CN108940143A - A kind of pigment is the preparation method and applications of the titanium silica aerogel of template - Google Patents
A kind of pigment is the preparation method and applications of the titanium silica aerogel of template Download PDFInfo
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- CN108940143A CN108940143A CN201811147389.7A CN201811147389A CN108940143A CN 108940143 A CN108940143 A CN 108940143A CN 201811147389 A CN201811147389 A CN 201811147389A CN 108940143 A CN108940143 A CN 108940143A
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- silica aerogel
- titanium
- titanium silica
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 59
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000010936 titanium Substances 0.000 title claims abstract description 55
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 55
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 54
- 239000000049 pigment Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000005516 engineering process Methods 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 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 239000000428 dust Substances 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000013019 agitation Methods 0.000 claims abstract description 6
- 239000010453 quartz Substances 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 0.000 claims abstract description 3
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims description 40
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 claims description 29
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 235000012754 curcumin Nutrition 0.000 claims description 20
- 239000004148 curcumin Substances 0.000 claims description 20
- 229940109262 curcumin Drugs 0.000 claims description 20
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 claims description 20
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 19
- 244000017020 Ipomoea batatas Species 0.000 claims description 17
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000011282 treatment Methods 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims 1
- 125000004494 ethyl ester group Chemical group 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 39
- 230000009467 reduction Effects 0.000 abstract description 12
- 238000001816 cooling Methods 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 31
- 238000010531 catalytic reduction reaction Methods 0.000 description 24
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical group [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 18
- 239000000463 material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- 230000000694 effects Effects 0.000 description 11
- 238000006722 reduction reaction Methods 0.000 description 11
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 9
- 229910052804 chromium Inorganic materials 0.000 description 8
- 239000004964 aerogel Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 4
- 238000007540 photo-reduction reaction Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 239000001055 blue pigment Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 230000007704 transition Effects 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation method and applications for the titanium silica aerogel that pigment is template, by a certain amount of pigmentolysis, ultrasound to pigment is completely dissolved in a solvent first, then tetraethyl orthosilicate is added, after stirring one hour, solvent, butyl titanate, dust technology and distilled water are successively added dropwise again, constant agitation speed is stirred to solution at colloidal sol, after standing aging into gel, high-temperature high-voltage reaction in quartz reaction kettle liner is placed in for a period of time, to be taken out after cooling up to target product.The present invention all has photocatalytic activity under visible light and simulated solar irradiation irradiation using pigment as the titanium silica aerogel of template, has good reduction to Cr VI in water body.
Description
Technical field
The invention belongs to the preparation technical fields of nano structural material, and in particular to a kind of pigment is the titanium silicon airsetting of template
The preparation method and applications of glue.
Background technique
In nature, the compound of chromium and chromium is a kind of important industrial chemicals, has been widely used in chemical industry, system
Medicine is printed and dyed, plating, process hides, the industries such as coating.With the increase industrially to chromium and compound demand, make the life of chromic salts
Yield is gradually increased, and chromate waste water, exhaust gas, the waste residue generated in industrial production is unprocessed to be just arbitrarily discharged into natural environment
In, environment can be caused and its serious pollution, wherein the discharge of wastewater of the industry containing chromium is the main way of chromium diffusion mobility
Diameter.Now, China part surface water, underground water have been subjected to different degrees of pollution of chromium.
Currently, the method for removing Cr VI in water body mainly has: chemical method (such as reduction method, the precipitation method), physics
Chemical method (such as membrane filter method, ion-exchange, absorption method), bioanalysis and photo-reduction, the original of photo-reduction
Reason main process is exactly: being added into water sample by photochemical catalyst (such as TiO2), under the irradiation of specific light source, catalyst generates electricity
Sub- transition forms electrons and holes to rear, generates free radicals with water, by hexavalent chrome reduction is trivalent chromium by illumination.It is other normal
The processing method of Cr VI is compared with photo-reduction in water body, photo-reduction have it is environmentally protective,
Free of contamination feature is a more popular in recent years advanced technology.If can be the absorbing wavelength of photochemical catalyst from ultraviolet
Increase to visible region, can directly utilize sunlight, the application prospect of photochemical catalyst can be more wide.
Aeroge is a kind of solid material with multifrequency nature, it has the characteristics that loose porous, and porosity can be high
Up to 80-90%, specific surface area can be up to 1000m2The density of/g, aeroge can be down to 2mg/cm3, therefore have the current world
The title of the smallest solid material of upper density.Since the pore structure and solid phase of aeroge are all nanometer scales, so also often claiming
It is a kind of typical mesoporous material.Meanwhile aeroge also has that elasticity is good, has lower refractive index and thermal conductivity and acoustic resistance
The features such as anti-, aeroge show good application value in many aspects such as optics, thermodynamics and acoustics.In environmental protection and catalysis
Aspect, aeroge determine that it, with stronger adsorption capacity, can be adsorbed in water with porous and high-specific surface area characteristic
Pollutant can also adsorb the pernicious gas in air.So in today of problem of environmental pollution sternness, aeroge application
In one of the focus that the processing of waste water, exhaust gas and waste residue is scientific circles.
TiO2It is that a kind of property is stable, nontoxic photochemical catalyst, there is fabulous practical application value.But pure titanium dioxide
Titanium aeroge network structure is poor, is unfavorable for the practical application of catalyst, moreover, the forbidden bandwidth of titanium dioxide is 3.2ev, only
Energy absorbing wavelength cannot make full use of solar energy in 387nm ultraviolet radioactive below, and photocatalytic activity is low, especially for
The degradation property of some hardly degraded organic substances is poor.In order to further improve the performance of photocatalysis material of titanium dioxide, state at present
Inside and outside to have carried out a large amount of doping vario-property research work to titania aerogel, such as precious metal doping is silica-doped, narrow
Bandgap semiconductor is compound and doping, alkali metal oxide adulterate, metal ion mixing etc..Using these different modified methods with
Afterwards, nano-TiO2Two problems existing for photochemical catalyst obtain solution to a certain extent.However, these modified methods urge this
Two defects of agent have different emphasis.It is dependent on this, the application is that template prepares titanium silicon compound aerogel using pigment,
Be expected to collection pigment, composite aerogel each advantage and can also photocatalytic activity with higher under visible light, at present also not
Seeing has relevant report.
Summary of the invention
The purpose of the present invention is intended to provide a kind of preparation method and applications for the titanium silica aerogel that pigment is template, with color
Element is titanium silicon compound aerogel material made of template and sensitizer, be expected to collection pigment, composite aerogel each advantage and energy
Also photocatalytic activity with higher under visible light, to improve photocatalytic activity of the aeroge in visible-range, sufficiently
Technical support is provided using sunlight.
The present invention is realized especially by following technical scheme:
A kind of pigment is the preparation method of the titanium silica aerogel of template, comprising the following steps:
1) ultrasound to pigment in solvent is added in pigment to be completely dissolved, positive silicon is added in the case where magnetic stirrer
Sour tetra-ethyl ester continues stirring one hour；
2) solvent, butyl titanate, 1.4mol/L dust technology and distilled water, constant agitation are successively added dropwise in the above solution
Speed is stirred to solution into colloidal sol, places 6-12h aging into gel；
3) obtained gel will be prepared to be put into quartz reaction kettle liner, be passed through N2Booster reaction is started to warm up, is reacted
After be slowly cooled to room temperature to get target product.
Further, the pigment is methylene blue, curcumin or one of the red kind of purple sweetpotato.
Further, the solvent is selected from methanol or ethyl alcohol.
Further, the amount of added pigment is 0.01-0.05g/ml, solvent and tetraethyl orthosilicate volume in step (1)
Than for 2:1.
Further, the volume ratio of institute's solubilizer in step (2), butyl titanate, dust technology and distilled water is 33:10:
0.35:3。
Further, it is 3:1 that the pigment, which is the titanium silicon mol ratio in the titanium silica aerogel of template,.
The reaction condition of the reaction kettle are as follows: pressure 80-100psi, 240-270 DEG C of temperature, time 40-70min.
What is be prepared by method made above is the titanium silica aerogel of template also in protection model of the invention using pigment
In enclosing.
What the present invention was prepared is the titanium silica aerogel of template under visible light and simulated solar irradiation irradiation using pigment, tool
There is good photocatalytic activity, reduction effect is better than the reduction effect without mould material.
It is the titanium silica aerogel of template in hexavalent chromium-treatments that another object of the present invention is to provide described using pigment
Application.
The invention has the benefit that
What the present invention was prepared is the titanium silica aerogel of template under visible light and simulated solar irradiation irradiation using pigment, three
Kind pigment is the titanium Silica Aerogels of template as photochemical catalyst, their photo catalytic reduction effect sequence are as follows: curcumin mould
Plate > methylene blue pigment template > purple sweet potato haematochrome template；Wherein, photo catalytic reduction rate of the curcumin under simulated solar irradiation
Up to 54.88%, under visible light, the photo catalytic reduction rates of three kinds of pigments is up to 20% or more.Technical solution of the present invention is in water body
The processing method of Cr VI has certain impetus, also urges to how improving the light of titania aerogel under visible light
Change activity, sunlight is made full use of to provide technical support.
Detailed description of the invention
Fig. 1 is the SEM figure for the titanium silica aerogel that methylene blue is template；
Fig. 2 is the SEM figure for the titanium silica aerogel that curcumin is template；
Fig. 3 be curcumin be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr (VI) curve graph；
Fig. 4 be methylene blue be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr (VI) curve graph；
Fig. 5 be purple sweet potato haematochrome be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr (VI) curve
Figure；
Fig. 6 is photo catalytic reduction Cr (VI) curve graph of three kinds of pigments under visible light for template institute prepared material；
Fig. 7 is photocatalytic activity comparison diagram of the different pigment template institute's prepared materials under visible light and simulated solar irradiation.
Specific embodiment
Below in conjunction with specific embodiment of the present invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
1 methylene blue of embodiment is the preparation of the titanium silica aerogel of template
1) methylene blue for weighing 0.2g is placed in 100ml beaker rear addition 10ml methanol, and ultrasound to pigment is completely dissolved；
5ml tetraethyl orthosilicate is added in the case where magnetic stirrer, continues certain mixing speed, it is one small to continue stirring
When.
2) 66ml methanol, 20ml butyl titanate, 0.7ml dust technology, 6ml distilled water are successively added dropwise into above-mentioned solution,
Constant agitation speed is stirred to solution plastic (or persistently stirring two hours or more), stands 12 hours into gel.
3) obtained gel will be prepared to be put into quartz reaction kettle liner, then to being passed through enough N in reaction kettle2,
The air in kettle is removed, sealing when pressure reaches 80psi, reacts 70min, discharges pressure therein after reaction by 260 DEG C of temperature
Power, and be slowly cooled to room temperature.
The shape characteristic of material surface is directly observed using scanning electron microscope (JSM-6700) herein.It can from Fig. 1
To find out that methylene blue has particle tiny as the titanium silica aerogel of template, uniformly, there is loose, porous popular feature.
2 curcumin of embodiment is the preparation of the titanium silica aerogel of template
1) curcumin for weighing 0.1g is placed in 100ml beaker the rear appropriate 5ml methanol of addition, and ultrasound is completely molten to pigment
Solution；Suitable 2.5ml tetraethyl orthosilicate is added in the case where magnetic stirrer, continues certain mixing speed, after
One hour of continuous stirring.
2) 33ml methanol, 10ml butyl titanate, 0.35ml dust technology, 3ml distilled water are successively added dropwise into above-mentioned solution,
Constant agitation speed is stirred to solution plastic (or persistently stirring two hours or more), stands 8 hours into gel.
3) obtained gel will be prepared to be put into quartz reaction kettle liner, then to being passed through enough N in reaction kettle2,
The air in kettle is removed, sealing when pressure reaches 100psi, reacts 50min by 270 DEG C of temperature, and reaction kettle discharges after showing
Pressure therein, and be slowly cooled to room temperature, so that solution therein sufficiently removes.
The shape characteristic of material surface is directly observed using scanning electron microscope (JSM-6700) herein.It can from Fig. 2
The phenomenon that see reunion, in addition, from can also be seen that the titanium aerogel particles that curcumin is template are tiny with aeroge,
Uniformly, there is loose, porous popular feature.
The preparation of the red titanium silica aerogel for template of 3 purple sweetpotato of embodiment
1) appropriate 5ml methanol is added in red be placed in 100ml beaker of purple sweetpotato for weighing 0.1g afterwards, and ultrasound is completely molten to pigment
Solution；Suitable 2.5ml tetraethyl orthosilicate is added in the case where magnetic stirrer, continues certain mixing speed, after
One hour of continuous stirring.
2) 33ml methanol, 10ml butyl titanate, 0.35ml dust technology, 3ml distilled water are sequentially added into above-mentioned solution,
Constant agitation speed is stirred to solution plastic (or persistently stirring two hours or more), stands 8 hours into gel.
3) obtained gel will be prepared to be put into quartz reaction kettle liner, then to being passed through enough N in reaction kettle2,
The air in kettle is removed, sealing when pressure reaches 90psi, reacts 60min by 250 DEG C of temperature, and reaction kettle discharges it after showing
In pressure, and be slowly cooled to room temperature.
Pigment is that the titanium silica aerogel of template is catalyzed reduction of hexavalent chromium under 4 simulated solar irradiation of embodiment
According to three steps of the light-catalyzed reaction of photo catalytic reduction Cr VI, respectively with curcumin, methylene blue and purple
Sweet potato haematochrome is that the titanium silica aerogel photo catalytic reduction Cr VI of template carries out under conditions of simulated solar irradiation and visible light
Experiment (hexavalent chromium solution initial concentration is 20ppm, catalyst charge 2.5g/L).
1) curcumin be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr VI.
Fig. 3 be different titanium silicon that curcumin is template than aeroge the photo catalytic reduction Cr VI curve under simulated solar irradiation
(wherein A: blank, B: titanium silicon is than being 3:1 without template aeroge, and C: titanium silicon is than the titanium silicon gas that the curcumin for 3:1 is template for figure
Gel, D: titanium silicon is than the titanium silica aerogel that the curcumin for 1:1 is template, E: titanium silicon is the titanium of template than the curcumin for 1:3
Silica aerogel).It follows that the different titanium silicon that curcumin is template are superior to non-additive color element than the photocatalytic activity of aeroge is
The activity of mould material.And when titanium silicon ratio is 3:1, the photo catalytic reduction effect of Cr VI is best, photocatalysis when knowing 5h by table 1
Reduction rate is up to 54.88%.
2) methylene blue be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr VI
Fig. 4 is titanium silica aerogel that methylene blue is template photo catalytic reduction Cr (VI) curve graph under simulated solar irradiation
(wherein A: blank, B: titanium silicon is than being 3:1 without template aeroge, and C: titanium silicon is than the titanium silicon gas that the methylene blue for 3:1 is template
Gel, D: titanium silicon is than the titanium silica aerogel that the methylene blue for 1:1 is template, and E: titanium silicon is template than the methylene blue for 1:3
Titanium silica aerogel).According to the titanium silica aerogel that methylene blue is template, photo catalytic reduction Cr VI is bent under simulated solar irradiation
It follows that when titanium silicon ratio is 3:1, the photo catalytic reduction effect of Cr VI is best for line chart and table 1, when 5h, photo catalytic reduction rate
Up to 46.90%.
3) purple sweet potato haematochrome be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr VI
Fig. 5 purple sweet potato haematochrome be template titanium silica aerogel under simulated solar irradiation photo catalytic reduction Cr (VI) curve
Figure；(A: blank, B: titanium silicon is than being 3:1 without template aeroge, C: titanium silicon is the titanium of template than the purple sweet potato haematochrome for 3:1
Silica aerogel, D: titanium silicon is than the titanium silica aerogel that the purple sweet potato haematochrome for 1:1 is template, and E: titanium silicon is than the purple sweetpotato for 1:3
Haematochrome is the titanium silica aerogel of template).According to purple sweet potato haematochrome be template titanium silica aerogel under simulated solar irradiation light
Reduction of hexavalent chromium curve graph and table 1 are catalyzed it follows that the photo catalytic reduction effect of Cr VI is best, 5h when titanium silicon ratio is 3:1
When photocatalysis reduction rate up to 45.37%.
Under 1 simulated solar irradiation of table when 5h pigment mould material with no mould material to the reduction rate of Cr VI
| Template | Curcumin | Methylene blue | Purple sweetpotato is red | Non-pigment |
| Reduction rate % | 54.88 | 46.90 | 45.37 | 38.90 |
Pigment is the titanium silica aerogel photo catalytic reduction Cr VI of template under the different light sources of embodiment 5
(wherein A: blank, B: titanium silicon is than the titanium silica aerogel that the curcumin for 3:1 is template, C: titanium silicon ratio as shown in Figure 6
Methylene blue for 3:1 is the titanium silica aerogel of template, and D: titanium silicon is than the titanium silicon airsetting that the purple sweet potato haematochrome for 3:1 is template
Glue).In order to observe the activity of aeroge under visible light, herein to using curcumin, methylene blue, purple sweet potato haematochrome as mould
Plate, titanium silicon ratio are the titanium silica aerogel of 3:1, have carried out the photocatalytic activity research under visible light, photo catalytic reduction six when 5h
The reduction rate of valence chromium is respectively 29.19%, 27.63%, 22.41%.Under visible light, three kinds of pigments are the titanium silica aerogel of template
Material is effective to the photo catalytic reduction of Cr VI.Activity sequence of the pigment template to photo catalytic reduction Cr VI: curcumin >
Methylene blue > purple sweet potato haematochrome.
The photocatalytic activity comparison diagram that Fig. 7 is institute's prepared material under visible light and simulated solar irradiation, as can be seen, pigment mould
Photocatalytic activity of the plate titanium silica aerogel under visible light and simulated solar irradiation is better than the photocatalysis of no template titanium silica aerogel
Activity.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understand without departing from the principles and spirit of the present invention can to these examples carry out it is a variety of variation, modification, replacement and
Modification, the scope of the present invention is defined by the appended.
Claims (9)
1. the preparation method that a kind of pigment is the titanium silica aerogel of template, which comprises the following steps:
1) ultrasound to pigment in solvent is added in pigment to be completely dissolved, positive silicic acid four is added in the case where magnetic stirrer
Ethyl ester continues stirring one hour；
2) solvent, butyl titanate, 1.4mol/L dust technology and distilled water, constant agitation speed are successively added dropwise in the above solution
Stirring at colloidal sol, places 6-12h aging into gel to solution,
3) obtained gel will be prepared to be put into quartz reaction kettle liner, be passed through N2Booster reaction is started to warm up, after reaction
It is slowly cooled to room temperature to get target product.
2. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that described
Pigment be methylene blue, curcumin or one of the red kind of purple sweetpotato.
3. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that described
Solvent be selected from methanol or ethyl alcohol.
4. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that step
(1) amount of added pigment is 0.01-0.05g/ml in, and solvent and tetraethyl orthosilicate volume ratio are 2:1.
5. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that step
(2) institute's solubilizer in, butyl titanate, dust technology and distilled water volume ratio be 33:10:0.35:3.
6. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that described
Pigment be titanium silicon mol ratio in the titanium silica aerogel of template be 3:1.
7. the preparation method that a kind of pigment according to claim 1 is the titanium silica aerogel of template, which is characterized in that step
(3) reaction condition of the reaction kettle described in are as follows: pressure 80-100psi, 240-270 DEG C of temperature, time 40-70min.
8. preparation method described in claim 1 be prepared using pigment as the titanium silica aerogel of template.
9. the application as claimed in claim 7 using pigment as the titanium silica aerogel of template in hexavalent chromium-treatments.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479204A (en) * | 2019-08-13 | 2019-11-22 | 云南大学 | A kind of high adsorption TiO2The application of the preparation method and its absorbing heavy metal ions in water of aeroge |
| CN111203159A (en) * | 2020-01-16 | 2020-05-29 | 苏州科技大学 | Preparation method and application of curcumin-titanium dioxide-three-dimensional graphene composite aerogel |
| CN113292078A (en) * | 2021-04-20 | 2021-08-24 | 西安理工大学 | Preparation method of titanium dioxide aerogel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219279A (en) * | 2011-04-13 | 2011-10-19 | 同济大学 | Visible light catalytic degradation method of organic pollutants based on TiO2/carbon aerogel electrode |
| WO2013118940A1 (en) * | 2012-02-08 | 2013-08-15 | Photo & Environmental Technology Co. | Porous composite, preparation method thereof, and cement composition containing porous composite |
-
2018
- 2018-09-29 CN CN201811147389.7A patent/CN108940143B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219279A (en) * | 2011-04-13 | 2011-10-19 | 同济大学 | Visible light catalytic degradation method of organic pollutants based on TiO2/carbon aerogel electrode |
| WO2013118940A1 (en) * | 2012-02-08 | 2013-08-15 | Photo & Environmental Technology Co. | Porous composite, preparation method thereof, and cement composition containing porous composite |
Non-Patent Citations (2)
| Title |
|---|
| 邓忠生 等: "TiO2-SiO2复合半导体气凝胶制备及光催化活性研究", 《功能材料与器件学报》 * |
| 高文宇: "色素模板TiO2气凝胶光催化处理水中Cr（VI）及焦化废水", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110479204A (en) * | 2019-08-13 | 2019-11-22 | 云南大学 | A kind of high adsorption TiO2The application of the preparation method and its absorbing heavy metal ions in water of aeroge |
| CN111203159A (en) * | 2020-01-16 | 2020-05-29 | 苏州科技大学 | Preparation method and application of curcumin-titanium dioxide-three-dimensional graphene composite aerogel |
| CN113292078A (en) * | 2021-04-20 | 2021-08-24 | 西安理工大学 | Preparation method of titanium dioxide aerogel |
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