CN101947449A - Method for preparing nano Ti-based montmorillonite Cu catalyst and application of catalyst to HC-SCR - Google Patents
Method for preparing nano Ti-based montmorillonite Cu catalyst and application of catalyst to HC-SCR Download PDFInfo
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- CN101947449A CN101947449A CN 201010279857 CN201010279857A CN101947449A CN 101947449 A CN101947449 A CN 101947449A CN 201010279857 CN201010279857 CN 201010279857 CN 201010279857 A CN201010279857 A CN 201010279857A CN 101947449 A CN101947449 A CN 101947449A
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- montmorillonite
- base montmorillonite
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- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 32
- 239000010949 copper Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 12
- 238000005342 ion exchange Methods 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 2
- 239000012691 Cu precursor Substances 0.000 abstract 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 239000012495 reaction gas Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 206010014561 Emphysema Diseases 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- Catalysts (AREA)
Abstract
本发明公开了一种纳米Ti基蒙脱土Cu催化剂的制备方法及其在HC-SCR中的应用，属于无机纳米催化材料领域。其制备方法是先制备柱化剂溶液和蒙脱土悬浮液，然后将柱化剂溶液加入到蒙脱土悬浮液中，最后将蒙脱土悬浮液滴加到铜前驱体溶液中。本发明涉及的催化剂的制备方法操作简单、成本低、热稳定性高、重复性高。制得的Ti基蒙脱土Cu催化剂具有较宽的介孔结构(孔径为2.2-6.8nm)，较高的比表面积(178-312m2/g)和较强的抗硫和抗水性能，可应用于HC-SCR反应中；在以烃类物质为还原剂、氧含量＝8-15vol.％的情况下，N2的收率可达50-70％以上。The invention discloses a preparation method of a nano Ti-based montmorillonite Cu catalyst and its application in HC-SCR, belonging to the field of inorganic nano catalytic materials. The preparation method is to firstly prepare columnar agent solution and montmorillonite suspension, then add columnar agent solution to montmorillonite suspension, and finally add montmorillonite suspension dropwise to copper precursor solution. The preparation method of the catalyst involved in the invention is simple in operation, low in cost, high in thermal stability and high in repeatability. The prepared Ti-based montmorillonite Cu catalyst has a wider mesoporous structure (pore diameter of 2.2-6.8nm), higher specific surface area (178-312m 2 /g) and stronger sulfur and water resistance. It can be applied to HC-SCR reaction; when hydrocarbons are used as reducing agents and the oxygen content is 8-15vol.%, the yield of N2 can reach more than 50-70%.
Description
Technical field
The invention belongs to inorganic nano catalysis material field, relate to a kind of nanometer Ti base montmorillonite Cu Preparation of catalysts method and this nanometer Ti base montmorillonite Cu catalyst and be applied to the reaction of middle low temperature (150-350 ℃) selection Reduction of NO.
Background technology
NO
xBe mainly derived from power plant emission gas and vehicle exhaust, can make diseases such as human generation pulmonary emphysema, hypopsia, bronchitis, and crops and ecological environment are had great harm.Therefore, restriction NO has been formulated in countries in the world
xThe every rules and the policy of discharging are so effectively remove NO
XHave very important significance for aspects such as environment and people's lives.At various removal NO
xIn the method, (SelectiveCatalytic Reduction SCR) has low-cost and high efficiency feature, is present unique industrialized denitration technology to select catalytic reduction method.This technology is mainly with V
2O
5-WO
3/ TiO
2For catalyst is removed NO
x, but this catalyst has toxicity, has limited it in industrial extensive use.
Transition-metal catalysts such as Cu are cheap, output is big, nontoxic, but at present in denitrification process reaction temperature higher, more than 300 ℃.Y. Wan etc. utilizes ion-exchange to make the Cu-Al-MCM-41 catalyst, and this catalyst NO in the time of 350 ℃ obtains the highest conversion ratio, N
2Yield (Y.Wan, J.X.Ma, Z.Wang, W.Zhou, S.Kaliaguine, J.Catal.227 (2004) 242-252) about 40%.Employing sol-gal processes such as X.Jiang make CuO-TiO
2Catalyst is obtained the highest NO conversion ratio (Y.Jiang, G Ding, L.Lou, Y.Chen, X.Zheng, Catal.Today 93-95 (2004) 811-818) in the time of 300 ℃.
Summary of the invention
The invention provides a kind of nanometer Ti base montmorillonite Cu Preparation of catalysts method and the application in HC-SCR thereof.Adopt ion-exchange process to prepare the Cu-Ti-PILC catalyst with meso-hole structure, the aperture is 2.2-6.8nm, and specific area is 178-312m
2/ g.Wherein the quality percentage composition of Cu is 1-5wt%, tests simple, the simple operation, with low cost of used instrument.This Cu-Ti-PILC catalyst is applied to the selection Reduction of NO, under middle low temperature (150-350 ℃), N
2Yield more than 50-70%.
A kind of nanometer Ti base montmorillonite Cu Preparation of catalysts method of the present invention may further comprise the steps:
(1) preparation of pillaring agent
Get the precursor TiCl of a certain amount of Ti
4Join in the HCl solution of 0.5-2M, the mol ratio that makes Ti and HCl is 5-10, adds deionized water again under continue stirring, and 20-40 ℃ is stirred the pillaring agent that obtains stable transparent behind the 12-30h.
(2) preparation of montmorillonite suspension liquid
A certain amount of imvite is joined in the deionized water of 500ml, stir 12-30h, imvite is fully expanded at 20-60 ℃.
(3) preparation of Ti base montmorillonite
Under 20-60 ℃, step (1) solution is joined in step (2) suspension, this moment, the mass ratio of Ti and imvite was 5-30.After stirring 12-30h, filters centrifugally, wash with the removal chlorion with deionized water, dry 6-24h under 80-120 ℃ of temperature then is at last as in the Muffle furnace, at 300-700 ℃ of temperature lower calcination 3-8h.
(4) Preparation of catalysts
Copper presoma (as Schweinfurt green, copper nitrate, copper sulphate) is dissolved in the deionized water, makes active component solution.Add the Ti base montmorillonite carrier that step (3) makes then, once reach ion-exchange for several times, make that the quality percentage composition of copper is 1-5wt%.Solution after the ion-exchange filters centrifugal, spends deionised water for several times, and dry 6-24h under 80-120 ℃ of temperature again at 200-600 ℃ of temperature lower calcination 3-8h, just can obtain Ti base montmorillonite Cu catalyst.
The application of nanometer Ti base montmorillonite Cu catalyst in HC-SCR that above-mentioned preparation method obtains, the technical scheme of employing is: the volume ratio of hydro carbons (as the hydro carbons of methane, propylene, other kinds) reducing agent and NO is 1: 1, O
2Content be 8-15vol.%, air speed is 25000-45000h
-1, the active testing temperature is 150-350 ℃.The catalyst that the present invention makes is obtained the highest activity in the time of 250 ℃, at this moment N
2Yield can reach more than the 50-70%, have bigger prospects for commercial application.
Compared with prior art, the present invention has following advantage:
(1) the present invention is that raw material makes Ti base montmorillonite carrier with the imvite, and is simple to operate, with low cost, heat endurance is high, repeatability is high, can improve the anti-sulphur and the water repelling property of catalyst.
(2) prepared Ti base montmorillonite Cu catalyst have broad meso-hole structure (aperture is 2.2-6.8nm) and higher specific surface area (178-312m
2/ g).
(3) Zhi Bei Ti base montmorillonite Cu catalyst has higher catalyzing N O activity in the time of 150-350 ℃.
The specific embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme.
Embodiment 1
(1) preparation of pillaring agent
The HCl of 1M is solution-stabilized at 40 ℃, with the TiCl of 4.5ml
4Slowly be added drop-wise in the HCl solution, add deionized water again behind the stirring 1h, the cumulative volume that makes final solution is 100ml, obtains the pillaring agent of stable transparent behind the lasting stirring 24h.
(2) preparation of montmorillonite suspension liquid
The 4g imvite is joined in the deionized water of 500ml, stir 24h, imvite is fully expanded at 40 ℃.
(3) preparation of Ti base montmorillonite
Under 40 ℃, (1) solution slowly is added drop-wise in (2) suspension, this moment, the mass ratio of Ti and imvite was 10.After stirring 12-30h, filter centrifugally, wash, then at 80-120 ℃ temperature 6-24h, at last as in the Muffle furnace, at 450 ℃ temperature lower calcination 3-8h with deionized water.
(4) Preparation of catalysts
Schweinfurt green is dissolved in the deionized water, under continuing stirring, adds the Ti base montmorillonite carrier that makes in the step (3), filtration, centrifugal, washing.Repeat this process once, the quality percentage composition that can make copper is 4.2wt%.Solution after the ion-exchange filters centrifugal, spends deionised water for several times, and dry 6-24h under 80-120 ℃ of temperature at 400 ℃ of temperature lower calcination 3-8h, can obtain the catalyst finished product again.
Embodiment 2
As in the U type reactor, preliminary treatment 2h under 400 ℃ inert atmosphere is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 1
3H
6, 8vol.%, all the other are He, air speed is 25000h
-1), N in the time of 250 ℃
2Obtaining the highest yield is 72%.
Embodiment 3
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 1
3H
6, 10vol.%, all the other are He, air speed is 35000h
-1), N in the time of 250 ℃
2The highest yield be 61%.
Embodiment 4
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 1
3H
6, 15vol.%, all the other are He, air speed is 45000h
-1), N in the time of 250 ℃
2The highest yield be 48%
Embodiment 5
(1) preparation of pillaring agent
The HCl of 1M is solution-stabilized at 40 ℃, with the TiCl of 4.5ml
4Slowly be added drop-wise in the HCl solution, add deionized water again behind the stirring 1h, making final solution is 100ml, obtains the pillaring agent of stable transparent behind the lasting stirring 24h.
(2) preparation of montmorillonite suspension liquid
The 12g imvite is joined in the deionized water of 500ml, stir 24h, imvite is fully expanded at 60 ℃.
(3) preparation of Ti base montmorillonite
Under 60 ℃, step (1) solution is slowly dripped in step (2) suspension, this moment, the mass ratio of Ti and imvite was 30.After stirring 12-30h, filter centrifugally, wash, then at 80-120 ℃ temperature drying 6-24h, at last as in the Muffle furnace, at 700 ℃ temperature lower calcination 3-8h with deionized water.
(4) Preparation of catalysts
Schweinfurt green is dissolved in deionized water, is continuing to add the Ti base montmorillonite carrier that step (3) makes under the stirring, filtration, centrifugal, washing.Repeat this process once, the quality percentage composition that can make copper is 2.6wt%.Solution after the ion-exchange filters centrifugal, spends deionised water for several times, and dry 6h under 120 ℃ of temperature at 600 ℃ of temperature lower calcination 8h, can obtain the catalyst finished product again.
Embodiment 6
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 10vol.%, all the other are He, air speed is 25000h
-1), N in the time of 250 ℃
2The highest yield be 69%.
Embodiment 7
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppm C then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 10vol.%, all the other are He, air speed is 35000h
-1), N in the time of 250 ℃
2Obtaining the highest yield is 52%.
Embodiment 8
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 10vol.%, all the other are He, air speed is 45000h
-1), N in the time of 250 ℃
2Obtaining the highest yield is 42%.
Embodiment 9
(1) preparation of pillaring agent
The HCl of 1M is solution-stabilized at 40 ℃, with the TiCl of 4.5ml
4Slowly be added drop-wise in the HCl solution, add deionized water again behind the stirring 1h, making final solution is 100ml, obtains the pillaring agent of stable transparent behind the lasting stirring 24h.
(2) preparation of montmorillonite suspension liquid
The 2g imvite is joined in the deionized water of 500ml, stir 24h, imvite is fully expanded at 60 ℃.
(3) preparation of Ti base montmorillonite
Under 20 ℃, step (1) solution is slowly dripped in step (2) suspension, this moment, the mass ratio of Ti and imvite was 5.After stirring 12-30h, filters centrifugally, wash with the Cl ion in the removal solution, then at 80-120 ℃ temperature drying 6-24h, at last as in the Muffle furnace, at 300 ℃ temperature lower calcination 3-8h with deionized water.
(4) Preparation of catalysts
Schweinfurt green is dissolved in deionized water, is continuing to add the Ti base montmorillonite carrier that step (3) makes under the stirring, filtration, centrifugal, washing.Repeat this process once, the quality percentage composition that can make copper is 2.9wt%.Solution after the ion-exchange filters centrifugal, spends deionised water for several times, and dry 6h under 120 ℃ of temperature at 200 ℃ of temperature lower calcination 8h, can obtain the catalyst finished product again.
Embodiment 10
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 15vol.%, all the other are He, air speed is 25000h
-1), N in the time of 250 ℃
2The highest yield be 62%.
Embodiment 11
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppm C then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 15vol.%, all the other are He, air speed is 35000h
-1), N in the time of 250 ℃
2Obtaining the highest yield is 43%.
Embodiment 12
As in the U type reactor, preliminary treatment 2h under 400 ℃ of following inert atmospheres is reaction gas (1000ppmNO, 1000ppmC then with the preliminary treatment cyclostrophic with the catalyst 0.2g that makes among the embodiment 5
3H
6, 15vol.%, all the other are He, air speed is 45000h
-1), N in the time of 250 ℃
2Obtaining the highest yield is 31%.
Claims (5)
1. nanometer Ti base montmorillonite Cu Preparation of catalysts method is characterized in that may further comprise the steps:
(1) preparation pillaring agent: under continue stirring, the precursor of Ti is joined in the HCl solution, add again in the deionized water to cumulative volume be 100ml, stir and ageing obtains the pillaring agent of stable transparent;
(2) preparation montmorillonite suspension liquid: imvite is joined in the deionized water of 500ml,, imvite is fully expanded 20-60 ℃ of stirring;
(3) preparation of Ti base montmorillonite: step (1) solution is joined in step (2) suspension, after stirring ageing, filter, spend deionised water for several times, then under 80-120 ℃ of temperature dry 6-24h, behind 300-700 ℃ of temperature lower calcination 3-8h, obtain Ti base montmorillonite carrier;
(4) Preparation of catalysts: the copper presoma is dissolved in the deionized water, adds the Ti base montmorillonite that step (3) makes and carry out ion-exchange, centrifugal after filtration, washing for several times, dry, calcining obtains Ti base montmorillonite Cu catalyst; The baking temperature of the Cu catalyst of Ti base montmorillonite is 80-120 ℃, and be 6-24h drying time, and calcining heat is 200-600 ℃, and calcination time is 3-8h.
2. preparation method according to claim 1 is characterized in that, the mol ratio of Ti and HCl is 5-10 in the step (1).
3. preparation method according to claim 1 is characterized in that, the mass ratio of Ti and imvite is 5-30 in the step (3).
4. preparation method according to claim 1 is characterized in that, the load capacity of copper is 1-5wt% in the step (4).
5. the application of a nanometer Ti base montmorillonite Cu catalyst in HC-SCR, it is characterized in that: the volume ratio of hydro carbons reducing agent and NO is 1: 1, O
2Content be 8-15vol.%, air speed is 25000-45000h
-1, the active testing temperature is 150-350 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404864A (en) * | 2018-04-16 | 2018-08-17 | 贵州大学 | Activated carbon supported titanium pillared montmorillonite composite material |
| CN108554410A (en) * | 2018-05-03 | 2018-09-21 | 东华大学 | A kind of Fe/Ti-PILC catalyst, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404864A (en) * | 2018-04-16 | 2018-08-17 | 贵州大学 | Activated carbon supported titanium pillared montmorillonite composite material |
| CN108554410A (en) * | 2018-05-03 | 2018-09-21 | 东华大学 | A kind of Fe/Ti-PILC catalyst, preparation method and application |
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