CN111841532B - Preparation method of ethanol-SCR catalyst - Google Patents
Preparation method of ethanol-SCR catalyst Download PDFInfo
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- CN111841532B CN111841532B CN201910348965.2A CN201910348965A CN111841532B CN 111841532 B CN111841532 B CN 111841532B CN 201910348965 A CN201910348965 A CN 201910348965A CN 111841532 B CN111841532 B CN 111841532B
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
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Abstract
The invention discloses a preparation method of an ethanol-SCR catalyst. The method comprises the following steps: placing the honeycomb ceramic matrix into an alumina coating precursor for dip coating, removing residual liquid on the surface of the matrix and in the pore channels, drying and roasting; repeating the above process; then carrying out hydrothermal treatment by using ammonium bicarbonate aqueous solution under a closed condition, removing residual liquid, drying and roasting; and loading active metal silver to obtain the ethanol-SCR catalyst. The active components on the catalyst prepared by the method can be better anchored with the coating carrier, and meanwhile, the surface of the coating has a certain number of stacking pore channels, so that the influence of fly ash in flue gas and carbon deposition of the catalyst in the reaction process can be reduced to a certain extent. The catalyst prepared by the method is particularly suitable for a selective catalytic reduction process with ethanol as a reducing agent.
Description
Technical Field
The invention belongs to the technical field of nitrogen oxide removal, and particularly relates to a preparation method of an ethanol-SCR catalyst.
Background
SCR (Selective Catalytic Reduction) -selective catalytic reduction is the most widely used flue gas denitration technology in the world at present, and has the advantages of high removal efficiency, simple device structure, reliable operation, convenient maintenance and the like. The method mainly uses ammonia as a reducing agent, but NH is generated due to incomplete reaction of ammonia in the flue gas denitration process 3 Ammonia slip occurs during SCR denitration; meanwhile, the active component of the SCR catalyst can also enable part of SO in the flue gas 2 Oxidation to form SO 3 SO generated by the reaction 3 Further reacts with escaped ammonia in the flue gas to generate ammonium bisulfate, which is a substance with strong viscosity. At normal operating temperatures, the dew point of ammonium bisulfate is 147 ℃, which accumulates as a liquid on the surface of objects or as dropletsThe fly ash is adhered to the flue gas after the form is dispersed in the flue gas, and the corrosion of downstream equipment such as an air preheater and the like can be caused after water is absorbed from the flue gas; if it forms on a low temperature catalyst, it can cause partial fouling and plugging of the catalyst, increase catalyst pressure drop or cause catalyst failure. In addition, the escaped ammonia also causes pollution to the environment and harm to the health and safety of human bodies.
In order to solve the problem, a new idea of converting the reducing agent, namely HC-SCR denitration technology, is provided, and the research so far shows that: NH removal 3 In addition, hydrocarbons (HC) such as methane, propylene, ethanol, propanol, and the like can also selectively reduce NOx. The hydrocarbon replaces ammonia as a reducing agent, so that the influence of escaped ammonia on the reactor can be effectively avoided, the service life of the catalyst is prolonged, and the stable operation of the denitration device is protected. HC-SCR catalyst is generally Ag/Al 2 O 3 、Cu/Al 2 O 3 And many studies have been conducted. With NH 3 Catalysts for SCR like those for HC-SCR, alumina in HC-SCR catalysts is generally applied as a coating to the surface of a ceramic honeycomb substrate, where the mode of action of the active metal with Al on the surface of the coating is widely recognized as an important factor affecting catalyst activity and NOx removal. Meanwhile, fly ash in the flue gas and carbon deposition of the catalyst also put higher requirements on the coating pore channels, and the service life of the catalyst can be prolonged by a certain number of macropores.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of an ethanol-SCR catalyst. The active components on the catalyst prepared by the method can be better anchored with the coating carrier, and meanwhile, the surface of the coating has a certain number of stacking pore channels, so that the influence of fly ash in flue gas and carbon deposition of the catalyst in the reaction process can be reduced to a certain extent.
The preparation method of the ethanol-SCR catalyst comprises the following steps:
(1) Putting the honeycomb ceramic matrix into an alumina coating precursor for dip coating, removing residual liquid on the surface of the matrix and in the pore channels, drying and roasting; then repeating the above process;
(2) Putting the material obtained in the step (1) into a pressure-resistant container filled with ammonium bicarbonate aqueous solution, performing hydrothermal treatment under a closed condition, removing residual liquid, drying and roasting to obtain a honeycomb ceramic matrix carrying a coating;
(3) And (3) loading active metallic silver on the honeycomb ceramic matrix with the loaded coating obtained in the step (2) to obtain the ethanol-SCR catalyst.
In the method of the present invention, the honeycomb ceramic matrix material in the step (1) may be a conventional ceramic material, such as cordierite. The size of the honeycomb ceramic matrix is generally prepared as desired. The honeycomb ceramic matrix may be pretreated, for example, by removing surface powder with compressed air, or may be treated by conventional treatment methods such as hydrothermal treatment, acid treatment or alkali treatment, in order to further improve the surface properties of the matrix.
In the process of the present invention, the alumina coating precursor of step (1) is an alumina sol and can be prepared according to methods well known in the art. Further, the solid content of the aluminum sol is 20% -40% by mass.
In the method of the present invention, the number of times of repeated dip coating of the alumina coating precursor in the step (1) is generally at least 1 time, further 1 to 5 times, and still further 1 to 3 times.
In the method of the invention, the total amount of the alumina coating precursor in the step (1) is such that the alumina coating loaded on the honeycomb ceramic substrate accounts for 8% -30%, preferably 8% -22% of the mass of the honeycomb ceramic substrate in the step (1) in terms of alumina. The total amount of the alumina coating precursor of step (1) refers to the total amount of the alumina coating precursor used until the end of the dip-coating of the alumina coating precursor of step (1).
In the method of the invention, the dipping treatment in the step (1) is generally carried out at room temperature, and compressed air is adopted to remove residual liquid on the surface of the substrate and in the pore canal after dipping.
In the method of the invention, after each impregnation of the alumina coating precursor in step (1), drying and roasting are required, wherein the drying temperature is 100-120 ℃ and the drying time is 2-6 hours. The roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours; calcination is in an oxygen-containing atmosphere, preferably air.
In the method, in the step (2), when the material obtained in the step (1) is subjected to hydrothermal treatment by adopting an ammonium bicarbonate aqueous solution, the mass concentration of the ammonium bicarbonate aqueous solution is 12% -20%, preferably 14% -18%, the dosage of the ammonium bicarbonate aqueous solution at least needs to be less than that of the material obtained in the step (1), and the mass ratio of the material obtained in the general step (1) to the ammonium bicarbonate aqueous solution is 1: 3.5-10.
In the method of the invention, the hydrothermal treatment conditions in the step (2) are as follows: the temperature is 120-160 ℃, preferably 120-150 ℃, and the time is 4-20 hours, preferably 5-10 hours.
In the method, the drying temperature in the step (2) is 100-120 ℃ and the drying time is 2-6 hours. The roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours; calcination is in an oxygen-containing atmosphere, preferably air.
In the method of the present invention, the active metallic silver loading mode in step (3) adopts an impregnation process, such as an over-volume impregnation, an equal-volume impregnation or a spray impregnation, and the like, and the over-volume impregnation is preferred. The impregnating solution is silver-containing soluble saline solution, such as nitrate water solution, silver acetate water solution, silver chloride water solution, etc.; the specific concentration of the impregnation fluid may depend on the active metal content on the final catalyst. After impregnating and loading active metallic silver, drying and roasting to obtain the ethanol-SCR catalyst, wherein the drying temperature is 100-120 ℃ and the drying time is 2-6 hours. The roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours; calcination is in an oxygen-containing atmosphere, preferably air. The loading of the active metal silver in the step (3) accounts for 0.2% -4.0% of the mass of the obtained ethanol-SCR catalyst, and is preferably 0.5% -2.0%.
The catalyst prepared by the method can be used in flue gas denitration technology, and is particularly suitable for selective catalytic reduction technology with ethanol as a reducing agent. When ethanol is used as a reducing agent for flue gas denitration, the operation conditions are as follows: the reaction temperature is 230-260 ℃, ethanol (gas)/NO x =3 to 8:1 (molar ratio), and the space velocity of the flue gas is 2000-12000 h -1 。
According to the prior art, enol-type species (rch=ch-O-) and NO 3 The species is a main reaction intermediate, the mutual reaction performance of the two is very strong, isocyanate (-NCO) surface adsorption species which are key reaction intermediates can be generated, so that the removal rate of NOx is very high, the reducing agent quality standard which takes the formation of high-activity enol type species as a criterion is provided, and the oxidized Ag and the contact boundary of the oxidized Ag and a carrier are active centers formed by the surface enol type species. According to the invention, the alumina coating is coated by dipping for multiple times and combined with ammonium bicarbonate hydrothermal treatment, the columnar alumina is covered on the surface of the alumina coating on the honeycomb ceramic matrix, so that the contact boundary between the oxidized Ag and the carrier is greatly increased, and enol-type species are more easily formed; meanwhile, the columnar alumina exposes more (110) and (100) crystal faces, so that the anchoring effect of active metal silver and Al is further improved, the active site of the catalyst is greatly increased, the surface adsorption of key intermediate isocyanate (-NCO) is facilitated, and a higher NOx conversion rate can be obtained at a lower reaction temperature; meanwhile, the surface structure forms a certain number of stacking pore channels, so that the fly ash and carbon deposition resistance of the catalyst is improved, and the flue gas working condition with large dust content can be dealt with.
Drawings
FIG. 1 is a scanning electron microscope image of the cut surface of the coated honeycomb ceramic substrate obtained in step (2) of example 1.
Detailed Description
The technical scheme of the invention is described in more detail by specific examples.
The microstructure of the carrier is characterized by applying a scanning electron microscope, and the specific operation is as follows: the JSM-7500F scanning electron microscope is adopted to characterize the microstructure of the carrier, the accelerating voltage is 5KV, the accelerating current is 20 mu A, and the working distance is 8mm.
The cordierite honeycomb ceramic substrates used in the examples and comparative examples of the present invention were cubes of 4.5X4.5X5 cm in size. The honeycomb ceramic matrix is freed from surface powder by compressed air prior to use.
Example 1
The catalyst A was prepared in this example as follows:
(1) Putting the honeycomb ceramic matrix into aluminum sol (solid content is 30wt%) for dip coating, then blowing out residual sol on the surface of the matrix and in the pore canal by compressed air, drying at 110 ℃ for 3h, and roasting at 600 ℃ for 3h; repeating the above process for 2 times; the aluminum oxide coating coated on the honeycomb ceramic matrix accounts for 14% of the mass of the honeycomb ceramic matrix in terms of aluminum oxide;
(2) Putting the material obtained in the step (1) into a pressure-resistant container filled with ammonium bicarbonate aqueous solution (the mass concentration is 17%), performing hydrothermal treatment at 130 ℃ for 8 hours under a closed condition, removing residual liquid, drying at 110 ℃ for 6 hours, and roasting at 500 ℃ for 4 hours to obtain a honeycomb ceramic matrix carrying a coating; wherein the mass ratio of the material obtained in the step (1) to the ammonium bicarbonate aqueous solution is 5:21, a step of;
(3) Preparing a silver nitrate solution by taking silver nitrate as a precursor, immersing the material obtained in the step (2) into the silver nitrate solution for impregnation loading, drying at 110 ℃ for 3h, and roasting at 600 ℃ for 3h to obtain a catalyst A, wherein the silver content in the catalyst A is 1.2wt%.
As can be seen from FIG. 1, after the closed hydrothermal treatment of the ammonium bicarbonate aqueous solution in the step (2), the surface of the obtained honeycomb ceramic matrix carrying the coating is obviously covered with columnar alumina, so that a certain number of stacking pore channels are formed on the surface.
Example 2
Catalyst B was prepared in this example by the following procedure:
(1) The procedure is as in example 1; the aluminum oxide coating coated on the honeycomb ceramic matrix accounts for 18% of the mass of the honeycomb ceramic matrix in terms of aluminum oxide;
(2) Putting the material obtained in the step (1) into a pressure-resistant container filled with ammonium bicarbonate aqueous solution (the mass concentration is 14%), carrying out hydrothermal treatment at 145 ℃ for 6 hours under a closed condition, removing residual liquid, drying at 110 ℃ for 4 hours, and roasting at 500 ℃ for 4 hours to obtain a honeycomb ceramic matrix carrying a coating; wherein the mass ratio of the material obtained in the step (1) to the ammonium bicarbonate aqueous solution is 5:21, a step of;
(3) The procedure is as in example 1 to give catalyst B, wherein the silver content of catalyst B is 1.0% by weight.
Example 3
Catalyst C was prepared in this example as follows:
(1) The procedure is as in example 1; the difference is that: repeating the alumina sol dip coating process for 1 time; the aluminum oxide coating coated on the honeycomb ceramic matrix accounts for 10% of the mass of the honeycomb ceramic matrix in terms of aluminum oxide;
(2) Putting the material obtained in the step (1) into a pressure-resistant container filled with ammonium bicarbonate aqueous solution (the mass concentration is 14%), performing hydrothermal treatment at 140 ℃ for 7 hours under a closed condition, removing residual liquid, drying at 110 ℃ for 3 hours, and roasting at 500 ℃ for 4 hours to obtain a honeycomb ceramic matrix carrying a coating; wherein the mass ratio of the material obtained in the step (1) to the ammonium bicarbonate aqueous solution is 1:6, preparing a base material;
(3) The procedure is as in example 1 to give catalyst C, wherein the silver content of catalyst C is 0.8% by weight.
Comparative example 1
Catalyst D was obtained as in example 3, except that step (2) was absent, wherein the silver content of catalyst D was 0.8wt%. Wherein, the surface of the honeycomb ceramic matrix which is not subjected to closed hydrothermal treatment by ammonium bicarbonate aqueous solution is free of columnar alumina.
Comparative example 2
The same procedure as in example 3 was followed except that the dip coating process of step (1) was conducted only once, and the total amount of the alumina coating precursor was 5% by mass of the honeycomb ceramic matrix in terms of alumina to obtain catalyst E. Wherein the silver content of the catalyst is 0.8wt%
Example 4
This example is an evaluation experiment.
The activity of the catalyst denitration catalysts a to E of examples 1 to 3 and comparative examples 1 to 2 were evaluated, respectively, and a laboratory microreaction device was used to simulate the smoke composition: n (N) 2 To balance the qi, NO x At a concentration of 800ppm (V), O 2 Ethanol as reducing agent, ethanol (gaseous)/NO x =5: 1 (molar ratio), the space velocity of the flue gas is 5000h -1 At a reaction temperature of 250 DEG CThe long-period operation results are shown in Table 1.
TABLE 1 run test results
| Catalyst numbering | A | B | C | D | E |
| Denitration rate,% (operation 1 h) | 95.0 | 93.4 | 91.5 | 81.6 | 84.8 |
| Denitration rate,% (running 500 h) | 94.8 | 93.3 | 91.4 | 78.4 | 81.9 |
Claims (20)
1. A method of preparing an ethanol-SCR catalyst, comprising:
(1) Putting the honeycomb ceramic matrix into an alumina coating precursor for dip coating, removing residual liquid on the surface of the matrix and in the pore channels, drying and roasting; then repeating the above process;
(2) Putting the material obtained in the step (1) into a pressure-resistant container filled with ammonium bicarbonate aqueous solution, performing hydrothermal treatment under a closed condition, removing residual liquid, drying and roasting to obtain a honeycomb ceramic matrix carrying a coating;
(3) And (3) loading active metallic silver on the honeycomb ceramic matrix with the loaded coating obtained in the step (2) to obtain the ethanol-SCR catalyst.
2. A method according to claim 1, characterized in that: the honeycomb ceramic matrix in the step (1) is made of cordierite.
3. A method according to claim 1, characterized in that: the alumina coating precursor in the step (1) is aluminum sol, and the solid content of the aluminum sol is 20% -40% by mass.
4. A method according to claim 1, characterized in that: the step (1) of dip coating the alumina coating precursor is repeated at least 1 time.
5. The method of claim 4, wherein: and (3) repeating the step (1) for 1-5 times of dip coating the alumina coating precursor.
6. A method according to claim 1, characterized in that: the total usage of the alumina coating precursor in the step (1) is that the alumina coating on the honeycomb ceramic matrix accounts for 8% -30% of the mass of the honeycomb ceramic matrix in the step (1) in terms of alumina.
7. The method of claim 6, wherein: the total usage of the alumina coating precursor in the step (1) is that the alumina coating on the honeycomb ceramic matrix accounts for 8% -22% of the mass of the honeycomb ceramic matrix in the step (1) in terms of alumina.
8. A method according to claim 1, characterized in that: drying and roasting are needed after the alumina coating precursor is impregnated in the step (1) each time, wherein the drying temperature is 100-120 ℃ and the drying time is 2-6 hours; the roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours; roasting in an oxygen-containing atmosphere.
9. The method according to claim 8, wherein: the oxygen-containing atmosphere is air.
10. A method according to claim 1, characterized in that: in the step (2), when the material obtained in the step (1) is subjected to hydrothermal treatment by adopting an ammonium bicarbonate aqueous solution, the mass concentration of the ammonium bicarbonate aqueous solution is 12% -20%, and the mass ratio of the material obtained in the step (1) to the ammonium bicarbonate aqueous solution is 1: 3.5-10.
11. The method of claim 10, wherein: the mass concentration of the ammonium bicarbonate aqueous solution is 14% -18%.
12. A method according to claim 1, characterized in that: the hydrothermal treatment conditions in the step (2) are as follows: the temperature is 120-160 ℃ and the time is 4-20 hours.
13. The method of claim 12, wherein: the hydrothermal treatment conditions in the step (2) are as follows: the temperature is 120-150 ℃ and the time is 5-10 hours.
14. A method according to claim 1, characterized in that: the drying temperature in the step (2) is 100-120 ℃, the drying time is 2-6 hours, the roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours; roasting in an oxygen-containing atmosphere.
15. The method of claim 14, wherein: the oxygen-containing atmosphere is air.
16. A method according to claim 1, characterized in that: and (3) adopting an impregnation process in the active metal silver loading mode.
17. The method of claim 16, wherein: and (3) carrying out over-volume impregnation on the active metal silver in the loading mode.
18. The method of claim 16, wherein: after the active metal silver is impregnated and loaded, drying and roasting are carried out to obtain the ethanol-SCR catalyst, wherein the drying temperature is 100-120 ℃, the drying time is 2-6 hours, the roasting temperature is 450-650 ℃, and the roasting time is 2-6 hours.
19. A method according to claim 1, characterized in that: the loading amount of the active metal silver in the step (3) accounts for 0.2% -4.0% of the mass of the obtained ethanol-SCR catalyst.
20. The method of claim 19, wherein: the loading amount of the active metal silver in the step (3) accounts for 0.5% -2.0% of the mass of the obtained ethanol-SCR catalyst.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10244155A (en) * | 1997-03-03 | 1998-09-14 | Sekiyu Sangyo Kasseika Center | Catalyst for catalytic reduction of nox |
| CN101554581A (en) * | 2009-05-14 | 2009-10-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Denitrifying catalyst with selective catalytic reduction and a preparation method |
| CN103785396A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of hydrodemetalization catalyst for heavy oil |
| CN108067218A (en) * | 2016-11-15 | 2018-05-25 | 中国石油化工股份有限公司 | The preparation method of denitrating catalyst |
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- 2019-04-28 CN CN201910348965.2A patent/CN111841532B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10244155A (en) * | 1997-03-03 | 1998-09-14 | Sekiyu Sangyo Kasseika Center | Catalyst for catalytic reduction of nox |
| CN101554581A (en) * | 2009-05-14 | 2009-10-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Denitrifying catalyst with selective catalytic reduction and a preparation method |
| CN103785396A (en) * | 2012-11-01 | 2014-05-14 | 中国石油化工股份有限公司 | Preparation method of hydrodemetalization catalyst for heavy oil |
| CN108067218A (en) * | 2016-11-15 | 2018-05-25 | 中国石油化工股份有限公司 | The preparation method of denitrating catalyst |
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Effective date of registration: 20231225 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |