CN105964235B - A kind of preparation method of poriferous titanium dioxide-silica bulk - Google Patents
A kind of preparation method of poriferous titanium dioxide-silica bulk Download PDFInfo
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- CN105964235B CN105964235B CN201610293407.7A CN201610293407A CN105964235B CN 105964235 B CN105964235 B CN 105964235B CN 201610293407 A CN201610293407 A CN 201610293407A CN 105964235 B CN105964235 B CN 105964235B
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- titanium dioxide
- poriferous titanium
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- silica bulk
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000010936 titanium Substances 0.000 title claims description 33
- 229910052719 titanium Inorganic materials 0.000 title claims description 28
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 23
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001879 gelation Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 229960001484 edetic acid Drugs 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 125000003158 alcohol group Chemical group 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004408 titanium dioxide Substances 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 229960003511 macrogol Drugs 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- TZBAVQKIEKDGFH-UHFFFAOYSA-N n-[2-(diethylamino)ethyl]-1-benzothiophene-2-carboxamide;hydrochloride Chemical compound [Cl-].C1=CC=C2SC(C(=O)NCC[NH+](CC)CC)=CC2=C1 TZBAVQKIEKDGFH-UHFFFAOYSA-N 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910003978 SiClx Inorganic materials 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon ion Chemical class 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- 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
- B01J21/08—Silica
-
- B01J35/40—
-
- B01J35/651—
-
- B01J35/653—
Abstract
The invention discloses a kind of preparation methods of poriferous titanium dioxide silica bulk, using butyl titanate, ethyl orthosilicate as raw material, it is added into respectively in the absolute ethyl alcohol containing specific dispersant and the mixed solution of deionized water, by containing butyl titanate solution carry out water-bath formed semigel state when after, teos solution is added thereto, it is stirred to react to gelation, gained powder body material direct pressing molding after will be dry, then can be obtained poriferous titanium dioxide silica bulk through sintering.This method technique has the characteristics that equipment is simple, the period is short, at low cost.
Description
Technical field
The invention belongs to field of material technology, more particularly to the preparation side of a kind of poriferous titanium dioxide-silica bulk
Method.
Background technology
Nano-titanium dioxide-silicon dioxide composite material is a kind of efficient photochemical catalyst, in air purification, organic matter
The fields such as degradation have a wide range of applications.Influence the photocatalysis of nano-titanium dioxide-silicon dioxide composite powder material
The principal element of performance includes morphology microstructure, grain size, crystalline phase composition and degree of scatter, titania-silica composite granule
The reduction of material particle size, surface-active is bigger, and photocatalytic activity is bigger.But the increase of specific surface area easily causes titanium dioxide
The agglomeration of titanium-silica composite nano powder, the photocatalysis effect of titania-silica composite granule also by
To limitation.Poriferous titanium dioxide-silica bulk is synthesized, sufficiently fine trepanning composition can keep nano-titanium dioxide-two
The efficient catalytic of silica composite material, this method efficiently solve the agglomeration traits of composite nano-powder material.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of poriferous titanium dioxide-dioxies
The preparation method of SiClx bulk has the characteristics that simple production process, equipment requirement are simple, the period is short.
To achieve the goals above, the technical solution adopted by the present invention is：
A kind of preparation method of poriferous titanium dioxide-silica bulk, includes the following steps：
(1) it is 1 in volume ratio：In 2~3 absolute ethyl alcohol and the mixed liquor of deionized water, dispersant stirring and dissolving is added
Form solution A；
(2) it is spare to be dissolved in wherein formation solution B by the solution A for taking 1/5 for ethyl orthosilicate；Butyl titanate is dissolved in residue
Solution C is formed in solution A, adjusting the pH value of solution C with ammonium hydroxide obtains colloidal sol C to 5~7；
(3) by colloidal sol C at 80~85 DEG C 20~30min of water-bath, solution B is added thereto under constant stirring, continue
In this water bath condition down toward gelation, then drying forms xerogel at 140~160 DEG C, is ground after natural drying at room temperature
Honed sieve obtains xerogel powder；
(4) dry powder after sieving is directly dry-pressing formed, blocky blank of material is formed, finally carries out blocky blank of material
It is thermally treated resulting in poriferous titanium dioxide-silica bulk.
In the step (1), the dispersant is by ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, winestone
Acid, ethylene glycol and polyethylene glycol form, and in solution A, the concentration range of dispersant each component is 0~0.5mol/L.
In the step (2), the molar ratio of Si and Ti are 1：(4~8), and the sum of Si ions and Ti ions and citric acid
Molar ratio is 1：(0.5~1).
In the step (4), the heat treatment is to carry out burying burning in ZnO powders, and temperature is 700~900 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：Poriferous titanium dioxide-silica provided by the invention
In the preparation method of bulk, with ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, poly- second two
Alcohol (such as polyethylene glycol 400, Macrogol 4000, Macrogol 6000) directly carries out the gel of complexing foaming as dispersant
Change process, by controlling the concentration of each substance, the dosage of especially each dispersant, being formed by intermediate powder substance after dry can
Straight forming is at bulk material, in this preparation method, so that titanium ion and silicon ion is equably existed merely with dispersant
In system, keep the crystallization of poriferous titanium dioxide-silica bulk and recombination process more uniform, and reduces and be granulated, is old
Rotten process makes crystallization process be completed with one step of sintering, this all makes manufacturing cycle shorten, cost reduction.At the heat for burying burning
Reason process forms poriferous titanium dioxide-silica bulk using the foaming of organic matter and decomposition combustion process, can get and open
The poriferous titanium dioxide in hole-silica bulk.
Specific implementation mode
With reference to the embodiment embodiment that the present invention will be described in detail.
Embodiment 1
A kind of preparation method of poriferous titanium dioxide-silica bulk, includes the following steps：
(1) mixed liquor (V of 50mL absolute ethyl alcohols and deionized water is measuredAbsolute ethyl alcohol：VDeionized water=1：2) it, weighs a certain amount of
Dispersant (it is made of ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol, wherein
Polyethylene glycol includes polyethylene glycol 400, Macrogol 4000 and Macrogol 6000 again) it is added thereto, stirring and dissolving forms molten
The concentration of liquid A, dispersant each component are controlled in 0.5mol/L.
(2) it is spare to be dissolved in wherein formation solution B by the solution A for measuring 1/5 for ethyl orthosilicate；Butyl titanate is dissolved in surplus
Solution C is formed in remaining solution A, wherein Si：Ti (molar ratio)=1：4, ion：Citric acid (molar ratio)=1：0.5.Use ammonium hydroxide
(volumetric concentration 25~28%) adjusts pH value to 5~7 i.e. acquisition colloidal sol C.
(3) by colloidal sol C at 85 DEG C 20~30min of water-bath, solution B is added thereto under constant stirring, continue herein
Water bath condition is down toward gelation.Drying forms xerogel at 140 DEG C again, is at room temperature after natural drying ground powder
Sieve.
(4) the direct dry pressing of dry powder after sieving is formed into blocky blank of material, finally by blocky blank of material in ZnO
It carries out burying burning in powder, that is, obtains poriferous titanium dioxide-silica block materials, heat treatment temperature is 900 DEG C.Institute is much
Be open-celled structure in porous titanium dioxide-silica bulk, crystallite dimension is about 50nm~400nm, gap size be 50nm~
200nm。
Embodiment 2
A kind of preparation method of poriferous titanium dioxide-silica bulk, includes the following steps：
(1) mixed liquor (V of 50mL absolute ethyl alcohols and deionized water is measuredAbsolute ethyl alcohol：VDeionized water=1：3) it, weighs a certain amount of
Dispersant (being made of ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol) is added
Wherein, stirring and dissolving forms solution A, and the concentration of dispersant each component is controlled in 0.5mol/L.
(2) it is spare to be dissolved in wherein formation solution B by the solution A for measuring 1/5 for ethyl orthosilicate；Butyl titanate is dissolved in surplus
Solution C is formed in remaining solution A, wherein Si：Ti (molar ratio)=1：8, ion：Citric acid (molar ratio)=1：1.With ammonium hydroxide (body
Product concentration 25~28%) pH value is adjusted to 5~7 i.e. acquisition colloidal sol C.
(3) by colloidal sol C at 80 DEG C 20~30min of water-bath, solution B is added thereto under constant stirring, continue herein
Water bath condition is down toward gelation.Drying forms xerogel at 160 DEG C again, is at room temperature after natural drying ground powder
Sieve.
(4) by the direct dry pressing of dry powder after sieving, blocky blank of material is formed, finally blocky blank of material exists
It carries out burying burning i.e. acquisition poriferous titanium dioxide-silica block materials in ZnO powders, heat treatment temperature is 700 DEG C.Gained
It is open-celled structure in poriferous titanium dioxide-silica bulk, crystallite dimension is about 50nm~400nm, gap size 50nm
~200nm.
Embodiment 3
A kind of preparation method of poriferous titanium dioxide-silica bulk, includes the following steps：
(1) mixed liquor (V of 50mL absolute ethyl alcohols and deionized water is measuredAbsolute ethyl alcohol：VDeionized water=1：2) it, weighs a certain amount of
Dispersant (being made of ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol) is added
Wherein, stirring and dissolving forms solution A, the concentration control of dispersant each component 0.01,0.12,0.11,0.15,0.33,
0.5mol/L。
(2) it is spare to be dissolved in wherein formation solution B by the solution A for measuring 1/5 for ethyl orthosilicate；Butyl titanate is dissolved in surplus
Solution C is formed in remaining solution A, wherein Si：Ti (molar ratio)=1：6, ion：Citric acid (molar ratio)=1：0.6.Use ammonium hydroxide
(volumetric concentration 25~28%) adjusts pH value to 5~7 i.e. acquisition colloidal sol C.
(3) by colloidal sol C at 85 DEG C 20~30min of water-bath, solution B is added thereto under constant stirring, continue herein
Water bath condition is down toward gelation.Drying forms xerogel at 150 DEG C again, is at room temperature after natural drying ground powder
Sieve.
(4) by the direct dry pressing of dry powder after sieving, blocky blank of material is formed, finally blocky blank of material exists
It carries out burying burning i.e. acquisition poriferous titanium dioxide-silica block materials in ZnO powders, heat treatment temperature is 800 DEG C.Gained
It is open-celled structure in poriferous titanium dioxide-silica bulk, crystallite dimension is about 50nm~400nm, gap size 50nm
~200nm.
Claims (3)
1. a kind of preparation method of poriferous titanium dioxide-silica bulk, which is characterized in that include the following steps：
(1) it is 1 in volume ratio：In 2~3 absolute ethyl alcohol and the mixed liquor of deionized water, dispersant stirring and dissolving is added and is formed
Solution A, the dispersant is by ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and poly- second two
Alcohol forms, and the concentration range of dispersant each component is 0~0.5mol/L and cannot take 0；
(2) it is spare to be dissolved in wherein formation solution B by the solution A for taking 1/5 for ethyl orthosilicate；Butyl titanate is dissolved in surplus solution A
Middle formation solution C adjusts the pH value of solution C with ammonium hydroxide and obtains colloidal sol C to 5~7；
(3) by colloidal sol C at 80~85 DEG C 20~30min of water-bath, solution B is added thereto under constant stirring, continue herein
Water bath condition is down toward gelation, then drying forms xerogel at 140~160 DEG C, is ground after natural drying at room temperature
Sieve obtains xerogel powder；
(4) dry powder after sieving is directly dry-pressing formed, blocky blank of material is formed, blocky blank of material is finally subjected to hot place
Reason obtains poriferous titanium dioxide-silica bulk.
2. the preparation method of poriferous titanium dioxide-silica bulk according to claim 1, which is characterized in that the step
Suddenly in (2), the molar ratio of Si and Ti are 1：(4~8), and the molar ratio of the sum of Si ions and Ti ions and citric acid is 1：(0.5
~1).
3. the preparation method of poriferous titanium dioxide-silica bulk according to claim 1, which is characterized in that the step
Suddenly in (4), the heat treatment is to carry out burying burning in ZnO powders, and temperature is 700~900 DEG C.
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|---|---|---|---|---|
| CN101891974A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite powder |
| CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
| CN101891206A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Preparation method of SiO2/TiO2 composite microspheres |
| CN101890326A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite microspheres |
| CN104003411A (en) * | 2014-05-16 | 2014-08-27 | 北京科技大学 | Preparation method of lithium silicate porous material used for absorption of high temperature CO2 |
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2016
- 2016-05-05 CN CN201610293407.7A patent/CN105964235B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891974A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite powder |
| CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
| CN101891206A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Preparation method of SiO2/TiO2 composite microspheres |
| CN101890326A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite microspheres |
| CN104003411A (en) * | 2014-05-16 | 2014-08-27 | 北京科技大学 | Preparation method of lithium silicate porous material used for absorption of high temperature CO2 |
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