CN108786865A - A kind of catalyst and preparation method thereof for flue gas demercuration - Google Patents

A kind of catalyst and preparation method thereof for flue gas demercuration Download PDF

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Publication number
CN108786865A
CN108786865A CN201810522422.3A CN201810522422A CN108786865A CN 108786865 A CN108786865 A CN 108786865A CN 201810522422 A CN201810522422 A CN 201810522422A CN 108786865 A CN108786865 A CN 108786865A
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catalyst
flue gas
demercuration
titanium dioxide
mercury
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CN201810522422.3A
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Inventor
郭瑞堂
王�忠
王忠一
施旭
柳星宇
秦浩
刘健
孙晓
刘帅伟
李明圆
孙鹏
刘树明
潘卫国
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Shanghai University of Electric Power
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Priority to CN201810522422.3A priority Critical patent/CN108786865A/en
Publication of CN108786865A publication Critical patent/CN108786865A/en
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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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06—Halogens; Compounds thereof
    • B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
    • 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
    • B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (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 present invention provides a kind of catalyst for flue gas demercuration, and using titanium dioxide as carrier, doped with manganous bromide in the carrier, the mass ratio of the manganous bromide and titanium dioxide is 4 ~ 15：100.The present invention also provides a kind of preparation methods of above-mentioned catalyst for flue gas demercuration, including soluble manganous bromide is dissolved in deionized water, are stirred under room temperature；After manganous bromide is completely dissolved, titanium dioxide is added in bromination manganese solution, the mass ratio of the manganous bromide and titanium dioxide is 4 ~ 15：100；Mixed liquor is subjected to ultrasonic water bath processing；After ultrasonic water bath, mixed liquor is stood at room temperature；Mixed liquor after standing is placed in baking oven, the catalyst for flue gas demercuration is can be obtained after dry.The catalyst of the present invention is attained by 100% demercuration efficiency at 200 DEG C or more, and preparation method is simple and fast, and flue gas demercuration efficiency can be significantly improved under conditions of no HCl, has certain anti-poisoning ability.

Description

A kind of catalyst and preparation method thereof for flue gas demercuration
Technical field
The invention belongs to chemical fields, are related to a kind of catalyst, specifically a kind of catalyst for flue gas demercuration And preparation method thereof.
Background technology
Hazards in Power Plant is most important artificial mercury emissions source, is counted according to Environmental Protection Agency, about 31% in atmospheric environment Mercury comes from thermal power plant's burning of coal, and coal-fired mercury pollution has become after coal-burning boiler sulfur dioxide, nitrogen oxides pollution again One big pollution problem.China formally becomes within 2016《Minamata pact about mercury》Pi Yue states, under its requirement, the coal-fired electricity in China Factory may implement most stringent of mercury emissions limit value (0.003mg/m3), this brings sternness to coal-burning power plant's mercury control and chooses War.Further, since in sludge mercury concentration several times in etc. quality fire coal, sludge mixed burning boiler mercury emissions are often exceeded, with More and more sludge mix the landing of burning project, and the demand of flue gas demercuration technology gradually increases.
Flue gas desulfurization device and selective catalytic reduction equipment can trap mercury well.It can be with using wet desulphurization device In flue gas 80%~95% oxidation state mercury is removed, but not notable for gaseous mercury capture effect not soluble in water, needs to make First Elemental Mercury is aoxidized with oxidant.Therefore, this technology develop it is a kind of can be by Hg on the basis of SCR technologies0It urges Change is oxidized to Hg2+Catalyst have secondary pollution and higher production cost the problems such as.And mercurial is disclosed in currently available technology, Its demercuration performance is undesirable, since the mercury removal agent that the mercury of mercury removal agent holds and demercuration efficiency is all smaller and many is required for vulcanization It can work, this makes in the not only preparation or use in adsorbent all there may be secondary pollution problem in addition, current institute The oxidability of the monometallic mercury removal agent of use is low, it is difficult to the mercury of metallic state is converted into the mercury for the oxidation state that steam forces down, institute Not generate there is an urgent need to a kind of high-performance and more metal active mercury removal agents of secondary pollution.
Various technologies have been proposed, to develop for the technology from coal-burning power plant's high-efficient mercury removing, such as utilize absorption The demercuration technology of agent and catalyst.In many catalyst studied, the SCR catalyst of titanium dichloride load is considered as It is most promising, and its mechanism is by in-depth study.For most of adsorbents and catalyst, such as transiting metal oxidation Object and noble metal sill, HCl is in Hg in flue gas0Key effect is played in removal process.But in some kinds of coal only There are a small amount of Cl, therefore the Hg in these flue gases0It is difficult to remove.
Therefore how in the environment of no HCl, design that a kind of demercuration efficiency is high, and preparation method is simple and convenient, and with compared with The demercuration catalyst of wide temperature window, becoming the art has problem to be solved.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides a kind of catalyst for flue gas demercuration and its Preparation method, described this catalyst for flue gas demercuration and preparation method thereof will solve catalyst pair in the prior art Hg in flue gas0The bad technical problem of removal effect.
The present invention provides a kind of catalyst for flue gas demercuration, using titanium dioxide as carrier, in the carrier Doped with manganous bromide, the mass ratio of the manganous bromide and titanium dioxide is 4~15：100.
Further, the mass percent of the manganous bromide and titanium dioxide is respectively 4：100,7：100, 10：100 Or 15：100.
It is preferred that being 10 by mass ratio：100 manganous bromide and titanium dioxide mixes.
The present invention also provides a kind of preparation methods of above-mentioned catalyst for flue gas demercuration, include the following steps：
1) soluble manganous bromide is dissolved in deionized water, a concentration of 10mg/mL, temperature is lower to stir 15-20min；
2) after manganous bromide is completely dissolved, titanium dioxide is added in bromination manganese solution, the manganous bromide and dioxy The mass ratio for changing titanium is 4~15：100；
3) mixed liquor is subjected to ultrasonic water bath processing；
4) after ultrasonic water bath, mixed liquor is stood at room temperature；
5) mixed liquor after standing is placed in baking oven, the catalyst for flue gas demercuration is can be obtained after dry.
Further, the manganous bromide is MnBr2·4H2O。
Further, the temperature that ultrasonic water bath is carried out in step 2) is 40 DEG C, and processing time is 1.5~2h.
Further, the time stood at room temperature in step 3) is 24~36h.
Further, the temperature requirement of step 4) drying is 110 DEG C, and the time is 12~15h.
Preferably, the time of step (2) stirring is about 10~15 minutes, to promote filling for titanium dioxide and bromination manganese solution Tap is touched, so that dipping as possible uniform.
The present invention also provides a kind of above-mentioned application for the catalyst of flue gas demercuration in flue gas mercury control, packets Include following steps：
1) it before demercuration starts, is first passed through nitrogen by-passing and makes mercury source constant without catalyst, until mercury source is stablized 130μg/m3；
2) it opens main road and closes bypass, i.e., at normal temperatures catalyst is passed through, achieve the purpose that pre- absorption so that catalysis Agent is to Hg0Physical absorption close to saturation, avoid subsequently calculate demercuration efficiency error；
3) when pre- absorption reaches saturation, opening program opens mixed flue gas and is sent to fixed bed reactors, control reaction temperature Degree is 100 DEG C -350 DEG C, flow velocity 1000ml/min.Air speed is 160000h-1, under the effect of the catalyst, by Hg0It is oxidized to Hg2+；
4) flue gas is by the front and back Hg of demercuration catalyst reaction0Concentration is recorded by VM3000 mercury vapourmeters, according to cigarette Mercury quantity variation calculates demercuration efficiency of the catalyst to flue gas in gas.
Further, simulated flue gas composition：NH3For 500ppm, oxygen 4%, Hg0A concentration of 130 μ g/m3, Remaining gas is the Ar as Balance Air.
The specific preparation method of catalyst of the present invention is：Four water manganous bromides are dissolved in deionized water, stirs, it is made to add Instant solution.A certain amount of titania powder is impregnated into obtained bromination manganese solution, after ultrasonic water bath processing, in room Temperature is lower to impregnate diel.Mixture is put into drying in baking oven later and removes water, you can obtains required catalyst.The present invention In, several groups of best catalyst of ratio are attained by 100% demercuration efficiency at 200 DEG C or more, and preparation method is simple and fast, and And flue gas demercuration efficiency can be significantly improved under conditions of no HCl, have certain anti-poisoning ability, there is stronger industry to answer With value, the removing of mercury in flue gas can be widely applied to.
The present invention is using manganous bromide as active component, using titanium dioxide as active carrier, the preparation of catalyst using Four quantitative water manganous bromides are first dissolved into quantitative deionized water, then titanium dioxide direct impregnation are got on by infusion process.
The present invention is compared with prior art, and technological progress is significant.Demercuration catalyst of the present invention not sulfur-bearing, , using titanium dioxide as carrier, manganous bromide is active component for it, and there is demercuration catalyst obtained the mercury more than 10%wt to hold, Demercuration efficiency can reach 99.9% or more.Method for preparing catalyst of the present invention is simple and practicable, prepares raw material and is easily obtained, can be extensive In removing process applied to mercury metal in flue gas air source.Demercuration catalyst of the present invention can thoroughly break away from flue gas demercuration pair The dependence of HCl has wider demercuration temperature window and high demercuration efficiency.
Description of the drawings
Fig. 1 is a kind of XRD characterization figure of catalyst for flue gas demercuration of the invention.
Fig. 2 is a kind of SEM figures of catalyst for flue gas demercuration of the invention of 10%-manganous bromide/titanium dioxide.
Fig. 3 is a kind of EDS elemental analyses of catalyst for flue gas demercuration of the invention.
Specific implementation mode
The present invention is expanded on further in used specific embodiment below, but is not intended to limit the present invention.
The present invention example used in catalytic reactor use be purchased from Zhejiang Fan Tai Instrument Ltd. outer diameter for The 4100 type fixed bed micro anti-evaluation devices of 16mm, long 480mm, unstripped gas enter reactor by preheating, and reaction temperature exists 100-350 DEG C, flow velocity 1000ml/min, air speed ratio is 108000h-1。
Simulated flue gas forms：Hg0For 130 μ g/m3, NH3For 600ppm and O2It is 5%, remaining gas Ar is as balance Gas, gas flow is by the CS200 type mass flowmenters control purchased from Beijing Co., Ltd of Sevenstar Huachuang Electronic.
NO used in the present invention, NH3Molar concentration is 1%, O2It is 5%, remaining gas Ar is purchased from Shanghai as Balance Air Wei Chuan calibrating gas Co., Ltd；
Drug used is purchased from Aladdin.
Embodiment 1
It is used for catalysis oxidation Hg according to what the present invention made0Catalyst, the mass ratio of wherein active component and carrier is 4:100.Specific preparation process is as follows：
Tetra- water manganous bromides of 0.267g are dissolved in 30 ml deionized waters, stirs at room temperature 15 minutes and accelerates dissolving；It connects Addition 5g titanium dioxide solids, stirring makes titanium dioxide and solution come into full contact in 5 minutes；By the mixed liquor ultrasonic water bath of gained Processing 2 hours, then stands diel at room temperature；Finally, above-mentioned mixed liquor is placed in drying 12 hours in 110 DEG C of baking ovens, A kind of high-efficiency mercury removal catalyst (A) is made.
Embodiment 2
It is used for catalysis oxidation Hg according to what the present invention made0Catalyst, the mass ratio of wherein active component and carrier is 7:100.Specific preparation process is as follows：
Tetra- water manganous bromides of 0.4674g are dissolved in 30 ml deionized waters, stirs at room temperature 15 minutes and accelerates dissolving；It connects Addition 5g titanium dioxide solids, stirring makes titanium dioxide and solution come into full contact in 5 minutes；By the mixed liquor ultrasonic water bath of gained Processing 2 hours, then stands diel at room temperature；Finally, above-mentioned mixed liquor is placed in drying 12 hours in 110 DEG C of baking ovens, A kind of high-efficiency mercury removal catalyst (B) is made.
Embodiment 3
It is used for catalysis oxidation Hg according to what the present invention made0Catalyst, the mass ratio of wherein active component and carrier is 10:100.Specific preparation process is as follows：
Tetra- water manganous bromides of 0.668g are dissolved in 30 ml deionized waters, stirs at room temperature 15 minutes and accelerates dissolving；It connects Addition 5g titanium dioxide solids, stirring makes titanium dioxide and solution come into full contact in 5 minutes；By the mixed liquor ultrasonic water bath of gained Processing 2 hours, then stands diel at room temperature；Finally, above-mentioned mixed liquor is placed in drying 12 hours in 110 DEG C of baking ovens, A kind of high-efficiency mercury removal catalyst (C) is made.
Embodiment 4
It is used for catalysis oxidation Hg according to what the present invention made0Catalyst, the mass ratio of wherein active component and carrier is 15:100.Specific preparation process is as follows：
Tetra- water manganous bromides of 1.002g are dissolved in 30 ml deionized waters, stirs at room temperature 15 minutes and accelerates dissolving；It connects Addition 5g titanium dioxide solids, stirring makes titanium dioxide and solution come into full contact in 5 minutes；By the mixed liquor ultrasonic water bath of gained Processing 2 hours, then stands diel at room temperature；Finally, above-mentioned mixed liquor is placed in drying 12 hours in 110 DEG C of baking ovens, A kind of high-efficiency mercury removal catalyst (D) is made.
Experiment test first uses the gaseous state Hg in simulated flue gas before starting0It is passed through fixed bed micro anti-evaluation device, allows catalyst Saturation is reached to the absorption of gaseous mercury, avoids causing the Hg detected because of suction-operated when reaction0Reduction；Simulate gas (flue gas flow rate 1000ml/min, gas concentration：Hg0For 130 μ g/m3, NO 600ppm, NH3For 600ppm and O2It is 5%, Remaining gas is Ar) fixed bed micro anti-evaluation device is sent into after mixing, at 100 DEG C~350 DEG C, made by the oxidation of catalyst With by Hg0It is oxidized to Hg2+, the Hg of inlet and outlet0Concentration is detected using VM3000 mercury vapourmeters, and demercuration effect is as shown in table 1.
The Activity evaluation tables of data of 1 different catalysts of table
Element proportion in 2 catalyst of table
Element Line type Apparent concentration K ratios Wt% Wt%Sigma Atomic percent
O K linear systems 96.17 0.84248 34.05 0.98 62.74
Ti L linear systems 177.60 1.77597 51.91 1.36 31.95
Mn L linear systems 1.66 0.01660 0.83 0.95 0.45
Br L linear systems 44.30 0.40655 13.21 0.50 4.87
Total amount: 100.00 100.00
It can show that manganous bromide is sufficiently impregnated on carrier titanium dioxide from Fig. 1, Fig. 2, table 2, distribution is good.Pass through table 1 it is found that the demercuration catalyst demercuration significant effect that the catalyst preparation of the present invention obtains, can reach close at 200 DEG C or more 100% demercuration efficiency.Demercuration efficiency described here refers to the percentage of the mercury quantity and the amount of mercury in Primordial Qi source of removing.It can See there is higher demercuration activity using demercuration catalyst of the present invention, and there is wider reaction temperature window, and The dependence to HCl has been broken away from demercuration reaction, and preparation process is easy, has very good application prospect.
The wave crest in addition to titanium dioxide is found no in the characterization result (Fig. 1) of XRD to occur, and shows manganous bromide well It has loaded on carrier.In addition, in SEM characterization results (Fig. 2) and EDS elemental analyses (Fig. 3, table 2), load has also been embodied The presence of manganous bromide above body titanium dioxide.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.

Claims (9)

1. a kind of catalyst for flue gas demercuration, it is characterised in that：Using titanium dioxide as carrier, adulterated in the carrier There is a manganous bromide, the mass ratio of the manganous bromide and titanium dioxide is 4~15：100.
2. a kind of catalyst for flue gas demercuration according to claim 1, it is characterised in that：The manganous bromide and two The mass percent of titanium oxide is respectively 4：100,7：100,10：100 or 15：100.
3. a kind of preparation method of catalyst for flue gas demercuration described in claim 1, it is characterised in that including following step Suddenly：
1) soluble manganous bromide is dissolved in deionized water, makes its a concentration of 10mg/mL, 15-20min is stirred under room temperature；
2) after manganous bromide is completely dissolved, titanium dioxide is added in bromination manganese solution, the manganous bromide and titanium dioxide Mass ratio be 4~15：100；
3) mixed liquor is subjected to ultrasonic water bath processing；
4) after ultrasonic water bath, mixed liquor is stood at room temperature；
5) mixed liquor after standing is placed in baking oven, the catalyst for flue gas demercuration is can be obtained after dry.
4. a kind of preparation method of catalyst for flue gas demercuration according to claim 2, it is characterised in that：Described Manganous bromide is MnBr2·4H2O。
5. a kind of preparation method of catalyst for flue gas demercuration according to claim 2, it is characterised in that：Step 2) The middle temperature for carrying out ultrasonic water bath is 40 DEG C, and processing time is 1.5~2h.
6. a kind of preparation method of catalyst for flue gas demercuration according to claim 2, it is characterised in that：Step 3) In time for standing at room temperature be 24~36h.
7. a kind of preparation method of catalyst for flue gas demercuration according to claim 2, it is characterised in that：Step 4) The temperature requirement of drying is 110 DEG C, and the time is 12~15h.
8. a kind of application for the catalyst of flue gas demercuration in flue gas mercury control described in claim 1, feature exist In including the following steps：
1) it before demercuration starts, is first passed through nitrogen by-passing and makes mercury source constant without catalyst, until mercury source is stablized in 130 μ g/m3；
2) it opens main road and closes bypass, i.e., at normal temperatures catalyst is passed through, achieve the purpose that pre- absorption so that catalyst pair Hg0Physical absorption close to saturation, avoid subsequently calculate demercuration efficiency error；
3) when pre- absorption reaches saturation, opening program opens mixed flue gas and is sent to fixed bed reactors, and controlling reaction temperature is 100 DEG C -350 DEG C, flow velocity 1000ml/min.Air speed is 160000h-1, under the effect of the catalyst, by Hg0It is oxidized to Hg2+；
4) flue gas is by the front and back Hg of demercuration catalyst reaction0Concentration is recorded by VM3000 mercury vapourmeters, according to mercury in flue gas Amount variation calculates demercuration efficiency of the catalyst to flue gas.
9. a kind of catalyst for flue gas demercuration answering in flue gas mercury control according to claim 8 With, which is characterized in that the simulated flue gas composition：NH3For 500ppm, oxygen 4%, Hg0A concentration of 130 μ g/m3, remaining Gas is the Ar as Balance Air.
CN201810522422.3A 2018-05-28 2018-05-28 A kind of catalyst and preparation method thereof for flue gas demercuration Pending CN108786865A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110523419A (en) * 2019-08-09 2019-12-03 上海电力大学 Catalyst for flue gas demercuration and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102366722A (en) * 2011-11-21 2012-03-07 国电科学技术研究院 Denitrition catalyst with mercury removal effect and its preparation method
CN102962083A (en) * 2012-11-29 2013-03-13 昆明冶金研究院 Modified catalyst for gaseous-state elemental mercury oxidation and preparation method of modified catalyst

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102366722A (en) * 2011-11-21 2012-03-07 国电科学技术研究院 Denitrition catalyst with mercury removal effect and its preparation method
CN102962083A (en) * 2012-11-29 2013-03-13 昆明冶金研究院 Modified catalyst for gaseous-state elemental mercury oxidation and preparation method of modified catalyst

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110523419A (en) * 2019-08-09 2019-12-03 上海电力大学 Catalyst for flue gas demercuration and preparation method thereof

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Application publication date: 20181113