CN103706348A - Composite TiO2-SiO2 aerogel and application thereof - Google Patents
Composite TiO2-SiO2 aerogel and application thereof Download PDFInfo
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- CN103706348A CN103706348A CN201310738831.4A CN201310738831A CN103706348A CN 103706348 A CN103706348 A CN 103706348A CN 201310738831 A CN201310738831 A CN 201310738831A CN 103706348 A CN103706348 A CN 103706348A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 229910003082 TiO2-SiO2 Inorganic materials 0.000 title abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 235000019441 ethanol Nutrition 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000002360 explosive Substances 0.000 claims abstract description 6
- 239000002351 wastewater Substances 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 41
- 239000011240 wet gel Substances 0.000 claims description 23
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 19
- 150000001875 compounds Chemical class 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000010936 titanium Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- 238000013022 venting Methods 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 8
- 229910052681 coesite Inorganic materials 0.000 abstract 4
- 229910052906 cristobalite Inorganic materials 0.000 abstract 4
- 239000000377 silicon dioxide Substances 0.000 abstract 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract 4
- 229910052682 stishovite Inorganic materials 0.000 abstract 4
- 229910052905 tridymite Inorganic materials 0.000 abstract 4
- 230000000593 degrading effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000000352 supercritical drying Methods 0.000 abstract 1
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 16
- 239000000015 trinitrotoluene Substances 0.000 description 16
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 238000001354 calcination Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
The invention provides composite TiO2-SiO2 aerogel and an application thereof. The aerogel material has the adsorption performance of SiO2 and the photocatalytic performance of TiO2. A preparation method for the composite TiO2-SiO2 aerogel comprises the following steps of 1, preparing SiO2 sol; 2, preparing TiO2 sol; 3, dropping the SiO2 sol into the TiO2 sol, uniformly stirring the SiO2 sol and the TiO2 sol, standing the sol under room temperature until the sol is condensed, aging the sol mixture through anhydrous ethanol for multiple days, and performing supercritical drying through ethyl alcohol. The preparation technology for the TiO2-SiO2 aerogel is simple; the composite TiO2-SiO2 aerogel has an extremely good effect of degrading explosive powder wastewater.
Description
Technical field
The invention belongs to photocatalytic degradation field, relate to a kind of TiO
2-SiO
2composite aerogel and application thereof.
Background technology
Chemical organic compounds has become to the pollution problem of water resource the key problem that current improvement water pollutes.In process of production, the various waste water that produce, contain a large amount of poisonous and hazardous chemical organic pollutions to fire explosive, and environment and the mankind are had to immeasurable harm.Chemical organic pollution in fire explosive waste water is stable chemical nature mostly, and more difficult decomposition, has limited the use of many method for treating water to a certain extent.
In recent years, with TiO
2photochemical catalyst for representative, is having good application prospect aspect the photocatalytic degradation of chemical organic pollution.But, due to nano-TiO
2there is the problems such as easily gathering, easy inactivation, more difficult recovery and reuse in powder, so recent domestic is all being carried out TiO
2the load study of powder.For load TiO
2the carrier of powder has glass microballoon, active carbon, zeolite, natural minerals, SiO
2in adsorbent class carrier, the advantage of such carrier is that this is as porous material, strong adhesion, specific area are large, microcellular structure is abundant, has good performance during as catalyst carrier.
Summary of the invention
The object of the invention is to provide in order to improve the deficiencies in the prior art a kind of TiO
2-SiO
2composite aerogel, another object of the present invention is to provide above-mentioned TiO
2-SiO
2the application of composite aerogel in photocatalytic degradation fire explosive waste water.
Technical scheme of the present invention is: a kind of TiO
2-SiO
2composite aerogel, is characterized in that being prepared by following methods, and its concrete preparation process is as follows:
(1) SiO
2the preparation of colloidal sol
By silicon source, absolute ethyl alcohol, deionized water by volume 1: ﹙ 1.3～1.6 ﹚: ﹙ 0.2～0.5 ﹚ evenly mixes, adding acid-conditioning solution pH value is 3～5, at 30～50 ℃, is hydrolyzed 3.5～4.5h, constantly stirs and makes SiO
2colloidal sol;
(2) TiO
2the preparation of colloidal sol
By titanium source and absolute ethyl alcohol by volume 1: ﹙ 2～3 ﹚ evenly mix, adding acid-conditioning solution pH value is 3～5, obtain solution A, by absolute ethyl alcohol and deionized water by volume 4～5:1 evenly mix, adding acid-conditioning solution pH value is 3～5, obtains solution B, under stirring, solution B is added drop-wise in solution A, the volume ratio of solution A and solution B is 4～5:1, at 30～50 ℃, is hydrolyzed 0.5～1h, constantly stirs and makes TiO
2colloidal sol;
(3) TiO
2-SiO
2the preparation of compound wet gel
Under stirring, by (Si), be 1:(1～8 with (Ti) mol ratio) by SiO
2colloidal sol is added drop-wise to TiO
2in colloidal sol, after stirring, take out, standing to condensing at 30～50 ℃, obtain TiO
2-SiO
2compound wet gel;
(4) TiO
2-SiO
2compound wet gel aging
By TiO
2-SiO
2compound wet gel, at 50～80 ℃, carries out solvent exchange with ethanol solution, replaces 6～8 days;
(5) TiO
2-SiO
2being dried of compound wet gel
By TiO
2-SiO
2compound wet gel is dried with ethanol is overcritical, obtains TiO
2-SiO
2composite aerogel.This composite aerogel had both had SiO
2absorption property, there is again TiO
2photocatalysis performance,
Silicon source described in preferred steps (1) be in tetraethyl orthosilicate, waterglass or Ludox any; In step (1), acid used is HCl or HNO
3in any, acid concentration be 1mol/L～3mol/L.
Titanium source described in preferred steps (2) be in butyl titanate, titanium tetrachloride any; HCl or HNO that in step (2), acid used is 1mol/L～3mol/L
3in any.
Preferred steps (2) is added drop-wise to solution A neutralization procedure (3) by SiO by solution B
2colloidal sol is added drop-wise to TiO
2rate of addition in colloidal sol is 0.3ml/s～0.6ml/s, in order to avoid mix inhomogeneous.
In step (5), by TiO
2-SiO
2when compound wet gel is dried with ethanol is overcritical, preferably baking temperature is 260～280 ℃, and pressure is 10～12MPa, maintains 2～3 hours under constant temperature and pressure state, and then sample is taken out in venting.
The present invention also provides above-mentioned TiO
2-SiO
2the application of composite aerogel in photocatalytic degradation fire explosive waste water, as trinitrotoluene (TNT), hexogen, HMX etc., the more preferably application aspect degraded TNT.
Beneficial effect:
Feature with TiO2-SiO2 composite aerogel photocatalytic degradation TNT of the present invention is:
(1) high to the degradation rate of TNT: test shows, photocatalytic degradation TNT solution 2.5h, degradation rate reaches 98.51%.
(2) catalyst can reuse.
Accompanying drawing explanation
Fig. 1 figure that affects on TNT degradation rate in solution that is TiO2-SiO2 composite aerogel A1 with the difference of initial concentration solution;
Fig. 2 figure that affects on TNT degradation rate in solution that is TiO2-SiO2 composite aerogel A2 with the difference of calcining heat;
Fig. 3 figure that affects on TNT degradation rate in solution that is TiO2-SiO2 composite aerogel A3 with the difference of degradation time.
The specific embodiment
Below in conjunction with embodiment, the invention will be further described, but the protection domain of invention is not limit therewith.
The preparation of 1.TiO2-SiO2 composite aerogel
Example 1 by tetraethyl orthosilicate, absolute ethyl alcohol, deionized water by volume 1:1.32:0.21 evenly mix, use 1.2mol/L HNO
3regulator solution pH value is 3.2, at 33 ℃, is hydrolyzed 3.5h, constantly stirs and makes SiO
2colloidal sol; By butyl titanate and absolute ethyl alcohol by volume 1:2.3 evenly mix, use 1.2mol/L HNO
3regulator solution pH value is 3.1, obtains solution A, by absolute ethyl alcohol and deionized water by volume 4.2:1 evenly mix, use 1.2mol/L HNO
3regulator solution pH value is 3.1, obtains solution B, and the speed with 0.3ml/s under stirring is added drop-wise to solution B in solution A, and the volume ratio of solution A and solution B is 4.2:1, at 33 ℃, is hydrolyzed 0.5h, constantly stirs and makes TiO
2colloidal sol; Under stirring, by n (Si): n (Ti)=1:1, with the speed of 0.3ml/s by SiO
2colloidal sol is added drop-wise to TiO
2in colloidal sol, after stirring, take out, standing to condensing at 33 ℃, obtain the compound wet gel of TiO2-SiO2.The compound wet gel of TiO2-SiO2, at 55 ℃, is carried out to solvent exchange with ethanol solution, replace 6 days; The compound wet gel of TiO2-SiO2 is dried to processing with ethanol is overcritical, and baking temperature is 260 ℃, and pressure is 10MPa, under constant temperature and pressure state, maintains 2 hours, and then venting obtains TiO2-SiO2 composite aerogel, is labeled as A1.
Fig. 1 is that to take 0.1g calcining heat be the beaker that the A1 of 700 ℃ puts into 100ml, then add 50ml, the TNT solution to be degraded of 30mg/L, 50mg/L, 80mg/L, 110mg/L, 150mg/L, 2.5h degrades under the condition of ultraviolet light, the impact effect figure of the initial concentration of comparison different solutions to TNT Photocatalytic Degradation Property, from scheming, can find out that initial concentration solution is 50mg/L, degradation rate is the highest.
Example 2 by waterglass, absolute ethyl alcohol, deionized water by volume 1:1.45:0.36 evenly mix, use 2.3mol/LHNO
3regulator solution pH value is 4, at 40 ℃, is hydrolyzed 4h, constantly stirs and makes SiO
2colloidal sol; By butyl titanate and absolute ethyl alcohol by volume 1:2.6 evenly mix, use 2.3mol/L HNO
3regulator solution pH value is 4.2, obtains solution A, by absolute ethyl alcohol and deionized water by volume 4.5:1 evenly mix, use 2.3mol/L HNO
3regulator solution pH value is 4.1, obtains solution B, and the speed with 0.45ml/s under stirring is added drop-wise to solution B in solution A, and the volume ratio of solution A and solution B is 4.5:1, at 40 ℃, is hydrolyzed 0.7h, constantly stirs and makes TiO
2colloidal sol; Under stirring, by n (Si): n (Ti)=1:5, with the speed of 0.45ml/s by SiO
2colloidal sol is added drop-wise to TiO
2in colloidal sol, after stirring, take out, standing to condensing at 40 ℃, obtain the compound wet gel of TiO2-SiO2.The compound wet gel of TiO2-SiO2, at 65 ℃, is carried out to solvent exchange with ethanol solution, replace 7 days; The compound wet gel of TiO2-SiO2 is dried to processing with ethanol is overcritical, and baking temperature is 268 ℃, and pressure is 11MPa, under constant temperature and pressure state, maintains 2.5 hours, and then venting obtains TiO2-SiO2 composite aerogel, is labeled as A2.
Fig. 2 takes the beaker that A2 that 0.1g calcining heat is respectively 500 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃ puts into 100ml, then add 50ml, the TNT solution to be degraded of 50mg/L, 2.5h degrades under the condition of ultraviolet light, the impact effect figure of more different calcining heats to TNT Photocatalytic Degradation Property, from scheming, can find out that TiO2-SiO2 composite aerogel is best to the Photocatalytic Degradation Property of TNT when calcining heat is 700 ℃.
Example 3 by Ludox, absolute ethyl alcohol, deionized water by volume 1:1.59:0.5 evenly mix, by 3mol/L HCl regulator solution pH value, be 4.8, at 48 ℃, be hydrolyzed 4.5h, constantly stir and make SiO
2colloidal sol; By titanium tetrachloride and absolute ethyl alcohol by volume 1:2.9 evenly mix, by 3mol/L HCl regulator solution pH value, be 4.8, obtain solution A, by absolute ethyl alcohol and deionized water by volume 4.9:1 evenly mix, by 3mol/L HCl regulator solution pH value, be 4.8, obtain solution B, speed with 0.6ml/s under stirring is added drop-wise to solution B in solution A, the volume ratio of solution A and solution B is 4.9:1, at 50 ℃, is hydrolyzed 1h, constantly stirs and makes TiO
2colloidal sol; Under stirring, by n (Si): n (Ti)=1:8, with the speed of 0.6ml/s by SiO
2colloidal sol is added drop-wise to TiO
2in colloidal sol, after stirring, take out, standing to condensing at 50 ℃, obtain the compound wet gel of TiO2-SiO2.The compound wet gel of TiO2-SiO2, at 80 ℃, is carried out to solvent exchange with ethanol solution, replace 8 days; The compound wet gel of TiO2-SiO2 is dried to processing with ethanol is overcritical, and baking temperature is 280 ℃, and pressure is 12MPa, under constant temperature and pressure state, maintains 3 hours, and then venting obtains TiO2-SiO2 composite aerogel, is labeled as A3.
Fig. 3 is that to take 0.1g calcining heat be the beaker that the A3 of 700 ℃ puts into 100ml, then add 50ml, the TNT solution to be degraded of 50mg/L, 15min, 30min, 60min, 120min, 150min, 180min degrade respectively under the condition of ultraviolet light, the impact effect figure of more different photocatalytic degradation time to TNT degradation property, from scheming, can find out that degradation rate no longer changes after photocatalytic degradation 2.5h, now reaches maximum.
Claims (6)
1. a TiO
2-SiO
2composite aerogel, is characterized in that being prepared by following methods, and its concrete preparation process is as follows:
(1) SiO
2the preparation of colloidal sol
By silicon source, absolute ethyl alcohol, deionized water by volume 1: ﹙ 1.3～1.6 ﹚: ﹙ 0.2～0.5 ﹚ evenly mixes, adding acid-conditioning solution pH value is 3～5, at 30～50 ℃, is hydrolyzed 3.5～4.5h, constantly stirs and makes SiO
2colloidal sol;
(2) TiO
2the preparation of colloidal sol
By titanium source and absolute ethyl alcohol by volume 1: ﹙ 2～3 ﹚ evenly mix, adding acid-conditioning solution pH value is 3～5, obtain solution A, by absolute ethyl alcohol and deionized water by volume 4～5:1 evenly mix, adding acid-conditioning solution pH value is 3～5, obtains solution B, under stirring, solution B is added drop-wise in solution A, the volume ratio of solution A and solution B is 4～5:1, at 30～50 ℃, is hydrolyzed 0.5～1h, constantly stirs and makes TiO
2colloidal sol;
(3) TiO
2-SiO
2the preparation of compound wet gel
Under stirring, by (Si), be 1:(1～8 with (Ti) mol ratio) by SiO
2colloidal sol is added drop-wise to TiO
2in colloidal sol, after stirring, take out, standing to condensing at 30～50 ℃, obtain TiO
2-SiO
2compound wet gel;
(4) TiO
2-SiO
2compound wet gel aging
By TiO
2-SiO
2compound wet gel, at 50～80 ℃, carries out solvent exchange with ethanol solution, replaces 6～8 days;
(5) TiO
2-SiO
2being dried of compound wet gel
By TiO
2-SiO
2compound wet gel is dried with ethanol is overcritical, obtains TiO
2-SiO
2composite aerogel.
2. TiO according to claim 1
2-SiO
2composite aerogel, it is characterized in that silicon source described in step (1) be in tetraethyl orthosilicate, waterglass or Ludox any; In step (1), acid used is HCl or HNO
3in any, acid concentration be 1mol/L～3mol/L.
3. TiO according to claim 1
2-SiO
2composite aerogel, it is characterized in that titanium source described in step (2) be in butyl titanate, titanium tetrachloride any; HCl or HNO that in step (2), acid used is 1mol/L～3mol/L
3in any.
4. TiO according to claim 1
2-SiO
2composite aerogel, is characterized in that step (2) is added drop-wise to solution A neutralization procedure (3) by SiO by solution B
2colloidal sol is added drop-wise to TiO
2rate of addition in colloidal sol is 0.3ml/s～0.6ml/s.
5. TiO according to claim 1
2-SiO
2composite aerogel, is characterized in that in step (5), by TiO
2-SiO
2when compound wet gel is dried with ethanol is overcritical, baking temperature is 260～280 ℃, and pressure is 10～12MPa, maintains 2～3 hours under constant temperature and pressure state, and then sample is taken out in venting.
6. a TiO as claimed in claim 1
2-SiO
2the application of composite aerogel in photocatalytic degradation fire explosive waste water.
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