CN104549280A - Preparation method of SCR denitration catalyst - Google Patents
Preparation method of SCR denitration catalyst Download PDFInfo
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- CN104549280A CN104549280A CN201510039629.1A CN201510039629A CN104549280A CN 104549280 A CN104549280 A CN 104549280A CN 201510039629 A CN201510039629 A CN 201510039629A CN 104549280 A CN104549280 A CN 104549280A
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Abstract
The invention discloses a preparation method of an SCR denitration catalyst. The preparation method of the SCR denitration catalyst comprises the following steps: firstly, preparing a mixed solution; secondly, pumping and filtering; thirdly, carrying out extrusion moulding and drying; fourthly, calcining; and fifthly, grinding and sieving, wherein the main ingredient of the SCR denitration catalyst is iron trioxide, the particle size is 35-65 meshes, the specific surface area is large and is up to 93.76m<2>/g, and the aperture is 12nm. Aiming at overcoming the defects in the prior art, the invention provides the SCR denitration catalyst which has high low temperature catalytic activity and strong anti-sulphide-poisioning property and can be used for effectively removing nitrogen oxide in flue gas; meanwhile, the SCR denitration catalyst is simple in preparation process, the cost is low, and the yield can be 99%, so that the SCR denitration catalyst is applicable to industrial mass production and has a great application prospect in the field of denitration of industrial flue gas.
Description
Technical field
The invention belongs to catalysis technical field, relate to a kind of preparation method of SCR denitration, be specifically related to SCR denitration that a kind of low-temperature catalytic activity is high, resisting sulfide poisoning capability is strong and preparation method thereof.
Background technology
Along with the national economic development, population increase and the quickening of urbanization process, thing followed problem of environmental pollution highlights day by day, especially SO
2and NO
xemission problem.NO in air
xacid rain, photochemical fog, surface water eutrophication etc. can be caused to destroy ecological environment and jeopardize the series of problems of human health." 12 " environmental protection plans proposes, NO
xto attach most importance to control polluted articles, specified national NO by 2015
xtotal emission volumn, lower than 2046.2 ten thousand tons, reduced 10% than 2010.NO
xbecome the emphasis of China's next stage pollution emission reduction.Therefore, to NO
xprocess particularly important.Current gas denitrifying technology has wet denitration and Dry denitration, mainly contains several classes such as gas-phase reaction method, liquid absorption method, absorption method, liquid-film method, microbial method.Wherein gas-phase reaction method divides again 3 classes: 1. electron beam irradiation method and impulse electric corona plasma method; 2. selective catalytic reduction (SCR), selective non-catalytic reducing process (SNCR) and red-hot carbon reduction method; 3. low temperature normal atmosphere plasma decomposition method.Current denitration efficiency technology that is the highest, maturation the most is SCR (SCR) technology.
SCR method is current most widely used gas denitrifying technology in the world, in most of power plant of the countries such as Japan, Europe, the U.S., all apply this technology.NH
3-SCR refers in temperature range (80 ~ 400 DEG C) in aerobic situation, suitable, reducing agent NH
3under the effect of catalyst, by NO
xselective reduction is N
2and water.Its reaction equation is as follows:
4NH
3+4NO+O
2→4N
2+6H
2O (1)
4NH
3+2NO
2+O
2→3N
2+6H
2O (2)
8NH
3+6NO
2→7N
2+12H
2O (3)
Most of NO in industry
xremove mainly to react (1).Do not wish in SCR process to generate N
2o, it not only can reduce the selective of reaction, but also as depletion of the ozone layer gas and greenhouse gases.
Catalyst at present for SCR reaction mainly contains three types: noble metal catalyst, molecular sieve catalyst and metal oxide catalyst.Noble metal catalyst due to selective poor and cost higher, in common SCR reaction replace by the metal oxide catalyst of routine.Current most study, be also the most ripe catalyst be metal oxide-type catalyst, mainly comprise V
2o
5, C
uo, C
ro
x, M
no, M
go, M
oo
3in metal oxide or its mixture; Using maximum is with the sharp ore deposit TiO that admires
2for the vanadium class catalyst V of carrier
2o
5/ TiO
2, this type of catalyst often adds a certain amount of WO
3, M
oo
3deng, be used for strengthening the activity of denitrating catalyst, surface acidity, heat endurance suppress SO
2oxidation.The feature of molecular sieve catalyst is that reaction temperature is higher, reaches as high as 600 DEG C, NO
xconversion ratio is higher, NH
3leak few, but higher reaction temperature limit the commercial Application of molecular sieve catalyst.These catalyst great majority at high temperature use, and sulfur resistance is poor, and the existence of sulfide is easy to cause the poisoning of catalyst, makes it lose efficacy.But under low dust-laden arrangement, flue-gas temperature have dropped a lot, and between 150 ~ 200 DEG C, this proposes challenge to the low temperature active of catalyst.
Therefore develop and there is low temperature active and ability SO
2poisoning denitrating catalyst has very important significance for the fume treatment tool of thermal power plant and Industrial Stoves.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of preparation method of SCR denitration.Denitrating catalyst provided by the invention has very high catalytic activity at flue-gas temperature 130 ~ 260 DEG C, effectively can remove the nitrogen oxide in flue gas, and there is stronger resisting sulfide poisoning performance, can as the denitrating catalyst of the fume treatment of the thermal power plant of the overwhelming majority and Industrial Stoves.
The present invention is achieved by the following technical solutions:
The invention provides a kind of preparation method of SCR denitration, described preparation method specifically comprises following steps:
Step one, preparation mixed solution: take ferric sulfate solid and ferrous sulfate solid respectively, add water, after being uniformly mixed, ultrasonic with ultrasonic equipment, leave standstill, then add ammoniacal liquor, stir until pH is alkalescence, obtain mixed solution;
Step 2, suction filtration: left standstill by described mixed solution, occur sediment, through suction filtration, rinse repeatedly, obtains pure sediment;
Step 3, extrusion molding and drying: put described pure sediment into mould, extrusion molding; By described shaping after sediment be placed in 110 ~ 120 DEG C at dry 8 ~ 12h, obtain dry sediment;
Step 4, calcining: calcine 5 ~ 8h at described dry sediment is placed in 350 ~ 450 DEG C, take out, and under drying condition, room temperature cooling, obtains calcining sediment;
Step 5, to crush and screen: will forge after described burning sediment pulverizes, and sift out 35 ~ 65 order powder, namely obtain SCR denitration.
Preferably, in step one, the parts by weight of described ferric sulfate solid are 20 ~ 80 parts, and the parts by weight of described ferrous sulfate solid are 2 ~ 6 parts.
Preferably, in step one, described water is deionized water; Described ultrasonic equipment ultrasonic time is 30min.
Preferably, in step one, described ammoniacal liquor volume is 1/2 of mixed liquor volume.
Preferably, in step one, described alkalescence specifically refers to that the pH value of solution is 8.0.
Preferably, in step 2, described flushing refers to uses deionized water rinsing.
Preferably, in step 3, the equipment of described drying comprises baking oven.
Preferably, in step 4, the equipment of described calcining comprises Muffle furnace.
Preferably, in step 4, described drying is included in drier dry.
Preferably, in step 5, described pulverizing comprises pulverizes with pulverizer.
The main component of SCR denitration prepared by the inventive method is di-iron trioxide, and particle diameter is 35 ~ 65 orders, and specific area reaches 93.76m
2/ g, aperture is 12nm.
Compared with prior art, the present invention has following beneficial effect:
(1) adopt above-mentioned method for preparing catalyst, obtain a kind of novel denitrating catalyst Fe
2o
3.Powder Fe
2o
3denitrating catalyst has very high catalytic activity at low temperatures, and specific area is comparatively large, reaches 93.76m
2/ g, aperture is 12nm; Resistance to sulfur dioxide toxicity is comparatively strong, is applicable to most thermal power plants and the fume treatment of Industrial Stoves, effectively can improves the removal efficiency of the nitrogen oxide of industrial smoke;
(2) whole preparation process is simple, economy with low cost, and simple to operate, productive rate can reach 99%, is suitable for industrialized mass; Due to nanometer Fe
2o
3catalyst has above-mentioned good characteristic, has larger application prospect in the denitration field of industrial smoke.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.In following examples, ferric sulfate, ferrous sulfate and ammoniacal liquor are all purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
embodiment 1
The present embodiment prepares a kind of SCR denitration, and preparation method comprises the following steps:
(1) mixed solution is prepared: the ferrous sulfate solid of the ferric sulfate solid and 2.4g that take 20g is respectively inserted in 250mL beaker, adds 150mL deionized water, after being uniformly mixed, with the ultrasonic 30min of ultrasonic equipment; After leaving standstill a period of time, in solution, then slowly add ammoniacal liquor (volume ratio is 1:1), stir until solution ph is 8.0 simultaneously;
(2) suction filtration: after above-mentioned (1) solution left standstill a period of time, there is a large amount of sediments, carry out suction filtration by Suction filtration device to containing sedimentary solution, constantly by deionized water, sediment is rinsed repeatedly, obtain purer sediment;
(3) extrusion molding and drying: put the sediment that above-mentioned (2) obtain into mould, carry out extrusion molding, then puts into baking oven by the sediment after shaping, at 110 ~ 120 DEG C, dries 8h;
(4) calcine: the sediment after drying is put in Muffle furnace, at 350 DEG C, calcines 5h, after taking-up, put in drier and at room temperature cool.
(5) crush and screen: the solids after calcining is put into pulverizer, after being pulverized, therefrom sieves out 35 ~ 65 object powder, namely obtain pulverous denitrating catalyst Fe
2o
3.
embodiment 2
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method comprises the following steps:
(1) mixed solution is prepared: the ferrous sulfate solid of the ferric sulfate solid and 4.2g that take 40g is respectively inserted in 250mL beaker, adds 150mL deionized water, after being uniformly mixed, with the ultrasonic 30min of ultrasonic equipment; After leaving standstill a period of time, in solution, then slowly add ammoniacal liquor (volume ratio is 1:1), stir until the pH value of solution is 8.0 simultaneously;
(2) suction filtration: after above-mentioned (1) solution left standstill a period of time, there is a large amount of sediments, carry out suction filtration by Suction filtration device to containing sedimentary solution, constantly by deionized water, sediment is rinsed repeatedly, obtain purer sediment;
(3) extrusion molding and drying: put the sediment that above-mentioned (2) obtain into mould, carry out extrusion molding, then puts into baking oven by the sediment after shaping, at 110 ~ 120 DEG C, dries 9h;
(4) calcine: the sediment after drying is put in Muffle furnace, at 410 DEG C, calcines 6h, after taking-up, put in drier and at room temperature cool;
(5) crush and screen: the solids after calcining is put into pulverizer, after being pulverized, therefrom sieves out 35 ~ 65 object powder, namely obtain pulverous denitrating catalyst Fe
2o
3.
embodiment 3
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method comprises the following steps:
(1) mixed solution is prepared: the ferrous sulfate solid of the ferric sulfate solid and 4.2g that take 50g is respectively inserted in 250mL beaker, adds 150mL deionized water, after being uniformly mixed, with the ultrasonic 30min of ultrasonic equipment.After leaving standstill a period of time, in solution, then slowly add ammoniacal liquor (volume ratio is 1:1), stir until the pH value of solution is 8.0 simultaneously;
(2) suction filtration: after above-mentioned (1) solution left standstill a period of time, there is a large amount of sediments, carry out suction filtration by Suction filtration device to containing sedimentary solution, constantly by deionized water, sediment is rinsed repeatedly, obtain purer sediment;
(3) extrusion molding and drying: put the sediment that above-mentioned (2) obtain into mould, carry out extrusion molding, then puts into baking oven by the sediment after shaping, at 110 ~ 120 DEG C, dries 10h;
(4) calcine: the sediment after drying is put in Muffle furnace, at 380 DEG C, calcines 8h, after taking-up, put in drier and at room temperature cool;
(5) crush and screen: the solids after calcining is put into pulverizer, after being pulverized, therefrom sieves out 35 ~ 65 object powder, namely obtain pulverous denitrating catalyst Fe
2o
3.
embodiment 4
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method comprises the following steps:
(1) mixed solution is prepared: the ferrous sulfate solid of the ferric sulfate solid and 5.1g that take 60g is respectively inserted in 250mL beaker, adds 150mL deionized water, after being uniformly mixed, with the ultrasonic 30min of ultrasonic equipment; After leaving standstill a period of time, in solution, then slowly add ammoniacal liquor (volume ratio is 1:1), stir until the pH value of solution is 8.0 simultaneously;
(2) suction filtration: after above-mentioned (1) solution left standstill a period of time, there is a large amount of sediments, carry out suction filtration by Suction filtration device to containing sedimentary solution, constantly by deionized water, sediment is rinsed repeatedly, obtain purer sediment;
(3) extrusion molding and drying: put the sediment that above-mentioned (2) obtain into mould, carry out extrusion molding, then puts into baking oven by the sediment after shaping, at 110 ~ 120 DEG C, dries 11h;
(4) calcine: the sediment after drying is put in Muffle furnace, at 430 DEG C, calcines 7h, after taking-up, put in drier and at room temperature cool;
(5) crush and screen: the solids after calcining is put into pulverizer, after being pulverized, therefrom sieves out 35 ~ 65 object powder, namely obtain pulverous denitrating catalyst Fe
2o
3.
embodiment 5
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method comprises the following steps:
(1) mixed solution is prepared: the ferrous sulfate solid of the ferric sulfate solid and 6.0g that take 80g is respectively inserted in 250mL beaker, adds 150mL deionized water, after being uniformly mixed, with the ultrasonic 30min of ultrasonic equipment; After leaving standstill a period of time, in solution, then slowly add ammoniacal liquor (volume ratio is 1:1), stir until the pH value of solution is 8.0 simultaneously;
(2) suction filtration: after above-mentioned (1) solution left standstill a period of time, there is a large amount of sediments, carry out suction filtration by Suction filtration device to containing sedimentary solution, constantly by deionized water, sediment is rinsed repeatedly, obtain purer sediment;
(3) extrusion molding and drying: put the sediment that above-mentioned (2) obtain into mould, carry out extrusion molding, then puts into baking oven by the sediment after shaping, at 110 ~ 120 DEG C, dries 12h;
(4) calcine: the sediment after drying is put in Muffle furnace, at 450 DEG C, calcines 5h, after taking-up, put in drier and at room temperature cool;
(5) crush and screen: the solids after calcining is put into pulverizer, after being pulverized, therefrom sieves out 35 ~ 65 object powder, namely obtain pulverous denitrating catalyst Fe
2o
3.
embodiment 6
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method is identical with embodiment 5, and difference is only that the weight of ferric sulfate solid in step (1) is 80g, the weight of ferrous sulfate solid is 2.0g.
embodiment 7
The present embodiment provides a kind of SCR denitration and preparation method thereof, and described preparation method is identical with embodiment 5, and difference is only that the weight of ferric sulfate solid in step (1) is 20g, the weight of ferrous sulfate solid is 6.0g.
performance Detection
With BASF denitrating catalyst for contrasting 1, with the sharp ore deposit TiO that admires
2for the vanadium class catalyst V of carrier
2o
5/ TiO
2compare 2, di-iron trioxide prepared by conventional method is contrast 3, detect the performance of SCR denitration prepared by embodiment 1 ~ 7, result as in the table below.
(1) reaction condition: NO content 600ppm, NH in mist
3content 600ppm, SO
2content 100ppm, O
2content is 3% (volume ratio), and gas flow rate is 150L/h, N
2for Balance Air, under this condition, denitrating catalyst performance test results is as shown in table 1 below:
The denitration efficiency of table 1 catalyst when sulfide concentration is lower
(2) reaction condition: NO content 600ppm, NH in mist
3content 600ppm, SO
2content 600ppm, O
2content is 3% (volume ratio), and gas flow rate is 150L/h, N
2for Balance Air, under this condition, denitrating catalyst performance test results is as shown in table 2 below:
The denitration efficiency of table 2 catalyst when sulfide concentration is higher
From table 1 and table 2, when sulfide concentration is higher, the denitration efficiency of denitrating catalyst of the present invention reduces by 10% ~ 15% than denitration efficiency during sulfide low concentration; Under similarity condition, when sulfide concentration is higher, and the denitration efficiency of commercially available BASF SCR denitration reduces by 20% ~ 30% than denitration efficiency during sulfide low concentration, vanadium class catalyst V
2o
5/ TiO
2, the di-iron trioxide prepared of conventional method is also larger by the impact of sulfoxide concentration.
In sum, compared with prior art, the performance of the SCR denitration prepared by preparation method of the present invention is better, and namely preparation method of the present invention has significant advantageous effect and technological progress.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. a preparation method for SCR denitration, is characterized in that, described preparation method specifically comprises following steps:
Step one, preparation mixed solution: take ferric sulfate solid and ferrous sulfate solid respectively, add water, after being uniformly mixed, ultrasonic with ultrasonic equipment, leave standstill, then add ammoniacal liquor, stir until pH is alkalescence, obtain mixed solution;
Step 2, suction filtration: left standstill by described mixed solution, occur sediment, through suction filtration, rinse repeatedly, obtains pure sediment;
Step 3, extrusion molding and drying: put described pure sediment into mould, extrusion molding; By described shaping after sediment be placed in 110 ~ 120 DEG C at dry 8 ~ 12h, obtain dry sediment;
Step 4, calcining: calcine 5 ~ 8h at described dry sediment is placed in 350 ~ 450 DEG C, take out, and under drying condition, room temperature cooling, obtains calcining sediment;
Step 5, to crush and screen: will forge after described burning sediment pulverizes, and sift out 35 ~ 65 order powder, namely obtain SCR denitration.
2. the preparation method of SCR denitration according to claim 1, is characterized in that, in step one, the parts by weight of described ferric sulfate solid are 20 ~ 80 parts, and the parts by weight of described ferrous sulfate solid are 2 ~ 6 parts.
3. the preparation method of SCR denitration according to claim 1, is characterized in that, in step one, described water is deionized water; Described ultrasonic equipment ultrasonic time is 30min.
4. the preparation method of SCR denitration according to claim 1, is characterized in that, in step one, described ammoniacal liquor volume is 1/2 of mixed liquor volume.
5. the preparation method of SCR denitration according to claim 1, is characterized in that, in step one, described alkalescence specifically refers to that the pH value of solution is 8.0.
6. the preparation method of SCR denitration according to claim 1, is characterized in that, in step 2, described flushing refers to uses deionized water rinsing.
7. the preparation method of SCR denitration according to claim 1, is characterized in that, in step 3, the equipment of described drying comprises baking oven.
8. the preparation method of SCR denitration according to claim 1, is characterized in that, in step 4, the equipment of described calcining comprises Muffle furnace.
9. the preparation method of SCR denitration according to claim 1, is characterized in that, in step 4, described drying is included in drier dry.
10. the preparation method of SCR denitration according to claim 1, is characterized in that, in step 5, described pulverizing comprises pulverizes with pulverizer.
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Cited By (1)
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CN105771990A (en) * | 2015-12-17 | 2016-07-20 | 西华师范大学 | Iron oxide catalyst, preparation method therefor and application of iron oxide catalyst |
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Cited By (2)
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