CN104475084A - Preparation method of low-temperature high-efficiency denitrification catalyst MnO2 - Google Patents
Preparation method of low-temperature high-efficiency denitrification catalyst MnO2 Download PDFInfo
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- CN104475084A CN104475084A CN201410715755.XA CN201410715755A CN104475084A CN 104475084 A CN104475084 A CN 104475084A CN 201410715755 A CN201410715755 A CN 201410715755A CN 104475084 A CN104475084 A CN 104475084A
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- catalyst
- mno
- mno2
- hydrochloric acid
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- 239000003054 catalyst Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- NUJOXMJBOLGQSY-UHFFFAOYSA-N Manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title abstract 12
- 229910000949 MnO2 Inorganic materials 0.000 title abstract 6
- 239000002244 precipitate Substances 0.000 claims abstract description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N n-butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004743 Polypropylene Substances 0.000 claims abstract description 4
- -1 polypropylene Polymers 0.000 claims abstract description 4
- 229920001155 polypropylene Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 4
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 claims description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 229920000428 triblock copolymer Polymers 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 6
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract description 6
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract 2
- 238000001035 drying Methods 0.000 abstract 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- DZGCGKFAPXFTNM-UHFFFAOYSA-N ethanol;hydron;chloride Chemical compound Cl.CCO DZGCGKFAPXFTNM-UHFFFAOYSA-N 0.000 abstract 1
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 abstract 1
- 230000002349 favourable Effects 0.000 abstract 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 abstract 1
- 230000001264 neutralization Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- 239000003546 flue gas Substances 0.000 description 8
- 229910052813 nitrogen oxide Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 230000037250 Clearance Effects 0.000 description 3
- 230000035512 clearance Effects 0.000 description 3
- 229910002089 NOx Inorganic materials 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000003197 catalytic Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000000607 poisoning Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Abstract
The invention relates to a preparation method of a low-temperature high-efficiency denitrification catalyst MnO2, which comprises the following steps: dissolving P123 in a deionized water-hydrochloric acid mixed solution, sequentially adding butanol and ethyl orthosilicate, and stirring; pouring into a closed polypropylene reaction kettle to react, collecting the solid, and drying; cleaning with an ethanol-hydrochloric acid mixed solution, and calcining to obtain a KIT-6 template; dropwisely adding into a manganous nitrate-ethanol mixed solution, stirring, separating the precipitate, cleaning with a sodium hydroxide solution and deionized water to a neutral state, and drying; and calcining in a muffle furnace to obtain the target substance. Compared with the traditional MnO2 catalyst, the mesoporous-structure MnO2 catalyst has the advantages of large specific area, more adsorbed oxygen and high removal ratio of oxynitrides; the MnO2 catalyst has high stability, and the mesoporous structure is still stable after denitrification treatment; and the MnO2 catalyst has higher selective catalytic reduction activity at low temperature, and thus, has favorable application prospects.
Description
Technical field
The present invention relates to the technology of preparing of SCR technology (SCR) catalyst, particularly a kind of efficient cryogenic denitrating catalyst MnO
2preparation method.
Background technology
NOx becomes because causing the series of environmental problems such as acid rain, ozone, haze the object needing keypoint treatment.So far, the mainstream technology removing NOx in air is selective catalytic reduction flue gas denitration technology, the business denitrating catalyst that selective catalytic reduction flue gas denitration technology uses the temperature range that is suitable for narrower and only have and at high temperature just have higher denitration effect, therefore, the high dust arrangement technology of the many employings of flue-gas denitration process (i.e. SCR Plant arrangement before electrostatic precipitator to avoid heating again coal-fired flue-gas).But this technology arrangement not only cost is high, but also catalyst poisoning can be caused to make its inactivation.Therefore the high-efficiency denitration catalyst studying a kind of low temperature has very large meaning.But traditional MnO
2low temperature catalyst denitration effect is poor, therefore improves MnO
2the denitration effect of low temperature catalyst is significant.
The MnO of meso-hole structure
2specific surface area of catalyst is larger than traditional catalyst, such MnO
2the avtive spot of catalyst will increase, and it is removed nitrogen oxide efficiency and will improve.The MnO of meso-hole structure
2catalyst because of the restriction of meso-hole structure, MnO
2the growth restriction of particle and make its particle size less, can make MnO like this
2the reducing power of catalyst strengthens and then improves its nitrogen oxide removal efficiency.The MnO of meso-hole structure
2the content of Catalyst Adsorption oxygen is than traditional MnO
2catalyst is high, and adsorb oxygen accounts for consequence in SCR technology, therefore the MnO of meso-hole structure
2catalyst nitrogen oxide removal efficiency is high.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of efficient cryogenic denitrating catalyst MnO is provided
2preparation method, the MnO of prepared by the method have meso-hole structure
2specific surface area of catalyst is large, and adsorb oxygen is many, the clearance of nitrogen oxide is high; Good stability, after carrying out denitration process, meso-hole structure is still stablized, and SCR activity is at low temperatures higher.。
Technical scheme of the present invention:
A kind of efficient cryogenic denitrating catalyst MnO
2preparation method, step is as follows:
1) PEO-PPOX-PEO triblock copolymer (P123) is dissolved in the mixed liquor of deionized water and 35wt% hydrochloric acid, add butanols, stir 1 hour under 35oC, then add ethyl orthosilicate (TEOS), stir 24 hours under 35oC, obtain mixed liquor;
2) above-mentioned mixed liquor is poured in closed polypropylene agitated reactor, react 24 hours under 100oC, gained solid collected by centrifugation is dried at 100oC;
3) by the solid volume ratio of above-mentioned oven dry be 1:1 ethanol-35wt% hydrochloric acid mixed solution cleaning, then calcine under 550oC, obtain KIT-6 template;
4) above-mentioned KIT-6 template being added concentration is in the manganese nitrate-alcohol mixeding liquid of 0.12g/mL, stirs 8-10 hour, obtains the mixed liquor containing powdery precipitate;
5) above-mentioned powdery precipitate is separated, with the cleaning of 2mol/L sodium hydroxide solution to remove the KIT-6 template in powdery precipitate, and with after washed with de-ionized water to neutrality, dry for standby;
6) above-mentioned powdery precipitate is placed in Muffle furnace rise to 350oC from room temperature with the speed of 1oC/min and keep 5 hours, obtains meso-hole structure MnO
2catalyst.
The mol ratio of described ethyl orthosilicate, PEO-PPOX-PEO triblock copolymer (P123), hydrochloric acid, water and butanols is: 1: 0.017: 1.83: 195: 1.31.
Advantage of the present invention and beneficial effect are:
With traditional MnO
2catalyst is compared, the MnO of prepared by the present invention have meso-hole structure
2specific surface area of catalyst is large, and adsorb oxygen is many, the clearance of nitrogen oxide is high; Good stability, after carrying out denitration process, meso-hole structure is still stablized, and SCR activity is at low temperatures higher, has good application prospect.
Accompanying drawing explanation
Fig. 1 is mesoporous MnO
2the transmission electron micrograph of catalyst.
Fig. 2 is mesoporous MnO
2catalyst and traditional MnO
2the N of catalyst
2adsorption-desorption curve.
Fig. 3 is mesoporous MnO
2catalyst and traditional MnO
2catalyst x-ray photoelectron power spectrum.
Fig. 4 is mesoporous MnO
2catalyst and traditional MnO
2the SCR activity design sketch of catalyst.
Detailed description of the invention
Mesoporous MnO of the present invention is further described below by specific embodiment
2the preparation of catalyst and effect.Illustrate simultaneously, these embodiments the technology contents that describes be illustrative, instead of determinate, protection scope of the present invention should do not limited to according to this.
embodiment:
A kind of efficient cryogenic denitrating catalyst MnO
2preparation method, step is as follows:
1) 6g PEO-PPOX-PEO triblock copolymer (P123) is dissolved in the mixed liquor of 217g deionized water and 11.8g 35wt% hydrochloric acid, add 6g butanols, stir 1 hour under 35oC, then 12.9g ethyl orthosilicate (TEOS) is added, stir 24 hours under 35oC, obtain mixed liquor;
2) above-mentioned mixed liquor is poured in closed polypropylene agitated reactor, react 24 hours under 100oC, gained solid collected by centrifugation is dried at 100oC;
3) by the solid volume ratio of above-mentioned oven dry be 1:1 ethanol-35wt% hydrochloric acid mixed solution cleaning, then calcine under 550oC, obtain KIT-6 template;
4) 3g manganese nitrate is added in 25mL ethanol to dissolve and obtain manganese nitrate-alcohol mixeding liquid, above-mentioned for 1g KIT-6 template is added in manganese nitrate-alcohol mixeding liquid, stirs 8 hours, obtain the mixed liquor containing powdery precipitate;
5) above-mentioned powdery precipitate is separated, with the cleaning of 2mol/L sodium hydroxide solution to remove the KIT-6 template in powdery precipitate, and with after washed with de-ionized water to neutrality, dry for standby;
6) above-mentioned powdery precipitate is placed in Muffle furnace rise to 350oC from room temperature with the speed of 1oC/min and keep 5 hours, obtains meso-hole structure MnO
2catalyst.
Fig. 1 is mesoporous MnO
2the transmission electron micrograph of catalyst.Significantly MnO can be found out from figure
2uniform meso-hole structure.
Fig. 2 is mesoporous MnO
2catalyst and traditional MnO
2the N of catalyst
2adsorption-desorption curve.Show in figure: mesoporous MnO
2catalyst is than traditional MnO
2specific surface area of catalyst is much larger, because mesoporous MnO
2catalyst is pore passage structure, and pore volume is than traditional MnO
2catalyst is large.
Fig. 4 is mesoporous MnO
2catalyst and traditional MnO
2the SCR activity design sketch of catalyst.Show in figure: mesoporous MnO
2the surface adsorbed oxygen of catalyst is than traditional MnO
2catalyst is high a lot, therefore, and mesoporous MnO
2the SCR activity of catalyst is than traditional MnO
2catalyst is high.
Application experiment:
Weigh catalyst prepared by 0.5g and put into fixed bed reactors, SCR reactor is measured respectively at the temperature of setting, design temperature is 100 ° of C, 120 ° of C, 150 ° of C, 200 ° of C, 220 ° of C, 250 ° of C, 300 ° of C, 350 ° of C, open each road source of the gas simultaneously, simulated flue gas, through gas mixer, enters into SCR reactor after temperature control preheater.Simulated flue gas flows through in the process of catalytic bed, NH
3under catalyst action, optionally NO is reduced to N
2and H
2o.In simulated flue gas, each constituent concentration is: flue gas total flow is 200mL/min, 500 ppm NO, 500 ppm NH
3, 3% O
2, 5% H
2during O(application), N
2balance Air.
Fig. 4 is mesoporous MnO
2catalyst and traditional MnO
2the SCR activity design sketch of catalyst.Show in figure: mesoporous MnO
2the SCR activity of catalyst is obviously than traditional MnO
2the SCR activity of catalyst is high a lot, proves mesoporous MnO
2catalyst has very high clearance to NO.
Claims (2)
1. an efficient cryogenic denitrating catalyst MnO
2preparation method, it is characterized in that step is as follows:
1) PEO-PPOX-PEO triblock copolymer (P123) is dissolved in the mixed liquor of deionized water and 35wt% hydrochloric acid, add butanols, stir 1 hour under 35oC, then add ethyl orthosilicate (TEOS), stir 24 hours under 35oC, obtain mixed liquor;
2) above-mentioned mixed liquor is poured in closed polypropylene agitated reactor, react 24 hours under 100oC, gained solid collected by centrifugation is dried at 100oC;
3) by the solid volume ratio of above-mentioned oven dry be 1:1 ethanol-35wt% hydrochloric acid mixed solution cleaning, then calcine under 550oC, obtain KIT-6 template;
4) above-mentioned KIT-6 template being added concentration is in the manganese nitrate-alcohol mixeding liquid of 0.12g/mL, stirs 8-10 hour, obtains the mixed liquor containing powdery precipitate;
5) above-mentioned powdery precipitate is separated, with the cleaning of 2mol/L sodium hydroxide solution to remove the KIT-6 template in powdery precipitate, and with after washed with de-ionized water to neutrality, dry for standby;
6) above-mentioned powdery precipitate is placed in Muffle furnace rise to 350oC from room temperature with the speed of 1oC/min and keep 5 hours, obtains meso-hole structure MnO
2catalyst.
2. efficient cryogenic denitrating catalyst MnO according to claim 1
2preparation method, it is characterized in that: the mol ratio of described ethyl orthosilicate, PEO-PPOX-PEO triblock copolymer (P123), hydrochloric acid, water and butanols is: 1: 0.017: 1.83: 195: 1.31.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105396579A (en) * | 2015-12-22 | 2016-03-16 | 盐城工学院 | Fire coal flue gas denitration demercuration catalyst and preparation method and application thereof |
| CN110124683A (en) * | 2019-06-19 | 2019-08-16 | 南开大学 | Mesoporous NiMn2O4The preparation method of catalyst, the catalyst thus prepared and application thereof |
| CN110548502A (en) * | 2019-08-12 | 2019-12-10 | 广东工业大学 | vanadium oxide modified manganese-based catalyst for low-temperature SCR denitration and preparation method and application thereof |
| CN111644180A (en) * | 2020-03-18 | 2020-09-11 | 河北科技大学 | Catalyst for low-temperature combustion of VOCs (volatile organic compounds) and preparation method thereof |
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2014
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| JPH03275126A (en) * | 1990-03-23 | 1991-12-05 | Kawasaki Heavy Ind Ltd | Method and apparatus for cleaning exhaust gas |
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Non-Patent Citations (1)
| Title |
|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105396579A (en) * | 2015-12-22 | 2016-03-16 | 盐城工学院 | Fire coal flue gas denitration demercuration catalyst and preparation method and application thereof |
| CN105396579B (en) * | 2015-12-22 | 2017-09-15 | 盐城工学院 | A kind of coal-fired flue gas denitration demercuration catalyst and its preparation method and application |
| CN110124683A (en) * | 2019-06-19 | 2019-08-16 | 南开大学 | Mesoporous NiMn2O4The preparation method of catalyst, the catalyst thus prepared and application thereof |
| CN110548502A (en) * | 2019-08-12 | 2019-12-10 | 广东工业大学 | vanadium oxide modified manganese-based catalyst for low-temperature SCR denitration and preparation method and application thereof |
| CN110548502B (en) * | 2019-08-12 | 2022-06-14 | 广东工业大学 | Vanadium oxide modified manganese-based catalyst for low-temperature SCR denitration and preparation method and application thereof |
| CN111644180A (en) * | 2020-03-18 | 2020-09-11 | 河北科技大学 | Catalyst for low-temperature combustion of VOCs (volatile organic compounds) and preparation method thereof |
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Application publication date: 20150401 |