CN101333004A - Process for preparing titania microspheres of mesoporous structure - Google Patents
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- CN101333004A CN101333004A CNA2008101154444A CN200810115444A CN101333004A CN 101333004 A CN101333004 A CN 101333004A CN A2008101154444 A CNA2008101154444 A CN A2008101154444A CN 200810115444 A CN200810115444 A CN 200810115444A CN 101333004 A CN101333004 A CN 101333004A
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- titanium dioxide
- titanium
- mesoporous structure
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- titania microspheres
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000004005 microsphere Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 4
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 10
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229910000348 titanium sulfate Inorganic materials 0.000 claims abstract description 9
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 235000010215 titanium dioxide Nutrition 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- -1 deionized water compound Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 238000012856 packing Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 235000002492 Rungia klossii Nutrition 0.000 description 1
- 244000117054 Rungia klossii Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 238000000366 colloid method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a technology for preparing a powder material with porous structure, in particular to a preparation method of a titanium dioxide microsphere material with mesopore structure. The preparing process includes the following steps: titanium sulfate solution with the concentration of 0.1-0.5M and 0.4-1.2M of basic precipitant solution of ammonia, ammonium acid carbonate or sodium carbonate are added in a flow reactor for titanium ion precipitation reaction and crystallization; the precipitate is filtered, washed, dried in air at 60-80 DEG C for 10-12 hours to obtain titanium dioxide microsphere precursors; finally, the titanium dioxide microsphere precursors are baked at 500-700 DEG C for 1-3 hours to obtain the titanium dioxide microsphere powder. The method of the invention has simple technique and equipment and low cost and is suitable for mass production.
Description
Technical field
The present invention relates to a kind of technology of preparing of porous structural powder material, particularly relate to a kind of titania microspheres of mesoporous structure preparation methods.
Background technology
Chromatographic column filler is the core of high performance liquid chromatography (HPLC) technology, and the ideal column packing should have the superficiality of homogeneous, suitable aperture, pore volume and smaller particle size distributes, and certain rigid and chemical stability be arranged.The used HPLC column packing overwhelming majority is silica gel or modified silica-gel at present.But the column packing of silica matrix has two big defectives: the one, and chemical instability causes the silica matrix stationary phase only can use in the scope of pH2-8, and the 2nd, the silicon hydroxyl of silica gel remained on surface is to the irreversible adsorption of basic cpd.Though the appearance of various new technologies such as coated polymer, individual layer bonding, terminal sealing etc. is greatly improved column performance or stability, but still can not tackle the problem at its root.Therefore, novel inorganic carrier such as titanium dioxide, zirconium dioxide and the aluminum oxide etc. of exploitation replacement of silicon dioxide have received increasing attention.
Chromatographic column has the part bibliographical information with the synthetic method of titanium dioxide microballoon sphere.(U.Trudinger, G.Muller and K.K.Unger, J.Chromatogr.A such as Trudinger, 1990,535:111-125) reported oily emulsion process, Tani (K.Tani and Y.Suzuki, J.Chromatogr., 1996,722:129-13) and Yoshida (A.Yoshida, K.Takahashi, Chemitopia, 1994,15:18-29) having reported with the tetraisopropoxy titanium is the sol-gel method of raw material.The result shows that the titanium dioxide microballoon sphere aperture of these two kinds of method preparations is less, and size distribution very wide (2 ~ 50 microns), necessary classification during use, and chromatographic property is also undesirable.Chinese patent 00121097.1 has been reported a kind of polymerisation induced coacervation of colloid method, successfully synthesize the micron order titanium dioxide microballoon sphere of vesicular, narrow diameter distribution, stability better, but this method technology is complicated, long flow path, the titanium source cost height that uses, and a large amount of organic compositions have been used in the preparation process, as formaldehyde, polymeric alcohol etc., produce a large amount of organic waste water, cause environmental pollution.
Goal of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art; provide that a kind of to have nanostructure, narrow diameter distribution, chemical stability good, and technology is simple, technical process is short; with low cost, the preparation method of the titania microspheres of mesoporous structure of easy large-scale production.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of titania microspheres of mesoporous structure is characterized in that the step of its preparation process comprises:
(1) with concentration be the titanium sulfate solution of 0.1-0.5M and 0.4-1.2M be ammoniacal liquor or bicarbonate of ammonia or yellow soda ash alkaline sedimentation agent solution, in feed rate is 5-15mL/min, stirring velocity is at 600-1000 commentaries on classics/min, the pH value is under the 6-8 condition, feed simultaneously by in the churned mechanically flow reactor, carry out titanium ion precipitin reaction crystallization;
(2) throw out is filtered, washs, in air,, obtain the titanium dioxide microballoon sphere presoma in 60-80 ℃ of dry 10-12h;
(3) with the titanium dioxide microballoon sphere presoma at 500-700 ℃ of roasting temperature 1-3 hour, obtain the titania microspheres of mesoporous structure powder.
A kind of titania microspheres of mesoporous structure preparation method of the present invention is characterized in that described titanium sulfate solution is the waste liquid that Titanium White Production By Sulfuric Acid Process produced, and molecular formula is Ti
2(SO4)
3, mass content can commercially availablely obtain at 15%-40%.
The titanium dioxide microballoon sphere powder list that adopts the inventive method to make disperses, and spherical in shape or subsphaeroidal, particle diameter is at 10-20 μ m; Specific surface area reaches 120-136m
2/ g has TypeIV type adsorption isothermal line and the aperture that is distributed in 2 ~ 12nm, is typical mesoporous material; And titanium dioxide after heat treatment obtains pure anatase octahedrite phase easily; The specific surface area of this titanium dioxide microballoon sphere material Yin Qigao and meso-hole structure can be given full play to the activity of unit mass titanium dioxide, have better chemical stability, and the filler that can be used as liquid-phase chromatographic column uses.This microballoon has good settleability in the aqueous solution simultaneously, can be used as photocatalyst and uses.
The inventive method adopts control reactive crystallization-roasting method to prepare the titania microspheres of mesoporous structure powder, compares with existing titanium dioxide powder material preparation process, and technology, equipment is simple, with low cost, be easy to large-scale production.
Description of drawings
Fig. 1 is the meso-hole structure TiO of the embodiment of the invention 1
2The microballoon stereoscan photograph;
Fig. 2 is prepared TiO among the embodiment of the invention 1 and the embodiment 2
2Microballoon X-ray diffraction result;
Fig. 3 is the meso-hole structure TiO of the embodiment of the invention 1
2The nitrogen adsorption of microballoon-desorption curve;
Fig. 4 is the meso-hole structure TiO of the embodiment of the invention 1
2The pore size distribution curve of microballoon.
Embodiment
A kind of preparation method of titania microspheres of mesoporous structure, the step of its preparation process comprises:
(1) with the deionized water compound concentration be the technical grade titanium sulfate solution of 0.1-0.5M and 0.4-1.2M be ammoniacal liquor or bicarbonate of ammonia or yellow soda ash alkaline sedimentation agent solution, in feed rate is 5-15mL/min, stirring velocity is at 600-1000 commentaries on classics/min, the pH value is under the 6-8 condition, feed by in the churned mechanically flow reactor control titanium ion precipitin reaction crystallization simultaneously.
(2) continuous charging, reaction at room temperature filtered throw out, wash more than 48 hours, in 60-80 ℃ of dry 10-12h, promptly obtained the titanium dioxide microballoon sphere presoma in air.
(3) with the titanium dioxide microballoon sphere presoma in retort furnace in 500-700 ℃ of following roasting 1-3 hour, promptly obtain the titania microspheres of mesoporous structure powder.
The titanium dioxide microballoon sphere powder list that adopts the present invention to obtain disperses, and spherical in shape or subsphaeroidal, particle diameter is at 10-20 μ m, as Fig. 1; Specific surface area reaches 120-136m
2/ g has TypeIV type adsorption isothermal line and the aperture that is distributed in 2 ~ 12nm, for typical mesoporous material, and as Fig. 3,4; And titanium dioxide after heat treatment obtains pure anatase octahedrite phase, as Fig. 2.
1, be the technical grade titanium sulfate solution of 0.1M and the ammonium bicarbonate soln of 1.2M with the deionized water compound concentration, in feed rate is 10mL/min, and stirring velocity is at 600 commentaries on classics/min, and the pH value is under 6 conditions, feed by in the churned mechanically 5L plastic beaker control titanium ion precipitin reaction crystallization simultaneously.
2, continuous charging, reaction at room temperature is 48 hours, and throw out is filtered, washs, and in 80 ℃ of dry 12h, promptly obtains the titanium dioxide microballoon sphere presoma in air.
3, with the titanium dioxide microballoon sphere presoma in retort furnace in 500 ℃ of following roastings 3 hours, promptly obtain the titania microspheres of mesoporous structure powder.Prepared microballoon powder is seen accompanying drawing 1,2,3,4, and size distribution is at 10 ~ 20 μ m, and specific surface reaches 136m
2/ g has TypeIV type adsorption isothermal line and is distributed in the aperture of 2 ~ 12nm, and is pure anatase octahedrite phase.
1, be the technical grade titanium sulfate solution of 0.5M and the sodium carbonate solution of 1.0M with the deionized water compound concentration, in feed rate is 5mL/min, and stirring velocity is at 800 commentaries on classics/min, and the pH value is under 7 conditions, feed by in the churned mechanically 5L plastic beaker control titanium ion precipitin reaction crystallization simultaneously.
2, continuous charging, reaction at room temperature is 60 hours, and throw out is filtered, washs, and in 60 ℃ of dry 12h, promptly obtains the titanium dioxide microballoon sphere presoma in air.
3, with the titanium dioxide microballoon sphere presoma in retort furnace in 700 ℃ of following roastings 1 hour, promptly obtain the titania microspheres of mesoporous structure powder.Prepared microballoon diameter of particle is at 10 ~ 18 μ m, and specific surface reaches 120m
2/ g has TypeIV type adsorption isothermal line and is distributed in the aperture of 5 ~ 12nm, and is pure anatase octahedrite phase.
Embodiment 3
1, be the technical grade titanium sulfate solution of 0.2M and the ammonia soln of 0.4M with the deionized water compound concentration, in feed rate is 15mL/min, and stirring velocity is at 1000 commentaries on classics/min, and the pH value is under 8 conditions, feed by in the churned mechanically 5L glass beaker control titanium ion precipitin reaction crystallization simultaneously.
2, continuous charging, reaction at room temperature is 72 hours, and throw out is filtered, washs, and in 80 ℃ of dry 10h, promptly obtains the titanium dioxide microballoon sphere presoma in air.
3, with the titanium dioxide microballoon sphere presoma in retort furnace in 700 ℃ of following roastings 2 hours, promptly obtain the titania microspheres of mesoporous structure powder.Prepared microballoon diameter of particle is at 11 ~ 20 μ m, and specific surface reaches 134m
2/ g has TypeIV type adsorption isothermal line and is distributed in the aperture of 2 ~ 8nm, and is pure anatase octahedrite phase.
Claims (2)
1. the preparation method of a titania microspheres of mesoporous structure is characterized in that the step of its preparation process comprises:
(1) with concentration be the titanium sulfate solution of 0.1-0.5M and 0.4-1.2M be ammoniacal liquor or bicarbonate of ammonia or yellow soda ash alkaline sedimentation agent solution, in feed rate is 5-15mL/min, stirring velocity is at 600-1000 commentaries on classics/min, the pH value is under the 6-8 condition, feed simultaneously by in the churned mechanically flow reactor, carry out titanium ion precipitin reaction crystallization;
(2) throw out is filtered, washs, in air,, obtain the titanium dioxide microballoon sphere presoma in 60-80 ℃ of dry 10-12h;
(3) with the titanium dioxide microballoon sphere presoma at 500-700 ℃ of roasting temperature 1-3 hour, obtain the titania microspheres of mesoporous structure powder.
2. a kind of titania microspheres of mesoporous structure preparation method according to claim 1 is characterized in that described titanium sulfate solution is the waste liquid that Titanium White Production By Sulfuric Acid Process produced, and molecular formula is Ti
2(SO4)
3, mass content is at 15%-40%.
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| CNA2008101154444A CN101333004A (en) | 2008-06-24 | 2008-06-24 | Process for preparing titania microspheres of mesoporous structure |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101958415A (en) * | 2010-08-20 | 2011-01-26 | 华南师范大学 | Power lithium ion battery titanium dioxide microsphere cathode material and preparation method thereof |
| CN102491415A (en) * | 2011-12-02 | 2012-06-13 | 西安电子科技大学 | Preparation method of monodispersed anatase titanium dioxide nano porous microspheres |
| CN107662942A (en) * | 2017-10-30 | 2018-02-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Nano-TiO2Preparation method |
| CN108686635A (en) * | 2018-05-09 | 2018-10-23 | 南通龙翔新材料科技股份有限公司 | A kind of titanium dioxide loaded ruthenium catalyst and preparation method thereof |
| CN111089759A (en) * | 2019-12-29 | 2020-05-01 | 南通欧萨环境检测技术有限公司 | Automobile exhaust collecting and detecting method |
| CN114425330A (en) * | 2022-01-14 | 2022-05-03 | 山东大学 | Double-noble-metal-loaded nano titanium dioxide and preparation method and application thereof |
| CN116102056A (en) * | 2022-11-16 | 2023-05-12 | 攀枝花学院 | Superfine titanium dioxide powder and preparation method thereof |
-
2008
- 2008-06-24 CN CNA2008101154444A patent/CN101333004A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101958415A (en) * | 2010-08-20 | 2011-01-26 | 华南师范大学 | Power lithium ion battery titanium dioxide microsphere cathode material and preparation method thereof |
| CN101958415B (en) * | 2010-08-20 | 2012-11-14 | 华南师范大学 | Power lithium ion battery titanium dioxide microsphere cathode material and preparation method thereof |
| CN102491415A (en) * | 2011-12-02 | 2012-06-13 | 西安电子科技大学 | Preparation method of monodispersed anatase titanium dioxide nano porous microspheres |
| CN107662942A (en) * | 2017-10-30 | 2018-02-06 | 攀钢集团攀枝花钢铁研究院有限公司 | Nano-TiO2Preparation method |
| CN108686635A (en) * | 2018-05-09 | 2018-10-23 | 南通龙翔新材料科技股份有限公司 | A kind of titanium dioxide loaded ruthenium catalyst and preparation method thereof |
| CN108686635B (en) * | 2018-05-09 | 2019-08-06 | 南通龙翔新材料科技股份有限公司 | A kind of titanium dioxide loaded ruthenium catalyst and preparation method thereof |
| CN111089759A (en) * | 2019-12-29 | 2020-05-01 | 南通欧萨环境检测技术有限公司 | Automobile exhaust collecting and detecting method |
| CN114425330A (en) * | 2022-01-14 | 2022-05-03 | 山东大学 | Double-noble-metal-loaded nano titanium dioxide and preparation method and application thereof |
| CN116102056A (en) * | 2022-11-16 | 2023-05-12 | 攀枝花学院 | Superfine titanium dioxide powder and preparation method thereof |
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Open date: 20081231 |