CN102233267A - Integrated photocatalyst and preparation method thereof - Google Patents
Integrated photocatalyst and preparation method thereof Download PDFInfo
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- CN102233267A CN102233267A CN 201010165861 CN201010165861A CN102233267A CN 102233267 A CN102233267 A CN 102233267A CN 201010165861 CN201010165861 CN 201010165861 CN 201010165861 A CN201010165861 A CN 201010165861A CN 102233267 A CN102233267 A CN 102233267A
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Abstract
The invention discloses an integrated photocatalyst and a preparation method thereof. In the integrated photocatalyst, epoxy resin with a three-dimensional skeleton structure is used as a template, a large-aperture three-dimensional SiO2 ultrathin film compounded on the template is used as a carrier, a nano TiO2 ultrathin film is coated on the carrier, the porosity of the three-dimensional SiO2 ultrathin film is 50-95 percent, the thickness of the three-dimensional SiO2 ultrathin film is 15-90 nanometers, and the thickness of the nano TiO2 ultrathin film is 20-100 nanometers. The preparation method comprises the following steps of: preparing the three-dimensional skeleton structure by using the epoxy resin, soaking the three-dimensional skeleton structure in tetraethyl orthosilicate, roasting the three-dimensional skeleton structure in a muffle furnace to obtain the three-dimensional SiO2 ultrathin film, soaking the three-dimensional SiO2 ultrathin film into a mixed solution of butyl titanate and cyclohexane, drying, and roasting the three-dimensional SiO2 ultrathin film in the muffle furnace to obtain the integrated photocatalyst. The integrated photocatalyst does not need a grid, has the advantages of strong practicability, good light transmission and strong adsorption, and can be directly used as an air purification material; and the preparation method is mild, easily controlled and easy for large-scale production.
Description
Technical field
The present invention relates to the catalysis material technical field, especially a kind of with TiO2/SiO
2The ultrathin membrane compound is type photochemical catalyst and preparation method thereof as a whole.
Background technology
A kind of in recent years based on nano-TiO
2The indoor air purification technology of photochemical catalytic oxidation characteristic is developed, and the core component of this technology all is a surface applied nano-TiO basically
2The net grid.When air flow through the net grid, pollutant just may be by nano-TiO
2Degrade, yet the air purifier of this structure is incomplete, verified its photocatalytic degradation effect does not almost detect, one of them chief reason is that pollutant is not enriched in nano-TiO
2On every side.The someone expected having the material of adsorption function as nano-TiO by some afterwards
2Carrier, pollutant can be adsorbed then effectively and be degraded like this.There have been some loose structure adsorbents to be used to loaded with nano TiO at present
2But, porous carrier itself and load TiO
2After catalyst generally all be particle or powder, can't directly use, they can only be bonded in and just may be used on the net grid purify air.As the patent No. 02112266.0, a kind of air cleaning nanocatalyst and preparation method thereof, photochemical catalyst is made up of carrier and nano particle or film, carrier by spherical silica gel or granular colloidal silica or KSG or/and silochrom or Kiselgel A form, the silica gel aperture that wherein is used for the gel-sol process is the 5-30 nanometer, and the silica gel aperture that is used for slurry impregnation technology method is greater than 30 nanometers, wherein TiO
2The nano-photocatalyst percentage by weight is 1.0-5.0%, and the catalytic activity body in this invention photochemical catalyst adopts slurry dipping, gel-sol technology with TiO
2Nano particle or film are carried in carrier surface and the space, form the composite nano photochemical catalyst.This patent has improved photocatalytic activity, has realized the immobilization and the high-specific surface areaization of nano particle and film, and technology is simple, but photochemical catalyst need be fixed with woven wire when being to use, and just needs net grid structure.
There are some problems in the clarifier of net grid structure, and wherein most importantly polymer binder is subjected to nano-TiO
2The influence of photocatalytic degradation and losing efficacy, catalyst just comes off from the net grid easily like this, thereby can't use for a long time; Secondly, the net grid block ultraviolet light easily, and the illumination rate of catalyst is reduced, and influence its clean effect; The 3rd, the amount of the catalyst of net grid load is very limited, and this also can restrict the efficient of air cleaning; The 4th, present most supporter mostly is a wire netting, and light-catalysed product is water and carbon dioxide, and use can make metal get rusty for a long time.In a word, the root problem of the air purifier of releasing is that catalyst, carrier and this three of net grid exist weak link in linking at present, thereby can't well work in coordination with and further optimization.Someone thinks that the key that tackles the problem at its root is to prepare suitable porous carrier, this carrier can either be effectively, loaded with nano TiO2 catalyst easily, can replace simultaneously traditional net grid support again, realize the air cleaning mode of catalyst, carrier and net grid three in oneization.
Summary of the invention
Primary technical problem to be solved by this invention provides that a kind of light transmission is good, adsorptivity is strong and need not the monolithic devices photochemical catalyst of net grid structure.
Second technical problem to be solved by this invention provides a kind of preparation method of monolithic devices photochemical catalyst.
The present invention solves the technical scheme that above-mentioned primary technical problem adopts: a kind of monolithic devices photochemical catalyst, it is characterized in that described monolithic devices photochemical catalyst be with epoxy resin with three-dimensional framework structure as template, on template, be compounded with wide-aperture D S iO
2Ultrathin membrane is coated with nano-TiO as carrier on the carrier
2Ultrathin membrane, the pore diameter range of described macropore is between 100nm to 2 μ m.
As improvement, described D S iO
2The porosity of ultrathin membrane is 50%～95%, and thickness is 15～90 nanometers, described nano-TiO
2Ultrathin membrane thickness is 20～100 nanometers.
The present invention solves above-mentioned second technical scheme that technical problem adopted: a kind of preparation method of monolithic devices photochemical catalyst is characterized in that may further comprise the steps:
1) preparation of three-dimensional framework template: with mass ratio is that 1: 4～4: 1 epoxy resin and polyethylene glycol mix and be heated to 40～90 ℃, stir became clear solution in 5～15 minutes after, adding and epoxy resin mass ratio are 1: 2～1: 10 polyamines liquid rapidly, pour into after stirring in the polytetrafluoroethylene (PTFE) mould and finalize the design, keep setting temperature in 40～90 ℃, to form the solid shaped polymer blend of white after 1～10 hour, remove the polyethylene glycol phase with the pure water immersion fully after 2～20 hours, stay the epoxy resin of three-dimensional framework structure, air dry at room temperature 1～5 day;
2) D S iO
2The preparation of ultrathin membrane: the epoxy resin template of the three-dimensional framework structure that step 1 is made was soaked 1～5 hour in positive tetraethyl orthosilicate, formed SiO expose 10～20 hours in 30～60 ℃ in ammoniacal liquor atmosphere after
2/ epoxy resin composite, the heating rate with 5～10 ℃ in Muffle furnace rose to 600～900 ℃, kept can obtaining D S iO in 10～60 minutes with the ethanol of removing generation and the ammoniacal liquor of absorption in dry 1～5 hour
2Ultrathin membrane;
3) preparation of monolithic devices photochemical catalyst: the D S iO that step 2 is made
2Ultrathin membrane places 100～200 ℃ of down dry 0.5～2h, be immersed in then in the mixed solution of butyl titanate and cyclohexane, take out behind immersion 5～10h, dry naturally also and in Muffle furnace, calcine 1～3h behind hydrolysis 8～12h, calcining heat is 500～700 ℃, calcining back nano-TiO
2Just can load on SiO with the form of film
2On the carrier.
As improvement, described step 2 can repeatedly repeat to increase D S iO
2The thickness of ultrathin membrane or dilute positive tetraethyl orthosilicate by cyclohexylamine and reduce D S iO
2The thickness of ultrathin membrane so just can be regulated D S iO as required
2The thickness of ultrathin membrane.
As improvement, described step 3 can repeatedly repeat to reach TiO
2The thickness that film is required or reduce nano-TiO by cyclohexane dilution butyl titanate
2The thickness of film so just can be regulated TiO as required
2The thickness of film.
As improvement, described cyclohexylamine is 1: 3～3: 1 with the mass ratio of positive tetraethyl orthosilicate.
As improvement, the volume ratio of described butyl titanate and cyclohexane is 1: 3～1: 1.
As preferably, described polyethylene glycol is that molecular weight is one or both in 600,1000,2000,4000 or 6000.
As preferably, described polyamines liquid is diethylenetriamine or triethylene tetramine.
Described monolithic devices photochemical catalyst can directly use as material for air purification.
Compared with prior art, the invention has the advantages that:
(1) practical: this material collection catalyst, carrier, fixing function with the net grid are one, have solved a series of problems such as catalytic efficiency, catalyst recovery, carrier be fixing, the large-scale commercial applications application may height;
(2) light transmission is good: the thin only 20-30nm of microcosmic wall, so have higher light transmittance, ultraviolet light sees through easily;
(3) adsorptivity is strong; Aperture big (1-2 μ m) and connect IPN continuously helps the circulation diffusion of material; By adjusting polymer template, can make three-dimensional ultra-thin Si O
2Crooked thin layer surrounds the little space of micro-meter scale in the structure of framework material, increases the high light catalytic effect greatly;
(4) condition control easily: many hydroxyls are arranged, easy and TiO in high-temperature process on the wall
2Generate the Ti-O-Si key, increased and TiO
2Active force between the film, load fastness and uniformity strengthen; Butyl titanate in-situ hydrolysis in the duct generates TiO
2, be not easy to reunite and be nano-scale particle, two dimensional surface relatively, just as enclosure space, solution solubility is certain for the solution that is immersed in the inside in its three-dimensional microcosmic space that is made of the duct, and then concentration is the same everywhere in the template, can control TiO by concentration
2Thickness, therefore have macro-size and the controlled advantage of microcosmic;
(5) physical property is excellent: stability is high, and is high temperature resistant, is difficult for breaking into pieces; Large aperture macroporosity, little apparent density, bigger serface, moulding is simple.
Description of drawings
Fig. 1 is D S iO
2The ultrathin membrane micro-structure diagram;
Fig. 2 is the micro-structure diagram of monolithic devices photochemical catalyst;
Fig. 3 is the outside drawing of monolithic devices photochemical catalyst.
The specific embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment 1
Step 1: the preparation of three-dimensional framework polymer template: with mass ratio is that 1: 2 epoxy resin E-51 and polyethylene glycol mix and be heated to 60 ℃, stir became clear solution in 10 minutes after, adding and epoxy resin mass ratio are 1: 6 polyamines liquid rapidly, pour into after stirring in the polytetrafluoroethylene (PTFE) mould and finalize the design, keep setting temperature in 60 ℃, to form the solid shaped polymer blend of white after 2 hours, remove the polyethylene glycol phase with the pure water immersion fully after 5 hours, stay the epoxy resin of three-dimensional framework structure, air dry at room temperature 3 days;
Wherein the molecular weight of polyethylene glycol is 1000, and polyamines liquid is diethylenetriamine.
Step 2: D S iO
2The preparation of ultrathin membrane, the epoxy resin that is about to three-dimensional framework structure in the step 1 soaked 2 hours in positive tetraethyl orthosilicate, and exposure formed SiO after 15 hours in 49 ℃ in ammoniacal liquor atmosphere
2/ epoxy resin composite, the heating rate with 10 ℃ in Muffle furnace rose to 800 ℃, kept can obtaining D S iO in 20 minutes with the ethanol of removing generation and the ammoniacal liquor of absorption in dry 2 hours
2Ultrathin membrane;
Step 3: D S iO
2Ultrathin membrane places 120 ℃ of dry 0.5h down, is immersed in then in the mixed solution of butyl titanate and cyclohexane (volume ratio is 1: 3), takes out behind the immersion 5h, dries naturally also and calcines 1h behind the hydrolysis 8h in Muffle furnace, and calcining heat is 500 ℃, calcining back nano-TiO
2Just can load on SiO with the form of film
2On the carrier.
After testing, place this photochemical catalyst of 30g in 2 * 3 meters spaces, under the uviol lamp effect, concentration of formaldehyde drops to 0.06ppm from 1.3ppm in the 45min, the clearance of formaldehyde reaches 95.3%, reaches the safety standard (concentration of formaldehyde≤0.08ppm) of national regulation fully.
Embodiment 2
Step 1: the preparation of three-dimensional framework polymer template: with mass ratio is that 1: 2 epoxy resin E-51 and polyethylene glycol mix and be heated to 60 ℃, stir became clear solution in 10 minutes after, adding and epoxy resin mass ratio are 1: 6 polyamines liquid rapidly, pour into after stirring in the polytetrafluoroethylene (PTFE) mould and finalize the design, keep setting temperature in 60 ℃, to form the solid shaped polymer blend of white after 2 hours, remove the polyethylene glycol phase with the pure water immersion fully after 5 hours, stay the epoxy resin of three-dimensional framework structure, air dry at room temperature 3 days;
Wherein the molecular weight of polyethylene glycol is 1000, and polyamines liquid is diethylenetriamine.
Repeat above-mentioned steps once.
Step 2: D S iO
2The preparation of ultrathin membrane, the epoxy resin that is about to three-dimensional framework structure in the step 1 soaked 2 hours in positive tetraethyl orthosilicate, and exposure formed SiO after 15 hours in 49 ℃ in ammoniacal liquor atmosphere
2/ epoxy resin composite, the heating rate with 10 ℃ in Muffle furnace rose to 800 ℃, kept can obtaining D S iO in 20 minutes with the ethanol of removing generation and the ammoniacal liquor of absorption in dry 2 hours
2Ultrathin membrane.
Step 3: D S iO
2Ultrathin membrane places 200 ℃ of dry 2h down, is immersed in then in the mixed solution of butyl titanate and cyclohexane (volume ratio is 1: 1), takes out behind the immersion 10h, dries naturally also and calcines 3h behind the hydrolysis 12h in Muffle furnace, and calcining heat is 700 ℃, calcining back nano-TiO
2Just can load on SiO with the form of film
2On the carrier.
After testing, place this photochemical catalyst of 30g in 2 * 3 meters spaces, under the uviol lamp effect, concentration of formaldehyde drops to 0.05ppm from 1.3ppm in the 45min, the clearance of formaldehyde reaches 96.2%, reaches the safety standard (concentration of formaldehyde≤0.08ppm) of national regulation fully.
Embodiment 3
Step 1: the preparation of three-dimensional framework polymer template; With mass ratio is that 1: 2.5 epoxy resin E-51 and polyethylene glycol mix and be heated to 80 ℃, stir became clear solution in 10 minutes after, adding and epoxy resin mass ratio are 1: 8 polyamines liquid rapidly, pour into after stirring in the polytetrafluoroethylene (PTFE) mould and finalize the design, keep setting temperature in 60 ℃, to form the solid shaped polymer blend of white after 2 hours, remove the polyethylene glycol phase with the pure water immersion fully after 5 hours, stay the epoxy resin of three-dimensional framework structure, air dry at room temperature 3 days;
Wherein the molecular weight of polyethylene glycol is 2000, and polyamines liquid is diethylenetriamine.
Step 2: D S iO
2The preparation of ultrathin membrane, the epoxy resin that is about to three-dimensional framework structure in the step 1 soaked 2 hours in positive tetraethyl orthosilicate/cyclohexylamine (mass ratio is 1: 1), and exposure formed SiO after 15 hours in 49 ℃ in ammoniacal liquor atmosphere
2/ epoxy resin composite, the heating rate with 10 ℃ in Muffle furnace rose to 900 ℃, kept can obtaining D S iO in 20 minutes with the ethanol of removing generation and the ammoniacal liquor of absorption in dry 2 hours
2Ultrathin membrane.
Step 3: D S iO
2Ultrathin membrane places 150 ℃ of dry 1h down, is immersed in then in the mixed solution of butyl titanate and cyclohexane (volume ratio is 1: 2), takes out behind the immersion 8h, dries naturally also and calcines 2h behind the hydrolysis 10h in Muffle furnace, and calcining heat is 600 ℃; Calcining back nano-TiO
2Just can load on SiO with the form of film
2On the carrier.
After testing, place this photochemical catalyst of 30g in 2 * 3 meters spaces, under the uviol lamp effect, concentration of formaldehyde drops to 0.06ppm from 1.3ppm in the 45min, the clearance of formaldehyde reaches 95.3%, reaches the safety standard (concentration of formaldehyde≤0.08ppm) of national regulation fully.
Claims (9)
1. monolithic devices photochemical catalyst, it is characterized in that described monolithic devices photochemical catalyst be with epoxy resin with three-dimensional framework structure as template, on template, be compounded with wide-aperture D S iO
2Ultrathin membrane is coated with nano-TiO as carrier on carrier
2Ultrathin membrane, the pore diameter range of described macropore is between 100nm to 2 μ m.
2. monolithic devices photochemical catalyst according to claim 1 is characterized in that described D S iO
2The porosity of ultrathin membrane is 50%～95%, and thickness is 15～90 nanometers, described nano-TiO
2The thickness of ultrathin membrane is 20～100 nanometers.
3. the preparation method of a monolithic devices photochemical catalyst is characterized in that may further comprise the steps:
1) preparation of three-dimensional framework polymer template: with mass ratio is that 1: 4～4: 1 epoxy resin and polyethylene glycol mix and be heated to 40～90 ℃, stir became clear solution in 5～15 minutes after, adding and epoxy resin mass ratio are 1: 2～1: 10 polyamines liquid, pour in the mould after stirring and finalize the design, keep setting temperature in 40～90 ℃, to form the solid shaped polymer blend of white after 1～10 hour, remove the polyethylene glycol phase with the pure water immersion after 2～20 hours, stay the epoxy resin of three-dimensional framework structure, air dry at room temperature 1～5 day;
2) D S iO
2The preparation of ultrathin membrane: the epoxy resin of the three-dimensional framework structure that step 1 is made soaked 1～5 hour in positive tetraethyl orthosilicate, formed SiO expose 10～20 hours in 30～60 ℃ in ammoniacal liquor atmosphere after
2/ epoxy resin composite, the heating rate with 5～10 ℃ in Muffle furnace rose to 600～900 ℃, kept can obtaining D S iO in 10～60 minutes with the ethanol of removing generation and the ammoniacal liquor of absorption in dry 1～5 hour
2Ultrathin membrane;
3) preparation of monolithic devices photochemical catalyst is about to D S iO
2Ultrathin membrane places 100～200 ℃ of down dry 0.5～2h, be immersed in then in the mixed solution of butyl titanate and cyclohexane, take out behind immersion 5～10h, dry naturally also and in Muffle furnace, calcine 1～3h behind hydrolysis 8～12h, calcining heat is 500～700 ℃, calcining back nano-TiO
2Just can load on SiO with the form of film
2On the carrier.
4. preparation method according to claim 3 is characterized in that described step 2 can repeatedly repeat to increase D S iO
2The thickness of ultrathin membrane or dilute positive tetraethyl orthosilicate by cyclohexylamine and reduce D S iO
2The thickness of ultrathin membrane.
5. preparation method according to claim 3 is characterized in that described step 3 can repeatedly repeat to increase TiO
2The thickness of film or reduce nano-TiO by cyclohexane dilution butyl titanate
2The thickness of film.
6. preparation method according to claim 4 is characterized in that the described cyclohexylamine and the mass ratio of positive tetraethyl orthosilicate are 1: 3～3: 1.
7. according to claim 3 or 5 described preparation methods, the volume ratio that it is characterized in that described butyl titanate and cyclohexane is 1: 3～1: 1.
8. preparation method according to claim 3 is characterized in that described polyethylene glycol is that molecular weight is one or both in 600,1000,2000,4000 or 6000.
9. preparation method according to claim 3 is characterized in that described polyamines liquid is diethylenetriamine or triethylene tetramine.
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|---|---|---|---|---|
| CN104107690A (en) * | 2013-04-18 | 2014-10-22 | 宁波大学 | [Gamma]-bismuth trioxide/silicon dioxide composite photocatalyst and preparation method thereof |
| CN104437650A (en) * | 2013-09-25 | 2015-03-25 | 宁波大学 | Ternary composite biomimetic photocatalyst and preparation method thereof |
| CN106390966A (en) * | 2016-08-31 | 2017-02-15 | 王贤福 | Photocatalytic microsphere material |
| CN107899421A (en) * | 2017-12-13 | 2018-04-13 | 深圳市格绿丝纳米科技有限公司 | A kind of photocatalysis air-cleaning filter core module processing technology |
| CN112203746A (en) * | 2018-04-26 | 2021-01-08 | Ifp 新能源公司 | Method for capturing and purifying gaseous media in the presence of a monolith comprising TiO2 and silica |
| CN112933686A (en) * | 2021-01-29 | 2021-06-11 | 云南电网有限责任公司电力科学研究院 | Preparation method of super-hydrophobic filter cloth filter element |
| CN115301223A (en) * | 2022-08-15 | 2022-11-08 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Zinc oxide or nickel oxide photocatalyst and preparation method thereof |
| CN115337920A (en) * | 2022-08-15 | 2022-11-15 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Catalyst carrier and preparation method thereof |
-
2010
- 2010-05-06 CN CN 201010165861 patent/CN102233267A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《无机化学学报》 20090731 龙能兵等 大尺寸TiO2/SiO2大孔材料的制备及光降解性能 第1153-1158页 1-9 第25卷, 第7期 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104107690A (en) * | 2013-04-18 | 2014-10-22 | 宁波大学 | [Gamma]-bismuth trioxide/silicon dioxide composite photocatalyst and preparation method thereof |
| CN104107690B (en) * | 2013-04-18 | 2016-05-25 | 宁波大学 | A kind of γ-bismuth oxide/silica composite photocatalyst and preparation method thereof |
| CN104437650A (en) * | 2013-09-25 | 2015-03-25 | 宁波大学 | Ternary composite biomimetic photocatalyst and preparation method thereof |
| CN104437650B (en) * | 2013-09-25 | 2016-08-24 | 宁波大学 | A kind of tri compound biomimetic photocatalysis agent and preparation method thereof |
| CN106390966A (en) * | 2016-08-31 | 2017-02-15 | 王贤福 | Photocatalytic microsphere material |
| CN107899421A (en) * | 2017-12-13 | 2018-04-13 | 深圳市格绿丝纳米科技有限公司 | A kind of photocatalysis air-cleaning filter core module processing technology |
| CN112203746A (en) * | 2018-04-26 | 2021-01-08 | Ifp 新能源公司 | Method for capturing and purifying gaseous media in the presence of a monolith comprising TiO2 and silica |
| CN112933686A (en) * | 2021-01-29 | 2021-06-11 | 云南电网有限责任公司电力科学研究院 | Preparation method of super-hydrophobic filter cloth filter element |
| CN115301223A (en) * | 2022-08-15 | 2022-11-08 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Zinc oxide or nickel oxide photocatalyst and preparation method thereof |
| CN115337920A (en) * | 2022-08-15 | 2022-11-15 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Catalyst carrier and preparation method thereof |
| CN115337920B (en) * | 2022-08-15 | 2023-11-03 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Catalyst carrier and preparation method thereof |
| CN115301223B (en) * | 2022-08-15 | 2023-11-21 | 诺丁汉大学卓越灯塔计划(宁波)创新研究院 | Zinc oxide or nickel oxide photocatalyst and preparation method thereof |
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Application publication date: 20111109 |