CN102698771A - Catalyst for removing mercury from flue gas and preparation method of same - Google Patents
Catalyst for removing mercury from flue gas and preparation method of same Download PDFInfo
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- CN102698771A CN102698771A CN2012101798077A CN201210179807A CN102698771A CN 102698771 A CN102698771 A CN 102698771A CN 2012101798077 A CN2012101798077 A CN 2012101798077A CN 201210179807 A CN201210179807 A CN 201210179807A CN 102698771 A CN102698771 A CN 102698771A
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Abstract
The invention discloses a catalyst for removing mercury from flue gas and a preparation method of the catalyst. The catalyst is prepared in the way that manganese salt and ferric salt are loaded with modified coal ash, wherein the total load of manganese element and iron element is 2-25 wt%. The experimental result shows that the catalyst is an efficient and economical mercury removal adsorbent. The catalyst has the advantages as follows: the raw material is easy to purchase; the catalyst is easy to prepare, low in cost and high in performance-price ratio; the catalyst can stably maintain high activity for a longer time; and mercuric oxide formed on the surface of the catalyst can be stably adsorbed on the surface of the catalyst at the temperature of less than 300 DEG C, which facilitates regeneration processing of the catalyst and recycling of mercury.
Description
Technical field
The present invention relates to the comprehensive utilization and the flue gas demercuration field of flyash, be specifically related to a kind of flue gas demercuration adsorbent by the preparation of manganese salt and molysite modified coal ash and preparation method thereof.
Background technology
In recent years, it should be noted that the poisonous metal element that produces in the coal combustion process has bigger influence to environment, wherein mercury is exactly one of very harmful element.Mercury is a kind ofly to have permanent cumulative noxious material in vivo with in the food chain, also is global cyclic elements, can produce certain influence to human ecological environment.
Coal-burning boiler is as causing the main anthropogenic discharge source of environment mercury pollution to cause extensive concern at world wide.According to the data of Environmental Protection Agency, about 31% mercury comes from the coal combustion of coal-burning power plant in the atmospheric environment, in artificial mercury emissions source, occupies first.The average content of mercury is 0.22mg/kg in China's coal; Simultaneously, China is a big coal country, and annual coal consumption amount is about 2,000,000,000 tons; Wherein be used as coal fired power generation more than 70%, so the mercury emissions in the control coal-fired flue-gas has become a main direction of mercury in the control atmosphere.
Mercury in the flue gas has gaseous elemental mercury (Hg
0), gaseous state divalence mercury (Hg
2+) and particle mercury (Hg
p) wait 3 kinds of forms.When flue gas process SCR reactor, section H g
0Be oxidized to and be easier to be absorbed Hg
2+, Hg during through electrostatic precipitator
pBe removed, flue gas passes through Hg behind the desulfurization absorption plant at last
2+Be absorbed and remove, but SCR is to Hg
0Oxidability limited, some Hg of flue gas
0Not oxidized, so because its character is relatively stable difficult to its control through existing after-treatment device, so this part Hg
0Row has caused the Hg pollution to atmosphere.At present, the method for control mercury pollution discharging mainly is an adsorbents adsorb, and wherein effective adsorbent is an active carbon the most, but its cost is very high, has limited the application of adsorbent demercuration.Therefore seek simply, cheap adsorbent becomes present urgency problem to be solved.
China all can produce a large amount of flyash every year, and at present, the comprehensive utilization of flyash has expanded to fields such as agricultural, material, building, and for demercuration, domestic only have a minority report.Absorption comprises physical absorption and chemisorbed, and absorption has shortcomings such as the absorption of being prone to is saturated, poor activity, consumption height, regeneration poor performance, so the effect that catalytic oxidation is replaced being adsorbed in the demercuration becomes the technical problem that present urgent need solves.
Summary of the invention
The purpose of this invention is to provide a kind of coal-fired flue-gas Hg that is used for removing
0Catalyst, replace the effect of absorption with catalytic oxidation, its demercuration efficient is high, tolerance time is long, and is with low cost, product does not produce secondary pollution, reaches requirement on industrial application.
Another object of the present invention provides a kind of above-mentioned Preparation of catalysts method.
The object of the invention can reach through following measure:
A kind of flue gas demercuration catalyst, this catalyst are manganese salt and the loaded modified flyash of molysite, and wherein the total load amount of manganese element and ferro element is 2～25wt%.
The total load amount of manganese element and ferro element is preferably 5～15wt% in this catalyst, further is preferably 8～12wt%, most preferably is 10wt%.
The manganese element of load and the mol ratio between the ferro element are preferably 0.1～10:3 in this catalyst, further are preferably 0.5～5:3, and more preferably 1～4:3 most preferably is 2～3:3.
Manganese salt among the present invention is the acylate or the inorganic acid salt of manganese, like manganese carbonate, sodium permanganate, nitric acid, manganese acetate etc., preferably adopts manganese acetate (CH3COO) 2Mn4H2O.
Molysite is the acylate or the inorganic acid salt of iron, like ironic citrate, ferric sulfate, ferric nitrate, iron chloride, ferric phosphate etc., preferably adopts ferric nitrate Fe (NO
3)
39H
2O.
The invention also discloses the loaded modified method or the preparation method of this catalyst; Be specially: after the dry also pulverizing of flyash washing; Putting into the mixed solution that is dissolved with manganese salt and molysite floods; At 60 ℃～100 ℃ following evaporate to dryness solution, in 450 ℃～550 ℃ calcinings down, the cooling of calcining back grinds with the flyash oven dry back that obtains.
In said method, flyash washing drying and crushing method is: after flyash spends deionised water, in 110 ℃～130 ℃ (preferred 120 ℃) oven dry down, ground 200 mesh sieves after the cooling.
Each raw material among the preparation method and consumption as stated, wherein manganese salt and molysite feed intake by the molar ratio computing between manganese in the catalyst and the ferro element.Above-mentioned flyash calcining back cooling grinds to crossing 200 mesh sieves.
The catalyst of the present invention's preparation can be applicable to remove Hg in the coal-fired flue-gas
0The present invention is at simulated flue gas (air and Hg
0) under the atmosphere research catalyst to Hg
0Adsorption capacity.Manganese salt and molysite that mechanism of the present invention is to load on the flyash interact, and the surface produces a large amount of cation vacancy and Mn
4+, Hg
0At first be adsorbed on the cation vacancy, at last by Mn
4+Be oxidized to HgO, Mn
4+Be reduced into Mn
3+, but at O
2Mn under the condition
3+Be oxidized to Mn
4+Thereby, make catalyst maintain higher activity always.Experimental result shows that catalyst of the present invention is a kind of efficient, economic demercuration adsorbent, is in particular in:
(1) raw material is prone to buy, and catalyst is prone to preparation, and cost is low, and cost performance is high.
(2) catalyst in a long time can the certain high activity of stable maintenance, and what it played is not general suction-operated, but catalytic action.
(3) HgO that forms of catalyst surface is adsorbed on catalyst surface stablizing below 300 ℃, helps the Regeneration Treatment of catalyst and the recycling of mercury.
Description of drawings
Fig. 1 removes the experimental stand sketch map for air atmosphere mercury;
Fig. 2 is under the 10% load capacity condition, and the mol ratio modified coal ash of different Mn/Fe is to Hg
0Removal effect.Wherein FA is pure flyash.
The specific embodiment
Comparative Examples 1
Mn (0)-Fe (3)-FA (the mol ratio 0:3 of Mn/Fe) Preparation of Catalyst: take by weighing the 2.4g ferric nitrate; Put into the crucible of 100ml, add the 50ml deionized water again, be stirred to and add 3g flyash behind the homogeneous solution; Mix, under 80 ℃, be stirred to the solution evaporate to dryness.The flyash of oven dry is calcined 4h with 500 ℃ in Muffle furnace, the catalyst of calcining out ground 200 mesh sieves after cooling off naturally, promptly made Mn (0)-Fe (3)-FA and removed Hg
0Catalyst.
Comparative Examples 2
Mn (1)-Fe (0)-FA (the mol ratio 1:0 of Mn/Fe) Preparation of Catalyst: take by weighing the 1.48g manganese acetate; Put into the crucible of 100ml, add the 50ml deionized water again, be stirred to and add 3g flyash behind the homogeneous solution; Mix, under 80 ℃, be stirred to the solution evaporate to dryness.The flyash of oven dry is calcined 4h with 500 ℃ in Muffle furnace, the catalyst of calcining out ground 200 mesh sieves after cooling off naturally, promptly made Mn (1)-Fe (0)-FA and removed Hg
0Catalyst.
Mn (1)-Fe (3)-FA (the mol ratio 1:3 of Mn/Fe) Preparation of Catalyst: take by weighing 1.8g ferric nitrate and 0.37g manganese acetate respectively; Put into the crucible of 100ml, add the 50ml deionized water again, be stirred to and add 3g flyash behind the homogeneous solution; Mix, under 80 ℃, be stirred to the solution evaporate to dryness.The flyash of oven dry is calcined 4h with 500 ℃ in Muffle furnace, the catalyst of calcining out ground 200 mesh sieves after cooling off naturally, promptly made Mn (1)-Fe (3)-FA and removed Hg
0Catalyst.
Mn (2)-Fe (3)-FA (the mol ratio 2:3 of Mn/Fe) Preparation of Catalyst: take by weighing 1.45g ferric nitrate and 0.59g manganese acetate respectively; Put into the crucible of 100ml, add the 50ml deionized water again, be stirred to and add 3g flyash behind the homogeneous solution; Mix, under 80 ℃, be stirred to the solution evaporate to dryness.The flyash of oven dry is calcined 4h with 500 ℃ in Muffle furnace, the catalyst of calcining out ground 200 mesh sieves after cooling off naturally, promptly made Mn (1)-Fe (3)-FA and removed Hg
0Catalyst.
For understanding the performance of catalyst of the present invention, the spy studies it to Hg under air conditions
0Adsorption capacity.The mercury removal experimental bench is shown in figure one, and it is by source of the gas (carrier gas N
2, air), flowmeter, water-bath, U-shaped pipe, mercury osmos tube, heating furnace, QM201H mercury vapourmeter form.Wherein reactor is a quartz ampoule in the fixed bed, and what use in the pipeline is that polyfluortetraethylene pipe prevents Hg
0Adsorption condensing.Catalyst amount is 1g in the test; Getting into the online total gas flow rate of mercury is 1000mL/min, wherein passes through the N of mercury osmos tube
2Throughput is 200mL/min, N
2Be carrier gas; Mercury vapour is by N
2Provide through thermostat water bath heating mercury osmos tube, the pipeline in the experimental provision is wrapped with the heating tape and is incubated; Mercury concentration is about 20 μ g/m3 in the test.Mercury concentration is measured by QM201H mercury vapourmeter and online recording system.
To modified coal ash catalyst removal Hg in embodiment and the Comparative Examples
0Experiment show that the flyash of manganese salt and the common modification of molysite has higher demercuration efficient, and can in 8 hours of experiment, keep stable high activity always, do not have the absorption saturated phenomenon, what it rose is not general suction-operated, but stable catalytic action.Adopt the flyash mercury removal agent of manganese salt and molysite modification, can reach industrial application requirements.
To modified coal ash catalyst removal Hg in embodiment 1 and 2
0Experiment show that along with the increase of manganese salt dopping amount, the removal efficiency of mercury increases, the mercury removal rate is considered the economic problems in the practical application near 100% when the mol ratio of Mn/Fe is 2:3, this is the catalyst of best proportioning.
Claims (10)
1. a flue gas demercuration catalyst is characterized in that this catalyst is manganese salt and the loaded modified flyash of molysite, and wherein the total load amount of manganese element and ferro element is 2～25wt%.
2. flue gas demercuration catalyst according to claim 1 is characterized in that the total load amount of manganese element and ferro element is 5～15wt% in this catalyst.
3. flue gas demercuration catalyst according to claim 1 is characterized in that the manganese element of load in this catalyst and the mol ratio between the ferro element are 0.1～10:3.
4. flue gas demercuration catalyst according to claim 3 is characterized in that the manganese element of load in this catalyst and the mol ratio between the ferro element are 0.5～5:3.
5. flue gas demercuration catalyst according to claim 1 is characterized in that acylate or inorganic acid salt that said manganese salt is manganese, and said molysite is the acylate or the inorganic acid salt of iron.
6. flue gas demercuration catalyst according to claim 5 is characterized in that said manganese salt is manganese acetate, and said molysite is a ferric nitrate.
7. flue gas demercuration catalyst according to claim 1; The loaded modified method that it is characterized in that this catalyst is: after the dry also pulverizing of flyash washing; Putting into the mixed solution that is dissolved with manganese salt and molysite floods; At 60 ℃～100 ℃ following evaporate to dryness solution, in 450 ℃～550 ℃ calcinings down, the cooling of calcining back grinds with the flyash oven dry back that obtains.
8. flue gas demercuration catalyst according to claim 7 is characterized in that said flyash washing drying and crushing method is: after flyash spends deionised water, 110 ℃～130 ℃ oven dry down, ground 200 mesh sieves after the cooling.
9. the said flue gas demercuration Preparation of catalysts of claim 1 method; It is characterized in that after the dry also pulverizing of flyash washing; Putting into the mixed solution that is dissolved with manganese salt and molysite floods; At 60 ℃～100 ℃ following evaporate to dryness solution, in 450 ℃～550 ℃ calcinings down, the cooling of calcining back grinds with the flyash oven dry back that obtains; Wherein manganese salt is the acylate or the inorganic acid salt of manganese, and said molysite is the acylate or the inorganic acid salt of iron; The manganese element of load and the mol ratio between the ferro element are 0.1～10:3 in this catalyst.
10. method according to claim 9 is characterized in that said flyash washing drying and crushing method is: after flyash spends deionised water, 110 ℃～130 ℃ oven dry down, ground 200 mesh sieves after the cooling; Said manganese salt is manganese acetate, and said molysite is a ferric nitrate; The manganese element of load and the mol ratio between the ferro element are 0.5～5:3 in the catalyst; Flyash calcining back cooling grinds to crossing 200 mesh sieves.
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|---|---|---|---|
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111128A (en) * | 2013-02-22 | 2013-05-22 | 广东电网公司电力科学研究院 | Dust-removal mercury-removal filter bag for bag-type dust remover and preparation method of filter bag |
| CN105148841A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | High temperature resistant mercury adsorbing agent |
| CN105148865A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Gas adsorbent |
| CN105148840A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Coal ash flue gas demercuration adsorbent |
| CN105148863A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Pump adsorbent |
| CN105148862A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Adsorbent having long storage time and low failure rate |
| CN105148873A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Dust-removing and smoke-removing adsorbent |
| CN105148874A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Composite porous flue gas adsorbent |
| CN105148861A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Multifunctional adsorbent |
| CN105148864A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Fly ash-based heavy metal absorbent |
| CN105195104A (en) * | 2015-09-01 | 2015-12-30 | 安徽省含山县天顺环保设备有限公司 | Adsorbing agent capable of purifying car exhaust |
| CN105688931A (en) * | 2016-03-09 | 2016-06-22 | 铜仁学院 | Novel method for preparing coal-fired flue gas mercury-removal catalyst from rhodochrosite |
| CN105688800A (en) * | 2016-01-22 | 2016-06-22 | 安庆师范学院 | MnO2/flyash-attapulgite catalyst/adsorbent and method thereof for removing elemental mercury in smoke |
| CN105921143A (en) * | 2016-05-16 | 2016-09-07 | 南通南京大学材料工程技术研究院 | Vanadate smoke zero-valent mercury oxidation catalyst based on attapulgite |
| CN108993375A (en) * | 2018-07-02 | 2018-12-14 | 上海电力学院 | A kind of demercuration manganese iron cerium adsorbent and preparation method thereof |
| CN115779892A (en) * | 2022-12-08 | 2023-03-14 | 华北电力大学（保定） | Catalyst for high-efficiency demercuration of flue gas and preparation method thereof |
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| CN103111128A (en) * | 2013-02-22 | 2013-05-22 | 广东电网公司电力科学研究院 | Dust-removal mercury-removal filter bag for bag-type dust remover and preparation method of filter bag |
| CN105148861A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Multifunctional adsorbent |
| CN105148874A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Composite porous flue gas adsorbent |
| CN105148840A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Coal ash flue gas demercuration adsorbent |
| CN105148863A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Pump adsorbent |
| CN105148864A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Fly ash-based heavy metal absorbent |
| CN105148873A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Dust-removing and smoke-removing adsorbent |
| CN105148865A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Gas adsorbent |
| CN105148841A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | High temperature resistant mercury adsorbing agent |
| CN105148862A (en) * | 2015-09-01 | 2015-12-16 | 安徽省含山县天顺环保设备有限公司 | Adsorbent having long storage time and low failure rate |
| CN105195104A (en) * | 2015-09-01 | 2015-12-30 | 安徽省含山县天顺环保设备有限公司 | Adsorbing agent capable of purifying car exhaust |
| CN105688800A (en) * | 2016-01-22 | 2016-06-22 | 安庆师范学院 | MnO2/flyash-attapulgite catalyst/adsorbent and method thereof for removing elemental mercury in smoke |
| CN105688931A (en) * | 2016-03-09 | 2016-06-22 | 铜仁学院 | Novel method for preparing coal-fired flue gas mercury-removal catalyst from rhodochrosite |
| CN105688931B (en) * | 2016-03-09 | 2017-11-28 | 铜仁学院 | A kind of new method that coal-fired flue gas mercury removal catalyst is prepared using manganese spar |
| CN105921143A (en) * | 2016-05-16 | 2016-09-07 | 南通南京大学材料工程技术研究院 | Vanadate smoke zero-valent mercury oxidation catalyst based on attapulgite |
| CN108993375A (en) * | 2018-07-02 | 2018-12-14 | 上海电力学院 | A kind of demercuration manganese iron cerium adsorbent and preparation method thereof |
| CN115779892A (en) * | 2022-12-08 | 2023-03-14 | 华北电力大学（保定） | Catalyst for high-efficiency demercuration of flue gas and preparation method thereof |
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Application publication date: 20121003 |