CN101244383A - Process for producing absorbent charcoal loading titanium dioxide photocatalyst - Google Patents
Process for producing absorbent charcoal loading titanium dioxide photocatalyst Download PDFInfo
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- CN101244383A CN101244383A CNA2008100345548A CN200810034554A CN101244383A CN 101244383 A CN101244383 A CN 101244383A CN A2008100345548 A CNA2008100345548 A CN A2008100345548A CN 200810034554 A CN200810034554 A CN 200810034554A CN 101244383 A CN101244383 A CN 101244383A
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- active carbon
- titanium dioxide
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- dioxide photocatalyst
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Abstract
The invention relates to a preparation method of activated carbon supported titanium dioxide photocatalyst, belonging to the preparation technical field of titanium dioxide photocatalyst, comprising a plurality of steps as followings: pretreating, washing and drying the activated carbon; at the condition of ice-water bath, adding meta-titanic acid and ammonia according to a molar ratio of 1:2 into 20 to 40 milliliter hydrogen peroxide with a concentration of 30%, and agitating for 50 to 70 minutes to obtain a yellowish green sol; then adding the pretreated activated carbon into the yellowish green sol and agitating for 3 to 5 hours, filtering the activated carbon after standing for 12 to 24 hours, then calcining with the protection of inert gas to obtain the activated carbon supported titanium dioxide photocatalyst. The weight ratio of the pretreated activated carbon and the meta-titanic acid is 1:1 to 3:1. The preparation method has the advantages of simple technology, cheap raw material, mild preparation conditions, easy operation, granular shape, good organic pollutant degradation effect, easy separation, regeneration and long service life of the supported photocatalyst prepared by the preparation method, nonuse of organic solvent, non-pollution in the whole production process, accordance with the requirement of sustainable development and environment-friendly integrated technology.
Description
Technical field
The invention belongs to the preparing technical field of titanium dioxide optical catalyst, be specifically related to a kind of method that is used to prepare absorbent charcoal loading titanium dioxide photocatalyst.
Background technology
TiO
2Photochemical catalyst has extensive studies and application in the fields such as purifying, air cleaning, disinfecting, antimicrobial and sewage disposal of water.TiO
2Be a kind of N-type semiconductor section bar material, its chemical property is stable, and fast light corrosion has bigger energy gap, oxidation-reduction potential height, big, the photocatalytic activity advantages of higher of light-catalyzed reaction driving force, and the chemical reaction that can make some heat absorptions is by the TiO of light radiation
2Surface accomplished and acceleration, TiO in addition
2Inexpensive, be easy to get, at the bottom of nontoxic, the cost, so TiO
2Photocatalysis research very active.Nano-TiO
2Be to study at present and most widely used photochemical catalyst.Yet, nano-TiO
2Shortcomings such as photochemical catalyst exists easy cohesion, be difficult to reclaim, active ingredient loss is big are unfavorable for the recovery and reuse of catalyst.In addition, owing to pollutant levels pending in the water are very little, be mg/L or lower all generally, pollutant and TiO during photocatalytic degradation
2Contact frequency low, cause reaction rate slower.Activated carbon supported type nano-TiO
2Photochemical catalyst then can overcome the above problems to a certain extent.
Absorbent charcoal carrier has stronger adsorptivity, organic matter can be enriched in catalyst surface, can be TiO
2The organic matter environment of high concentration is provided and accelerates pollutant photocatalytic degradation speed.Simultaneously, by diffusion, the organic matter that is adsorbed is to TiO
2Surface migration, TiO
2The organic matter of degrading activity carbon surface makes carrier realize in-situ regeneration again, and this cooperative interaction further improves TiO
2Photocatalytic activity.
At present, preparation loaded nano TiO
2The technology of photochemical catalyst is very many, mainly contains powder sintering method, sol-gel process, ion-exchange, coupling method, hydrolytic precipitation method, chemical vapour deposition technique etc.But up to now, be not the titanium source also, prepare activated carbon supported TiO by sol impregnation-calcination method with the metatitanic acid
2The report of photochemical catalyst.
Summary of the invention
The objective of the invention is to propose the preparation method of a kind of easy and simple to handle, environmental friendliness, the economic absorbent charcoal loading titanium dioxide photocatalyst that can be used for large-scale production.
The present invention proposes a kind of preparation method of absorbent charcoal loading titanium dioxide photocatalyst, and concrete steps are as follows:
(1) active carbon is carried out preliminary treatment, make activated carbon surface generate oxygen-containing functional group, cooling spends deionised water (being generally 3-5 time), oven dry;
(2) under the ice-water bath condition, metatitanic acid and ammoniacal liquor joined by 1: 2 mol ratio in 30% the 20-40ml hydrogen peroxide, stirred 50-70 minute, obtain yellow green colloidal sol;
(3) active carbon after the processing that step (1) is obtained joins in the colloidal sol that step (2) obtains, and stirs after 3-5 hour, leaves standstill after 12-24 hour active carbon is leached, and calcines under inert gas shielding, promptly obtains required product; The active carbon after the processing and the mass ratio of metatitanic acid are 1: 1-3: 1.
Among the present invention, active carbon is pulverized earlier before using in the step (1), and making its particle diameter is 50～150 orders.
Among the present invention, step is carried out preliminary treatment to active carbon in (1), can adopt diverse ways, can increase TiO
2Load capacity at activated carbon surface.As: can adopt the HNO that active carbon is placed 1-10mol/L
3In the solution or the H of 10%-30%
2O
2In the solution, under the 333K-373K temperature, soak 0.5-2h, or granular active carbon is through using O
3Handle a kind of of 1-3h.
Among the present invention, calcining heat is 500-700 ℃ in the step (3), and calcination time is 1-3 hour.
Among the present invention, can be by regulating the addition of metatitanic acid and ammoniacal liquor, the addition of active carbon and dip time are controlled TiO on the absorbent charcoal loading titanium dioxide photocatalyst
2Load capacity, the single-steeping load capacity is 0～15%, the double-steeping load capacity is 15%～25%.
Utilize structure, pattern, the content of the inventive method products therefrom, the mensuration of performance can adopt X-ray powder diffraction (XRD), SEM (SEM), specific surface area analysis instrument (BET), ultraviolet-visible spectrophotometer (UV-Vis) to characterize and measure respectively.
The invention has the advantages that:
1. technology of the present invention is simple, the raw material cheapness, and the preparation condition gentleness, easy and simple to handle, therefore, be easy to promote and industrialization.
2. obtaining loaded photocatalyst is graininess, and degradable organic pollutant is effective, is easy to separate, regenerate and increase the service life.
3. the present invention does not with an organic solvent produce the accessory substance that environment is had pollution in preparation process, and promptly whole process of production is almost pollution-free, meets the requirement of sustainable development, is a kind of environment-protecting comprehensive technology.
Description of drawings
Fig. 1 be among the embodiment 1 the XRD figure of product.
Fig. 2 is the SEM figure of products obtained therefrom among the embodiment 1.
Fig. 3 be among the embodiment 1 products obtained therefrom at 12W, under the 254nm ultraviolet light, photocatalysis effect assessment figure.
Fig. 4 be among the embodiment 1 products obtained therefrom at 12W, under the 254nm ultraviolet light, the recycling performance evaluation map of photocatalysis after 2.5 hours.
The specific embodiment
Further describe the present invention below by some embodiment.
Embodiment 1:
(1) after merchandise active carbon was pulverized, 50～100 orders sieved, and obtained granular active carbon and spent deionised water for several times, oven dry.
(2) under the ice-water bath condition, 1.5g metatitanic acid and 4.5ml ammoniacal liquor join in the hydrogen peroxide of 20mL30%, stir after 50 minutes, obtain yellow green colloidal sol.
(3) granular active carbon that 4g step (1) is obtained joins in the colloidal sol that step (2) obtains, stir 4h after, leave standstill 24h.Active carbon is leached 600 ℃ of calcining 2h under inert gas shielding.Products therefrom is anatase titanium dioxide absorbent charcoal loading titanium dioxide photocatalyst, TiO
2Content 9wt%.
Products obtained therefrom in the step (3) is characterized it with XRD, SEM respectively, and as can be seen from Fig. 1, product is the anatase phase.As can be seen from Fig. 2, TiO
2Particle relatively is evenly distributed in activated carbon surface, and the particle spheroiding has slight reunion.As can be seen from Fig. 3, the activated carbon supported TiO of this method preparation
2Photochemical catalyst has good effect of removing to methyl orange under ultraviolet light, close with the photo-catalysis capability of the P25 of same ratio and Mixture of Activated Carbon.Among Fig. 4 as seen, the activated carbon supported TiO of the method preparation
2Photochemical catalyst is after recycling 5 times, and catalytic performance is constant substantially, has well to reuse performance.
Embodiment 2:
(1) after merchandise active carbon was pulverized, 50～100 orders sieved, and obtain granular active carbon through O
3Spend deionised water to neutral, oven dry after handling 2h.
(2) under the ice-water bath condition, 1.5g metatitanic acid and 4.5ml ammoniacal liquor join in the hydrogen peroxide of 30mL30%, obtain yellow green colloidal sol behind the stirring 1h.
(3) the 4g preliminary treatment is good granular active carbon joins in the colloidal sol, behind the stirring 4h, leaves standstill 24h.Active carbon is leached 600 ℃ of calcining 2h under inert gas shielding.Products therefrom is anatase titanium dioxide absorbent charcoal loading titanium dioxide photocatalyst, TiO
2Content 13wt%.
Embodiment 3:
(1) after merchandise active carbon was pulverized, 100～150 orders sieved, and obtain powdered active carbon through O
3Spend deionised water to neutral, oven dry after handling 2h.
(2) under the ice-water bath condition, 1.0g metatitanic acid and 3ml ammoniacal liquor join in the hydrogen peroxide of 20mL30%, obtain yellow green colloidal sol after the stirring.
(3) the 3g preliminary treatment is good powdered active carbon joins in the colloidal sol, behind the stirring 4h, leaves standstill 24h.Active carbon is leached 600 ℃ of calcining 2h under inert gas shielding.Products therefrom is anatase titanium dioxide absorbent charcoal loading titanium dioxide photocatalyst, TiO
2Content 10wt%.
Embodiment 4:
(1) after merchandise active carbon was pulverized, 100～150 orders sieved, and obtain the HNO that powdered active carbon places 10mol/L
3In the solution, under the 333K temperature, soak 1h, after spend deionised water to neutral, oven dry.
(2) under the ice-water bath condition, 1.5g metatitanic acid and 4.5ml ammoniacal liquor join in the hydrogen peroxide of 20mL30%, obtain yellow green colloidal sol behind the stirring 1h.
(3) the 4g preliminary treatment is good powdered active carbon joins in the colloidal sol, behind the stirring 2h, leaves standstill 20h.Active carbon is leached 600 ℃ of calcining 2h under inert gas shielding.Products therefrom is anatase titanium dioxide absorbent charcoal loading titanium dioxide photocatalyst, TiO
2Content 15wt%.
Embodiment 5:
(4) after merchandise active carbon was pulverized, 50～100 orders sieved, and obtain the HNO that granular active carbon places 10mol/L
3In the solution, under the 333K temperature, soak 1h, after spend deionised water for several times, oven dry.
(5) under the ice-water bath condition, 1.5g metatitanic acid and 4.5ml ammoniacal liquor join in the hydrogen peroxide of 20mL30%, obtain yellow green colloidal sol behind the stirring 1h.
(6) the 4g preliminary treatment is good granular active carbon joins in the colloidal sol, behind the stirring 4h, leaves standstill 24h.Active carbon is leached 700 ℃ of calcining 2h under inert gas shielding.Products therefrom is anatase titanium dioxide absorbent charcoal loading titanium dioxide photocatalyst, TiO
2Content 15wt%.
Claims (4)
1, a kind of preparation method of absorbent charcoal loading titanium dioxide photocatalyst is characterized in that concrete steps are as follows:
(1) active carbon is carried out preliminary treatment, make activated carbon surface generate oxygen-containing functional group, cooling spends deionised water, oven dry;
(2) under the ice-water bath condition, metatitanic acid and ammoniacal liquor joined by 1: 2 mol ratio in 30% the 20-40ml hydrogen peroxide, stirred 50-70 minute, obtain yellow green colloidal sol;
(3) active carbon after the processing that step (1) is obtained joins in the colloidal sol that step (2) obtains, and stirs after 3-5 hour, leaves standstill after 12-24 hour active carbon is leached, and calcines under inert gas shielding, promptly obtains required product; The active carbon after the processing and the mass ratio of metatitanic acid are 1: 1-3: 1.
2, the preparation method of absorbent charcoal loading titanium dioxide photocatalyst according to claim 1 is characterized in that active carbon is pulverized earlier before using in the step (1), and making its particle diameter is 50～100 orders.
3, the preparation method of absorbent charcoal loading titanium dioxide photocatalyst according to claim 1 is characterized in that in the step (1) active carbon being carried out preliminary treatment, adopts the HNO that active carbon is placed 1-10mol/L
3In the solution or the H of 10%-30%
2O
2In the solution, under the 333K-373K temperature, soak 0.5-2h, or granular active carbon is through using O
3Handle a kind of of 1-3h.
4, the preparation method of absorbent charcoal loading titanium dioxide photocatalyst according to claim 1 is characterized in that calcining heat is 500-700 ℃ in the step (3), and calcination time is 1-3 hour.
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| CN102188955A (en) * | 2010-03-03 | 2011-09-21 | 株式会社科特拉 | Optical-regenerable absorption material and use thereof |
| CN102580727A (en) * | 2011-01-11 | 2012-07-18 | 同济大学 | Preparation method of active carbon loaded titanium dioxide silver-doped photochemical catalyst |
| US20120232261A1 (en) * | 2009-09-15 | 2012-09-13 | Ildong Pharm Co., Ltd. | Method for manufacturing low molecular weight hyaluronic acid |
| CN102978902A (en) * | 2012-12-26 | 2013-03-20 | 西南大学 | Natural color-rendering sorting method for polyester fabrics |
| CN103021666A (en) * | 2012-12-03 | 2013-04-03 | 彩虹集团公司 | Method for preparing compound titanium dioxide film |
| CN103100378A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of activated carbon fiber loaded titanium dioxide photocatalyst |
| CN103599766A (en) * | 2013-11-25 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Catalyst for photocatalytic water splitting hydrogen production and preparation method and application of catalyst |
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| CN104399447A (en) * | 2014-11-24 | 2015-03-11 | 东北大学 | Method for preparing photocatalyst by immersing blast-furnace slags with dilute acid and using filtrate loaded with activated carbon |
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| US20120232261A1 (en) * | 2009-09-15 | 2012-09-13 | Ildong Pharm Co., Ltd. | Method for manufacturing low molecular weight hyaluronic acid |
| CN102188955A (en) * | 2010-03-03 | 2011-09-21 | 株式会社科特拉 | Optical-regenerable absorption material and use thereof |
| CN102188955B (en) * | 2010-03-03 | 2015-12-09 | 株式会社科特拉 | Can the sorbing material of photo reversal and utilization thereof |
| CN102580727A (en) * | 2011-01-11 | 2012-07-18 | 同济大学 | Preparation method of active carbon loaded titanium dioxide silver-doped photochemical catalyst |
| CN102580727B (en) * | 2011-01-11 | 2013-12-04 | 同济大学 | Preparation method of active carbon loaded titanium dioxide silver-doped photochemical catalyst |
| CN103100378A (en) * | 2011-11-09 | 2013-05-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of activated carbon fiber loaded titanium dioxide photocatalyst |
| CN103021666A (en) * | 2012-12-03 | 2013-04-03 | 彩虹集团公司 | Method for preparing compound titanium dioxide film |
| CN102978902B (en) * | 2012-12-26 | 2014-07-09 | 西南大学 | Natural color-rendering sorting method for polyester fabrics |
| CN102978902A (en) * | 2012-12-26 | 2013-03-20 | 西南大学 | Natural color-rendering sorting method for polyester fabrics |
| CN103599766A (en) * | 2013-11-25 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Catalyst for photocatalytic water splitting hydrogen production and preparation method and application of catalyst |
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| CN103785371A (en) * | 2014-03-04 | 2014-05-14 | 湘潭大学 | Porous carbon microsphere @TiO2 composite material and preparation method and application thereof |
| CN104399447A (en) * | 2014-11-24 | 2015-03-11 | 东北大学 | Method for preparing photocatalyst by immersing blast-furnace slags with dilute acid and using filtrate loaded with activated carbon |
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