CN105032417B - A kind of SCR denitration and the preparation method and application thereof of high sulfur resistive - Google Patents
A kind of SCR denitration and the preparation method and application thereof of high sulfur resistive Download PDFInfo
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- CN105032417B CN105032417B CN201510305306.2A CN201510305306A CN105032417B CN 105032417 B CN105032417 B CN 105032417B CN 201510305306 A CN201510305306 A CN 201510305306A CN 105032417 B CN105032417 B CN 105032417B
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Abstract
The invention belongs to the technical fields of catalyst, disclose a kind of SCR denitration and the preparation method and application thereof of high sulfur resistive.The catalyst is using cordierite honeycomb ceramic as matrix, and described matrix load has catalyst coat, the catalyst coat to be prepared by composite alumina support and precious metal salt；The composite alumina support is prepared by transition metal salt and aluminium oxide, wherein the dosage relation of each substance is：Aluminium oxide：Transition metal salt：The mass ratio of precious metal salt is (75~100)：(5~50)：(5~10)；The catalyst coat is the 5~10% of the SCR denitration gross mass of high sulfur resistive.The catalyst of the present invention has very good low-temperature catalytic activity and stability, high antisulphuric ability, while non-noble metal introducing greatly reduces the use of noble metal, to reduce the cost of catalyst；It is mainly used in denitrating flue gas field.
Description
Technical field
The invention belongs to the technical fields of catalyst, are related to a kind of denitrating catalyst, more particularly to a kind of SCR of high sulfur resistive
Denitrating catalyst and the preparation method and application thereof.
Background technology
With Chinese Urbanization development and urban population sharply increase and industry rapid development, China city
Atmosphere pollution is extremely serious, and the city that atmospheric environment meets national standard reference is less than the 1% of total amount, wherein 62% city
Nitrogen oxides (NO in airx), sulfur dioxide whole year daily mean of concentration be more than 3 grades of standard (100mg/m3).It is defended according to the world
The monitoring in 10~15 years of raw 60 countries of tissue pair finds that in 10 cities of global pollution most serious, China just accounts for 8
It is a, moreover, NO in China's urban atmospherex、SO2Concentration with total suspended particles is also highest in the world.Currently, utilizing selection
Property catalysis reduction (SCR) technology by the method for the removal of nitrogen oxide in flue gas be denitrification process on our times mainstream, and
Catalyst is the core and key of entire SCR system.
In recent years, commercial SCR catalyst is mainly with WO3For the V of catalyst aid2O5/TiO2, but it is only higher at one
Inversion temperature (350 DEG C~400 DEG C) under just show high catalytic activity[1].Although vanadium series catalyst fires in power plant and diesel oil
Machine field has been realized in extensive commercialization, but still remains some problems, because of SO at high temperature2Be oxidized easily for
SO3, which results in when temperature is higher than 550 DEG C, the catalytic activity and selectivity of catalyst reduce rapidly, while vanadium system is catalyzed
The toxicity of agent is also harmful to environment[2-4].In addition, the operation temperature of this kind of catalyst is generally 350 DEG C~400 DEG C,
Its NO under the operation temperaturexRemoval efficiency is generally 80% or so.The catalyst abrasion applied currently on the market is larger, easy poisoning,
Low temperature active and sulfur resistance are not fine yet.Therefore, either academia or industrial researchers is dedicated to
A kind of novel catalyst is developed, NO significantly more efficient is removed in wide temperature section with thisx, while bavin can also be adapted to
The tail gas denitrification apparatus of oily combustion engine.
Bibliography is：
[1] E.V.Kondratenko, V.A.Kondratenko, M.Richter, R.Fricke.Influence of
02and H2on NO reduction by NH3over Ag/Al2O3：A transient isotopic approach [J],
CataL 2006,239：23-33.
[2] Beijing Shen uncle hero Air Pollution Control Engineering [M]:Chemical Industry Press .2007.
[3] Beijing Hao Jiming, horse numerous Air Pollution Control Engineering [M], Higher Education Publishing House, 2002.
[4] E.C.Corbos, M.Haneda, X.Courtois, P.Marecot, D.Duprez,
H.Hamada.Cooperative effect of Pt-Rh/Ba/AI and CuZSM-5catalysts for NOx
Reduction during periodic lean-rich atmosphere [J], Catal.Cornmun.2008,10：137-
141.
Invention content
In order to overcome the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is that providing a kind of SCR of high sulfur resistive
Denitrating catalyst.Activity is high at low temperature for prepared catalyst, and the removal efficiency of oxynitrides is high, and sulfur resistance is preferable.
Another object of the present invention is to provide the preparation methods of the SCR denitration of above-mentioned high sulfur resistive.
It is still another object of the present invention to provide the applications of the SCR denitration of above-mentioned high sulfur resistive.
The purpose of the present invention is achieved through the following technical solutions：
A kind of SCR denitration of high sulfur resistive is using cordierite honeycomb ceramic as matrix, and described matrix load has catalysis
Agent coating, the catalyst coat are prepared by composite alumina support and precious metal salt；The composite alumina support by
Transition metal salt is prepared with aluminium oxide, wherein the dosage relation of each substance is：Aluminium oxide：Transition metal salt：Precious metal salt
Mass ratio be (75~100)：(5~50)：(5~10)；The catalyst coat is the total matter of SCR denitration of high sulfur resistive
The 5~10% of amount.
The transition metal salt is soluble transition metal salt, a kind of preferably in ammonium heptamolybdate or four oxalic acid hydrate niobium amine
More than.
The precious metal salt is more than one in palladium nitrate or chloroplatinic acid.
The grain size of the aluminium oxide is 30-40nm, and crystalline form is α phases, is purchased from the auxiliary reagent factories Wei Bo of Jiangyan City, technical grade；
The transition metal salt is purchased from Chengdu Ke Long chemical reagents factory, and analysis is pure；
The cordierite honeycomb ceramic is purchased from Corning Incorporated, volume 2.5cm3, 62 holes/cm2,
The precious metal salt is purchased from Kunming Institute of Precious Metals, and analysis is pure.
The preparation method of the SCR denitration of the high sulfur resistive, specifically includes following steps：
(1) wiring solution-forming in 100g deionized waters is added in transition metal salt, adds aluminium oxide, at the uniform velocity stir 1~2h,
Re-ultrasonic dispersion obtains dispersion liquid 1；
(2) use Rotary Evaporators that dispersion liquid 1 in step (1) is rotated solvent evaporated, then at 90~110 DEG C dry 5~
7h is finally warming up to 400~500 DEG C of 3~5h of roasting in Muffle furnace, compound Al is made in air atmosphere2O3Carrier, that is, compound
Alumina support；
(3) by the compound Al in step (2)2O3Carrier impregnation stirs 1~2h, then ultrasound point in precious metal salt solution
It dissipates, obtains dispersion liquid 2, dispersion liquid is rotated into solvent evaporated using Rotary Evaporators, then at 90~110 DEG C of dry 5~7h, finally
400~500 DEG C of 3~5h of roasting are warming up in Muffle furnace in air atmosphere, catalyst coat is made；
(4) deionized water is added in catalyst coat in step (3), ball milling slurry is made in ball milling, and ball milling slurry is coated on violet
On green stone ceramic honey comb matrix, dry 8~10h, heat up calcining in Muffle furnace, then is down to room temperature naturally, obtains high sulfur resistive
SCR denitration.
Transition metal salt described in step (1) and the mass ratio of deionized water are (5~50)：100.
The rotating speed stirred described in step (1) is 100~200r/min, and the frequency of the ultrasonic disperse is 40KHz, described
The time of ultrasonic disperse is 30~40min.
The temperature that evaporation is rotated described in step (2) is 80 DEG C；The heating rate is 2 DEG C/min.
A concentration of 1~5mol/L of precious metal salt solution described in step (3)；The rotating speed of the stirring is 100~200r/
The frequency of min, the ultrasonic disperse are 40KHz, and the time of the ultrasonic disperse is 30~40min；
The temperature that evaporation is rotated described in step (3) is 80 DEG C；The heating rate is 2 DEG C/min.
The mass ratio of deionized water described in step (4) and aluminium oxide in catalyst coat is (100~150)：(75~
100).Rotational speed of ball-mill described in step (4) is 300~500r/min, preferably 400r/min；The Ball-milling Time is 5~6h.
Dry temperature described in step (4) is 80~100 DEG C；The heating rate is 2 DEG C/min；The temperature of the calcining
Degree is 350~450 DEG C, preferably 400 DEG C；The time of the calcining is 2.5~3.5h.
The SCR denitration of the high sulfur resistive is applied to denitrating flue gas field.
Compared with prior art, the invention has the advantages that：
The present invention is using first impregnated transition base metal solution, then impregnates the sequence of precious metal solution, obtains combined type gold
Metal catalyst.The composite metal catalyst compared to for single metallic catalyst have very good low-temperature catalytic activity
And stability, high antisulphuric ability, while non-noble metal introducing greatly reduces the use of noble metal, to reduce catalyst
Cost.
Description of the drawings
Fig. 1 is the denitrating catalyst catalytic performance test curve graph at different temperatures prepared by Examples 1 to 4；
Fig. 2 is the denitrating catalyst stability test curve graph prepared by Examples 1 to 4.
Specific implementation mode
The present invention will be further specifically described in detail with reference to specific embodiments, but embodiments of the present invention are not
It is limited to this, for not specifically specified technological parameter, can refer to routine techniques progress.
Embodiment 1
A kind of preparation method of the denitrating catalyst of high sulfur resistive, specifically includes following steps：
(1) wiring solution-forming in 100g deionized waters is added in 25g ammonium heptamolybdates, adds 75gAl2O3Carrier, at room temperature
1h, rotating speed 100r/min are at the uniform velocity stirred, re-ultrasonic dispersion 30min (supersonic frequency 40KHz) obtains dispersion liquid 1；
(2) dispersion liquid 1 of step (1) is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in 100 DEG C
Dry 6h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 450 DEG C of roastings 4h, obtained compound Al2O3
Carrier, that is, composite alumina support；
(3) 10g chloroplatinic acids are added in 100g deionizations and are made into platinum acid chloride solution, then by the compound Al of step (2)2O3
Carrier is impregnated in platinum acid chloride solution again, at the uniform velocity stirs 1h at room temperature, and rotating speed 100r/min, re-ultrasonic dispersion 30min are (super
Acoustic frequency is 40KHz), obtain dispersion liquid 2；The dispersion liquid 2 of step (1) rotation is carried out in 80 DEG C using Rotary Evaporators to be evaporated
Solvent, then in 100 DEG C of dry 6h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 450 DEG C of roastings
Catalyst coat is made in 4h；
(4) catalyst coat of step (3) is added in 100g deionized waters, ball milling 5h, obtains ball milling slurry (rotational speed of ball-mill
For 400r/min), ball milling slurry is coated on cordierite honeycomb ceramic matrix (2.5cm3, 62 holes/cm2) on, it is dry in baking oven
9h (dry temperature is 90 DEG C), in Muffle furnace ramped heating schedule to 400 DEG C of (heating rate is 2 DEG C/min) calcining 3h, then
Naturally it is down to room temperature, obtains the denitrating catalyst of high sulfur resistive, wherein catalyst coat is the denitrating catalyst gross mass of high sulfur resistive
7%.
Embodiment 2
A kind of preparation method of the denitrating catalyst of high sulfur resistive, specifically includes following steps：
(1) wiring solution-forming in 100g deionized waters is added in 5g ammonium heptamolybdates, adds 90gAl2O3Carrier, at room temperature
1.5h, rotating speed 200r/min are at the uniform velocity stirred, re-ultrasonic dispersion 35min (supersonic frequency 40KHz) obtains dispersion liquid 1；
(2) dispersion liquid 1 of step (1) is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in 110 DEG C
Dry 5h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 400 DEG C of roastings 5h, obtained compound Al2O3
Carrier, that is, composite alumina support；
(3) 5g palladium nitrates are added in 100g deionizations and are made into palladium nitrate solution, then by the compound Al of step (2)2O3It carries
Body is impregnated in palladium nitrate solution, at the uniform velocity stirs 1.5h, rotating speed 200r/min, re-ultrasonic dispersion 35min (ultrasound at room temperature
Frequency is 40KHz), obtain dispersion liquid 2；Dispersion liquid 2 is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in
110 DEG C of dry 5h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 400 DEG C of roasting 5h, obtained catalysis
Agent coating；
(4) catalyst coat in step (3) is added in 120g deionized waters, ball milling 6h, obtains ball milling slurry (rotational speed of ball-mill
For 400r/min), ball milling slurry is coated on cordierite honeycomb ceramic matrix (2.5cm3, 62 holes/cm2) on, it is dry in baking oven
8h (dry temperature is 80 DEG C), in Muffle furnace ramped heating schedule to 400 DEG C of (heating rate is 2 DEG C/min) calcining 3h, then
Naturally it is down to room temperature, obtains the denitrating catalyst of high sulfur resistive, wherein catalyst coat is the denitrating catalyst gross mass of high sulfur resistive
10%.
Embodiment 3
A kind of preparation method of the denitrating catalyst of high sulfur resistive, specifically includes following steps：
(1) wiring solution-forming in 100g deionized waters is added in tetra- oxalic acid hydrate niobium amine of 50g, adds 100gAl2O3Carrier,
2h, rotating speed 150r/min are at the uniform velocity stirred at room temperature, and re-ultrasonic dispersion 40min (supersonic frequency 40KHz) obtains dispersion liquid
1；
(2) dispersion liquid 1 of step (1) is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in 90 DEG C
Dry 7h, under air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 500 DEG C of roasting 3h, compound Al is made2O3Carrier
That is composite alumina support；
(3) 10g chloroplatinic acids are added in 100g deionizations and are made into platinum acid chloride solution, then by compound Al obtained2O3Carrier
It is impregnated in platinum acid chloride solution again, at the uniform velocity stirs 2h, rotating speed 150r/min, re-ultrasonic dispersion 40min (supersonic frequencies at room temperature
Rate is 40KHz), obtain dispersion liquid 2；Dispersion liquid 2 is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in
120 DEG C of dry 7h, under air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 500 DEG C of roasting 3h, catalyst is made and applies
Layer；
(4) 150g deionized waters are added in the catalyst coat of step (3) and ball milling slurry, rotational speed of ball-mill is made in ball milling 5.5h
For 400r/min, ball milling slurry is coated on cordierite honeycomb ceramic matrix (2.5cm3, 62 holes/cm2) on, it is dry in baking oven
10h (dry temperature is 100 DEG C) calcines 3h in Muffle furnace ramped heating schedule to 400 DEG C (heating rate is 2 DEG C/min),
It is down to room temperature naturally again, obtains the denitrating catalyst of high sulfur resistive, wherein catalyst coat is the total matter of denitrating catalyst of high sulfur resistive
The 5% of amount.
Embodiment 4
A kind of preparation method of the denitrating catalyst of high sulfur resistive, specifically includes following steps：
(1) wiring solution-forming in 100g deionized waters is added in tetra- oxalic acid hydrate niobium amine of 25g, adds 100gAl2O3Carrier,
2h is at the uniform velocity stirred at room temperature, and rotating speed 150r/min, re-ultrasonic dispersion 40min, (supersonic frequency 40KHz) is disperseed
Liquid 1；
(2) dispersion liquid 1 of step (1) is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in 110 DEG C
Dry 7h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 500 DEG C of roastings 3h, obtained compound Al2O3
Carrier, that is, composite alumina support；
(3) 7g palladium nitrates are added in 100g deionizations and are made into palladium nitrate solution, then by compound Al obtained2O3Carrier
It is impregnated in palladium nitrate solution again, at the uniform velocity stirs 2h, rotating speed 150r/min, re-ultrasonic dispersion 40min (supersonic frequencies at room temperature
Rate is 40KHz), obtain dispersion liquid 2；Dispersion liquid 2 is subjected to rotation solvent evaporated in 80 DEG C using Rotary Evaporators, then in
120 DEG C of dry 7h, then in air atmosphere in Muffle furnace with the temperature programming of 2 DEG C/min to 500 DEG C of roasting 3h, obtained catalysis
Agent coating；
(4) 150g deionized waters are added in the catalyst coat of step (3) and ball milling slurry, rotational speed of ball-mill is made in ball milling 5.5h
For 400r/min, ball milling slurry is coated on cordierite honeycomb ceramic matrix (2.5cm3, 62 holes/cm2) on, it is dry in baking oven
10h (dry temperature is 100 DEG C) calcines 3h in Muffle furnace ramped heating schedule to 400 DEG C (heating rate is 2 DEG C/min),
It is down to room temperature naturally again, obtains the denitrating catalyst of high sulfur resistive, wherein catalyst coat is the total matter of denitrating catalyst of high sulfur resistive
The 8% of amount.
Preparation-obtained catalyst in above-described embodiment is subjected to denitration efficiency evaluation.
Performance test conditions are as follows：
NO=800ppm, C3H8=800ppm, SO2=100ppm, O2=3vol.%, gas flow rate=2000ml/min,
Air speed=40000h-1。
Under different temperatures, catalyst catalytic performance testing result is as shown in Figure 1.From Fig. 1 it will be seen that example 1,
2, the catalyst prepared by 3,4 all presents good catalytic performance, even in high SO2In the presence of gas.It is real
Catalyst prepared by example 1 can reach 90% NO conversion ratios at 185 DEG C or so, and the catalyst prepared by example 2 exists
195 DEG C or so are the NO conversion ratios that can reach 90%, and the catalyst prepared by example 3 can reach 90% at 225 DEG C or so
NO conversion ratios, the catalyst prepared by example 4 can reach 90% NO conversion ratios at 200 DEG C or so
Detection of Stability test condition is as follows：
NO=800ppm, C3H8=800ppm, SO2=100ppm, O2=3vol.%, gas flow rate=2000ml/min,
Air speed=40000h-1, T=250 DEG C.
The results are shown in Figure 2 for the Detection of Stability of catalyst.Even from Fig. 2 it will be seen that in high SO2Gas
In the presence of, the catalyst prepared by example 1,2,3,4 all presents the stability of good low-temperature catalyzed performance, i.e.,
Continuous operation 100h is set also still to maintain higher activity.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement etc., should be included in the protection of the claims in the present invention made by within spirit and principle
Within the scope of.
Claims (8)
1. a kind of SCR denitration of high sulfur resistive, it is characterised in that：It is the described matrix using cordierite honeycomb ceramic as matrix
Load has catalyst coat, the catalyst coat to be prepared by composite alumina support and precious metal salt；The composite oxygen
Change alumina supporter to be prepared by transition metal salt and aluminium oxide, wherein the dosage relation of each substance is：Aluminium oxide：Transition metal
Salt：The mass ratio of precious metal salt is（75~100）：（5~50）：（5~10）；The catalyst coat is that the SCR denitration of high sulfur resistive is urged
The 5 ~ 10% of agent gross mass；
The precious metal salt is more than one in palladium nitrate or chloroplatinic acid；
The transition metal salt is more than one in ammonium heptamolybdate or four oxalic acid hydrate niobium amine.
2. the preparation method of the SCR denitration of high sulfur resistive according to claim 1, it is characterised in that：Specifically include with
Lower step：
（1）Wiring solution-forming in 100g deionized waters is added in transition metal salt, adds aluminium oxide, at the uniform velocity stirs 1 ~ 2h, then surpass
Sound disperses, and obtains dispersion liquid 1；
（2）Using Rotary Evaporators by step（1）The rotation of middle dispersion liquid 1 is evaporated, and then at 90 ~ 110 DEG C of dry 5 ~ 7 h, is finally existed
400 ~ 500 DEG C of 3 ~ 5 h of roasting are warming up under air atmosphere in Muffle furnace, compound Al is made2O3Carrier, that is, composite alumina carries
Body；
（3）By step（2）In compound Al2O3Carrier impregnation stirs 1 ~ 2h in precious metal salt solution, and re-ultrasonic dispersion obtains
Dispersion liquid is rotated solvent evaporated by dispersion liquid 2 using Rotary Evaporators, then at 90 ~ 110 DEG C of dry 5 ~ 7 h, finally in air
400 ~ 500 DEG C of 3 ~ 5 h of roasting are warming up under atmosphere in Muffle furnace, catalyst coat is made；
（4）By step（3）Deionized water is added in middle catalyst coat, and ball milling slurry is made in ball milling, and ball milling slurry is coated on cordierite
On ceramic honey comb matrix, dry 8 ~ 10h, heat up calcining in Muffle furnace, then is down to room temperature naturally, and the SCR for obtaining high sulfur resistive is de-
Denox catalyst.
3. the preparation method of the SCR denitration of high sulfur resistive according to claim 2, it is characterised in that：Step（1）Middle institute
The mass ratio for stating transition metal salt and deionized water is（5~50）：100；
Step（1）Described in the rotating speed that stirs be 100 ~ 200r/min, the frequency of the ultrasonic disperse is 40KHz, the ultrasound
The time of dispersion is 30 ~ 40min.
4. the preparation method of the SCR denitration of high sulfur resistive according to claim 2, it is characterised in that：Step（3）Middle institute
State a concentration of 1 ~ 5mol/L of precious metal salt solution；The rotating speed of the stirring is 100 ~ 200r/min, the frequency of the ultrasonic disperse
Rate is 40KHz, and the time of the ultrasonic disperse is 30 ~ 40min.
5. the preparation method of the SCR denitration of high sulfur resistive according to claim 2, it is characterised in that：Step（2）Middle institute
The temperature for stating revolving evaporation is 80 DEG C；The heating rate is 2 DEG C/min；
Step（3）Described in rotate evaporation temperature be 80 DEG C；The heating rate is 2 DEG C/min.
6. the preparation method of the SCR denitration of high sulfur resistive according to claim 2, it is characterised in that：Step（4）Middle institute
It states deionized water and the mass ratio of aluminium oxide in catalyst coat is（100~150）：（75~100）；
Step（4）Described in rotational speed of ball-mill be 300 ~ 500 r/min；The Ball-milling Time is 5 ~ 6h.
7. the preparation method of the SCR denitration of high sulfur resistive according to claim 2, it is characterised in that：Step（4）Middle institute
The temperature for stating heating calcining is 350 ~ 450 DEG C, and the time of the calcining is 2.5 ~ 3.5h；
The temperature of the drying is 80 ~ 100 DEG C；The heating rate is 2 DEG C/min.
8. the application of the SCR denitration of high sulfur resistive according to claim 1, it is characterised in that：The SCR of the high sulfur resistive
Denitrating catalyst is applied to denitrating flue gas field.
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