CN106362733A - High-temperature resistant manganite catalyst and preparation method thereof - Google Patents

High-temperature resistant manganite catalyst and preparation method thereof Download PDF

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Publication number
CN106362733A
CN106362733A CN201610844375.5A CN201610844375A CN106362733A CN 106362733 A CN106362733 A CN 106362733A CN 201610844375 A CN201610844375 A CN 201610844375A CN 106362733 A CN106362733 A CN 106362733A
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catalyst
manganese
source
preparation
temperature resistant
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耿阳
单文坡
陈晓玲
刘丁仪
尹纯强
向梦玲
杨士建
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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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
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • 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
    • 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
    • B01D53/90—Injecting reactants
    • 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
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B01D2258/0283—Flue gases
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

The invention discloses a high-temperature resistant manganite catalyst for catalytic purification of nitric oxides and a preparation method thereof. The preparation method comprises the steps that firstly, a composite oxide Mn0.5W0.1TiOx is obtained through a homogeneous precipitation method, and an oxide catalyst (MnOx)0.5-(WO3)0.1-TiO2 is obtained after calcination is performed. Non-toxic and harmless raw materials are adopted, the manganite catalyst prepared through the simple and easy method has the non-toxicity, excellent low-temperature activity and high temperature resistance, and on the aspect of stationary source De-NOx, the manganite catalyst can be adopted as the catalyst replacing a vanadium-based catalyst; the manganite catalyst has the quite excellent NOx adsorption capacity, NO independent oxidizing capacity and high-temperature NH3 independent oxidizing capacity; the manganite catalyst is applicable to a nitric oxide catalyst purification device with a stationary source represented by coal-fired power plant flue gas and a mobile source represented by diesel vehicle exhaust gas.

Description

A kind of high temperature resistant manganese-base oxide catalyst and preparation method thereof
Technical field
The present invention relates to catalyst and preparation method thereof, particularly a kind of manganio oxidation for catalytic cleaning nitrogen oxide Thing catalyst and preparation method thereof.
Background technology
Nitrogen oxides (nox, refer mainly to no and no2) it is one of major pollutants in air, gray haze, photochemical can be led to Learn the great environmental problem such as smog and acid rain, health can also be produced and directly endanger.Therefore, control noxDischarge gesture Must go, very urgent.
noxSource can be divided into natural source and artificial source, in artificial source noxIn discharge, with coal-fired plant flue gas as representative Stationary source and the moving source with exhaust gas from diesel vehicle as representative be China's topmost discharged nitrous oxides source.At present according to nitrogen oxygen Compound (nox) generation mechanism difference, control nitrogen oxides technology to be broadly divided into following three kinds: to start the burning controlling from Combustion Source Front control；By transforming the structure of burner, control burning condition, reduce in the combustion process that thermal NO generates and control System；Control after the burning nitrogen oxides of generation in flue gas being converted and being processed.The denitration skill of domestic and international main flow at present Art is the selective catalytic reduction (scr) in controlling after burning, and SCR technology is according to the difference of reducing agent, main Nh to be divided into3- scr technology and hc-scr technology, because hc-scr low-temperature reactivity difference and water resistant resistance to SO_2 difference the shortcomings of, Limit the development of hc-scr, therefore, current research worker is mainly carried out with nh3Nh for reducing agent3The research of-scr technology.
The R and D of catalyst are whole nh3The core of-scr system and key.Using the preparation of traditional infusion process v2o5-wo3/tio2Catalyst is in nearly 40 years of stationary source denitration field industrial applications, and is introduced into exhaust gas from diesel vehicle nox The field of catalytic purification.But vanadio nh3- scr catalyst yet suffers from bio-toxicity, poor high temperature stability, operation temperature The shortcomings of window is narrower, therefore, is highly desirable to traditional v2o5-wo3/tio2Catalyst improves.Numerous for nh3- In the metal oxide catalyst systems of scr reaction, mn base oxide catalyst is due to having excellent low temperature nh3- scr activity Widely paid close attention to cheap price.Therefore, noxious substance v is replaced preparation have excellent catalysis activity, High temperature heat-resistant stability, wide temperature window, high n2Generate selective mnox-wo3-tio2Catalyst has to commercial Application Very important meaning.
Content of the invention
It is an object of the invention to, for existing v2o5-wo3/tio2The deficiency that catalyst exists, the present invention provides first One kind replaces v with mn, and dispersed for tri- kinds of species of mn, w, ti formation had excellent catalysis activity, high-temperature stability And n2Generate selective metal oxide catalyst and preparation method thereof.
In order to achieve the above object, present invention employs following technical scheme:
A kind of resistant to elevated temperatures manganese-base oxide catalyst for catalytic cleaning nitrogen oxide, catalyst is metal-oxide Catalyst (mnox)0.5-(wo3)0.1-tio2, described mnoxFor mn2+、mn3+And mn4+Mixed oxide, 1 < x < 2.
The preparation method of the manganese-base oxide catalyst of the present invention is sluggish precipitation, and it comprises the following specific steps that:
Step 1, adds manganese source, tungsten source and titanium source to generate mixed solution, stirs under normal temperature condition；
Step 2, adds slow release precipitator in the mixed solution in step 1；
Step 3, is heated to 70～95 DEG C, and under this temperature conditions, continues stirring precipitation 3～24h；
Step 4, the precipitate generating is separated and washed in step 3；
Step 5, the precipitate after washing is carried out drying, roasting, obtains (mnox)0.5-(wo3)0.1-tio2Catalyst.
In step 1, one or more of the preferred manganese nitrate of manganese source, manganese chloride or manganese sulfate.Tungsten source is preferably ammonium tungstate One or more of with ammonium paratungstate.Titanium source is preferably one or more of titanium sulfate, titanium tetrachloride or butyl titanate. Wherein, the mol ratio of manganese source, tungsten source and titanium source is 5:1:10.
In step 2, one or more of the preferred ammonium carbonate of slow release precipitator, ammonium hydrogen carbonate or carbamide.Slow release precipitator Molal quantity is 8～20 times of the total mole number of manganese source, tungsten source and titanium source.
In step 3, preferably 80～90 DEG C of heating-up temperature.The stirring sedimentation time is preferably 6～12h.
In step 5, drying temperature is 90～110 DEG C.Roasting is carried out in air atmosphere, and sintering temperature is 400～800 DEG C, preferably 500 DEG C；Described roasting time is 1～24h, preferably 4～6h.
Compared with prior art, the present invention has the advantage that
(1) the manganese-base oxide catalyst of present invention preparation has avirulence, excellent low temperature active and resistance to elevated temperatures, In terms of stationary source denitrating flue gas, can be used as the alternative catalysts of catalytic component based on vanadium；
(2) the manganese-base oxide catalyst of present invention preparation has very excellent noxAbsorbability.
(3) the manganese-base oxide catalyst of present invention preparation has the independent oxidability of very excellent no；
(4) the manganese-base oxide catalyst of present invention preparation has very excellent high temperature nh3Individually oxidability, can prevent During only using, nh occurs3Leakage；
(5) preparation process of manganese-base oxide catalyst of the present invention makes tri- kinds of species of mn, w, ti dispersed, so that its Possesses above-mentioned excellent catalytic performance.
Specific embodiment
For the present invention is better described, readily appreciate technical scheme, the present invention's is typical but non-limiting Embodiment is as follows:
Embodiment 1
It is 5:1:10 according to mn, w, ti mol ratio, titanium sulfate is dissolved in deionized water, is subsequently adding ammonium tungstate and nitric acid Manganese, and add manganese source, tungsten source and titanium source 20 times of total mole number carbamide as precipitant, be then heated to 90 DEG C and continuously stir Mix 12h, then filtered and wash, by gained solid content put in baking oven in 100 DEG C dry 12h, after through Muffle furnace in 500 DEG C of in the air roasting 5h are obtained (mnox)0.5-(wo3)0.1-tio2Powder catalyst, referred to as catalyst a.
Comparative example 2
It is 5:1 according to mn:w mol ratio, ammonium tungstate is dissolved in oxalic acid, is continuously stirring to ammonium tungstate and is completely dissolved, then to In this solution add manganese nitrate, and add manganese source and tungsten source 20 times of total mole number carbamide as precipitant, be then heated to 90 DEG C and continuous stirring 12h, are then filtered and are washed, and gained solid content is put in baking oven and dries 12h in 100 DEG C, Powder catalyst, referred to as catalyst b are obtained by Muffle furnace in 500 DEG C of in the air roasting 5h.
Comparative example 3
It is 1:10 according to w:ti mol ratio, ammonium tungstate is dissolved in titanium sulfate solution, is continuously stirring to ammonium tungstate complete Dissolving, then add 20 times of precipitant carbamide of the total mole number of tungsten source and titanium source in this solution, it is then heated to 90 DEG C and connect Continuous stirring 12h, is then filtered and is washed, gained solid content is put in baking oven and dries 12h in 100 DEG C, after through Muffle Stove is obtained powder catalyst, referred to as catalyst c in 500 DEG C of in the air roasting 5h.
Comparative example 4
It is 1:2 according to mn:ti mol ratio, prepares manganese nitrate and titanium sulfate mixed solution, be subsequently adding manganese source and titanium source The carbamide that 20 times of total mole number, is then heated to 90 DEG C and continuous stirring 12h, is then filtered and wash, by gained solid Thing put in baking oven in 100 DEG C dry 12h, after through Muffle furnace in 500 DEG C of in the air roasting 5h be obtained powder catalyst, claim For catalyst d.
Comparative example 5
Conventional impregnation is adopted to be prepared for tio2For carrier, load 1wt%v2o5And 10wt%wo3V2o5-wo3/tio2 Catalyst.By c2h2o·2h2o、nh4vo3, and h4n10o41w12·xh2O is dissolved in 100ml deionized water, then in mixed solution Add tio2Dust carrier, stirring more than 1h is mixed with abundant, then by mixed solution rotary evaporation until moisture fully volatilizees, Dry overnight in the baking oven putting into 100 DEG C, then through the Muffle furnace roasting 5h under the conditions of 500 DEG C, produce powder catalyst, referred to as Catalyst e.
Application examples 1
Sample a, b, c, d, e of being obtained are carried out tabletting, grind, sieve, takes 40～60 mesh granules in fixed bed reactors On carry out nh3SCR nox(nh3- scr) reactivity investigation.
The usage amount of catalyst is 0.24ml, the consisting of of reaction mixture gas: [no]=[nh3]=500ppm, [o2]= 5%, n2Make Balance Air, total gas flow rate is 200ml/min, air speed is 50,000h-1, 100～300 DEG C of reaction temperature.No and nh3And by-product n2o、no2All measured using nicolet antaris igs infrared gas analyser.noxConversion ratio and n2Generate Selectivity is respectively as shown in Table 1 and Table 2.
The no of the different sample of table 1xConversion ratio
As shown in Table 1, under the same reaction conditions, catalyst d is in 100～150 DEG C of temperature section noxTransformation efficiency highest, Show that it has excellent low temperature active；The no of catalyst cxTransformation efficiency is relatively low, shows that mn element has very to catalyst activity Important contribution；Catalyst a is in the no of 150～300 DEG C of temperature sectionsxTransformation efficiency, all more than 80%, shows that it has excellent Nh3The active and wider temperature window of-scr.The catalyst a of the method preparation being provided using the present invention is in (250 DEG C of low-temperature zone No below)xTransformation efficiency, apparently higher than the catalyst e using traditional infusion process preparation, shows that mn replaces v and can play very well Catalytic effect.
Application examples 2
Sample a, c, d, e of being obtained are carried out tabletting, grind, sieve, takes 40～60 mesh granules on fixed bed reactors Investigate the no of catalystxAbsorbability.
The usage amount of catalyst is 0.3g, the consisting of of reaction mixture gas: [no]=500ppm, [o2]=5%, n2Put down Weighing apparatus gas, total gas flow rate is 200ml/min.No and by-product n2o、no2All using nicolet antaris igs infrared-gas Analysis-e/or determining.nox、n2o、no2Adsorbance is as shown in table 2.
The different sample of table 2 is in 50 DEG C of nox、no、no2Adsorbance
As shown in Table 2, under the same reaction conditions, the manganese-base oxide catalyst of the method preparation being provided using the present invention A, d have excellent noxAbsorbability, primary attachment for no.The no of the catalyst d of method preparation being provided using the present inventionx Absorbability is far above the catalyst e using traditional infusion process preparation, shows that mn replaces v and is conducive to improving the no of catalystxInhale Attached ability.
Application examples 3
Sample a, c, d, e of being obtained are carried out tabletting, grind, sieve, takes 40～60 mesh granules on fixed bed reactors Investigate the independent oxidability of catalyst.
The consisting of of reaction mixture gas: [no]=500ppm or [nh3]=500ppm, [o2]=5%, n2Make Balance Air, gas Body total flow is 200ml/min, 100～300 DEG C of reaction temperature.The usage amount of catalyst is 0.24ml, corresponding reaction velocity For 50,000h-1.No and nh3And by-product n2o、no2All measured using nicolet antaris igs infrared gas analyser. The no that no individually aoxidizes2Growing amount and nh3The individually nh of oxidation3Conversion ratio is as shown in Table 3 and Table 4.
The no of the different sample independent no oxidation of table 32Growing amount
As shown in Table 3, under the same reaction conditions, the no of the catalyst a of method preparation being provided using the present invention2Generate Amount is very high, is above the catalyst e using traditional infusion process preparation, illustrates that catalyst a has excellent in whole temperature range Different no oxidability, mn replaces v and is conducive to improving the no oxidability of catalyst.
The different independent nh of sample of table 43The nh of oxidation3Conversion ratio
As shown in Table 4, under same reaction conditions, the nh of the catalyst a of method preparation being provided using the present invention3Conversion ratio It is far above the catalyst e using traditional infusion process preparation in whole temperature range, show that mn replaces v and is conducive to improving catalyst Nh3Oxidability.
When actually used, catalyst is placed in exhaust pipe way, sprays into reducing agent in the upstream of catalyst and tail gas mixes Close, reducing agent adopt ammonia or carbamide (can get ammonia after hydrolysis), reducing agent consumption be nitrogen oxide in tail gas 0.8～ 1.2 times, can be by no in very wide temperature window under excess oxygenxIt is reduced to n2And h2O, is provided simultaneously with very high n2Generate Selectivity and water repelling property.
Tail gas is stationary source gas containing nitrogen oxide, such as coal-fired plant flue gas, or moving source gas containing nitrogen oxide, Such as exhaust gas from diesel vehicle.
Applicant states, the present invention illustrates detailed composition and the method for the present invention by above-described embodiment, but the present invention It is not limited to above-mentioned detailed composing method, that is, do not mean that the present invention has to rely on above-mentioned detailed composition and method could be real Apply.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, equivalent to each raw material of product of the present invention The interpolation of replacement and auxiliary element, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosure.

Claims (7)

1. a kind of high temperature resistant manganese-base oxide catalyst is it is characterised in that described catalyst is manganio metal-oxide (mnox)0.5-(wo3)0.1-tio2Catalyst, described mnoxFor mn2+、mn3+And mn4+Mixed oxide, 1 < x < 2.
2. a kind of preparation method of high temperature resistant manganese-base oxide catalyst, comprises the following specific steps that:
Step 1, adds manganese source, tungsten source and titanium source to generate mixed solution, stirs under normal temperature condition；
Step 2, adds slow release precipitator in the mixed solution in step 1；
Step 3, is heated to 70～95 DEG C, and under this temperature conditions, continues stirring precipitation 3～24h；
Step 4, the precipitate generating is separated and washed in step 3；
Step 5, the precipitate after washing is carried out drying, roasting, obtains (mnox)0.5-(wo3)0.1-tio2Catalyst.
3. the preparation method of high temperature resistant manganese-base oxide catalyst according to claim 2 is it is characterised in that in step 1, Described manganese source is one or more of manganese nitrate, manganese chloride and manganese sulfate；Described tungsten source is ammonium tungstate, in ammonium paratungstate One or more；Described titanium source is one or more of titanium sulfate, titanium tetrachloride and butyl titanate；Described manganese The mol ratio in source, tungsten source and titanium source is 5:1:10.
4. the preparation method of high temperature resistant manganese-base oxide catalyst according to claim 2 is it is characterised in that in step 2, Described slow release precipitator is one or more of ammonium carbonate, ammonium hydrogen carbonate and carbamide；Described slow release precipitator molal quantity For the total mole number of manganese source, tungsten source and titanium source 8～20 times.
5. the preparation method of high temperature resistant manganese-base oxide catalyst according to claim 2 is it is characterised in that in step 3, Described heating-up temperature is 80～90 DEG C；The described stirring sedimentation time is 6～12h.
6. the preparation method of high temperature resistant manganese-base oxide catalyst according to claim 2 is it is characterised in that in step 5, Described drying temperature is 90～110 DEG C.
7. the preparation method of high temperature resistant manganese-base oxide catalyst according to claim 2 is it is characterised in that in step 5, Described roasting is carried out in air atmosphere；Sintering temperature is 400～800 DEG C, and roasting time is 1～24h.
CN201610844375.5A 2016-09-22 2016-09-22 High-temperature resistant manganite catalyst and preparation method thereof Pending CN106362733A (en)

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CN116099529A (en) * 2023-01-28 2023-05-12 中国科学院城市环境研究所 Transition metal modified vanadium-based catalyst and preparation method and application thereof

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CN112844428A (en) * 2019-11-28 2021-05-28 中冶京诚工程技术有限公司 Vanadium-free modified manganese-based NH3-SCR denitration catalyst and preparation method and application thereof
CN115193432A (en) * 2022-07-06 2022-10-18 四川大学 High-temperature-aging-resistant lanthanum-doped spherical manganese oxide catalyst and preparation thereof
CN116099529A (en) * 2023-01-28 2023-05-12 中国科学院城市环境研究所 Transition metal modified vanadium-based catalyst and preparation method and application thereof

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