CN107469847A - A kind of preparation method of denitrating catalyst - Google Patents
A kind of preparation method of denitrating catalyst Download PDFInfo
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- CN107469847A CN107469847A CN201710995475.2A CN201710995475A CN107469847A CN 107469847 A CN107469847 A CN 107469847A CN 201710995475 A CN201710995475 A CN 201710995475A CN 107469847 A CN107469847 A CN 107469847A
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/187—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01D53/34—Chemical or biological purification of waste gases
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Abstract
The invention discloses a kind of preparation method of the slag based denitration catalyst of modification, load what is obtained by pretreatment of slag → slag modification → active component, it is by the way that the slag after activation is added in sucrose solution that wherein slag, which is modified, 2 ~ 4h is handled at 180 ~ 220 DEG C, filtered, washing, dries, be calcined the modified steel scoria for obtaining being covered with carbosphere coating.The denitrating catalyst of the present invention as catalyst carrier, not only reduces the producing cost of catalyst using modified steel scoria；More make the specific surface area of slag from 4 ~ 54m2/ g brings up to 400 ~ 600m2/ g, while catalytic reaction temperature is widened to 150 ~ 450 DEG C；Its anti-sulfur poisonous performance is improved, there is important promotional value.
Description
Technical field
The present invention relates to environmental catalysis technical field, is related to a kind of denitrating catalyst and preparation method thereof, more particularly to
A kind of preparation method of the slag based denitration catalyst of modification.
Background technology
In recent years, China NOxDischarge constantly increase, ecological environment and human body health are caused huge harm and
NO in toxic action, particularly precipitation3 -/SO4 2-Ratio is just increasing year by year in China, and Acid Rain Pollution is via sulfuric acid type
To sulfuric acid, the compound transformation of nitric acid, city atmospheric environment situation is still severe, and regional atmosphere polluting problem becomes clear day by day.NOx
Pollution is mostly derived from the fixed source emission and motor-vehicle tail-gas etc. such as coal-fired plant flue gas and moves source emission.According to the statistics made by the departments concerned
China's nitrogen oxide emission total amount reaches 20,000,000 tons within 2008, turns into the first in the world discharge state.If without control, nitrogen oxides
Discharge capacity is up to 30,000,000 tons the year two thousand twenty is estimated, and grave danger is brought to China's atmospheric environment.
How NO is effectively removedxAs the important topic of current field of environment protection.With NH3Urged for the selectivity of reducing agent
Change reduction NOx(NH3 - SCR) technology is because it has higher denitration efficiency, N2Selectivity and well economical, at present
As in the world using most, the most ripe effective denitration technologies.NH3 The core of-SCR technology is catalyst, at present China
The SCR catalyst of research and development is mainly with anatase titanium dioxide TiO2Or molecular sieve be carrier catalyst, but its production cost it is higher and
Technology barriers be present in some key links and then inhibit it to obtain extensive use.Therefore, the system of cheap SCR catalyst is sought
Preparation Method, for promoting stationary source denitrating flue gas to have important practical significance and economic value.
The patent of invention of Application No. 201310282608.3 disclose a kind of SCR denitration based on slag and its
Preparation method, using solid metallurgical steel slag as raw material, it is 4.8174 ~ 54.6885m that surface area is made after pickling is dried for it2/ g, put down
The SCR denitration that equal aperture is 64 ~ 110nm.It is simple that the catalyst does not add active component, preparation technology, but its
Reaction temperature window is narrower by 150 ~ 250oC, denitration efficiency are only 78 ~ 84%, and water resistant sulfur tolerance does not embody, in a word its
Overall catalytic effect is further improved.
The content of the invention
In order to solve problems of the prior art, the present invention disclose a kind of modification slag based denitration catalyst and its
Preparation method.
The present invention adopts the following technical scheme that realization.
A kind of preparation method of the slag based denitration catalyst of modification, is achieved by the steps of：
（1）Pretreatment of slag：By raw material slag crushing grinding, screening out the slags of 40 ~ 60 mesh, to be dissolved in mass concentration be 2 ~ 3wt%
Salpeter solution in, handle 12-24h under 250 ~ 350r/min stirring condition, then filtered, washing, and 105 ~ 130
10 ~ 14h is dried under the conditions of DEG C, the slag after being activated, raw material slag impurity can not only be removed, can more improve slag surface
Roughness, to facilitate in step（2）More preferable slag modification is carried out, wherein, the mass volume ratio of slag and salpeter solution is
0.5~1.0g/mL；
（2）Slag is modified：At ambient temperature, sucrose is completely dissolved in deionized water, then adds step thereto（1）Institute
Slag after the activation obtained, and stir 10min and obtain mixture A；Then mixture A is transferred in hydrothermal reaction kettle in 180 ~
220 DEG C of 2 ~ 4h of processing, obtain mixture B；Mixture B is filtered, and after washing 2 ~ 4 times with absolute ethyl alcohol, is placed in 110 DEG C of bar
Drying process 6h under part, 4h is calcined under 500 DEG C of nitrogen atmosphere, obtains being covered with the modified steel scoria of carbosphere coating；Wherein,
Sucrose and the mass volume ratio of deionized water are 0.5g/mL, and the weight ratio of slag and sucrose is 1:1；
（3）Active component loads：By WO3Presoma and oxalic acid are dissolved in deionized water, are stirred at room temperature to being completely dissolved；So
Cerium salt is added afterwards and molysite continues to stir 30min, adds step（2）The modified steel scoria of middle gained, obtains mixture C；Will be mixed
Compound C is placed in 60 ~ 80 DEG C of water-bath carries out slow evaporation under agitation, until the moisture on its surface disappears, then puts
10 ~ 14h of drying process under the conditions of 105 ~ 130 DEG C, and then be transferred in high-temperature heater, in N2In 500 under the atmosphere of protection
DEG C 5h is continued with, obtain catalyst；Wherein, WO3Presoma is ammonium tungstate or ammonium paratungstate；Cerium salt is cerous sulfate or cerous sulfate
Ammonium；Molysite is ferric sulfate or iron ammonium sulfate；nw:nFe:nCeElemental mole ratios be 1：（0.5~5）：（0.5~5）, WO3Presoma
Weight and modified steel scoria weight ratio be 3% ~ 10%.
As a kind of preferred embodiment, step（1）In raw material slag it is molten using planetary mills crushing grinding, nitric acid
The concentration of liquid is 3wt%.
Compared with prior art, the advantage of the invention is that：
（1）For the catalyst of the present invention using modified steel scoria as catalyst carrier, it greatly reduces the producing cost of catalyst,
The overall preparation technology of catalyst is simple, is easy to amplify；A new way is provided for the recycling of slag simultaneously, makes it
Added value is lifted；
（2）The catalyst of the present invention is using nitric acid pre-treatment pore-creating and surface coating carbosphere, so as to so that its specific surface area
From 4 ~ 54m2/ g brings up to 400 ~ 600m2/ g, its one side is advantageous to active component W, Fe and Ce and disperseed on its surface, to urge
Change reaction and more reactivity sites are provided；On the other hand higher specific surface area is advantageous to NO and NH3Suction on its surface
It is attached, so as to strengthen the progress of catalytic reaction；Covering of the ammonium sulfate to its active sites can be suppressed to a certain extent simultaneously, from
And improve its anti-sulfur poisonous performance；
（3）The catalyst of the present invention itself contains component Fe using slag as carrier2O3、FeO、MnO2It can also join etc. component
With NH3- SCR, its active component collective effect with load so as to so that slag catalytic reaction temperature window from 150 ~
250oC is widened to 150 ~ 450 DEG C；Simultaneously as using the sulfate of cerium and iron as active component, it can be prevented due to work
Property component occur sulphation caused by sulfur poisoning, so as to enhance the anti-sulfur poisonous performance of catalyst.
Embodiment
In order that those skilled in the art more fully understands technical scheme, and make the present invention features described above,
Purpose and advantage become apparent from understandable, are further explained explanation to the present invention in conjunction with embodiment, it is noted that herein
All embodiments listed are merely illustrative, are not meant to be defined the scope of the invention.Institute in following examples
It is as shown in the table for the composition composition of the slag used
。
Embodiment 1
A kind of preparation method of the slag based denitration catalyst of modification, is achieved by the steps of：
（1）Pretreatment of slag：Using planetary mills by slag crushing, screening out the slags of 40 ~ 60 mesh, to be dissolved in mass concentration be 3wt%
Salpeter solution in, wherein, the mass volume ratio of slag and salpeter solution is 1.0g/mL, by its 300r/min stirring bar
16h is handled under part, not molten slag is then subjected to filtration washing until then the pH value of filtrate is placed on 105 to 6.8-7.2
Drying process 14h under conditions of DEG C；
（2）Slag is modified：Weigh 100g sucrose to be dissolved in 200mL deionized waters, 20min, which is stirred at room temperature, makes it completely molten
Solution, 100g steps are then added thereto（1）Slag after the activation of middle gained, and continue stir process 10min and obtain mixture
A, then mixture A is transferred in hydrothermal reaction kettle and handles 3h in 200 DEG C, obtains mixture B, the mixture B of gained is passed through
Washed 3 times using absolute ethyl alcohol after filtering, and drying process 6h under conditions of being placed on 110 DEG C, then at 500 DEG C of nitrogen gas
Calcination process 4h obtains being covered with the modified steel scoria of carbosphere coating under atmosphere；
（3）Active component loads：The oxalic acid of the ammonium tungstate and 10g that weigh 10g respectively is dissolved in 200mL deionized waters, in room temperature
Lower stirring 20min is completely dissolved it；Cerous sulfate and ferric sulfate are then added thereto and continues to stir 30min, then to it
Middle addition 100g steps（2）The modified steel scoria of middle gained, obtains mixture C；Mixture C is placed in 80 DEG C of water-bath and stirred
Under the conditions of carry out slow evaporation, until its surface moisture disappear；Drying process 12h under conditions of being subsequently placed in 115 ± 1 DEG C,
And then be transferred in high-temperature heater, in N25h is continued with 500 DEG C under the atmosphere of protection, that is, obtains denitrating catalyst A.Its
Middle nw:nFe:nCeElemental mole ratios be 1：1：1.
Embodiment 2
A kind of preparation method of the slag based denitration catalyst of modification, is achieved by the steps of：
（1）Pretreatment of slag：Using planetary mills by slag crushing, screening out the slags of 40 ~ 60 mesh, to be dissolved in mass concentration be 2wt%
Salpeter solution in, wherein, the mass volume ratio of slag and salpeter solution is 0.5g/mL, by its 350r/min stirring bar
12h is handled under part, not molten slag is then subjected to filtration washing until then the pH value of filtrate is placed on 120 to 6.8-7.2
Drying process 12h under conditions of DEG C；
（2）Slag is modified：Weigh 100g sucrose and be dissolved in 200mL deionized waters and be stirred at room temperature to sucrose dissolving completely,
Then 100g steps are added thereto（1）Slag after the activation of middle gained simultaneously continues stir process 10min, obtains mixture A,
Then mixture A is transferred in hydrothermal reaction kettle and handles 4h in 180 DEG C, obtain mixture B；Mixture B is adopted after filtering
Washed 2 times with absolute ethyl alcohol, drying process 6h under conditions of being placed in 110 DEG C, the calcination process 4h under 500 DEG C of nitrogen atmosphere
Obtain being covered with the modified steel scoria of carbosphere coating；
（3）Active component loads：The oxalic acid of the ammonium paratungstate and 10g that weigh 10g respectively is dissolved in 200mL deionized waters, in room
The lower stirring of temperature is completely dissolved ammonium paratungstate and oxalic acid；Then a certain amount of Cericammoniumsulfate and iron ammonium sulfate are added thereto simultaneously
Continue to stir 30min, then add 100g steps thereto（2）The modified steel scoria of middle gained；Gained mixture is placed in 60 DEG C
Water-bath in carry out slow evaporation under agitation, until its surface moisture disappear；Done under conditions of being subsequently placed in 105 DEG C
Dry processing 14h, and then be transferred in high-temperature heater, in N25h is continued with 500 DEG C under the atmosphere of protection, that is, obtains denitration
Catalyst B.Wherein nw:nFe:nCeElemental mole ratios be 1：0.5：0.5.
Embodiment 3
A kind of preparation method of the slag based denitration catalyst of modification, is achieved by the steps of：
（1）Pretreatment of slag：Using planetary mills by slag crushing, screening out the slags of 40 ~ 60 mesh, to be dissolved in mass concentration be 3wt%
Salpeter solution in, wherein, the mass volume ratio of slag and salpeter solution is 0.70g/mL, by its 250r/min stirring bar
18h is handled under part, not molten slag is then subjected to filtration washing until the pH value of filtrate is 7, is then placed on 130 DEG C of bar
Drying process 10h under part；
（2）Slag is modified：Weigh 100g sucrose and be dissolved in 200mL deionized waters dissolving completely at room temperature, then thereto
Add 100g steps（1）Slag after the activation of middle gained, and continue stir process 10min, mixture A；Then it is mixed by what is obtained
Compound A is transferred in hydrothermal reaction kettle handles 2h in 220 DEG C, by the mixture of gained after filtering using absolute ethyl alcohol washing 4
It is secondary, drying process 6h under conditions of being placed in 110 DEG C, the calcination process 4h under 500 DEG C of nitrogen atmosphere, obtain being covered with carbosphere
The modified steel scoria of coating；
（3）Active component loads：The oxalic acid of the ammonium tungstate and 10g that weigh 10g respectively is dissolved in 200mL deionized waters, in room temperature
Under be completely dissolved；A certain amount of cerous sulfate and ferric sulfate are then added thereto and continues to stir 30min, are then added thereto
100g steps（2）The modified steel scoria of middle gained；Gained mixture is placed in 70 DEG C of water-bath and carried out under agitation slowly
Evaporation, until the moisture of catalyst support surface disappears；Drying process 10h, enters under conditions of gained catalyst is placed in into 130 DEG C
And it is transferred in high-temperature heater in N25h is continued with 500 DEG C under the atmosphere of protection, that is, obtains denitrating catalyst C.Wherein
nw:nFe:nCeElemental mole ratios be 1：5：5.
Performance test is carried out to the gained catalyst of above-described embodiment 1 ~ 3, test condition is：Enter in fixed bed reactors
OK, simulated flue gas composition is：1000ppmNH3, 1000ppm NO, 6% O2, 300ppm SO2(when needing), 10%H2O (needs
When), N2For Balance Air, total flow 600mL/min, reaction velocity is 30000 h-1, reaction temperature is 150 ~ 450 DEG C, reaction
NO and NO in product2Content carries out analysis measure with flue gas analyzer KM9106, and specific test result is as shown in table 2 below.
Table 2
。
Embodiment 4
By obtained catalyst A in embodiment 1, SO is investigated on fixed bed reactors2And H2Shadows of the O to catalytic reaction activity
Ring.The composition of reaction mixture gas is [NH3]=[NO]=1000ppm, [O2]=6%, [SO2]=300ppm, [H2O]=10%, N2For balance
Gas, reaction velocity 30,000h-1, reaction temperature 300oC.Test result indicates that：It is being passed through SO2And H2After O 10h, NOx's
Conversion ratio is declined slightly 3 ~ 9%, remains within more than 90%, the kept stable in the 48h that experiment is investigated, works as SO2And H2O
Catalytic activity substantially returns to 95% NO after removalxConversion ratio.
Claims (2)
1. the preparation method of the slag based denitration catalyst of a kind of modification, it is characterised in that be achieved by the steps of：
Pretreatment of slag：By raw material slag crushing grinding, the slag for screening out 40 ~ 60 mesh is dissolved in the nitre that mass concentration is 2 ~ 3wt%
In acid solution, 12-24h is handled under 250 ~ 350r/min stirring condition, then filtered, washing, and in 105 ~ 130 DEG C of bars
Dry 10 ~ 14h under part, the slag after being activated, wherein, the mass volume ratio of slag and salpeter solution is 0.5 ~ 1.0g/mL；
Slag is modified：At ambient temperature, sucrose is completely dissolved in deionized water, then adds step thereto（1）Gained
Activation after slag, and stir 10min and obtain mixture A；Then mixture A is transferred in hydrothermal reaction kettle in 180 ~
220 DEG C of 2 ~ 4h of processing, obtain mixture B；Mixture B is filtered, and after washing 2 ~ 4 times with absolute ethyl alcohol, is placed in 110 DEG C of bar
Drying process 6h under part, 4h is calcined under 500 DEG C of nitrogen atmosphere, obtains being covered with the modified steel scoria of carbosphere coating；Wherein,
Sucrose and the mass volume ratio of deionized water are 0.5g/mL, and the weight ratio of slag and sucrose is 1:1；
Active component loads：By WO3Presoma and oxalic acid are dissolved in deionized water, are stirred at room temperature to being completely dissolved；Then plus
Enter cerium salt and molysite continues to stir 30min, add step（2）The modified steel scoria of middle gained, obtains mixture C；By mixture C
It is placed in 60 ~ 80 DEG C of water-bath and carries out slow evaporation under agitation, until the moisture on its surface disappears, it is subsequently placed in 105 ~
10 ~ 14h of drying process under the conditions of 130 DEG C, and then be transferred in high-temperature heater, in N2In 500 DEG C of continuation under the atmosphere of protection
5h is handled, obtains catalyst；Wherein, WO3Presoma is ammonium tungstate or ammonium paratungstate；Cerium salt is cerous sulfate or Cericammoniumsulfate；Iron
Salt is ferric sulfate or iron ammonium sulfate；nw:nFe:nCeElemental mole ratios be 1：（0.5~5）：（0.5~5）, WO3The weight of presoma
The weight ratio of amount and modified steel scoria is 3% ~ 10%.
2. the preparation method for the slag based denitration catalyst being modified as claimed in claim 1, it is characterised in that：Step（1）In
Raw material slag using planetary mills crushing grinding, the concentration of salpeter solution is 3wt%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550495A (en) * | 2018-11-15 | 2019-04-02 | 西安科技大学 | W adulterates CeO2The preparation method of the novel steel slag based cementitious material of different loads amount |
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| CN103801192A (en) * | 2014-02-21 | 2014-05-21 | 陕西理工学院 | Flue gas denitrification process for cement kiln |
| CN105478133A (en) * | 2015-12-11 | 2016-04-13 | 福建工程学院 | Low-cost SCR denitration catalyst and preparation method thereof |
| CN105478161A (en) * | 2015-12-11 | 2016-04-13 | 福建工程学院 | Selective catalytic reduction(SCR)denitration catalyst based on titanium slag and preparation method thereof |
| CN105618069A (en) * | 2014-11-03 | 2016-06-01 | 中国石油化工股份有限公司 | High-activity flue gas desulfurization catalyst and preparation method thereof |
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2017
- 2017-10-23 CN CN201710995475.2A patent/CN107469847A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103301863A (en) * | 2013-07-05 | 2013-09-18 | 上海交通大学 | Steel-slag-based selective catalytic reduction (SCR) denitration catalyst and preparation method thereof |
| CN103801192A (en) * | 2014-02-21 | 2014-05-21 | 陕西理工学院 | Flue gas denitrification process for cement kiln |
| CN105618069A (en) * | 2014-11-03 | 2016-06-01 | 中国石油化工股份有限公司 | High-activity flue gas desulfurization catalyst and preparation method thereof |
| CN105478133A (en) * | 2015-12-11 | 2016-04-13 | 福建工程学院 | Low-cost SCR denitration catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109550495A (en) * | 2018-11-15 | 2019-04-02 | 西安科技大学 | W adulterates CeO2The preparation method of the novel steel slag based cementitious material of different loads amount |
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Effective date of registration: 20200805 Address after: Room 0, Office Building of Anhui Jinsenyuan Environmental Protection Engineering Co., Ltd., 28 Xingye Road, Xinhua Street Office, Yingdong District, Fuyang City, Anhui Province Applicant after: ANHUI JINSENYUAN ENVIRONMENTAL ENGINEERING Co.,Ltd. Address before: No. 684, information new material industrial park, Dongba Town, Gaochun District, Nanjing City, Jiangsu Province Applicant before: Zhang Junjie |
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Effective date of abandoning: 20201002 |
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