CN106975482A - Denitrating catalyst and preparation method thereof - Google Patents
Denitrating catalyst and preparation method thereof Download PDFInfo
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- CN106975482A CN106975482A CN201710279653.1A CN201710279653A CN106975482A CN 106975482 A CN106975482 A CN 106975482A CN 201710279653 A CN201710279653 A CN 201710279653A CN 106975482 A CN106975482 A CN 106975482A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20707—Titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20723—Vanadium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/2073—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20776—Tungsten
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Abstract
The invention discloses a kind of denitrating catalyst and preparation method thereof.Wherein, the preparation method comprises the following steps：Manganese active component is synthesized, and prepared by vanadium maceration extract, carrier, manganese active component, vanadium maceration extract mixed grinding, and spray drying, roasting obtains denitrating catalyst.Apply the technical scheme of the present invention, production procedure is short, utilization rate of equipment and installations is high, production efficiency is high, labor intensity is small, energy consumption is low；And the catalyst prepared can be used steadily in the long term.
Description
Technical field
The present invention relates to technical field of chemistry, in particular to a kind of denitrating catalyst and preparation method thereof.
Background technology
NOx is a series of one of arch-criminal of ecological environment problems such as acid rain, photochemical fog, depletion of the ozone layer, and NOx is also
One of inducement of haze formation, NOx, SOx are PM2.5 predecessors, by its transformation Lai PM2.5 account for total amount 40%~
50%.
The NOx of China is mainly derived from industrial discharge, focus primarily upon thermoelectricity, steel (including coking), cement, glass and
Other industries.Thermal Power Generation Industry accounts for the 40% of national total emission volumn as AND ENERGY RESOURCES CONSUMPTION IN CHINA and the rich and influential family of pollutant emission, long
It has been always the emphasis of China's industrial pollution source domain preventing and treating since phase.During " 13 ", minimum discharge is still that power industry is big
The main keynote of gas contamination control.Although Thermal Power Generation Industry NOx improvement has obtained interim success, haze is increasingly serious, air
Contaminating enterprises have gradually been put into the scope of blowdown improvement, such as coking industry, cement industry, domestic glass industry, biomass
Industry etc..
Due to technical limitation, the industry such as coking industry, cement industry, domestic glass industry, biomass, at present still without
The denitrating catalyst that can be used steadily in the long term.
The content of the invention
The present invention is intended to provide a kind of denitrating catalyst and preparation method thereof, a kind of it can be used steadily in the long term with providing
Denitrating catalyst.
To achieve these goals, according to an aspect of the invention, there is provided a kind of preparation method of denitrating catalyst.
The preparation method comprises the following steps：Manganese active component is synthesized, prepared by vanadium maceration extract, and carrier, manganese active component, vanadium maceration extract are mixed
Grinding is closed, spray drying, roasting obtains denitrating catalyst.
Further, manganese active component synthesis includes：1) potassium permanganate and manganese nitrate are added to the water dissolving, obtain first
Slurries；2) the first slurries are heated to 100~120 DEG C, keep 10h~16h, obtain the second slurries；3) the second slurries are carried out
Filtering, obtains manganese active component.
Further, 3) specifically include：Second slurries are moved into knob gram Multifunction filtering machine and carry out filtration washing, washing 3
~6 times.
Further, the mass ratio of potassium permanganate, manganese nitrate and water is 10 in 1)：17：320.
Further, carrier is titanium tungsten powder.
Further, vanadium maceration extract is ammonium metavanadate aqueous solution, the mass percentage concentration of vanadium maceration extract for 0.65%~
1.94%.
Further, by carrier, manganese active component and vanadium maceration extract using mass ratio as 92~98：1~5：200 are mixed
Close, grind 1h~2h.
Further, the slurries for grinding completion are spray-dried at 110 DEG C~180 DEG C, dry duration 1h~2h.
Further, the product completed will be dried, in car type furnace, 500 DEG C~650 DEG C roasting 6h.
Apply the technical scheme of the present invention, production procedure is short, utilization rate of equipment and installations is high, production efficiency is high, labor intensity is small, raw
Production capacity consumption is low；And the catalyst prepared can be used steadily in the long term, in 180 DEG C~380 DEG C of temperature range
Reach more than 90% denitration efficiency.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing a further understanding of the present invention, and of the invention shows
Meaning property embodiment and its illustrate be used for explain the present invention, do not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the preparation flow schematic diagram of denitrating catalyst according to embodiments of the present invention 1；And
Fig. 2 shows the preparation flow schematic diagram according to denitrating catalyst in comparative example 1 of the present invention.
Embodiment
It should be noted that in the case where not conflicting, the feature in embodiment and embodiment in the application can phase
Mutually combination.Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
In order to provide a kind of denitrating catalyst used steadily in the long term, SCR (SCR technology) denitration is improved
The scope of application of catalyst, applicant has developed a kind of while having the denitration catalyst of interval wide, the alkali resistant metal of reaction temperature
Agent, the catalyst can reach more than 90% denitration efficiency in 180 DEG C~380 DEG C of temperature range.
The catalyst using vanadium, manganese oxide as active component, titanium dioxide is carrier, tungsten, molybdenum, cobalt, iron, cerium, lanthanum,
One or more in praseodymium, copper are auxiliary agent (vanadium：Manganese：Auxiliary agent：The mass ratio of carrier is：1~3：1~5：6-10：82~92,
Element herein refers both to its oxide in addition, and wherein auxiliary agent can be contained in known or commercially available carrier, it is not necessary to add in addition
Plus).Proto industrialization production technology：Manganese active component is synthesized, and is washed, and is dried, and is calcined, grinding；Carrier, the mixing of manganese active component,
Vanadium maceration extract is impregnated, and catalyst is dried, is calcined, grinding.Drying and roasting grinding twice need to be carried out, production process is complicated, repeats work
Sequence is more, low production efficiency, and equipment investment is big, and production cost is high.Manganese active component is manufactured separately in original production process, can strictly control
The granularity of active powder processed, it is ensured that the uniformity of mixing uniformity and vanadium the active powder dipping of itself and titanium tungsten powder.
In order to solve the technical problem of above-mentioned technique, according to a kind of typical embodiment of the present invention, there is provided a kind of denitration
The preparation method of catalyst.The preparation method comprises the following steps：Manganese active component is synthesized, prepared by vanadium maceration extract, and carrier, manganese are lived
Property component, vanadium maceration extract mixed grinding, spray drying, roasting obtain denitrating catalyst.
Technical scheme, also can guarantee that manganese active component and the mixing uniformity and vanadium active powder of titanium tungsten powder soak
The uniformity of stain, and production procedure is short, utilization rate of equipment and installations is high, production efficiency is high, labor intensity is small, energy consumption is low；And make
Standby obtained catalyst can be used steadily in the long term, can reach in 180 DEG C~380 DEG C of temperature range more than 90% it is de-
Nitre efficiency.
It is preferred that, the synthesis of manganese active component includes：1) potassium permanganate and manganese nitrate are added to the water dissolving, obtain the first slurry
Liquid；2) the first slurries are heated to 100~120 DEG C, keep 10h~16h, obtain the second slurries；3) the second slurries were carried out
Filter, obtains manganese active component.
It is preferred that, 3) specifically include：Second slurries are moved into knob gram Multifunction filtering machine and carry out filtration washing, washing 3~6
It is secondary, remove other soluble-salts of the soluble impurity brought into raw material and reaction generation.It is preferred that, 1) in potassium permanganate, nitre
The mass ratio of sour manganese and water is 10：17：320.In this proportion, it is ensured that raw material fully dissolves.
According to a kind of typical embodiment of the present invention, carrier is titanium tungsten powder (commercially available titanium tungsten powder contains auxiliary agent).
According to a kind of typical embodiment of the present invention, vanadium maceration extract is ammonium metavanadate aqueous solution, it is preferred that vanadium maceration extract
Mass percentage concentration be 0.65%-1.94%, in this proportion, ensure catalyst activity while, can avoid compared with
High oxidation rate of sulfur dioxide.
It is preferred that, by carrier, manganese active component and vanadium maceration extract using mass ratio as 92~98：1~5：200 are mixed,
Grind 1h~2h.In this proportion, the uniformity and mobility of slurry can be ensured within this range, it is to avoid cause lower one
The blocking of process spraying system.
It is preferred that, the slurries for grinding completion are spray-dried at 110 DEG C~180 DEG C, duration 1h~2h is dried.
In this temperature range, it can control temperature of charge and be no more than 120 DEG C, it is to avoid product property caused by drying process temperature of charge is too high
Change.
It is preferred that, the product of completion will be dried, in car type furnace, 500 DEG C~650 DEG C roasting 6h.In this temperature range
The stability of the catalyst of preparation is good.Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
To improve the production technology of rear catalyst described in the present embodiment, as shown in figure 1, mainly including：Manganese activearm division
Into prepared by filtering, washing, vanadium maceration extract, carrier, manganese active component, vanadium maceration extract mixed grinding are spray-dried, roasting, and are urged
Agent is packed.Comprise the following steps that：
1) weigh respectively 31.6kg potassium permanganates, 53.69kg manganese nitrates add agitator tank in, correspondence add potassium permanganate and
Manganese nitrate is separately added into 500L water (not specified, water refers both to deionized water), and stirring is allowed to be completely dissolved.
2) liquor potassic permanganate and manganese nitrate solution are transferred in reactor, 100 are risen to reactor heating-up temperature~
120 DEG C, keep 10h~16h.
3) slurries are moved into the multi-functional carry out filtration washing of knob gram, washed 3~6 times.
4) it is 92~98 according to carrier, manganese active component and vanadium maceration extract mass ratio：1~5：200,92.5kg is weighed respectively
Titanium tungsten powder, 12kg active powder wet feeds, and all move in controlling wet-type finishing machine.
5) 3.25kg ammonium metavanadates are weighed, are dissolved in water, the mass percentage concentration of vanadium maceration extract for 0.65%~
1.94%, and be transferred in grinder.
6) add water the solid-liquid ratio adjusted in grinder, and grinds 1h~2h.
7) slurries for grinding completion are spray-dried at 110 DEG C~180 DEG C, dry duration 1h~2h.
8) catalyst completed will be dried, in car type furnace, 500 DEG C~650 DEG C roasting 6h.
9) catalyst for producing completion is packed according to packing instructions, finished product 97.2kg can be obtained, yield is
97.2%.
Comparative example 1
It is the production technology of raw catalyst described in this comparative example 1, as shown in Fig. 2 manganese active component is synthesized, filtering, washing,
Dry, be calcined, grinding；Prepared by vanadium maceration extract, carrier, the mixing of manganese active component, vanadium maceration extract dipping, catalyst are dried, roasting,
Grinding, and catalyst packing.Comprise the following steps that：
1) weigh respectively 31.6kg potassium permanganates, 53.69kg manganese nitrates add agitator tank in, correspondence add potassium permanganate and
Manganese nitrate is separately added into 500L water (not specified, water refers both to deionized water), and stirring is allowed to be completely dissolved.
2) liquor potassic permanganate and manganese nitrate solution are transferred in reactor, 100 are risen to reactor heating-up temperature~
120 DEG C, keep 10h~16h.
3) slurries are moved into knob gram Multifunction filtering machine and carries out filtration washing, washed 3~6 times.
4) active powder that will filter out dries 12h~18h in blowing-type drying box at 120 DEG C.
5) after the completion of drying, in car type furnace, 350 DEG C~500 DEG C are calcined 6 hours.
6) powder completed will be calcined, 1h~2h is ground in horizontal mill.
7) it is 92~98 according to carrier, manganese active component and vanadium maceration extract mass ratio：1~5：200,92.5kg is weighed respectively
Titanium tungsten powder, 5kg active powders, and all move in kneading machine, mixed.
8) 3.25kg ammonium metavanadates are weighed, are dissolved in water, the mass percentage concentration of vanadium maceration extract for 0.65%~
1.94%, and it is transferred to kneading machine.
9) add water pug in regulation kneading machine water content to 30%~40%.
10) catalyst pug is dried into 12h~16h in blowing-type drying box at 120 DEG C.
11) after the completion of drying, in car type furnace, 500 DEG C~650 DEG C roasting 6h.
12) pug for being calcined completion is ground into 1h~2h in horizontal mill.
13) catalyst for producing completion according to packing instructions pack that finished product 93.6kg can be obtained, yield is
93.6%.
Contrasted by embodiment 1 and comparative example 1, new technology simplified drying in manganese active powder preparation process,
Roasting, grinding step；And the dipping of kneading machine completion titanium tungsten powder, the mixing of active powder and vanadium is replaced with controlling wet-type finishing machine；Adopt
The dried forms of spray drying are taken, can ensure that material accurately matches and greatly shortens drying time.
New production process shortens technological process while product quality is ensured, reduces material without process is repeated
Transfer, product yield is high；The new technology production cycle shortens 30h~40h, and production efficiency is high；New technology has simplified manganese active powder
Drying, roasting, the reduction of grinding step energy consumption in preparation process.
As can be seen from the above description, the above embodiments of the present invention realize following technique effect：
1st, using the production technology of wet lapping, vanadium dipping solution is lapping liquid.Catalysis is completed in process of lapping
The grinding of agent, completes carrier and the mixing of manganese active component and the dipping of vanadium active component again.
2nd, wet lapping with spray drying combine, solve manganese active component dry, roasting, grinding with finished catalyst into
Product are dried, are calcined, the process replication problem of grinding, are shortened Catalyst Production technological process, are reduced material transfer process, improve
Product yield, reduce energy consumption.
3rd, integral processing is short, and labor intensity is low, and product yield is high, and energy consumption is low.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of denitrating catalyst, it is characterised in that comprise the following steps：Manganese active component is synthesized, vanadium dipping
Prepared by liquid, carrier, the manganese active component, the vanadium maceration extract mixed grinding, and spray drying, roasting obtains the denitration catalyst
Agent.
2. preparation method according to claim 1, it is characterised in that the manganese active component synthesis includes：
1) potassium permanganate and manganese nitrate are added to the water dissolving, obtain the first slurries；
2) first slurries are heated to 100~120 DEG C, keep 10h~16h, obtain the second slurries；
3) second slurries are filtered, obtains the manganese active component.
3. preparation method according to claim 2, it is characterised in that described 3) to specifically include：Second slurries are moved
Filtration washing is carried out to knob gram Multifunction filtering machine, is washed 3~6 times.
4. preparation method according to claim 1, it is characterised in that it is described 1) in potassium permanganate, manganese nitrate and water matter
Amount is than being 10：17：320.
5. preparation method according to claim 1, it is characterised in that the carrier is titanium tungsten powder.
6. preparation method according to claim 1, it is characterised in that the vanadium maceration extract is ammonium metavanadate aqueous solution, institute
The mass percentage concentration for stating vanadium maceration extract is 0.65%~1.94%.
7. preparation method according to claim 1, it is characterised in that by the carrier, the manganese active component and described
Vanadium maceration extract is using mass ratio as 92~98：1~5：200 are mixed, and grind 1h~2h.
8. preparation method according to claim 7, it is characterised in that the slurries completed will be ground at 110 DEG C~180 DEG C
It is spray-dried, dries duration 1h~2h.
9. preparation method according to claim 8, it is characterised in that the product of completion, in car type furnace, 500 will be dried
DEG C~650 DEG C of roasting 6h.
10. a kind of denitrating catalyst, it is characterised in that be prepared into as the preparation method any one of claim 1 to 9
Arrive.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111068708A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Denitration catalyst, preparation method and application |
| CN111068707A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Low-temperature denitration catalyst, preparation method and application |
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| CN101590404A (en) * | 2009-06-26 | 2009-12-02 | 清华大学 | A kind of low-vanadium denitration catalyst and its production and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111068708A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Denitration catalyst, preparation method and application |
| CN111068707A (en) * | 2018-10-22 | 2020-04-28 | 中国石油化工股份有限公司 | Low-temperature denitration catalyst, preparation method and application |
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