CN106186076A - Tungstic anhydride. and the method for ammonium metavanadate is reclaimed from SCR denitration - Google Patents
Tungstic anhydride. and the method for ammonium metavanadate is reclaimed from SCR denitration Download PDFInfo
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- CN106186076A CN106186076A CN201610498651.7A CN201610498651A CN106186076A CN 106186076 A CN106186076 A CN 106186076A CN 201610498651 A CN201610498651 A CN 201610498651A CN 106186076 A CN106186076 A CN 106186076A
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- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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Abstract
The present invention relates to a kind of recovery Tungstic anhydride. and method of ammonium metavanadate from SCR denitrating catalyst, catalyst fines is made after comprising the steps: SCR denitration is pulverized, sieved, stir after mixing sodium carbonate, then mixed-powder is put into calcining in sintering furnace and becomes sintering feed, pulverize after being incubated 1 hour, sieve and make sintering feed powder, pouring warm water again into makes Na2WO4 and NaVO 3 in sintering feed powder fully dissolve, and obtains Na2WO4 and NaVO 3 mixed solution after filtering, discarding precipitation;Regulation pH value, to after 6.5 ~ 7.5, adds ammonium hydrogen carbonate or ammonium chloride solution, separates out ammonium metavanadate precipitate, first washs 23 times with dilute ammonium bicarbonate soln after filtration, then with 30% washing with alcohol 12 times, obtain ammonium metavanadate finished product after drying;Na2WO4 in surplus solution has been converted into ammonium paratungstate, surplus solution evaporation is prepared order of ammoniumparatungstate crystal, then carries out calcining prepared Tungstic anhydride..The present invention not only can reclaim ammonium metavanadate and Tungstic anhydride., decreases pollutant emission simultaneously.
Description
Technical field
The present invention relates to a kind of method reclaiming Tungstic anhydride. and ammonium metavanadate, particularly to one from SCR denitration catalyst
Agent is reclaimed Tungstic anhydride. and the method for ammonium metavanadate.
Background technology
The nitrogen oxides pollution of flue gas is on the rise at present, and country increases the dynamics forcing denitration.Denitration method for flue gas
It is divided into dry and wet two class.Wherein dry method selective catalysis reduction (is called for short SCR, Selective
CatalyticRedution), SNCR (SNCR), non-selective catalytic reduction (NSCR), electron beam, molecule
Sieve, active carbon adsorption and combined desulphurization and denitrification process etc..
In SCR denitrating technique, nitrogen oxides is reduced to harmless nitrogen and water by ammonia under the effect of catalyst:
4NO+4NH3+O2 → 4N2+6H2O ;4NH3+2NO2+O2 → 3N2+6H2O ;1NO2+1NO+ 2NH3 → 4N2+
3H2O ;Under catalyst action, there is side reaction: 2SO2+O2 → 2SO3 simultaneously;NH3+ SO3+H2O → NH4H SO4.
Side reaction is by selecting suitable catalyst and reaction condition to avoid as far as possible, in SCR denitrating technique, because employing catalyst,
Reaction generally can be carried out at temperature 300 ~ 450 DEG C.
SCR denitrating catalyst must be changed after using 3 years, and containing a certain amount of WO3 and V2O5 in catalyst, W is
Heavy metal, V2O5 is environmental poisonous substance, deals with improperly and environment all can cause the most serious pollution.Meanwhile, WO3 and V2O5
It it is the most all the raw material of expensive manufacture catalyst.Therefore WO3 and V2O5 is reclaimed, not only there is significant economy
Benefit, and there is good environmental benefit.
Summary of the invention
It is an object of the invention to, overcome problems of the prior art, it is provided that be a kind of from SCR denitrating catalyst
Reclaim Tungstic anhydride. and the method for ammonium metavanadate, WO3 and V2O5 in waste and old SCR denitrating catalyst can be reclaimed
Utilize, reduce disposal of pollutants simultaneously.
For solve above technical problem, one provided by the present invention reclaims from SCR denitrating catalyst Tungstic anhydride. with
The method of ammonium metavanadate, in turn includes the following steps: (1) by containing WO3 and V2O5 waste and old SCR denitrating catalyst pulverize,
After sieving, making the catalyst fines of 150-180 mesh, the percentage by weight of WO3 described in catalyst fines is 5% ~ 7%, institute
The percentage by weight stating V2O5 is 3% ~ 4%;(2) in above-mentioned catalyst fines, mix the sodium carbonate of 150-180 mesh, carbonic acid
The incorporation weight ratio of sodium is catalyst fines: sodium carbonate=100: (20 ~ 30), stir after incorporation become catalyst and
Sodium carbonate mixed-powder;(3) above-mentioned catalyst and sodium carbonate mixed-powder are put in sintering furnace, with intensification per minute 10 DEG C ~
The speed of 15 DEG C be warming up to 800 DEG C of WO3, V2O5 made in sintering feed, catalyst and sodium carbonate mixed-powder and
Na2CO3 is converted into Na2WO4 and NaVO3 in sintering feed, after described sintering feed is incubated 1 hour, with cooling 10 per minute
DEG C ~ speed of 15 DEG C is cooled to 20 DEG C ~ 30 DEG C;(4) above-mentioned sintering feed is pulverized, sieved, make the sintering of 200-250 mesh
Material powder, then in sintering feed powder, pour the warm water of 30 DEG C-45 DEG C into, weight ratio is sintering feed powder: warm water=1: (2 ~ 3),
It is continuously agitated, makes Na2WO4 and NaVO3 contained in sintering feed powder fully dissolve, obtain after filtering, discarding precipitation
The mixed solution of Na2WO4 and NaVO3;(5) add ammonia the pH value of Na2WO4 and NaVO3 mixed solution to be regulated extremely
After 6.5 ~ 7.5, adding precipitant and make temperature control at 25 DEG C~28 DEG C in mixed solution, weight ratio is mixed solution:
Precipitant=1: (0.3 ~ 0.4), precipitation ammonium metavanadate precipitate stirring while adding, after filtration, is first the carbonic acid of 5% by weight concentration
Hydrogen ammonium salt solution washing precipitate 2-3 time, then with 30% washing with alcohol precipitate 1-2 time, after drying ammonium metavanadate becomes
Product;(6) in the surplus solution after extracting ammonium metavanadate, Na2WO4 has been converted into ammonium paratungstate, is added by described surplus solution
Heat is evaporated preparing order of ammoniumparatungstate crystal to 100 DEG C, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, and prepares three
Tungsten oxide.
Relative to prior art, the present invention achieves following beneficial effect: containing WO3 in waste and old SCR denitrating catalyst
And V2O5, it being sintered after mixing sodium carbonate, WO3 and V2O5 reacts with sodium carbonate respectively, WO3+Na2CO3 →
Na2WO4+CO2 ↑ ;V2O5+Na2CO3 → 2NaVO3+CO2 ↑, generate Na2WO4 and NaVO3, after adding warm water dissolving
Obtain the mixed solution of Na2WO4 and NaVO3, after adjusting pH value, add precipitant, complete to ammonium metavanadate precipitate, 2NaVO3
+ 2NH4HCO3 → 2NH4VO3 ↓ + Na2CO3+ H2O+ CO2 ↑ ;Or NaVO3+ NH4Cl → NH4VO3 ↓+
NaCl ;Precipitate is washed with dilute ammonium bicarbonate soln, then the washing with alcohol with 30%, obtain ammonium metavanadate finished product after drying;?
Extracting in the surplus solution after ammonium metavanadate, Na2WO4 has been converted into ammonium paratungstate, Na2WO4+2NH4HCO3 → (NH4)
2WO4+2NaHCO3, or Na2WO4+2NH4Cl → (NH4) 2WO4+2NaCl, re-evaporation prepares order of ammoniumparatungstate crystal, then forges
Fire to obtain Tungstic anhydride., (NH4) 2WO4 → WO3+ 2NH3 ↑+H2O ↑;By the method for the present invention not only from waste and old
SCR denitrating catalyst reclaims ammonium metavanadate and Tungstic anhydride., has obtained good economic benefit, decrease heavy metal W simultaneously
And the discharge of environmental poisonous substance V2O5, obtain good environmental benefit.
As the preferred version of the present invention, described precipitant be weight concentration be the ammonium bicarbonate soln of 20% ~ 30%, or
Person is 20% ~ 30% ammonium chloride solution for weight concentration.
As the preferred version of the present invention, in turn include the following steps: (1) is by the waste and old SCR containing WO3 and V2O5
Denitrating catalyst pulverize, sieve after, make the catalyst fines of 150-180 mesh, the weight hundred of WO3 described in catalyst fines
Proportion by subtraction is 5%, and the percentage by weight of described V2O5 is 3%;(2) in above-mentioned catalyst fines, mix the carbonic acid of 150-180 mesh
Sodium, the incorporation weight ratio of sodium carbonate is catalyst fines: sodium carbonate=100: 20, stirs and become catalyst after incorporation
With sodium carbonate mixed-powder;(3) above-mentioned catalyst and sodium carbonate mixed-powder are put in sintering furnace, with intensification per minute 10 DEG C
Speed be warming up to 800 DEG C of WO3, V2O5 and Na2CO3 made in sintering feed, catalyst and sodium carbonate mixed-powder
Na2WO4 and NaVO3 being converted in sintering feed, after described sintering feed is incubated 1 hour, with the speed of cooling per minute 10 DEG C
It is cooled to 20 DEG C;(4) above-mentioned sintering feed is pulverized, sieved, make the sintering feed powder of 200-250 mesh, then to sintered material powder
Pouring the warm water of 30 DEG C in end into, weight ratio is sintering feed powder: warm water=1: 2, is continuously agitated, and makes to contain in sintering feed powder
Na2WO4 and NaVO3 fully dissolve, after filtering, discarding precipitation, obtain the mixed solution of Na2WO4 and NaVO3;(5)
Add ammonia the pH value of Na2WO4 and NaVO3 mixed solution to be regulated after 6.5, in mixed solution, add weight concentration
Be 20% ammonium bicarbonate soln as precipitant and make reaction temperature control at 25 DEG C, weight ratio is mixed solution: ammonium hydrogen carbonate
Solution=1: 0.3, precipitation ammonium metavanadate precipitate stirring while adding, after filtration, is first the ammonium bicarbonate soln of 5% by weight concentration
Washing precipitate 2 times, then with 30% washing with alcohol precipitate 1 time, after drying ammonium metavanadate finished product;(6) extracting
Crossing in the surplus solution after ammonium metavanadate, Na2WO4 has been converted into ammonium paratungstate, described surplus solution is heated to 100 DEG C and enters
Row evaporation prepares order of ammoniumparatungstate crystal, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, and prepares Tungstic anhydride..
As the preferred version of the present invention, in turn include the following steps: (1) is by the waste and old SCR containing WO3 and V2O5
Denitrating catalyst pulverize, sieve after, make the catalyst fines of 150-180 mesh, the weight hundred of WO3 described in catalyst fines
Proportion by subtraction is 7%, and the percentage by weight of described V2O5 is 4%;(2) in above-mentioned catalyst fines, mix the carbonic acid of 150-180 mesh
Sodium, the incorporation weight ratio of sodium carbonate is catalyst fines: sodium carbonate=100: 30, stirs and become catalyst after incorporation
With sodium carbonate mixed-powder;(3) above-mentioned catalyst and sodium carbonate mixed-powder are put in sintering furnace, with intensification per minute 15 DEG C
Speed be warming up to 800 DEG C of WO3, V2O5 and Na2CO3 made in sintering feed, catalyst and sodium carbonate mixed-powder
Na2WO4 and NaVO3 being converted in sintering feed, after described sintering feed is incubated 1 hour, with the speed of cooling per minute 15 DEG C
It is cooled to 30 DEG C;(4) above-mentioned sintering feed is pulverized, sieved, make the sintering feed powder of 200-250 mesh, then to sintered material powder
Pouring the warm water of 45 DEG C in end into, weight ratio is sintering feed powder: warm water=1: 3, is continuously agitated, and makes to contain in sintering feed powder
Na2WO4 and NaVO3 fully dissolve, after filtering, discarding precipitation, obtain the mixed solution of Na2WO4 and NaVO3;(5)
Add ammonia the pH value of Na2WO4 and NaVO3 mixed solution to be regulated after 7.5, in mixed solution, add weight concentration
Be 30% ammonium bicarbonate soln as precipitant and make reaction temperature control at 28 DEG C, weight ratio is mixed solution: ammonium hydrogen carbonate
Solution=1: 0.4, precipitation ammonium metavanadate precipitate stirring while adding, after filtration, is first the ammonium bicarbonate soln of 5% by weight concentration
Washing precipitate 3 times, then with 30% washing with alcohol precipitate 2 times, after drying ammonium metavanadate finished product;(6) extracting
Crossing in the surplus solution after ammonium metavanadate, Na2WO4 has been converted into ammonium paratungstate, described surplus solution is heated to 100 DEG C and enters
Row evaporation prepares order of ammoniumparatungstate crystal, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, and prepares Tungstic anhydride..
Detailed description of the invention
Embodiment one
Embodiment one reclaims the method for Tungstic anhydride. and ammonium metavanadate from SCR denitrating catalyst and in turn includes the following steps:
(1), after the waste and old SCR denitrating catalyst containing WO3 and V2O5 being pulverized, sieved, the catalyst powder of 150-180 mesh is made
End, in catalyst fines, the percentage by weight of WO3 is 5%, and the percentage by weight of V2O5 is 3%;(2) to above-mentioned catalyst powder
Mixing the sodium carbonate of 150-180 mesh in end, the incorporation weight ratio of sodium carbonate is catalyst fines: sodium carbonate=100: 20, mixes
After stir and become catalyst and sodium carbonate mixed-powder;(3) above-mentioned catalyst and sodium carbonate mixed-powder are put into
In sintering furnace, it is warming up to 800 DEG C with the speed of intensification per minute 10 DEG C and makes sintering feed, catalyst and sodium carbonate mixed powder
WO3, V2O5 and Na2CO3 in end is converted into Na2WO4 and NaVO3 in sintering feed, WO3+Na2CO3 → Na2WO4+
CO2 ↑ ;V2O5+Na2CO3 → 2NaVO3+CO2 ↑, after sintering feed is incubated 1 hour, with the speed of cooling per minute 10 DEG C
It is cooled to 20 DEG C;
(4) above-mentioned sintering feed is pulverized, sieved, make the sintering feed powder of 200-250 mesh, then pour in sintering feed powder
The warm water of 30 DEG C, weight ratio is sintering feed powder: warm water=1: 2, is continuously agitated, and makes the Na2WO4 contained in sintering feed powder
Fully dissolve with NaVO3, after filtering, discarding precipitation, obtain the mixed solution of Na2WO4 and NaVO3;(5) ammonia is added
The pH value of Na2WO4 and NaVO3 mixed solution being regulated after 6.5, adding weight concentration in mixed solution is 20%
Ammonium bicarbonate soln is as precipitant and makes reaction temperature control at 25 DEG C, and weight ratio is mixed solution: ammonium bicarbonate soln=1
: 0.3, precipitation ammonium metavanadate precipitate stirring while adding, 2NaVO3+ 2NH4HCO3 → 2NH4VO3 ↓+Na2CO3+ H2O+
After CO2 ↑ filtration, first with the ammonium bicarbonate soln washing precipitate that weight concentration is 5% 2 times, then with 30% washing with alcohol
Precipitate 1 time, obtains ammonium metavanadate finished product after drying;(6) in the surplus solution after extracting ammonium metavanadate, Na2WO4+
2NH4HCO3 → (NH4) 2WO4+2NaHCO3, Na2WO4 has been converted into ammonium paratungstate, surplus solution is heated to 100 DEG C and enters
Row evaporation prepares order of ammoniumparatungstate crystal, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, and prepares Tungstic anhydride.,
(NH4)2WO4 → WO3+ 2NH3 ↑ +H2O ↑。
Embodiment two
Embodiment two reclaims Tungstic anhydride. and the method for ammonium metavanadate from SCR denitrating catalyst, in turn includes the following steps:
(1), after the waste and old SCR denitrating catalyst containing WO3 and V2O5 being pulverized, sieved, the catalysis of 150-180 mesh is made
Agent powder, in catalyst fines, the percentage by weight of WO3 is 7%, and the percentage by weight of V2O5 is 4%;(2) to above-mentioned catalysis
Mixing the sodium carbonate of 150-180 mesh in agent powder, the incorporation weight ratio of sodium carbonate is catalyst fines: sodium carbonate=100: 30,
Stir after incorporation and become catalyst and sodium carbonate mixed-powder;(3) by above-mentioned catalyst and sodium carbonate mixed-powder
Putting in sintering furnace, being warming up to 800 DEG C with the speed of intensification per minute 15 DEG C, to make sintering feed, catalyst and sodium carbonate mixed
Na2WO4 and NaVO3, WO3+Na2CO3 that WO3, V2O5 and Na2CO3 in conjunction powder is converted in sintering feed →
Na2WO4+CO2 ↑ ;V2O5+Na2CO3 → 2NaVO3+CO2 ↑, after sintering feed is incubated 1 hour, with cooling 15 per minute
DEG C speed be cooled to 30 DEG C;(4) above-mentioned sintering feed is pulverized, sieved, make the sintering feed powder of 200-250 mesh, then to burning
Pouring the warm water of 45 DEG C in ramming material powder into, weight ratio is sintering feed powder: warm water=1: 3, is continuously agitated, and makes sintering feed powder
In Na2WO4 and NaVO3 that contain fully dissolve, the mixing obtaining Na2WO4 and NaVO3 after filtering, discarding precipitation is molten
Liquid;(5) add ammonia the pH value of Na2WO4 and NaVO3 mixed solution to be regulated after 7.5, in mixed solution, add weight
Measuring the ammonium bicarbonate soln that concentration is 30% as precipitant and makes reaction temperature control at 28 DEG C, and weight ratio is mixed solution:
Ammonium bicarbonate soln=1: 0.4, precipitation ammonium metavanadate precipitate stirring while adding, 2NaVO3+ 2NH4HCO3 → 2NH4VO3 ↓+
After Na2CO3+ H2O+ CO2 ↑ filtration, first with the ammonium bicarbonate soln washing precipitate that weight concentration is 5% 3 times, then use
The washing with alcohol precipitate of 30% 2 times, obtains ammonium metavanadate finished product after drying;(6) surplus solution after extracting ammonium metavanadate
In, Na2WO4+2NH4HCO3 → (NH4) 2WO4+2NaHCO3, Na2WO4 has been converted into ammonium paratungstate, is added by surplus solution
Heat is evaporated preparing order of ammoniumparatungstate crystal to 100 DEG C, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, and prepares three
Tungsten oxide, (NH4) 2WO4 → WO3+ 2NH3 ↑+H2O ↑.These are only the preferable possible embodiments of the present invention, non-
Therefore the scope of patent protection of the present invention is limited to.
In addition to the implementation, the present invention can also have other embodiments.All employing equivalents or equivalent transformation shape
The technical scheme become, all falls within the protection domain of application claims.
Claims (1)
1. one kind is reclaimed Tungstic anhydride. and the method for ammonium metavanadate from SCR denitrating catalyst, it is characterised in that include successively
Following steps: after the waste and old SCR denitrating catalyst containing WO3 and V2O5 is pulverized, sieved by (1), make 150-180 purpose
Catalyst fines, the percentage by weight of WO3 described in catalyst fines is 5% ~ 7%, the percentage by weight of described V2O5 is 3% ~
4% ;(2) mixing the sodium carbonate of 150-180 mesh in above-mentioned catalyst fines, the incorporation weight ratio of sodium carbonate is catalyst powder
End: sodium carbonate=100: (20 ~ 30), stirs after incorporation and becomes catalyst and sodium carbonate mixed-powder;(3) by above-mentioned
Catalyst and sodium carbonate mixed-powder are put in sintering furnace, are warming up to 800 DEG C with the speed of intensification per minute 10 DEG C ~ 15 DEG C and make
WO3, V2O5 and Na2CO3 of becoming in sintering feed, catalyst and sodium carbonate mixed-powder be converted in sintering feed
Na2WO4 and NaVO3, after described sintering feed is incubated 1 hour, is cooled to 20 DEG C with the speed of cooling per minute 10 DEG C ~ 15 DEG C
~30℃;(4) above-mentioned sintering feed is pulverized, sieved, make the sintering feed powder of 200-250 mesh, then fall in sintering feed powder
Entering the warm water of 30 DEG C-45 DEG C, weight ratio is sintering feed powder: warm water=1: (2 ~ 3), is continuously agitated, and makes in sintering feed powder
Na2WO4 and NaVO3 contained fully dissolves, and obtains the mixed solution of Na2WO4 and NaVO3 after filtering, discarding precipitation;
(5) add ammonia the pH value of Na2WO4 and NaVO3 mixed solution to be regulated after 6.5 ~ 7.5, add in mixed solution
Precipitant also makes temperature control at 25 DEG C~28 DEG C, and weight ratio is mixed solution: precipitant=1: (0.3 ~ 0.4), and limit edged stirs
Mix precipitation ammonium metavanadate precipitate, after filtration, first with the ammonium bicarbonate soln washing precipitate that weight concentration is 5% 2-3 time, connect
Washing with alcohol precipitate 1-2 time with 30%, after drying ammonium metavanadate finished product;(6) remaining after extracting ammonium metavanadate
In remaining solution, Na2WO4 has been converted into ammonium paratungstate, described surplus solution is heated to 100 DEG C and is evaporated preparing para-tungstic acid
Ammonium crystal, then order of ammoniumparatungstate crystal is heated to 700 DEG C calcines, prepare Tungstic anhydride..
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109252048A (en) * | 2018-10-19 | 2019-01-22 | 天津大学 | A method of recycling Titanium, tungsten, vanadium from useless SCR denitration |
CN113046562A (en) * | 2021-03-08 | 2021-06-29 | 北京华电光大环境股份有限公司 | Method for recovering tungsten element in waste catalyst |
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CN102557142A (en) * | 2012-02-16 | 2012-07-11 | 江苏万德电力环保有限公司 | Method for recovering tungsten trioxide and ammonium metavanadate from selective catalytic reduction (SCR) denitration catalyst |
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- 2016-06-30 CN CN201610498651.7A patent/CN106186076A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102557142A (en) * | 2012-02-16 | 2012-07-11 | 江苏万德电力环保有限公司 | Method for recovering tungsten trioxide and ammonium metavanadate from selective catalytic reduction (SCR) denitration catalyst |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109252048A (en) * | 2018-10-19 | 2019-01-22 | 天津大学 | A method of recycling Titanium, tungsten, vanadium from useless SCR denitration |
CN113046562A (en) * | 2021-03-08 | 2021-06-29 | 北京华电光大环境股份有限公司 | Method for recovering tungsten element in waste catalyst |
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Application publication date: 20161207 |