CN102728347B - 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
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material and preparation method thereof.
Background technology:
Along with controlling NO
xbeing gradually improved of Abgasgesetz, NO
xthe air pollution causing more and more causes people's attention.At present, control NO
xthe measure of discharge is roughly divided into two classes: a class is combustion control technology, by various technological means, and the NO that suppresses or reduce in combustion process
x, reach and reduce NO
xthe object of discharge; Another kind of is flue gases purification, removes the NO in flue gas
x.Flue-gas denitrification technology has wet method denitrogenation, catalytic decomposition, solid absorption method, liquid absorption method, plasma activation method, microbial method, SNCR (SNCR) method and SCR (SCR) method etc.Wherein SCR method is considered to best flue-gas denitrification technology at present, and it is under the effect of some special catalyst, uses ammonia (or other reducing agent) optionally by NO
xbe reduced to N
2and H
2the method of O.
Catalyst is parts most crucial in SCR flue gas denitrification system, and its performance quality directly affects the overall denitration effect of SCR flue gas denitrification system.In flue gas, contain a large amount of flue dust, due to the long-term operation of denitrating catalyst, thereby flue dust causes catalyst activity to reduce in catalyst surface deposition.In addition, the temperature of flue gas is lower, if use catalyst reaction temperatures too low, can reduce the activity of catalyst, and denitration efficiency is declined, and does not finally reach the effect of denitration.Therefore the low-temperature denitration catalyst that, has self-cleaning function is for the very important meaning of vigor power plant denitration.
Summary of the invention:
The object of the invention is to overcome the defect of existing denitrating catalyst, utilize high-specific surface area and porosity, the charge transport properties of Graphene uniqueness and the self-cleaning function of fluorohydrocarbon resin material of inorganic ceramic membrane, provide a kind of and there is self-cleaning, catalytic efficiency is high, corrosion-resistant, mechanical strength is large, Stability Analysis of Structures is indeformable and the MnO of long service life
2-TiO
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material and preparation method thereof.
The technical solution adopted in the present invention is:
This low-temperature catalyzed denitration self-cleaning material is taking porous, inorganic ceramic membrane as carrier, by MnO
2, TiO
2be carried on carrier surface with the compound of Graphene, form 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.
The preparation method of described low-temperature catalyzed denitration self-cleaning material, is specifically divided into following steps:
Step (1): be SiO by main component
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 in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and ground, obtain porous, inorganic ceramic membrane;
Step (2): under room temperature, Graphene is put into absolute ethyl alcohol, ultrasonic wave adds tetrabutyl titanate after processing for the first time, and proceed ultrasonic processing for the second time, and the porous, inorganic ceramic membrane of successively acetic acid and manganese nitrate mixed solution and step (1) being produced is joining in above-mentioned solution in ultrasonic processing procedure for the second time; Ultrasonic processing until colloidal sol stop while occurring, aging a couple of days under room temperature condition;
Step (3): the aged samples that step (2) is obtained is dried, roasting, obtains described catalyst, and in the catalyst that makes to obtain, 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 room temperature, cellulose, defoamer, glycosidal resin, filler and deionized water are mixed, and grind with 500 ~ 800r/min speed, the catalyst that adds step (3) to prepare, rises to rotating speed 5000 r/min and continue 30min; Last washed with de-ionized water catalyst 2 ~ 3 times, dry under 80 oC, can obtain described low-temperature denitration catalyst.
The grinding particle diameter of the cinder in described 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 pulverized coal-ash-based porous potsherd after calcining is 0.1mm ~ 0.3mm.
In described step (2), the ultrasonic processing time is 15min for the first time, and secondary ultrasonic processing time is 30min; The concentration of acetic acid is 0.5 mol/L, and the mol ratio of manganese nitrate and acetic acid is 1:2.
Being dried as common air dry oven in described step (3) 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.
Defoamer in described step (4) is polyethers, and filler is 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 is using porous, inorganic ceramic membrane as carrier, its loose structure with and specific area greatly, can make active material be scattered in uniformly carrier surface, for catalytic reaction provides more active centre, and then increase NO
xconversion ratio.MnO
2as the main active of catalyst, there is at low temperatures very high catalytic performance.In addition, Graphene has higher specific 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, ensures the permanently effective operation of catalyst.
Detailed description of the invention:
The invention provides a kind of MnO
2-TiO
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material and preparation method thereof, is further elaborated the present invention below by specific embodiment.
Percentage composition in following example is quality percentage composition if no special instructions.
Embodiment 1
A kind of MnO
2-TiO
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, its preparation method is as follows:
Step (1): be SiO by main component
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, adopts the pressure dip mold moulding of semidry method taking briquetting pressure as 38 MPa on forcing press, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under room temperature, 0.310 g Graphene is put into absolute ethyl alcohol, add 35.570g tetrabutyl titanate after common ultrasonic processing 15 min, again ultrasonic processing 30 min.Be acetic acid and the 3.790 g Mn (NO of 0.5 mol/L successively by 60 ml concentration
3)
24H
2o manganese nitrate mixed solution and 10.000 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80oC and is dried 550oC roasting 1.5 h under 10 h, Muffle furnace nitrogen atmosphere, 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 area, excellence, and the mass percent of compound is respectively 50% and 50%; MnO
2/ TiO
2in/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 deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst of having prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, is dried under 80 oC, 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 pass into simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows, within the scope of 80-150 oC, the catalytic efficiency of catalyst is all very high.And after 16 h use, the catalytic activity of catalyst does not have obviously decline and catalyst surface almost there is no the deposition of flue dust.
Embodiment 2
A kind of MnO
2-TiO
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, its preparation method is as follows:
Step (1): be SiO by main component
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, adopts the condition dip mold moulding of semidry method taking briquetting pressure as 38 MPa on forcing press, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3 mm.
Step (2): under room temperature, 0.250 g Graphene is put into absolute ethyl alcohol, add 28.480g tetrabutyl titanate after common ultrasonic processing 15 min, again ultrasonic processing 30 min.Be acetic acid and the 3.050 g Mn (NO of 0.5 mol/L successively by 48 ml concentration
3)
24H
2o manganese nitrate mixed solution and 12.000 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80oC and is dried 550oC roasting 1.5h under 10 h, Muffle furnace nitrogen atmosphere, 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/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 deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst of having prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, is dried under 80 oC, 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 pass into simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows, within the scope of 80 ~ 150 oC, the catalytic efficiency of catalyst is all very high.And after 16 h use, the catalytic activity of catalyst does not have obviously decline and catalyst surface almost there is no the deposition of flue dust.
Embodiment 3
A kind of MnO
2-TiO
2the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, its preparation method is as follows:
Step (1): be SiO by main component
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, adopts the condition dip mold moulding of semidry method taking briquetting pressure as 38 MPa on forcing press, is pressed into the thin slice of φ 10 × 5 mm; The thin slice of compacting is calcined in Muffle furnace to 2 h under 1100 oC and obtained pulverized coal-ash-based porous potsherd, and be ground to particle diameter 0.1 mm ~ 0.3mm.
Step (2): under room temperature, 0.120 g Graphene is put into absolute ethyl alcohol, add 14.240 g tetrabutyl titanates after common ultrasonic processing 15 min, again ultrasonic processing 30 min.Be acetic acid and the 1.900 g Mn (NO of 0.5 mol/L successively by 30 ml concentration
3)
24H
2o manganese nitrate mixed solution and 16.000 g inoranic membranes join in above-mentioned solution in ultrasonic processing.Ultrasonic processing is until the appearance of colloidal sol.Aging a couple of days under room temperature condition.
Step (3): the aged samples that step (2) is obtained is placed under common air dry oven 80oC and is dried 550 oC roasting 1.5 h under 10h, Muffle furnace nitrogen atmosphere, 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/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 deionized water, and grind with 500 ~ 800r/min speed.Add the catalyst of having prepared, rotating speed is risen to 5000 r/min and continues 30 min.Deionized water washing 2 ~ 3 times, is dried under 80 oC, 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 pass into simulated flue gas the performance of above-mentioned catalyst is tested.Experiment shows, within the scope of 80-150oC, the catalytic efficiency of catalyst is all very high.And after 16 h use, the catalytic activity of catalyst does not have obviously decline and catalyst surface almost there is no the deposition of flue dust.
Claims (5)
1. a MnO
2-TiO
2the preparation method of the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, is characterized in that, this material is taking porous, inorganic ceramic membrane as carrier, by MnO
2, TiO
2be carried on carrier surface with the compound of Graphene, form catalyst, and at catalyst surface load fluorocarbon resin material; Wherein, the mass percent of fluorocarbon resin material and catalyst is respectively 30% and 70%;
This preparation method is specifically divided into following steps:
Step (1): be SiO by main component
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 0.02mm, adopts the condition dip mold moulding that semidry method is 38MPa in briquetting pressure on forcing press, is pressed into thin slice; The thin slice of compacting is calcined in Muffle furnace to 2h at 1100 DEG C and obtained pulverized coal-ash-based porous potsherd, and ground, obtain porous, inorganic ceramic membrane;
Step (2): under room temperature, Graphene is put into absolute ethyl alcohol, ultrasonic wave adds tetrabutyl titanate after processing for the first time, and proceed ultrasonic wave processing for the second time, and the porous, inorganic ceramic membrane of successively acetic acid and manganese nitrate mixed solution and step (1) being produced is joining in above-mentioned solution in ultrasonic wave processing procedure for the second time; Ultrasonic wave is processed until colloidal sol stops while occurring, aging a couple of days under room temperature condition;
Step (3): the aged samples that step (2) is obtained is dried, roasting, obtains described catalyst, and in the catalyst that makes to obtain, 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 room temperature, cellulose, defoamer, glycosidal resin, filler and deionized water are mixed, and grind with 500～800r/min speed, the catalyst that adds step (3) to prepare, rises to rotating speed 5000r/min and continue 30min; Last washed with de-ionized water catalyst 2～3 times, dry at 80 DEG C, can obtain low-temperature denitration catalyst.
2. a kind of MnO according to claim 1
2-TiO
2the preparation method of the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, is characterized in that, the grinding particle diameter of the cinder in described 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 pulverized coal-ash-based porous potsherd after calcining is 0.1mm～0.3mm.
3. a kind of MnO according to claim 1
2-TiO
2the preparation method of the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, is characterized in that, in described step (2), ultrasonic treatment time is 15min for the first time, and secondary ultrasonic treatment time is 30min; The concentration of acetic acid is 0.5mol/L, and the mol ratio of manganese nitrate and acetic acid is 1:2.
4. a kind of MnO according to claim 1
2-TiO
2the preparation method of the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, is characterized in that, being dried as common air dry oven in described step (3) is dry, and baking temperature is 80 DEG C, and be 10h drying time; Roasting is carried out under nitrogen atmosphere, and sintering temperature is 550 DEG C, and roasting time is 1.5h.
5. a kind of MnO according to claim 1
2-TiO
2the preparation method of the low-temperature catalyzed denitration self-cleaning of Graphene-porous, inorganic ceramic membrane material, is characterized in that, the defoamer in described step (4) is polyethers, and filler is whisker; Wherein, the mass ratio of cellulose, polyethers, glycosidal resin, whisker is: 7.8:0.3:52.5:39.4; The mass percent of fluorocarbon resin material and catalyst is respectively 30% and 70%.
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| 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 |
| 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 |
| 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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| 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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| 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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