CN103263913B - Preparation method for high-specific surface anti-alkalosis denitration catalyst applicable to cement kiln - Google Patents
Preparation method for high-specific surface anti-alkalosis denitration catalyst applicable to cement kiln Download PDFInfo
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Abstract
The invention provides a preparation method for a high-specific surface anti-alkalosis denitration catalyst applicable to a cement kiln, which belongs to the field of reduction of NOx in the cement kiln. The preparation method comprises the following steps: uniformly mixing a titanium source solution with SiO2 sol, then adding a manganese salt, a cerium salt and an auxiliary agent and continuing stirring so as to obtain a mixed solution; successively adding a urea solution, ammonia water and hydrogen peroxide into the mixed solution until no precipitate is produced and continuing stirring for 1 to 3 h; and then carrying out centrifugal washing sequentially with distilled water and absolute ethyl alcohol and carrying out drying at a temperature of 75 to 110 DEG C for 6 to 24 h and then calcining at a temperature of 450 to 650 DEG C for 2 to 6 h so as to prepare the 40-mesh to 60-mesh catalyst. Compared with catalysts having same components and prepared by using a sol-gel method and an impregnation method, the catalyst prepared in the invention has the advantages of a high specific surface area, a high denitration rate and alkali resistance. The preparation method for the catalyst is simple, easy to operate and applicable to industrial production.
Description
Technical field
The invention belongs to the NOx decrement field of cement kiln.
Background technology
The major pollutants of burning clinker of cement process discharge have NOx and dust, and in burning clinker of cement process, NOx mainly comes from the nitrogen in high-temperature fuel and the nitrogen-containing compound in raw material.Carried out the data of first time national Pollutant source investigation according to 2007, new dry process rotary kiln NOx average emission coefficient is 1100mg/Nm
3.Within 2010, China's cement output is more than 1,800,000,000 tons, and clinker output about 1,200,000,000 tons, estimates by above-mentioned emission factor, and cement industry discharge NOx about 2,200,000 tons, accounts for 1/10th of national NOx discharge in 2010.Therefore decrement treatment is carried out to the NOx of cement kiln, have great importance.
The honeycomb type denitration catalyst material that existing SCR technology adopts, reaction temperature requires at 300 ~ 400 DEG C, and generally, the tail gas of cement kiln is in middle temperature about 300 DEG C ~ 400 DEG C, but after employing cogeneration, its flue-gas temperature is down to about 180 DEG C, after reentering mill drying material, flue-gas temperature is down to 80 ~ 100 DEG C, and catalysis material all long-term works under relatively high dust atmosphere in cement kiln, with use specific aim, higher requirement is proposed to the low temperature adaptability of denitration catalyst material.
Both at home and abroad to the low temperature research of denitrating catalyst much but relatively less for the research that catalyst alkali metal is poisoning.Relative SO in cement kiln
2, alkali-metal Poisoning Effect is larger, and what study herein is exactly under this specific environment of cement kiln, and the catalyst prepared by coprecipitation is compared catalyst prepared by additive method and had good alkali resistance.Li Feng have studied graininess V
2o
5/ TiO
2the impact of catalyst based middle co-catalyst, comprises the Poisoning Effect of alkalies and alkaline earth to catalyst, find that CaO is different to the poisoning of catalyst and alkali metal, and degree of intoxication is not as seriously alkali-metal.Shen Baixiong, Ma Juan have prepared V with pottery sol-gal process and infusion process
2o
5-MoO
3/ TiO
2catalyst, and use SiO
2carry out modification, modified fresh catalyst reduction temperature moves about 10 DEG C to low temperature direction, and redox ability is improved, and its surface acid strength and acid amount are also greatly improved.When Wu Zhongbiaos etc. have studied Selective Catalytic Reduction of NO x, alkali metal has poisoning effect to Ce-Ti catalyst, and discloses the PASSIVATION MECHANISM of alkali metal to catalyst with theory by experiment.
The titanium silicon complex carrier that the present invention is prepared for titanium source by utilizing the intermediate product titanyl sulfate of method for producing gtitanium dioxide with sulphuric acid, the denitration catalyst under cement kiln low temperature environment studying rear-earth-doped transition metal (Mn) base composite oxidate catalysis material is active, the catalyst material system of development of new, to obtain flue gas change strong adaptability and the SCR catalyst material of the lower alkali resistant metal poisoning of the cost of raw material.
Summary of the invention
The object of this invention is to provide a kind of preparation method being applicable to the low-temperature denitration catalyst of cement kiln of rear-earth-doped transition metal (Mn) base composite oxidate.
Be applicable to a preparation method for the poisoning denitrating catalyst of high-ratio surface alkali resistant of cement kiln, it is characterized in that preparation process is as follows:
By titanium source solution and SiO
2continue stirring after adding manganese salt, cerium salt and auxiliary agent after colloidal sol mixes and obtain mixed solution, urea liquid, ammoniacal liquor, hydrogen peroxide is sequentially added into no longer producing precipitation in above-mentioned mixed solution, continue to stir 1-3 hour, then priority distilled water and absolute ethyl alcohol centrifuge washing, at 75-110 DEG C of dry 6-24 hour, 450-650 DEG C of calcining, after 2-6 hour, is prepared into 40-60 object catalyst;
Wherein, keep bath temperature 65-95 DEG C when adding urea liquid, in catalyst preparation process, manganese salt is any one in manganese acetate, manganese nitrate, manganese sulfate, manganese chloride; Described cerium salt is any one in cerous chlorate, cerous nitrate, ammonium ceric nitrate or cerous sulfate; Described titanium source solution is any one in titanyl sulfate, titanium sulfate, butyl titanate; The auxiliary agent added is any one in ferric nitrate, copper nitrate, nickel nitrate, chromic nitrate;
Described SiO
2colloidal sol is self-control SiO
2the Ludox of colloidal sol or 30wt%; Self-control SiO
2the preparation method of colloidal sol is ethyl orthosilicate: ethanol: the solution that water is made into by 1:2-5:4-8 volume ratio; The mol ratio of wherein elements Si: Ti is 0.08-0.5:1.
Further, titanium source solution molar concentration 0.1-0.5mol/L, the molar concentration 0.5-3mol/L of urea liquid.
Further, titanium source: urea: ammoniacal liquor: the mol ratio=1:0.5-2:0.5-2:0.8-1.2 of hydrogen peroxide; Titanium source: manganese salt: cerium salt: the mol ratio=1:0.1-0.6:0.04-0.1:0-0.1 of auxiliary agent.
Catalytic reaction condition of the present invention: 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.The catalyst denitration rate that with this understanding prepared by the present invention can reach 98%, and when alkali metal is poisoning, the highest denitration rate can reach 93%, and specific area is 220m
2/ more than g.
The present invention uses coprecipitation to pass through to add the SCR catalyst material that the preparation of different auxiliary agent has anti-alkalotic titanium silicon complex carrier.
Detailed description of the invention
Example one: distilled water 16g titanyl sulfate being dissolved in 150ml, settled solution is dissolved as stir 1h under 60 DEG C of water-baths after, by 5ml ethyl orthosilicate, 10ml ethanol, 20ml distilled water mix and blend 1h prepares SiO2 colloidal sol, 19.6g manganese acetate is added after being mixed under 60 DEG C of water-baths by above-mentioned two kinds of solution, 3.04g cerous nitrate continues to stir, the mixed solution prepared adds 2mol/L urea liquid 50ml respectively and stirs 1h at water-bath 95 DEG C, the ammoniacal liquor 100ml of 25% concentration, the hydrogen peroxide 60ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 75 DEG C dry 12h, catalyst fines is prepared into after 450 DEG C of calcining 4h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 95%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 89%.
Example two: distilled water 16g titanyl sulfate being dissolved in 1000ml, settled solution is dissolved as stir 1h under 60 DEG C of water-baths after, 7g silicon sol solution (content of SiO2 is 30%(wt%) is added in above-mentioned mixed solution) continue to stir 1h, 9.8g manganese acetate is added after being mixed under 60 DEG C of water-baths by above-mentioned two kinds of solution, 3.04g cerous nitrate, 2.83g ferric nitrate continues to stir, the mixed solution prepared adds 2mol/L urea liquid 50ml respectively and stirs 1h at water-bath 95 DEG C, the ammoniacal liquor 85ml of 25% concentration, the hydrogen peroxide 50ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 90 DEG C dry 6h, catalyst fines is prepared into after 600 DEG C of calcining 2h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 98%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 90%.
Example three: distilled water 16g titanyl sulfate being dissolved in 500ml, settled solution is dissolved as stir 1h under 60 DEG C of water-baths after, by 3ml ethyl orthosilicate, 16ml ethanol, 35ml distilled water mix and blend 1h prepares SiO2 colloidal sol, 7.16g manganese nitrate is added after being mixed under 60 DEG C of water-baths by above-mentioned two kinds of solution, 3.04g cerous nitrate, 2.03g nickel nitrate continues to stir, the mixed solution prepared adds 1mol/L urea liquid 100ml respectively and stirs 3h at water-bath 65 DEG C, the ammoniacal liquor 80ml of 25% concentration, the hydrogen peroxide 50ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 90 DEG C dry 8h, catalyst fines is prepared into after 550 DEG C of calcining 3h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 98%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 93%.
Example four: be dissolved as settled solution after 10g titanium sulfate solution being dissolved in the distilled water stirring 2h of 50ml, by 7ml ethyl orthosilicate, 10ml ethanol, 20ml distilled water mix and blend 1h prepares SiO2 colloidal sol, 19.6g manganese acetate is added by after above-mentioned two kinds of solution mixing, 2.6g cerous chlorate, 2.03g nickel nitrate continues to stir, the mixed solution prepared adds 2mol/L urea liquid 50ml respectively and stirs 2h at water-bath 80 DEG C, the ammoniacal liquor 100ml of 25% concentration, the hydrogen peroxide 30ml of 30% concentration stirs 4h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 75 DEG C dry 12h, catalyst fines is prepared into after 600 DEG C of calcining 3h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 92%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 85%.
Example five: get 34g tetrabutyl titanate and 5g ethyl orthosilicate and be dissolved in 18.5g absolute ethyl alcohol and stir 1h, above-mentioned solution is mixed under ice-water bath and adds 19.6g manganese acetate, 3.04g cerous nitrate continues stirring, the mixed solution prepared adds 2mol/L urea liquid 50ml respectively and stirs 1h at water-bath 95 DEG C, the ammoniacal liquor 80ml of 25% concentration, the hydrogen peroxide 40ml of 30% concentration stir 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 90 DEG C dry 6h, be prepared into catalyst fines after 600 DEG C of calcining 2h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 93%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 80%.
Example six: get 34g tetrabutyl titanate be dissolved in stir in 18.5g absolute ethyl alcohol after add 5g silicon sol solution (content of SiO2 is 30%(wt%)) continue stir 1h, 13.38g manganese sulfate is added in above-mentioned solution, 3.04g cerous nitrate continues to stir, the mixed solution prepared adds 0.5mol/L urea liquid 200ml respectively and stirs 2.5h at water-bath 65 DEG C, the ammoniacal liquor 75ml of 25% concentration, the hydrogen peroxide 30ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 75 DEG C dry 12h, catalyst fines is prepared into after 500 DEG C of calcining 3h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 94%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 83%.
Example seven: be dissolved as settled solution after 10g titanium sulfate solution being dissolved in the distilled water stirring 2h of 100ml, by 5ml ethyl orthosilicate, 10ml ethanol, 20ml distilled water mix and blend 1h prepares SiO2 colloidal sol, 19.6g manganese acetate is added by after above-mentioned two kinds of solution mixing, 2.6g cerous chlorate continues to stir, the mixed solution prepared adds 2mol/L urea liquid 50ml respectively and stirs 1h at water-bath 95 DEG C, the ammoniacal liquor 100ml of 25% concentration, the hydrogen peroxide 60ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 105 DEG C dry 6h, catalyst fines is prepared into after 450 DEG C of calcining 4h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 95%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 83%.
Example eight: be dissolved as settled solution after 10g titanium sulfate solution being dissolved in the distilled water stirring 2h of 50ml, add 5g silicon sol solution (content of SiO2 is 30%(wt%)) continue to stir 1h, 11.9 manganese chlorides are added by after above-mentioned two kinds of solution mixing, 2.6g cerous chlorate continues to stir, the mixed solution prepared adds 3mol/L urea liquid 40ml respectively and stirs 1h at water-bath 90 DEG C, the ammoniacal liquor 100ml of 25% concentration, the hydrogen peroxide 60ml of 30% concentration stirs 2h, by the precipitation distilled water centrifuge washing that obtains 2 times, after absolute ethyl alcohol centrifuge washing 2 times at 105 DEG C dry 6h, catalyst fines is prepared into after 450 DEG C of calcining 4h.
Denitration rate is tested: catalytic reaction condition is 1000ppmNO, 1000ppmNH
3, 5%O
2, N
2for carrier gas, gas flow rate is 2000ml/min, and air speed is 27000h
-1.Denitration rate is up to 95%.
Alkali resistant metal poisoning is tested: in 1.5g catalyst, add water after load 0.1g potassium nitrate mix, 95 DEG C of dry 1h, and carry out catalytic performance test after 450 DEG C of calcining 3h, denitration rate reaches as high as 83%.
Claims (2)
1. be applicable to a preparation method for the poisoning denitrating catalyst of high-ratio surface alkali resistant of cement kiln, it is characterized in that preparation process is as follows:
By titanium source solution and SiO
2continue stirring after adding manganese salt, cerium salt and auxiliary agent after colloidal sol mixes and obtain mixed solution, urea liquid, ammoniacal liquor, hydrogen peroxide is sequentially added into no longer producing precipitation in above-mentioned mixed solution, continue to stir 1-3 hour, then priority distilled water and absolute ethyl alcohol centrifuge washing, at 75-110 DEG C of dry 6-24 hour, 450-650 DEG C of calcining, after 2-6 hour, is prepared into 40-60 object catalyst;
Wherein, keep bath temperature 65-95 DEG C when adding urea liquid, in catalyst preparation process, manganese salt is any one in manganese acetate, manganese nitrate, manganese sulfate, manganese chloride; Described cerium salt is any one in cerous chlorate, cerous nitrate, ammonium ceric nitrate or cerous sulfate; Described titanium source solution is any one in titanyl sulfate, titanium sulfate, butyl titanate; The auxiliary agent added is any one in ferric nitrate, copper nitrate, nickel nitrate, chromic nitrate;
Described SiO
2colloidal sol is self-control SiO
2the Ludox of colloidal sol or 30wt%; Self-control SiO
2the preparation method of colloidal sol is ethyl orthosilicate: ethanol: the solution that water is made into by 1:2-5:4-8 volume ratio; The mol ratio of wherein elements Si: Ti is 0.08-0.5:1;
Wherein titanium source: urea: ammoniacal liquor: the mol ratio=1:0.5-2:0.5-2:0.8-1.2 of hydrogen peroxide; Titanium source: manganese salt: cerium salt: the mol ratio=1:0.1-0.6:0.04-0.1:0-0.1 of auxiliary agent.
2. method according to claim 1, is characterized in that: titanium source solution molar concentration 0.1-0.5mol/L, the molar concentration 0.5-3mol/L of urea liquid.
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| CN103537279B (en) * | 2013-10-15 | 2015-12-02 | 北京工业大学 | A kind of low-temperature denitration catalyst adding auxiliary agent and preparation method thereof |
| CN103638942B (en) * | 2013-12-17 | 2017-01-18 | 中国建筑材料科学研究总院 | SCR (selective catalytic reduction) catalyst for denitrating low-temperature smoke of cement kiln and preparation method thereof |
| CN103894186B (en) * | 2014-03-29 | 2015-09-02 | 北京工业大学 | A kind of acid-dissolved titanium slag prepares the method for manganese titanium system low-temperature denitration catalysis material |
| CN104001501B (en) * | 2014-05-27 | 2016-04-06 | 北京工业大学 | A kind of acid hydrolysis residue prepares the method for denitration catalyst material |
| CN115819769B (en) * | 2022-12-31 | 2023-11-03 | 杭州瑞思新材料有限公司 | Catalyst for organic silicon and preparation method thereof |
| CN116637614A (en) * | 2023-05-10 | 2023-08-25 | 安徽工业大学 | Cerium-manganese-based denitration catalyst with high alkali resistance, and preparation method and application thereof |
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| US6521559B1 (en) * | 1999-09-27 | 2003-02-18 | The Regents Of The University Of Michigan | Superior pillared clay catalysts for selective catalytic reduction of nitrogen oxides for power plant emission control |
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| US6521559B1 (en) * | 1999-09-27 | 2003-02-18 | The Regents Of The University Of Michigan | Superior pillared clay catalysts for selective catalytic reduction of nitrogen oxides for power plant emission control |
| CN102101048A (en) * | 2011-01-25 | 2011-06-22 | 清华大学 | Cerium-based denitration catalyst with titanium-silicon compound oxide as carrier and preparation and application thereof |
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