CN101940920A - Method for preparing modified bauxite supported titanium dioxide - Google Patents
Method for preparing modified bauxite supported titanium dioxide Download PDFInfo
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- CN101940920A CN101940920A CN 201010289026 CN201010289026A CN101940920A CN 101940920 A CN101940920 A CN 101940920A CN 201010289026 CN201010289026 CN 201010289026 CN 201010289026 A CN201010289026 A CN 201010289026A CN 101940920 A CN101940920 A CN 101940920A
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- bauxite
- ethyl alcohol
- titanium dioxide
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Abstract
The invention relates to a method for preparing modified bauxite supported titanium dioxide, and the photocatalytic property of the titanium dioxide for degrading methyl orange under ultraviolet light is researched. The method comprises the following steps of: (1) adding a certain amount of butyl titanate into absolute ethyl alcohol and rapidly stirring for 1 hour to form light yellow transparent sol; (2) performing hydrothermal treatment on raw bauxite at the temperature of between 130 and 170 DEG C for 48 to 72 hours, drying at the temperature of 110 DEG C, calcining at the temperature of 400 DEG C for 4 hours, adding a certain amount of absolute ethyl alcohol and stirring to form suspension of the modified bauxite; and (3) slowly dripping the sol into the suspension of the modified bauxite, stirring for 1 hour in a sealed mode, stirring in an open mode until all absolute ethyl alcohol is volatilized, drying and calcining. The modified bauxite is adopted as a carrier, acid and alkali are not needed to be added in the preparation process, nano titanium dioxide with small grain size is prepared, and the preparation method has the characteristics of simpleness, convenience and low cost.
Description
Technical field
The invention belongs to chemical field, more specifically relating to a kind of is the preparation method of carrier loaded titanium dioxide with modified bauxite.
Background technology
Along with deepening continuously of process of industrialization, global environmental pollution is serious day by day.Reported light radiation TiO in photocell from Fujishima in 1972 and Honda
2The redox reaction of water can take place and produced since the hydrogen TiO
2, advantages such as catalytic activity high, non-selectivity, good stability nontoxic with it become the photochemical catalyst of being paid attention to most and having broad prospect of application.But owing to using TiO
2There are problems such as easily cohesion, difficult recovery, cost height during powder-processed waste water, restricted its extensive use.Therefore develop a kind of high photocatalysis performance that has, easily recovery and loaded photocatalyst with low cost have crucial meaning.Existing a lot of at present researchers attempt being fixed, and are carried on the carrier, as glass, pottery, fiber, active carbon, zeolite, silica gel etc.
Publication number discloses the method for a kind of metal surface loaded titanium dioxide photocatalyst for " CN 1410158A ", this method is pressed the clean metal surface successively, in acid medium, anodic oxidation is carried out in the metal surface, hydrolysis process, and then under the weak base condition, be raw material with butyl titanate and titanium dioxide, with colloidal sol-gel-suspending powder method lixiviate, smear film forming, carry out in steps such as proper temperature calcinations.Its technology is comparatively complicated, has used acid, organic solvents such as alkali, and cost is higher.
Modified bauxite used among the present invention has bigger specific area because of the special of its structure, chemical property is stable, and characteristics such as high adsorption capacity can be used as desirable catalyst carrier.Butyl titanate utilizes airborne moisture to be hydrolyzed, and need not to add soda acid and regulates its hydrolysis rate, has reduced production cost, has avoided the influence of the inorganic ions in the soda acid to catalyst efficiency simultaneously.The sample for preparing can be used as adsorbent and catalyst carrier is having good prospects for application aspect processing waste water and the waste gas.
Summary of the invention
The objective of the invention is to overcome the problem that existing catalyst difficulty reclaims, cost is high, providing a kind of is the preparation method of the composite photo-catalyst of carrier loaded titanium dioxide with modified bauxite, prepared sample has been realized the immobilized of titanium dioxide, is convenient to reclaim, and has reduced cost.
Comprise the steps:
(1) butyl titanate is added in the absolute ethyl alcohol, and the volume ratio of absolute ethyl alcohol and butyl titanate is 2.5:1, and 1h is stirred in sealing fast, forms the Sol A of transparent faint yellow, and is stand-by;
(2) former bauxite is placed in the band teflon-lined autoclave, 130-170 ℃ of following hydro-thermal 48-72h, 110 ℃ of dry 4h, 400 ℃ of roasting 4h naturally cool to room temperature.The absolute ethyl alcohol that adds 7-12ml, ultrasonic 10min stirs 1h, and forming mass fraction is the suspension B of the modified bauxite of 15-25%;
(3) Sol A is slowly splashed into the suspension B of modified bauxite, 1h is stirred in sealing earlier, and open then the stirring all volatilized until absolute ethyl alcohol; 110 ℃ of dry 8h, 400 ℃ of roasting 4h naturally cool to room temperature, obtain powder sample.
Preparation method's of the present invention advantage is:
(1) with the modified bauxite is carrier.Bauxite after the modification has big specific area, not only can realize TiO
2Immobilized, and its big specific area can be adsorbed to TiO effectively with the organic matter in the waste water
2Grain surface, the contact probability of increase catalyst and pollutant reaches the raising the disposal efficiency, increases the purpose of degradation rate; Strengthen its photocatalytic activity;
(2) preparation method is simple.Compare with traditional sol-gal process, in the preparation process of the present invention, butyl titanate utilizes airborne moisture to be hydrolyzed, and need not to add soda acid and regulates its hydrolysis rate.Divide lessly because of water in air, so hydrolysis rate is slow and stable, helps forming the less and uniform particle of size; And avoided the influence of the inorganic ions in the soda acid to catalyst efficiency.
(3) realize the immobilized of titanium dioxide, be convenient to reclaim, reduced cost asepsis environment-protecting.
Description of drawings
Fig. 1 is the activity figure of the prepared different catalysts degraded methyl orange of the inventive method.
A: bauxite carrier, b:20%-TiO
2/ bauxite,, c:40%-TiO
2/ bauxite,, d:60%-TiO
2/ bauxite,, e:Pure TiO
2
The specific embodiment
Embodiment 1
(1) get the 2.19ml butyl titanate and be added in the absolute ethyl alcohol, the volume ratio of absolute ethyl alcohol and butyl titanate is 1.5:1, and 1h is stirred in sealing fast, forms the Sol A of transparent faint yellow, and is stand-by;
(2) former bauxite is placed in the band teflon-lined autoclave, 150 ℃ of following hydro-thermal 60h, 110 ℃ of dry 4h, 400 ℃ of roasting 4h naturally cool to room temperature.Add the 7mL absolute ethyl alcohol, ultrasonic 10min stirs 1h, forms mass fraction and be the suspension B of 15% modified bauxite;
(3) Sol A is slowly splashed into the suspension B of modified bauxite, 1h is stirred in sealing earlier, and open then the stirring all volatilized until absolute ethyl alcohol; 110 ℃ of dry 8h, 400 ℃ of roasting 4h naturally cool to room temperature, obtain powder sample.
This be in the composite photo-catalyst of carrier loaded titanium dioxide with modified bauxite, the about titanium dioxide of load 20% mass fraction.With 5 * 10
-5The methyl orange solution of mol/L carries out the photocatalysis experiment for the degraded object, gets the 100mg powder sample, and the 100ml methyl orange solution is a light source with the 400w/D metal halide lamp.Every 10min gets sample one time, uses ultraviolet specrophotometer according to its absorbance change calculations degradation rate.Behind embodiment 1 prepared photochemical catalyst 60min, degradation rate is 25.63%.
Embodiment 2
(1) get the 5.68ml butyl titanate and be added in the absolute ethyl alcohol, the volume ratio of absolute ethyl alcohol and butyl titanate is 2.5:1, and 1h is stirred in sealing fast, forms the Sol A of transparent faint yellow, and is stand-by;
(2) former bauxite is placed in the band teflon-lined autoclave, 130 ℃ of following hydro-thermal 72h, 110 ℃ of dry 4h, 400 ℃ of roasting 4h naturally cool to room temperature.Add the 10mL absolute ethyl alcohol, ultrasonic 10min stirs 1h, forms mass fraction and be the suspension B of 20% modified bauxite;
(3) Sol A is slowly splashed into the suspension B of modified bauxite, 1h is stirred in sealing earlier, and open then the stirring all volatilized until absolute ethyl alcohol; 110 ℃ of dry 8h, 400 ℃ of roasting 4h naturally cool to room temperature, obtain powder sample.
This be in the composite photo-catalyst of carrier loaded titanium dioxide with modified bauxite, approximately load the titanium dioxide of 40% mass fraction.Test its photocatalysis performance with experiment condition identical among the embodiment 1.Behind the 60min, its degradation rate reaches 95.48%.
Embodiment 3
(1) get the 12.78ml butyl titanate and be added in the absolute ethyl alcohol, the volume ratio of absolute ethyl alcohol and butyl titanate is 3.5:1, and 1h is stirred in sealing fast, forms the Sol A of transparent faint yellow, and is stand-by;
(2) former bauxite is placed in the band teflon-lined autoclave, 170 ℃ of following hydro-thermal 48h, 110 ℃ of dry 4h, 400 ℃ of roasting 4h naturally cool to room temperature.Add the 12mL absolute ethyl alcohol, ultrasonic 10min stirs 1h, forms mass fraction and be the suspension B of 25% modified bauxite;
(3) Sol A is slowly splashed into the suspension B of modified bauxite, 1h is stirred in sealing earlier, and open then the stirring all volatilized until absolute ethyl alcohol; 110 ℃ of dry 8h, 400 ℃ of roasting 4h naturally cool to room temperature, obtain powder sample.
This be in the composite photo-catalyst of carrier loaded titanium dioxide with modified bauxite, approximately load the titanium dioxide of 60% mass fraction.Test its photocatalysis performance with experiment condition identical among the embodiment 1.Behind the 60min, its degradation rate is 63.75%.
Comparative Examples 1
Get the 12.78ml butyl titanate and be added in the absolute ethyl alcohol, the volume ratio of absolute ethyl alcohol and butyl titanate is 2.5:1, and 1h is stirred in sealing fast, and open then the stirring all volatilized until absolute ethyl alcohol; 110 ℃ of dryings, 400 ℃ of roasting 4h obtain the pure titinium dioxide powder sample.
Get the pure titinium dioxide suitable and test its photocatalysis performance with experiment condition identical among the embodiment 1 with each sample load capacity.Behind the 60min, its degradation rate is 61.64%.
Claims (3)
1. one kind is the preparation method of carrier loaded titanium dioxide with modified bauxite, it is characterized in that: comprise the steps:
(1) butyl titanate joins in the absolute ethyl alcohol, and the volume ratio of absolute ethyl alcohol and butyl titanate is 1.5-3.5:1, and 1h is stirred in sealing fast, forms faint yellow vitreosol A;
(2) former bauxite is placed in the band teflon-lined autoclave, behind 130 ~ 170 ℃ of following hydro-thermal 48-72h, take out at 110 ℃ of dry 4h, 400 ℃ of roasting 4h are cooled to room temperature; The absolute ethyl alcohol that adds 7-12mL, ultrasonic 10min stirs 1h, and forming mass fraction is the suspension B of the modified bauxite of 15-25%;
(3) Sol A is slowly splashed into the suspension B of modified bauxite, 1h is stirred in sealing earlier, and openly then be stirred to absolute ethyl alcohol and all volatilize, 110 ℃ of dry 8h, 400 ℃ of roasting 4h are cooled to room temperature and obtain powder sample.
2. as claimed in claim 1 is the preparation method of carrier loaded titanium dioxide with modified bauxite, and it is characterized in that: used carrier is a modified bauxite, and specific area is big, and the composition that itself contains helps improving catalyst activity.
3. as claimed in claim 1 is the preparation method of carrier loaded titanium dioxide with modified bauxite, and it is characterized in that: prepared powder sample has photocatalytic.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007911A (en) * | 2012-12-01 | 2013-04-03 | 福州大学 | Preparation method of compound catalyst for surface treating agent |
| CN104549542A (en) * | 2013-10-28 | 2015-04-29 | 福建三聚福大化肥催化剂国家工程研究中心有限公司 | Carrier, carbonyl sulfide hydrolysis catalyst based on carrier and preparation method of carbonyl sulfide hydrolysis catalyst |
| CN105994261A (en) * | 2016-06-06 | 2016-10-12 | 佛山市聚成生化技术研发有限公司 | Photodegradable organophosphorus pesticide insecticide preparation method and photodegradable organophosphorus pesticide insecticide prepared by method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242880A (en) * | 1992-05-27 | 1993-09-07 | Eastman Kodak Company | Photoactive catalyst of barium phosphate or calcium phosphate supported on anatase titanium dioxide |
| CN1400158A (en) * | 2001-08-07 | 2003-03-05 | 福州大学化肥催化剂国家工程研究中心 | High-temp. conversion catalyst for preparing impregnated load type CO by using bauxite as carrier |
| CN1425497A (en) * | 2003-01-07 | 2003-06-25 | 福州大学 | Preparing CO sulfur-resistant changing catalyst by active bauxite ore |
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2010
- 2010-09-21 CN CN2010102890264A patent/CN101940920B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5242880A (en) * | 1992-05-27 | 1993-09-07 | Eastman Kodak Company | Photoactive catalyst of barium phosphate or calcium phosphate supported on anatase titanium dioxide |
| CN1400158A (en) * | 2001-08-07 | 2003-03-05 | 福州大学化肥催化剂国家工程研究中心 | High-temp. conversion catalyst for preparing impregnated load type CO by using bauxite as carrier |
| CN1425497A (en) * | 2003-01-07 | 2003-06-25 | 福州大学 | Preparing CO sulfur-resistant changing catalyst by active bauxite ore |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007911A (en) * | 2012-12-01 | 2013-04-03 | 福州大学 | Preparation method of compound catalyst for surface treating agent |
| CN103007911B (en) * | 2012-12-01 | 2014-04-30 | 福州大学 | Preparation method of compound catalyst for surface treating agent |
| CN104549542A (en) * | 2013-10-28 | 2015-04-29 | 福建三聚福大化肥催化剂国家工程研究中心有限公司 | Carrier, carbonyl sulfide hydrolysis catalyst based on carrier and preparation method of carbonyl sulfide hydrolysis catalyst |
| CN104549542B (en) * | 2013-10-28 | 2017-02-01 | 福建三聚福大化肥催化剂国家工程研究中心有限公司 | Carrier, carbonyl sulfide hydrolysis catalyst based on carrier and preparation method of carbonyl sulfide hydrolysis catalyst |
| CN105994261A (en) * | 2016-06-06 | 2016-10-12 | 佛山市聚成生化技术研发有限公司 | Photodegradable organophosphorus pesticide insecticide preparation method and photodegradable organophosphorus pesticide insecticide prepared by method |
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