CN101293170B - Composite sulphur dioxide desulfurizing agent and preparation method thereof - Google Patents
Composite sulphur dioxide desulfurizing agent and preparation method thereof Download PDFInfo
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- CN101293170B CN101293170B CN2008100139146A CN200810013914A CN101293170B CN 101293170 B CN101293170 B CN 101293170B CN 2008100139146 A CN2008100139146 A CN 2008100139146A CN 200810013914 A CN200810013914 A CN 200810013914A CN 101293170 B CN101293170 B CN 101293170B
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Abstract
The invention discloses a desulphurizer for sulfur dioxide in composite material, which is characterized in that the desulphurizer comprises the following compositions in a mass percentage of 50- 80% of white mud in an alkali factory, 10-40% of red mud in a steel plant, 5.0- 8.0% of binder, 3.0% - 8.0% of pore-forming agent and 0.1- 1.0% of lubricant. A preparation method is as follows: firstly, the white mud in the alkali factory and the red mud in the steel plant are smashed into a particle above 40 meshes and are mixed with the binder, the pore-forming agent and the lubricant in a proportion above-mentioned; and then the water is added to mix evenly into a pasty state for the extrusion molding and the drying; finally the desulphurizer is obtained by high-temperature roasting. The invention has the advantages that industrial waste material such as the white mud and the red mud are utilized to prepare the desulphurizer which has the advantages of good desulphurizing effect, extensive material source, low price and no secondary pollution; the products of desulphurization can also be used for building sea dams and paving, etc., thereby being extensively used for the desulphurization and the purification of exhaust gas in a coal-fired power plant, a coal-burning boiler and a coal-fired furnace in the environmental protection industries.
Description
Technical field
The present invention relates to a kind of desulfurizing agent that is used for flue gas desulfurization industries such as coal-burning power plant, coal-burning boiler and coal-fired furnace and preparation method thereof, a kind of SO that utilizes alkali factory white clay and steel mill's red mud preparation more specifically says so
2Desulfurizing agent and preparation method thereof.
Background technology
It is reported Chinese SO in 2005
2Total emission volumn up to 2,550 ten thousand tons, rank first in the world.Increased by 27% than 2000, and 2006 rose 1.8% than 2005 years.China atmosphere SO
2Capacity performance index is 474 tons/year, actually to 2006 exceeds 4.6 times.SO
2A large amount of dischargings environmental problem of having caused acid rain etc. to be on the rise, on January 27th, 2005, State Environmental Protection Administration requires acid rain control district and SO
2The not desulfurization thermal power plant time limit rectification of 46 families of control zone.On February 17th, 2005, one the containment global warming include in rules international convention---Kyoto Protocol is formally effective, Chinese government's active response has also started " environmental protection storm ".Yet how to SO
2Effectively administer very urgent a, problem demanding prompt solution that has become China's pollution control.According to statistics, China SO
2Total emission volumn 90% from coal-fired process, wherein, the discharge capacity of coal-fired power plant occupies the first place.SO is controlled in flue gas desulfurization (Flue Gas Desulfurization) at present in the world
2Therefore the main desulfurization method that pollute, control acid rain endangers controls the SO of coal-fired power plant
2Discharging be the most important thing of China's flue gas desulfurization cause.
How many methods of flue gas desulfurization can be divided into wet method and dry method by absorbent and desulfurization product water content.The wet desulphurization technology maturation, the desulfuration efficiency height, but have waste water post processing problem, and complicated operation, equipment is huge, and energy consumption is big, the cost height, and washing back flue-gas temperature is low, is unfavorable for purifying the discharging of flue gas.The dry desulfurizing process process is simple, and investment and operating cost are low, and energy consumption is little, and non-secondary pollution purifies back flue-gas temperature height, helps the diffusion of chimney exhaust.Although desulfuration efficiency is low slightly, also be enough to satisfy environmental requirement, both at home and abroad so the research and development of dry flue gas desulphurization was subjected to generally paying attention in recent years.Dry desulfurization mainly contains burner hearth dry powder injection desulfurization method, high energy electron active oxidation method, charged dry powder injection desulfurization method, metal oxide doctor treatment and active carbon or flyash doctor treatment.Owing to do not need the high energy electron generating means, reduced the trouble that charged dry powder injection desulfurization has solid waste to handle, inherited the adsorbable performance and the autocatalysis performance of active carbon adsorption again, the metal oxide desulfurization is a dark horse in dry desulfurization, enjoys people to pay close attention to.Removal methods also develops into composite metal oxide from single metal oxide, and from generally being adsorbed onto catalysis absorption or catalytic oxidation, growth momentum is swift and violent, and prospect is unlimited.
Along with the expansion of China's output of steel, the red mud of steelmaking converter byproduct will be increasing, and various steel industry exhaust gas discharging also will increase thereupon, and this certainly will cause certain pressure to environment.In addition, steel-making waste gas calorific value is low, and sulphur and other impurity (as dust) content height are unsuitable for long distance and carry, and by being that a steel-making enterprise is increased economic efficiency to carrying out combined cycle generation behind the waste gas purification, reduce the good way of environmental pollution.The waste residue that produces when red mud is pneumatic steelmaking, its composition mainly contains Fe, Fe
2O
3, Fe
3O
4, FeO, CaCO
3Deng.The annual soda-manufacturing waste residue white clay that produces of Qingdao Alkali Plant surpasses 180,000 tons (butt), and its composition mainly contains CaCO
3, Mg (OH)
2, CaSO
4, NaCl, CaCl
2, metal oxide R
2O
3Deng.Because products such as the contained Cl ion pair production of white clay wall covering are influential, the market capacity of product is limited, and can't consume white clay in a large number, to such an extent as to can't find the good method of effective improvement white clay.Iron-based, calcium based oxide flue gas desulfurization all have been proved respond well, therefore use to contain the fume desulfurizing agent that " refuse " white clay that enriches calcium base, magnesium base oxide can be made into efficient and cheap.But because sodium chloride, calcium chloride imbibition in the white clay, and produce harm such as etching apparatus.And generate product C aSO
4Easily stop up the reaction duct, make that the independent desulfurizing agent desulfurized effect of white clay preparation that uses is not ideal enough.The white clay sea water desulfuration is respond well, but serviceability temperature is low, causes active ingredient Ca in the white clay
2+, Mg
2+Can't play desulfidation, and have that smoke evacuation difficulty, energy consumption are big, secondary pollution, Cl
-Shortcomings such as etching apparatus.
Summary of the invention
At the shortcoming of above-mentioned single use white clay desulfurization, the purpose of this invention is to provide a kind of efficient, inexpensive, easy composite SO of preparation
2Desulfurizing agent and preparation method thereof.
A kind of composite SO that utilizes alkali factory white clay and steel mill's red mud preparation
2Desulfurizing agent is characterized in that comprising following composition (all being mass percents): alkali factory white clay 50～80%, the red mud 10-40% of steel mill, binding agent 5.0～8.0%, pore creating material 3.0%～8.0%, lubricant 0.1～1.0%.
The oxide content of total iron is greater than 50% in the wherein said steel mill red mud, CaCO in the alkali factory white clay
3Content is greater than 50%;
Described steel mill red mud main component is: Fe, Fe
2O
3, FeO, Fe
3O
4, CaCO
3Deng, main component is in the alkali factory white clay: CaCO
3, Mg (OH)
2, CaSO
4, NaCl, CaCl
2Deng;
Described binding agent is kaolin, bentonite, carclazyte or diatomite;
Described pore creating material is starch, semicoke or polyacrylamide;
Described lubricant is a graphite.
The preparation method of described desulfurizing agent is as follows: at first alkali factory white clay and steel mill's red mud powder are broken to greater than 40 purpose granularities, mix according to the above ratio with binding agent, pore creating material and lubricant, add water then and be mixed into pasty state, extruded moulding, oven dry are handled by high-temperature roasting at last and are promptly got desulfurizing agent.Wherein said oven dry is 100 ℃～110 ℃ dryings 4～8 hours in baking oven; High-temperature roasting is meant in muffle furnace 350 ℃～650 ℃ roastings 1～6 hour.
The activity of desulfurizing agent and Sulfur capacity test are carried out in atmospheric fixed bed reactor.Reactor is the tubular type stainless steel reactor of internal diameter 14mm, length 320mm.Desulfurizing agent is 4～10 orders, and admission space is 5ml desulfurizing agent, the broken ceramics of 20ml (for inert filler), and the reactor beds layer height is 150mm, removes SO
2Temperature is 350～600 ℃, and air speed is 300～1500h
-1, the particle diameter ratio is 0.1～0.15, flue gas consists of SO
21200～3000ppm, O
20～8%, H
2O 0～12%, all the other are by N
2Balance.Sulfur capacity is to penetrate Sulfur capacity with desulfurization degree greater than the accumulative total of calculating at 80% o'clock.
Red mud itself also has good flue gas desulfurization effect, makes it to generate iron chloride as add the red mud contain a large amount of iron-based oxides again in white clay, fixing chlorion, and generate solid solution with other materials, reduce equipment corrosion.The oxide desulfurizing agent is active high under higher temperature, and desulfurized effect is good, and these just in time higher with the boiler flue outlet temperature (200～1050 ℃) are consistent, and need not heating source again in this temperature range, and desulfurizing agent has just had excellent desulfurizing effect.White clay and red mud are made shaping desulfurizing agent, reduce pressure drop, make desulfurized effect better, be enterprise's energy efficient, subsidiary dust and the heavy metal of removing.
Characteristics of the present invention are that white clay and raw material sources such as red mud and auxiliary agent are extensive, low price, and prepared desulfurizing agent desulfurized effect is fine, and non-secondary pollution, desulfurization product can also the Xiu Hai dams, build the road etc.Can be widely used in the desulfurizing and purifying environmental protection industry of flue gases such as coal-burning power plant, coal-burning boiler and coal-fired furnace, the treatment of wastes with processes of wastes against one another, thus realize economy and environmental protection win-win.
The specific embodiment
Describe the present invention in detail below by specific embodiment.
Employed white clay and red mud are respectively from Qingdao alkali industry group and Qingdao iron and steel group among the following embodiment, and concrete composition sees the following form:
Table 1 alkali factory white clay composition (butt/%)
| Composition | CaCO 3 | ?CaSO 4 | ?NaCl | ?Mg(OH) 2 | SiO 2 | Fe 2O 3 | Acid is not tolerant | Other |
| Content | 53.21 | ?2.69 | ?7.01 | ?13.43 | ?9.09 | ?6.89 | ?3.66 | - |
Table 2 steel mill red mud composition (butt/%)
| Composition | α-Fe | ?FeO | ?Fe 3O 4 | ?CaCO 3 | ?Ca(OH) 2 | SiO 2And other |
| Content | 10.5 | ?25.6 | ?27.0 | ?17.8 | 3.0 | 16.1 |
Embodiment 1-4 and Comparative Examples 1:
The white clay and the red mud of different percentage compositions are carried out proportioning, and again with 5.0% bentonite, 4.9% starch and 0.1% graphite add water and are mixed into pasty state after mixing, extruded moulding, and oven dry is handled by high-temperature roasting at last, prepares several desulfurizing agents.Wherein white clay and red mud are 40 orders, and 105 ℃ were descended dry 6 hours, and sintering temperature is 500 ℃, roasting time 2h.The desulfurizing agent for preparing is carried out desulphurizing activated evaluation test, the results are shown in Table 3.
The different proportionings of table 3 (mass ratio) desulfurizing agent desulfurized effect
| Project | Comparative Examples 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| White clay percentage composition (%) red mud percentage composition (%) Sulfur capacity (%) time of break-through (h) | 90 0 3.81 2.44 | 80 10 4.27 2.92 | 70 20 11.13 8.24 | 60 30 13.03 11.42 | 50 40 7.59 6.20 |
Experiment condition: temperature: 400 ℃; Air speed: 1200h
-1SO
2Concentration: 6290mg/m
3(2200ppm); O
2:～5%; H
2O (g): 8%.
As can be seen from the table, when not having red mud when having only white clay, desulfurizing agent Sulfur capacity minimum, desulfurized effect is not good; And when white clay: during red mud=2: 1, desulfurizing agent Sulfur capacity maximum, time of break-through is the longest, desulfurized effect the best.
Embodiment 5-8 and Comparative Examples 2:
White clay and red mud are carried out proportioning by 60% and 30% respectively, add 5.0% bentonite again, 4.9% starch, 0.1% graphite adds water and is mixed into pasty state, extruded moulding after mixing, oven dry is handled by high-temperature roasting at last, prepares several desulfurizing agents according to the difference of white clay red mud order number.Wherein 105 ℃ were descended dry 6 hours, and sintering temperature is 400 ℃, roasting time 2h.White clay red mud order number average is respectively 16,40,60,80,100 orders.The desulfurizing agent for preparing is carried out desulphurizing activated evaluation test.The results are shown in Table 4.
The desulfurizing agent desulfurized effect of table 4 different meshes preparation
| Project | Comparative Examples 2 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 |
| White clay red mud order is counted Sulfur capacity (%) time of break-through (h) | 16 14.21 11.13 | 40 15.20 12.30 | 60 16.00 13.45 | 80 17.14 14.85 | 100 17.93 16.61 |
Experiment condition: temperature: 400 ℃; Air speed: 1200h
-1SO
2Concentration: 6290mg/m
3(2200ppm); O
2:～5%; H
2O (g): 8%
As can be seen from the table: along with used white clay red mud order number increases, promptly particle diameter attenuates, and time of break-through prolongs gradually, and Sulfur capacity increases gradually, and desulfurized effect is better.
Embodiment 9-12:
White clay and red mud are carried out proportioning by 60% and 30% respectively, add 5% different binding agents again, 4.9% starch is pore creating material, after 0.1% graphite mixes, add water and be mixed into pasty state, and extruded moulding, oven dry is handled by high-temperature roasting at last, prepares several desulfurizing agents.Equal 40 orders of white clay and red mud wherein, 105 ℃ dry 6 hours down, sintering temperature is 500 ℃ of roasting time 2h.Binding agent is respectively kaolin, bentonite, carclazyte, diatomite.The desulfurizing agent for preparing is carried out desulphurizing activated evaluation test.
The results are shown in Table 5.
The desulfurizing agent desulfurized effect comparison sheet of the different adhesive preparation of table 5
| Project | Embodiment 9 | Embodiment 10 | Embodiment 11 | Embodiment 12 |
| Different binding agent Sulfur capacity (%) times of break-through (h) | Kaolin 15.20 12.30 | Bentonite 14.98 12.02 | Carclazyte 14.30 10.97 | Diatomite 11.31 8.24 |
Experiment condition: temperature: 400 ℃; Air speed: 1200h
-1SO
2Concentration: 6290mg/m
3(2200ppm); O
2:～5%; H
2O (g): 8%
As can be seen from the table, binding agent has very big effect, desulfurized effect the best when kaolin is used for binding agent on the sulfur capacity that improves desulfurizing agent.
Embodiment 13-14 and Comparative Examples 3:
White clay and red mud are carried out proportioning by 60% and 30% respectively, and adding 5.0% kaolin again is binding agent, 4.9% different pore creating materials, after 0.1% graphite mixes, add water and be mixed into pasty state, extruded moulding, oven dry is handled by high-temperature roasting at last, prepares several desulfurizing agents.Equal 40 orders of white clay and red mud wherein, 105 ℃ dry 6 hours down, sintering temperature is 500 ℃, roasting time 2h.The desulfurizing agent for preparing is carried out desulphurizing activated evaluation test.The results are shown in Table 6.
The desulfurizing agent desulfurized effect of the different pore creating material preparations of table 6
| Project | Comparative Examples 3 | Embodiment 13 | Embodiment 14 |
| Pore creating material time of break-through (h) Sulfur capacity (%) | Do not have 11.08 13.85 | Starch 12.30 15.20 | Semicoke 12.05 15.02 |
Experiment condition: temperature: 400 ℃; Air speed: 1200h
-1SO
2Concentration: 6290mg/m
3(2200ppm); O
2:～5%; H
2O (g): 8%
As can be seen from the table, the high desulfurization rate of the desulfurizing agent of different pore creating materials: starch＞semicoke＞no pore creating material; Desulfurized effect: starch＞semicoke＞no pore creating material.Starch is used for pore creating material, desulfurized effect the best.For the desulfurizing agent that does not add pore creating material, desulfurization degree and Sulfur capacity are all on the low side.
Claims (9)
1. composite SO
2Desulfurizing agent is characterized in that comprising following composition (all being mass percents): alkali factory white clay 50～80%, the red mud 10-40% of steel mill, binding agent 5.0～8.0%, pore creating material 3.0%～8.0%, lubricant 0.1～1.0%.
2. composite SO according to claim 1
2Desulfurizing agent, the oxide mass percentage composition that it is characterized in that in the described steel mill red mud total iron be greater than 50%, CaCO in the alkali factory white clay
3The quality percentage composition is greater than 50%.
3. composite SO according to claim 1 and 2
2Desulfurizing agent is characterized in that described steel mill red mud main component is: Fe, Fe
2O
3, FeO, Fe
3O
4, CaCO
3Main component is in the alkali factory white clay: CaCO
3, Mg (OH)
2, CaSO
4, NaCl, CaCl
2
4. composite SO according to claim 1
2Desulfurizing agent is characterized in that described binding agent is kaolin, bentonite, carclazyte or diatomite.
5. composite SO according to claim 1
2Desulfurizing agent is characterized in that described pore creating material is starch, semicoke or polyacrylamide.
6. composite SO according to claim 1
2Desulfurizing agent is characterized in that described lubricant is a graphite.
7. composite SO according to claim 1
2The preparation method of desulfurizing agent, it is characterized in that it comprises the steps: at first alkali factory white clay and steel mill's red mud powder to be broken to greater than 40 purpose granularities, mix in the described ratio of claim 1 with binding agent, pore creating material and lubricant, add water then and be mixed into pasty state, extruded moulding, oven dry are handled by high-temperature roasting at last and are promptly got desulfurizing agent.
8. composite SO according to claim 7
2The preparation method of desulfurizing agent is characterized in that wherein said oven dry is 100 ℃～110 ℃ dryings 4～8 hours in baking oven.
9. composite SO according to claim 7
2The preparation method of desulfurizing agent is characterized in that wherein said high-temperature roasting is meant in muffle furnace 350 ℃～650 ℃ roastings 1～6 hour.
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| CN101293170A (en) | 2008-10-29 |
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