CN114904503A - TiO 2 Preparation method, testing device and testing method of/ACF composite material - Google Patents
TiO 2 Preparation method, testing device and testing method of/ACF composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000012360 testing method Methods 0.000 title claims description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 168
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000002101 nanobubble Substances 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000001699 photocatalysis Effects 0.000 claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000002791 soaking Methods 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 10
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 239000007789 gas Substances 0.000 claims description 29
- 239000010453 quartz Substances 0.000 claims description 26
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
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- 238000001179 sorption measurement Methods 0.000 claims description 13
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
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- 238000006731 degradation reaction Methods 0.000 claims description 5
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- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 230000015556 catabolic process Effects 0.000 claims description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
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- 238000000696 nitrogen adsorption--desorption isotherm Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/007—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 irradiation
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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
- B01D53/34—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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- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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Abstract
The invention discloses a TiO2 2 The preparation method of the/ACF composite material comprises the following steps: (1) cleaning ACF cutting dust; (2) soaking in ammonia water solution and drying the water in the ACF; (3) soaking the ACF treated by the ammonia water in a nitric acid solution to press the water of the ACF to be dry as much as possible; (4) placing the treated ACF in a second containerSoaking in alcoholic solution for 25-35min and oven drying; (5) measuring absolute ethyl alcohol, and dripping tetrabutyl titanate to dissolve completely; (6) adding acetylacetone as a solution A, quickly and uniformly mixing absolute ethyl alcohol, micro/nano bubble water and acetic acid, and adjusting the pH =2.5 by using concentrated nitric acid to obtain a solution B; (7) dripping the B solution into the A solution, and activating the ACF after the dripping is finished; (8) putting the dried and dipped ACF into a tube furnace, and roasting under the protection of nitrogen to obtain TiO 2 the/ACF composite material. The TiO2/ACF composite photocatalytic material synthesized by the micro/nano bubble method has high removal efficiency on toluene.
Description
Technical Field
The present invention relates to TiO 2 A preparation method, a testing device and a testing method of an ACF composite material belong to the field of material chemistry.
Background
There are many processing techniques available on the market for the industrial removal of VOCs including adsorption, condensation, biodegradation, low temperature plasma, catalytic combustion, photocatalysis, etc. Wherein, the adsorption method is easy to operate and is popular in the market due to low price. The Active Carbon Fiber (ACF) can remove VOCs with medium and low concentration, is used as one of adsorbents, has larger adsorption capacity and faster adsorption kinetic performance compared with SiO2, molecular sieve, zeolite, granular active carbon and the like, and has larger specific surface area and surface adsorption reactivity. However, the activated carbon fibers after saturation adsorption can not purify the VOCs any more, and when the external environment changes, such as temperature rise or air pressure drop, the VOCs can be volatilized again to harm the environment and human health.
The photocatalysis method is used as a method for degrading VOCs safely and efficiently without secondary pollution. Titanium dioxide is one of the most environmentally-friendly photocatalysts with stable chemical properties, low cost and no toxicity, but because of TiO 2 The hole-photon-generated electron high recombination leads to the change of surface states such as low utilization rate of photon-generated carriers, low surface area VOCs intermediate growth, coke accumulation and the like, so that the photocatalytic activity of the material is gradually reduced, and even the catalyst is inactivated. The carbon material has excellent photoinduced electron transfer capability, and the graphite/TiO 2 The material can effectively improve the migration and separation of photo-generated charges and inhibit the recombination of the photo-generated charges and holes, thereby improving the photocatalytic efficiency. In addition, the following problems were found in the course of conducting the experiment: firstly, the mass transfer efficiency of the common deionized water is not high during the dipping process, which results in Ti (OH) 4 The gel does not impregnate well with the ACF. Secondly, TiO obtained after roasting 2 The ACF material is subjected to scanning electron microscope and shaking to find partial TiO 2 The powder is exfoliated, resulting in reduced photocatalytic stability.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention provides TiO 2 Preparation method, testing device and testing method of/ACF composite material, TiO synthesized with assistance of micro/nano bubble method 2 The ACF composite photocatalytic material has high removal efficiency on toluene, the removal efficiency on toluene can be kept above 98% before 10h, more adsorption and reaction sites can be provided for gaseous toluene by virtue of the huge specific surface area of the ACF, the generation of toluene and toluene intermediates is reduced, and the ACF composite photocatalytic material has good reproducibility.
The technical scheme is as follows: in order to solve the technical problems, the invention provides TiO 2 Of ACF composite materialThe preparation method comprises the following steps:
(1) cutting the ACF into square blocks of 2.5cm multiplied by 2mm, and cleaning impurities and dust on the surface of the active carbon fiber by using deionized water;
(2) soaking in an ammonia water solution with the volume ratio of ammonia water to water being 0.5mol/L for 25-35min, then washing for 3 times by using deionized water, and pressing water in the ACF to be dry;
(3) preparing 45% nitric acid solution, soaking the ACF treated by ammonia water in 45% nitric acid solution for 25-35min, washing with deionized water for 3 times, and pressing the water of the ACF to dry as much as possible with tweezers;
(4) preparing ethanol and water with the volume of 1: 1, soaking the processed ACF in ethanol solution for 25-35min, ultrasonically cleaning for 3 times, 8-12min each time, cleaning with deionized water for 3 times, drying in a drying oven at 105 deg.C for 2h, and weighing the mass m of the activated carbon fiber 1 ，m 2 ，m 3 ；
(5) Measuring 34mL of absolute ethyl alcohol, dripping 17mL of tetrabutyl titanate (TBT) under the stirring condition, and continuously stirring for 25-35min to completely dissolve the tetrabutyl titanate;
(6) adding 2.5mL of acetylacetone, stirring for 25-35min by a magnetic stirrer to obtain a solution A, quickly and uniformly mixing 10mL of absolute ethyl alcohol, 40mL of micro/nano bubble water and 2mL of acetic acid, adjusting the pH value to 2.5 by using concentrated nitric acid, and stirring for 20min to obtain a solution B;
(7) controlling the magnetic stirring speed at about 800r/min, dropping the liquid B into the liquid A at 0.5 drop/s, stirring for 2h after the dropping is finished, aging for 24h at 25 ℃, placing the activated ACF into the aged sol for ultrasonic treatment for 25-35min, and soaking for 25-35min after the treatment is finished;
(8) taking out the impregnated composite material, drying in an oven at 105 deg.C for 0.5h, cooling to room temperature to obtain 1 time of impregnation, repeating the impregnation for 3 times, putting the dried and impregnated ACF into a tube furnace, heating to 450 deg.C at a heating rate of 10 deg.C/min under the protection of nitrogen, and calcining for 2h to obtain TiO 2 the/ACF composite material.
A photocatalytic performance testing device comprises a first air pump and a second air pumpThe device comprises an air pump, a quartz reactor and a gas chromatograph, wherein the first air pump is connected with a toluene generation device sequentially through a first silica gel drying tube and a first flow controller, the second air pump is connected with a buffer bottle sequentially through a second silica gel drying tube and a second flow controller, the toluene generation device is positioned in a constant-temperature water tank and is connected with the buffer bottle through an air duct, and the buffer bottle is connected with the quartz reactor, the gas chromatograph and a tail gas collection device sequentially; the TiO is placed in the quartz reactor 2 the/ACF composite material is characterized in that a light source is arranged outside the quartz reactor.
Preferably, the light source is a 300w xenon lamp.
Preferably, the tail gas collecting device is a tail gas collecting bottle.
The photocatalytic performance testing method comprises the following steps:
(1) connecting a testing device as required;
(2) TiO prepared by the process of claim 1 2 the/ACF composite material is placed in a quartz reactor, and a light source is arranged outside the quartz reactor;
(3) when the toluene gas passes through the gas phase photocatalysis micro-reaction device, the reaction device adjusts the toluene concentration through adjusting the toluene peak area, the sample measurement is started after the toluene reaches the adsorption balance, and a water cooling circulation system in the reaction device maintains the temperature stability of the reactor;
(4) starting a light source, wherein the distance between the light source and the quartz reactor is 9-11cm, continuously introducing 40ppm of toluene standard gas into the quartz reactor, and the flow is 30 ml/min;
(5) measuring the initial concentration of the toluene and the outlet concentration of the toluene after t time of the photocatalytic reaction,
and when the degradation rate concentration of the toluene is stable, shooting a spectrum by using a gas chromatograph.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the TiO2/ACF composite photocatalytic material synthesized by the micro/nano bubble method has high removal efficiency on toluene. The removal efficiency of the toluene can be kept above 98% before 10h, more adsorption and reaction sites can be provided for the gaseous toluene by virtue of the huge specific surface area of the ACF, the generation of toluene and toluene intermediates is reduced, and the regeneration performance of the gaseous toluene and toluene intermediates is good.
(2) In the exfoliation experiment, TiO 2 ACF (micro/Nano bubble Water) compared with TiO 2 the/ACF has stronger adhesion, and in 5 times of long-time cycle experiments, TiO 2 The ACF composite photocatalytic material has better stability, and the removal efficiency of 100 percent can be kept for the first four times, so the addition of the micro/nano bubble water enhances the removal effect of the catalyst and improves the durability of the material in use.
Drawings
FIG. 1 shows TiO prepared by micro-nano bubble water 2 ACF section view;
FIG. 2 is a flow chart of a photocatalytic reaction.
FIG. 3 shows ACF and TiO 2 SEM photograph of/ACF series composite material.
FIG. 4 shows ACF and TiO 2 N2 adsorption-desorption isotherms of/ACF series composites.
FIG. 5 shows ACF and TiO 2 XRD patterns of/ACF series composite materials.
FIG. 6 is TiO 2 The removal efficiency of the/ACF series composite material to toluene is shown.
FIG. 7 is TiO 2 Stability analysis chart of/ACF (micro/nano bubble water).
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
The invention relates to a TiO 2 The preparation method of the/ACF composite material comprises the steps of preparing a reagent, an experimental device and an instrument, wherein the reagent, the experimental device and the instrument comprise tetrabutyl titanate (mass fraction is more than or equal to 99.0 percent), absolute ethyl alcohol, acetic acid, ammonia water, nitric acid and acetylacetone, which are all analytically pure and Activated Carbon Fibers (ACF), and are products of Jiuzhou Longtong environmental protection equipment manufacturing Limited company in Suzhou. AMM-9T type magnetic stirrer, DHG-9140AS type electric heating constant temperature blast drying oven, SB-3200DTD type ultrasonic cleaning machine, SK-G08123K type tubular heating furnaceThe micro/nano bubble generator is a micro/nano bubble generator, a PXSJ-216 type thunder magnetic PH meter, an FA2004 type analytical balance, a Quanta type scanning electron microscope (FEI corporation, USA), a SmartLab type X-ray diffractometer (Nippon science and technology Co., Ltd.), an ASAP2460 type specific surface area and porosity analyzer (Mike instruments Co., Ltd., USA), a GC9800 type gas chromatograph (Shanghai science and technology Instrument Co., Ltd.), a CEL-300-T3 gas phase photocatalysis micro reaction device (HXF science and technology Co., Ltd., Beijing) and a commercial micro/nano bubble generator.
The method specifically comprises the following steps:
(1) cutting the ACF into square blocks of 2.5cm multiplied by 2mm, and cleaning impurities and dust on the surface of the active carbon fiber by using deionized water;
(2) soaking in an ammonia water solution with the volume ratio of ammonia water to water of 0.5mol/L for 25-35min, then washing with deionized water for 3 times, and pressing water in the ACF to dry;
(3) preparing 45% nitric acid solution, soaking the ACF treated by ammonia water in 45% nitric acid solution for 25-35min, washing with deionized water for 3 times, and pressing the water of the ACF to dry as much as possible with tweezers;
(4) preparing ethanol and water with the volume of 1: 1, soaking the processed ACF in ethanol solution for 25-35min, ultrasonically cleaning for 3 times, 8-12min each time, cleaning with deionized water for 3 times, drying in a drying oven at 105 deg.C for 2h, and weighing the mass m of the activated carbon fiber 1 ，m 2 ，m 3 ；
(5) Measuring 34mL of absolute ethyl alcohol, dripping 17mL of tetrabutyl titanate (TBT) under the stirring condition, and continuously stirring for 25-35min to completely dissolve the tetrabutyl titanate;
(6) adding 2.5mL of acetylacetone, stirring for 25-35min by a magnetic stirrer to obtain a solution A, quickly and uniformly mixing 10mL of absolute ethyl alcohol, 40mL of micro/nano bubble water and 2mL of acetic acid, adjusting the pH value to 2.5 by using concentrated nitric acid, and stirring for 20min to obtain a solution B;
(7) controlling the magnetic stirring speed at about 800r/min, dripping the liquid B into the liquid A at 0.5 drop/s, stirring for 2h after the dripping is finished, aging for 24h at 25 ℃, putting the activated ACF into the aged sol, performing ultrasonic treatment for 25-35min, and soaking for 25-35min after the treatment is finished;
(8) taking out the impregnated composite material, drying in an oven at 105 deg.C for 0.5h, cooling to room temperature to obtain 1 time of impregnation, repeating the impregnation for 3 times, putting the dried and impregnated ACF into a tube furnace, heating to 450 deg.C at a heating rate of 10 deg.C/min under the protection of nitrogen, and calcining for 2h to obtain TiO 2 the/ACF composite material.
In the invention, an emission Scanning Electron Microscope (SEM) is adopted to observe the size and the appearance of the composite material; analyzing the crystal structure of the sample by using an X-ray diffractometer, and observing and comparing the crystal structure with ACF, TiO2/ACF and TiO 2 Characteristic peak of ACF (micro/nano bubble water), and determination of TiO 2 And (4) calculating the specific surface area, the pore volume and the pore size distribution of the sample according to a BET method and a BJH model.
To verify micro/nano bubble water to TiO 2 The acting force of the/ACF composite material interface is firstly flushed by running water for 3min, the turbidity degree of the beaker water is observed, the beaker water is dried in an oven for 1h after being flushed, the material is placed in a test bag for sealing, ultrasonic treatment is carried out for 0.5h, and the TiO of the material is observed by using a scanning electron microscope 2 Loading of the particles in the ACF.
As shown in fig. 2, a photocatalytic performance testing device comprises a first air pump 1, a second air pump, a quartz reactor 7 and a gas chromatograph 8, wherein the first air pump 1 is connected with a toluene generating device 4 sequentially through a first silica gel drying tube 2 and a first flow controller 3, the second air pump is connected with a buffer bottle 6 sequentially through a second silica gel drying tube and a second flow controller, the toluene generating device 4 is located in a constant-temperature water tank 5, the toluene generating device 4 is connected with the buffer bottle 6 through an air duct, and the buffer bottle 6 is connected with the quartz reactor 7, the gas chromatograph 8 and a tail gas collecting device 9 sequentially; the above TiO is placed in the quartz reactor 7 2 the/ACF composite material is provided with a light source outside the quartz reactor 7.
The photocatalytic performance testing method comprises the following steps:
(1) connecting a testing device as required;
(2) TiO prepared by the process of claim 1 2 the/ACF composite material is placed in a quartz reactor 7, and a light source is arranged outside the quartz reactor 7;
(3) when the toluene gas passes through the gas phase photocatalysis micro-reaction device, the reaction device adjusts the toluene concentration through adjusting the toluene peak area, the sample measurement is started after the toluene reaches the adsorption balance, and a water cooling circulation system in the reaction device maintains the temperature stability of the reactor;
(4) starting a light source, wherein the distance between the light source and the quartz reactor 7 is 9-11cm, continuously introducing 40ppm of toluene standard gas into the quartz reactor 7, and the flow is 30 ml/min;
(5) measuring the initial concentration of the toluene and the outlet concentration of the toluene after t time of the photocatalytic reaction,
when the toluene degradation rate concentration is stable, the gas chromatograph 8 photographs a spectrum.
About 0.1g of TiO 2 the/ACF composite material is put into a quartz reactor 7 as a reactor to carry out a photodegradation experiment, a 300w xenon lamp is used as a light source, a catalyst is about 10cm away from the material to irradiate the reactor, 40ppm of toluene standard gas is continuously introduced into the reactor, and the flow rate is 30 ml/min.
Before radiation, toluene is adsorbed on the photocatalyst to reach balance, and circulating water is introduced to the outer layer of the quartz tube to maintain the temperature inside the reactor stable. And then, turning on a xenon lamp, automatically sampling by an instrument in the process of illumination, and finally analyzing the degradation rate and the mineralization rate of the toluene by using a gas chromatograph through an internal standard method. The reaction was carried out for at least 4h until the reaction gas concentration was stable.
As shown in fig. 3, it can be observed from fig. a that the surface of the ACF is clean and free of impurities, and each fiber is randomly interwoven, and the surface of each fiber is smooth and has linear grooves and ridges arranged along the longitudinal direction. As shown in the diagrams b-d, the ACF is wrapped with TiO with a certain shape 2 From the graph b, it can be observed that TiO supported on the ACF surface 2 The particles fall off, so that the application value of the material in the VOCs treatment process is seriously influenced. Under the same test conditions, the comparison of the graphs c-d shows thatTiO using micro/nano bubble water 2 TiO loaded by ACF composite material 2 More particles than TiO without micro/nano bubble water 2 the/ACF may have a higher stability. As can be seen from the graph f, the TiO on the ACF surface after the flow water washing and the ultrasonic treatment 2 The load is significantly reduced. As shown by the comparison of the graphs e-f, the ACF surface showed no evidence of peeling off after the micro/nano bubbles were added, and TiO was observed in comparison with the ACF surface without the micro/nano bubble water 2 The load is more uniform, and the load capacity is obviously higher than that of the material without the micro/nano bubble water. Proves that the micro/nano bubbles are used as an interface inducer, and improves TiO 2 And the ACF. Make TiO react 2 the/ACF composite material has better catalytic stability.
N of 3 materials as shown in FIG. 4 2 The shape and size of the adsorption-desorption isotherms are approximately the same. Adsorbing under the relative atmospheric pressure lower than 0.1, and having obvious adsorption hysteresis loop between 0.4 and 1.0, belonging to IV type isotherm in IUPAC classification, which shows that the pore structure is very irregular and the mixture of micropores and mesopores exists. The specific surface areas of the 3 materials are all larger, and compared with the specific surface area of a blank Activated Carbon Fiber (ACF), TiO is 2 /ACF due to TiO loading 2 So that the specific surface area is reduced, and under the condition of soaking for 3 times, micro/nano bubble water TiO is added 2 The specific surface area of the composite material of/ACF is 611.1419m2.g at the lowest -1 Probably because the micro-nano bubble water strengthens TiO 2 Acting with ACF to cause TiO 2 The amount of (2) increases to reduce the specific surface area.
As shown in FIG. 5, ACF and TiO 2 /ACF、TiO 2 XRD crystal form characterization pattern of ACF (micro/nano bubble water). The broad peaks of pure ACF at 25 °, 44 °, 71.5 ° indicate that ACF has a graphite-like crystal structure, which is typically amorphous. TiO2 2 There are three crystal phases, rutile, anatase and brookite, anatase and rutile are mostly studied, compared with rutile TiO 2 Anatase type TiO 2 Has larger specific surface area, more lattice defects and stronger capture capability to electrons, and is favorable for the separation of electron-hole pairs [17]。TiO 2 6 TiO atoms of the ACF composite material appear at 2 theta 25.3 DEG, 37.8 DEG, 48 DEG and 55 DEG 2 Diffraction peaks, known from JCPDS standard cards, are all TiO 2 Anatase characteristic peak, but no amorphous characteristic peak of ACF, indicating TiO 2 TiO in/ACF composite material 2 Mainly in the anatase crystal form supported on ACF.
Under the experimental conditions that the initial concentration of toluene is 40ppm, the gas flow of toluene is 30ml/min and a 300w xenon lamp is used as a light source, TiO is respectively measured in a photocatalytic reactor 2 /ACF (micro/nano bubble water), TiO 2 /ACF、TiO 2 The removal efficiency and mineralization rate of the/ACF (sonicated at 1.4) composite for toluene are shown in FIGS. 6(a), (b).
As can be seen from fig. 6(a), the toluene removal efficiency among the 3 experimental samples increased with the increase of the reaction time, and after 30min of reaction, all three experimental samples reached 80% or more, and after 60min of reaction, all reached 90% or more, and the final reaction stabilized at 98% as the reaction proceeded. The result shows that the adsorption enrichment effect formed by the huge specific surface area of the ACF can greatly increase the toluene, the toluene intermediate and the TiO 2 The reaction probability on the surface improves the mass transfer efficiency, thereby effectively improving the TiO 2 The photocatalytic efficiency of (c). As can be seen from fig. 6(b), the mineralization rate is rather decreased with the increase of the reaction time, because as the reaction proceeds, the intermediate product of toluene generated by the degradation reaction is more and more abundant and the ring-opening reaction of benzene ring is more complicated, the accumulated intermediate is further dehydrated to form carbonaceous deposit (coke), the toluene is subjected to competitive oxidation reaction with the intermediate product and the coke, the accumulation of the coke and the intermediate is intensified to cause the mineralization efficiency to become lower, but the TiO is increased under the action of the micro/nano bubble water 2 Adding micro/nano bubble water TiO 2 ACF composite material and TiO treated by ultrasonic wave 2 The mineralization rate of the/ACF composite material is higher than that of TiO without micro/nano bubble water after 60min 2 the/ACF composite material. Namely, the stability and the catalytic activity of the catalyst are enhanced by adding the micro/nano bubble water.
The stability is that the catalyst shouldBy an important index towards incorporation of TiO 2 42ppm of toluene standard gas is introduced into a quartz reactor of/ACF (micro/nano bubble water), the flow rate is 30ml/min, and the stability of the composite material is observed after 5-cycle experiments (after the sample is tested, the heat treatment is carried out at 150 ℃ and nitrogen purging is carried out for 1h) are carried out for 350min each time. The test result of fig. 7 shows that in the long-time reaction, the removal efficiency of the first four times is 100%, and the removal efficiency of the 5 th time is still as high as 89.61%, so that the removal effect is better. This shows that the stability of the composite material can be better improved by adding the micro/nano bubble water.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (5)
1. TiO2 2 The preparation method of the/ACF composite material is characterized by comprising the following steps:
(1) cutting the ACF into square blocks, and cleaning impurities and dust on the surface of the active carbon fiber by using deionized water;
(2) soaking in an ammonia water solution with the volume ratio of ammonia water to water being 0.5mol/L for 25-35min, then washing for 3 times by using deionized water, and pressing water in the ACF to be dry;
(3) preparing 45% nitric acid solution, soaking the ACF treated by ammonia water in 45% nitric acid solution for 25-35min, washing with deionized water for 3 times, and pressing water of the ACF with tweezers;
(4) preparing ethanol and water with the volume of 1: 1, soaking the processed ACF in ethanol solution for 25-35min, ultrasonically cleaning for 3 times, 8-12min each time, cleaning with deionized water for 3 times, drying in a drying oven at 105 deg.C for 2h, and weighing the mass m of the activated carbon fiber 1 ，m 2 ，m 3 ；
(5) Measuring 34mL of absolute ethyl alcohol, dripping 17mL of tetrabutyl titanate under the stirring condition, and continuously stirring for 25-35min to completely dissolve the tetrabutyl titanate;
(6) adding 2.5mL of acetylacetone, stirring for 25-35min by a magnetic stirrer to obtain a solution A, quickly and uniformly mixing 10mL of absolute ethyl alcohol, 40mL of micro/nano bubble water and 2mL of acetic acid, adjusting the pH value to 2.5 by using concentrated nitric acid, and stirring for 20min to obtain a solution B;
(7) controlling the magnetic stirring speed at about 800r/min, dropping the liquid B into the liquid A at 0.5 drop/s, stirring for 2h after the dropping is finished, aging for 24h at 25 ℃, placing the activated ACF into the aged sol for ultrasonic treatment for 25-35min, and soaking for 25-35min after the treatment is finished;
(8) taking out the impregnated composite material, drying at 105 ℃ for 0.5h in an oven, cooling to room temperature to obtain the impregnated composite material, impregnating for 1 time, repeatedly impregnating for 3 times, putting the dried and impregnated ACF into a tube furnace, heating to 450 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, and roasting for 2h to obtain TiO 2 the/ACF composite material.
2. A photocatalytic performance testing device is characterized in that: the device comprises a first air pump, a second air pump, a quartz reactor and a gas chromatograph, wherein the first air pump is connected with a toluene generation device sequentially through a first silica gel drying tube and a first flow controller; the quartz reactor is filled with TiO prepared according to claim 1 2 the/ACF composite material is characterized in that a light source is arranged outside the quartz reactor.
3. The photocatalytic performance testing device according to claim 2, characterized in that: the light source is a 300w xenon lamp.
4. The photocatalytic performance testing device according to claim 2, characterized in that: the tail gas collecting device is a tail gas collecting bottle.
5. The method for testing photocatalytic performance of claim 2, comprising the steps of:
(1) connecting a testing device as required;
(2) TiO prepared by the process of claim 1 2 the/ACF composite material is placed in a quartz reactor, and a light source is arranged outside the quartz reactor;
(3) when the toluene gas passes through the gas phase photocatalysis micro-reaction device, the reaction device adjusts the toluene concentration through adjusting the toluene peak area, the sample measurement is started after the toluene reaches the adsorption balance, and a water cooling circulation system in the reaction device maintains the temperature stability of the reactor;
(4) starting a light source, wherein the distance between the light source and the quartz reactor is 9-11cm, continuously introducing 40ppm of toluene standard gas into the quartz reactor, and the flow is 30 ml/min;
(5) measuring the initial concentration of the toluene and the outlet concentration of the toluene after t time of the photocatalytic reaction,
and when the degradation rate concentration of the toluene is stable, shooting a spectrum by using a gas chromatograph.
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