CN102198392A - Preparation method and application of carbon-wrapped titanium dioxide composite material - Google Patents
Preparation method and application of carbon-wrapped titanium dioxide composite material Download PDFInfo
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- CN102198392A CN102198392A CN2011100766604A CN201110076660A CN102198392A CN 102198392 A CN102198392 A CN 102198392A CN 2011100766604 A CN2011100766604 A CN 2011100766604A CN 201110076660 A CN201110076660 A CN 201110076660A CN 102198392 A CN102198392 A CN 102198392A
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Abstract
The invention discloses a method for preparing a carbon-wrapped titanium dioxide composite material, which comprises the following steps of: mixing 150 to 500 milligrams of titanium dioxide and 1 to 10 mass percent cane sugar solution fully with magnetic stirring in a mass ratio of 1:(2-10); putting the mixed solution into a constant temperature box, and reacting at the temperature of between 100 and 150 DEG C for 2 to 6 hours, so that cane sugar is carbonized; and grinding the obtain material into powder, and calcining at the constant temperature of between 400 and 700 DEG C in the air atmosphere for 2 to 6 hours to prepare a required product. In the carbon-wrapped titanium dioxide composite material, carbon-wrapped titanium dioxide granules can solve the problems that carbon dioxide nanometer powder is dispersed, difficult to separate and the like. The carbon-wrapped titanium dioxide composite material has large specific surface area and high adsorbability, and bonding among the granules is reduced, so the catalytic efficiency of titanium dioxide is improved.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of titanic oxide material, particularly a kind of preparation method and application thereof of carbon parcel composite titania material.
Background technology
From 1972, it is found that semi-conducting material titanium dioxide can be since brine electrolysis under the UV-irradiation produces hydrogen, titanium dioxide as a kind of photocatalytic is strong, nontoxic, inexpensive, chemical property is stable photochemical catalyst in the extensive studies that obtains Chinese scholars aspect sewage disposal, air cleaning, organic matter light degradation and the solar cell.But the practical application of titanium dioxide also is subjected to all multifactor restrictions, mainly be the wide 3.2eV of being in forbidden band of the stronger anatase titanium dioxide of photocatalytic, can only be demonstrated photocatalytic less than the ultraviolet excitation of 387.5nm by wavelength, and ultraviolet light only accounts for about 5% of sunshine, has therefore limited the utilization of titanium dioxide to sunshine greatly; Simultaneously, titanium dioxide powder exists and easily reunites, runs off when handling organic wastewater, and shortcomings such as difficult separation, difficult recovery are therefore not high to the photocatalytic degradation efficient of pollutant.Therefore, titanium dioxide being carried out modification, widen its photoresponse scope and solve it be difficult to the deficiency of separating in liguid phase pollutant, is at present both at home and abroad in the another challenging research topic in environmental improvement field.
For the photoresponse scope of expanding titanium dioxide to visible region, adopt coated metal or nonmetallic mode to reduce its energy gap usually.Since Asahi in reported first on the Science behind the nitrogen parcel titanium dioxide, the parcel nonmetalloid as: nitrogen, fluorine, sulphur and carbon etc. become the focus of research.Though it is visible light-responded that the titanium dioxide behind the parcel has, and can not guarantee that still photocatalysis efficiency effectively improves, and still not solve the difficult problem that titanium dioxide powder is difficult to separate from solution.
Summary of the invention
The objective of the invention is at the optically catalytic TiO 2 efficient for preparing in the prior art lowly, the problem that powder is difficult to separate from the aqueous solution provides the preparation method of a kind of carbon parcel composite titania material.
Another object of the present invention is to provide a kind of application process of carbon parcel composite titania material.
For achieving the above object, the technical solution adopted for the present invention to solve the technical problems is:
A kind of preparation method of carbon parcel composite titania material comprises the steps:
A, under magnetic agitation be that 1%～10% sucrose solution fully mixes according to mass ratio 1:2～10 with 150～500mg titanium dioxide and mass concentration;
B, the mixed solution of steps A is put into insulating box, under 100 ℃～150 ℃ temperature, reaction 2～6h makes the sucrose carbonization;
C, with the material of gained among the step B pulverize last in 400～700 ℃ air atmosphere calcining at constant temperature 2～6 hours, make required product.
As optimal way, among the described step C, material is grind into powder in agate mortar.
As optimal way, in the described steps A, titanium dioxide is Degussa P25 titanium dioxide.
The carbon parcel composite titania material of the inventive method preparation can be applicable to photocatalysis or photoelectric catalysis degrading organic pollution in the water processing reactor.
The application of the carbon parcel composite titania material of the inventive method preparation, the ultraviolet light and the visible light that produce with electrion carry out photocatalysis as excitation source, and the light-catalyzed reaction step is:
With the anode of porous titanium alloy material as reactor, many stainless pin parallel connections are negative electrode, add carbon parcel composite titania material in reactor, and dosage is 0.5～6g/L, and feeding flow by anode is 0.2～0.5m
3The air or oxygen of/h is degraded to pollutant.
Described reactor is pulsed discharge reactor or discharging plasma reactor.
The present invention makes the sucrose carbonization prepare the composite of graphitized carbon film wrapped titanium dioxide by heating sucrose and titanium dioxide mixed solution.The carbon film is transparent, does not influence the permeability of light and the photocatalytic of titanium dioxide; And graphitic carbon has high conductivity, is beneficial to the transmission of the electronics of titanium dioxide conduction band, improves the separative efficiency in light induced electron and hole.The granular size of the composite of the present invention preparation is between 2～5 microns, and nanometer P25 titanium dioxide particle size is about 21 nanometers, and nano titanium oxide is wrapped among the transparent carbon film, has avoided the reunion of nano-titania particle.
The nonequilibrium plasma water technology is meant in specific reactor, and the high pressure of steep-front, burst pulse is put on earth polar and the discharge electrode, and the high-strength electric field of two interpolars makes electronics moment obtain energy becomes high energy electron, with H
2O and O
2Collision is dissociated it, produces OH, HO
2, O, H, H
2O
2And O
3The isoreactivity material, the organic matter reaction in these active materials and the water makes its degraded.Ionization, transition meeting owing to molecule in the discharge process produce some physical effects, as ultra-violet radiation, ultrasonic wave, shock wave etc.The emission spectrum that the pulsed discharge process obtains shows that therefore the Wavelength distribution of light radiation, adds TiO in 200～1000 nanometer range in the pulsed discharge water processing reactor
2Photochemical catalyst can effectively utilize the ultraviolet light and the visible light of Pulsed Discharge, is the feasible method that further improves degradation efficiency and reactor energy efficiency.
Beneficial effect of the present invention is:
Material with carbon element is a kind of desirable catalyst carrier, not only strong acid-base resistance corrosion, and also chemical property is stable.Carbon parcel titanium dioxide nanoparticle can solve problems such as the carbon dioxide nano-powder disperses, difficult separation.Carbon parcel composite titania material specific area is big, and excellent adsorption has reduced intergranular bonding, thereby has improved the catalytic efficiency of titanium dioxide.
The specific embodiment
Disclosed all features in this specification, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Embodiment 1: the preparation method of carbon parcel composite titania material comprises the steps:
(1) the 150mg sucrose dissolved being made mass fraction in the 20ml water is 1% sucrose solution;
(2) under magnetic agitation, fully mix in the sucrose solution with 20mgDegussa P25 titanium dioxide adding 1%;
(3) drying box of mixed solution being put into 100 ℃ heated 12 hours, made the sucrose carbonization;
(4) grind into powder in agate mortar of the composite material after the carbonization is put into activation furnace is raised to 500 ℃ with the heating rate of 2-5 ℃/min air atmosphere calcining at constant temperature 2 hours then.Promptly obtain phosphorus content and be 0.5% carbon parcel composite titania material.
Embodiment 2: the preparation method of carbon parcel composite titania material comprises the steps:
(1) the 500mg sucrose dissolved being made mass fraction in the 50ml water is 1% sucrose solution;
(2) under magnetic agitation, fully mix in the sucrose solution with 500mgDegussa P25 titanium dioxide adding 1%;
(3) drying box of mixed solution being put into 150 ℃ heated 6 hours, made the sucrose carbonization;
(4) grind into powder in agate mortar of the composite material after the carbonization is put into activation furnace is raised to 600 ℃ with the heating rate of 2～5 ℃/min air atmosphere calcining at constant temperature 4 hours then.Promptly obtain phosphorus content and be 1.5% carbon parcel composite titania material.
Embodiment 3: the preparation method of carbon parcel composite titania material comprises the steps:
(1) the 150mg sucrose dissolved being made mass fraction in the 40ml water is 5% sucrose solution;
(2) under magnetic agitation, fully mix in the sucrose solution with 20mgDegussa P25 titanium dioxide adding 5%;
(3) drying box of mixed solution being put into 150 ℃ heated 8 hours, made the sucrose carbonization;
(4) grind into powder in agate mortar of the composite material after the carbonization is put into activation furnace is raised to 600 ℃ with the heating rate of 2-5 ℃/min air atmosphere calcining at constant temperature 4 hours then.Promptly obtain phosphorus content and be 3% carbon parcel composite titania material.
Embodiment 4: the preparation method of carbon parcel composite titania material comprises the steps:
(1) the 5g sucrose dissolved being made mass fraction in the 50ml water is 10% sucrose solution;
(2) under magnetic agitation, fully mix in the sucrose solution with 50mgDegussa P25 titanium dioxide adding 10%;
(3) drying box of mixed solution being put into 150 ℃ heated 12 hours, made the sucrose carbonization;
(4) grind into powder in agate mortar of the composite material after the carbonization is put into activation furnace is raised to 700 ℃ with the heating rate of 2～5 ℃/min air atmosphere calcining at constant temperature 6 hours then.Promptly obtain phosphorus content and be 5% carbon parcel composite titania material.
Embodiment 5: present embodiment is a photochemical catalyst for wrapping up composite titania material with carbon, the application process in the pulsed discharge water processing reactor.
With the anode of porous titanium alloy material as the pulsed discharge water processing reactor, 5 stainless pin parallel connections are negative electrode, by the porous anode aerating oxygen, in reactor, add carbon parcel composite titania material 0.5g/L, simulating pollution thing methyl orange is degraded.
Experimental condition: electrode spacing is 13mm, and oxygen flow is 0.18m
3/ h, methyl orange solution concentration is 80mg/L, and treating capacity is 250mL, and pulse voltage is 40kV, and frequency is 110Hz, degradation time 6min.
As a comparison, in reactor, do not add carbon parcel composite titania material under the same terms, simulating pollution thing methyl orange is degraded.
Result of the test shows: when not adding carbon parcel composite titania material, the degradation rate of methyl orange is 80%, and when adding carbon parcel composite titania material, the degradation rate of methyl orange is 90%.Explanation produces at high pressure pulse discharge under the effect of ultraviolet light, and carbon parcel composite titania material has good photocatalysis, can increase substantially the energy efficiency of discharge reactor.
Embodiment 5: present embodiment is photocatalysis for wrapping up composite titania material with carbon, the application process in the pulsed discharge water processing reactor.
With the anode of porous titanium alloy material as the gas-liquid mixed discharge plasma reactor, 5 stainless pin parallel connections are negative electrode, in reactor, add 1.5g/L carbon parcel composite titania material,, simulating pollution thing methyl orange is degraded by the porous anode aerating oxygen.
Experimental condition: electrode spacing is 13mm, and oxygen flow is 0.18m
3/ h, methyl orange solution concentration is 80mg/L, and treating capacity is 250mL, and pulse voltage is 40kV, and frequency is 110Hz, degradation time 6min.
As a comparison, in reactor, do not add carbon parcel composite titania material under the same terms, simulating pollution thing methyl orange is degraded.
Result of the test shows: during without the titanium dioxide of carbon parcel, the degradation rate of methyl orange is 80%, when adding carbon parcel composite titania material, the degradation rate of methyl orange is 94%, explanation produces under the effect of ultraviolet light at high pressure pulse discharge, carbon parcel composite titania material has good photocatalysis, can increase substantially the energy efficiency of discharge reactor.
Embodiment 6: present embodiment is photocatalysis for wrapping up composite titania material with carbon, the application process in the pulsed discharge water processing reactor.
With the anode of porous titanium alloy material as the gas-liquid mixed discharge plasma reactor, 5 stainless pin parallel connections are negative electrode, carbon parcel composite titania material addition in reactor is 3g/L, by the porous anode aerating oxygen, simulating pollution thing methyl orange is degraded.
Experimental condition: electrode spacing is 13mm, and oxygen flow is 0.18m
3/ h, methyl orange solution concentration is 80mg/L, and treating capacity is 250mL, and pulse voltage is 40kV, and frequency is 110Hz, degradation time 6min.
Result of the test shows: the degradation rate of methyl orange is 97%, illustrates under the effect of Pulsed Discharge ultraviolet light, and carbon parcel composite titania material has good photocatalysis, can increase substantially the energy efficiency of discharge reactor.
Embodiment 7: present embodiment is photocatalysis for wrapping up composite titania material with carbon, the application process in the pulsed discharge water processing reactor.
With the anode of porous titanium alloy material as the gas-liquid mixed discharge plasma reactor, 5 stainless pin parallel connections are negative electrode, carbon parcel composite titania material addition in reactor is 6g/L, by the porous anode aerating oxygen, simulating pollution thing methyl orange is degraded.
Experimental condition: electrode spacing is 13mm, and oxygen flow is 0.18m
3/ h, methyl orange solution concentration is 80mg/L, and treating capacity is 250mL, and pulse voltage is 40kV, and frequency is 110Hz, degradation time 6min.
As a comparison, under the same terms, add the titanium dioxide optical catalyst that does not wrap up carbon of equivalent, simulating pollution thing methyl orange is degraded.
Result of the test shows: when adding the titanium dioxide optical catalyst that does not wrap up carbon, the degradation rate of methyl orange is 95%, when adding carbon parcel composite titania material, the degradation rate of methyl orange is 98%, explanation is under the effect of Pulsed Discharge ultraviolet light, carbon parcel composite titania material has good photocatalysis, can increase substantially the energy efficiency of discharge reactor, and carbon parcel composite titania material has better photocatalysis than the titanium dioxide optical catalyst that does not wrap up.
The present invention is not limited to the aforesaid specific embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (6)
1. the preparation method of a carbon parcel composite titania material is characterized in that comprising the steps:
A, under magnetic agitation be that 1%～10% sucrose solution fully mixes according to mass ratio 1:2～10 with 150～500mg titanium dioxide and mass concentration;
B, the mixed solution of steps A is put into insulating box, under 100 ℃～150 ℃ temperature, reaction 2～6h makes the sucrose carbonization;
C, with the material of gained among the step B pulverize last in 400～700 ℃ air atmosphere calcining at constant temperature 2～6 hours, make required product.
2. the preparation method of a kind of carbon parcel composite titania material as claimed in claim 1, it is characterized in that: among the described step C, material is grind into powder in agate mortar.
3. the preparation method of a kind of carbon parcel composite titania material as claimed in claim 1, it is characterized in that: in the described steps A, titanium dioxide is Degussa P25 titanium dioxide.
4. the application of the carbon parcel composite titania material of method preparation according to claim 1 is characterized in that: be applied to photocatalysis or photoelectric catalysis degrading organic pollution in the water processing reactor.
5. the application of carbon parcel composite titania material as claimed in claim 4, it is characterized in that: the ultraviolet light and the visible light that produce with electrion carry out photocatalysis as excitation source, and the light-catalyzed reaction step is:
With the anode of porous titanium alloy material as reactor, many stainless pin parallel connections are negative electrode, add carbon parcel composite titania material in reactor, and dosage is 0.5～6g/L, and feeding flow by anode is 0.2～0.5m
3The air or oxygen of/h is degraded to pollutant.
6. as the application of claim 4 or 5 described carbon parcel composite titania materials, it is characterized in that: described reactor is pulsed discharge reactor or discharging plasma reactor.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103028386A (en) * | 2012-12-21 | 2013-04-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Ti<3+> and carbon codoped TiO2 photocatalyst with visible-light activity and preparation method of TiO2 photocatalyst |
| CN104852023A (en) * | 2015-04-01 | 2015-08-19 | 廖楚宏 | Carbon composite material and preparation method therefor |
| CN109876791A (en) * | 2017-12-06 | 2019-06-14 | 中国石油化工股份有限公司 | A kind of ozone oxidation catalyst and preparation method thereof |
| CN110240429A (en) * | 2019-05-14 | 2019-09-17 | 上海万铭环保科技股份有限公司 | A kind of preparation method of carbon package titanium dioxide nanocrystalline exterior wall dressing agent |
| CN111111659A (en) * | 2020-01-17 | 2020-05-08 | 中山大学 | Method for preparing carbon dioxide reduction photocatalyst by utilizing saccharides and metal ions |
| CN113083273A (en) * | 2021-04-13 | 2021-07-09 | 四川微纳之光科技有限公司 | Method for modifying titanium dioxide by plasma-induced carbon doping and photocatalyst |
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| CN1857769A (en) * | 2006-04-20 | 2006-11-08 | 华中师范大学 | Low temperature process of preparing carbon-doped mesoporous TiO2 visible light catalyst |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028386A (en) * | 2012-12-21 | 2013-04-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Ti<3+> and carbon codoped TiO2 photocatalyst with visible-light activity and preparation method of TiO2 photocatalyst |
| CN103028386B (en) * | 2012-12-21 | 2014-11-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Ti<3+> and carbon codoped TiO2 photocatalyst with visible-light activity and preparation method of TiO2 photocatalyst |
| CN104852023A (en) * | 2015-04-01 | 2015-08-19 | 廖楚宏 | Carbon composite material and preparation method therefor |
| CN109876791A (en) * | 2017-12-06 | 2019-06-14 | 中国石油化工股份有限公司 | A kind of ozone oxidation catalyst and preparation method thereof |
| CN109876791B (en) * | 2017-12-06 | 2021-10-08 | 中国石油化工股份有限公司 | Ozone oxidation catalyst and preparation method thereof |
| CN110240429A (en) * | 2019-05-14 | 2019-09-17 | 上海万铭环保科技股份有限公司 | A kind of preparation method of carbon package titanium dioxide nanocrystalline exterior wall dressing agent |
| CN111111659A (en) * | 2020-01-17 | 2020-05-08 | 中山大学 | Method for preparing carbon dioxide reduction photocatalyst by utilizing saccharides and metal ions |
| CN113083273A (en) * | 2021-04-13 | 2021-07-09 | 四川微纳之光科技有限公司 | Method for modifying titanium dioxide by plasma-induced carbon doping and photocatalyst |
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