CN103551174A - Iron phosphate-wrapped photocatalytic nano titanium dioxide powder and application thereof - Google Patents
Iron phosphate-wrapped photocatalytic nano titanium dioxide powder and application thereof Download PDFInfo
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- CN103551174A CN103551174A CN201310502913.9A CN201310502913A CN103551174A CN 103551174 A CN103551174 A CN 103551174A CN 201310502913 A CN201310502913 A CN 201310502913A CN 103551174 A CN103551174 A CN 103551174A
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- titanium dioxide
- ferric phosphate
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Abstract
The invention provides photocatalytic yellow powder capable of being applied to environment purifying. Each titanium dioxide particle is wrapped by iron phosphate particles, and the degrading function of the titanium dioxide to a macromolecule organic matter is selectively shielded or weakened. The photocatalytic solid powder can be extensively applied to various organic polymer setting products, especially organic fibers or plastic products or colored paint.
Description
Technical field
The present invention relates to a kind of photocatalytic powder and production method thereof that can be applicable to the depollution of environment, this powder can be used for removing foul smell, removes harmful substance or pollutant in air, particularly as benzene, and the small-molecule substances such as formaldehyde; This powder is applied to draining or purification of water quality simultaneously, removes harmful substance and bacterium in water.By this powder of various physical means (as mediated or embedding or mixing etc.), be particularly suitable for being admixed in organic fiber or plastics.
Background technology
Air pollution has become the environmental problem of countries in the world extensive concern, and major pollutants have the volatile organic matters such as sulfide, nitrogen oxide, formaldehyde and benzene.Administering the method summary of polluting has: absorption method, ozone purification method, chemical reaction method, plant purification method, biochemical treatment process and photocatalytic degradation method etc.Because traditional purification method just shifts pollutant as filtered absorption etc., fundamentally pollution abatement, the research of therefore carrying out the technology of purifying air has strategic importance.
What photocatalytic degradation method mainly relied on is photochemical catalyst.Photochemical catalyst is that a kind of under the irradiation of light, self does not change, and but can promote the material of chemical reaction, just as the chlorophyll in the photosynthesis of plant.Concrete operation principle is that photochemical catalyst nano particle is under the light of certain wavelength irradiates, generation hole-electron pair is stimulated, the water of hole decomposition catalyst adsorption, produce hydroxyl free radical, electronics makes hydrogen reduction around become active ion-oxygen, thereby possesses extremely strong oxidation-reduction, the various pollutants of photocatalyst surface are destroyed, photocatalysis can be oxidized to nontoxic material by airborne organic pollution at normal temperatures, and can not produce secondary pollution, on not impact of environmental and human health impacts.Therefore, photocatalysis technology is considered to most promising High Technology on Environmental Protection, and has strategic meaning.
The general TiO that adopts
2photochemical catalyst is removed pollutant, in processing or use, has many difficulties, as the photochemical catalyst of using is difficult to reclaim; As photocatalysis titanium dioxide, the emulsion that forms organic articles is had to very strong photocatalytic degradation effect as macromolecular compound polyethylene acetic acid, acrylate, propyl benzene emulsion etc., when titanium dioxide is mediated in fiber or plastics, aging to fiber or plastics itself of titanium dioxide under high light catalytic action.Therefore novel nano TiO is prepared in research
2photocatalytic powder, isolated photocatalysis component is a problem that must solve to the destruction of resin.
Ferric phosphate has unique catalysis characteristics, ion-exchange capacity and electric property.Because ferric phosphate has abundant skeleton structure, research mainly concentrates on the synthetic micropore ferric phosphate material with spacious skeleton structure.The research of meso-porous nano ferric phosphate is more late, has had the synthetic report of ferric phosphate of the patterns such as one dimension tubulose, two-dimensional layer, three-dimensional manometer particle now, and the mesoporous ferric phosphate of still usining is less as the research of parcel shell.
Chinese patent literature CN-1286649A(is for photocatalytic powder, the polymer composition that contains described powder and molded article and the production method of the depollution of environment) a kind of preparation method of photocatalytic powder of the particle that wraps up titanium dioxide proposed.But this photocatalytic powder only relates to calcium salt parcel, for some, is not suitable for the system of calcium salt, and limitation must be larger.
Summary of the invention
Consider the variety of issue of conventional production photocatalytic powder, one of object of the present invention is to provide a kind of photocatalytic nanometer titania powder that is applied to the ferric phosphate parcel of the depollution of environment, this powder can be used for removing foul smell, remove harmful substance or pollutant in air, particularly as benzene, the small-molecule substances such as formaldehyde; This powder is applied to draining or purification of water quality simultaneously, removes the harmful substance in water, and kill bacteria, for flowing water system.By various physical means (as mediated or embedding or mixing etc.), this powder is particularly suitable for being admixed in organic fiber or plastics or in coating.
Two of object of the present invention is to provide a kind of production method of photocatalytic nanometer titania powder of the ferric phosphate parcel that is applied to the depollution of environment.
Three of object of the present invention is to provide a kind of organic composite that is wherein mixed with the photocatalytic powder of this depollution of environment.
Four of object of the present invention is to provide polymer molded article in a kind of organic composite of the photocatalytic powder that is wherein mixed with this depollution of environment, and this molded article can adopt various organic coloring agents.
For realizing above various objects, after conducting in-depth research, we find, to under photocatalysis titanium dioxide nano particle and certain pH value, add anion surfactant, method by autotelic deposition ferric phosphate layer pore-creating can obtain durability and strengthen, selective clear and definite micropore ferric phosphate shell, and this shell can selectively pass through little molecule pernicious gas material, make the photo-catalysis function of nano titanium oxide not weakened.When by this particle with physical method load or be combined in organic polymer medium or coating system, the durability of organic media is obviously improved, based on these, we have completed the present invention.
Therefore function of the present invention has met aforementioned all object requirements.
The preparation method of the titanium dioxide of ferric phosphate parcel of the present invention, comprises following steps:
1) adopt nano titanium oxide to mix mutually with pH cushioning liquid, after add anion surfactant, concussion dispersion.Adding of anion surfactant is in order to strengthen the adhesive effect of titanium dioxide and integument, and improves the monodispersity of titanium dioxide.
2) by certain stoichiometric proportion, molysite and phosphate are dissolved in distilled water, after stirring, add anionic surface dispersant, sonic oscillation;
3) mixed solution step 1) being obtained joins step 2) mixed solution that obtains, by lye pH adjustment value, to alkalescence, agitating heating obtains gel; After gel oven dry is ground, under atmosphere protection, successively pyrolysis under uniform temperature, calcines under high temperature.
For light-catalysed nano titanium dioxide crystal form, may be wherein anatase titanium dioxide, may be rutile-type, or mix crystal formation.Wherein mix crystal formation and can form pn knot, its anatase: when rutile-type mixed proportion is 8:2, effect is best.
For the average grain diameter of light-catalysed nano titanium oxide, preferably in 0.001～0.3 micrometer range, if being less than 0.001 micron, the average grain diameter diameter of nano titanium oxide is unfavorable for disperseing and follow-up parcel, and inapplicable in production practices; And if the average grain diameter diameter of nano titanium oxide is less than 0.3 micron, more preferably average primary particle diameter is in the scope of 0.005～0.05 micron.
Production method for light-catalysed nano titanium oxide of the present invention is not particularly limited, sulfuric acid process, chloridising all can, but the titanium dioxide of a kind of high degree of dispersion of AEROSIL200 explained hereafter is good method, wherein by certain dispersion means, can use scanning electron microscopic observation to its coherent condition.
Can be by adding alkali lye in step, as sodium carbonate, NaOH, sodium acid carbonate, ammoniacal liquor, urea etc. are controlled its pH value.
In aqueous solution, add anion surfactant, the effect of anion sub-surface activating agent is to control interfacial phenomenon, and causes electrodissolution, is conducive to the parcel of titanium dioxide, and it can be removed by the method for roasting.
The object lesson of anion surfactant has various carboxylates, as fatty acid sodium soap, and oleic acid potash soap; Various sulfonate, as neopelex, alpha-olefin sodium sulfonate, Negel, alpha-sulfo monocarboxylate, aliphatic acid sulfoalkyl ester, succinate sodium sulfonate, alkyl glycerylether sodium sulfonate; Various phosphate ester salts, as the mono phosphoric acid ester of the phosphate mono-ester/diester sodium salt of calgon, AEO and APES, dibasic acid esters sylvite; Various sulfate, as lauryl sodium sulfate, higher alcohol sulfate.These anion surfactants can be used separately, or are used in combination.
Step 2) in, select molysite as ferric nitrate, iron chloride, ferric sulfate, ferric acetate etc., phosphate has dibastic sodium phosphate, sodium dihydrogen phosphate, ammonium hydrogen phosphate etc.
The atmosphere of step 3) can be the inert atmospheres such as nitrogen, argon gas.
The pyrolysis temperature of step 3) is 200～400 ℃ of times to keep 4～6h.Sintering temperature is 400～600 ℃, and the retention time is 2～3h.
The titanium dioxide of the ferric phosphate parcel finally obtaining has unbodied ferric phosphate hole layer, and this coating can cover titanium dioxide surface particle uniformly, plays the effect of protection titanium dioxide.
Weight based on titanium dioxide is calculated, if the weight of the ferric phosphate of deposition of titanium oxide is preferably the very few effectively cladding titanium dioxide of the amount of 1～70%. porous calcium phosphate iron, starting is to the effect of protection organic polymer and pigment.Otherwise the amount of porous calcium phosphate iron is too large, make coated hole too little or sealing, light-catalysed activity does not reach requirement.
Finally complete after the controlled ferric phosphate parcel titanium dioxide in aperture, obtain having the faint yellow photocatalytic powder of porous.This powder can be used for removing foul smell, removes harmful substance or pollutant in air, particularly as benzene, and the small-molecule substances such as formaldehyde; This powder is applied to draining or purification of water quality simultaneously, removes the harmful substance in water, kill harmful bacterium.
Especially when by various physical means (as kneading, embedding, simple mixing etc.), this powder is admixed to organic polymer medium as in fiber or plastics, adopt fluorescent lamp, incandescent lamp, black light, uviol lamp, mercury lamp, xenon lamp, Halogen lamp LED sunshine to irradiate continuously or fast, can remove airborne various harmful substance as foul smell H
2s, NO
xor benzene etc., and organic fiber or plastic products itself can not decompose.
This photocatalytic powder can be added in coating, by formula, adjust, this powder can be applied in exterior coating formula, for the exploitation of the coating for wall surface of yellow exterior wall or other non-white, make coating and have and prevent that outer linear light is self-cleaning, remove the effect of airborne various pernicious gas materials.
The present invention's application has the photocatalytic powder of the depollution of environment applicable to polymer molded article, as organic fiber or shaping plastic goods or the coating that organic polymer formed.All organic polymers are had no particular limits, and can be the various polyolefin of mentioning as its concrete example, as polyethylene and polypropylene, polystyrene, polyvinyl chloride, the sub-ethene of poly-1,2-dichloro; Polyamide is as nylon; Various polyalkamers are as PEO; Various polyalcohols are as polyethylene glycol, polyvinyl alcohol; Various polyesters are as organic siliconresin, poly terephthalic acid diethylester, phenolic resins, vinyl acetal resin, poly-acetic acid esters, ABS resin, epoxy resin, styrene-acrylic resin, vinyl acetate resin, polyurethanes, Merlon, urea resin, fluororesin, phenol resin; Cellulose and various cellulose derivative, chitin, lignin, starch.Generally speaking, in the production process of polymer molded article by various physical means (as mediated, embedding, simple mixed compaction etc.), this photocatalytic powder is admixed to organic polymer medium as in fiber or plastics, total weight based on polymeric compositions, the concentration of photocatalytic powder in polymer is generally 0.1～70%, is preferably 0.5～50%.
The present invention compared with prior art has following features:
(1) integrate multi-functional, there is removing and harmful gas, sterilization, anti-oxidant, absorb ultraviolet effect;
(2) low, the environmental protection of cost;
(3) easy to use, good dispersion, mixes easily mutually with other macromolecular material; Resin is not had to destruction.
(4) Selective adsorption good, the little molecule of specific pernicious gas is had to effect.
(5) have specifically faint yellowly, be widely used.
The specific embodiment
At each following working example, will the photocatalytic powder that be applied to the depollution of environment of the present invention be described.
Embodiment 1: the titanium dioxide of 100g (P25-adopts the titanium dioxide of a kind of high degree of dispersion of AEROSIL200 explained hereafter, and average grain diameter is 21nm) is poured in 200mL water and added Na
2cO
3controlling pH value is 8.0, and adds 2g polyvinylpyrrolidone (PVP--is from Chinese traditional Chinese medicines), and fully concussion disperses.
Four water ferric nitrate 200g and ammonium dihydrogen phosphate (ADP) 400g are dissolved in 500mL distilled water to the 5g polyvinylpyrrolidone (PVP) adding after stirring, sonic oscillation; After add gained titania solution to mix, by lye pH adjustment value to 8.0, agitating heating obtains gel; After gel dry is ground under nitrogen atmosphere protection, pyrolysis 2h at 400 ℃ successively, calcining at 500 ℃.
Adopt liquid Acetaldehyde as degraded marker, the performance of the little molecular contaminants of photocatalytic degradation of the photocatalytic nanometer titania powder of mensuration ferric phosphate layer parcel:
Concrete steps are as follows: first, to the acetaldehyde solution that adds the 10mg/L of 500mL in reactor, then add 1g synthesis of nano TiO
2catalyst, magnetic agitation makes it to suspend.Lucifuge is filled air stirring 30min, makes acetaldehyde solution on the surface of catalyst, reach absorption/desorption balance, pipettes 10mL solution in centrifuge tube.Then open cooling water, and open to eliminate and carry out light-catalyzed reaction 25min, every 5min, pipette 10mL reactant liquor, after centrifugation, get supernatant and carry out visible spectrophotometry analysis.According to measurement result, judge its degradation rate to acetaldehyde.Discovery is in 2h, and the degradation rate of acetaldehyde is 100%, and methyl orange becomes colourless simultaneously.
In addition this photocatalytic powder of 300g and polyethylene terephthalate resin are adopted forcing press compacting to obtain containing the bar of 30% photocatalytic powder, used the ultra violet lamp of 246nm, resin can flavescence, aging.
This photocatalytic powder of 50g is mixed mutually with water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin can variable color, aging.
Embodiment 2: by implementing program same as Example 1, difference adopts calgon (Chinese traditional Chinese medicines) as anion surfactant, and it is identical that other all conditions all keeps, and obtains for photocatalysis pale yellow powder.The photocatalytic powder of gained, 2h can degradable acetaldehyde, and methyl orange becomes colourless simultaneously.
Mix and extrude mutually with plastic components polyethylene terephthalate resin, obtain containing the bar of 30% photocatalytic powder, used ultra violet lamp, resin one day can variable color, aging.Be used in coating system water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin can variable color through one day, aging.
Embodiment 3: by implementing program same as Example 1, difference adopts titanium dioxide (University of Fuzhou provides) particle of 15nm, and it is identical that other all conditions all keeps, and obtains for photocatalytic powder.The photocatalytic powder of gained is for degrade acetaldehyde or methyl orange, and measurement result shows that synthetic photocatalytic powder can degradable acetaldehyde to 2h, and methyl orange becomes colourless simultaneously.
Mix and extrude mutually with plastic components polyethylene terephthalate resin, obtain containing the bar of 30% photocatalytic powder, used the ultra violet lamp of 246nm, variable color in resin one day, aging.Be used in coating system water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin can variable color, aging.
Comparative example 1: adopt photocatalysis P25 to be directly used in degrade acetaldehyde or methyl orange, measurement result titanium oxide P25 powder 2h can 100% degrade acetaldehyde, and methyl orange becomes colourless.
P25 mixes and extrudes mutually with plastic components polyethylene terephthalate resin, obtains containing the bar of 30% photocatalytic powder, is used the ultra violet lamp of 246nm, and resin can variable color, aging.Be used in coating system water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin solution quick color-changing is aging.
Comparative example 2: by implementing program same as Example 1, difference is not adopt anion surfactant dispersed titanium dioxide nano particle, and it is identical that other all conditions all keeps, and obtains for photocatalytic powder.The photocatalytic powder of gained is for degrade acetaldehyde, and measurement result shows can degradable acetaldehyde, and methyl orange becomes colorless.
Photocatalytic powder is mixed and is extruded mutually with plastic components polyethylene terephthalate resin, obtains containing the bar of 30% photocatalytic powder, is used the ultra violet lamp of 246nm, and resin can flavescence, aging.Be used in coating system water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin quick color-changing is aging.
Comparative example 3: by implementing program same as Example 1, difference is that the pH value of the hierarchy of control is in neutrality 7, and it is identical that other all conditions all keeps, and obtains for photocatalytic powder.Now the sedimentation effect of ferric phosphate is poor.The photocatalytic powder of gained is for degrade acetaldehyde or methyl orange, and measurement result shows can degradable acetaldehyde, and methyl orange becomes colorless.
Photocatalytic powder is mixed and is extruded mutually with plastic components polyethylene terephthalate resin, obtains containing the bar of 30% photocatalytic powder, is used the ultra violet lamp of 246nm, and resin can variable color, aging.Be used in coating system water-soluble alcohol urea formaldehyde solution (the Dow Chemical Company's production), make the coating system of the photocatalytic powder that contains 30%, adopt the ultra violet lamp of 246nm, resin quick color-changing is aging.
Claims (10)
1. a photocatalytic nanometer titania powder for ferric phosphate parcel, is characterized in that: it comprises titania nanoparticles, at least coated one deck ferric phosphate in the titanium dioxide granule surface disperseing separately at each.
2. the photocatalytic nanometer titania powder that ferric phosphate according to claim 1 wraps up, it is characterized in that: the average grain diameter of described titanium dioxide is preferably 0.001～0.3 micron, described titanium dioxide crystal form can be anatase titanium dioxide, also can be rutile-type, or any mixing of two types.
3. the photocatalytic nanometer titania powder of ferric phosphate parcel according to claim 1, is characterized in that: in the titanium dioxide of described parcel ferric phosphate layer, the total mass ratio that ferric phosphate accounts for the titanium dioxide that has wrapped up ferric phosphate layer is 1～70%.
4. the photocatalytic nanometer titania powder that ferric phosphate according to claim 2 wraps up, it is characterized in that: when described titanium dioxide crystal form adopts two kinds to mix, wherein mix crystal formation and can form pn knot, when its anatase titanium dioxide and rutile-type mixed proportion are 8:2, effect is best.
5. a preparation method for the titania powder that ferric phosphate as claimed in claim 1 wraps up, is characterized in that: comprise the following steps:
1) adopt nano titanium oxide to mix mutually with pH cushioning liquid, after add anion surfactant, concussion dispersion; In described homogeneous mixture, the content of titanium dioxide is 50～200g/L, and the mass ratio of anion surfactant and titanium dioxide is 1:500～1:5; The concentration of pH cushioning liquid is 0.1mol/L～0.5mol/L.
2) molysite and phosphate are dissolved in distilled water to the anion surfactant adding after stirring, sonic oscillation; In described homogeneous mixture, the concentration of calcium salt soln is 0.1～150mol/L, and the concentration of phosphide is 0.1～150mol/L;
3) mixed solution step 1) being obtained joins step 2) mixed solution that obtains, with ammoniacal liquor adjust pH to alkalescence, agitating heating, after dry a gel;
4) gel dry is ground after under inert atmosphere protection, first at high temperature pyrolysis, after at high temperature calcining, obtain the faint yellow photocatalytic powder of titanium dioxide of modification.
6. in the preparation method of the titania powder of ferric phosphate parcel according to claim 5, it is characterized in that: step 1) is identical with the pH value in step 3), and pH value is 7.0～9.0.
7. in the preparation method of the titania powder of ferric phosphate parcel according to claim 5, it is characterized in that: the pyrolysis reaction temperature of step 4) is 250～400 ℃, the retention time is 4～6h.
8. in the preparation method of the titania powder of ferric phosphate parcel according to claim 5, it is characterized in that: the calcining heat of step 4) is 400～600 ℃.
9. a coating with the photocatalytic nanometer titania powder of the parcel of the ferric phosphate described in any one in claim 1-4.
10. an organic polymer medium with the photocatalytic nanometer titania powder of the parcel of the ferric phosphate described in any one in claim 1-4, total weight based on polymeric compositions, the concentration of the photocatalytic nanometer titania powder of described ferric phosphate parcel in polymer is generally 0.1～70%, is preferably 0.5～50%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413722A (en) * | 2015-11-27 | 2016-03-23 | 河南金丹乳酸科技股份有限公司 | Compound catalyst used for chemically catalyzing and oxidizing lactic acid to be derived and converted to produce pyroracemic acid |
| CN106311296A (en) * | 2016-10-19 | 2017-01-11 | 常州大学 | Preparation method of iron phosphate/yttrium phosphate composite catalyst |
| CN111389197A (en) * | 2020-03-27 | 2020-07-10 | 铭牌精工机械(山东)有限公司 | Waste gas purification treatment method |
| CN111574871A (en) * | 2020-04-23 | 2020-08-25 | 武汉中科先进技术研究院有限公司 | Modified fluorosilane composite sol, preparation method thereof, coating containing modified fluorosilane composite sol, and preparation method and application of coating |
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| JPH09276706A (en) * | 1996-04-17 | 1997-10-28 | Agency Of Ind Science & Technol | Photocatalyst particle and its production |
| CN1286649A (en) * | 1997-12-25 | 2001-03-07 | 工业技术院 | Photocatalyst powder for environmental purification, polymer composition contg. said powder and molded article thereof, and processes for producing these |
| JP2009179497A (en) * | 2008-01-30 | 2009-08-13 | Tayca Corp | Titanium oxide dispersion stable in neutral region |
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2013
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09276706A (en) * | 1996-04-17 | 1997-10-28 | Agency Of Ind Science & Technol | Photocatalyst particle and its production |
| CN1286649A (en) * | 1997-12-25 | 2001-03-07 | 工业技术院 | Photocatalyst powder for environmental purification, polymer composition contg. said powder and molded article thereof, and processes for producing these |
| JP2009179497A (en) * | 2008-01-30 | 2009-08-13 | Tayca Corp | Titanium oxide dispersion stable in neutral region |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105413722A (en) * | 2015-11-27 | 2016-03-23 | 河南金丹乳酸科技股份有限公司 | Compound catalyst used for chemically catalyzing and oxidizing lactic acid to be derived and converted to produce pyroracemic acid |
| CN106311296A (en) * | 2016-10-19 | 2017-01-11 | 常州大学 | Preparation method of iron phosphate/yttrium phosphate composite catalyst |
| CN111389197A (en) * | 2020-03-27 | 2020-07-10 | 铭牌精工机械(山东)有限公司 | Waste gas purification treatment method |
| CN111574871A (en) * | 2020-04-23 | 2020-08-25 | 武汉中科先进技术研究院有限公司 | Modified fluorosilane composite sol, preparation method thereof, coating containing modified fluorosilane composite sol, and preparation method and application of coating |
| CN111574871B (en) * | 2020-04-23 | 2021-07-23 | 武汉中科先进技术研究院有限公司 | Modified fluorosilane composite sol, preparation method thereof, coating containing modified fluorosilane composite sol, and preparation method and application of coating |
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Application publication date: 20140205 |