CN107694551A - The preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide - Google Patents
The preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide Download PDFInfo
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- CN107694551A CN107694551A CN201711104044.9A CN201711104044A CN107694551A CN 107694551 A CN107694551 A CN 107694551A CN 201711104044 A CN201711104044 A CN 201711104044A CN 107694551 A CN107694551 A CN 107694551A
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- titanium dioxide
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- titanium
- water
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002245 particle Substances 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- 239000004005 microsphere Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 150000002978 peroxides Chemical class 0.000 claims abstract description 8
- 238000007598 dipping method Methods 0.000 claims abstract description 6
- 239000003518 caustics Substances 0.000 claims abstract description 4
- 235000010215 titanium dioxide Nutrition 0.000 claims description 80
- 239000011521 glass Substances 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 229960001866 silicon dioxide Drugs 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- LHJQIRIGXXHNLA-UHFFFAOYSA-N calcium peroxide Chemical compound [Ca+2].[O-][O-] LHJQIRIGXXHNLA-UHFFFAOYSA-N 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium superoxide Chemical compound [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- -1 alkyl oxygen titanium Chemical compound 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000004343 Calcium peroxide Substances 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 235000019402 calcium peroxide Nutrition 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000006187 pill Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- 238000004887 air purification Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000011806 microball Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000011805 ball Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D49/00—Separating dispersed particles from gases, air or vapours by other methods
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide, category material for air purification field, technical scheme to be：Water-soluble titanium source is soluble in water, lower addition weak caustic solution is stirred, wherein, titanium source, water, the quality parts ratio of weak base are 1：10‑100：1 50,10 120min are stood, peroxide is added, obtains solation titania systems；By solation titania systems even application in inorganic microsphere surface or dipping inorganic microsphere, room temperature to 100 DEG C of dry 13 h, less than 600 800 DEG C 1 10 h of sintering.Beneficial effect is：Process of preparing is simple, and decentralization of the titanium dioxide on inorganic microsphere surface is high, does not reunite persistently, and firm position, difficult for drop-off, substantially increases catalytic efficiency；The energy is saved, it is more green.
Description
Technical field
The present invention relates to material for air purification field, and in particular to photocatalyst material preparation technology, especially a kind of table
The preparation technology of the inorganic microspheroidal particles of face uniform location titanium dioxide.
Background technology
TiO2As the catalysis material found earliest, there is nontoxic, catalytic activity（Degraded purification and water decomposition hydrogen manufacturing）
It is high, oxidability is strong, stability is good, cost is low, the characteristic such as environment-friendly, be most possible practical catalysis material, with
The rapid development of nanometer technology, preparation, modification and its application of nano titanium oxide are hot as the research of air purification field
Point.However, because nano titanium oxide is easily reunited, on the other hand, TiO2Wider energy gap（3.2 eV）Determine
It can only play photocatalytic activity under ultraviolet light, and very low to the utilization rate of sunshine, these all greatly limit its application.
The preparation method of titanium dioxide and modifying titanium dioxide is more, such as alkoxide hydrolysis, Hydrothermal preparation method, collosol and gel
Method, chemical precipitation method and solid phase method etc., wherein, sol-gal process is prepared simply, and operation is convenient, condition is easily-controllable etc., it is conventional
Preparation method.In order to improve the photocatalysis performance of titanium dioxide, be on the one hand by controlling reaction condition, such as concentration, temperature,
The decentralization of titanium dioxide is improved, so as to increase contact surface to improve catalytic performance；On the other hand it is by ion doping, bears
The method of modifying such as carry, defective locations can be introduced on surface by doping or change crystallinity, so as to influence answering for electronics and hole
The absorption bands of light is closed or expands, so as to improve the photocatalytic activity of titanium dioxide.However, current method still have it is many
Problem, as preparation process is more complicated；Titanium dioxide made from reaction can not be deposited, and with time lengthening, reunion rate greatly increases, and urges
Change effect to substantially reduce, how to improve and keep the decentralization of titanium dioxide is this area technical barrier urgently to be resolved hurrily.
The content of the invention
To solve, existing titanium dioxide decentralization is poor, can not deposit the technical problem for causing activity low, this hair the long period
It is bright that a kind of preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide is provided, by the way that colloidal sol oxide/titanium dioxide is applied
Inorganic microsphere surface is overlying on, and titanium oxide dispersion is realized inorganic micro- by the technique sintered under drying, dynamic disturbances
The twice dispersing of ball surface and sintering positioning, ensure that the decentralization of titanium dioxide, and substantially increase titanium dioxide and keep high
The degree scattered time, so as to improve the catalytic performance of titanium dioxide.
The technical solution adopted by the present invention is：The preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide,
Characterized in that, the preparation technology comprises the following steps：
（1）Water-soluble titanium source is soluble in water, lower addition weak caustic solution is stirred, wherein, titanium source, water, the quality parts ratio of weak base
For 1：10-100：1-50,10-120min is stood, add peroxide, obtain solation titania systems；
（2）By solation titania systems even application in inorganic microsphere surface or dipping inorganic microsphere, room temperature to 100 DEG C it is dry
Dry 1-3 h, less than 600-800 DEG C sintering 1-10 h, obtain the inorganic microspheroidal particles of surface uniform location titanium dioxide.
Further, the step（1）Solation titania systems through centrifuging or filtering, will precipitation or filter cake with water
Resuspension is uniformly further purified, and controls the mass ratio of titanium dioxide and waterkFor 1：10~1000 .
Further, the step（2）By solation titania systems even application in inorganic microsphere surface or dipping
The mass ratio relation that titanium dioxide and inorganic microsphere are controlled during inorganic microsphere is mT/mQ=KC,Whereinm TFor titanium dioxide quality,m QFor inorganic microsphere quality,CFor inorganic microsphere water absorption rate.
Further, the peroxide include but is not limited to hydrogen peroxide, sodium peroxide, potassium peroxide, calper calcium peroxide,
One or more in sodium peroxydisulfate, potassium peroxydisulfate.
Further, the water-soluble titanium source is titanyl sulfate, titanium tetrachloride, titanium trichloride, titanium tetrafluoride or alkyl oxygen
More than one or both of titanium, the weak base is ammoniacal liquor.
Further, the inorganic microsphere includes but is not limited to glass microballoon, silica-gel sphere, haydite, zeolite microballon, aluminum oxide
Microballon, silicon-carbide particle, steel ball, aluminium pill or copper bead microballoon.
The present invention also provides the inorganic microspheroidal particles of above-mentioned surface uniform location titanium dioxide answering in fluidized bed plant
With.
In above-mentioned technical proposal, there is provided a kind of preparation technology of inorganic microsphere surface positioning monodisperse titanium dioxide, specifically
Comprise the following steps：Water-soluble titanium source is soluble in water, lower addition weak caustic solution is stirred, wherein, titanium source, water, the quality of weak base
Portion rate is 1：10-100：1-50,10-120min is stood, is surface-treated with peroxide, obtains colloidal sol oxide/titanium dioxide body
System, now the nano-particle in system is not grown up fully also, and crystallinity is very low, belongs to amorphous state mostly, scattered to ensure
Degree, solation titania systems concentration general control is below 10%；By solation titania systems be uniformly coated or impregnated with
Inorganic microsphere surface, room temperature to 100 DEG C of dry 1-3 h because titanium oxide is in aqueous scattered be it is very uniform, its
Specific surface area is very big, after solation titania systems even application is in inorganic microsphere surface or dipping inorganic microsphere, by
The suction-operated of water, form uniform water film simultaneously, colloidal sol oxide/titanium dioxide uniformly loads to inorganic microsphere surface, by model moral
Magnificent power connection, with room temperature to 100 DEG C of dry 1-3 h, slowly removes moisture removal, prevents quick heating from causing vapor to surface dioxy
Change the impact of titanium.And unadsorbed unnecessary titanium dioxide can be washed with water after drying at room temperature, greatly reduce titanium oxide
Reunion.After deionized water gently rinses the unadsorbed titanium dioxide of removal, 0.1-10 h, the temperature are sintered at 400-800 DEG C
The lower rutile titanium dioxide crystallinity that can be obtained of degree is high, and activity height, temperature will be low, causes sintering time oversize, activity
Reduce, high energy consumption, and temperature is too high is also easy to produce crystal transfer, in sintering process, the peroxy of titanium dioxide surface grafting
Group occurs the cross-linking reaction between particle and forms bridging oxygen chemical bond with microsphere surface, uniform, firmly negative so as to obtain surface
Carry the inorganic microspheroidal particles of monodisperse titanium dioxide.
The beneficial effects of the invention are as follows：（1）Process of preparing provided by the invention is simple, and titanium dioxide is in inorganic microsphere
The decentralization on surface is high, does not reunite persistently, and firm position, difficult for drop-off, substantially increases catalytic efficiency；（2）Preparation method
In be not related to organic solvent, save the energy, it is more green；（3）In further improved technical scheme, by control system
All moisture content are exactly equal to inorganic microsphere saturated water adsorptive value so that the moisture film on inorganic microsphere surface is stable to be adsorbed, and no free water is deposited
So as to ensure that inorganic microsphere surface titanium dioxide is individual layer monodisperse status nano particle；By controlling titanium dioxide body
The concentration and titanium dioxide of system and the ratio of inorganic microsphere so that the monodisperse titanium dioxide quantity of inorganic microsphere surface positioning
More, decentralization height, it is evenly distributed, catalytic efficiency greatly improves.
Brief description of the drawings
Fig. 1, Fig. 2 are the glass microballoon that monodisperse titanium dioxide nanometer particle is located in the gained surface of the embodiment of the present invention 1
The scanning electron microscope (SEM) photograph of different amplification.
Fig. 3 is the datagram of embodiment 1-4 products obtained therefroms degraded acetaldehyde effect.
Embodiment
The present invention provides a kind of preparation technology of inorganic microsphere surface positioning monodisperse titanium dioxide, below by way of specific reality
Apply example and describe the present invention in detail in order to understanding, but the invention is not limited in any way, in embodiment involved reagent for example without
Special instruction, it can be bought and obtained by commercial sources, institute's application method, be conventional method unless otherwise instructed.
Embodiment 1：
10g titanyl sulfates are dissolved in 500ml water, the lower ammoniacal liquor for adding 110mL concentration 2.5% is stirred, staticly settles reaction
30min, being centrifuged with 8000-10000r/min, then remove supernatant, centrifugation gained solid precipitation is resuspended with 90ml water, by
Stirring and ultrasound make the system after resuspension uniform, add 60g hydrogen peroxide（Mass concentration is 30%）, obtain colloidal sol oxide/titanium dioxide
System；
（2）The glass microsphere of 20 μm of average grain diameter is chosen, washing, alcohol are washed, oil removing and after drying, and colloidal sol oxide/titanium dioxide is sprayed
In glass microballoon surface, 45 DEG C of 3 h of drying, 800 DEG C sinter 1 h, obtain the glass microsphere particle of surface uniform location titanium dioxide
（S1）, scanning electron microscope (SEM) photograph is visible on figure as shown in Fig. 1, Fig. 2, glass microsphere area load layer of titanium dioxide nano particle,
Uniformly, monodispersity can be good for grain dispersiveness, and the particle diameters of titania nanoparticles is 50-100nm, size uniform.Further lead to
Cross the front and rear contrast of quality and find that the load capacity of titania nanoparticles is the 1% of glass microsphere quality.
Embodiment 2：
10g titanium tetrachlorides are dissolved in 300ml water, the lower ammoniacal liquor for adding 100ml concentration 2.5% is stirred, staticly settles reaction
30min, being centrifuged with 8000-10000r/min, then remove upper liquid, centrifugation gained solid precipitation is resuspended with 100ml water, by
Stirring and ultrasound make the system after resuspension uniform, add 50g hydrogen peroxide, obtain dissolved colloidal state titania systems；
（2）Colloidal sol oxide/titanium dioxide is sprayed to 100 μm of silica gel microball surface, 35 DEG C of 3 h of drying, 600 DEG C of 3 h of sintering, obtained
The silica gel microball particle of monodisperse titanium dioxide is located in surface（S2）, the front and rear contrast discovery of quality, titania nanoparticles
Load capacity be silica gel microball quality 0.89%.
Embodiment 3：
10g titanium trichlorides are dissolved in 300ml water, the lower ammoniacal liquor for adding 200ml concentration 2.5% is stirred, staticly settles reaction
30min, filter, gained filter cake is resuspended with 100ml water, is made the system after resuspension uniform by stirring and ultrasound, is added 70g peroxides
Change hydrogen, obtain dissolved colloidal state titania systems；
（2）Colloidal sol oxide/titanium dioxide is sprayed to 100 μm of ceramic fine bead surface, 50 DEG C of 2 h of drying, 700 DEG C of sintering 3h, obtains table
Face sinters the ceramic fine bead that monodisperse titanium dioxide is located（S3）, the front and rear contrast discovery of quality, titania nanoparticles
Load capacity is the 0.94% of ceramic fine bead quality.
Embodiment 4：
The mixture of 10g titanium trichlorides and alkyl oxygen titanium is dissolved in 300ml water and stirred, stirs lower addition 150ml concentration
2.5% ammoniacal liquor, reaction 50min is stood, is filtered, gained filter cake is resuspended with 100ml water, and stirring and ultrasound make the system after resuspension
Uniformly, 70g hydrogen peroxide is added, obtains dissolved colloidal state titania systems；
（2）Colloidal sol oxide/titanium dioxide is sprayed to 3 μm of copper bead microsphere surface, 65 DEG C of 1 h of drying, 600 DEG C of 3 h of sintering, obtains table
The copper bead microsphere particle of monodisperse titanium dioxide is located in face, and the front and rear contrast of quality is found, the load of titania nanoparticles
Measure as the 0.91% of ceramic fine bead quality.
Experimental performance is tested
Each product in above-described embodiment is subjected to acetaldehyde degradation performance test according to following test method respectively.
The setting of test chamber：It is 1.5m that corresponding each sample prepares volume respectively3Laboratory Module, separately prepare a 1.5m3Sky
White control cabin, the inorganic microsphere of the above-mentioned surface positioning monodisperse titanium dioxides of 200g, blank are respectively put into each Laboratory Module
Control is put into 2g titanium dioxide dry powder in cabin（Step 1 gained dissolved colloidal state titania systems are spray-dried, 600 DEG C of 3 h of sintering
Grinding gained afterwards）And the glass microsphere in 198g embodiments 1, then it is filled with respectively into Laboratory Module and blank control cabin identical dense
Degree（5mg/m3）Acetaldehyde, close test chamber；The fan of test chamber is then opened simultaneously, makes Cabin contamination thing cycle balance, 24h
The concentration of pollutant in test chamber is sampled simultaneously again afterwards, analysis test, calculates acetaldehyde residual rate, computational methods are with reference to such as
Lower formula：Acetaldehyde residual rate=sample experiments cabin acetaldehyde concentration value ÷ blank controls cabin acetaldehyde concentration value × 100%.As a result referring to figure
3, as shown by data, with particle obtained by the inorganic microspheroidal particles of the surface uniform location titanium dioxide of preparation method of the present invention preparation
Titania nanoparticles maintain good high dispersion, it is easy to substantially improve titanium dioxide obtained by current preparation method
The defects of reunion, contact area of the titanium dioxide in use with ambient atmos is improved, ensure that its efficient catalytic is imitated
Rate, while caused by also largely avoided titanium dioxide micro-nano particle in itself the problems such as PM2.5 dust pollutions.
As fully visible, the inorganic microsphere of uniform location titanium dioxide in surface provided by the invention, the letter of its manufacturing process steps
Victory, operation is simple, improves gained titanium dioxide monodisperse status, is stored beneficial to long-time, improves its activity and urges
Change performance；It is used for fluidized bed plant as catalysis filtrate, substantially increases the catalytic efficiency of fluid bed and the service life of filtrate,
It can also be filled in the devices such as air purifier, for improving IAQ.
Claims (8)
1. the preparation technology of the inorganic microspheroidal particles of surface uniform location titanium dioxide, it is characterised in that the preparation technology bag
Include following steps：
（1）Water-soluble titanium source is soluble in water, lower addition weak caustic solution is stirred, wherein, titanium source, water, the quality parts ratio of weak base
For 1：10-100：1-50,10-120min is stood, add peroxide, obtain solation titania systems；
（2）By solation titania systems even application in inorganic microsphere surface or dipping inorganic microsphere, room temperature to 100 DEG C it is dry
Dry 1-3 h, less than 400-800 DEG C sintering 0.1-10 h, obtain the inorganic microspheroidal particles of surface uniform location titanium dioxide.
2. preparation technology according to claim 1, it is characterised in that the step（1）Solation titania systems
Through centrifuging or filtering, precipitation or filter cake are resuspended with water and are uniformly further purified, controls the mass ratio of titanium dioxide and waterkFor 1：
10~1000 。
3. preparation technology according to claim 2, it is characterised in that the step（2）By solation titania systems
It is m that even application controls the mass ratio relation of titanium dioxide and inorganic microsphere when inorganic microsphere surface or dipping inorganic microsphereT/
mQ=KC,Whereinm TFor titanium dioxide quality,m QFor inorganic microsphere quality,CFor inorganic microsphere water absorption rate.
4. preparation technology according to claim 1, it is characterised in that titanium member in the addition and titanium source of the peroxide
The mol ratio of element is 5:1~20:1.
5. preparation technology according to claim 1, it is characterised in that the peroxide includes but is not limited to peroxidating
One or more in hydrogen, sodium peroxide, potassium peroxide, calper calcium peroxide, sodium peroxydisulfate, potassium peroxydisulfate, the weak base are ammoniacal liquor.
6. preparation technology according to claim 1, it is characterised in that the water-soluble titanium source is titanyl sulfate, four chlorinations
It is more than one or both of titanium, titanium trichloride, titanium tetrafluoride or alkyl oxygen titanium.
7. preparation technology according to claim 1, it is characterised in that it is micro- that the inorganic microsphere includes but is not limited to glass
Pearl, silica-gel sphere, haydite, zeolite microballon, aluminum oxide microballon, silicon-carbide particle, steel ball, aluminium pill or copper bead microballoon.
A kind of 8. application of inorganic microspheroidal particles of surface uniform location titanium dioxide in fluidized bed plant.
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