substrate, deposits, on its surface, the zinc oxide crystal layer that a layer thickness is 500nm～1 μm by dip-coating method；Profit
Serve as the adhesive between nano titanium oxide and active carbon fiber felt with this crystal layer, effectively prevent active carbon fiber felt surface
Material falls back, then immerses the active carbon fiber felt of load zinc oxide crystal layer in the precursor liquid of nano titanium oxide, passes through
Hydro-thermal method grows anatase-phase nano titanium dioxide in zinc oxide crystal layer surface in situ, prepares gained nano titanium oxide and depends on work
Property Carbon fibe growth, the duct of active carbon fiber felt itself will not be blocked.Method safety, simple to operation, economical and to environment
Friendly.
(2) nano titanium oxide/active carbon fiber felt three-dimensional porous material of present invention preparation, has larger specific surface
Long-pending, and the nano titanium oxide of active carbon fiber felt substrate surface be particle diameter between 50nm to 1 μm of microsphere, there is porous knot
Structure.This microspheric superstructure can provide more avtive spots in Photocatalytic Degradation Process.There is the work of stronger absorption property
Property Carbon fibe felt is mutually collaborative with the nanometer titanium dioxide micro-sphere of superstructure, substantially increases photocatalysis efficiency.
(3) nano titanium oxide/active carbon fiber felt three-dimensional porous material of present invention preparation, has suitable mechanicalness
Can there are stronger absorption property, higher photocatalysis performance and excellent filter effect, process with good processability
During volatile organic gas, secondary pollution is not resulted in environment, be easy to it and be fully utilized in photocatalysis field, net in air
Change field has broad application prospects.
Brief description
Fig. 1 be embodiment 1 preparation nano titanium oxide/active carbon fiber felt three-dimensional porous material SEM image, a, b,
C is the zinc oxide crystal layer/active carbon fiber felt of different multiples.
SEM photograph, d, e, f are the SEM photograph of the nano titanium oxide/active carbon fiber felt of different multiples.
The graph of pore diameter distribution of the active carbon fiber felt that Fig. 2 is used by embodiment 1.
Fig. 3 is the pore-size distribution of the nano titanium oxide/active carbon fiber felt three-dimensional porous material prepared by embodiment 1
Figure.
Fig. 4 is the nano titanium oxide/active carbon fiber felt three-dimensional porous material nano surface titanium dioxide of embodiment 1 preparation
The TEM photo of titanium, wherein a, b are high low power TEM photo, and c is electronic diffraction ring piece.
Fig. 5 is the XRD spectrum of the nano titanium oxide/active carbon fiber felt three-dimensional porous material of embodiment 1 preparation, and a is
The XRD spectra of active carbon fiber felt, b is the XRD spectra of nano titanium oxide/active carbon fiber felt.
Fig. 6 is that the nano titanium oxide/active carbon fiber felt three-dimensional porous material absorption variable concentrations of embodiment 1 preparation are waved
Toluene adsorption curve after the property sent out organic gas toluene experiment, the consumption of curve (a) toluene is 2 μ L, and concentration is 1734mg/m3
(460ppm)；The consumption of curve (b) toluene is 3.5 μ L, and concentration is 3305mg/m3(877ppm)；The consumption of curve (c) toluene is
5 μ L, concentration is 4335mg/m3(1150ppm).
Fig. 7 is that the nano titanium oxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation of embodiment 1 preparation is different
CO after intensity volatile organic gas toluene experiment2Generating rate curve, the consumption of curve (a) toluene is 2 μ L, and concentration is
1734mg/m3(460ppm)；The consumption of curve (b) toluene is 3.5 μ L, and concentration is 3305mg/m3(877ppm)；Curve (c) toluene
Consumption be 5 μ L, concentration be 4335mg/m3(1150ppm).
Fig. 8 is that the nano titanium oxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation of embodiment 1 preparation is different
CO generating rate curve after intensity volatile organic gas toluene experiment, the consumption of curve (a) toluene is 2 μ L, and concentration is
1734mg/m3(460ppm)；The consumption of curve (b) toluene is 3.5 μ L, and concentration is 3305mg/m3(877ppm)；Curve (c) toluene
Consumption be 5 μ L, concentration be 4335mg/m3(1150ppm).
Fig. 9 is that the nano titanium oxide/active carbon fiber felt three-dimensional porous material photocatalytic degradation of embodiment 1 preparation is different
Degradation rate curve after intensity volatile organic gas toluene experiment.The consumption of curve (a) toluene is 2 μ L, and concentration is 1734mg/
m3(460ppm)；The consumption of curve (b) toluene is 3.5 μ L, and concentration is 3305mg/m3(877ppm)；The consumption of curve (c) toluene
For 5 μ L, concentration is 4335mg/m3(1150ppm).
Instantiation mode
Below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1
(1) accurately weigh 1.10g bis- acetate hydrate zinc (5mmol) to be added in 50mL (0.65mol) isopropanol (AR),
Stir 15min under the conditions of 85 DEG C, be subsequently adding 0.7mL (5mmol) triethylamine (AR), under the conditions of 85 DEG C, stir 5min, and in
It is aged 3h under room temperature condition, obtain final product 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, put
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 ethanol purge, under the conditions of 60 DEG C, 1hr is dried.
(3) by step (2) pretreatment and in the zinc oxide crystal layer solution of active carbon fiber felt immersion step (1) of drying,
Dipping 5min, then vertically lifts active carbon fiber felt upwards with the speed of 1mm/s, and 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
After drying 1h, you can 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 sulphuric acid (AR) is mixed with 10mL redistilled water, stirs 30min under room temperature condition, is then aged 1h, that is,
Obtain nano titanium oxide growth-promoting media.
(5) add the nano titanium oxide growth-promoting media of 10mL in water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
In dimension felt immersion growth-promoting media, water heating kettle is sealed, hydro-thermal 4h under the conditions of 180 DEG C, treat that water heating kettle is cooled to room temperature, take out and produce
Thing, is rinsed 2～5 times with ethanol and redistilled water, obtains final product nano titanium oxide/active carbon fiber felt three-dimensional porous material.
Active carbon fiber felt to the load zinc oxide crystal layer of embodiment 1 gained and nano titanium oxide/active carbon fibre
The pattern of dimension felt three-dimensional porous material is mutually characterized with thing, gained scanning electron microscope image (SEM), pore-size distribution collection of illustrative plates, transmission
Sem image (TEM) and Radix Rumiciss x ray diffraction collection of illustrative plates (XRD) are respectively as shown in Fig. 1,2,3,4,5.
From the SEM picture of Fig. 1 (a, d), the material preparing gained has three-dimensional porous structure, and wherein a figure is blank
The low power microscope photo of active carbon fiber felt, d figure is the low power of nano titanium oxide/active carbon fiber felt three-dimensional porous material
Microphotograph.From the SEM picture of Fig. 1 (b, c), active carbon fiber felt (ACFF) surface deposited one layer of fine and close oxidation
Zinc crystal layer (thickness 500nm～1 μm), and this crystal layer by nano-particle pile up form.From the SEM of Fig. 1 (e, f), after hydro-thermal
Grow some spherical nano-particle in zinc oxide crystal layer surface in situ, diameter is about 900nm, through XRD spectra (Fig. 2) card
Bright, this spherical nanoparticle is the nano titanium oxide of Anatase.TEM photo (a) of Fig. 4 proves NACF further
The titanium dioxide on felt surface be micro-sphere structure, electronic diffraction ring piece (c) show this microsphere be polycrystalline structure, if illustrate it be by
Dry titanium dioxide nanoparticle is piled up and is formed, and some irregular stacking holes in microsphere inner dispersion.SEM picture (e, f)
Display titanium dioxide nanoparticle is grown on active carbon fiber felt surface, rather than reunites in the duct of fiber felt, does not affect
The absorption property of active carbon fiber felt.And, compared with the Titanium dioxide/active carbon fiber felt obtaining with prior art mixing method,
The nano titanium oxide that embodiment 1 is obtained/active carbon fiber felt three-dimensional porous material through touch after, the titanium dioxide of attachment
Nano-particle is not allowed easy to fall off.Fig. 2,3 respectively blank active carbon fiber felts and nano titanium oxide/active carbon fiber felt three
The graph of pore diameter distribution of dimension porous material, the graph of pore diameter distribution spectrum of Fig. 2 shows that active carbon fiber felt has loose structure, and aperture is main
It is distributed in 25～40 μm；The graph of pore diameter distribution spectrum of Fig. 3 shows, after its area load nano titanium oxide, active carbon fiber felt
The three-dimensional porous structure of itself is not destroyed, with the attachment of material, aperture increases, is mainly distributed on 35～50 μm.Three
The specific surface area about 1100m of dimension porous material2/g.
The low power TEM photo of Fig. 4 three-dimensional porous material surface nano-titanium dioxide and electronic diffraction ring piece show,
The porous microsphere structure that the epontic titanium dioxide of active carbon fiber felt is piled up for nano-particle.
Embodiment 2
Nano titanium oxide to embodiment 1 gained/active carbon fiber felt three-dimensional porous material carries out the organic gas of volatility
The absorption of body toluene and photocatalytic degradation experiment：
(1) take 4 nano titanium oxides/active carbon fiber felt three-dimensional porous material (quality about 0.2g), be placed in retort
Bottom.Then, it is injected separately into 2 μ L, 3.5 μ L, 5 μ L toluene in retort with microsyringe.Carry out under room temperature no light condition
Half-light adsorbs 1.5h, and every 1min gathers a gaseous sample, carries out online content with INNOVA-1412i infrared photo acoustic chromatograph
Analysis.
(2), after adsorption equilibrium, open ultraviolet source (high voltage mercury lamp, 32W) and carry out photocatalytic degradation experiment, illumination 35h, often
1min gathers a gaseous sample, carries out content analysis by INNOVA-1412i infrared photo acoustic chromatograph.Dense according to toluene
Degree change and CO2, the generating rate of CO, compare nano titanium oxide under variable concentrations gradient/active carbon fiber felt three-dimensional many
The adsorption-photocatalytic degradation activity of Porous materials.
Absorption to above-mentioned volatile organic gas toluene-photocatalysis experiment the data obtained has carried out drawing and has analyzed, no
With concentration toluene adsorption curve as shown in fig. 6, CO during variable concentrations Photocatalytic Degradation of Toluene2, CO generating rate curve
As shown in Figure 7,8.Test result indicate that, the nano titanium oxide/first to variable concentrations for the active carbon fiber felt three-dimensional porous material
Benzene all shows stronger absorption property, adsorption efficiency up to 95%～98% within 1.5h.To degraded variable concentrations toluene
During CO2, the generating rate curve of CO carry out linear fit, fitting result shows, three-dimensional porous material in 500min after turning on light
Material is very fast to the degradation rate of toluene, can attribution be absorption and light-catalysed mutual synergism；After 500min, CO, CO2Life
Become and keep good linear relationship between speed and the concentration of toluene, illustrate that nano titanium oxide/active carbon fiber felt is three-dimensional many
Porous materials stability in whole Photocatalytic Degradation Process is stronger.Contrast CO and CO2Growing amount, due to whole photocatalytic degradation
During CO growing amount less than CO2During the 1% of growing amount, therefore Photocatalytic Degradation of Toluene, CO is negligible.
The degradation rate curve of variable concentrations toluene is as shown in Figure 9.Concentration with toluene increases, toluene in same time
Degradation rate is respectively 81.5%, 61.6%, 57.0%, and nano titanium oxide/active carbon fiber felt three-dimensional porous material pair is described
Degraded in high concentration toluene still remains preferable Photocatalytic Degradation Property, and this experimental result is that the reality of composite should
With providing strong theoretical foundation.
Embodiment 3
(1) accurately weigh 1.10g bis- acetate hydrate zinc (5mmol) to be added in 100mL (1.31mol) isopropanol (AR),
Stir 15min under the conditions of 85 DEG C, be subsequently adding 1.4mL (10mmol) triethylamine (AR), under the conditions of 85 DEG C, stir 5min, and
It is aged 3h under room temperature condition, obtain final product 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 dried after process, with embodiment 1 step (2).
(3) by step (2) pretreatment and in the zinc oxide crystal layer solution of active carbon fiber felt immersion step (1) of drying,
Dipping 2min, then vertically lifts active carbon fiber felt upwards with the speed of 5mm/s, and products therefrom is dried under the conditions of 80 DEG C
1h, then repeats above-mentioned Best-Effort request process 8 times, the activated fibre substrate of drying is again placed in baking oven, does again for 180 DEG C
Dry, 4h is dried, you can in active carbon fiber felt surface depositing zinc oxide crystal layer.
(4) with embodiment 1 step (4).
(5) with embodiment 1 step (5).
Obtained three-dimensional porous material electron microscope, XRD spectra result is with embodiment 1, and has good light to toluene
Catalytic degradation performance.
Embodiment 4
(1) (2) are with embodiment 1 step (1) (2).
(3) by pretreatment and dry active carbon fiber felt immersion zinc oxide crystal layer solution, impregnate 20min, so
Afterwards active carbon fiber felt is vertically lifted upwards with the speed of 5mm/s, products therefrom dries 1h under the conditions of 30 DEG C, then repeat on
State Best-Effort request process 5 times, the activated fibre substrate of drying is again placed in baking oven, 180 DEG C of after drying, 1h is dried, that is,
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 sulphuric acid (AR) is mixed with 10mL redistilled water, stirs 1h, be then aged 3h, obtain final product and receive under room temperature condition
Rice titania growth liquid.
(5) add the nano titanium oxide growth-promoting media of 10mL in water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
In dimension felt immersion growth-promoting media, water heating kettle is sealed, hydro-thermal 24h under the conditions of 100 DEG C, treat that water heating kettle is cooled to room temperature, take out and produce
Thing, is rinsed for several times with ethanol and redistilled water, obtains final product nano titanium oxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result is with embodiment 1, and has good light to toluene
Catalytic degradation performance.
Embodiment 5
(1) with embodiment 3 step (1).
(2) active carbon fiber felt is cut into 2cm*2cm*1mm (thickness：1mm, specific surface area 1100m2/ g) bulk, in advance
It is dried after process, with embodiment 1 step (2).
(3) by pretreatment and dry active carbon fiber felt immersion zinc oxide crystal layer solution, impregnate 10min, so
Afterwards active carbon fiber felt is vertically lifted upwards with the speed of 1mm/s, products therefrom dries 1h under the conditions of 80 DEG C, then repeat on
State Best-Effort request process 5 times, the activated fibre substrate dried is dried under the conditions of 30 DEG C, drying 4h, you can in active carbon fibre
Dimension felt surface depositing zinc oxide crystal layer.
(4) with embodiment 4 step (4).
(5) add the nano titanium oxide growth-promoting media of 10mL in water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
In dimension felt immersion growth-promoting media, water heating kettle is sealed, hydro-thermal 14h under the conditions of 180 DEG C, treat that water heating kettle is cooled to room temperature, take out and produce
Thing, is rinsed for several times with ethanol and redistilled water, obtains final product nano titanium oxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result is with embodiment 1, and has good light to toluene
Catalytic degradation performance.
Embodiment 6
(1) accurately weigh 1.10g bis- acetate hydrate zinc (5mmol) to be added in 25mL (0.33mol) isopropanol (AR),
Stir 1h under the conditions of 30 DEG C, be subsequently adding 0.35mL (2.5mmol) triethylamine (AR), under the conditions of 30 DEG C, stir 1h, and in room
It is aged 5h under the conditions of temperature, obtain final product zinc oxide crystal layer solution.
(2) with embodiment 5 step (2).
(3) by the active carbon fiber felt being dried immersion zinc oxide crystal layer solution, impregnate 10min, then with the speed of 2mm/s
Degree vertically lifts active carbon fiber felt upwards, and products therefrom is dried 1h under the conditions of 30 DEG C, then repeated above-mentioned Best-Effort request mistake
Journey 5 times, the activated fibre substrate dried is dried under the conditions of 60 DEG C, dries 4h, you can in active carbon fiber felt surface deposition
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 sulphuric acid (AR) is mixed with 10mL redistilled water, stirs 1h, be then aged 3h under room temperature condition,
Obtain final product nano titanium oxide growth-promoting media.
(5) add the nano titanium oxide growth-promoting media of 10mL in water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
In dimension felt immersion growth-promoting media, water heating kettle is sealed, hydro-thermal 2h under the conditions of 200 DEG C, treat that water heating kettle is cooled to room temperature, take out and produce
Thing, is rinsed for several times with ethanol and redistilled water, obtains final product nano titanium oxide/active carbon fiber felt three-dimensional porous material.
Obtained three-dimensional porous material electron microscope, XRD spectra result is with embodiment 1, and has good light to toluene
Catalytic degradation performance.
Embodiment 7
(1)～(3) are with embodiment 6 step (1)～(3).
(4) by pretreatment and dry active carbon fiber felt immersion zinc oxide crystal layer solution, impregnate 5min, then
Active carbon fiber felt is vertically lifted upwards with the speed of 2mm/s, products therefrom is dried 30min under the conditions of 60 DEG C, then repeated
Above-mentioned Best-Effort request process 4 times, the activated fibre substrate dried is dried under the conditions of 100 DEG C, drying 2h, you can in activated carbon
Fiber felt surface depositing zinc oxide crystal layer.
(4) with embodiment 5 step (4).
(5) add the nano titanium oxide growth-promoting media of 10mL in water heating kettle, by the active carbon fibre of depositing zinc oxide crystal layer
In dimension felt immersion growth-promoting media, water heating kettle is sealed, hydro-thermal 14h under the conditions of 150 DEG C, treat that water heating kettle is cooled to room temperature, take out and produce
Thing, is rinsed for several times with ethanol and redistilled water, obtains final product nano titanium oxide/active carbon fiber felt three-dimensional porous material.
Nano titanium oxide obtained by embodiment 3～7/active carbon fiber felt three-dimensional porous material, its electron microscope, XRD
Spectrogram result is with embodiment 1, and has good Photocatalytic Degradation Property to toluene, and titanium dioxide nanoparticle is not easy
Come off.
Above-described embodiment is the present invention preferably embodiment, but protection scope of the present invention is not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine, simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.The term occurring in the present invention is used for this
The elaboration of inventive technique scheme and understanding, are not construed as limiting the invention.
Claims (9)
1. a kind of three-dimensional porous composite of nano titanium oxide/active carbon fiber felt of high absorption-photocatalysis performance, its feature
It is, with active carbon fiber felt as base material, and nano titanium oxide is attached in active carbon fiber felt；
Described composite has three-dimensional porous structure, and aperture is 1～100 μm；Specific surface area is 200～3000m2/g；
Described nano titanium oxide particle diameter is 50nm～1 μm.
2. the three-dimensional porous composite wood of nano titanium oxide/active carbon fiber felt of high absorption-photocatalysis performance described in claim 1
Expect it is characterised in that being the zinc oxide crystal layer of 500nm～1 μm in described active carbon fiber felt surface deposit thickness, nano-silica
Change titanium and be attached to zinc oxide crystal layer surface, and described nano titanium oxide is mainly anatase.
3. the three-dimensional porous composite wood of nano titanium oxide/active carbon fiber felt of high absorption-photocatalysis performance described in claim 1
Material is it is characterised in that described nano titanium oxide particle diameter is 500nm～1 μm.
4. described in any one of claims 1 to 3, the nano titanium oxide/active carbon fiber felt of high absorption-photocatalysis performance is three-dimensional
The preparation method of porous material is it is characterised in that step includes：
(1) by the active carbon fiber felt immersion zinc oxide crystal layer solution of activating pretreatment, using Best-Effort request method, obtain table
The active carbon fiber felt of face depositing zinc oxide crystal layer；
Described zinc oxide crystal layer solution is the alcoholic solution containing soluble zinc salt, triethylamine；Wherein zinc ion content is 0.02
～0.3mol/L, zinc ion is 1 with the mol ratio of triethylamine：0.2～3；
(2) the active carbon fiber felt immersion nano titanium oxide growth-promoting media of the surface depositing zinc oxide crystal layer prepared by step (1)
In, hydro-thermal reaction 2～24hr at 100～200 DEG C, washing is dried to obtain high absorption-photocatalysis performance nano titanium oxide/activity
Carbon fibe felt three-dimensional porous material；
In described nano titanium oxide growth-promoting media, TiO 2 precursor content is 0.05～0.25mol/L, also contains 0.3
～1mol/L sulphuric acid and 0.5～5mol/L hydrochloric acid；TiO 2 precursor is 1 with the mol ratio of sulphuric acid:1～8, sulphuric acid and hydrochloric acid
Mol ratio be 1：0.2～8；
Described TiO 2 precursor is butyl titanate, isopropyl titanate or titanium tetrachloride.
5. the three-dimensional porous material of nano titanium oxide/active carbon fiber felt of high absorption-photocatalysis performance according to claim 4
The preparation method of material is it is characterised in that in step (1) described zinc oxide crystal layer solution；Soluble zinc salt is two acetate hydrate zinc
Or zinc nitrate hexahydrate；Described alcohol is selected from methanol, ethanol, propanol, n-butyl alcohol, isobutanol or the tert-butyl alcohol；Wherein zinc ion contains
Measure as 0.04～0.25mol/L, zinc ion is 1 with the mol ratio of triethylamine：0.4～2.5.
6. nano titanium oxide/the active carbon fiber felt of a kind of high absorption-photocatalysis performance according to claim 4 or 5
The preparation method of three-dimensional porous material is it is characterised in that described zinc oxide crystal layer solution compound method comprises the following steps：Will
Soluble zinc salt is dissolved in alcohol；It is subsequently adding triethylamine, under the conditions of 30～100 DEG C, stir 10min～1hr, and in 10～40
DEG C ageing 1～5hr, obtain zinc oxide crystal layer solution.
7. a kind of nano titanium oxide of high absorption-photocatalysis performance according to claim 4/active carbon fiber felt is three-dimensional
Porous material and preparation method thereof it is characterised in that in nano titanium oxide growth-promoting media described in step (2), before titanium dioxide
Drive body burden 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
Titanium precursors are 1 with the mol ratio of sulphuric acid:6～8, sulphuric acid is 1 with the mol ratio of hydrochloric acid：0.5～6.
8. a kind of nano titanium oxide of high absorption-photocatalysis performance according to claim 4/active carbon fiber felt is three-dimensional
Porous material and preparation method thereof is it is characterised in that the specific surface area 200～3000m of the described active carbon fiber felt of step (1)2/
G, the preprocess method of described active carbon fiber felt is active carbon fiber felt to be cut into required form, is then placed on and contains
Have in the pretreatment fluid of Triton-X100, citric acid and sodium hydroxide, stir 1～2h under the conditions of 50～120 DEG C, respectively
After deionized water and ethanol purge, it is dried under the conditions of 30～80 DEG C；
In described 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.
9. a kind of nano titanium oxide of high absorption-photocatalysis performance according to claim 4/active carbon fiber felt is three-dimensional
Porous material and preparation method thereof it is characterised in that in step (1) Best-Effort request method be：
A (), by the active carbon fiber felt of activating pretreatment immersion zinc oxide crystal layer solution, impregnates 2～10min, then with 1～
The slowly lifting taking-up upwards of the speed of 5mm/s, products therefrom is dried 20min～1hr under the conditions of 30～80 DEG C；
B () repeats above-mentioned Best-Effort request and dry run 1～8 time；
(c) after drying 0.5～6hr at 60～180 DEG C by the active carbon fiber felt dried.
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