CN103894186B - A kind of acid-dissolved titanium slag prepares the method for manganese titanium system low-temperature denitration catalysis material - Google Patents
A kind of acid-dissolved titanium slag prepares the method for manganese titanium system low-temperature denitration catalysis material Download PDFInfo
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Abstract
The method that acid-dissolved titanium slag prepares manganese titanium system low-temperature denitration catalysis material belongs to an environmentally conscious materials, environmental catalysis and field of environment protection.The present invention is on the basis of Production By Sulfuric Acid Process titanium white technique, cut down technological process to remain with the element helping improve denitration activity, take acid-dissolved titanium slag as raw material, acidolysis obtains titanium liquid, titanium hydrolysis generates metatitanic acid, take metatitanic acid as carrier, adopt coprecipitation, add the preparation method that manganese acetate preparation is applicable to the low-temperature denitration catalysis material of cement kiln.Described catalysis material preparation method cost is low, is applicable to suitability for industrialized production.
Description
Technical field
The invention belongs to environmental catalysis material and field of environment protection, be specially a kind of cement kiln low temperature SCR denitration catalysis material.
Background technology
Nitrogen oxide is the one of the main reasons causing acid rain, photochemical fog and PM2.5.Nitrogen oxide can produce strong impulse effect to human body respiration organ mucous membrane, and long-term suction may cause lung's structural change, brings very large threat to we are healthy.Along with the steady growth of national economy, the development of domestic cement industry fast manganese, cement output rises to 21.8 hundred million t of 2012 by 10.6 hundred million t of 2006, average annual growth rate more than 10%, cement industry NO simultaneously
xa large amount of discharges also bring huge load to environment.Cement industry NO
xdischarge accounts for national industrial NO
x10% ~ 12% of discharge, its discharge capacity is only second to coal-burning power plant and motor vehicle exhaust emission.Therefore, country at " energy-saving and emission-reduction " 12 " planning " middle clear stipulaties cement industry NO
xthe binding indicator of the atmosphere pollution of discharge, requires cement industry NO in 2015
xbasis in 2010 cuts down 12%, controls at 1,500,000 t.
SCR (Selective Catalytic Reduction, SCR) is current most important a kind of denitration method for flue gas.It is with ammoniacal liquor or urea for denitrfying agent, and make catalysis Selective absorber under the catalysis material effect in absorption tower, denitration rate can reach 85% ~ 95%.The business SCR catalysis material of denitrating flue gas consist of V
2o
5(WO
3)/TiO
2(anatase), its running temperature, generally at 350 ~ 400 DEG C, is difficult in smoke processing system end use application, and installation and operation costly.
The feature of the flue gas of cement kiln discharge is: flue-gas temperature is about 300 DEG C, and dust concentration is high.If directly carry out denitration to flue gas, the dust in flue gas can block the active hole of catalysis material, causes catalysis material inactivation.Therefore in order to extend catalysis material life-span and after SCR is placed in desulfation dust-extraction device, but after desulfurization and dedusting, flue-gas temperature is general all lower than 200 DEG C, just must carry out Repeat-heating to flue gas, this will consume more multiple resource, increase denitration cost.Therefore, develop low-temperature SCR catalysis material and technique very necessary.
SCR is the denitration technology of main application in the world at present.This technological core is catalysis material, and its cost accounts for overall cost 30% ~ 50%; Investment, the maintenance cost of this technology are all higher.At present, SCR technology at home cement industry not yet drop into.Therefore research and development have good low temperature active, efficient, low cost catalysis material is the key breaking this bottleneck, have also responded current NO
xthe reduction of discharging policy of compound, is significant to the improvement of the ecological environment of Chinese national economy high speed development and green.
Based on denitration low temperature active and the TiO of Mn oxide excellence
2the stability of carrier, prepares manganese titanium system catalysis material both at home and abroad and substantially all uses titanium white for raw material, and add the auxiliary agents such as Fe to improve denitration activity.China produces titanium white mainly based on sulfuric acid process, and raw material is ilmenite, containing elements such as Ti, Fe, Si, Al, Mn, V.Production By Sulfuric Acid Process titanium white master operation has: acidolysis slaking, leaching reduction, the sedimentation of titanium liquid, freezing and crystallizing centrifugation, controlling filtration, evaporation and concentration, hydrolysis, the evolution (rinsing and bleaching) of metatitanic acid, Ficus caricaL, calcining, pulverizing.The process of Production By Sulfuric Acid Process titanium white prepares the inverse process of manganese titanium system catalysis material just.
The present invention selects acid-dissolved titanium slag to be raw material, acid-dissolved titanium slag by ilmenite concentrate through electric furnace reduction melting gained, TiO
2grade is about 75%, is suitable for sulfuric acid process and produces titanium white.Relative ilmenite, acid-dissolved titanium slag application industrially not only eliminates freezing iron removal step, can not produce ferrous sulfate, can not build ferrous storage, can also save construction investment.Simultaneously because the content of acid-dissolved titanium slag titanium is at a middle or low price higher, do not need to add iron powder in leaching process or iron filings reduce.Owing to using acid-dissolved titanium slag consumption few, refuse amount reduces, and can realize the target reduced discharging.And acid titanium slag stable components, is also suitable as the raw material of denitration catalyst material.
We do not wish impurity to eliminate in the present invention, so plate compression, evaporating concentration process are saved, and save the step of pulverizing-calcining-Ficus caricaL-rinsing-bleaching, at hydrolysate metatitanic acid (TiO
2xSO
3yH
2o) denitration catalyst material is prepared on basis.
Summary of the invention
The present invention is on the basis of Production By Sulfuric Acid Process titanium white technique, cut down technological process to remain with the element helping improve denitration activity, take acid-dissolved titanium slag as raw material, acidolysis obtains titanium liquid, titanium hydrolysis generates metatitanic acid, take metatitanic acid as carrier, preparation is applicable to the preparation method of the low-temperature denitration catalysis material of cement kiln.
Acid-dissolved titanium slag prepares a method for manganese titanium system low-temperature denitration catalysis material, comprises the following steps:
The first step, it is 98% sulfuric acid that acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:1.8 ~ 3.0,200 ~ 220 DEG C of reaction 4 ~ 8h in closed container;
The acid hydrolysate of the first step is 5% ~ 10% sulfuric acid to leach with water or mass percent concentration by second step under 60 ~ 80 DEG C of water-baths, magnetic agitation 2 ~ 3h; Centrifugal, isolate top titanium liquid, remove bottom residues;
3rd step, is preheating to 96 DEG C by isolated for second step titanium liquid, then is added in 96 DEG C of water, and titanium liquid and water quality are than being 4:1; By solution warms to boiling; Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs; After 45min, again heat, stir, arrive boiling, and keep boiling 3h, be diluted with water, then cool after stirring 10 ~ 30min;
4th step, after the reactant mixture cooling of the 3rd step, centrifugal, washing obtains metatitanic acid; By metatitanic acid in 80 ~ 120 DEG C of drying 10 ~ 15h;
5th step, metatitanic acid is water-soluble, mix with manganese acetate solution, magnetic agitation 20 ~ 30min;
6th step, by mixed solution 80 ~ 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid, magnetic agitation 30min; Add ammoniacal liquor, to pH=10 ~ 11; Drip hydrogen peroxide, cool after magnetic agitation 30min; Wherein metatitanic acid: urea: ammoniacal liquor: the mol ratio of hydrogen peroxide is 1:0.5 ~ 2:0.5 ~ 2:0.8 ~ 1.2;
7th step, centrifugation goes out bottom precipitation, washing, alcohol wash; 75 ~ 100 DEG C of drying 10 ~ 15h; 450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate of the present invention test is with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, reacts under 90 DEG C ~ 350 DEG C temperature conditions, and catalytic material catalyzes transformation efficiency of the oxides of nitrogen prepared by the present invention can reach 99%.
Preferably, the particle diameter of the raw material acid-dissolved titanium slag in described step one is 150 ~ 170 orders.
Preferably, in described step one, reaction temperature is 220 DEG C.
Preferably, be the sulfuric acid to leach of 10% with mass percent concentration under 80 DEG C of water-baths in described step 2.
Preferably, be 10g/min ~ 20g/min by the speed that titanium liquid is added to the water in described step 3.
Detailed description of the invention
In examples of implementation, the particle diameter of acid-dissolved titanium slag is 150 ~ 170 orders.Be 10g/min ~ 20g/min by the speed that titanium liquid is added to the water in 3rd step.But be not limited to above-mentioned feature.
Embodiment one:
The first step, it is 98% sulfuric acid 90g that 50g acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:1.8,200 DEG C of reaction 4h in closed container.
Second step, uses 200ml water extraction by the acid hydrolysate of the first step, magnetic agitation 2h under 60 DEG C of water-baths.Centrifugal, isolate top titanium liquid, remove bottom residues.
3rd step, titanium liquid and water quality are than being 4:1.Isolated for second step titanium liquid 130g is preheating to 96 DEG C, and titanium liquid is added in 33g96 DEG C of water by 15min.By solution warms to boiling.Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs.After 45min, again heat, stir, arrive boiling, and keep boiling 3h, be diluted with water, then cool after stirring 10min.
4th step, after the reactant mixture cooling of the 3rd step, centrifugal.
5th step, is dissolved in 100ml water by metatitanic acid and 8.0g manganese acetate, and 60 DEG C mix, magnetic agitation 30min.
6th step, by mixed solution 80 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid 50ml, magnetic agitation 30min.Add ammoniacal liquor 50g, hydrogen peroxide 50g, cool after magnetic agitation 30min.
7th step, centrifugation goes out bottom precipitation, washes 3 times, alcohol wash 2 times.75 DEG C of dry 15h.450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate is tested: with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, and react under 90 DEG C ~ 350 DEG C temperature conditions, denitration rate is up to 92%.
Embodiment two:
The first step, it is 98% sulfuric acid 120g that 50g acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:2.4,220 DEG C of reaction 6h in closed container.
The acid hydrolysate of the first step is that 5% sulfuric acid 200ml leaches with mass percent concentration by second step under 60 DEG C of water-baths, magnetic agitation 3h.Centrifugal, isolate top titanium liquid, remove bottom residues.
3rd step, titanium liquid and water quality are than being 4:1.Isolated for second step titanium liquid 300g is preheating to 96 DEG C, then is added in 75g 96 DEG C of water.By solution warms to boiling, boiling temperature 108 DEG C.Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs.After 45min, again heat, stir, arrive boiling, and keep boiling 3h, add the dilution of 100ml water, then cool after stirring 20min.
4th step, after the reactant mixture cooling of the 3rd step, centrifugal.
5th step, is dissolved in 100ml water by metatitanic acid and 2.0g manganese acetate, and 60 DEG C mix, magnetic agitation 30min.
6th step, by mixed solution 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid 20ml, magnetic agitation 30min.Add ammoniacal liquor 20g, drip hydrogen peroxide 15g, cool after magnetic agitation 20min.
7th step, centrifugation goes out bottom precipitation, washes 3 times, alcohol wash 2 times.90 DEG C of dry 14h.450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate is tested: with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, and react under 90 DEG C ~ 350 DEG C temperature conditions, denitration rate is up to 98%.
Embodiment three:
The first step, it is 98% sulfuric acid 150g that 50g acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:3,220 DEG C of reaction 5h in closed container.
The acid hydrolysate of the first step is that 10% sulfuric acid 400ml leaches with mass percent concentration by second step under 80 DEG C of water-baths, magnetic agitation 2h.Centrifugal, isolate top titanium liquid, remove bottom residues.
3rd step, titanium liquid and water quality are than being 4:1.Isolated for second step titanium liquid 400g is preheating to 96 DEG C, and titanium liquid is added in 100g 96 DEG C of water by 23min.By solution warms to boiling.Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs.After 45min, again heat, stir, arrive boiling, and keep boiling 3h, add the dilution of 100ml water, then cool after stirring 30min.
4th step, after the reactant mixture cooling of the 3rd step, centrifugal, washing.By the metatitanic acid after washing in 100 DEG C of dry 15h.After cooling, XRF detects, wherein TiO
287.84%, SO
311.70%, SiO
20.11%, Fe
2o
30.11%, MgO0.09%, Al
2o
30.07%, CaO0.06%, NbO0.02%.
5th step, is dissolved in 100ml water by 5g metatitanic acid and 5.44g manganese acetate, and 60 DEG C mix, magnetic agitation 30min.
6th step, by mixed solution 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid 25ml, magnetic agitation 30min.Add ammoniacal liquor 25g, to pH=10 ~ 11.Drip hydrogen peroxide 25g, cool after magnetic agitation 20min.
7th step, centrifugation goes out bottom precipitation, washes 3 times, alcohol wash 2 times.100 DEG C of dry 15h.450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate is tested: with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, and react under 90 DEG C ~ 350 DEG C temperature conditions, denitration rate is up to 98%.
Embodiment four:
The first step, it is 98% sulfuric acid 150g that 50g acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:3,220 DEG C of reaction 7h in closed container.
The acid hydrolysate of the first step is that 10% sulfuric acid 400ml leaches with mass percent concentration by second step under 60 DEG C of water-baths, magnetic agitation 3h.Centrifugal, isolate top titanium liquid, remove bottom residues.
3rd step, titanium liquid and water quality are than being 4:1.Isolated for second step titanium liquid 400g is preheating to 96 DEG C, and titanium liquid is added in 100g 96 DEG C of water by 20min.By solution warms to boiling, boiling temperature 108 DEG C.Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs.After 45min, again heat, stir, arrive boiling, and keep boiling 3h, add the dilution of 200ml water, then cool after stirring 30min.
4th step, after the reactant mixture cooling of the 3rd step, centrifugal, washing.By the metatitanic acid after washing in 100 DEG C of dry 13h.After cooling, XRF detects, wherein TiO
285.75%, SO
313.97%, SiO
20.11%, Fe
2o
30.11%, CaO0.06%.
5th step, is dissolved in 100ml water by 6g metatitanic acid and 6.37g manganese acetate, and 60 DEG C mix, magnetic agitation 30min.
6th step, by mixed solution 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid 40ml, magnetic agitation 30min.Add ammoniacal liquor, to pH=10.Drip hydrogen peroxide 10g, cool after magnetic agitation 30min.
7th step, centrifugation goes out bottom precipitation, washes 3 times, alcohol wash 2 times.100 DEG C of dry 10h.450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate is tested: with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, and react under 90 DEG C ~ 350 DEG C temperature conditions, denitration rate is up to 99%, and 150 DEG C of denitration rates can reach 90%.
Embodiment five:
The first step, it is 98% sulfuric acid 150g that 50g acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:3,220 DEG C of reaction 8h in closed container.
The acid hydrolysate of the first step is that 10% sulfuric acid 300ml leaches with mass percent concentration by second step under 80 DEG C of water-baths, magnetic agitation 3h.Centrifugal, isolate top titanium liquid, remove bottom residues.
3rd step, titanium liquid and water quality are than being 4:1.Isolated for second step titanium liquid 450g is preheating to 96 DEG C, and titanium liquid is added in 120g 96 DEG C of water by 30min.By solution warms to boiling, boiling temperature 108 DEG C.Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs.After 45min, again heat, stir, arrive boiling, and keep boiling 3h, add the dilution of 200ml water, then cool after stirring 30min.
4th step, after the reactant mixture cooling of the 3rd step, centrifugal, washing.By the metatitanic acid after washing in 100 DEG C of dry 12h.After cooling, XRF detects, wherein TiO
287.67%, SO
312.04%, MgO0.09%, Fe
2o
30.08%, CaO0.05%, SiO
20.04%.
5th step, is dissolved in 200ml water by 10g metatitanic acid and 10.80g manganese acetate, and 60 DEG C mix, magnetic agitation 30min.
6th step, by mixed solution 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid 50ml, magnetic agitation 30min.Add ammoniacal liquor 50g, to pH=10.Drip hydrogen peroxide 40g, cool after magnetic agitation 30min.
7th step, centrifugation goes out bottom precipitation, washes 3 times, alcohol wash 2 times.100 DEG C of dry 15h.450 DEG C of roasting 3h obtain catalysis material powder.
Denitration rate is tested: with NH
3during for reducing gas, by the NH of the NO of 1000ppm, 1000ppm
3, the O of 5%
2mixing, carrier gas is all N
2, gas flow rate 2000ml/min, reaction velocity is 27000h
-1.Catalysis material powder, through granulation, is got 40-60 object particle, is measured 3ml, and react under 90 DEG C ~ 350 DEG C temperature conditions, denitration rate is up to 99.7%, and 140 DEG C of denitration rates can reach 92%.
Claims (5)
1. acid-dissolved titanium slag prepares a method for manganese titanium system low-temperature denitration catalysis material, it is characterized in that comprising the following steps:
The first step, it is 98% sulfuric acid that acid-dissolved titanium slag adds mass percent concentration by solid-liquid mass ratio 1:1.8 ~ 3.0,200 ~ 220 DEG C of reaction 4 ~ 8h in closed container;
The acid hydrolysate of the first step is 5% ~ 10% sulfuric acid to leach with water or mass percent concentration by second step under 60 ~ 80 DEG C of water-baths, magnetic agitation 2 ~ 3h; Centrifugal, isolate top titanium liquid, remove bottom residues;
Isolated for second step titanium liquid is preheating to 96 DEG C by the 3rd step, then is added in 96 DEG C of water, and titanium liquid and water quality are than being 4:1; By solution warms to boiling; Solution becomes olive-green from black, when then becoming again steel grey, stops heating and stirs; After 45min, again heat, stir, arrive boiling, and keep boiling 3h, be diluted with water, then cool after stirring 10 ~ 30min;
4th step, after the reactant mixture cooling of the 3rd step, centrifugal, washing obtains metatitanic acid; By metatitanic acid in 80 ~ 120 DEG C of drying 10 ~ 15h;
5th step, metatitanic acid is water-soluble, mix with manganese acetate solution, magnetic agitation 20 ~ 30min;
6th step, by mixed solution 80 ~ 95 DEG C of water-baths of the 5th step, adds 2mol/L urea liquid, magnetic agitation 30min; Add ammoniacal liquor, to pH=10 ~ 11; Drip hydrogen peroxide, cool after magnetic agitation 30min; Wherein metatitanic acid: urea: ammoniacal liquor: the mol ratio of hydrogen peroxide is 1:0.5 ~ 2:0.5 ~ 2:0.8 ~ 1.2;
7th step, centrifugation goes out bottom precipitation, washing, alcohol wash; 75 ~ 100 DEG C of drying 10 ~ 15h; 450 DEG C of roasting 3h obtain catalysis material powder.
2. method according to claim 1, is characterized in that: the particle diameter of described step one Raw acid-dissolved titanium slag is 150 ~ 170 orders.
3. method according to claim 1, is characterized in that: in described step one, reaction temperature is 220 DEG C.
4. method according to claim 1, is characterized in that: be the sulfuric acid to leach of 10% with mass percent concentration under 80 DEG C of water-baths in described step 2.
5. method according to claim 1, is characterized in that: be 10g/min ~ 20g/min by the speed that titanium liquid is added to the water in described step 3.
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| CN104258872A (en) * | 2014-09-21 | 2015-01-07 | 北京工业大学 | Preparation method of denitration catalytic material of low-temperature wide-active-temperature-range window |
| CN105217664B (en) * | 2015-09-15 | 2017-04-12 | 中国科学院过程工程研究所 | Treating and using method for titanium-containing blast furnace slag |
| CN106944040B (en) * | 2017-03-14 | 2019-07-23 | 上海大学 | Using containing Titanium slag and the method for preparing catalyst for purification of nitrogen oxides containing manganese mud |
| CN107519862B (en) * | 2017-08-23 | 2020-02-04 | 北京工业大学 | Method for preparing medium-temperature denitration catalytic material from ferrosilicon slag |
| CN108993529A (en) * | 2018-07-26 | 2018-12-14 | 北京工业大学 | A method of improving Industrial Stoves low-temperature denitration catalysis material catalytic activity using tourmaline |
| CN112058271B (en) * | 2020-06-28 | 2023-04-18 | 重庆大学 | Method for preparing SCR (selective catalytic reduction) low-temperature flue gas denitration catalyst by acid-modified low-titanium blast furnace slag |
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| CN103263913A (en) * | 2013-04-27 | 2013-08-28 | 北京工业大学 | Preparation method for high-specific surface anti-alkalosis denitration catalyst applicable to cement kiln |
| CN103240081A (en) * | 2013-05-01 | 2013-08-14 | 北京工业大学 | Manganese-based low-temperature denitration catalyst taking TiO2-SiO2 as carrier and preparation method thereof |
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