CN103285867A - Preparation method of CuO nano catalyst taking TixSn(1-x)O2 composite oxide as carrier - Google Patents
Preparation method of CuO nano catalyst taking TixSn(1-x)O2 composite oxide as carrier Download PDFInfo
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- CN103285867A CN103285867A CN2013102591995A CN201310259199A CN103285867A CN 103285867 A CN103285867 A CN 103285867A CN 2013102591995 A CN2013102591995 A CN 2013102591995A CN 201310259199 A CN201310259199 A CN 201310259199A CN 103285867 A CN103285867 A CN 103285867A
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Abstract
The invention discloses a preparation method of a CuO nano catalyst taking a TixSn(1-x)O2 composite oxide as a carrier, which comprises the following steps of: under a violent stirring condition, dropwise adding dilute NH3.H2O very slowly into a mixed solution of TiCl4 and SnCl4 so that the dilute NH3.H2O is completely precipitated; aging overnight; drying at 110 DEG C, and grinding; roasting for 4 hours at different temperatures in a muffle furnace to obtain a TixSn(1-x)O2 composite oxide; by taking the obtained TixSn(1-x)O2 composite oxide as a carrier, soaking the carrier TixSn(1-x)O2 composite oxide in a copper nitrate solution, and stirring for 1 hour; performing oil bath at 110 DEG C, and stirring and evaporating water to dryness; drying at 110 DEG C for 12 hours; and roasting for 4 hours in an air atmosphere at 450 DEG C to obtain a CuO/TixSn(1-x)O2 nano catalyst. The preparation method disclosed by the invention has the advantages that the method is simple and convenient, the equipment is simple, and the obtained catalyst has good thermal stability and higher activity than a single carrier.
Description
Technical field
The present invention relates to a kind of preparation method of nanocatalyst.Specifically be a kind of with Ti
xSn
1-xO
2Composite oxides are the preparation method of the CuO nanocatalyst of carrier.
Background technology
Because factors such as automotive emissions, CO is discharged into the more a kind of gas pollutant of content in the air.In addition, at CO laser gas purifying, CO gas detector, breath for gas purifier, eliminate in the closed system trace amounts of CO etc. and also relate to the CO catalytic oxidation.In petrochemical industry, the catalyst surface carbon distribution causes the catalyst performance variation down to inactivation in most hydro carbons process, and the catalyst oxidation regenerative process also relates to the CO catalytic oxidation.For these reasons, the CO oxidation reaction becomes one of heat subject of catalytic field research.
The catalyst that is used for the CO low-temperature catalytic oxidation of research at present mainly contains noble metal catalyst and non-precious metal catalyst.Broad research be noble metal (Pt, Pd, Rh, Ru, Au etc.) catalyst because noble metal catalyst has advantages such as catalytic activity height, good stability, life-span be long.But also there is following shortcoming in noble metal catalyst, as bullion content in the catalyst all than higher, preparation process is loaded down with trivial details, post processing is complicated, the catalyst of inactivation is non-renewable and poor storage stability etc., so rest on the laboratory research stage basically.By contrast, the non-precious metal catalyst price is general relatively more cheap, Mckinney etc. finds that first transition group metallic oxide has facilitation to the CO oxidation reaction since the thirties in 20th century, particularly catalyst based because the active and stability that shows in this reaction of Cu and people's attention extremely.
Because CuO/TiO
2Catalyst shows good properties and is widely used in CO in heterogeneous catalysis eliminates reaction.Therefore, in the past few decades, people have carried out a large amount of research to this catalyst, confirm to be dispersed in TiO
2CuO on the carrier is the active specy of CO oxidation, and catalytic activity is influenced by concentration, existence and the reproducibility etc. of copper species simultaneously.Yet because sharp titanium thermal instability and be transformed into shortcoming such as rutile easily, the general employing changes its structure and other the metal of mixing improves the stability of sharp titanium.
Ti
xSn
1-xO
2Composite oxides are a kind of emerging materials, and it all has been subjected to paying close attention to widely in application facet such as low pressure rheostat, air-sensitive original paper and photocatalysis.In recent years, by our Ti that discovers
xSn
1-xO
2Composite oxides have than simple TiO in CO and NO elimination reaction as carrier
2And SnO
2Do carrier and have more significant advantage.And high temperature easy-sintering not.We have successfully synthesized a series of with Ti by a kind of easy method
xSn
1-xO
2Composite oxides are the CuO nanocatalyst of carrier.Because this method synthesis material is easy to get, simple to operate, no especial equipment requirements makes it at catalytic field good prospects for application be arranged.
Summary of the invention
The object of the present invention is to provide a kind of good a kind of with Ti of high activity, high-temperature stability that prepare
xSn
1-xO
2Composite oxides are the CuO nanocatalyst metal oxide nano Preparation of catalysts method of carrier, thereby are expected to find broad application in actual applications.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A kind of with Ti
xSn
1-xO
2Composite oxides are the preparation method of the CuO nanocatalyst of carrier, and operating procedure is as follows:
Step 1. is with TiCl
4And SnCl
45H
2O mixes according to a certain percentage, makes Ti ︰ Sn mol ratio be respectively 3 ︰ 1,1 ︰ 1 or 1 ︰ 3, mixes solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.600 ℃ of roasting 4h in Muffle furnace obtain Ti then
xSn
1-xO
2Composite oxides, identified as samples is designated as Ti
0.75Sn
0.25O
2, Ti
0.5Sn
0.5O
2Or Ti
0.25Sn
0.75O
2The Ti that does not have roasting with above preparation
0.75Sn
0.25O
2Sample obtains the Ti of roasting under the different temperatures respectively 450 ℃, 600 ℃, 850 ℃ or 1200 ℃ of roastings
0.75Sn
0.25O
2Sample is labeled as 450 ℃ of Ti respectively
0.75Sn
0.25O
2, 600 ℃ of Ti
0.75Sn
0.25O
2, 850 ℃ of Ti
0.75Sn
0.25O
2Or 1200 ℃ of Ti
0.75Sn
0.25O
2
Step 3. is with 5%CuO/Ti
0.75Sn
0.25O
2, 5%CuO/Ti
0.5Sn
0.5O
2, 5%CuO/Ti
0.25Sn
0.75O
2, 5%CuO/450 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/600 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/850 ℃ Ti
0.75Sn
0.25O
2Or 5%CuO/1200 ℃ of Ti
0.75Sn
0.25O
2Cross the 60-80 mesh sieve behind the nanocatalyst compressing tablet.
Step 4. is put into microreactor respectively with the nanocatalyst compressing tablet that step 3 obtains, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph; The result shows, 600 ℃ of roastings, and titanium tin mol ratio is the 5%CuO/600 ℃ of Ti of 1 ︰ 1
0.75Sn
0.25O
2Catalyst activity is best, and under 200 ℃, the conversion ratio of CO is 100%.
Preparation method's of the present invention advantage is:
1. method is simple, and production equipment is simple and easy, and technological operation is easy.
2. the catalyst Heat stability is good that obtains, and have higher activity.
Description of drawings
Fig. 1 is the 5%CuO/Ti of the present invention's preparation
xSn
1-xO
2The XRD collection of illustrative plates of catalyst.
Fig. 2 is the 5%CuO/Ti of the present invention's preparation
xSn
1-xO
2The CO oxidation activity of catalyst.
Fig. 3 is the 5%CuO/Ti of roasting under the different temperatures of the present invention's preparation
0.75Sn
0.25O
2The XRD collection of illustrative plates of catalyst.
Fig. 4 is the 5%CuO/Ti of roasting under the different temperatures of the present invention's preparation
0.75Sn
0.25O
2The CO oxidation activity of catalyst.
Specific implementation method
Principle of the present invention is as follows: because the K of titanium tin hydroxide
SpDifference, even in order to guarantee two kinds of ion mixed precipitations, with rare NH
3H
2O joins in the mixed solution of two kinds of ions very lentamente, makes its precipitation fully, and aging, roasting obtains Ti then
xSn
1-xO
2Composite oxides, and as carrier, adopt the method for dipping, make active component CuO be dispersed in carrier surface, the preparation nanocatalyst.
Be further described below in conjunction with the present invention of embodiment.
Embodiment 1
With Ti
0.75Sn
0.25O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 3 ︰ 1 mix solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.600 ℃ of roasting 4h in Muffle furnace obtain Ti then
0.75Sn
0.25O
2Sample.
Step 3. is crossed 60～80 mesh sieves with the catalyst compressing tablet of step 2.
Step 4. is put into microreactor with the catalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70～220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃ of reaction temperatures, the Catalyst for CO conversion ratio was 100%.
With Ti
0.5Sn
0.5O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 1 ︰ 1 mixes solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.600 ℃ of roasting 4h in Muffle furnace obtain Ti then
0.5Sn
0.5O
2Sample.
Step 3. is crossed 60～80 mesh sieves with the catalyst compressing tablet of step 2,
Step 4. is put into microreactor with the catalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃ of reaction temperatures, the Catalyst for CO conversion ratio was 89%.Comparative Examples 1 poor activity.
Embodiment 3
With Ti
0.25Sn
0.75O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 1 ︰ 3 mixes solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.600 ℃ of roasting 4h in Muffle furnace obtain Ti then
0.25Sn
0.75O
2Sample.
Step 3. is crossed the 60-80 mesh sieve after with the nanocatalyst compressing tablet of step 2.
Step 4. is put into microreactor with the nanocatalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃, the Catalyst for CO conversion ratio was 82%.Comparative Examples 1 and 2 poor activity.
Embodiment 4
With 450 ℃ of Ti
0.75Sn
0.25O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 3 ︰ 1 mix solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.450 ℃ of roasting 4h in Muffle furnace obtain 450 ℃ of Ti then
0.75Sn
0.25O
2Sample.
Step 3. is crossed the 60-80 mesh sieve after with the nanocatalyst compressing tablet of step 2.
Step 4. is put into microreactor with the nanocatalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃ of reaction temperatures, the Catalyst for CO conversion ratio was 60.3%.
Embodiment 5
With 850 ℃ of Ti
0.75Sn
0.25O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 3 ︰ 1 mix solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.850 ℃ of roasting 4h in Muffle furnace obtain 850 ℃ of Ti then
0.75Sn
0.25O
2Sample.
Step 3. is crossed the 60-80 mesh sieve after with the nanocatalyst compressing tablet of step 2.
Step 4. is put into microreactor with the nanocatalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃ of reaction temperatures, the Catalyst for CO conversion ratio was 81.5%.Comparative Examples 1 poor activity, Comparative Examples 4 is active good.
Embodiment 6
With 1200 ℃ of Ti
0.75Sn
0.25O
2Composite oxides are the preparation of the CuO nanocatalyst of carrier:
Step 1. is with TiCl
4And SnCl
45H
2O mixes, and making Ti ︰ Sn mol ratio is that 3 ︰ 1 mix solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight.Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind.1200 ℃ of roasting 4h in Muffle furnace obtain 1200 ℃ of Ti then
0.75Sn
0.25O
2Sample.
Step 3. is crossed the 60-80 mesh sieve after with the nanocatalyst compressing tablet of step 2.
Step 4. is put into microreactor with the nanocatalyst compressing tablet of step 3, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph.When the result showed 200 ℃ of reaction temperatures, the Catalyst for CO conversion ratio was 38%.Comparative Examples 4 and 5 poor activity.
The crystalline phase of these catalyst changes as Fig. 1, and shown in 3, active testing the results are shown in Figure 2,4.From Fig. 1,3 as can be seen, the CuO/Ti of gained
xSn
1-xO
2The crystal formation of catalyst is rutile-type.
Active testing, the optimization of titanium tin ratio, obtaining titanium tin ratio is the 5%CuO/Ti of 3 ︰ 1
0.75Sn
0.25O
2The Catalyst for CO oxidation activity is best.The optimization of titanium tin carrier sintering temperature obtains Ti
0.75Sn
0.25O
2When the sample sintering temperature is 600 ℃, 5%CuO/600 ℃ of Ti
0.75Sn
0.25O
2The Catalyst for CO oxidation activity is best.
Claims (1)
1. one kind with Ti
xSn
1-xO
2Composite oxides are the preparation method of the CuO nanocatalyst of carrier, it is characterized in that operating procedure is as follows:
Step 1. is with TiCl
4And SnCl
45H
2O mixes according to a certain percentage, makes Ti ︰ Sn mol ratio be respectively 3 ︰ 1,1 ︰ 1 or 1 ︰ 3, mixes solution 1h, slowly at the uniform velocity drips weak aqua ammonia then while stirring to mixed solution, until pH=10, makes its precipitation fully, age overnight; Gained precipitation 0.25molL
-1Ammonia scrubbing and suction filtration are dried 12h again in 110 ℃ of baking ovens, grind; 600 ℃ of roasting 4h in Muffle furnace obtain Ti then
xSn
1-xO
2Composite oxides, identified as samples is designated as Ti
0.75Sn
0.25O
2, Ti
0.5Sn
0.5O
2Or Ti
0.25Sn
0.75O
2The Ti that does not have roasting with above preparation
0.75Sn
0.25O
2Sample obtains the Ti of roasting under the different temperatures respectively 450 ℃, 600 ℃, 850 ℃ or 1200 ℃ of roastings
0.75Sn
0.25O
2Sample is labeled as 450 ℃ of Ti respectively
0.75Sn
0.25O
2, 600 ℃ of Ti
0.75Sn
0.25O
2, 850 ℃ of Ti
0.75Sn
0.25O
2Or 1200 ℃ of Ti
0.75Sn
0.25O
2
Step 2. is got the Ti that 1g step 1 obtains respectively
0.75Sn
0.25O
2, Ti
0.5Sn
0.5O
2, Ti
0.25Sn
0.75O
2, 450 ℃ of Ti
0.75Sn
0.25O
2, 600 ℃ of Ti
0.75Sn
0.25O
2, 850 ℃ of Ti
0.75Sn
0.25O
2Or 1200 ℃ of Ti
0.75Sn
0.25O
2Composite oxides are carrier, use 0.1molL respectively
-1Cu (NO
3)
2Solution 6.25ml dipping stirs 1h, and evaporating water is stirred in 110 ℃ of oil baths, and dry 12h under 110 ℃ grinds again, and the following 450 ℃ of roasting 4h of air atmosphere obtain 5%CuO/Ti
0.75Sn
0.25O
2, 5%CuO/Ti
0.5Sn
0.5O
2, 5%CuO/Ti
0.25Sn
0.75O
2, 5%CuO/450 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/600 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/850 ℃ Ti
0.75Sn
0.25O
2Or 5%CuO/1200 ℃ of Ti
0.75Sn
0.25O
2Nanocatalyst;
Step 3. is with 5%CuO/Ti
0.75Sn
0.25O
2, 5%CuO/Ti
0.5Sn
0.5O
2, 5%CuO/Ti
0.25Sn
0.75O
2, 5%CuO/450 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/600 ℃ Ti
0.75Sn
0.25O
2, 5%CuO/850 ℃ Ti
0.75Sn
0.25O
2Or 5%CuO/1200 ℃ of Ti
0.75Sn
0.25O
2Cross the 60-80 mesh sieve behind the nanocatalyst compressing tablet;
Step 4. is put into microreactor respectively with the nanocatalyst compressing tablet that step 3 obtains, at 2%CO/N
2Flow velocity be 20mLmin
-1, O
2Flow velocity be 5mLmin
-1, air speed is 60.000mLg
-1H
-1, reaction temperature is to carry out catalytic reaction under 70-220 ℃ the condition, the activity data of catalyst compressing tablet is gathered after reaction reaches balance; After separating, the packed column of product after the catalytic reaction through the 5A molecular sieve is housed analyze at gas chromatograph; The result shows, 600 ℃ of roastings, and titanium tin mol ratio is the 5%CuO/600 ℃ of Ti of 1 ︰ 1
0.75Sn
0.25O
2Catalyst activity is best, and under 200 ℃, the conversion ratio of CO is 100%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769113A (en) * | 2013-12-09 | 2014-05-07 | 广西大学 | Supported binary metal oxide nano-catalyst and preparation method thereof |
| CN108987712A (en) * | 2018-07-20 | 2018-12-11 | 福建师范大学 | A kind of preparation method of novel anode material of lithium-ion battery |
| CN111437814A (en) * | 2020-05-08 | 2020-07-24 | 清华大学盐城环境工程技术研发中心 | Tin-doped platinum-titanium catalyst and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799692A (en) * | 2006-01-19 | 2006-07-12 | 北京科技大学 | Method for preparing visible light-inducing stannum-doped highly catalytic nano photocatalyst of titanium dioxide |
| CN102500355A (en) * | 2011-11-07 | 2012-06-20 | 南京大学 | Preparation method for supported metal oxide nanocatalyst using TixSn1-xO2 solid solution as carrier |
-
2013
- 2013-06-26 CN CN2013102591995A patent/CN103285867A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799692A (en) * | 2006-01-19 | 2006-07-12 | 北京科技大学 | Method for preparing visible light-inducing stannum-doped highly catalytic nano photocatalyst of titanium dioxide |
| CN102500355A (en) * | 2011-11-07 | 2012-06-20 | 南京大学 | Preparation method for supported metal oxide nanocatalyst using TixSn1-xO2 solid solution as carrier |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769113A (en) * | 2013-12-09 | 2014-05-07 | 广西大学 | Supported binary metal oxide nano-catalyst and preparation method thereof |
| CN108987712A (en) * | 2018-07-20 | 2018-12-11 | 福建师范大学 | A kind of preparation method of novel anode material of lithium-ion battery |
| CN108987712B (en) * | 2018-07-20 | 2021-10-01 | 福建师范大学 | Preparation method of sodium ion battery negative electrode material |
| CN111437814A (en) * | 2020-05-08 | 2020-07-24 | 清华大学盐城环境工程技术研发中心 | Tin-doped platinum-titanium catalyst and preparation method and application thereof |
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Application publication date: 20130911 |