CN109833865A - A kind of load type sulfur-tolerant combustion catalyst and preparation method - Google Patents
A kind of load type sulfur-tolerant combustion catalyst and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of load type sulfur-tolerant combustion catalyst and preparation method, the catalyst is made of active component and carrier；Catalyst carrier is the CeO for loading sulfate radical2、ZrO2, cerium zirconium molar ratio be 0~10 cerium zirconium sosoloid, TiO2、Al2O3、SnO2One or more of combination, the combination of one or more of noble metals such as catalyst activity component Pd, Pt, Rh.The catalyst significantly improves the sulfur tolerance of catalyst by the sulphation processing in carrier surface.Catalyst produced by the present invention is suitable for the catalyticing combustion process of sulfurous gas, can in sulfur-bearing atmosphere activity with higher, and there is good stability, overcome conventional combustion catalyst under sulfur-bearing atmosphere the shortcomings that easy in inactivation.
Description
Technical field
The invention belongs to CH4, CO, volatile organic matter (VOCs) and soot catalysis burning and exhaust gas from diesel vehicle nitrogen oxidation
Object removes field, and in particular to a kind of load type sulfur-tolerant combustion catalyst and preparation method.
Background technique
In recent years, the concentration of the surface ozone concentration and Organic aerosol of China city and rural area significantly rises,
It produces serious influence to the health of air quality and the mankind.Research is it has been confirmed that organic exhaust gas is these photochemistry both at home and abroad
Oxidant and the most important predecessor of Organic aerosol.Organic exhaust gas endangers the dirt of human health and natural environment as one
Dye source is increasingly valued by people, therefore the removal of organic exhaust gas has become necessity.Catalysis burning processing exhaust gas concentration is wide,
It is without secondary pollution, it is the most effectual way of domestic and international cleaning organic waste gas.And with the raising of environmental protection standard, catalysis burning is having
The application in machine waste gas purification field will further enhance.
Some sulfur-containing organic waste gas can be converted into SO by oxidation2Although its content environment allow in the range of,
Long Term Contact sulfurous gas will generate serious damage to the service life of combustion catalyst.Such as in tail-gas from gasoline automobiles, fuel and
The SO that sulfur-containing compound in lubricating additive is generated through oxidation2It is the poisonous substance of especially severe, it is big in lean-burn condition and temperature
SO at 200 DEG C, in tail gas2Sulfate species can be generated on carrier and active component, be exposed to low concentration SO for a long time2
In be unfavorable for the catalytic activity of exhaust gas treatment catalyst.Therefore, how to reduce the Sulfur tolerance of catalyst is to realize that catalyst is long-term
Stablize the key used.104271243 A of CN discloses a kind of loaded noble metal catalyst of high-temp combustion for hydrocarbon,
By the carried noble metal in refractory metal oxide carriers material and stable metal, reaches catalyst and keep stable at high temperature
Activity.103052446 A of CN discloses the combustion catalyst of porous aluminium oxide loaded noble metal for diesel motor exhaust
In processing, which can make light oil burn at relatively low temperatures.But the above catalyst all can not be for a long time in sulfur-bearing
Steady operation in atmosphere.For this purpose, 102553585 A of patent CN discloses one kind with precious metals pt and transition metal M o as activity
Component, a kind of sulfur resistant catalyst for device in Gas deoxidation of the rare-earth oxide as co-catalyst.Patent CN
It is Zr that 103143347 B, which disclose a kind of noble-metal-supported in general formula,xTi1-xO2Sulfur-tolerant type diesel oxidation on compound
Agent.
Summary of the invention
The present invention is intended to provide a kind of combustion catalyst with high activity and resistant to sulfur stability, suitable for sulfurous gas
Catalyticing combustion process, can in sulfur-bearing atmosphere activity with higher, and have good stability, overcome traditional combustion
Burning catalyst is under sulfur-bearing atmosphere the shortcomings that easy in inactivation.
To achieve the goals above, present invention employs following technical solutions:
A kind of load type sulfur-tolerant combustion catalyst, is made of active component and carrier, and the carrier is load sulfate radical
CeO2(SO4 2-/CeO2)、ZrO2(SO4 2-/ZrO2), cerium zirconium molar ratio be 0~10 cerium zirconium sosoloid (SO4 2-/CexZr1-xO2),
TiO2(SO4 2-/TiO2)、Al2O3(SO4 2-/Al2O3)、SnO2(SO4 2-/SnO2) one or more of combination；Catalyst activity
Group is divided into the combination of one or more of noble metals such as Pd, Pt, Rh, and noble metal weight fraction accounts for the 0.01%- of catalyst
1%, remaining is the carrier for loading sulfate radical.
A kind of preparation method of load type sulfur-tolerant combustion catalyst, specific steps are as follows:
(1) catalyst carrier is impregnated to ie in solution processing in certain density sulfuric acid or sulfate liquor；Or one
Sulfurous gas is passed through at a temperature of fixed makes its presulfurization i.e. gas treatment；
The solution processing methods include the following steps: to weigh a certain amount of CeO2、ZrO2, zirconium molar ratio be 0~10 cerium zirconium
Solid solution, TiO2、Al2O3、SnO2One or more of, it is placed in SO4 2-The sulfuric acid or sulfate that mass concentration is 0.1~20%
In solution, 0~100 DEG C of stirring or 0.1~10h of ultrasonic immersing, preferably 0.5~5h.
The gas processing method includes the following steps: to weigh a certain amount of CeO2、ZrO2, zirconium molar ratio be 0~10 cerium zirconium
Solid solution, TiO2、Al2O3、SnO2One or more of, by metal oxide in 0~600 DEG C of sulfurous gas, processing
0.1~10h, preferably 0.5~5h；Sulfurous gas used is SO2、SO3、H2The group of one or more of S or sulfurous organic compound
It closes；Temperature used is 0~600 DEG C；Gas flow rate is 10~500mL/min, preferably 50~200mL/min；Gas concentration be 0~
500ppm, preferably 10~200ppm.
(2) 2-24 hours dry at 40~200 DEG C by sample made from step (1), then at 300~800 DEG C, roasting
1-6 hours；
It (3) is 2mg/ml~120mg/ml containing Pd, Pt, Rh in concentration by the carrier of sulfuric acid treatment made from step (2)
0.5min-5min is impregnated in the solution of one or more of equal noble metals；Then 2-24 hours dry at 40~200 DEG C；?
It 300~600 DEG C, roasts 1-6 hours；Catalyst is made.
Preferably, the presoma of noble metal used is its acetate, nitrate or HCI solution.
Sulfate used is (NH4)2S2O8Or (NH4)2SO4。
Catalyst of the invention significantly improves the sulfur tolerance of catalyst by the sulphation processing in carrier surface.
Catalyst produced by the present invention is suitable for the catalyticing combustion process of sulfurous gas, being capable of the work with higher in sulfur-bearing atmosphere
Property, and there is good stability, conventional combustion catalyst is overcome under sulfur-bearing atmosphere the shortcomings that easy in inactivation.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
Take CeO2It is 40~60 mesh, the H for being 0.5% by 5mL mass concentration that granular size, which is made,2SO4It is mixed with 10g carrier,
Obtained solid is placed in 120 DEG C of oven drying 10h after standing 6h at room temperature.In air atmosphere by dry solid 600
2h is roasted at DEG C.Pd (the NO for being 13.0% by 1.25mL mass fraction3)2Solution is mixed with the deionized water of 1.25mL, then will
The mixed solution is added drop-wise to 5g treated on carrier, is placed in 120 DEG C of dry 12h in baking oven, it is dry after solid at 550 DEG C
Roast 2h.Obtain CeO2- Pd-H catalyst.
Embodiment 2
Take CeO2It is 40~60 mesh that granular size, which is made, takes 10g to be placed in reaction tube, is passed through 100ppm's into reaction tube
SO2Gas, in 500 DEG C of holding 2h.Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.It is 13.0% by 1.25mL mass fraction
Pd (NO3)2Solution is mixed with the deionized water of 1.25mL, is then added drop-wise to 5g treated on carrier the mixed solution, set
120 DEG C of dry 12h in baking oven, the solid after drying roast 2h at 550 DEG C.Obtain CeO2- Pd-G catalyst.
Embodiment 3
Take ZrO2It is 40~60 mesh, the H for being 0.5% by 5mL mass concentration that granular size, which is made,2SO4It is mixed with 10g carrier,
Obtained solid is placed in 120 DEG C of oven drying 10h after standing 6h at room temperature.In air atmosphere by dry solid 600
2h is roasted at DEG C.Pd (the NO for being 13.0% by 1.25mL mass fraction3)2Solution is mixed with the deionized water of 2.40mL, then will
The mixed solution is added drop-wise to 5g treated on carrier, is placed in 120 DEG C of dry 12h in baking oven, it is dry after solid at 550 DEG C
Roast 2h.Obtain ZrO2- Pd-H catalyst.
Embodiment 4
Take ZrO2It is 40~60 mesh that granular size, which is made, takes 10g to be placed in reaction tube, is passed through 100ppm's into reaction tube
SO2Gas, in 500 DEG C of holding 2h.Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.It is 13.0% by 1.25mL mass fraction
Pd (NO3)2Solution is mixed with the deionized water of 2.40mL, is then added drop-wise to 5g treated on carrier the mixed solution, set
120 DEG C of dry 12h in baking oven, the solid after drying roast 2h at 550 DEG C.Obtain ZrO2- Pd-G catalyst.
Embodiment 5
The method referring to disclosed in patent CN106268856A, prepares cerium zirconium sosoloid as carrier (Ce/Zr=1), particle
Size is 40~60 mesh, the H for being 0.5% by 5mL mass concentration2SO4It is mixed with 10g carrier, at room temperature by gained after standing 6h
Solid is placed in 120 DEG C of oven drying 10h.Dry solid is roasted into 2h at 600 DEG C in air atmosphere.By 1.25mL mass
Pd (the NO that score is 13.0%3)2Solution is mixed with the deionized water of 1.75mL, and the mixed solution is then added drop-wise to 5g processing
On carrier afterwards, 120 DEG C of dry 12h in baking oven are placed in, the solid after drying roasts 2h at 550 DEG C.C1Z1-Pd-H is obtained to urge
Agent.
Embodiment 6
The method referring to disclosed in patent CN106268856A, prepares cerium zirconium sosoloid as carrier (Ce/Zr=1), particle
Size is 40~60 mesh, takes 10g to be placed in reaction tube, the SO of 100ppm is passed through into reaction tube2Gas, in 500 DEG C of holding 2h.
Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.Pd (the NO for being 13.0% by 1.25mL mass fraction3)2Solution and 1.75mL
Deionized water mixing, then the mixed solution is added drop-wise to 5g treated on carrier, is placed in 120 DEG C of dry 12h in baking oven,
Solid after drying roasts 2h at 550 DEG C.Obtain C1Z1-Pd-G catalyst.
Embodiment 7
The method referring to disclosed in patent CN106268856A, prepares cerium zirconium sosoloid as carrier (Ce/Zr=1), particle
Size is 40~60 mesh, the H for being 0.5% by 5mL mass concentration2SO4It is mixed with 10g carrier, at room temperature by gained after standing 6h
Solid is placed in 120 DEG C of oven drying 10h.Dry solid is roasted into 2h at 600 DEG C in air atmosphere.By 1.25mL mass
Pt (the NO that score is 13.0%3)2Solution is mixed with the deionized water of 1.75mL, and the mixed solution is then added drop-wise to 5g processing
On carrier afterwards, 120 DEG C of dry 12h in baking oven are placed in, the solid after drying roasts 2h at 550 DEG C.C1Z1-Pt-H is obtained to urge
Agent.
Embodiment 8
The method referring to disclosed in patent CN106268856A, prepares cerium zirconium sosoloid as carrier (Ce/Zr=1), particle
Size is 40~60 mesh, takes 10g to be placed in reaction tube, the SO of 100ppm is passed through into reaction tube2Gas, in 500 DEG C of holding 2h.
Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.Pt (the NO for being 13.0% by 1.25mL mass fraction3)2Solution and 1.75mL
Deionized water mixing, then the mixed solution is added drop-wise to 5g treated on carrier, is placed in 120 DEG C of dry 12h in baking oven,
Solid after drying roasts 2h at 550 DEG C.Obtain C1Z1-Pt-G catalyst.
Embodiment 9
Take Al2O3It is 40~60 mesh, the H for being 0.5% by 5mL mass concentration that granular size, which is made,2SO4It is mixed with 10g carrier
It closes, obtained solid is placed in 120 DEG C of oven drying 10h after standing 6h at room temperature.Dry solid is existed in air atmosphere
2h is roasted at 600 DEG C.Pt (the NO for being 13.0% by 1.25mL mass fraction3)2Solution is mixed with the deionized water of 3.25mL, so
The mixed solution is added drop-wise to 5g treated on carrier afterwards, is placed in 120 DEG C of dry 12h in baking oven, it is dry after solid 550
2h is roasted at DEG C.Obtain Al2O3- Pt-H catalyst.
Embodiment 10
Take Al2O3It is 40~60 mesh that granular size, which is made, takes 10g to be placed in reaction tube, is passed through 100ppm's into reaction tube
SO2Gas, in 500 DEG C of holding 2h.Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.It is 13.0% by 1.25mL mass fraction
Pt (NO3)2Solution is mixed with the deionized water of 3.25mL, is then added drop-wise to 5g treated on carrier the mixed solution, set
120 DEG C of dry 12h in baking oven, the solid after drying roast 2h at 550 DEG C.Obtain Al2O3- Pt-G catalyst.
Embodiment 11
Take TiO2It is 40~60 mesh, the H for being 0.5% by 5mL mass concentration that granular size, which is made,2SO4It is mixed with 10g carrier,
Obtained solid is placed in 120 DEG C of oven drying 10h after standing 6h at room temperature.In air atmosphere by dry solid 600
2h is roasted at DEG C.Pd (the NO for being 13.0% by 1.25mL mass fraction3)2Solution is mixed with the deionized water of 1.00mL, then will
The mixed solution is added drop-wise to 5g treated on carrier, is placed in 120 DEG C of dry 12h in baking oven, it is dry after solid at 550 DEG C
Roast 2h.Obtain TiO2- Pd-H catalyst.
Embodiment 12
Take TiO2It is 40~60 mesh that granular size, which is made, takes 10g to be placed in reaction tube, is passed through 100ppm's into reaction tube
SO2Gas, in 500 DEG C of holding 2h.Stop SO2600 DEG C of roasting 2h are warming up to after being passed through.It is 13.0% by 1.25mL mass fraction
Pd (NO3)2Solution is mixed with the deionized water of 1.00mL, is then added drop-wise to 5g treated on carrier the mixed solution, set
120 DEG C of dry 12h in baking oven, the solid after drying roast 2h at 550 DEG C.Obtain TiO2- Pd-G catalyst.
Comparative example
Take Al2O3It is 40~60 mesh, the Pt (NO for being 13.0% by 1.25mL mass fraction that granular size, which is made,3)2Solution with
The deionized water of 3.25mL mixes, and then the mixed solution is added drop-wise on 5g carrier, is placed in 120 DEG C of dry 12h in baking oven, does
Solid after dry roasts 2h at 550 DEG C, obtains Al2O3- Pt-F catalyst.
Performance test
The Catalyst packing that embodiment 1~12 and comparative example are obtained carries out CH in fixed bed reactors4Oxidation
Reaction test.Test process are as follows: the internal diameter of quartz ampoule fixed bed reactors is 8mm, and the dosage of catalyst is 150mg.Reaction gas
It is passed through fixed bed reactors after mixing to be reacted, reaction temperature is 250~600 DEG C, and reaction pressure is normal pressure, reaction gas group
As 1%CH4, 4%O2, 10ppmSO2, N2For Balance Air, gas overall flow rate 100mL/min.Gas chromatography after reaction exists
Line analysis, it is as a result shown in table 1.
Table 1
Note: conversion ratio refers to conversion ratio of the catalyst at 550 DEG C after initial conversion and 50h.
Claims (10)
1. a kind of load type sulfur-tolerant combustion catalyst, it is characterised in that the catalyst is made of active component and carrier；It is described
Carrier is the CeO for loading sulfate radical2、ZrO2, cerium zirconium molar ratio be 0~10 cerium zirconium sosoloid, TiO2、Al2O3、SnO2In one
Kind or several combinations；Catalyst activity component is the combination of one or more of noble metals such as Pd, Pt, Rh, your gold
Belong to the 0.01%-1% that weight fraction is catalyst, remaining is the carrier for loading sulfate radical.
2. a kind of preparation method of load type sulfur-tolerant combustion catalyst as described in claim 1, which is characterized in that including as follows
Step:
(1) a certain amount of CeO is weighed2、ZrO2, zirconium molar ratio be 0~10 cerium zirconium sosoloid, TiO2、Al2O3、SnO2In one
Kind is several；It is placed in SO4 2-In the sulfuric acid or sulfate liquor that mass concentration is 0.1~20%, 0~100 DEG C of stirring or ultrasound leaching
0.1~10h of stain；Either by above-mentioned metal oxide in 0~600 DEG C of sulfurous gas, 0.1~10h is handled；
(2) 2-24 hours dry at 40~200 DEG C by sample made from step (1), then at 300~800 DEG C, roasting 1-6 is small
When；
(3) by the carrier of sulfuric acid treatment made from step (2), concentration be 2~120mg/ml containing Pd, Pt, Rh and other are expensive
0.5-5min is impregnated in the precursor solution of metal；Then 2-24 hours dry at 40~200 DEG C；At 300~600 DEG C, roasting
1-6 hours；Catalyst is made.
3. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (3)
The presoma of the noble metal is its acetate, nitrate or hydrochloride.
4. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Sulfate used is (NH4)2S2O8Or (NH4)2SO4。
5. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Sulfurous gas is SO2、SO3、H2The combination of one or more of S or sulfurous organic compound.
6. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Middle stirring or ultrasonic immersing preferably 0.5~5h；Metal oxide handles 0.5~5h in 0~600 DEG C of sulfurous gas.
7. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Sulfurous gas flow velocity used is 10~500mL/min.
8. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Sulfurous gas volumetric concentration used is 0~500ppm, remaining is air.
9. a kind of preparation method of load type sulfur-tolerant combustion catalyst as claimed in claim 2, which is characterized in that step (1)
Sulfurous gas flow velocity preferably 50~200mL/min used；Sulfurous gas volumetric concentration preferably 10~200ppm.
10. a kind of application of load type sulfur-tolerant combustion catalyst as described in claim 1, which is characterized in that the catalyst
The temperature range used is 200~700 DEG C.
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Application publication date: 20190604 |