CN104888806B - A kind of regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified - Google Patents

A kind of regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified Download PDF

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CN104888806B
CN104888806B CN201510229449.XA CN201510229449A CN104888806B CN 104888806 B CN104888806 B CN 104888806B CN 201510229449 A CN201510229449 A CN 201510229449A CN 104888806 B CN104888806 B CN 104888806B
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catalyst
denitration
demercuration
vanadium titanium
concentration
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CN104888806A (en
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闫巍
王磊
周扬
郜时旺
许世森
冯向程
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中国华能集团清洁能源技术研究院有限公司
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Abstract

The invention discloses a kind of regeneration methods that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified.First, by the detection to SCR denitration physics and chemical property, its deactivation cause is analyzed;Then reproducible SCR catalyst deionized water, highly basic or strong acid solution are cleaned by ultrasonic, remove dust stratification and poisoning element in catalyst;Then the catalyst after cleaning is immersed in combined denitration demercuration regenerated liquid, until catalyst activity is stablized;Finally, the catalyst after activation is transferred in micro-wave oven the drying and calcination by way of microwave heating.Catalyst after being regenerated according to the present invention has been successfully introduced into the ability of co-oxidation demercuration while restoring denitration activity, and at 350 DEG C, for denitration efficiency up to 90% or more, demercuration efficiency reaches 85% or more;Cost caused by due to avoid after the denitrating flue gas demercuration again increases, economic and environment-friendly, is suitble to commercial introduction.

Description

A kind of regeneration that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified Method

Technical field

The invention belongs to chemical technology field, more particularly to a kind of inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration The regeneration method that demercuration is modified.

Background technology

For the energy consumption in China based on coal, power generation is mainly derived from the direct burning of coal in thermal power plant.Thermoelectricity The pollutant of factory's discharge includes Atmospheric particulate matters, carbon dioxide, sulfur dioxide and nitrogen oxides (NOx) etc..Nitrogen oxidation Object is as one of Air Pollutants, due to that can cause acid rain, light pollution, global warming and reduction ozone layer etc., Cause the extensive concern of people.With the development of economy, ecological requirements grow to even greater heights, and China is to coal-burning power plant's discharged nitrous oxides The continuous reinforcement of concentration limitation, it is the state control after flue gas desulfurization to carry out emission control to the nitrogen oxides in coal steam-electric plant smoke Another emphasis behave of thermal power plant's pollutant emission.

NOxThe main divided combustion of control before and burning latter two:Control mainly has low nitrogen burning, skill of burning again before burning Art;Control is mainly divided to two kinds of wet method and dry method after burning, and selective catalytic reduction (SCR) method wherein in dry method is because at a low price and high It imitates and gains great popularity, be the most method of current commercial Application.Its principle is under the effect of the catalyst, (to be commonly used with reducing agent NH3With urea etc.) nitrogen oxides is selectively reduced to nitrogen.Catalyst is the core of entire SCR denitration system, performance Quality be directly related to the height of whole denitration efficiency.Being now widely used for the SCR denitration of coal-burning power plant is V2O5-WO3/TiO2System Catalyst, a 50MW unit need catalyst 100m3Left and right, about 6,000,000 yuan of RMB, price It is expensive.300~500 DEG C of the usual reaction temperature of SCR denitration, is arranged in air preheater and electric precipitator upstream in power plant (high ash side), therefore catalyst is highly susceptible to the shadow that ash content, alkali metal, alkaline-earth metal, arsenic, sulfur dioxide etc. are blocked and is poisoned It rings and inactivates.If the SCR catalyst of inactivation is directly discarded, not only waste of resource, also results in heavy metal secondary pollution etc. Problem.Therefore, the regeneration technology for studying SCR catalyst, for reducing the operating cost of denitrating system, alleviating waste catalyst Environmental hazard etc. is of great significance.

The country is related to carrying out decaying catalyst about the patent of denitrating catalyst regenerated liquid and regeneration method mostly at present Purging, pickling, alkali cleaning, activity supplement, make catalyst activity be restored.The patent of publication number CN102658215A provides one Kind SCR regenerating flue gas denitrifying catalyst methods, specific steps include purging catalyst to be regenerated, then use cleaning solution Cleaning, drying, then catalyst is impregnated in active supplement solution, it finally roasted, cooled down, obtain regenerated denitration catalyst Agent.The patent of publication number CN103055962A then provides a kind of SCR denitration regeneration method and its equipment, method include Gas cleaning is first used, liquid rinse is then used, finally dries, removes the pollutant in inactivation SCR denitration catalyst.But it is above-mentioned Drying and calcining process in technology uses drying box and Muffle furnace, and time-consuming for heating, and energy consumption is big, and is easy to make to urge after drying and calcining Agent mechanical strength reduces.

In addition, mercury pollution problem caused by coal-fired in recent years also begins to be paid attention to.The heavy metals such as mercury are in vivo With in food chain have permanently building up property, to higher organism have strong toxicity.And up to the present, there are no be suitble to big rule The flue gas demercuration technology that mould is promoted, and smoke mercury emission control is carried out using the existing equipment for denitrifying flue gas of coal fired power plant, it can be improved Utilization rate of equipment and installations reduces control cost.

The patent of publication number CN102716736A provides a kind of while denitration demercuration composite catalyst, including activearm Divide, carrier and auxiliary agent, the active component are CeO2And ZrO2, the carrier is ceramic honey comb, molecular sieve, ceramic wafer, activated carbon One or more in fiber, silica-gel carrier, diatomite, metal alloy, filter bag, the auxiliary agent is the oxygen of W, Cu, Fe, Ti, Ni The arbitrary combination of one or more of compound.The patent of publication number CN103480371A provides a kind of denitration demercuration and urges Agent and preparation method thereof, this method include:Ruthenium-containing substance, titanium-based denitrating catalyst and hydrogen peroxide are mixed, will be contacted It is roasted after mixture afterwards is dry or not dry.The above patent is added in the preparation process of fresh denitrating catalyst Demercuration substance makes catalyst have demercuration ability, has patent in inactivating denitrating catalyst regenerative process currently without discovery, Under the action of microwave technology, make catalyst that there is combined denitration demercuration ability.

Invention content

In order to overcome the disadvantages of the above prior art, it is cellular de- that the purpose of the present invention is to provide a kind of inactivation vanadium titanium-baseds The regeneration method that denox catalyst combined denitration demercuration is modified is restoring inactivation vanadium titanium-based Faveolate denitration catalyst denitration activity On the basis of, by modification, the CeO with catalysis oxidation nonvalent mercury performance is loaded to it2And CuO so that the catalyst after regeneration There is preferable nonvalent mercury oxidation characteristic simultaneously, meet the needs of flue gas combined denitration demercuration, to be provided simultaneously with denitration demercuration Performance.

To achieve the goals above, the technical solution adopted by the present invention is:

A kind of regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified, is first catalyzed inactivation Agent is evaluated, and sample is uniformly chosen from the different location of decaying catalyst, by catalyst denitration activity detection and BET, The characterization methods such as SEM, XRD, XRF, the deactivation cause of analysis of catalyst and regenerated possibility, for reproducible inactivation vanadium titanium Base Faveolate denitration catalyst executes following steps:

Step 1:Inactivation vanadium titanium-based Faveolate denitration catalyst is pre-processed with dedusting detoxification;

Step 2:Pretreated inactivation vanadium titanium-based Faveolate denitration catalyst is put into combined denitration demercuration regenerated liquid Dipping;

Step 3:Inactivation vanadium titanium-based Faveolate denitration catalyst after dipping is transferred to drying and calcination in micro-wave oven, is obtained To regenerated vanadium titanium-based Faveolate denitration catalyst.

Preprocess method is in the step 1:

Reproducible inactivation vanadium titanium-based Faveolate denitration catalyst is sequentially placed into deionized water and strong acid solution ultrasonic Processing, or be sequentially placed into deionized water, highly basic and strong acid solution and be ultrasonically treated, it is then rinsed with water and removes remained on surface acid Liquid is stood to the anhydrous drip in surface.Specifically:It is cleaned by ultrasonic 20~40min in deionized water, it is therefore an objective to remove catalyst Dust stratification in honeycomb and soluble alkali metal oxide;By the further alkali cleaning of catalyst after washing (if arsenic poisoning does not occur Without alkali cleaning) and pickling remove dust stratification and other and the unreacted poisoning substance of water in micropore;Alkali wash water is mass concentration 0.1 ~0.5% NaOH solution, is cleaned by ultrasonic 20~40min, and pickle is the H of mass concentration 0.1~0.2%2SO4Solution, ultrasound 20~40min is cleaned, the catalyst after pickling is rinsed with deionized water to ph=4~6, is stood and is spontaneously dried.

Combined denitration demercuration regenerated liquid is oxalic acid, ammonium metavanadate, ammonium metatungstate, cerous nitrate and copper chloride in the step 2 Mixed solution, wherein a concentration of 0.05wt%~0.1wt% of ammonium metavanadate, a concentration of 0.25wt% of ammonium metatungstate~ 0.5wt%, a concentration of 1wt%~2wt% of cerous nitrate, copper chloride concentration are 0.1wt%~0.5wt%, and concentration of oxalic acid is 0.2wt%~0.5wt%, 20~40min of dip time stand after dipping and flow down spare, catalyst and regenerated liquid to dripless Volume ratio be 1:4.

In the step 2, can pretreated inactivation vanadium titanium-based Faveolate denitration catalyst be first subjected to XRF detections, point Active component is analysed, then according to active component content, adjusts each component concentration and dip time of combined denitration demercuration regenerated liquid, The load capacity of active component is controlled, specific strategy is:

The load capacity of active component is 1~3 times of the corresponding loss of active component amount of decaying catalyst, when each group of regenerated liquid When point mass concentration is equal to the mass percent for needing load capacity, dip time 20min;When each component mass concentration of regenerated liquid Be need load capacity mass percent 1/2 when, dip time 40min.

Microwave power is 0.1~1.0kW, 5~30min of drying time, temperature 80~150 in step 3 drying process ℃.400~600 DEG C of temperature in calcination process, 2~4h of calcination time, 2~10 DEG C/min of heating rate.

Compared with prior art, the beneficial effects of the invention are as follows:

1, the present invention by adding CeO in the catalyst2With CuO active components, keep the vanadium titanium-based after regeneration cellular de- Denox catalyst restores have good oxidizing zero-valence mercury ability while denitration activity, that is, the vanadium titanium-based Faveolate denitration after regenerating Catalyst is provided simultaneously with denitration demercuration performance.

2、CeO2With CuO and the auxiliary agent for promoting SCR denitration to react, helps to improve the denitration activity of catalyst and widen The temperature window of catalytic activity and anti-SO2Poisoning capability passes through V2O5、WO3、CeO2, interaction between CuO, further carry The high denitration activity and mercury oxide ability of regenerated catalyst, makes catalyst all be showed within the temperature range of 200~450 DEG C Go out higher catalytic activity.

3, it is aided with microwave drying technology, the rapid draing technique of microwave improves dispersion of the active component in carrier surface Degree, increases catalytic reaction activity site, further improves the denitration demercuration activity of catalyst, the drying and calcination mistake of microwave The journey time is short, efficient, and energy consumption can be greatly reduced.

Specific implementation mode

With reference to the embodiment embodiment that the present invention will be described in detail.

Embodiment 1

This experiment uses the vanadium titanium-based Faveolate denitration catalyst that certain power plant has inactivated for experimental raw, catalyst section ruler Very little 150mm × 150mm, the fritter that 30mm × 30mm × 50mm is cut from raw material are regenerated, and steps are as follows:

Step 1:Deactivation cause is carried out to catalyst to analyze, it is as a result as follows:

(1) after certain time runs use, denitration efficiency is decreased obviously catalyst, decreases by 40% or more, It is judged to inactivating;

(2) decaying catalyst surface blocks apparent, but specific surface area and Kong Rongwei decline to a great extent;

(3) part variation, TiO occur for the crystal form of catalyst2Still exist with the Detitanium-ore-type with good catalytic activity, but Moulding material SiO2Crystalline structure changes, and catalytic mechanical toughness is made to change;

(4) catalyst examination of infrared spectrum, which is shown on old catalyst, has apparent sulfate to generate, and catalyst occurs in sulphur Malicious phenomenon;

(5) content of decaying catalyst surface Na, K, Ca, S dramatically increase, and show that alkali metal and sulfur poisoning occur for catalyst Phenomenon, poisoning are the main reason for causing catalyst inactivation.

Through being analyzed above it is found that the catalyst does not occur to be obviously sintered and the irreversible deactivation phenomenom such as arsenic poisoning, it is suitble to Regeneration.

Step 2:Reproducible catalyst is put into deionized water and is cleaned by ultrasonic 40min, removes catalyst monolith duct Interior dust stratification.

Step 3:Catalyst after water is cleaned is put into the H of mass concentration 0.2%2SO4It is cleaned by ultrasonic 40min in solution, acid Catalyst after washing is rinsed with water to ph=4~6, is stood to non-water flow.

Step 4:Catalyst after pickling is impregnated in combined denitration demercuration regenerated liquid, regenerated liquid medium-height grass acid concentration 0.5wt%, a concentration of 0.5wt% of ammonium metavanadate, a concentration of 2.5wt% of ammonium metatungstate, a concentration of 1wt% of cerous nitrate, chlorination Copper concentration is 0.1wt%, dip time 40min, stands to no liquid and flows down after dipping.

Step 5:Catalyst after dipping is put into microwave heating equipment dry 7min, microwave power 0.7kW.

Step 6:Catalyst calcines 2h, regeneration ending in micro-wave oven under the conditions of 450 DEG C.

Catalyst denitration efficiency and the evaluation condition of demercuration efficiency and calculating are as follows:

Catalyst after regeneration is crushed, sieving, obtains particle of the grain size between 40~60 mesh, take 0.308ml particles It is put into catalyst activity evaluating apparatus.Catalyst activity evaluation test is in internal diameter is 6mm quartz glass fixed bed reactors It carries out.Mercury vapour generating means be by mercury osmos tube water bath with thermostatic control and constant flow rate carrier gas (high-purity N2) under the conditions of formed it is special Determine the stabilization mercury vapour of concentration.Gas is simulated with N2Gas is carrier gas, wherein containing NO:499.55mg/Nm3、NH3:283.08mg/ Nm3、O2It is 3.4%, ammonia nitrogen molar ratio 1.03,37.7 μ g/m of mercury occurring source concentration3, air speed 360000h-1.Utilize mass flow Meter and spinner flowmeter control each gas flow.Into before reactor, gas first mixes in gas mixer, using pre- Hot device preheating.

Denitration efficiency δ (NOx) be defined as:

In formula, (NOx)IN、(NOx)OUTRespectively import and export NOXVolume fraction.

Demercuration efficiency δ (Hg) is defined as:

In formula, (Hg)IN、(Hg)OUTThe respectively volume fraction of import and export mercury.

The catalyst experiment raw material inactivated using certain power plant in above-mentioned detection method and experiment condition evaluation this patent is obtained: Under the conditions of 350 DEG C, decaying catalyst denitration efficiency is 43.96%, demercuration efficiency 14.05%, the non-deactivated catalysis under the conditions of Agent denitration efficiency is 97.32%, demercuration efficiency 32.15%.

Catalyst denitration demercuration Evaluation results such as following table after regeneration:

1 embodiment 1 of table denitration efficiency and demercuration efficiency at each temperature

Embodiment 2

Step 1:The fritter that 30mm × 30mm × 50mm is cut from certain same power plant's decaying catalyst raw material in embodiment 1 loses Catalyst living is regenerated, and catalyst is put into deionized water and is cleaned by ultrasonic 40min, removes the product in catalyst monolith duct Ash.

Step 2:Catalyst after water is cleaned is put into the H of mass concentration 0.2%2SO4It is cleaned by ultrasonic 40min in solution, acid Catalyst after washing is rinsed with water to ph=4~6, is stood to non-water flow.

Step 3:Catalyst after pickling is impregnated in combined denitration demercuration regenerated liquid, regenerated liquid medium-height grass acid concentration 0.5wt%, a concentration of 0.7wt% of ammonium metavanadate, a concentration of 3.5wt% of ammonium metatungstate, a concentration of 1wt% of cerous nitrate, chlorination Copper concentration is 0.1wt%, dip time 30min, stands to no liquid and flows down after dipping.

Step 4:Catalyst after dipping is put into microwave heating equipment dry 7min, microwave power 0.7kW.

Step 5:Catalyst calcines 2h, regeneration ending in micro-wave oven under the conditions of 450 DEG C.

Regenerated catalyst denitration efficiency and the evaluation condition of demercuration efficiency and calculating are with embodiment 1, as a result such as following table.

2 embodiment 2 of table denitration efficiency and demercuration efficiency at each temperature

Embodiment 3

Step 1:The fritter that 30mm × 30mm × 50mm is cut from certain same power plant's decaying catalyst raw material in embodiment 1 loses Catalyst living is regenerated, and catalyst is put into deionized water and is cleaned by ultrasonic 40min, removes the product in catalyst monolith duct Ash.

Step 2:Catalyst after water is cleaned, which is put into the NaOH solution of mass concentration 0.5%, is cleaned by ultrasonic 30min, after It is put into the H of mass concentration 0.2%2SO4It is cleaned by ultrasonic 40min in solution, the catalyst after pickling is rinsed with water to ph=4~6, It stands to non-water flow.

Step 3:Catalyst after pickling is impregnated in combined denitration demercuration regenerated liquid, regenerated liquid medium-height grass acid concentration 0.5wt%, a concentration of 1wt% of ammonium metavanadate, a concentration of 5wt% of ammonium metatungstate, a concentration of 2wt% of cerous nitrate, copper chloride are dense It is 0.5wt% to spend, dip time 30min, stands to no liquid and flows down after dipping.

Step 4:Catalyst after dipping is put into microwave heating equipment dry 10min, microwave power 0.9kW.

Step 5:Catalyst calcines 2h, regeneration ending in micro-wave oven under the conditions of 450 DEG C.

The evaluation condition and calculation of regenerated catalyst denitration efficiency and demercuration efficiency are as a result as follows with embodiment 1 Table.

3 embodiment 3 of table denitration efficiency and demercuration efficiency at each temperature

Embodiment 4

Step 1:The fritter that 30mm × 30mm × 50mm is cut from certain same power plant's decaying catalyst raw material in embodiment 1 loses Catalyst living is regenerated, and catalyst is put into ionized water and is cleaned by ultrasonic 40min, removes the product in catalyst monolith duct Ash.

Step 2:Catalyst after water is cleaned, which is put into the NaOH solution of mass concentration 0.5%, is cleaned by ultrasonic 30min, after It is put into the H of mass concentration 0.2%2SO4It is cleaned by ultrasonic 40min in solution, the catalyst after pickling is rinsed with water to ph=4~6, It stands to non-water flow.

Step 3:Catalyst after pickling is impregnated in modification regeneration liquid, regenerated liquid medium-height grass acid concentration 0.5wt%, inclined vanadium A concentration of 0.8wt% of sour ammonium, a concentration of 4wt% of ammonium metatungstate, a concentration of 1.5wt% of cerous nitrate, copper chloride concentration are 0.4wt%, dip time 20min stand to no liquid after dipping and flow down.

Step 4:Catalyst after dipping is put into microwave heating equipment dry 7min, microwave power 0.7kW.

Step 5:Catalyst calcines 2h, regeneration ending in micro-wave oven under the conditions of 450 DEG C.

The evaluation condition and calculation of regenerated catalyst denitration efficiency and demercuration efficiency are as a result as follows with embodiment 1 Table.

4 embodiment 4 of table denitration efficiency and demercuration efficiency at each temperature

After being regenerated to decaying catalyst according to the regeneration method of this patent it can be seen from above example experimental result, Catalyst denitration efficiency is obviously restored, and can reach the NO of raw catelyst substantiallyxRemoval effect, and regenerated catalyst Demercuration efficiency is also very high.

The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this A little simple variants all belong to the scope of protection of the present invention.

Claims (4)

1. a kind of regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified, which is characterized in that packet Include following steps:
Step 1:First decaying catalyst is evaluated, sample is uniformly chosen from the different location of decaying catalyst, passes through catalysis Agent denitration activity detects and BET, SEM, XRD and XRF characterization, the deactivation cause of analysis of catalyst and regenerated possibility;
Step 2:Reproducible inactivation vanadium titanium-based Faveolate denitration catalyst is pre-processed with dedusting detoxification, method is:
Reproducible inactivation vanadium titanium-based Faveolate denitration catalyst is sequentially placed into deionized water and strong acid solution and is ultrasonically treated, Or be sequentially placed into deionized water, highly basic and strong acid solution and be ultrasonically treated, it is then rinsed with deionized water and removes remained on surface Acid solution is stood to the anhydrous drip in surface;
Step 3:Pretreated inactivation vanadium titanium-based Faveolate denitration catalyst is put into combined denitration demercuration regenerated liquid and is impregnated, Specifically:
Pretreated inactivation vanadium titanium-based Faveolate denitration catalyst is first subjected to XRF detections, analyzes active component, then basis Active component content adjusts each component concentration and dip time of combined denitration demercuration regenerated liquid, controls the load of active component Amount, specific strategy are:
The load capacity of active component is 1~3 times of the corresponding loss of active component amount of decaying catalyst, when each group sub-prime of regenerated liquid When amount concentration is equal to the mass percent for needing load capacity, dip time 20 minutes;When each component mass concentration of regenerated liquid is When needing the mass percent 1/2 of load capacity, dip time 40 minutes;
The combined denitration demercuration regenerated liquid is that the mixing containing oxalic acid, ammonium metavanadate, ammonium metatungstate, cerous nitrate and copper chloride is molten Liquid, wherein a concentration of 0.2wt%~1wt% of ammonium metavanadate, a concentration of 1wt%~5wt% of ammonium metatungstate, cerous nitrate are a concentration of 1wt%~2wt%, copper chloride concentration are 0.1wt%~0.5wt%, and concentration of oxalic acid is 0.2wt%~0.5wt%, dip time 20~40min stands to dripless after dipping and flows down;
Step 4:Inactivation vanadium titanium-based Faveolate denitration catalyst after dipping is transferred to drying and calcination in micro-wave oven, is obtained again Raw vanadium titanium-based Faveolate denitration catalyst.
2. the regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified according to claim 1, It is characterized in that, the volume ratio of the catalyst and regenerated liquid is 1:4.
3. the regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified according to claim 1, It is characterized in that, in step 4 drying process microwave power be 0.1~1.0kW, 5~30min of drying time, temperature 80~ 150℃。
4. the regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified according to claim 1, It is characterized in that, 400~600 DEG C, 2~4h of calcination time of temperature in step 4 calcination process, 2~10 DEG C of heating rate/ min。
CN201510229449.XA 2015-05-07 2015-05-07 A kind of regeneration method that inactivation vanadium titanium-based Faveolate denitration catalyst combined denitration demercuration is modified CN104888806B (en)

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CN106082247B (en) * 2016-06-03 2018-05-29 辽宁石化职业技术学院 A kind of inactivation Ti (SO4)2-Zr(SO4)2Composite solid-acid catalyst recoverying and utilizing method
CN107185598B (en) * 2017-05-25 2019-09-27 清华大学 A kind of relieving haperacidity demercuration catalyst regeneration method
CN107837826B (en) * 2017-11-21 2021-01-12 沈阳航空航天大学 Regeneration process method of inactivated flue gas denitration catalyst
CN110152744A (en) * 2019-05-27 2019-08-23 中国华能集团清洁能源技术研究院有限公司 A kind of electrochemical process for treating of arsenic poisoning SCR denitration

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