CN112791738B - Dedusting and denitration integrated ceramic membrane material and preparation method thereof - Google Patents
Dedusting and denitration integrated ceramic membrane material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a dedusting and denitration integrated ceramic membrane material, which comprises the following steps: mixing and stirring a first precursor salt, a second precursor salt, urea, a binder and water to obtain a catalyst solution; coating the catalyst solution on a tubular porous ceramic membrane material to obtain a catalyst-loaded tubular porous ceramic membrane material; drying the tubular porous ceramic membrane material loaded with the catalyst; calcining the dried tubular porous ceramic membrane material to obtain a dedusting and denitration integrated ceramic membrane material; the first precursor salt is titanium sulfate and/or zirconium nitrate, the second precursor salt is one or more of copper nitrate, ferric nitrate, cerium nitrate, ammonium metatungstate, manganese nitrate or manganese acetate, and the binder is polyvinyl alcohol and/or silica sol. According to the invention, a clarified and stable catalyst solution is prepared, so that the porous ceramic membrane material with uniform catalyst loading is prepared.
Description
Technical Field
The invention belongs to the field of industrial flue gas purification, and particularly relates to a dust removal and denitration integrated ceramic membrane material and a preparation method thereof.
Background
Dust and nitrogen oxide are main air pollutants, and at present, the purification of dust and nitrogen oxide in flue gas is generally carried out by a dust removal device and a denitration device respectively, so that the defects of complex system, huge investment, high operation and maintenance cost, large occupied area and the like exist, and the popularization and implementation of the flue gas purification technology are hindered to a certain extent. Therefore, the combined removal technology that can simultaneously complete the purification of a plurality of pollutants is the main development reversal of the flue gas purification.
The denitration catalyst is loaded on the porous ceramic membrane material, an effective new method is provided for solving the problem, and the method becomes a research hotspot of flue gas purification treatment. At present, the method for loading a denitration catalyst on a porous ceramic membrane material mainly comprises the steps of loading the denitration catalyst inside or on the surface of a pore channel of the porous ceramic membrane material through processes such as one-time vacuum impregnation, distributed vacuum impregnation, coprecipitation, sol-gel and the like, and obtaining the porous ceramic membrane material with the dust removal and denitration functions after heat treatment.
However, the above processes all result in uneven catalyst loading, and if the required catalytic effect is to be achieved, multiple times of loading is required, so that the catalyst loading is large, channels are easy to block, and the filtration resistance of the ceramic membrane material is obviously increased; based on this, it is a problem to be solved urgently at present to improve the uniformity of catalyst loading and reduce the loading amount of the catalyst.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a dust denitration integrated ceramic membrane material, which prepares a clarified and stable catalyst solution, combines a negative pressure suction method or a pressure coating method to prepare a porous ceramic membrane material with uniform catalyst load and economically feasible load, integrates dust removal and denitration into a whole, can prevent the blockage and abrasion of dust in flue gas to active components, and the prepared material has uniform catalyst load and low filtration resistance increase before and after loading.
On one hand, the application provides a preparation method of a dedusting and denitration integrated ceramic membrane material, which comprises the following steps:
mixing and stirring a first precursor salt, a second precursor salt, urea, a binder and water to obtain a catalyst solution;
coating the catalyst solution on a tubular porous ceramic membrane material to obtain a catalyst-loaded tubular porous ceramic membrane material;
drying the tubular porous ceramic membrane material loaded with the catalyst;
calcining the dried tubular porous ceramic membrane material to obtain a dedusting and denitration integrated ceramic membrane material;
the first precursor salt is titanium sulfate and/or zirconium nitrate, the second precursor salt is one or more of copper nitrate, ferric nitrate, cerium nitrate, ammonium metatungstate, manganese nitrate or manganese acetate, and the binder is polyvinyl alcohol and/or silica sol.
Compared with the prior art, the invention has the following beneficial effects:
the existing catalyst slurry is usually prepared from titanium dioxide particles, certain suspension property is provided for ensuring slurry, the viscosity of the slurry can be increased, if the existing catalyst slurry is used, in the coating process, the slurry has certain viscosity, so that the catalyst is not easy to enter a porous ceramic membrane material pore channel, and the titanium dioxide particles can be intercepted on the surface of the porous ceramic membrane material to form a filter cake layer, so that the catalyst is not uniformly loaded, the denitration efficiency is influenced, and the air permeability resistance of the formed filter cake layer can be greatly increased.
The catalyst solution prepared by the method is a clear solution, has uniform and stable components, can be placed for a long time, enables the catalyst to be more uniformly loaded when being loaded into the pore channel of the tubular porous ceramic membrane material, can achieve the required catalytic effect without multiple loads because the catalyst is more uniformly loaded, and is more economical and controllable in loading capacity.
The water is used as a solvent, so that the stability and the safety of the solution can be ensured, the fluidity of the solution is good, and the drying condition is relatively loose; the first precursor salt selects titanium sulfate and/or zirconium nitrate as a titanium source or a zirconium source, and can obtain a stable solution in water; dissolving a second precursor salt in water to form a stable solution, and obtaining a catalyst active component after subsequent pyrolysis; the urea reacts with the titanium sulfate in the drying process to generate nano titanium dioxide, the polyvinyl alcohol can be used as a dispersing agent, the agglomeration of ceramic particles in the reaction process is reduced, the silica sol can improve the stability of the catalyst at high temperature, and the crystal form transformation of the titanium dioxide is inhibited. Because the components are matched with each other, the stability of the prepared catalyst solution is excellent, and the catalyst can be quickly adsorbed into the pore channel of the tubular porous ceramic membrane material.
According to the invention, titanium sulfate, zirconium nitrate, copper nitrate, ferric nitrate, cerium nitrate, ammonium metatungstate, manganese nitrate, manganese acetate and the like are used for preparing the denitration catalyst, so that on one hand, the denitration catalyst can replace a toxic component vanadium pentoxide in the traditional catalyst, and is low in toxicity or even non-toxic; and on the other hand, the denitration range is wide and the efficiency is high.
The catalyst solution is not required to be prepared at present, and is more uniform in coating, so that the dedusting and denitration integrated ceramic membrane material is convenient and quick to prepare, and the time cost and the raw material cost are both lower.
Preferably, the specific steps of coating the catalyst solution on the tubular porous ceramic membrane material are as follows:
closing one end of the tubular porous ceramic membrane material, putting the tubular porous ceramic membrane material into a container containing the catalyst solution, and performing first negative pressure suction on the other end of the tubular porous ceramic membrane material;
taking the tubular porous ceramic membrane material out of the container containing the catalyst solution, and then carrying out second negative pressure suction;
wherein the negative pressure absolute value during the second negative pressure suction is not less than the negative pressure absolute value during the first negative pressure suction.
The beneficial effect of this preferred scheme does: the catalyst solution forms an even thin layer in the pore channel of the tubular porous ceramic membrane material by a negative pressure suction method, the tubular porous ceramic membrane material is sucked by a first negative pressure when being placed in the catalyst solution, so that the catalyst solution flows in the pore channel of the tubular porous ceramic membrane material, and the situation that part of the internal pore channels cannot contact the catalyst solution due to surface tension and other reasons is avoided.
Preferably, when the first negative pressure is used for suction, the negative pressure value is-0.04 MPa to-0.08 MPa, and the time is 2 to 4min; and when the second negative pressure is used for suction, the negative pressure value is-0.08 MPa, and the time is 1min.
The beneficial effect of this preferred scheme does: too large or too small negative pressure and too long or too short time can affect the uniformity of the catalyst solution coated in the porous ceramic membrane material pore channel.
Preferably, the specific steps of coating the catalyst solution on the tubular porous ceramic membrane material are as follows:
controlling the tubular porous ceramic membrane material to rotate around the axis of the tubular porous ceramic membrane material, placing a conveying pipe capable of spraying the catalyst solution in the core part of the tubular porous ceramic membrane material, and axially moving the conveying pipe along the tubular porous ceramic membrane material so as to spray the catalyst solution on the inner surface of the pipe wall of the tubular porous ceramic membrane material.
The beneficial effect of this preferred scheme does: spraying a catalyst solution on the inner surface of the tube wall of the tubular porous ceramic membrane material, and diffusing and permeating the catalyst solution from the inner surface of the tube wall to the inside of a pore channel by rotating the tubular porous ceramic membrane material, wherein the catalyst loading thickness can be controlled by controlling the dosage of the catalyst, so that the catalyst is prevented from permeating to the outer surface, and the dust and sulfur poisoning of the catalyst on the outer surface are prevented; through controlling the axial moving speed of the conveying pipe and the pressure of liquid in the conveying pipe during spraying, the loading capacity of the catalyst can be accurately controlled, the using amount of the catalyst can be more reasonable, and the operation is simpler and easier to realize.
Preferably, the catalyst solution is sprayed to the inner surface of the tube wall of the tubular porous ceramic membrane material along a direction perpendicular to the axis of the tubular porous ceramic membrane material.
The beneficial effect of this preferred scheme does: the spraying direction of the catalyst liquid is vertical to the inner surface of the tube wall of the tubular porous ceramic membrane material, so that the catalyst slurry is more favorably and uniformly diffused, and the denitration and dust removal integrated porous ceramic membrane material with uniform load is prepared.
Preferably, the weight part ratio of the first precursor salt to the second precursor salt to the urea to the binder to the water is 5-10: 5-15: 1-3: 0.1-1.5: 50-70.
The beneficial effect of this preferred scheme does: by controlling the proportion of each component, the prepared catalyst solution is most convenient to coat and has better catalytic effect.
Preferably, the stirring time is 3 to 5 hours.
The beneficial effect of this preferred scheme does: the stirring time is controlled to obtain a clear and stable catalyst solution.
Preferably, the drying condition is that the temperature is kept at 70-100 ℃ for 8-10 h.
The beneficial effect of this preferred scheme does: the conditions are controlled so that the water evaporates at a suitable rate without affecting the uniformity of the catalyst.
Preferably, the calcining condition is heat preservation for 3-5 h at 400-500 ℃.
The beneficial effect of this preferred scheme does: and controlling the calcination condition to ensure that the precursor salt can be pyrolyzed into the active component of the catalyst and ensure the optimal activity.
On the other hand, the application also claims a dust removal and denitration integrated ceramic membrane material prepared by any one of the preparation methods.
Drawings
FIG. 1 is a graph of the denitration efficiency of the product obtained in example 2 of the present invention;
FIG. 2 is a denitration efficiency image of a product obtained in example 3 of the present invention;
FIG. 3 is a denitration efficiency image of the product obtained in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
A preparation method of a dedusting and denitration integrated ceramic membrane material comprises the following steps:
mixing a first precursor salt, a second precursor salt, urea, a binder and water in a weight ratio of 5-10: 5-15: 1-3: 0.1-1.5: 50-70, and stirring for 3-5 h to obtain a catalyst solution;
coating the catalyst solution on a tubular porous ceramic membrane material to obtain a catalyst-loaded tubular porous ceramic membrane material;
keeping the temperature of the tubular porous ceramic membrane material loaded with the catalyst at 70-100 ℃ for 8-10 h and drying;
calcining the dried tubular porous ceramic membrane material at 400-500 ℃ for 3-5 h to obtain a dedusting and denitration integrated ceramic membrane material;
the first precursor salt is titanium sulfate and/or zirconium nitrate, the second precursor salt is one or more of copper nitrate, ferric nitrate, cerium nitrate, ammonium metatungstate, manganese nitrate or manganese acetate, and the binder is polyvinyl alcohol and/or silica sol.
Preferably, the material of the tubular porous ceramic membrane material can be silicon carbide, cordierite or mullite.
Preferably, the tubular porous ceramic membrane material is a tubular porous ceramic fiber membrane material.
Preferably, the porosity of the tubular porous ceramic membrane material is 30-90%.
Preferably, the method for coating the catalyst solution on the tubular porous ceramic membrane material comprises the following specific steps:
closing one end of the tubular porous ceramic membrane material, putting the tubular porous ceramic membrane material into a container containing the catalyst slurry, and performing first negative pressure suction on the other end of the tubular porous ceramic membrane material, wherein the negative pressure value is-0.04 MPa to-0.08 MPa, and the time is 2-4 min; taking the tubular porous ceramic membrane material out of the container containing the catalyst solution, and then performing second negative pressure suction for 1min;
wherein the negative pressure absolute value during the second negative pressure suction is not less than the negative pressure absolute value during the first negative pressure suction.
Preferably, the method for coating the catalyst solution on the tubular porous ceramic membrane material comprises the following specific steps:
controlling the tubular porous ceramic membrane material to rotate around the axis of the tubular porous ceramic membrane material, placing a conveying pipe capable of spraying the catalyst solution in the core part of the tubular porous ceramic membrane material, and axially moving the conveying pipe along the tubular porous ceramic membrane material so as to spray the catalyst solution on the inner surface of the pipe wall of the tubular porous ceramic membrane material in the direction vertical to the axis of the tubular porous ceramic membrane material.
The embodiment also provides a dedusting and denitration integrated ceramic membrane material prepared by any one of the methods.
Example 2
A preparation method of a dedusting and denitration integrated ceramic membrane material comprises the following steps:
(1) According to the weight parts, titanium sulfate (5 parts), copper nitrate (2 parts), ferric nitrate (1 part), cerous nitrate (2 parts), urea (1 part) and polyvinyl alcohol (0.1 part) are added into water (50 parts), and stirred for 3 hours to obtain a catalyst solution.
(2) Selecting a tubular silicon carbide porous ceramic membrane material, pouring the prepared catalyst solution into a stainless steel container, horizontally placing the tubular silicon carbide porous ceramic membrane material with one closed end in the container, connecting the other end of the tubular silicon carbide porous ceramic membrane material with a suction pipe, sucking for 2min at-0.04 MP a, introducing the sucked catalyst solution into the stainless steel container again, taking out the tubular silicon carbide porous ceramic membrane material after all pore channels in the ceramic membrane material are coated with the catalyst solution, sucking for 1min at-0.06 MPa, and discharging all redundant liquid in the pore channels to obtain the catalyst-loaded tubular porous ceramic membrane material.
(3) And (3) preserving the temperature of the tubular porous ceramic membrane material loaded with the catalyst for 8 hours at 100 ℃ and drying.
(4) And (3) carrying out heat preservation on the dried tubular porous ceramic membrane material at 500 ℃ for 3h for calcination treatment.
The dedusting and denitration integrated ceramic membrane material prepared by the embodiment has the catalyst loading of 8wt%, the denitration efficiency of more than 80% at 260-460 ℃, and the denitration efficiency image of 1m/min under the standard condition is shown in fig. 1.
Example 3
A preparation method of a dedusting and denitration integrated ceramic membrane material comprises the following steps:
(1) According to the weight parts, adding titanium sulfate (10 parts), manganese acetate (3 parts), cerium nitrate (6 parts), urea (3 parts) and silica sol (0.5 part) into water (50 parts), and stirring for 5 hours to obtain a catalyst solution.
(2) Selecting a tubular porous ceramic fiber membrane material, pouring the prepared catalyst solution into a stainless steel container, horizontally placing the tubular porous ceramic fiber membrane material with one closed end in the container, connecting the other end of the tubular porous ceramic fiber membrane material with a suction pipe, sucking at-0.08 MP a for 2min, introducing the sucked catalyst solution into the stainless steel container again, taking out the tubular porous ceramic fiber membrane material after pore channels in the tubular porous ceramic fiber membrane material are completely coated with the catalyst solution, sucking at-0.08 MPa for 1min, and discharging all redundant liquid in the pore channels to obtain the catalyst-loaded tubular porous ceramic membrane material.
(3) Drying the tubular porous ceramic membrane material loaded with the catalyst at 70 ℃ for 10h.
(4) And calcining the dried tubular porous ceramic membrane material at 400 ℃ for 5 hours.
The dedusting and denitration integrated ceramic membrane material prepared by the embodiment has the catalyst loading of 10wt%, the denitration efficiency of more than 80% at 230-460 ℃, and the denitration efficiency image of 1m/min under the standard condition is shown in fig. 2.
Example 4
A preparation method of a dedusting and denitration integrated ceramic membrane material comprises the following steps:
(1) According to the weight parts, adding 5 parts of titanium sulfate, 3 parts of zirconium nitrate, 6 parts of ammonium metatungstate, 3 parts of urea, 0.5 part of polyvinyl alcohol and 1 part of silica sol into 70 parts of water, and stirring for 5 hours to obtain a catalyst solution.
(2) Controlling the tubular porous ceramic fiber membrane material to rotate around an axis, wherein the rotating speed is 200 revolutions per minute, arranging a conveying pipe capable of spraying the catalyst solution in the core part of the tubular porous ceramic fiber membrane material, axially moving the conveying pipe along the tubular porous ceramic fiber membrane material, and controlling the spraying amount to be 0.35kg/min so as to spray the catalyst solution to the inner surface of the pipe wall of the tubular porous ceramic fiber membrane material along the direction vertical to the axis of the tubular porous ceramic fiber membrane material to obtain the catalyst-loaded tubular porous ceramic membrane material.
(3) And (3) preserving the heat of the tubular porous ceramic membrane material loaded with the catalyst for 10h at 70 ℃ and drying.
(4) And (3) carrying out heat preservation on the dried tubular porous ceramic membrane material at 500 ℃ for 3h for calcination treatment.
The dedusting and denitration integrated ceramic membrane material prepared in the embodiment has the catalyst loading of 9wt%, the denitration efficiency of more than 80% at 370-480 ℃, and the denitration efficiency image of 1m/min under the standard condition is shown in fig. 3.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; all other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of a dedusting and denitration integrated ceramic membrane material is characterized by comprising the following steps:
mixing and stirring a first precursor salt, a second precursor salt, urea, a binder and water to obtain a catalyst solution;
coating the catalyst solution on a tubular porous ceramic membrane material to obtain a catalyst-loaded tubular porous ceramic membrane material;
drying the tubular porous ceramic membrane material loaded with the catalyst;
calcining the dried tubular porous ceramic membrane material to obtain a dedusting and denitration integrated ceramic membrane material;
the first precursor salt is titanium sulfate and/or zirconium nitrate, the second precursor salt is one or more of copper nitrate, ferric nitrate, cerium nitrate, ammonium metatungstate, manganese nitrate or manganese acetate, and the binder is polyvinyl alcohol and/or silica sol;
the specific steps of coating the catalyst solution on the tubular porous ceramic membrane material are as follows:
closing one end of the tubular porous ceramic membrane material, putting the tubular porous ceramic membrane material into a container containing the catalyst solution, and performing first negative pressure suction on the other end of the tubular porous ceramic membrane material; taking the tubular porous ceramic membrane material out of the container containing the catalyst solution, and then carrying out second negative pressure suction; wherein the negative pressure absolute value during the second negative pressure suction is not less than the negative pressure absolute value during the first negative pressure suction;
or controlling the tubular porous ceramic membrane material to rotate around the axis of the tubular porous ceramic membrane material, placing a conveying pipe capable of spraying the catalyst solution in the core part of the tubular porous ceramic membrane material, and axially moving the conveying pipe along the tubular porous ceramic membrane material so as to spray the catalyst solution on the inner surface of the pipe wall of the tubular porous ceramic membrane material.
2. The preparation method of the ceramic film material as claimed in claim 1, wherein the first negative pressure is pumped at a negative pressure value of-0.04 MPa to-0.08 MPa for 2 to 4min; and during the second negative pressure suction, the negative pressure value is-0.08 MPa, and the time is 1min.
3. The method for preparing a ceramic membrane material according to claim 1, wherein the catalyst solution is sprayed onto the inner surface of the tube wall of the tubular porous ceramic membrane material in a direction perpendicular to the axis of the tubular porous ceramic membrane material.
4. The preparation method of the ceramic film material as claimed in claim 1, wherein the weight part ratio of the first precursor salt, the second precursor salt, the urea, the binder and the water is 5-10: 5-15: 1~3: 0.1-1.5: 50-70.
5. The preparation method of the ceramic film material as claimed in claim 1, wherein the stirring time is 3 to 5 hours.
6. The preparation method of the ceramic film material as claimed in claim 1, wherein the drying condition is 70-100 ℃ and 8-10h.
7. The preparation method of the ceramic film material as claimed in claim 1, wherein the calcination condition is 400 to 500 ℃ and 3 to 5 hours of heat preservation.
8. A dust removal and denitration integrated ceramic membrane material, which is characterized in that the dust removal and denitration integrated ceramic membrane material is prepared according to the method of claim 1~7.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012119299A1 (en) * | 2011-03-07 | 2012-09-13 | 山东众禾环保科技股份有限公司 | Flue gas denitration catalyst, preparation method and use thereof |
| CN107243256A (en) * | 2017-06-21 | 2017-10-13 | 浙江大学 | The catalytic ceramics filter of flue gas ash removal denitrification integral |
| CN108358652A (en) * | 2018-01-31 | 2018-08-03 | 天津大学 | A kind of preparation method of the gasoline engine particles trap ceramic filter core with gradient pores structure |
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| JP2007277037A (en) * | 2006-04-05 | 2007-10-25 | National Institute Of Advanced Industrial & Technology | Ceramic body, ceramic catalyst body and their manufacturing methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012119299A1 (en) * | 2011-03-07 | 2012-09-13 | 山东众禾环保科技股份有限公司 | Flue gas denitration catalyst, preparation method and use thereof |
| CN107243256A (en) * | 2017-06-21 | 2017-10-13 | 浙江大学 | The catalytic ceramics filter of flue gas ash removal denitrification integral |
| CN108358652A (en) * | 2018-01-31 | 2018-08-03 | 天津大学 | A kind of preparation method of the gasoline engine particles trap ceramic filter core with gradient pores structure |
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