CN1342517A - Process for preparing mesoporous TiOw powder and film photocatalyst by sol-gel method - Google Patents
Process for preparing mesoporous TiOw powder and film photocatalyst by sol-gel method Download PDFInfo
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- CN1342517A CN1342517A CN 01130896 CN01130896A CN1342517A CN 1342517 A CN1342517 A CN 1342517A CN 01130896 CN01130896 CN 01130896 CN 01130896 A CN01130896 A CN 01130896A CN 1342517 A CN1342517 A CN 1342517A
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Abstract
A process for preparing the photocatalyst of mesoporous TiO2 powder or film by the sol-gel method includes such steps as preparing solution from n-butyl titanate, low-carbon alcohol and diethanolamine, adding polyethyleen glycol to obtain transparent precursor sol, evaporating solvent out, drying, crushing, and calcining to obtain the photocatalyst. It has high photocatalytic efficiency and activity. The mesoporous powder and film prepared by the said process has vertically open porous structure which benefits the photocatalytic reaction and high activity.
Description
Technical field:
The present invention relates to a kind ofly prepare the method for mesoporous TiO 2 powder and film photocatalyst with sol-gel process, belong to technical field of chemistry and chemical engineering.
Background technology:
The nano-TiO of commonsense method preparation
2Photochemical catalyst, especially film photocatalyst owing to there is not a pore structure, its photocatalytic activity corresponding a little less than.The mesoporous TiO of existing preparation
2The method of powder and film photocatalyst mainly contains two classes: (1) utilizes octadecylamine as the template agent, uses hydrothermal synthesis method to prepare mesoporous TiO
2The method of powder photocatalyst; (2) utilize inlay and break copolymer as the template agent, utilize organic titanate or the mesoporous TiO of titanium tetrachloride Prepared by Sol Gel Method
2The method of powder and film; Wherein in method (1) owing to adopt octadecylamine as the template agent, after hydro-thermal was synthetic, template was removed very difficult, is easy to produce the destruction of meso-hole structure, and is difficult to be prepared into film photocatalyst.The mesoporous photocatalytic agent of method (2) preparation has preferably pore structure, but not only exists the removing difficulty of template also to have the problem of template price, is difficult to produce in enormous quantities.
Summary of the invention:
The objective of the invention is to study and a kind ofly prepare the method for mesoporous TiO 2 powder and film photocatalyst,, control mesoporous pore size and hole density, make the mesoporous TiO of formation by molecular weight and the concentration of control PEG with sol-gel process
2Has the anatase phase structure.
What the present invention proposed prepares the method for mesoporous TiO 2 powder and film photocatalyst with sol-gel process, may further comprise the steps::
1., preparation presoma
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine (stabilizing agent) and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is that 1%~30% molecular weight is 200~4000 polyethylene glycol, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for the dissolving polyethylene glycol in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the diethanol amine alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.
Or titanium tetrachloride is added drop-wise to low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol) in the solvent, be that 200~4000 polyethylene glycol is dissolved in the alcoholic solvent again with molecular weight, both are mixed, obtain precursor solution at last, in the last precursor solution, the volume ratio that titanium tetrachloride accounts for solvent is 5%~30%, the mol ratio that polyethylene glycol accounts for titanium tetrachloride is 1%~30%, place saturated steam atmosphere fully to absorb water precursor solution, form precursor sol, the solution of firm preparation gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.
2. preparation mesopore titania photocatalyst
With the solvent in above-mentioned precursor sol evaporation, after the drying and crushing, under the air atmosphere condition, to calcine, initial heating rate is 10 ℃/minute, 250~600 ℃ temperature lower calcination 0.5~5 hour, promptly forms mesoporous TiO then
2Powder photocatalyst.
Or the method for utilizing repeatedly rotary plating or repeatedly lifting, (glass on base material, aluminium alloy, stainless steel) colloidal sol that obtains with above-mentioned any method prepares film, and each coating film thickness is no more than 100 nanometers, and gross thickness is 100~500 nanometers, the precursor thin-film sample of last air dry is calcined under the air atmosphere condition, initial heating rate is 10 ℃/minute, 250~600 ℃ temperature lower calcination 0.5~5 hour, promptly forms mesoporous TiO then
2Film photocatalyst.
The mesoporous TiO that method of the present invention is prepared
2Photochemical catalyst has advantages such as photocatalysis efficiency height and high activity, utilizes the mesoporous powder of this method preparation and the pore structure that film has vertical open, helps the carrying out and the active raising of light-catalyzed reaction.PEG is a kind of very common macromolecular material, and it is low to utilize this method to prepare cost, the simple mesoporous TiO of technology
2Powder or film photocatalyst.
The specific embodiment:
Embodiment one:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 2% PEG200, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment two:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 10% PEG200, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment three:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 25% PEG200, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment four:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG400, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment five:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG2000, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment six:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG400, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Utilize the method for rotary plating, prepare film at stainless steel-based bottom material, plated film is 4 times altogether, each coating film thickness is no more than 100 nanometers, the precursor thin-film sample of last air dry is calcined under the air atmosphere condition, initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, namely forms mesoporous TiO of the present invention then
2Film photocatalyst, this mesopore film has very high photocatalytic activity.
Embodiment seven:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 20% PEG400, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Utilize the method for rotary plating, prepare film at stainless steel-based bottom material, plated film is 4 times altogether, each coating film thickness is no more than 100 nanometers, the precursor thin-film sample of last air dry is calcined under the air atmosphere condition, initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, namely forms mesoporous TiO of the present invention then
2Film photocatalyst, this mesopore film has very high photocatalytic activity.
Embodiment eight:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG2000, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.Utilize the method for rotary plating, prepare film at stainless steel-based bottom material, plated film is 4 times altogether, each coating film thickness is no more than 100 nanometers, the precursor thin-film sample of last air dry is calcined under the air atmosphere condition, initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, namely forms mesoporous TiO of the present invention then
2Film photocatalyst, this mesopore film has very high photocatalytic activity.
Embodiment nine:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG2000, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.At room temperature, with preplating TiO
2The woven wire of transition zone immerses in the active colloidal sol of above-mentioned preparation, lift (20cm/min) with certain speed then, the centrifugal colloidal sol that removes attached to the silk screen surface, air dry, repeat this process, prepare 4 layers of active layer, THICKNESS CONTROL is in 400 nanometers, at last in heating furnace 400 ℃ the calcining 2 hours, form final TiO
2Film photocatalyst, photocatalysis performance evaluation show that this catalyst has very high catalytic activity.
Embodiment ten:
With tetrabutyl titanate [Ti (OC
4H
9)
4] be raw material, with raw material, low-carbon alcohols (methyl alcohol, ethanol, propyl alcohol), diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add and to account for Ti (OC
4H
9)
4Mol ratio is 8% PEG2000, at first will mix in water and the diethanol amine adding part alcohol during preparation, and part alcohol is used for dissolving PEG in addition, and then with tetrabutyl titanate Ti (OBu)
4In the mixed solution, add at last the PEG alcoholic solution before solution drips, can obtain like this solution of faint yellow homogeneous transparent, airtightly leave standstill gel in 5 days and obtain transparent precursor sol.At room temperature, with preplating TiO
2The glass marble of transition zone immerses in the active colloidal sol of above-mentioned preparation, lift (20cm/min) with certain speed then, the centrifugal colloidal sol that is attached to particle surface that removes afterwards, air dry, repeat this process, prepare 4 layers of active layer, at last in heating furnace 400 ℃ the calcining 2 hours, finally form TiO
2Film photocatalyst, photocatalysis performance evaluation show that this catalyst has very high catalytic activity.
Embodiment 11:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG200 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment 12:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG200 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 20%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment 13:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG400 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment 14:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG2000 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.Evaporating solvent obtains xerogel, calcines under the air atmosphere condition then, and initial heating rate is 10 ℃/minute, 400 ℃ temperature lower calcination 2 hours, promptly forms mesoporous TiO of the present invention then
2Powder photocatalyst.
Embodiment 15:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG400 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.At room temperature, with preplating TiO
2The glass marble of transition zone immerses in the active colloidal sol of above-mentioned preparation, lift (20cm/min) with certain speed then, the centrifugal colloidal sol that is attached to particle surface that removes afterwards, air dry, repeat this process, prepare 4 layers of active layer, at last in heating furnace 400 ℃ the calcining 2 hours, finally form TiO
2Film photocatalyst, this catalyst has very high catalytic activity.
Embodiment 16:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG400 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 20%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.At room temperature, with preplating TiO
2The glass marble of transition zone immerses in the active colloidal sol of above-mentioned preparation, lifts (20cm/min) with certain speed then, the centrifugal afterwards colloidal sol that removes attached to particle surface, air dry repeats this process, prepares 4 layers of active layer, at last in heating furnace 400 ℃ the calcining 2 hours, finally form TiO
2Film photocatalyst.
Embodiment 17:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG2000 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.At room temperature, with preplating TiO
2The glass marble of transition zone immerses in the active colloidal sol of above-mentioned preparation, lift (20cm/min) with certain speed then, the centrifugal colloidal sol that is attached to particle surface that removes afterwards, air dry, repeat this process, prepare 4 layers of active layer, at last in heating furnace 400 ℃ the calcining 2 hours, finally form TiO
2Film photocatalyst, this catalyst has very high catalytic activity.
Embodiment 18:
A certain amount of titanium tetrachloride is dripped in the ethanol, a certain amount of PEG2000 also is dissolved in earlier in the alcohol, both mix at last, and wherein to account for the volume ratio of solvent be 10% to titanium tetrachloride, and PEG accounts for TiCl
4Mol ratio is 8%, places saturated steam atmosphere fully to absorb water precursor solution, forms precursor sol, and the solution of just having prepared gained is faint yellow, and along with the increase color of digestion time shoals, becomes the vitreosol with certain viscosity.At room temperature, with preplating TiO
2The woven wire of transition zone immerses in the active colloidal sol of above-mentioned preparation, lift (20cm/min) with certain speed then, the centrifugal colloidal sol that removes attached to the silk screen surface, air dry, repeat this process, prepare 4 layers of active layer, THICKNESS CONTROL is in 400 nanometers, at last in heating furnace 400 ℃ the calcining 2 hours, form final TiO
2Film photocatalyst, photocatalysis performance evaluation show that this catalyst has very high catalytic activity.
Claims (2)
1, a kind ofly prepare the method for mesoporous TiO 2 powder photochemical catalyst, may further comprise the steps with sol-gel process::
(1) preparation presoma
With the tetrabutyl titanate is raw material, with raw material, low-carbon alcohols, diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add that to account for the tetrabutyl titanate mol ratio be that 1%-30%, molecular weight are 200~4000 polyethylene glycol, at first will mix in water and the diethanol amine adding part alcohol during preparation, part alcohol is used to dissolve polyethylene glycol in addition, and then before the tetrabutyl titanate drips of solution is added in the mixed solution, the alcoholic solution that adds polyethylene glycol at last airtightly obtains transparent precursor sol after leaving standstill gel;
Or titanium tetrachloride is added drop-wise in the low-carbon alcohols solvent, be that 200~4000 polyethylene glycol is dissolved in the alcoholic solvent again with molecular weight, both are mixed, obtain precursor solution at last, in the last precursor solution, the volume ratio that titanium tetrachloride accounts for solvent is 5%-30%, and the mol ratio that polyethylene glycol accounts for titanium tetrachloride is 1%-30%, place saturated steam atmosphere fully to absorb water precursor solution, form precursor sol;
(2) preparation mesopore titania photocatalyst
With the solvent in above-mentioned precursor sol evaporation, after the drying and crushing, under the air atmosphere condition, to calcine, initial heating rate is 10 ℃/minute, 250~600 ℃ temperature lower calcination 0.5~5 hour, promptly forms mesoporous TiO then
2Powder photocatalyst.
2, a kind ofly prepare the method for mesoporous titanium dioxide film photochemical catalyst, may further comprise the steps with sol-gel process::
(1) preparation presoma
With the tetrabutyl titanate is raw material, with raw material, low-carbon alcohols, diethanol amine and water in 1: 10: 0.125: 0.05625 ratio wiring solution-forming, and add that to account for the tetrabutyl titanate mol ratio be that 1%-30%, molecular weight are 200~4000 polyethylene glycol, at first will mix in water and the diethanol amine adding part alcohol during preparation, part alcohol is used to dissolve polyethylene glycol in addition, and then before the tetrabutyl titanate drips of solution is added in the mixed solution, the alcoholic solution that adds polyethylene glycol at last airtightly obtains transparent precursor sol after leaving standstill gel;
Or titanium tetrachloride is added drop-wise in the low-carbon alcohols solvent, be that 200~4000 polyethylene glycol is dissolved in the alcoholic solvent again with molecular weight, both are mixed, obtain precursor solution at last, in the last precursor solution, the volume ratio that titanium tetrachloride accounts for solvent is 5%-30%, and the mol ratio that polyethylene glycol accounts for titanium tetrachloride is 1%-30%, place saturated steam atmosphere fully to absorb water precursor solution, form precursor sol;
(2) method of utilizing repeatedly rotary plating or repeatedly lifting, the colloidal sol that obtains with the above-mentioned first step on base material prepares film, each coating film thickness is no more than 100 nanometers, gross thickness is 100~500 nanometers, precursor thin-film sample with air dry places the calcining of air atmosphere condition at last, initial heating rate is 10 ℃/minute, 250~600 ℃ temperature lower calcination 0.5~5 hour, promptly forms mesoporous TiO then
2Film photocatalyst.
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- 2001-08-31 CN CNB011308966A patent/CN1137771C/en not_active Expired - Fee Related
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