CN107497416A - A kind of recovery method for inactivating vanadium titanium tungsten system denitrating catalyst - Google Patents
A kind of recovery method for inactivating vanadium titanium tungsten system denitrating catalyst Download PDFInfo
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- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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Abstract
A kind of recycling method of waste and old vanadium titanium tungsten system denitrating catalyst, comprises the following steps, (1) pretreatment；(2) vanadium is reclaimed：After above-mentioned pretreatment catalyst is activated, it is impregnated in sodium bicarbonate solution, adds potassium chlorate, handle to obtain vanadic anhydride；(3) calcification, pickling；(4) recovery Pd：Above-mentioned filtrate is adjusted to alkalescent, adds MgCl2, stirring, filter to obtain TiO2；(5) denitrating catalyst regeneration is inactivated：Above-mentioned filtrate adds oxysalt, obtains regenerative mixed solution, and inactivation denitrating catalyst is immersed in above-mentioned regenerative mixed solution, dries, roasting, inactivation denitrating catalyst regeneration.Compared with prior art, the present invention has advantages below：Reclaim vanadic anhydride and titanium dioxide, the filtrate in removal process adds oxysalt and is prepared into new inactivation denitrating catalyst cleaning fluid, so as to realize spent catalyst active ingredient and clean the recycling of raffinate.
Description
Technical field
The present invention relates to waste flue gas denitration field, and in particular to a kind of recovery side for inactivating vanadium titanium tungsten system denitrating catalyst
Method.
Background technology
SCR (SCR) is the most important denitration technology of the current coal fired power plant in China, and catalyst is SCR system
Important component, its performance directly affects the denitration efficiency of SCR system.The main component of SCR catalyst is TiO at present2、
V2O5、WO3、MoO3.The current coal-fired plant flue gas denitration engineering in China is all using high-temperature high dust arrangement, waste flue gas denitration catalyst
During use due to the continuous erosion of the dust in flue gas, can cause catalyst blockage of the micro orifice or alkali metal, alkaline-earth metal,
The deactivation phenomenom of the poisonings such as arsenic, although the catalyst of inactivation can realize regeneration, the catalysis of regeneration by certain mode
Agent activity is decreased obviously, and certain access times be present, thus the decaying catalyst that final or presence can not recycle, but
It is that vanadic anhydride in catalyst, tungstic acid, titanium dioxide etc. can pollute to environment, the conventional processing of factory at present
Recovery method has washing regeneration, acid solution processing regeneration.
Wherein method for washing can wash away catalyst surface harmful constituent, single catalysis group that may also wash away catalyst simultaneously
Point, the effect of washing depends on the property of the intensity and catalyst of washing in itself；The effect of pickling is preferable, but useless after pickling
Therefore liquid discharge can produce new environmental problem again, need one kind effectively to recycle waste and old denitrating catalyst again at present
Can not be to the recovery method of environmental danger.
The content of the invention
In view of the above-mentioned problems, the present invention provides a kind of recycling method of waste and old vanadium titanium tungsten system denitrating catalyst, can
Effectively to reclaim the active ingredient in catalyst, while environment is not impacted.
The present invention is that by the following technical programs, solve above-mentioned technical problem：
A kind of recycling method of waste and old vanadium titanium tungsten system denitrating catalyst, comprises the following steps：
1) pre-process：The inactivation denitrating catalyst of regeneration be will be unable to successively by soot blowing, high pressure water washing, drying, crushing
Inactivation denitrating catalyst must be pre-processed；
2) vanadium is reclaimed：After above-mentioned pretreatment is inactivated into denitrating catalyst high-temperature activation, it is impregnated in sodium bicarbonate solution, adds
Enter potassium chlorate, handle to obtain vanadic anhydride；
3) calcification baking, pickling：Filtrate is dried in step (2), adds calcium carbonate, calcining, adds acid solution processing；
4) recovery Pd：Filtrate in step (3) is adjusted to alkalescent, MgCl2 is added, stirring, filters to obtain TiO2；
5) denitrating catalyst regeneration is inactivated：Filtrate adds oxysalt in step (4), obtains regenerative mixed solution, will inactivate
Denitrating catalyst is immersed in above-mentioned regenerative mixed solution, is dried, roasting, inactivation denitrating catalyst regeneration.
Further, in step (2), the sintering temperature of high-temperature activation is 300~400 DEG C, and roasting time is 3~5h；Carbonic acid
The concentration of hydrogen sodium solution is 0.1~0.5mol/L；The concentration of potassium chlorate is 0.1~0.8mol/L；Handle to pass through filtering successively,
200~300 DEG C of 3~5h of calcining.
Further, in step (3), filtrate drying temperature is 70~110 DEG C, and crushed after being dried to granularity is 200~400
Mesh；The amount for adding calcium carbonate is the 20%~50% of pulverized particles quality；Calcining heat is that 3~6h is calcined at 700~1100 DEG C.
Further, in step (3), crushed after calcining；Acid solution is the sulfuric acid or hydrochloric acid that mass fraction is 5%~10%
Solution, it is 2 to add quality with powder quality ratio:1~5:1；Handle as 60~90 DEG C of 3~6h of stirring in water bath.
Further, in step (3), after stirring in water bath, it is 1~100g/L to add deionized water and adjust to tungsten concentration.
Further, add ammoniacal liquor in step (4), in solution and be adjusted to PH=8~11；MgCl2 addition is in step (3)
The 1%~5% of powder after calcining；Stir 2~5h, filtered filtration residue deionized water rinsing.
Further, in step (4), oxysalt be antimony acetate, ammonium heptamolybdate, cerous nitrate, lanthanum nitrate and niobium oxalate in extremely
Few one or more mixing.
Further, in step (5), the ratio that oxysalt accounts for the filtrate is：10%~50%.
Further, in step (5), the catalyst for immersing mixed solution is placed in drying box, programming rate be 5~10 DEG C/
Min, drying temperature are 80~105 DEG C, and drying time is 2~4h.
Further, in step (5), to dry rear catalyst and be placed in roasting in Muffle furnace, programming rate is 4~10 DEG C/min,
400~600 DEG C are warming up to, 3~8h is incubated, cools to room temperature with the furnace.
Compared with prior art, the advantage of the invention is that：Waste and old vanadium titanium tungsten system denitrating catalyst is reclaimed again sharp
With reclaiming vanadic anhydride and titanium dioxide, the filtrate in removal process adds oxysalt and is prepared into new inactivation denitration
Catalyst wash liquid, so as to realize spent catalyst active ingredient and clean the recycling of raffinate.
Embodiment
The invention is further illustrated by the following examples, but the present invention is not limited only to following examples.
Embodiment 1
(1) pre-process：By waste and old denitrating catalyst block using high pressure airgun purging surface and duct, then pass through
Denitrating catalyst block duct is swept in giant spray, is placed in air dry oven and is dried, and drying temperature is 80 DEG C, dries 4h；Take
Crushed after going out, inactivation denitrating catalyst must be pre-processed.
(2) vanadium is reclaimed：By the catalyst of above-mentioned pretreatment after 300 DEG C of high-temperature activation 5h, 0.1mol/L carbonic acid is impregnated in
In hydrogen sodium solution, 0.8mol/L strong oxidizer potassium chlorate is added, agitating solution, adding ammonium chloride makes vanadium be sunk in the form of ammonium metavanadate
Form sediment, filtering, 90 DEG C of dry 3h, 200 DEG C of calcining 4h, obtain vanadic anhydride.
(3) calcification：By 70 DEG C of dry 3h of filtrate in step (2), crushed after being dried to granularity is 200 mesh, adds calcium carbonate
It is well mixed, wherein the quality for adding calcium carbonate accounts for the 20% of mixture gross mass, 700 DEG C of calcining 4h；
Pickling：Above-mentioned burnt solid matter is crushed, it is 1 to add with the mass ratio of powder:2 mass fraction is
5% dilution heat of sulfuric acid, 90 DEG C of stirring in water bath 3h, deionized water is added, the concentration for adjusting tungsten is 1~100g/L.
(4) recovery Pd：Pickling liquid in step (3) is added into ammoniacal liquor, adjusts solution PH=8, is well mixed and adds
MgCl2, wherein the quality for adding MgCl2 is 1% of calcining powder quality in step (3), 2h is stirred, filtering, obtains TiO2.
(5) denitrating catalyst regeneration is inactivated：The vinegar that mass fraction is 10% is separately added into filtrate into above-mentioned steps (4)
Sour antimony, 5% ammonium heptamolybdate, 10% cerous nitrate, 3% lanthanum nitrate and 8% niobium oxalate, the denitrating catalyst of inactivation is soaked
Enter in above-mentioned solution, soak 2h, taking-up is placed in drying box is warming up to 80 DEG C with 5 DEG C/min, dries 3h；
Above-mentioned dry catalyst is placed in Muffle kiln roasting, with 4 DEG C/min, is warming up to 400 DEG C, is incubated 5h, it is cold with stove
But to room temperature, regeneration denitrating catalyst is obtained.
Embodiment 2
(1) pre-process：By waste and old denitrating catalyst block using high pressure airgun purging surface and duct, then pass through
Denitrating catalyst block duct is swept in giant spray, is placed in air dry oven and is dried, and drying temperature is 90 DEG C, dries 5h；Take
Crushed after going out, inactivation denitrating catalyst must be pre-processed.
(2) vanadium is reclaimed：By the catalyst of above-mentioned pretreatment after 350 DEG C of high-temperature activation 4h, 0.3mol/L carbonic acid is impregnated in
In hydrogen sodium solution, 0.6mol/L strong oxidizer potassium chlorate is added, agitating solution, adding ammonium chloride makes vanadium be sunk in the form of ammonium metavanadate
Form sediment, filtering, 110 DEG C of dry 5h, 250 DEG C of calcining 5h, obtain vanadic anhydride.
(3) calcification：By 110 DEG C of dry 2h of filtrate in step (2), crushed after being dried to granularity is 300 mesh, adds calcium carbonate
It is well mixed, wherein the quality for adding calcium carbonate accounts for the 50% of mixture gross mass, 1100 DEG C of calcining 3h；
Pickling：Above-mentioned burnt solid matter is crushed, it is 1 to add with the mass ratio of powder:4 mass fraction is
7% dilute hydrochloric acid solution, 60 DEG C of stirring in water bath 6h, deionized water is added, the concentration for adjusting tungsten is 1~100g/L.
(4) recovery Pd：Pickling liquid in step (3) is added into ammoniacal liquor, adjusts solution PH=9, is well mixed and adds
MgCl2, wherein the quality for adding MgCl2 is 3% of calcining powder quality in step (3), 4h is stirred, filtering, obtains TiO2.
(5) denitrating catalyst regeneration is inactivated：The vinegar that mass fraction is 8% is separately added into filtrate into above-mentioned steps (4)
Sour antimony, 1% ammonium heptamolybdate, 5% cerous nitrate, 6% lanthanum nitrate, the denitrating catalyst of inactivation is immersed in above-mentioned solution,
4h is soaked, taking-up is placed in drying box is warming up to 90 DEG C with 8 DEG C/min, dries 4h；
Above-mentioned dry catalyst is placed in Muffle kiln roasting, with 8 DEG C/min, is warming up to 500 DEG C, is incubated 8h, it is cold with stove
But to room temperature, regeneration denitrating catalyst is obtained.
Embodiment 3
(1) pre-process：By waste and old denitrating catalyst block using high pressure airgun purging surface and duct, then pass through
Denitrating catalyst block duct is swept in giant spray, is placed in air dry oven and is dried, and drying temperature is 90 DEG C, dries 4h；Take
Crushed after going out, inactivation denitrating catalyst must be pre-processed.
(2) vanadium is reclaimed：By the catalyst of above-mentioned pretreatment after 400 DEG C of high-temperature activation 3h, 0.5mol/L carbonic acid is impregnated in
In hydrogen sodium solution, 0.1mol/L strong oxidizer potassium chlorate is added, agitating solution, adding ammonium chloride makes vanadium be sunk in the form of ammonium metavanadate
Form sediment, filtering, 110 DEG C of dry 4h, 300 DEG C of calcining 3h, obtain vanadic anhydride.
(3) calcification：By 80 DEG C of dry 2h of filtrate in step (2), crushed after being dried to granularity is 400 mesh, adds calcium carbonate
It is well mixed, wherein the quality for adding calcium carbonate accounts for the 40% of mixture gross mass, 800 DEG C of calcining 6h；
Pickling：Above-mentioned burnt solid matter is crushed, it is 1 to add with the mass ratio of powder:5 mass fraction is
10% dilute hydrochloric acid solution, 70 DEG C of stirring in water bath 4h, deionized water is added, the concentration for adjusting tungsten is 1~100g/L.
(4) recovery Pd：Pickling liquid in step (3) is added into ammoniacal liquor, adjusts solution PH=8.5, is well mixed and adds
MgCl2, wherein adding MgCl2Quality be 5% of calcining powder quality in step (3), stir 5h, filtering, obtain TiO2.
(5) denitrating catalyst regeneration is inactivated：The vinegar that mass fraction is 5% is separately added into filtrate into above-mentioned steps (4)
Sour antimony, 20% cerous nitrate, 8% lanthanum nitrate, 15% niobium oxalate immerse the denitrating catalyst of inactivation in above-mentioned solution, leaching
3h is steeped, taking-up is placed in drying box is warming up to 105 DEG C with 10 DEG C/min, dries 4h；
Above-mentioned dry catalyst is placed in Muffle kiln roasting, with 10 DEG C/min, is warming up to 600 DEG C, is incubated 3h, it is cold with stove
But to room temperature, regeneration denitrating catalyst is obtained.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of recycling method of waste and old vanadium titanium tungsten system denitrating catalyst, comprises the following steps：
1) pre-process：By waste and old denitrating catalyst successively by soot blowing, high pressure water washing, drying, crush that must to pre-process inactivation de-
Denox catalyst；
2) vanadium is reclaimed：After above-mentioned pretreatment is inactivated into denitrating catalyst high-temperature activation, it is impregnated in sodium bicarbonate solution, adds chlorine
Sour potassium, handle to obtain vanadic anhydride；
3) calcification, pickling：Filtrate is dried in step (2), adds calcium carbonate, calcining, adds acid solution processing；
4) recovery Pd：Filtrate in step (3) is adjusted to alkalescent, adds MgCl2, stirring, filter to obtain TiO2；
5) denitrating catalyst regeneration is inactivated：Filtrate adds oxysalt in step (4), obtains regenerative mixed solution, will inactivate denitration
Catalyst is immersed in above-mentioned regenerative mixed solution, is dried, roasting, inactivation denitrating catalyst regeneration.
2. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, in the step (2), the sintering temperature of high-temperature activation is 300~400 DEG C, and roasting time is 3~5h；The bicarbonate
The concentration of sodium solution is 0.1~0.5mol/L；The concentration of the potassium chlorate is 0.1~0.8mol/L；The processing is addition chlorine
Change ammonium, successively by stirring, filtering, 90~120 DEG C of dryings, 3~5h, 200~300 DEG C of 3~5h of calcining.
3. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, in the step (3), the filtrate drying temperature is 70~110 DEG C, and crushed after being dried to granularity is 200~400 mesh；
The amount for adding calcium carbonate is the 20%~50% of pulverized particles quality；The calcining heat is to calcine 3 at 700~1100 DEG C
~6h.
4. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, in the step (3), is crushed after the calcining；The acid solution is the sulfuric acid or salt that mass fraction is 5%~10%
Acid solution, it is 2 to add quality amount with powder quality ratio:1~5:1；The processing is 60~90 DEG C of 3~6h of stirring in water bath.
5. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 4, its feature
It is, in the step (3), after the stirring in water bath, it is 1~100g/L to add deionized water and adjust to tungsten concentration.
6. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, adding ammoniacal liquor in the step (4), in solution is adjusted to PH=8~9；The MgCl2Addition be institute in step (3)
State 1%~5% of powder after calcining；2~5h of the stirring.
7. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
Be, in the step (4), the oxysalt be antimony acetate, ammonium heptamolybdate, cerous nitrate, lanthanum nitrate and niobium oxalate at least
One or more mixing.
8. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, in the step (5), the ratio that the oxysalt accounts for the filtrate is：20%~50%.
9. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
Be, in the step (5), it is described immerse mixed solution catalyst be placed in drying box, programming rate be 5~10 DEG C/
Min, drying temperature are 80~105 DEG C, and drying time is 2~4h.
10. a kind of recycling method method of waste and old vanadium titanium tungsten system denitrating catalyst according to claim 1, its feature
It is, in the step (5), the dry rear catalyst roasting, programming rate is 4~10 DEG C/min, is warming up to 400~600
DEG C, 3~8h is incubated, cools to room temperature with the furnace.
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| CN112371109A (en) * | 2020-11-26 | 2021-02-19 | 西安建筑科技大学 | Preparation method of aged vanadium-based catalyst and rare earth regenerated denitration catalyst |
| CN112547046A (en) * | 2020-11-23 | 2021-03-26 | 安徽元琛环保科技股份有限公司 | Preparation method of environment-friendly denitration catalyst based on vanadium-titanium slag |
| CN113694937A (en) * | 2021-08-27 | 2021-11-26 | 山东天璨环保科技有限公司 | Method for regenerating vanadium-titanium denitration catalyst |
| CN115212893A (en) * | 2022-08-04 | 2022-10-21 | 苏州西热节能环保技术有限公司 | Regenerated catalyst capable of realizing synchronous denitration and dealcoholization and preparation method thereof |
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Application publication date: 20171222 |