CN107754799A - A kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material - Google Patents
A kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material Download PDFInfo
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- CN107754799A CN107754799A CN201711183713.6A CN201711183713A CN107754799A CN 107754799 A CN107754799 A CN 107754799A CN 201711183713 A CN201711183713 A CN 201711183713A CN 107754799 A CN107754799 A CN 107754799A
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- silicon slag
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Abstract
A kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material belongs to environmentally conscious materialses, environmental catalysis and field of environment protection.Ferro-silicon slag is the waste residue cleared out of during producing ferrosilicon from ladle, and the main component of ferro-silicon slag is:SiO2, CaO, MnO, MgO and Al2O3.The oxide of calcium in ferro-silicon slag, manganese, magnesium, aluminium is dissolved into mixed solution by this method using hydrochloric acid as lytic agent, according to the difference of each metal ion solubility product, pH=7~10 are adjusted as precipitating reagent using sodium hydroxide and produce precipitation, washing centrifugation, the content for reducing impurity element Ca and Mg is formed with SiO2、Al2O3For matrix, MnO is the manganese base demercuration catalysis material of active component.Demercuration catalysis material medium temperature demercuration activity prepared by the method is high, up to more than 90% in the range of 300 DEG C~450 DEG C.The present invention realizes the recycling of ferro-silicon slag, environmental protection, and the medium temperature demercuration catalysis material of preparation brings very big social benefit.
Description
Technical field
The invention belongs to environmental catalysis material and field of environment protection, is specially that one kind is prepared using industrial residue ferro-silicon slag
Medium temperature demercuration catalysis material.
Background technology
Mercury pollution is the global environmental problem currently to receive much concern.Manufacture of cement is the most important of global atmosphere mercury emissions
One of source.China's cement output occupies the first in the world for years.Government has put into effect relevant policies, revision《Water
Mud industrial atmosphere pollutant emission standard》(GB4915-2013) specific requirement, is proposed to the mercury emissions of cement kiln flue gas
0.05mg/m3.The discharge of mercury mainly passes through flue gas in manufacture of cement.The form of mercury in flue gas has gaseous state nonvalent mercury (Hg0), two
Valency ionic mercury (Hg2+) and particulate Hg (Hgp) 3 kinds.Tin ja et al. carried out on-the-spot test in 2010 to a cement plant, obtained
Nonvalent mercury, bivalent mercury, particulate Hg ratio are 65.7%, 34%, 0.3%.Yang Hai et al. gave birth in the cement to 5000t/d in 2014
Producing line gas mercury is tested, and is obtained the gaseous mercury of floss hole based on nonvalent mercury, is about accounted for more than 80%.
Ferro-silicon slag is the waste residue cleared out of during producing ferrosilicon from ladle, and the main component of ferro-silicon slag is:SiO2、
CaO, MnO, MgO and Al2O3If it can be effectively utilized for example for cement plant flue gas Hg0Removing, then can be to smoke pollution
The discharge of thing is controlled, while the cost of demercuration material is greatly reduced.This method can reduce impurity element Ca in ferro-silicon slag
Formed with Mg content with SiO2、Al2O3For matrix, MnO is that the manganese base demercuration of active component urges material.Jiangkun Xie etc.
People prepares the Mn-TiO of different manganese load capacity using template agent method2Catalyst, Mn-TiO2(10%) demercuration efficiency reaches at 300 DEG C
To 90%.Anchao Zhang prepare cobalt and manganese oxide modifying titanium dioxide (CoxMnyTi) catalyst using deposition-precipitation.
As a result show in Mn30Ti, with 6%Co optimum load amount, Hg0Oxidation efficiency can reach 98% or so at 150 DEG C.
MnOx (20%)-CeOx (10%)/SiO that Kuan-Hung Liu et al. are prepared using coprecipitation2Catalyst, at 150 DEG C
Demercuration efficiency reaches 96%.
Mn prepared by this methodxOy/SiO2-Al2O3The demercuration reaction of demercuration material follows Mars-Maessen mechanism:
Hg〔g)+MnxOy→Hg-O≡MnxOy-1 〔1)
Hg-O≡MnxOy-1→HgO+MnxOy-1 (2)
MnxOy-1+1/2O2→MnxOy (3)
Hg〔g)+2CuO→Hg-O≡Cu2O 〔4)
Hg-O≡Cu2O→HgO+Cu2O 〔5)
Cu2O+1/2O2→2CuO 〔6)
O ≡ represent the surface chemistry oxygen in catalyst in formula.
The content of the invention
It is the method that raw material prepares medium temperature demercuration catalyst it is an object of the invention to provide a kind of ferro-silicon slag.
A kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material, it is characterised in that:By ferro-silicon slag powder under 100 mesh sieves
Hydrochloric acid solution with 2.0~3.0mol/L is with solid-to-liquid ratio=1 gram:9 milliliters of ratio mixing, 2h, which is stirred at room temperature, becomes it
Mixed solution;Precipitating reagent is added, regulation mixed solution pH=7~10, continues to stir 30min;Deionized water centrifuges three times, separation
Go out bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material powder.
Further, one kind in precipitating reagent selection sodium hydroxide solution, ammonia spirit, sodium carbonate liquor.
A kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material, it is characterised in that:By ferro-silicon slag powder under 100 mesh sieves
Hydrochloric acid solution with 2.0mol/L is with solid-to-liquid ratio=1 gram:9 milliliters of ratio mixing, is stirred at room temperature 2h;Add copper nitrate,
The mass ratio for adding copper nitrate and ferro-silicon slag is 0.25~1.0, stirs 30min, adds NaOH solution regulation pH value of solution=9, after
Continuous stirring 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis
Material powder.
Demercuration efficiency of the present invention is in fixed reaction bed test.Simulated flue gas forms:60ug/m3Hg0, 6%O2, 12%
CO2, N2For Balance Air.Catalysis material is granulated first, takes particle of the granularity between the mesh of 40 mesh~60 to be tested, claims
Take 0.2000g catalyst to carry out demercuration performance test, test the demercuration efficiency of catalysis material under 100 DEG C~500 DEG C temperature conditionss,
The demercuration efficiency of catalysis material prepared by the present invention reaches as high as 96.2%.
Brief description of the drawings
Fig. 1 difference concentration of hydrochloric acid prepares catalysis material demercuration curve
Fig. 2 differences pH prepares catalysis material demercuration curve
Fig. 3 difference precipitating reagents prepare catalysis material demercuration curve
Fig. 4 different Cu load capacity prepares catalysis material demercuration curve
Embodiment
Case study on implementation one:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution;2h, which is stirred at room temperature, makes it become mixed solution, adds 2.0mol/L
NaOH solution adjust to pH=9.00, continue stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105℃
24h is dried, 300 DEG C of calcining 4h, catalysis material powder is made.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.95.2% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation two:
By ferro-silicon slag powder and 3.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, and the NaOH solution for adding 2.0mol/L is adjusted to pH=9.00, continues to stir
Mix 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material
Powder.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.84.2% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation three:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, and the NaOH solution for adding 2.0mol/L is adjusted to pH=7.00, continues to stir
Mix 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material
Powder.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.89.9% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation four:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, and the NaOH solution for adding 2.0mol/L is adjusted to pH=8.00, continues to stir
Mix 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material
Powder.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.77.1% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation five:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, and the NaOH solution for adding 2.0mol/L is adjusted to pH=10.00, is continued
Stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material
Feed powder end.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.75.2% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation six:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds and analyzes pure Na2CO3Particle is adjusted to pH=9.00, continues to stir
30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material powder
End.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3, 6%O2, 12%CO2, N2For Balance Air, at 100 DEG C~500 DEG C
Within the temperature range of carry out demercuration efficiency test.88.9% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation seven:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds ammonia spirit and adjusts to pH=9.00, continues to stir 30min;Go
Ionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material powder.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3, 6%O2, 12%CO2, N2For Balance Air, at 100 DEG C~500 DEG C
Within the temperature range of carry out demercuration efficiency test.93.1% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation eight:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds 3.1537g copper nitrates, continues to stir 0.5h, adds 2.0mol/L
NaOH solution adjust to pH=9.00, continue stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105℃
24h is dried, 300 DEG C of calcining 4h, catalysis material powder is made.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.92.1% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation nine:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds 6.1537g copper nitrates, continues to stir 0.5h, adds 2.0mol/L
NaOH solution adjust to pH=9.00, continue stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105℃
24h is dried, 300 DEG C of calcining 4h, catalysis material powder is made.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.96.2% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation ten:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds 9.1537g copper nitrates, continues to stir 0.5h, adds 2.0mol/L
NaOH solution adjust to pH=9.00, continue stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105℃
24h is dried, 300 DEG C of calcining 4h, catalysis material powder is made.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.92.9% is reached as high as in 350 DEG C of demercuration rates.
Case study on implementation 11:
By ferro-silicon slag powder and 2.0mol/L hydrochloric acid solution under 100 mesh sieves with solid-to-liquid ratio=1 gram:9 milliliters of ratio is mixed
Close, 2h, which is stirred at room temperature, makes it become mixed solution, adds 10.1537g copper nitrates, continues to stir 0.5h, adds 2.0mol/
L NaOH solution is adjusted to pH=9.00, continues to stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105℃
24h is dried, 300 DEG C of calcining 4h, catalysis material powder is made.
Demercuration rate is tested:Simulated flue gas composition 60ug/m3Hg0, 6%O2, 12%CO2, N2For Balance Air, 100 DEG C~500
Demercuration efficiency test is carried out within the temperature range of DEG C.89.4% is reached as high as in 350 DEG C of demercuration rates.
Claims (3)
1. a kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material, it is characterised in that:By ferro-silicon slag powder under 100 mesh sieves with
2.0~3.0mol/L hydrochloric acid solution is with solid-to-liquid ratio=1 gram:9 milliliters of ratio mixing, 2h, which is stirred at room temperature, makes it become mixed
Close solution;Precipitating reagent is added, regulation mixed solution pH=7~10, continues to stir 30min;Deionized water centrifuges three times, isolates
Bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material powder.
2. the method that a kind of ferro-silicon slag according to claim 1 prepares medium temperature demercuration catalysis material, it is characterised in that:Precipitation
One kind in agent selection sodium hydroxide solution, ammonia spirit, sodium carbonate liquor.
3. a kind of method that ferro-silicon slag prepares medium temperature demercuration catalysis material, it is characterised in that:By ferro-silicon slag powder under 100 mesh sieves with
2.0mol/L hydrochloric acid solution is with solid-to-liquid ratio=1 gram:9 milliliters of ratio mixing, is stirred at room temperature 2h;Copper nitrate is added, is added
It is 0.25~1.0 to add the mass ratio of copper nitrate and ferro-silicon slag, stirs 30min, adds NaOH solution regulation pH value of solution=9, continues
Stir 30min;Deionized water centrifuges three times, isolates bottom precipitation;105 DEG C of dry 24h, 300 DEG C of calcining 4h, are made catalysis material
Feed powder end.
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Cited By (2)
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CN109621944A (en) * | 2018-11-28 | 2019-04-16 | 上海大学 | The method for preparing integral catalyzer using waste sill |
CN111001376A (en) * | 2019-12-30 | 2020-04-14 | 北京工业大学 | SiO for efficiently adsorbing copper ions2-Al2O3Preparation method of-CaO-MgO quaternary system adsorbent |
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CN104001501A (en) * | 2014-05-27 | 2014-08-27 | 北京工业大学 | Method for preparing denitration catalytic material by using acidolysis residues |
CN104549356A (en) * | 2015-01-25 | 2015-04-29 | 北京工业大学 | Method for preparing low-temperature denitrification catalytic material from acidolysis residues |
CN105944662A (en) * | 2016-05-15 | 2016-09-21 | 清华大学 | Catalytic adsorbent for demercuration and denitration of flue gas in coal-fired power plant |
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CN102580743A (en) * | 2011-12-30 | 2012-07-18 | 浙江大学 | Method for preparing oxidation catalyst from gold ore tailing slag, and prepared oxidation catalyst and application thereof |
CN104001501A (en) * | 2014-05-27 | 2014-08-27 | 北京工业大学 | Method for preparing denitration catalytic material by using acidolysis residues |
CN104549356A (en) * | 2015-01-25 | 2015-04-29 | 北京工业大学 | Method for preparing low-temperature denitrification catalytic material from acidolysis residues |
CN105944662A (en) * | 2016-05-15 | 2016-09-21 | 清华大学 | Catalytic adsorbent for demercuration and denitration of flue gas in coal-fired power plant |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109621944A (en) * | 2018-11-28 | 2019-04-16 | 上海大学 | The method for preparing integral catalyzer using waste sill |
CN109621944B (en) * | 2018-11-28 | 2021-12-03 | 上海大学 | Method for preparing monolithic catalysts using waste-based materials |
CN111001376A (en) * | 2019-12-30 | 2020-04-14 | 北京工业大学 | SiO for efficiently adsorbing copper ions2-Al2O3Preparation method of-CaO-MgO quaternary system adsorbent |
CN111001376B (en) * | 2019-12-30 | 2022-05-17 | 北京工业大学 | SiO for efficiently adsorbing copper ions2-Al2O3Preparation method of-CaO-MgO quaternary system adsorbent |
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