CN114984948A - Preparation method of efficient economical low-temperature catalyst - Google Patents
Preparation method of efficient economical low-temperature catalyst Download PDFInfo
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- CN114984948A CN114984948A CN202210627898.XA CN202210627898A CN114984948A CN 114984948 A CN114984948 A CN 114984948A CN 202210627898 A CN202210627898 A CN 202210627898A CN 114984948 A CN114984948 A CN 114984948A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a preparation method of a high-efficiency economical low-temperature catalyst, which adopts the technical scheme that: the method comprises the following specific steps: s1, preparing a first solution; s2, preparing a second solution; s3, gel: adding TiO2, Mn and Ce into the acid burette, pouring the second solution into the acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, and standing until gel is formed; s4, drying; s5, grinding; s6, dipping; s7, drying; s8, grinding; s9, flue gas simulation, and the preparation method of the high-efficiency economical low-temperature catalyst has the beneficial effects that: the low-temperature catalyst is prepared by adopting a method combining gel and impregnation, the low-temperature activity of the catalyst is high, the service life of the catalyst is long, the requirement on the purity of chemical materials is low, the cost is low, the preparation efficiency is high, the NO conversion rate is high, the flow is clear, the preparation method is simple, the operation is safe, and the denitration performance is obvious.
Description
Technical Field
The invention relates to the technical field of preparation methods of low-temperature catalysts, in particular to a preparation method of an efficient and economical low-temperature catalyst.
Background
At present, almost all coke oven flue gas in China can not achieve standard emission of NO, a mature technology adopted in the world is to remove NO in the coke oven flue gas by an ammonia selective catalytic reduction method, and the development of mature high-efficiency low-temperature SCR denitration catalytic materials is necessary from the aspects of saving energy consumption and reducing original equipment as much as possible.
The existing catalyst has low activity, short service life, higher requirement on the purity of chemical materials, high cost, batch addition of various raw materials, difficulty in controlling a mixing process and low NO conversion rate.
Disclosure of Invention
Therefore, the invention provides a preparation method of an efficient and economical low-temperature catalyst, which aims to solve the problems of low activity of the catalyst, short service life of the catalyst, higher requirement on purity of chemical materials, high cost, batch addition of various raw materials, difficulty in controlling a mixing process and low NO conversion rate.
In order to achieve the above purpose, the invention provides the following technical scheme: a preparation method of a high-efficiency economical low-temperature catalyst comprises the following specific steps:
s1, preparation of a first solution: placing a small amount of butyl phthalate and 100mL of absolute ethyl alcohol in a beaker, adding glacial acetic acid to obtain a first solution, and placing the first solution on a magnetic stirrer for stirring until the first solution is uniformly mixed;
s2, preparing a second solution: pouring 45mL of absolute ethyl alcohol and a small amount of distilled water into the other beaker, stirring the mixture by using a stirring rod until the mixture is uniformly mixed to obtain a second solution, and dripping a small amount of concentrated nitric acid into the mixed second solution to adjust the pH value of the second solution so that the pH value of the second solution reaches 1-2;
s3, gel: adding TiO2, Mn and Ce into the acid burette, pouring the second solution into the acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, and standing until gel is formed;
s4, drying and adjusting the temperature of the oven, putting the gel liquid into the oven for drying, and after drying, putting the gel liquid into a muffle furnace for roasting to obtain catalyst carrier particles;
s5, grinding: grinding the obtained catalyst particles in a grinder into powder;
s6, dipping: putting 50% manganese nitrate solution and 40% cerous nitrate hexahydrate crystal into a beaker, dissolving the mixture in distilled water, mixing uniformly, soaking a certain amount of TiO2, Mn and Ce powder in the mixture to obtain a third solution, and putting catalyst carrier particles in S4 into the third solution for soaking together;
s7, drying: putting the third solution into an oven for drying, and after drying, putting the third solution into a muffle furnace for roasting to obtain new catalyst carrier particles;
s8, grinding: and (3) putting the obtained new catalyst carrier particles into a grinder for grinding and screening, and selecting the catalyst with 20-40 meshes for later use.
S9, flue gas simulation: the concentration of each component in the flue gas is detected by a flue gas analyzer, a catalyst is filled in the flue gas analyzer, and the inlet concentration and the outlet concentration of NO in the flue gas are detected and analyzed.
Preferably, in step S1, the amount of glacial acetic acid added is controlled to be 15-25 ml.
Preferably, in the step S2, the amount of the concentrated nitric acid to be added is controlled to be 4 to 8 ml.
Preferably, in the step S3, the rotation speed of the electric stirring rod is controlled to be 200 r/min.
Preferably, in the step S4, the oven temperature is controlled at 105 ℃, the drying time is controlled at 8-10h, the muffle temperature is controlled at 500 ℃, and the roasting time is controlled at 4-5 h.
Preferably, in the step S5, the grinding time is controlled to be 5-10 min.
Preferably, in the step S6, the dipping time is controlled to be 3-4 h.
Preferably, in the step S7, the oven temperature is controlled at 105 ℃, the drying time is controlled at 8-10h, the muffle temperature is controlled at 500 ℃, and the roasting time is controlled at 4-5 h.
Preferably, in the step S8, the grinding time is controlled to be 6-10 min.
The embodiment of the invention has the following advantages:
the low-temperature catalyst is prepared by adopting a method combining gel and impregnation, the low-temperature activity of the catalyst is high, the service life of the catalyst is long, the requirement on the purity of chemical materials is low, the cost is low, the preparation efficiency is high, the NO conversion rate is high, the flow is clear, the preparation method is simple, the operation is safe, and the denitration performance is obvious.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a preparation method of an efficient and economical low-temperature catalyst, which comprises the following specific steps:
s1, preparation of a first solution: placing a small amount of butyl phthalate and 100mL of absolute ethyl alcohol in a beaker, adding glacial acetic acid to obtain a first solution, placing the first solution on a magnetic stirrer, and stirring until the first solution is uniformly mixed, wherein the adding amount of the glacial acetic acid is controlled to be 15-25 mL;
s2, preparing a second solution: pouring 45mL of absolute ethyl alcohol and a small amount of distilled water into another beaker, stirring by a stirring rod until the absolute ethyl alcohol and the distilled water are uniformly mixed to obtain a second solution, and dripping a small amount of concentrated nitric acid into the mixed second solution to adjust the pH value of the second solution so as to enable the pH value of the second solution to reach 1-2, wherein the adding amount of the concentrated nitric acid is controlled to be 4-8 mL;
s3, gel: adding TiO2, Mn and Ce into the acid burette, pouring the second solution into the acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, standing until gel is formed, and controlling the rotating speed of the electric stirring rod at 200 r/min;
s4, drying and adjusting the temperature of the oven, putting the gel liquid into the oven for drying, putting the gel liquid into a muffle furnace for roasting after drying, and obtaining catalyst carrier particles, wherein the temperature of the oven is controlled at 105 ℃, the drying time is controlled at 8 hours, the temperature of the muffle furnace is controlled at 500 ℃, and the roasting time is controlled at 4 hours;
s5, grinding: grinding the obtained catalyst particles in a grinder for 5-10min to obtain powder;
s6, dipping: putting a 50% manganese nitrate solution and a 40% cerium nitrate hexahydrate crystal into a beaker, dissolving the solution in distilled water, mixing uniformly, soaking a certain amount of TiO2, Mn and Ce powder in the mixture to obtain a third solution, and soaking catalyst carrier particles in S4 in the third solution for 3 hours;
s7, drying: drying the third solution in an oven, and roasting in a muffle furnace to obtain new catalyst carrier particles, wherein the oven temperature is controlled at 105 ℃, the drying time is controlled at 8 hours, the muffle furnace temperature is controlled at 500 ℃, and the roasting time is controlled at 4 hours;
s8, grinding: and (3) putting the obtained new catalyst carrier particles into a grinder for grinding and screening, selecting a 20-40-mesh catalyst for later use, and controlling the grinding time to be 6-10 min.
S9, flue gas simulation: the concentration of each component in the flue gas is detected by a flue gas analyzer, a catalyst is filled in the flue gas analyzer, and the inlet concentration and the outlet concentration of NO in the flue gas are detected and analyzed.
Example 2:
the invention provides a preparation method of an efficient and economical low-temperature catalyst, which comprises the following specific steps:
s1, preparation of a first solution: placing a small amount of butyl phthalate and 100mL of absolute ethyl alcohol in a beaker, adding glacial acetic acid to obtain a first solution, placing the first solution on a magnetic stirrer, and stirring until the first solution is uniformly mixed, wherein the addition amount of the glacial acetic acid is controlled to be 15-25 mL;
s2, preparing a second solution: pouring 45mL of absolute ethyl alcohol and a small amount of distilled water into another beaker, stirring by a stirring rod until the absolute ethyl alcohol and the distilled water are uniformly mixed to obtain a second solution, and dripping a small amount of concentrated nitric acid into the mixed second solution to adjust the pH value of the second solution so as to enable the pH value of the second solution to reach 1-2, wherein the adding amount of the concentrated nitric acid is controlled to be 4-8 mL;
s3, gel: adding TiO2, Mn and Ce into the acid burette, pouring the second solution into the acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, standing until gel is formed, and controlling the rotating speed of the electric stirring rod at 200 r/min;
s4, drying and adjusting the temperature of the oven, putting the gel liquid into the oven for drying, putting the gel liquid into a muffle furnace for roasting after drying is finished, and obtaining catalyst carrier particles, wherein the temperature of the oven is controlled at 105 ℃, the drying time is controlled at 9 hours, the temperature of the muffle furnace is controlled at 500 ℃, and the roasting time is controlled at 4.5 hours;
s5, grinding: grinding the obtained catalyst particles in a grinder for 5-10min to obtain powder;
s6, dipping: putting a 50% manganese nitrate solution and a 40% cerium nitrate hexahydrate crystal into a beaker, dissolving the solution in distilled water, mixing uniformly, soaking a certain amount of TiO2, Mn and Ce powder in the mixture to obtain a third solution, and soaking catalyst carrier particles in S4 in the third solution for 3.5 hours;
s7, drying: drying the third solution in an oven, and roasting in a muffle furnace to obtain new catalyst carrier particles, wherein the oven temperature is controlled at 105 ℃, the drying time is controlled at 9 hours, the muffle furnace temperature is controlled at 500 ℃, and the roasting time is controlled at 4.5 hours;
s8, grinding: and (3) putting the obtained new catalyst carrier particles into a grinder for grinding and screening, selecting a 20-40-mesh catalyst for later use, and controlling the grinding time to be 6-10 min.
S9, flue gas simulation: the concentration of each component in the flue gas is detected by a flue gas analyzer, a catalyst is filled in the flue gas analyzer, and the inlet concentration and the outlet concentration of NO in the flue gas are detected and analyzed.
Example 3:
the invention provides a preparation method of an efficient and economical low-temperature catalyst, which comprises the following specific steps:
s1, preparation of a first solution: placing a small amount of butyl phthalate and 100mL of absolute ethyl alcohol in a beaker, adding glacial acetic acid to obtain a first solution, placing the first solution on a magnetic stirrer, and stirring until the first solution is uniformly mixed, wherein the adding amount of the glacial acetic acid is controlled to be 15-25 mL;
s2, preparing a second solution: pouring 45mL of absolute ethyl alcohol and a small amount of distilled water into another beaker, stirring by a stirring rod until the absolute ethyl alcohol and the distilled water are uniformly mixed to obtain a second solution, and dripping a small amount of concentrated nitric acid into the mixed second solution to adjust the pH value of the second solution so as to enable the pH value of the second solution to reach 1-2, wherein the adding amount of the concentrated nitric acid is controlled to be 4-8 mL;
s3, gel: adding TiO2, Mn and Ce into an acid burette, pouring the second solution into the acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, standing until gel is formed, and controlling the rotating speed of the electric stirring rod at 200 r/min;
s4, drying and adjusting the temperature of the oven, putting the gel liquid into the oven for drying, putting the gel liquid into a muffle furnace for roasting after drying, and obtaining catalyst carrier particles, wherein the temperature of the oven is controlled at 105 ℃, the drying time is controlled at 10 hours, the temperature of the muffle furnace is controlled at 500 ℃, and the roasting time is controlled at 5 hours;
s5, grinding: grinding the obtained catalyst particles in a grinder for 5-10min to obtain powder;
s6, dipping: putting a 50% manganese nitrate solution and a 40% cerium nitrate hexahydrate crystal into a beaker, dissolving the solution in distilled water, mixing uniformly, soaking a certain amount of TiO2, Mn and Ce powder in the mixture to obtain a third solution, and soaking catalyst carrier particles in S4 in the third solution for 4 hours;
s7, drying: drying the third solution in an oven, and roasting in a muffle furnace to obtain new catalyst carrier particles, wherein the oven temperature is controlled at 105 ℃, the drying time is controlled at 10 hours, the muffle furnace temperature is controlled at 500 ℃, and the roasting time is controlled at 5 hours;
s8, grinding: and (3) putting the obtained new catalyst carrier particles into a grinder for grinding and screening, selecting a 20-40-mesh catalyst for later use, and controlling the grinding time to be 6-10 min.
S9, flue gas simulation: the concentration of each component in the flue gas is detected by a flue gas analyzer, a catalyst is filled in the flue gas analyzer, and the inlet concentration and the outlet concentration of NO in the flue gas are detected and analyzed.
The denitration rates of the high-efficiency economical low-temperature catalyst prepared by the methods of the above examples 1 to 3 at different temperatures were compared as follows:
from the above, the efficient and economical low-temperature catalyst prepared in example 3 has high activity, long service life, high denitration rate and low cost.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the present invention or modify it to an equivalent technical solution by using the technical solution described above. Therefore, any simple modifications or equivalent replacements made according to the technical solution of the present invention belong to the protection scope of the present invention.
Claims (9)
1. A preparation method of a high-efficiency economical low-temperature catalyst is characterized by comprising the following steps: the method comprises the following specific steps:
s1, preparation of a first solution: placing a small amount of butyl phthalate and 100mL of absolute ethyl alcohol in a beaker, adding glacial acetic acid to obtain a first solution, and placing the first solution on a magnetic stirrer for stirring until the first solution is uniformly mixed;
s2, preparing a second solution: pouring 45mL of absolute ethyl alcohol and a small amount of distilled water into the other beaker, stirring the mixture by using a stirring rod until the mixture is uniformly mixed to obtain a second solution, and dripping a small amount of concentrated nitric acid into the mixed second solution to adjust the pH value of the second solution so that the pH value of the second solution reaches 1-2;
s3, gel: adding TiO into an acid burette 2、 Mn and Ce, pouring the second solution into an acid burette, slowly adding the first solution at a uniform and slow speed, continuously stirring by an electric stirring rod in the adding process, and standing until gel is formed;
s4, drying: adjusting the temperature of the oven, putting the gel liquid into the oven for drying, and after drying, putting the gel liquid into a muffle furnace for roasting to obtain catalyst carrier particles;
s5, grinding: grinding the obtained catalyst particles in a grinder into powder;
s6, dipping: putting 50% manganese nitrate solution and 40% cerous nitrate hexahydrate crystal into a beaker, dissolving the mixture in distilled water, mixing uniformly, soaking a certain amount of TiO2, Mn and Ce powder in the mixture to obtain a third solution, and putting catalyst carrier particles in S4 into the third solution for soaking together;
s7, drying: putting the third solution into an oven for drying, and after drying, putting the third solution into a muffle furnace for roasting to obtain new catalyst carrier particles;
s8, grinding: putting the obtained new catalyst carrier particles into a grinder for grinding and screening, and selecting a catalyst with 20-40 meshes for later use;
s9, flue gas simulation: the concentration of each component in the flue gas is detected by a flue gas analyzer, a catalyst is filled in the flue gas analyzer, and the inlet concentration and the outlet concentration of NO in the flue gas are detected and analyzed.
2. The method of claim 1, wherein the method comprises the following steps: in the step S1, the amount of glacial acetic acid added is controlled to be 15-25 ml.
3. The method according to claim 1, wherein the method comprises the following steps: in the step S2, the adding amount of the concentrated nitric acid is controlled to be 4-8 ml.
4. The method of claim 1, wherein the method comprises the following steps: in the step S3, the rotation speed of the electric stirring rod is controlled to be 200 r/min.
5. The method of claim 1, wherein the method comprises the following steps: in the step S4, the oven temperature is controlled at 105 ℃, the drying time is controlled at 8-10h, the muffle temperature is controlled at 500 ℃, and the roasting time is controlled at 4-5 h.
6. The method according to claim 1, wherein the method comprises the following steps: in the step S5, the grinding time is controlled to be 5-10 min.
7. The method of claim 1, wherein the method comprises the following steps: in the step S6, the dipping time is controlled to be 3-4 h.
8. The method of claim 1, wherein the method comprises the following steps: in the step S7, the oven temperature is controlled at 105 ℃, the drying time is controlled at 8-10h, the muffle temperature is controlled at 500 ℃, and the roasting time is controlled at 4-5 h.
9. The method of claim 1, wherein the method comprises the following steps: in the step S8, the grinding time is controlled to be 6-10 min.
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Citations (3)
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| CN111992203A (en) * | 2020-08-31 | 2020-11-27 | 上海应用技术大学 | NH (hydrogen sulfide)3-SCR low-temperature denitration catalyst and preparation method and application thereof |
| CN112121788A (en) * | 2020-09-22 | 2020-12-25 | 江苏大学 | Preparation method and application of B-modified vanadium-titanium low-temperature SCR catalyst |
| CN112808277A (en) * | 2020-12-30 | 2021-05-18 | 东北大学 | Low-temperature SCR denitration catalyst, preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111992203A (en) * | 2020-08-31 | 2020-11-27 | 上海应用技术大学 | NH (hydrogen sulfide)3-SCR low-temperature denitration catalyst and preparation method and application thereof |
| CN112121788A (en) * | 2020-09-22 | 2020-12-25 | 江苏大学 | Preparation method and application of B-modified vanadium-titanium low-temperature SCR catalyst |
| CN112808277A (en) * | 2020-12-30 | 2021-05-18 | 东北大学 | Low-temperature SCR denitration catalyst, preparation method and application thereof |
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