CN102921403B - Method for preparing V2O5-WO3/TiO2 powder for making denitration catalyst - Google Patents

Method for preparing V2O5-WO3/TiO2 powder for making denitration catalyst Download PDF

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CN102921403B
CN102921403B CN201210331981.9A CN201210331981A CN102921403B CN 102921403 B CN102921403 B CN 102921403B CN 201210331981 A CN201210331981 A CN 201210331981A CN 102921403 B CN102921403 B CN 102921403B
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dissolving
filter cake
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maceration extract
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CN102921403A (en
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陈建立
豆君
孙亮
邱巧锐
赵海娟
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Longbai Group Co.,Ltd.
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HENAN BAILILIAN CHEMICAL CO Ltd
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Abstract

The invention discloses a V2O5-WO3/TiO2powder for making a denitration catalyst, which comprises the following steps of: 1) making metatitanic acid into pulp at a concentration of 280 to 320g/L based on TiO2, heating the pulp to 60 DEG C, regulating the pH value to 5.0 with caustic soda, regulating the pH value to 5.5 to 5.7 with ammonia water, and filtering the pulp by pressure and washing the filter cake by water; 2) preparing an impregnation solution; 3) making the filter cake made by the step 1) into pulp at a concentration of 280 to 320g/L based on TiO2, heating to 60 DEG C, adding the pulp into the impregnation solution obtained by the step 2), stirring the mixture for 2 to 4 hours, and filtering the solution by pressure; 4) calcining the filter cake obtained by the step 3) at 400 to 550 DEG C for 2 to 5h; and 5) crushing the calcined material obtained by the step 4).

Description

A kind of denitrating catalyst V 2o 5-WO 3/ TiO 2the preparation method of powder
Technical field
The present invention relates to a kind of denitrating catalyst V 2o 5-WO 3/ TiO 2the preparation method of powder.
Background technology
The flue gas that coal combustion generates is the nitrogen oxide as leading take nitric oxide and nitrogen dioxide, and it is the major reason that forms photochemical fog and acid rain, is also a kind of important greenhouse gases simultaneously.So, in by the end of July, 2011 country put into effect " thermal power plant's air pollution emission standard ", after this standard-required 2012, the nitrogen oxide emission of all newly-built fired power generating unit must not exceed 100mg/m 3, after 2014, the nitrogen oxide emission of all fired power generating unit of key area must not exceed 100mg/m 3, non-key area must not exceed 200mg/m 3, therefore, it is the instant task of environmental protection that the denitration of flue gas is administered.SCR(SCR) gas denitrifying technology is the effective technology of the solution Pollution Index in Air Nitric Oxides that generally adopts in the world at present.Under the effect of catalyst, by the reducing agent such as ammonia, urea, nitrous oxides selectivity harmful in flue gas is catalysed and reduced into clean harmless nitrogen G&W, its denitration efficiency can reach more than 90%.The key of this technology and core are exactly denitrating catalyst.
Denitrating catalyst is take nano titanium oxide as carrier, and active component vanadic anhydride and co-catalyst tungstic acid in load, reported many about WO at present 3-TiO 2the preparation of composite granule, but about V 2o 5-WO 3/ TiO 2composite granule also rarely have report.This vanadium titanium tungsten composite powder is by active component V 2o 5with the even combination of carrier, avoid adding the inhomogeneous phenomenon of fashionable mixing at moulding process in advance, can bring into play better V 2o 5catalytic activity.
Summary of the invention
The object of the invention is to provide a kind of denitrating catalyst V 2o 5-WO 3/ TiO 2the preparation method of powder.
Technical scheme of the present invention is: a kind of denitrating catalyst V 2o 5-WO 3/ TiO 2the preparation method of powder, draws together following steps:
1) metatitanic acid is made to slurries, concentration is with TiO 2count 250-350g/L, be heated to 60 ℃, regulate its pH value to 4.0-5.0 with caustic soda, then regulate pH value to 5.0-6.0 with ammoniacal liquor, then filter-press water-washing;
2) prepare maceration extract: oxalic acid is joined in 60 ℃ of water, stirring is dissolved oxalic acid completely, then adds ammonium metatungstate, stirs and after ammonium metatungstate dissolves completely, slowly adds ammonium metavanadate again, all add after dissolving and leave standstill and be aged to color and no longer change, ammonium metavanadate addition V 2o 5/ TiO 2=0.8-1.2: 88-94, ammonium metatungstate addition WO 3/ TiO 2=5-10: 88-94, oxalic acid addition is 3 times of ammonium metavanadate quality;
3) filter cake making beating step 1) being obtained, concentration is with TiO 2count 250-350g/L, be heated to 60 ℃, then add step 2) maceration extract that obtains, stirs press filtration after 2 ~ 4h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 2-5h of 400-550 ℃;
5) calcining material step 4) being obtained is pulverized.
Further, the intermediate product that the metatitanic acid of step 1) is Titanium White Production By Sulfuric Acid Process.
Further, the filtrate that step 3) obtains is for step 2) prepare maceration extract.
The present invention uses NaOH to replace most of ammoniacal liquor, first regulate metatitanic acid slip pH to 4.0-5.0 with NaOH, be adjusted to 5.0-6.0 with a small amount of ammoniacal liquor again, and then washing is to remove sulfate radical free in filter cake and sodium ion, the method can reduce the consumption of ammonia, reduce the ammonia-nitrogen content in waste water, met the requirement of cleaner production.
Then adopt the method for dipping the predecessor of vanadium tungsten to be combined with metatitanic acid simultaneously, after calcining, vanadium tungsten component is just combined in titanium dioxide surface equably, powder prepared by the method has good denitration performance, under the condition of flue gas condition 100%, denitration rate when temperature window is 320-400 ℃ can reach more than 95%.
And after adopting dipping, press filtration dewatering process is easy and simple to handle compared to evaporation drying mode, is easy to large-scale production, has reduced energy consumption, the vanadium tungsten component simultaneously containing in filtrate can recycle in the time of preparation maceration extract, has reduced the waste of raw material.
The specific embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 250g/L, in the time of 60 ℃, regulate its pH value to 4.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.0, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 10.5kg oxalic acid, join 23.5L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 14.6kg, after stirring and dissolving, slowly add the ammonium metavanadate of 3.49kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 250g/L, the maceration extract that adds step 2 to prepare in the time of 60 ℃, press filtration after stirring 2h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 5h of 400 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 2
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 280g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.6, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 11.9kg oxalic acid, join 26.7L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 19.8kg, after stirring and dissolving, slowly add the ammonium metavanadate of 3.95kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 280g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 3h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 3h of 500 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 3
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 280g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.7, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 12.0kg oxalic acid, join 26.9L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 23.4kg, after stirring and dissolving, slowly add the ammonium metavanadate of 4.00kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 280g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 4h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 5h of 450 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 4
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 300g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.5, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 15.8kg oxalic acid, join 35.4L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 17.5kg, after stirring and dissolving, slowly add the ammonium metavanadate of 5.25kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 300g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 2h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 2h of 550 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 5
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 300g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.6, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 15.9kg oxalic acid, join 35.8L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 21.2kg, after stirring and dissolving, slowly add the ammonium metavanadate of 5.31kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 300g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 3h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 2h of 500 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 6
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 300g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.7, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 16.1kg oxalic acid, join 36.2L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 25.0kg, after stirring and dissolving, slowly add the ammonium metavanadate of 5.36kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 300g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 4h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 4h of 450 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 7
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 320g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.5, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 20.2kg oxalic acid, join 45.4L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 18.6kg, after stirring and dissolving, slowly add the ammonium metavanadate of 6.73kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 320g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 2h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 3h of 500 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 8
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 320g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.6, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 20.4kg oxalic acid, join 45.9L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 22.6kg, after stirring and dissolving, slowly add the ammonium metavanadate of 6.81kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 320g/L, the maceration extract that adds step 2 to prepare in the time of 60 ℃, press filtration after stirring 3h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 5h of 450 ℃;
5) calcining material step 4) being obtained is pulverized.
Embodiment 9
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 350g/L, in the time of 60 ℃, regulate its pH value to 5.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 6.0, regulated rear filter-press water-washing.
2) preparation of maceration extract, take 23.3kg oxalic acid, join 52.5L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 42.9kg, after stirring and dissolving, slowly add the ammonium metavanadate of 7.78kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas.
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 350g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 4h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 2h of 550 ℃;
5) calcining material step 4) being obtained is pulverized.
Above embodiment is only that the technical scheme that the present invention is recorded illustrates, and all simple distortion of making in the situation that not departing from core of the present invention or modification all fall into protection scope of the present invention.

Claims (2)

1. a denitrating catalyst V 2o 5-WO 3/ TiO 2the preparation method of powder, is characterized in that, the method comprises the following steps:
1) the intermediate product metatitanic acid of Titanium White Production By Sulfuric Acid Process is made to slurries 500L, concentration is with TiO 2count 250g/L, in the time of 60 ℃, regulate its pH value to 4.0 with caustic soda, then by ammoniacal liquor adjusting pH value to 5.0, regulated rear filter-press water-washing;
2) preparation of maceration extract, take 10.5kg oxalic acid, join 23.5L, in the water of 60 ℃, after dissolving completely, add the ammonium metatungstate of 14.6kg, after stirring and dissolving, slowly add the ammonium metavanadate of 3.49kg again, leave standstill and be aged to color and no longer change and stablize after all dissolving, this process can be produced a large amount of gas;
3) step 1) is washed to the filter cake making beating obtaining for concentration is with TiO 2the slurries 500L of meter 250g/L adds step 2 in the time of 60 ℃) maceration extract for preparing, stirs press filtration after 2h;
4) filter cake step 3) being obtained is at the lower calcining of the temperature 5h of 400 ℃;
5) calcining material step 4) being obtained is pulverized.
2. a kind of denitrating catalyst V according to claim 1 2o 5-WO 3/ TiO 2the preparation method of powder, is characterized in that, the filtrate that step 3) obtains is for step 2) prepare maceration extract.
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CN105478133B (en) * 2015-12-11 2017-09-29 福建工程学院 A kind of low cost SCR denitration catalyst and preparation method thereof
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