CN101053845A - Sol-gel method preparing active carbon-titanium dioxide composite photocatalyst method and application of the said photocatalyst - Google Patents
Sol-gel method preparing active carbon-titanium dioxide composite photocatalyst method and application of the said photocatalyst Download PDFInfo
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Abstract
A process for preparing a composite photocatalyst of active carbon-titanium dioxide by a sol-gel method, and use of the composite photocatalyst are disclosed in the invention. The process includes: firstly mixing butyl titanate having a certain quantity with absolute ethyl alcohol in a condition of continuously agitating and continuously agitating for 15 minutes, adding in drops with catalyst formed by water, acetic acid and absolute ethyl alcohol which volume ratio is 4:5:10 under intense agitation to obtain TiO2 sol after continuous agitation; then in the sol generating process, adding active carbon according to weight ratio of butyl titanate and carbon as 0.1:1, after completely agitating, oscillating in ultrasonic wave and placing the sol in a hourglass type hopper to vacuumize and filter extra sol, after drying, heat treating to obtain the composite photocatalyst. The composite photocatalyst of active carbon-titanium dioxide prepared by the invention can be used for degrading formaldehyde, and a performance testing result shows that the composite photocatalyst can be cooperated for harmful gas for effectively degrading microscale formaldehyde in water, which effect is superior to that by only using one of the catalyst.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst and the application of this photochemical catalyst thereof.The particularly application of the method for sol-gel method preparing active carbon-titanium dioxide composite photocatalyst and this photochemical catalyst thereof.
Background technology
In recent years along with interior decoration heat has also been brought indoor air pollution, pernicious gas mainly is the methyl mercaptan that produces in formaldehyde of emitting such as ornament materials and the living environment, hydrogen sulfide, ammonia etc.These gases just can make the people produce sense of discomfort when a few millionths.Wherein, formaldehyde is the higher material of toxicity, preferentially controls on the list formaldehyde at China's toxic chemical and is in second.Formaldehyde is defined as carcinogenic and teratogenesis shape material by the World Health Organization, is the allergen of generally acknowledging, also is one of potential strong mutagen.Formaldehyde mainly shows aspects such as allotriosmia, stimulation, allergy, abnormal pulmonary function, dysfunction of liver and immunologic dysfunction to health effects.Its concentration reaches 0.06-0.07mg/m in every cubic metres of air
3The time, slight asthma will take place in children.When formaldehyde in indoor air content is 0.1mg/m
3The time, peculiar smell and sense of discomfort are just arranged; Reach 0.5mg/m
3The time, can stimulate eyes, cause and shed tears; Reach 0.6mg/m
3, can cause throat discomfort or pain.When concentration is higher, the vomiting that can cause nausea, it is uncomfortable in chest to cough, asthma even pulmonary edema; Reach 30mg/m
3The time, meeting is the causing death immediately.
Show according to related data statistics: the mankind have 70% illness relevant with indoor environment, and China has 120,000 people to die from indoor pollution every year, and the child leukaemic more than 90% lives in new clothes and repairs the house ill in 1 year.Pernicious gases such as therefore effective degradation treatment formaldehyde, it is very important improving indoor environment, the pollution problem of PARA FORMALDEHYDE PRILLS(91,95) waste water simultaneously also can not be ignored.
In the existing method of administering formaldehyde, absorption method by force, can not cause advantage extensive uses such as secondary pollution because of its efficient height, enrichment function.Active carbon has big specific area and fast adsorption desorption speed, is a kind of superior adsorbent of administering formaldehyde.But active carbon reaches capacity after the absorption as a kind of adsorbent, must regeneration just can recover adsorption capacity.Photocatalytic degradation is a science and technology in the ascendant.In currently used photochemical catalyst, TiO
2With its active height, Heat stability is good, low price, characteristic such as harmless extremely people favor but simple TiO
2Photochemical catalyst exists as shortcomings such as recovery difficulties.If with active carbon and photocatalyst TiO
2Combine and administer the formaldehyde pollution, then advantage is more obvious.On the one hand, TiO
2Photocatalytic degradation is regenerated active carbon by the formaldehyde of charcoal absorption; On the other hand, the strong suction-operated of active carbon is TiO
2Photocatalysis the reaction environment of high concentration is provided, accelerated reaction rate.And, because catabolite is carbon dioxide and water directly, avoided the process that the formaldehyde of absorption is handled once more.But there is not well to prepare the method for active carbon-titanium dioxide composite photocatalyst at present.
Summary of the invention
The objective of the invention is in administering the formaldehyde pollution, be difficult to recover adsorption capacity and singly use TiO with active carbon in order to solve list
2The problem of photochemical catalyst recovery difficulty etc. provides a kind of method and the application of this composite photo-catalyst aspect the pollution of improvement formaldehyde thereof of sol-gel method preparing active carbon-titanium dioxide composite photocatalyst composite catalyst.Adopt the active carbon-titanium dioxide composite photocatalyst of preparation method's preparation of the present invention to have synergy: TiO
2Photocatalytic degradation is regenerated active carbon by the formaldehyde of charcoal absorption; The strong suction-operated of active carbon is TiO
2Photocatalysis the reaction environment of high concentration is provided, accelerated reaction rate; And, because catabolite is carbon dioxide and water directly, avoided the process that the formaldehyde of absorption is handled once more.And use it for the degraded of formaldehyde in the water, and the result shows that the active carbon-titanium dioxide composite photocatalyst that makes with said method can act synergistically on pernicious gas, the effective formaldehyde of trace in the degradation water, and effect is better than singly using one.
Purpose of the present invention can be achieved through the following technical solutions:
The method of sol-gel method preparing active carbon-titanium dioxide composite photocatalyst comprises the steps:
1, preparation nano titanium oxide
A certain amount of butyl titanate is mixed with absolute ethyl alcohol under constantly stirring and continue stirring after 15 minutes, under stirring, brute force drips the catalyst that water, acetate and absolute ethyl alcohol are made into, water wherein: acetate: the volume ratio of absolute ethyl alcohol is 4: 5: 10, obtains TiO after continuing to stir
2Colloidal sol;
2, preparation composite photo-catalyst
Press butyl titanate and 0.1: 1 amount of charcoal mass ratio and add active carbon in the colloidal sol forming process, after fully stirring, vibrate in ultrasonic wave, put into the sand mold funnel then and vacuumize and leach unnecessary colloidal sol, after the oven dry, heat treatment promptly gets composite photo-catalyst.
The active carbon-titanium dioxide composite photocatalyst of the present invention preparation can be used for degradation of formaldehyde.
The method of sol-gel method preparing active carbon-titanium dioxide composite photocatalyst composite catalyst of the present invention, simple possible, cost is low, the active carbon-titanium dioxide composite catalyst of its preparation, the result of transmission electron microscope shows the TiO as the composite catalyst main body
2Particle diameter is at nanoscale, and anatomical lens can find out that titanium dioxide is really attached to the surface of active carbon down.The performance test results shows this composite photocatalyst trace formaldehyde in the degradation water effectively.In the same way, this active carbon-titanium dioxide composite photocatalyst also can be applied to the removal of formaldehyde gas in the air, for the removal of pernicious gases such as formaldehyde provides a kind of new selection.
Description of drawings
The present invention is further described below in conjunction with the drawings and specific embodiments.
Fig. 1 TiO of the present invention
2The transmitted electron collection of illustrative plates of nano particle.
The surface topography map of Fig. 2 active carbon of the present invention.
Fig. 3 active carbon/TiO of the present invention
2Surface topography map.
Fig. 4 formaldehyde absorbance of the present invention and concentration curve.
The specific embodiment
The following examples only are used for further explaining the present invention, rather than limitation of the scope of the invention.
Embodiment 1:
The method of sol-gel method preparing active carbon-titanium dioxide composite photocatalyst comprises the steps:
1, preparation nano titanium oxide
A certain amount of butyl titanate is mixed with absolute ethyl alcohol under constantly stirring, and the lasting 15min that stirs, under brute force stirs, drip the about 10mL of catalyst that water, acetate and absolute ethyl alcohol are made into volume ratio at 4: 5: 10 then, continue stirring and obtained TiO in 6～8 hours
2Colloidal sol is standby.
2, preparation composite photo-catalyst
In the colloidal sol forming process, press butyl titanate and charcoal mass ratio and add active carbon at 0.1: 1, after fully stirring 1h, 1h vibrates in ultrasonic wave, putting into the sand mold funnel then vacuumizes and leaches unnecessary colloidal sol, 60 ℃ of about 15min of oven dry, repetitive coatings 3 times places 450 ℃ Muffle furnace heat treatment 2h promptly to get active carbon-titanium dioxide composite photocatalyst then.
Analysis and test
One, experimental technique
1, use transmission electron microscope and disecting microscope to sample analysis
The collosol and gel direct heat that takes a morsel is handled the TiO that obtains
2Nanometer powder, its transmitted spectrum was measured in ultrasonic dispersion in 15 minutes in ethanol solution.
Get clean active carbon and active carbon-titanium dioxide composite photocatalyst, place the optics that can amplify observation to dissect electron microscope and observe its surface topography down.
2, the drafting of formalin normal concentration curve
A peek 25mL tool plug graded tube adds 0.00,0.50,1.00,3.00,5.00 respectively, 8.00mL formaldehyde standard uses solution (every milliliter contains 10 microgram formaldehyde approximately), adds water to 25mL, adds 2.5mL acetylacetone,2,4-pentanedione solution, shakes up.In 45～60 ℃ of water-baths, heat 30min, take out cooling.Using the 1cm cuvette, is incident light with the light of wavelength 414nm, is the reference measurement absorbance with water, is respectively horizontal ordinate drawing standard curve with concentration and absorbance then.
3, the mensuration of concentration of formaldehyde in the sample
With active carbon-TiO
2Composite catalyst is put in the culture dish (Φ 90mm) that fills the certain density formalin of 25ml, apart from uviol lamp 12cm place.Uviol lamp power 30W utilizes the absorbance of formalin behind the spectrophotometric determination illumination 4h, finds the content of formaldehyde the sample from calibration curve.
Two, experimental result
1, TiO
2The TEM of nano particle characterizes
Fig. 1 is TiO
2The transmission electron microscope of nano particle (TEM) figure as shown in Figure 1, has made (Φ ≌ 90nm) spherical nanoparticles of size homogeneous by sol-gal process.According to method of the present invention with TiO
2After nano particle is assembled on the activated carbon surface, respectively gets 1 active carbon and active carbon-titanium dioxide composite and carry out the surface topography that 90 times of amplification observations obtain Fig. 2 and Fig. 3.As shown in Figure 3, TiO
2Distribution of particles on active carbon inside and hole surface, visible TiO
2Particle has been assembled on the active carbon, for the degraded of follow-up formaldehyde provides material base.
2, formaldehyde normal concentration curve map
It is that initial formaldehyde standard liquid is got respectively and is diluted to 25mL after a certain amount of that the formaldehyde standard is used solution, and the concentration of standard liquid is demarcated with the method in the water standard, and is as shown in table 1.
The relation of table 1 formaldehyde absorbance and concentration
| Concentration of formaldehyde (mL/25mL) | 0.5 | 1.0 | 3.0 | 5.0 | 8.0 |
| Absorbance (A) | 0.012 | 0.024 | 0.072 | 0.107 | 0.151 |
Its formaldehyde absorbance and concentration curve are as shown in Figure 4.
3, Degradation Formaldehyde rate
(1) degraded of different quality active carbon-titanium dioxide catalyst and active carbon PARA FORMALDEHYDE PRILLS(91,95) contrast
The active carbon-titanium dioxide catalyst of table 2 different quality and the degraded of active carbon PARA FORMALDEHYDE PRILLS(91,95) contrast
| Catalyst amount | 0.4g | 0.8g | 1.2g | 1.6g |
| Active carbon/TiO 2The PARA FORMALDEHYDE PRILLS(91,95) degradation rate | 19.4％ | 37.5％ | 56.9％ | 61.1％ |
| The adsorption rate of active carbon PARA FORMALDEHYDE PRILLS(91,95) | 6.94％ | 11.1％ | 20.83％ | 34.7％ |
Table 2 is degraded contrasts of the active carbon-titanium dioxide catalyst and the active carbon PARA FORMALDEHYDE PRILLS(91,95) of different quality, used formalin is to get 3mL formaldehyde standard to use liquid to be diluted to 25mL, the pH value coarse adjustment of solution is 11, as shown in table 2, the photocatalytic degradation rate of active carbon-titanium dioxide catalyst PARA FORMALDEHYDE PRILLS(91,95) is than the clearance height of independent active carbon PARA FORMALDEHYDE PRILLS(91,95), this is because when having only active carbon, what play a role only is its adsorption function, and when load on the active carbon during photochemical catalyst titanium dioxide, the formaldehyde that is adsorbed onto activated carbon surface can constantly be degraded under the irradiation of ultraviolet light, make the adsorption potential on the active carbon be available, can circulate plays a role.Simultaneously because the adsorption capacity of active carbon makes TiO
2Particle can big limit touch absorbate, thereby improved photocatalysis efficiency.
(2) degraded of different quality active carbon-titanium dioxide catalyst PARA FORMALDEHYDE PRILLS(91,95) solution
Table 3 is degradeds of different quality active carbon-titanium dioxide PARA FORMALDEHYDE PRILLS(91,95) solution, getting 3mL formaldehyde standard in the experiment uses liquid to be diluted to 25mL, the pH value coarse adjustment of solution is 11, measures after the absorbance and finds corresponding concentration from calibration curve, and then calculate the degradation rate of formaldehyde.
The degraded of table 3 different quality active carbon-titanium dioxide PARA FORMALDEHYDE PRILLS(91,95) solution
| Catalyst amount | 0.4g | 0.8g | 1.2g | 1.6g |
| Absorbance | 0.058 | 0.045 | 0.031 | 0.028 |
| The Degradation Formaldehyde rate | 19.4％ | 37.5％ | 56.9％ | 61.1％ |
As shown in table 3, the catalyst of different quality is different to the degradation rate of same concentrations formaldehyde, increase along with catalyst amount, the degradation rate of formaldehyde has obtained improving greatly, but from the amplitude that increases, it is many not as what increase under several situations in front that catalyst amount is increased to 1.6g Degradation Formaldehyde rate from 1.2g, and this ultraviolet ray that may be too much charcoal absorption makes the degradation rate decrease to some degree of titanium dioxide PARA FORMALDEHYDE PRILLS(91,95).Can draw also thus in actual applications that the applied amount of catalyst is not The more the better, should have the injected volume an of the best.
(3) equal in quality active carbon-titanium dioxide catalyst is to the degraded of variable concentrations formalin
Table 4 equal in quality active carbon-titanium dioxide catalyst is to the degraded of variable concentrations formalin
| Concentration of formaldehyde (mL/25mL) | 0.5 | 1.0 | 3.0 | 5.0 |
| Absorbance | 0.011 | 0.021 | 0.031 | 0.052 |
| The Degradation Formaldehyde rate | 8.3％ | 12.5％ | 56.9％ | 51.4％ |
The quality of catalyst system therefor is 1.2g in the present embodiment, and other condition is the same.As shown in table 4, along with the increase of concentration of formaldehyde, catalyst also increases its degradation rate, but degradation rate decreases on the contrary when concentration increases to a certain degree.Supposition may be because the catalytic performance of the catalyst of certain mass can't satisfy the needs of relatively large formaldehyde at short notice, should suitably increase catalyst consumption under the same conditions.
Claims (5)
1, the method for sol-gel method preparing active carbon-titanium dioxide composite photocatalyst is characterized in that, comprises the steps:
1), preparation nano titanium oxide
A certain amount of butyl titanate is mixed with absolute ethyl alcohol under constantly stirring and continue stirring after 15 minutes, under stirring, brute force drips the catalyst that water, acetate and absolute ethyl alcohol are made into, water wherein: acetate: the volume ratio of absolute ethyl alcohol is 4: 5: 10, obtains TiO after continuing to stir
2Colloidal sol;
2), preparation composite photo-catalyst
Press butyl titanate and 0.1: 1 amount of charcoal mass ratio and add active carbon in the colloidal sol forming process, after fully stirring, vibrate in ultrasonic wave, put into the sand mold funnel then and vacuumize and leach unnecessary colloidal sol, after the oven dry, heat treatment promptly gets composite photo-catalyst.
2, method according to claim 1 is characterized in that, the time of continuing to stir in step 1) is 6～8 hours.
3, method according to claim 1 is characterized in that, in step 2) in the oven dry temperature be 60 ℃, the time is 15 minutes.
4, method according to claim 1 is characterized in that, in step 2) in the temperature established of heat be 450 ℃, the time is 2 hours.
5, the active carbon-titanium dioxide composite photocatalyst of the method for the described sol-gel method preparing active carbon-titanium dioxide composite photocatalyst of a kind of claim 1 preparation can be used for degradation of formaldehyde.
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