CN102728347A - MnO2-TiO2 graphite-porous inorganic ceramic membrane low temperature catalyst denitration self-cleaning material and its preparation method - Google Patents
MnO2-TiO2 graphite-porous inorganic ceramic membrane low temperature catalyst denitration self-cleaning material and its preparation method Download PDFInfo
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Abstract
The invention relates to a MnO2-TiO2 graphite-porous inorganic ceramic membrane low temperature catalyst denitration self-cleaning material and its preparation method, which belong to the low temperature catalysis denitration field. According to the invention, the material takes a porous inorganic ceramic membrane as a carrier, a compound of MnO2, TiO2 and graphite is loaded on the surface of the carrier; thereby the catalyst is formed, a fluorine hydrocarbon resin material is loaded on the catalyst surface; the mass percent of the fluorine hydrocarbon resin material and the catalyst is respectively 30% and 70%; in the catalyst, the mass percent of the porous inorganic ceramic membrane is between 50% and 80%, the balance is a compound of MnO2, TiO2 and graphite; in the compound of MnO2, TiO2 and graphite, and the atomic ratio of Mn, Ti and C is 1: 6.9: 1.7. the porous inorganic ceramic membrane possesses a porous structure and a great specific surface area provide more activating centers for the catalytic reaction; graphite possesses high specific surface area and excellent electronic transport characteristic, mechanical performance and surface chemical performance, and can increase the catalysis performance of the material under the low temperature; the fluorine hydrocarbon resin compound on the catalyst surface possesses a self-cleaning function.
Description
Technical field:
The invention belongs to low-temperature catalyzed denitration technology field, be specifically related to a kind of MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material and preparation method thereof.
Background technology:
Along with control NO
xBeing gradually improved of Abgasgesetz, NO
xThe air pollution that causes more and more causes people's attention.At present, control NO
xThe measure of discharging roughly is divided into two types: one type is combustion control technology, promptly through various technological means, and the NO in inhibition or the reduction combustion process
x, reach and reduce NO
xThe purpose of discharging; Another kind of is flue gases purification, promptly removes the NO in the flue gas
xThe flue-gas denitrification technology has wet method denitrogenation, catalytic decomposition method, solid absorption method, liquid absorption method, plasma activation method, microbial method, SNCR (SNCR) method and SCR (SCR) method etc.Wherein the SCR method is considered to best flue-gas denitrification technology at present, and it is under the effect of some special catalyst, with ammonia (or other reducing agent) optionally with NO
xBe reduced to N
2And H
2The method of O.
Catalyst is parts most crucial in the SCR flue gas denitrification system, and its performance quality directly influences the whole denitration effect of SCR flue gas denitrification system.Contain a large amount of flue dust in the flue gas, because the long-time running of denitrating catalyst, thereby flue dust causes catalyst activity to reduce in the catalyst surface deposition.In addition, the temperature of flue gas is lower, if the utilization catalyst reaction temperatures is too low, can reduce activity of such catalysts, and denitration efficiency is descended, and does not reach the effect of denitration at last.Therefore, the low-temperature denitration catalyst that has self-cleaning function is for the crucial meaning of vigor power plant denitration.
Summary of the invention:
The objective of the invention is to overcome the defective of existing denitrating catalyst; Utilize the unique charge transport properties of high-specific surface area and porosity, the Graphene of inorganic ceramic membrane and the self-cleaning function of fluorohydrocarbon resin material, provide a kind of and have self-cleaning, catalytic efficiency is high, corrosion-resistant, mechanical strength is big, Stability Analysis of Structures is indeformable and the MnO of long service life
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material and preparation method thereof.
The technical scheme that the present invention adopted is:
This low-temperature catalyzed denitration self-cleaning material is a carrier with the porous, inorganic ceramic membrane, with MnO
2, TiO
2Be carried on carrier surface with the compound of Graphene, constitute catalyst, and at catalyst surface load fluorohydrocarbon resin material; Wherein, the mass percent of fluorohydrocarbon resin material and catalyst is respectively 30% and 70%; In catalyst, the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, MnO
2, TiO
2With the mass percent of the compound of Graphene be 20% ~ 50%; At MnO
2, TiO
2In the compound of Graphene, the atomic ratio of Mn, Ti and C is 1:6.9:1.7.
Described low-temperature catalyzed denitration self-cleaning preparation methods specifically is divided into following steps:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O grinds evenly, and adding particle diameter is the blowing agent of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa in briquetting pressure, is pressed into thin slice; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and, obtain the porous, inorganic ceramic membrane its grinding;
Step (2): under the room temperature; Graphene is put into absolute ethyl alcohol; Add tetrabutyl titanate after the ultrasonic Treatment for the first time; And proceed sonicated for the second time, and the porous, inorganic ceramic membrane of successively acetate and manganese nitrate mixed solution and step (1) being produced joins in the above-mentioned solution in the second time in the sonicated process; Sonicated stops when colloidal sol occurs, and room temperature condition wears out a couple of days down;
Step (3): the aged samples to step (2) obtains is carried out drying, roasting, promptly obtains said catalyst, and makes in the catalyst that obtains, and the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, MnO
2, TiO
2With the mass percent of the compound of Graphene be 20% ~ 50%; At MnO
2, TiO
2In the compound of Graphene, the atomic ratio of Mn, Ti and C is 1:6.9:1.7;
Step (4): under the room temperature, cellulose, antifoaming agent, glycosidal resin, filler and deionized water are mixed, and grind, add the catalyst of step (3) preparation, rotating speed is risen to 5000 r/min and continues 30min with 500 ~ 800r/min speed; Last washed with de-ionized water catalyst 2 ~ 3 times, dry under 80 oC, can obtain said low-temperature denitration catalyst.
The grinding particle diameter of the cinder in the said step (1) is 0.06mm ~ 0.09mm; Blowing agent is that charcoal and consumption are 10% of blowing agent and cinder gross weight; The grinding particle diameter of the fly ash base porous ceramics piece after the calcining is 0.1mm ~ 0.3mm.
The sonicated time first time is 15min in the said step (2), and secondary sonicated time is 30min; The concentration of acetate is 0.5 mol/L, and the mol ratio of manganese nitrate and acetate is 1:2.
Drying in the said step (3) is that common air dry oven is dry, and baking temperature is 80 oC, and be 10 h drying time; Roasting is carried out under nitrogen atmosphere, and sintering temperature is 550 oC, and roasting time is 1.5 h.
Antifoaming agent in the said step (4) is a polyethers, and filler is a whisker; Wherein, the mass ratio of cellulose, polyethers, glycosidal resin, whisker is: 7.8:0.3:52.5:39.4; The mass percent of fluorohydrocarbon resin material and catalyst is respectively 30% and 70%.
Beneficial effect of the present invention is:
The present invention with the porous, inorganic ceramic membrane as carrier, its loose structure with and great specific area, can make active material be scattered in carrier surface uniformly, for catalytic reaction provides more active centre, and then increase NO
xConversion ratio.MnO
2As the main active of catalyst, has very high catalytic performance at low temperatures.In addition, Graphene has higher specific surface area, excellent electronic transport performance, mechanical performance and surface chemistry performance, can improve the catalytic performance under the low temperature of material.In addition, the fluorohydrocarbon resin material of catalyst surface can prevent the deposition of flue dust, guarantees the permanently effective operation of catalyst.
The specific embodiment:
The invention provides a kind of MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material and preparation method thereof is done further elaboration through specific embodiment to the present invention below.
Percentage composition in the following instance is the quality percentage composition like no specified otherwise.
Embodiment 1
A kind of MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material, its preparation method is following:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O is ground to 0.06mm ~ 0.09 mm, and adding 10 wt.% particle diameters is the charcoal of 0.02 mm, and on forcing press, adopting semidry method is the pressure dip mold moulding of 38 MPa with briquetting pressure, is pressed into the thin slice of φ 10 * 5 mm; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under the room temperature, 0.310 g Graphene is put into absolute ethyl alcohol, add 35.570g tetrabutyl titanate, sonicated 30 min once more behind common sonicated 15 min.Be acetate and the 3.790 g Mn (NO of 0.5 mol/L successively with 60 ml concentration
3)
24H
2O manganese nitrate mixed solution and 10.000 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under the common air dry oven 80oC 550oC roasting 1.5 h under dry 10 h, the Muffle furnace nitrogen atmosphere, promptly obtains MnO
2/ Graphene-TiO
2/ inoranic membrane low-temperature denitration catalyst (inorganic ceramic membrane and MnO
2/ TiO
2/ Graphene has electronic transport performance, mechanical performance and the surface chemistry performance of higher specific surface area, excellence, and the mass percent of compound is respectively 50% and 50%; MnO
2/ TiO
2In/the graphene complex, the atomic ratio of Mn, Ti and C is 1:6.9:1.7).
Step (4): 0.680g cellulose, 0.023g polyethers, 4.514g glycosidal resin, 3.386g whisker are dissolved in the deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst that has prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, 80 oC are dry down, can obtain having the low-temperature denitration catalyst (mass percent of fluorohydrocarbon resin and catalyst is 30% and 70%) of self-cleaning function.
Adopt the small-sized simulated experiment platform of development voluntarily and feed simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows that in 80-150 oC scope, the catalytic efficiency of catalyst is all very high.And after 16 h used, the catalytic activity of catalyst did not have obviously decline and catalyst surface almost not to have the deposition of flue dust.
Embodiment 2
A kind of MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material, its preparation method is following:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O is ground to 0.06mm ~ 0.09mm, and adding 10 wt.% particle diameters is the charcoal of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa with briquetting pressure, is pressed into the thin slice of φ 10 * 5 mm; The thin slice of compacting is calcined 2 h under the 1100oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under the room temperature, 0.250 g Graphene is put into absolute ethyl alcohol, add 28.480g tetrabutyl titanate, sonicated 30 min once more behind common sonicated 15 min.Be acetate and the 3.050 g Mn (NO of 0.5 mol/L successively with 48 ml concentration
3)
24H
2O manganese nitrate mixed solution and 12.000 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under the common air dry oven 80oC 550oC roasting 1.5h under dry 10 h, the Muffle furnace nitrogen atmosphere, promptly obtains MnO
2/ Graphene-TiO
2/ inoranic membrane low-temperature denitration catalyst (inorganic ceramic membrane and MnO
2/ TiO
2The mass percent of/graphene complex is respectively 60% and 40%; MnO
2/ TiO
2In/the graphene complex, the atomic ratio of Mn, Ti and C is 1:6.9:1.7).
Step (4): 0.680 g cellulose, 0.023 g polyethers, 4.514 g glycosidal resins, 3.386 g whiskers are dissolved in the deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst that has prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, 80 oC are dry down, can obtain having the low-temperature denitration catalyst (mass percent of fluorohydrocarbon resin and catalyst is 30% and 70%) of self-cleaning function.
Adopt the small-sized simulated experiment platform of development voluntarily and feed simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows that in 80 ~ 150 oC scopes, the catalytic efficiency of catalyst is all very high.And after 16 h used, the catalytic activity of catalyst did not have obviously decline and catalyst surface almost not to have the deposition of flue dust.
Embodiment 3
A kind of MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material, its preparation method is following:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O is ground to 0.06 mm ~ 0.09 mm, and adding 10 wt.% particle diameters is the charcoal of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa with briquetting pressure, is pressed into the thin slice of φ 10 * 5 mm; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and it is ground to particle diameter 0.1 mm ~ 0.3mm.
Step (2): under the room temperature, 0.120 g Graphene is put into absolute ethyl alcohol, add 14.240 g tetrabutyl titanates, sonicated 30 min once more behind common sonicated 15 min.Be acetate and the 1.900 g Mn (NO of 0.5 mol/L successively with 30 ml concentration
3)
24H
2O manganese nitrate mixed solution and 16.000 g inoranic membranes join in sonicated in the above-mentioned solution.Sonicated is until the appearance of colloidal sol.Room temperature condition wears out a couple of days down.
Step (3): the aged samples that step (2) is obtained places under the common air dry oven 80oC 550 oC roastings, 1.5 h under dry 10h, the Muffle furnace nitrogen atmosphere, promptly obtains MnO
2/ Graphene-TiO
2/ inoranic membrane low-temperature denitration catalyst (inorganic ceramic membrane and MnO
2/ TiO
2The mass percent of/graphene complex is respectively 60% and 40%; MnO
2/ TiO
2In/the graphene complex, the atomic ratio of Mn, Ti and C is 1:6.9:1.7).
Step (4): 0.680 g cellulose, 0.023 g polyethers, 4.514 g glycosidal resins, 3.386 g whiskers are dissolved in the deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst that has prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, 80 oC are dry down, can obtain having the low-temperature denitration catalyst (mass percent of fluorohydrocarbon resin and catalyst is 30% and 70%) of self-cleaning function.
Adopt the small-sized simulated experiment platform of development voluntarily and feed simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows that in the 80-150oC scope, the catalytic efficiency of catalyst is all very high.And after 16 h used, the catalytic activity of catalyst did not have obviously decline and catalyst surface almost not to have the deposition of flue dust.
Claims (6)
1. MnO
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane material is characterized in that, is carrier with the porous, inorganic ceramic membrane, with MnO
2, TiO
2Be carried on carrier surface with the compound of Graphene, constitute catalyst, and at catalyst surface load fluorohydrocarbon resin material; Wherein, the mass percent of fluorohydrocarbon resin material and catalyst is respectively 30% and 70%; In catalyst, the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, MnO
2, TiO
2With the mass percent of the compound of Graphene be 20% ~ 50%; At MnO
2, TiO
2In the compound of Graphene, the atomic ratio of Mn, Ti and C is 1:6.9:1.7.
2. described MnO of claim 1
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane preparation methods is characterized in that, specifically is divided into following steps:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O grinds evenly, and adding particle diameter is the blowing agent of 0.02 mm, and on forcing press, adopting semidry method is the condition dip mold moulding of 38 MPa in briquetting pressure, is pressed into thin slice; The thin slice of compacting is calcined 2 h under 1100 oC promptly obtain the fly ash base porous ceramics piece in Muffle furnace, and, obtain the porous, inorganic ceramic membrane its grinding;
Step (2): under the room temperature; Graphene is put into absolute ethyl alcohol; Add tetrabutyl titanate after the ultrasonic Treatment for the first time; And proceed sonicated for the second time, and the porous, inorganic ceramic membrane of successively acetate and manganese nitrate mixed solution and step (1) being produced joins in the above-mentioned solution in the second time in the sonicated process; Sonicated stops when colloidal sol occurs, and room temperature condition wears out a couple of days down;
Step (3): the aged samples to step (2) obtains is carried out drying, roasting, promptly obtains said catalyst, and makes in the catalyst that obtains, and the mass percent of porous, inorganic ceramic membrane is 50% ~ 80%, MnO
2, TiO
2With the mass percent of the compound of Graphene be 20% ~ 50%; At MnO
2, TiO
2In the compound of Graphene, the atomic ratio of Mn, Ti and C is 1:6.9:1.7;
Step (4): under the room temperature, cellulose, antifoaming agent, glycosidal resin, filler and deionized water are mixed, and grind, add the catalyst of step (3) preparation, rotating speed is risen to 5000 r/min and continues 30min with 500 ~ 800r/min speed; Last washed with de-ionized water catalyst 2 ~ 3 times, dry under 80 oC, can obtain said low-temperature denitration catalyst.
3. a kind of MnO according to claim 2
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane preparation methods is characterized in that the grinding particle diameter of the cinder in the said step (1) is 0.06mm ~ 0.09mm; Blowing agent is that charcoal and consumption are 10% of blowing agent and cinder gross weight; The grinding particle diameter of the fly ash base porous ceramics piece after the calcining is 0.1mm ~ 0.3mm.
4. a kind of MnO according to claim 2
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane preparation methods is characterized in that, the sonicated time first time is 15min in the said step (2), and secondary sonicated time is 30min; The concentration of acetate is 0.5 mol/L, and the mol ratio of manganese nitrate and acetate is 1:2.
5. a kind of MnO according to claim 2
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane preparation methods is characterized in that, the drying in the said step (3) is that common air dry oven is dry, and baking temperature is 80 oC, and be 10 h drying time; Roasting is carried out under nitrogen atmosphere, and sintering temperature is 550 oC, and roasting time is 1.5 h.
6. a kind of MnO according to claim 2
2-TiO
2Graphene-low-temperature catalyzed denitration the self-cleaning of porous, inorganic ceramic membrane preparation methods is characterized in that the antifoaming agent in the said step (4) is a polyethers, and filler is a whisker; Wherein, the mass ratio of cellulose, polyethers, glycosidal resin, whisker is: 7.8:0.3:52.5:39.4; The mass percent of fluorohydrocarbon resin material and catalyst is respectively 30% and 70%.
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| CN104028266A (en) * | 2014-06-13 | 2014-09-10 | 上海应用技术学院 | (MnO2, TiO2)n nanosheet assembled film and preparation method and application thereof |
| CN104190409A (en) * | 2014-08-19 | 2014-12-10 | 南京师范大学 | Graphene-loaded titanium-based core-shell-structured low-temperature SCR sulfur-resisting catalyst and preparation method thereof |
| CN107029704A (en) * | 2017-05-19 | 2017-08-11 | 四川大学 | Catalyst and preparation method thereof, the method for removing nitrogen oxides |
| CN108380225A (en) * | 2018-02-07 | 2018-08-10 | 齐齐哈尔大学 | A kind of synthetic method of the anti-inactivation denitrating catalyst of efficient cryogenic |
| CN114632541A (en) * | 2021-12-10 | 2022-06-17 | 华北电力大学（保定） | Graphene-promoted low-temperature combined desulfurization and denitrification catalyst and preparation process thereof |
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| CN1583273A (en) * | 2004-06-11 | 2005-02-23 | 中山大学 | Preparing method for loaded metal oxide catalyst |
| CN102151561A (en) * | 2011-01-22 | 2011-08-17 | 浙江理工大学 | Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof |
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|---|---|---|---|---|
| CN104028266A (en) * | 2014-06-13 | 2014-09-10 | 上海应用技术学院 | (MnO2, TiO2)n nanosheet assembled film and preparation method and application thereof |
| CN104028266B (en) * | 2014-06-13 | 2016-06-22 | 上海应用技术学院 | A kind of (MnO2、TiO2)nThin film that nanometer sheet assembles and its preparation method and application |
| CN104190409A (en) * | 2014-08-19 | 2014-12-10 | 南京师范大学 | Graphene-loaded titanium-based core-shell-structured low-temperature SCR sulfur-resisting catalyst and preparation method thereof |
| CN104190409B (en) * | 2014-08-19 | 2016-08-17 | 南京师范大学 | The low-temperature SCR sulfur resistant catalyst of graphene-supported titanium-based core shell structure and preparation method |
| CN107029704A (en) * | 2017-05-19 | 2017-08-11 | 四川大学 | Catalyst and preparation method thereof, the method for removing nitrogen oxides |
| CN108380225A (en) * | 2018-02-07 | 2018-08-10 | 齐齐哈尔大学 | A kind of synthetic method of the anti-inactivation denitrating catalyst of efficient cryogenic |
| CN108380225B (en) * | 2018-02-07 | 2022-11-29 | 齐齐哈尔大学 | Synthetic method of low-temperature efficient deactivation-resistant denitration catalyst |
| CN114632541A (en) * | 2021-12-10 | 2022-06-17 | 华北电力大学（保定） | Graphene-promoted low-temperature combined desulfurization and denitrification catalyst and preparation process thereof |
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