CN101992112A - Titanium oxide coating/ceramic structural catalyst carrier and preparation method thereof - Google Patents
Titanium oxide coating/ceramic structural catalyst carrier and preparation method thereof Download PDFInfo
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- CN101992112A CN101992112A CN2009100134448A CN200910013444A CN101992112A CN 101992112 A CN101992112 A CN 101992112A CN 2009100134448 A CN2009100134448 A CN 2009100134448A CN 200910013444 A CN200910013444 A CN 200910013444A CN 101992112 A CN101992112 A CN 101992112A
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Abstract
The invention belongs to the field of structural catalyst carriers and particularly relates to a ceramic matrix structural catalyst carrier with a nanometer titanium oxide coating and a preparation method thereof. The application of the carrier can achieve the purposes of enhancing the mass and heat transferring effect, reducing the use amount of catalyst, lowering the conveying power consumption, and the like. The structural catalyst carrier consists of a ceramic matrix and a nanometer titanium oxide coating coated on the surface of the ceramic matrix, wherein the weight ratio of the titanium oxide to the ceramic matrix is (1-40):(99-60). In the invention, even and continuous nanometer titanium oxide coating is prepared on the frame surface of silicon carbide foaming ceramic, and the like in a coating way, wherein the coating is completely formed by nanometer titanium oxide, has large specific surface area, is firmly combined with the matrixes of the silicon carbide foaming ceramic, and the like and is unlikely to fall off. The preparation of the catalyst by using the carrier can effectively reduce the use amount of titanium oxide and noble metal active components, intensify the heat and mass transferring process of chemical reaction, prolong the service life of the catalyst and reduce the catalysis cost.
Description
Technical field:
The present invention relates to structure catalyst carrier field, be specially a kind of ceramic structure catalyst carrier and preparation method thereof with nano-titanium oxide coating layer.
Background technology:
Titanium dioxide (TiO
2) as a kind of semiconductor material with wide forbidden band, characteristics such as, safety non-toxic good with its chemical stability, cost are low obtain extensive studies and application in organic pollution light degradation and automatically cleaning field.Except can directly doing the photochemical catalyst, titanium oxide still is a kind of good catalyst carrier, can act synergistically with being carried on its surperficial catalytic activity constituent element, shows unique catalytic performance.
At present, titanium dioxide mainly forms at catalytic field with powder or the broken again forms such as particle that obtain of pressed powder and uses.The problem of powdery is the separation costs height of catalyst and reaction medium, complicated operation; Contradictions such as beaded catalyst then exists the beds heat-transfer capability poor, and bed pressure drop and diffusion path are difficult to take into account, catalyst abrasion is serious, thereby seriously restricted Application of Catalyst scope and service efficiency.
Summary of the invention:
The object of the present invention is to provide a kind of ceramic structure catalyst carrier and preparation method thereof with nano-titanium oxide coating layer, this carrier is by ceramic matrix and be coated on its surperficial nano-titanium oxide coating layer and constitute jointly, uses this carrier to reach in the chemical industry catalytic reaction process to strengthen the mass-and heat-transfer process, reduces catalyst amount, reduces purposes such as transporting power consumption.
For achieving the above object, the technical solution used in the present invention is:
A kind of ceramic structure catalyst carrier with nano-titanium oxide coating layer, at ceramic matrix surface-coated nano-titanium oxide coating layer, by weight, titanium oxide: ceramic matrix=(1～40): (99～60); Wherein, preferred range is titanium oxide: ceramic matrix=(5～25): (95～75).
The preparation method of said structure catalyst carrier specifically comprises the steps:
1) with the weight ratio butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: (5～50): (1～5): the ratio preparation slip of (5～20), and left standstill 3～8 hours, can obtain titanium oxide sol; Wherein, preferred range is butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: (10～40): (2～4): (8～18).
2) with the weight ratio titanium oxide sol: titanium oxide microparticle=100: the proportional arrangement suspension of (0～30), ball milling obtained slip in 0.5～2 hour; Wherein, preferred range is titanium oxide sol: titanium oxide microparticle=100: (5～25).
3) ceramic matrix after will cleaning and dry soaked in above-mentioned slip 1～5 minute, took out afterwards with compressed air and blew away unnecessary slip, 80～120 ℃ of oven dry down.
4) sample after will drying repeats 3) step, reach desired amount up to the load capacity of coating.
5), can obtain having the catalytic carrier of titanium oxide active coating at the ceramic matrix area load with sample 500 ℃～1000 ℃ roastings of air atmosphere 0.5～2 hour in Muffle furnace.
The preparation method of described structure catalytic carrier, the matrix that adheres to for titania coating is the ceramic material of other useful as catalysts carriers such as foam silicon carbide ceramics, aluminium oxide, cordierite or glass;
Described raw material butyl titanate also can be other titaniferous organic material, as: tetraisopropyl titanate, metatitanic acid four isobutyl esters, 2-methylpropanol titanium etc.;
Described feed ethanol also can be other organic solvents such as propyl alcohol or butanols;
Described raw material hydrochloric acid also can be other inorganic acids such as nitric acid.
Among the present invention, the titan oxide particles particle diameter of titania coating is between 10nm～100nm, and the hole diameter that is formed by the titan oxide particles overlap joint also is distributed between 10nm～100nm.
Among the present invention, the load capacity of coating is generally in (5～30) grams per liter carrier scope.
Among the present invention, the thickness of titania coating is generally in 0.1～50 mu m range.
Compare with powdery or granular titanium oxide, the present invention has following beneficial effect:
1, titanium oxide of the present invention is fixed on ceramic matrix surfaces such as foam silicon carbide ceramics, has avoided the separation problem of catalyst and reaction medium.
2, foam silicon carbide ceramics matrix of the present invention has the advantage of precise forming, not only can be processed as Common Shape, and can be processed into the complex configuration that closely mates with various reactors.
3, the material of foam silicon carbide ceramics matrix of the present invention and architectural characteristic have determined the present invention to have good heat transfer, mass-transfer performance, can significantly reduce the temperature difference of conversion zone, and guarantee the even dispersion of reaction mass.
4, the thickness of titania coating of the present invention is micron order, can guarantee fully contacting of titanium oxide and reaction medium, can make the utilization rate maximization of titanium oxide, reduces the titanium oxide consumption.
5, titania coating specific area of the present invention is big, and active sites is many, and the catalytic activity of Unit Weight is strong.
6, foam silicon carbide ceramics of the present invention has three-dimensional UNICOM structure, and the pressure that can effectively reduce catalytic bed falls, and reduces energy consumption.
7, there is not the catalyst abrasion problem in the present invention.
8, at the even continuous nano-titanium oxide coating layer of skeleton surface preparation such as foam silicon carbide ceramics, this coating is made of nano-titanium oxide fully with coating method in the present invention, and specific area is big, and firm with matrix bond such as foam silicon carbide ceramics, difficult drop-off.
9, the titania coating of the present invention's preparation constitutes novel structure catalyst carrier with matrixes such as foam silicon carbide ceramics, utilize this preparing carriers catalyst can effectively reduce the use amount of titanium oxide and noble metal active constituent element, and can strengthen heat transfer, the mass transfer effect of chemical reaction, prolong catalyst service life, reduce the catalysis cost.
Description of drawings
Fig. 1 is a photomacrograph of the present invention, and titania coating covers the foam silicon carbide ceramics surface uniformly;
Fig. 2 be in the embodiment of the invention 1 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface;
Fig. 3 be in the embodiment of the invention 2 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface;
Fig. 4 be in the embodiment of the invention 3 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface;
Fig. 5 be in the embodiment of the invention 4 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface;
Fig. 6 be in the embodiment of the invention 5 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface;
Fig. 7 be in the embodiment of the invention 6 titania coating at the fracture microphoto of the coverage condition on foam silicon carbide ceramics surface.
In Fig. 2～Fig. 7 photo, shown white and present the fine particle zone and be the section of titania coating, and color is dark and present that bulky grain is regional to be the section of foam silicon carbide ceramics matrix relatively.
The specific embodiment
It is specific as follows that present embodiment has the preparation process of foam silicon carbide ceramics structure catalyst carrier of nano-titanium oxide coating layer:
1, according to Chinese patent (patent No.: ZL00110479.9, denomination of invention: a kind of preparation method of high-strength foam silicon carbide ceramics) described step prepares foam silicon carbide ceramics;
2, with the weight ratio butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: 5: 1: 5 ratio adds above-mentioned raw materials successively, and stirs 0.5 hour, and room temperature left standstill 3 hours afterwards, obtained titanium oxide sol;
3, the foam silicon carbide ceramics after will cleaning and dry soaked 2 minutes in above-mentioned slip, took out afterwards with compressed air and blew away unnecessary slip, 100 ℃ of oven dry down;
4, the sample repeating step 3 after will drying reaches desired amount up to the load capacity of coating.In the present embodiment, in weight ratio, titania coating content is 5%, and all the other are ceramic matrix.
5, with sample 500 ℃ of roastings of air atmosphere 1 hour in Muffle furnace, can obtain having the catalytic carrier of titanium oxide (Detitanium-ore-type) active coating at the foam silicon carbide ceramics area load, the thickness of titania coating is 2 μ m, the titan oxide particles average grain diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 2).
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment 2
It is specific as follows that present embodiment has the preparation process of foam silicon carbide ceramics structure catalyst carrier of nano-titanium oxide coating layer:
1, according to Chinese patent (patent No.: ZL00110479.9, denomination of invention: a kind of preparation method of high-strength foam silicon carbide ceramics) described step prepares foam silicon carbide ceramics;
2, with the weight ratio butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: 10: 1: 10 ratio adds above-mentioned raw materials successively, and stirs 0.5 hour, and room temperature left standstill 5 hours afterwards, obtained titanium oxide sol;
3, with the weight ratio titanium oxide sol: the proportional arrangement suspension of titanium oxide microparticle=100: 5, ball milling obtained slip in 1 hour;
4, the foam silicon carbide ceramics after will cleaning and dry soaked 2 minutes in above-mentioned suspension, took out afterwards with compressed air and blew away unnecessary slip, 100 ℃ of oven dry down;
5, the sample after will drying repeats 4 steps, reaches desired amount up to the load capacity of coating.In the present embodiment, in weight ratio, titania coating content is 8%, and all the other are ceramic matrix.
6, with sample 800 ℃ of roastings of air atmosphere 1 hour in Muffle furnace, can obtain having the catalytic carrier of titanium oxide (anatase and rutile mixed type) active coating at the foam silicon carbide ceramics area load, the thickness of titania coating is 3 μ m, the titan oxide particles particle diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 3).
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment 3
Different with embodiment 2 be in:
With the weight ratio butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: 25: 2: 15 ratio adds above-mentioned raw materials successively, and stirs 0.5 hour, and room temperature leaves standstill and obtained titanium oxide sol in 5 hours afterwards;
With the weight ratio titanium oxide sol: the proportional arrangement suspension of titanium oxide microparticle=100: 10, ball milling obtained slip in 1 hour;
With sample 1000 ℃ of roastings of air atmosphere 1 hour in Muffle furnace, can obtain having the catalytic carrier of titanium oxide (rutile-type) active coating at the foam silicon carbide ceramics area load, the thickness of titania coating is 4 μ m, the titan oxide particles particle diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 4).In the present embodiment, in weight ratio, titania coating content is 10%, and all the other are ceramic matrix.
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment 4
Different with embodiment 2 be in:
With the weight ratio butyl titanate: ethanol: hydrochloric acid (37wt%): water=10: 50: 5: 20 ratio adds above-mentioned raw materials successively, and stirs 0.5 hour, and room temperature leaves standstill and obtained titanium oxide sol in 5 hours afterwards;
With the weight ratio titanium oxide sol: the proportional arrangement suspension of titanium oxide microparticle=100: 15, ball milling obtained slip in 1 hour;
With sample 1000 ℃ of roastings of air atmosphere 1 hour in Muffle furnace, can obtain having the catalytic carrier of titanium oxide (rutile-type) active coating at the foam silicon carbide ceramics area load, the thickness of titania coating is 6 μ m, the titan oxide particles particle diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 5).In the present embodiment, in weight ratio, titania coating content is 15%, and all the other are ceramic matrix.
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment 5
Different with embodiment 4 be in:
With the weight ratio titanium oxide sol: the proportional arrangement suspension of titanium oxide microparticle=100: 20, ball milling obtained slip in 1 hour;
The thickness of titania coating is 8 μ m, and the titan oxide particles particle diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 6).In the present embodiment, in weight ratio, titania coating content is 20%, and all the other are ceramic matrix.
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment 6
Different with embodiment 4 be in:
With the weight ratio titanium oxide sol: the proportional arrangement suspension of titanium oxide microparticle=100: 20, ball milling obtained slip in 1 hour;
The thickness of titania coating is 16 μ m, and the titan oxide particles particle diameter of titania coating is 50nm, and the hole diameter that is formed by the titan oxide particles overlap joint is 30nm (seeing Fig. 1, Fig. 7).In the present embodiment, in weight ratio, titania coating content is 40%, and all the other are ceramic matrix.
Used structure catalytic carrier is the foam silicon carbon pottery of (20 * 20 * 20) mm in the present embodiment, and volume fraction is 30%, average pore size 2mm.
Embodiment result shows, at foam silicon carbide ceramics surface preparation titanium oxide high-ratio surface film, use this carrier can reach enhancing mass-and heat-transfer effect in the chemical industry catalytic reaction process, reduce catalyst amount, reduce purposes such as transporting power consumption, this method has following advantage:
(1) titanium oxide is fixed on the foam silicon carbide ceramics surface, has avoided the separation problem of catalyst and reaction medium;
(2) thickness of titania coating is micron order, can guarantee fully contacting of titanium oxide and reaction medium, can make the utilization rate maximization of titanium oxide, reduces the titanium oxide consumption;
(3) the titania coating specific area is big, and active sites is many, and the catalytic activity of Unit Weight is strong;
(4) foam silicon carbide ceramics has three-dimensional UNICOM structure, the heat and mass transfer enhancement effect, and the pressure that effectively reduces catalytic bed falls, and reduces energy consumption;
(5) there is not the catalyst abrasion problem.
Claims (10)
1. titania coating/ceramic structure catalytic carrier is characterized in that, this structure catalytic carrier is by ceramic matrix and be coated on its surperficial nano-titanium oxide coating layer and constitute jointly, by weight, and titanium oxide: ceramic matrix=(1～40): (99～60).
2. according to the described titania coating of claim 1/ceramic structure catalytic carrier, it is characterized in that by weight, preferred range is titanium oxide: ceramic matrix=(5～25): (95～75).
3. according to the preparation method of the described titania coating of claim 1/ceramic structure catalytic carrier, it is characterized in that, titanium oxide sol is coated on the ceramic matrix surface obtains titania coating, specifically comprise the steps:
1) with the weight ratio butyl titanate: ethanol: hydrochloric acid: water=10: (5～50): (1～5): the ratio preparation slip of (5～20), and left standstill 3～8 hours, can obtain titanium oxide sol;
2) with the weight ratio titanium oxide sol: titanium oxide microparticle=100: the proportional arrangement suspension of (0～30), ball milling obtained slip in 0.5～2 hour;
3) ceramic matrix after will cleaning and dry soaked in above-mentioned slip 1～5 minute, took out afterwards with compressed air and blew away unnecessary slip, 80～120 ℃ of oven dry down;
4) sample after will drying repeats 3) step, reach desired amount up to the load capacity of coating;
5), can obtain having the catalytic carrier of titanium oxide active coating at the ceramic matrix area load with sample 500 ℃～1000 ℃ roastings of air atmosphere 0.5～2 hour in Muffle furnace.
4. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that, in the described step 1), by weight, preferred range is butyl titanate: ethanol: hydrochloric acid: water=10: (10～40): (2～4): (8～18).
5. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that in the described step 1), feed ethanol adopts propyl alcohol or butanols to replace.
6. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that in the described step 1), raw material hydrochloric acid adopts nitric acid to replace.
7. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that described step 2) in, the weight proportion of titanium oxide sol and titanium oxide microparticle is preferably colloidal sol: titanium oxide microparticle=100: (5～25).
8. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that in the described step 3), ceramic matrix is foam silicon carbide ceramics, aluminium oxide, cordierite or glass.
9. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that, the titan oxide particles particle diameter of titania coating is between 10nm～100nm, and the hole diameter that is formed by the titan oxide particles overlap joint also is distributed between 10nm～100nm.
10. according to the preparation method of the described titania coating of claim 3/ceramic structure catalytic carrier, it is characterized in that the crystalline phase of titanium oxide is the mixing phase of Detitanium-ore-type, rutile-type or two kinds of crystal formations.
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| CN102814188A (en) * | 2012-08-25 | 2012-12-12 | 中国科学院金属研究所 | Activated carbon coating/foam silicon carbide structural catalyst and preparation method thereof |
| CN103357443A (en) * | 2012-04-10 | 2013-10-23 | 中国科学院金属研究所 | Titanium oxide coating/foam silicon carbide structure catalytic carrier and preparation method thereof |
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| CN107413321A (en) * | 2017-05-31 | 2017-12-01 | 北京三聚环保新材料股份有限公司 | A kind of preparation method of hud typed carrier |
| CN109928759A (en) * | 2019-03-14 | 2019-06-25 | 武汉工程大学 | A kind of SiC ceramic membrane electrochemical reaction electrode and preparation method thereof |
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| CN103357443A (en) * | 2012-04-10 | 2013-10-23 | 中国科学院金属研究所 | Titanium oxide coating/foam silicon carbide structure catalytic carrier and preparation method thereof |
| CN103357443B (en) * | 2012-04-10 | 2015-06-03 | 中国科学院金属研究所 | Titanium oxide coating/foam silicon carbide structure catalytic carrier and preparation method thereof |
| CN102814188A (en) * | 2012-08-25 | 2012-12-12 | 中国科学院金属研究所 | Activated carbon coating/foam silicon carbide structural catalyst and preparation method thereof |
| CN106669661A (en) * | 2017-01-21 | 2017-05-17 | 杨林 | Preparation method for load type nanometer noble metal catalyst |
| CN107185595A (en) * | 2017-05-31 | 2017-09-22 | 北京三聚环保新材料股份有限公司 | One kind is with TiO2For the preparation method of the hud typed carrier of shell |
| CN107413321A (en) * | 2017-05-31 | 2017-12-01 | 北京三聚环保新材料股份有限公司 | A kind of preparation method of hud typed carrier |
| CN107413321B (en) * | 2017-05-31 | 2020-06-26 | 北京三聚环保新材料股份有限公司 | Preparation method of core-shell type carrier |
| CN109928759A (en) * | 2019-03-14 | 2019-06-25 | 武汉工程大学 | A kind of SiC ceramic membrane electrochemical reaction electrode and preparation method thereof |
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Application publication date: 20110330 |