CN106395896B - A kind of preparation method of micropore spherical titanium dioxide - Google Patents
A kind of preparation method of micropore spherical titanium dioxide Download PDFInfo
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- CN106395896B CN106395896B CN201611078855.1A CN201611078855A CN106395896B CN 106395896 B CN106395896 B CN 106395896B CN 201611078855 A CN201611078855 A CN 201611078855A CN 106395896 B CN106395896 B CN 106395896B
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- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- 239000012065 filter cake Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000003750 conditioning effect Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- WVOXLKUUVCCCSU-ZPFDUUQYSA-N Pro-Glu-Ile Chemical compound [H]N1CCC[C@H]1C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H]([C@@H](C)CC)C(O)=O WVOXLKUUVCCCSU-ZPFDUUQYSA-N 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
-
- B01J35/39—
-
- B01J35/51—
-
- B01J35/56—
-
- B01J35/61—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Biomedical Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Disclosed by the invention is a kind of preparation method of micropore spherical titanium dioxide, using nano titanium oxide, PEI, urea as raw material, it is raw material using ethylene glycol solution, by the high-temperature process of certain time, pH value is adjusted after cooling, vacuum filtration, dry sediment, the calcining passed through again under certain condition can obtain the spherical titanium dioxide of micropore, and preparation method step of the present invention is simple, efficiency high, yield is also high, obtained titanium dioxide specific surface area is big, has higher photocatalytic activity, is more widely applied it.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide, more specifically say, be related to a kind of spherical titanium dioxide of micropore
The preparation method of titanium.
Background technology
Energy shortage, environmental pollution have turned into the main problem that has faced of world today's development, development new energy with can be again
The raw energy, the presence for reducing pollutant in air, it has also become the common recognition of various circles of society.Photocatalysis technology is one kind in the energy and ring
There is the green technology of important application prospect in border field.Titanium dioxide is set to activate and give birth in the presence of daylight or light middle-ultraviolet lamp
Into the free radical with high catalytic activity, very strong photooxidation and reducing power can be produced, can be catalyzed, photodissociation is attached to object table
The organic matters such as the various formaldehyde in face and part inorganic matter.The function of purifying the air of a room can be played.
Titanium dioxide also has absorption function to pernicious gas, and for nano titanium oxide because particle diameter is small, activity is big, can be anti-
Penetrate, scatters ultraviolet, and can absorbs ultraviolet, so as to there is stronger obstructing capacity to ultraviolet, titanium dioxide non-toxic inexpensive and
Chemical property is stable, has excellent photosensitive, wet sensitive, air-sensitive and photoelectric properties, in functionality ceramic and photocatalysis field
Have a wide range of applications.
The content of the invention
The present invention is provided with the spherical dioxy of a kind of micropore for preparing the technical characterstics such as simple, efficiency high, excellent catalytic effect
Change the preparation method of titanium.
A kind of preparation method of micropore spherical titanium dioxide provided by the invention, it uses following steps：
1) mass fraction is pressed, takes 0.28-0.50 part titanium dioxide, 0.5-1.0 parts PEI, 1.8-2.5 part urea, 30-60 parts
Ethylene glycol solution mixes dissolving, is transferred in the autoclave of polytetrafluoroethyllining lining, anti-under conditions of 180-250 DEG C
12-16h is answered, after naturally cool to room temperature, 5-10min is centrifuged in the centrifuge that rotating speed is 3000-5000rpm, uses second respectively
Alcohol and water washs for several times, is then 9 with hydrochloric acid conditioning solution pH value, vacuum filtration obtains filter cake, and filter cake is placed in into 40-60 DEG C of bar
It is dried overnight in baking oven or high temperature furnace under part, obtain product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
500-700 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
A kind of preparation method of micropore spherical titanium dioxide provided by the invention, it uses following steps：
1) mass fraction is pressed, takes 0.28 part of titanium dioxide, 0.5 part of PEI, 1.8 parts of urea, 30 parts of ethylene glycol solutions, which mix, to be stirred
Dissolving is mixed, is transferred in the autoclave of polytetrafluoroethyllining lining, 12h is reacted under conditions of 180 DEG C, after naturally cool to room
Temperature, 10min is centrifuged in the centrifuge that rotating speed is 3000rpm, respectively with ethanol and water washing for several times, then adjusted with hydrochloric acid molten
Liquid pH value is 9, and vacuum filtration obtains filter cake, and filter cake is placed in dried overnight in the baking oven under the conditions of 50 DEG C or high temperature furnace, acquisition
Product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
600 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
The profitable effect of the present invention：This preparation method is green, pollution-free, efficiency high；Operating procedure is simple, without
Complicated template sacrifices method, only can obtain micropore spherical titanium dioxide by simple hydro-thermal method；The titanium dioxide ratio of acquisition
Surface area is big, and performance is better than ordinary titanium dioxide, excellent performance；With higher photocatalytic activity, it is more widely applied；Prepare
The catalysis of micropore spherical titanium dioxide, photodissociation be attached to the ability of the organic matters such as the various formaldehyde of body surface and part inorganic matter
It is more powerful, it is more obvious to the effect that purifies the air of a room；It can reflect, scatters ultraviolet, and can absorbs ultraviolet, has excellent
Photosensitive, wet sensitive, air-sensitive and photoelectric properties.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail：
The preparation method of a kind of micropore spherical titanium dioxide of the present invention, using following steps：
1) mass fraction is pressed, takes 0.28-0.50 part titanium dioxide, 0.5-1.0 parts PEI, 1.8-2.5 part urea, 30-60 parts
Ethylene glycol solution mixes dissolving, is transferred in the autoclave of polytetrafluoroethyllining lining, anti-under conditions of 180-250 DEG C
12-16h is answered, after naturally cool to room temperature, 5-10min is centrifuged in the centrifuge that rotating speed is 3000-5000rpm, uses second respectively
Alcohol and water washs for several times, is then 9 with hydrochloric acid conditioning solution pH value, vacuum filtration obtains filter cake, and filter cake is placed in into 40-60 DEG C of bar
It is dried overnight in baking oven or high temperature furnace under part, obtain product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
500-700 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Embodiment 1：A kind of preparation method of micropore spherical titanium dioxide, the preparation method use following steps：
1) mass fraction is pressed, takes 0.28 part of titanium dioxide, 0.5 part of PEI, 1.8 parts of urea, 30 parts of ethylene glycol solutions mixing,
Stirred with glass bar up to being completely dissolved, be transferred in the autoclave of polytetrafluoroethyllining lining, reacted under conditions of 180 DEG C
12h, it is placed on experimental bench and treats that it naturally cools to room temperature, centrifuges 5min in the centrifuge that rotating speed is 3000rpm, use second respectively
Alcohol and water centrifuge washing is 9 until measuring pH value with tubular type PH meters, vacuum is taken out then with hydrochloric acid conditioning solution for several times
Filter obtains filter cake, and filter cake is placed in dried overnight in the baking oven under the conditions of 40 DEG C or high temperature furnace, acquisition product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
500 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Embodiment 2：A kind of preparation method of micropore spherical titanium dioxide, the preparation method use following steps：
1) mass fraction is pressed, takes 0.39 part of titanium dioxide, 0.75 part of PEI, 2.15 parts of urea, 45 parts of ethylene glycol solutions mix
Close, stirred up to being completely dissolved, be transferred in the autoclave of polytetrafluoroethyllining lining, under conditions of 215 DEG C with glass bar
14h is reacted, is placed on experimental bench and treats that it naturally cools to room temperature, is to centrifuge 8min in 4000rpm centrifuges in rotating speed, uses respectively
Second alcohol and water centrifuge washing is 9 until measuring pH value with tubular type PH meters then with hydrochloric acid conditioning solution for several times, vacuum
Filter and obtain filter cake, filter cake is placed in dried overnight in the baking oven under the conditions of 50 DEG C or high temperature furnace, acquisition product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
600 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Embodiment 3：A kind of preparation method of micropore spherical titanium dioxide, the preparation method use following steps：
1) mass fraction is pressed, 0.5 part of titanium dioxide is taken, 1.0 parts of PEI, 2.5 parts of urea, 60 parts of ethylene glycol solution mixing, uses
Glass bar stirring is transferred in the autoclave of polytetrafluoroethyllining lining, reacted under conditions of 250 DEG C up to being completely dissolved
16h, it is placed on experimental bench and treats that it naturally cools to room temperature, is to centrifuge 10min in 5000rpm centrifuges in rotating speed, uses second respectively
Alcohol and water centrifuge washing is 9 until measuring pH value with tubular type PH meters, vacuum is taken out then with hydrochloric acid conditioning solution for several times
Filter obtains filter cake, is placed in dried overnight in the baking oven under the conditions of 60 DEG C or high temperature furnace, acquisition product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
700 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Embodiment 4：A kind of preparation method of micropore spherical titanium dioxide, the preparation method use following steps：
1) mass fraction is pressed, takes 0.28 part of titanium dioxide, 0.5 part of PEI, 1.8 parts of urea, 30 parts of ethylene glycol solutions, which mix, to be stirred
Dissolving is mixed, is transferred in the autoclave of polytetrafluoroethyllining lining, 12h is reacted under conditions of 200 DEG C, after naturally cool to room
Temperature, 10min is centrifuged in the centrifuge that rotating speed is 3000rpm, respectively with ethanol and water washing for several times, then adjusted with hydrochloric acid molten
Liquid pH value is 9, and vacuum filtration obtains filter cake, and filter cake is placed in dried overnight in the baking oven under the conditions of 50 DEG C or high temperature furnace, acquisition
Product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, be warming up to 1 DEG C/min heating rate
600 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Embodiment of the present invention is not limited to 4 embodiments described above, by foregoing disclosed number range,
With regard to carrying out any replacement in specific embodiment, so as to obtain numerous embodiment, this is not enumerated.
Claims (2)
1. a kind of preparation method of micropore spherical titanium dioxide, it is characterised in that the preparation method uses following steps：
1) mass fraction is pressed, takes 0.28-0.5 part titanium dioxide, 0.5-1.0 parts PEI, 1.8-2.5 part urea, 30-60 parts second two
Alcoholic solution mixes, and is stirred up to being completely dissolved, is transferred in the autoclave of polytetrafluoroethyllining lining, in 180- with glass bar
12-16h is reacted under conditions of 250 DEG C, after naturally cool to room temperature, 5- is centrifuged in the centrifuge that rotating speed is 3000-5000rpm
10min, it is then 9 with hydrochloric acid conditioning solution pH value, vacuum filtration obtains filter cake, will filter respectively with ethanol and water washing for several times
Cake is placed in dried overnight in the baking oven under the conditions of 40-60 DEG C or high temperature furnace, acquisition product A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, 500- is warming up to 1 DEG C/min heating rate
700 DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
2. a kind of preparation method of micropore spherical titanium dioxide, it is characterised in that the preparation method uses following steps：
1) mass fraction is pressed, takes 0.28 part of titanium dioxide, 0.5 part of PEI, 1.8 parts of urea, 30 parts of ethylene glycol solutions mix molten
Solution, is transferred in the autoclave of polytetrafluoroethyllining lining, reacts 12h under conditions of 200 DEG C, after naturally cool to room temperature,
10min is centrifuged in the centrifuge that rotating speed is 3000rpm, respectively with ethanol and water washing for several times, then uses hydrochloric acid conditioning solution
PH value is 9, and vacuum filtration obtains filter cake, filter cake is placed in dried overnight in the baking oven under the conditions of 50 DEG C or high temperature furnace, is produced
Thing A；
2) the product A that step 1) obtains is put into Muffle furnace and carries out aerobic calcining, 600 are warming up to 1 DEG C/min heating rate
DEG C, 2h is incubated, it is final to obtain micropore spherical titanium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611078855.1A CN106395896B (en) | 2016-11-30 | 2016-11-30 | A kind of preparation method of micropore spherical titanium dioxide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611078855.1A CN106395896B (en) | 2016-11-30 | 2016-11-30 | A kind of preparation method of micropore spherical titanium dioxide |
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| CN106395896B true CN106395896B (en) | 2018-01-05 |
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Effective date of registration: 20201208 Address after: Room 2, 2 / F, unit 1, building 4, No. 14, Hongxing Road, nuojiang Town, Tongjiang County, Bazhong City, Sichuan Province Patentee after: Wang Yajun Address before: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park No. 2 Street No. 928 Patentee before: Zhejiang University of Technology |
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Effective date of registration: 20211208 Address after: Unit 1077, room 05, 1f, No. 39, Ruiping Road, Xuhui District, Shanghai 200030 Patentee after: Huo Yikang (Shanghai) Technology Co.,Ltd. Address before: 636600 No.2, 2nd floor, unit 1, building 4, 14 Hongxing Road, nuojiang Town, Tongjiang County, Bazhong City, Sichuan Province Patentee before: Wang Yajun |