CN102260569A - Flyash-base porous ceramic membrane-based iron-based oxygen carrier and preparation method thereof - Google Patents
Flyash-base porous ceramic membrane-based iron-based oxygen carrier and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical chain combustion, in particular to a novel flyash-base porous ceramic membrane-based iron-based oxygen carrier and a preparation method thereof. By using Fe2O3 as an active component and using a flyash-base porous ceramic membrane as a carrier, an embedded loading type membranous iron-based oxygen carrier is obtained; and the oxygen carrier comprises 5-50 percent by mass of Fe2O3 and 50-95 percent by mass of carrier. The iron-based oxygen carrier prepared by using the flyash-base porous ceramic membrane as the carrier has great porosity and larger specific surface area and can highly disperse Fe2O3, increase the reaction area and prevent the sintering of Fe2O3 due to high temperature; the inert flyash-base porous ceramic membrane has stable performance at high temperature, can not react with Fe2O3, can prevent the loss of Fe2O3 and ensure the heat stability of the novel iron-based oxygen carrier; and the invention has the advantages of raw material source of preparation raw materials, low cost, environmental protection, and the like and is suitable for large-scale popularization.
Description
Technical field
The invention belongs to the chemical chain burning technology field, be specifically related to a kind of novel iron-based oxygen carrier based on the fly ash base porous ceramic film and preparation method thereof.
Background technology
Burning chemistry chains (CLC) technology is a kind of efficient, cleaning, economic novel flameless combustion technology.Be different from the direct catalytic burning of traditional fuel and air, it is by means of the effect of oxygen carrier, by oxygen carrier the oxygen in the air reactor is delivered in the fuel reaction device, and does not need fuel directly to contact, generate the CO of high density in the combustion processes at the fuel reaction device with air
2, so that CO
2Separate.Simultaneously can reduce high temperature NO
xGeneration.Chemical chain burning technology has enrichment CO with it
2Characteristics and enjoy people to pay close attention to.Wherein, selection has the key that the oxygen carrier of good physics and chemical property is the restriction chemical chain burning technology.
The leading indicator of oxygen carrier performance has: good reactivity, oxygen carrying capability, lasting circulation ability, physical strength, anti-sintering and reunion ability, anti-carbon deposition ability, heat-resisting ability, low cost and environmental friendliness.The oxygen carrier of main research has the oxide compound and the CaSO of transition metal such as Fe, Cu, Ni, Co, Mn, Cd at present
4Wherein most metal oxides all have good reactivity worth, preferably oxygen carrying capability, continue circulation ability and advantage such as high temperature resistant, but also there are some inherent defectives simultaneously, as the carbon distribution under the low temperature, price height, heavy metal secondary pollution problems, be the response capacity that improves oxygen carrier, physical strength, work-ing life, anti-caking power, specific surface area etc., oxygen carrier can load on some inert substances.These inert supports do not participate in reaction, but can greatly improve oxygen carrier granule specific surface area, increase the anti-caking power of particulate, realize the transmission ofenergy of air reactor to the fuel reaction device.At present, Chang Yong inert support has: Al
2O
3, SiO
2, TiO
2, ZrO
2, yttria-stabilized zirconia (YSZ), wilkinite, sepiolite, kaolin and inert substances such as aluminium, magnesate.The preparation main method of oxygen carrier has: the precipitator method, pickling process, colloidal sol-condensation method, mechanical mixing, freezing granulation, dispersion method, spray-drying process, deposition-precipitator method.Studies show that the kind of metal oxide, inert support kind and factors such as both blending ratios, preparation technology have remarkably influenced to the performance of oxygen carrier.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing oxygen carrier, utilize cinder that the fuel-burning power plant produces as raw material, provide that a kind of specific surface area is big, reactive behavior is high, oxygen carrying capability is strong, Heat stability is good, physical strength is big, Stability Analysis of Structures is indeformable, wear resistance is high and the burning chemistry chains oxygen carrier of long service life and preparation method thereof.
The technical solution adopted in the present invention is:
This oxygen carrier is on the vesicular structure of porous ceramic film, supported active composition Fe
2O
3And constitute; Wherein, in the load-type iron-based oxygen carrier of described embedding, Fe
2O
3The quality percentage composition shared separately with porous ceramic film is respectively 5-50% and 50-95%.
The effect owing to whipping agent in making processes of described porous ceramic film produces vesicular structure.
Preparation method based on the iron-based oxygen carrier of fly ash base porous ceramic film possesses following steps:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O grinds evenly, and (wood chip: particle diameter＜0.1mm), adopting semidrying on pressing machine is the condition dip mold moulding of 30MPa in forming pressure, is pressed into the thin slice of φ 10 * 5mm to add mass content and be the whipping agent of flyash quality 0%-30%;
Step (2): with the thin slice of compacting in retort furnace under 1100 ℃ of-1300 ℃ of temperature condition calcining 2h promptly obtain the fly ash base porous ceramics piece;
Step (3): measure molysite and be dissolved in the distilled water of capacity; With the preparation porous ceramics piece put into above-mentioned solution, with the strong aqua volumetric soiutions to PH be 9.0, leave standstill after the ultrasonication, filter and collect filter residue then;
Step (4): measure the distilled water of capacity, the filter residue that obtains in the step (3) is put into wherein and used ultrasonic wave to handle once more, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is carried out drying, roasting, promptly obtain iron-based oxygen carrier based on the flyash porous ceramic film, and in the load-type iron-based oxygen carrier that obtains, Fe
2O
3The quality percentage composition shared separately with porous ceramic film is respectively 5-50% and 50-95%.
Ultrasonic treatment time in the described step (3) is 1-10h, and time of repose is 2-20h.
Ultrasonic treatment time in the described step (4) is 30s-60s.
Drying in the described step (5) is common air dry oven drying, and drying temperature is 120 ℃, and be 10h time of drying.
Maturing temperature in the described step (5) is 550 ℃, and roasting time is 5h.
Described molysite is iron nitrate or iron(ic) chloride.
Beneficial effect of the present invention is:
The how empty ceramic membrane of fly ash base has very high porosities, great specific surface area, high temperature resistant, advantages such as physical strength big, Stability Analysis of Structures, thermal stability height, life-span length.It as carrier, is helped Fe
2O
3High dispersing, can provide more chain carrier for burning chemistry chains, thereby significantly improve the reactive behavior of oxygen carrier.And its thermal stability height, activeconstituents can not react with carrier under the high temperature, helps the repeatedly circulation of oxygen carrier, has strengthened oxygen carrier work-ing life.
Adopt the fly ash base porous ceramic film as carrier, in the sample making process, molysite can enter in the duct of porous ceramic film and be surperficial, most Fe after roasting
2O
3All be distributed in the how empty ceramic membrane duct, thereby effectively prevented Fe
2O
3Reunion and sintering.
Fly ash base porous ceramics film component is an inert substance all, is difficult to and Fe
2O
3React, therefore can guarantee Fe
2O
3Can be because of not reacting with carrier and lose, thus the life-span that recycles of catalyzer guaranteed.
Embodiment
The invention provides a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film and preparation method thereof, the present invention is further elaborated below by specific embodiment.
Percentage composition in the following example is weight percentage if no special instructions.
Embodiment 1
Based on the iron-based oxygen carrier of fly ash base, its preparation method is as follows:
Step (1): measuring the 20g main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O grinds evenly, and (wood chip: particle diameter＜0.1mm), adopt semidrying moulded section on pressing machine is pressed into the thin slice (forming pressure is 30MPa) of φ 10 * 5mm to add mass content and be the whipping agent of flyash quality 30%.
Step (2): thin slice 1100 ℃ of following calcinings in retort furnace of compacting were promptly obtained the flyash porous ceramics piece in 2 hours.
Step (3): the iron nitrate of weighing 11.2g (Fe (NO
3)
39H
2O) be dissolved in the capacity distilled water, the fly ash base porous ceramic film of weighing 20g preparation adds in the above-mentioned solution, with strong aqua with the solution titration to PH be 9.0, leave standstill 12h behind the supersound process 5h, filter and collect filter residue then;
Step (4): measure an amount of distilled water, the filter residue that obtains in the step (3) is put into wherein and supersound process 40s, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is placed 120 ℃ of common air dry ovens dry 10h, 550 ℃ of roasting 5h of retort furnace down, promptly obtain new iron-based oxygen carrier (Fe wherein
2O
3The quality percentage composition be 10%).
Adopt the small-sized fluidized bed simulated experiment platform of development voluntarily that the performance of above-mentioned oxygen carrier is tested.Adopt CO, H respectively
2, CH
4, biomass pyrolytic gas, coal is fuel, the efficiency of combustion in 500-1000 ℃ of scope is all higher.And through behind 30 circulating reactions, the reactive behavior of oxygen carrier, physical strength and oxygen carrying capability obviously do not descend.
Embodiment 2
Based on the iron-based oxygen carrier of fly ash base, its preparation method is as follows:
Step (1): measure 20g cinder (identical with embodiment 1), grind evenly, the adding mass percent is 10% whipping agent, in pressing machine top die moulding (semidrying), is pressed into the thin slice (forming pressure is 30MPa) of φ 10 * 5mm.
Step (2): the thin slice of compacting is calcined 2h under 1150 ℃ promptly obtain the flyash porous ceramics piece in retort furnace.
Step (3): the iron nitrate of weighing 43.3g (Fe (NO
3)
39H
2O) be dissolved in the capacity distilled water, the fly ash base porous ceramic film of weighing 20g preparation adds in the above-mentioned solution, with strong aqua with the solution titration to PH be 9.0, leave standstill 12h behind the supersound process 5h, filter and collect filter residue then;
Step (4): measure an amount of distilled water, the filter residue that obtains in the step (3) is put into wherein and supersound process 40s, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is placed 120 ℃ of common air dry ovens dry 10h, 550 ℃ of roasting 5h of retort furnace down, promptly obtain new iron-based oxygen carrier (Fe wherein
2O
3The quality percentage composition be 30%).
Adopt the small-sized fluidized bed simulated experiment platform of development voluntarily that the performance of above-mentioned oxygen carrier is tested.Adopt CO, H respectively
2, CH
4, biomass pyrolytic gas, coal is fuel, the efficiency of combustion in 500-1000 ℃ of scope is all higher.And through behind 30 circulating reactions, the reactive behavior of oxygen carrier, physical strength and oxygen carrying capability obviously do not descend.
Embodiment 3
Based on the iron-based oxygen carrier of fly ash base, its preparation method is as follows:
Step (1): measure 20g cinder (identical with embodiment 1), grind evenly, the adding mass percent is 20% whipping agent, in pressing machine top die moulding (semidrying), is pressed into the thin slice (forming pressure is 30MPa) of φ 10 * 5mm.
Step (2): the thin slice of compacting is calcined 2h under 1250 ℃ promptly obtain the flyash porous ceramics piece in retort furnace.
Step (3): the iron nitrate of weighing 101g (Fe (NO
3)
39H
2O) be dissolved in the capacity distilled water, the fly ash base porous ceramic film of weighing 20g preparation adds in the above-mentioned solution, with strong aqua with the solution titration to PH be 9.0, leave standstill 12h behind the supersound process 5h, filter and collect filter residue then;
Step (4): measure an amount of distilled water, the filter residue that obtains in the step (3) is put into wherein and supersound process 40s, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is placed 120 ℃ of common air dry ovens dry 10h, 550 ℃ of roasting 5h of retort furnace down, promptly obtain new iron-based oxygen carrier (Fe wherein
2O
3The quality percentage composition be 50%).
Adopt the small-sized fluidized bed simulated experiment platform of development voluntarily that the performance of above-mentioned oxygen carrier is tested.Adopt CO, H respectively
2, CH
4, biomass pyrolytic gas, coal is fuel, the efficiency of combustion in 500-1000 ℃ of scope is all very high.And through behind 30 circulating reactions, the reactive behavior of oxygen carrier, physical strength and oxygen carrying capability obviously do not descend.
Embodiment 4
Based on the iron-based oxygen carrier of fly ash base, its preparation method is as follows:
Step (1): measure 20g cinder (identical), grind evenly, add 20% whipping agent,, be pressed into the thin slice (forming pressure is 30MPa) of φ 10 * 5mm in pressing machine top die moulding (semidrying) with embodiment 1.
Step (2): the thin slice of compacting is calcined 2h under 1250 ℃ promptly obtain the flyash porous ceramics piece in retort furnace.
Step (3): the iron(ic) chloride (FeCl of weighing 67.6g
36H
2O) be dissolved in the quantitative distilled water, the fly ash base porous ceramic film of weighing 20g preparation adds in the above-mentioned solution, with strong aqua with the solution titration to PH be 9.0, leave standstill 12h behind the supersound process 5h, filter and collect filter residue then;
Step (4): measure an amount of distilled water, the filter residue that obtains in the step (3) is put into wherein and supersound process 40s, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is placed 120 ℃ of common air dry ovens dry 10h, 550 ℃ of roasting 5h of retort furnace down, promptly obtain new iron-based oxygen carrier (Fe wherein
2O
3The quality percentage composition be 50%).
Adopt the small-sized fluidized bed simulated experiment platform of development voluntarily that the performance of above-mentioned oxygen carrier is tested.Adopt CO, H respectively
2, CH
4, biomass pyrolytic gas, coal is fuel, the efficiency of combustion in 500-1000 ℃ of scope is all very high.And through behind 30 circulating reactions, the reactive behavior of oxygen carrier, physical strength and oxygen carrying capability obviously do not descend.
Claims (9)
1. the iron-based oxygen carrier based on the fly ash base porous ceramic film is characterized in that, this oxygen carrier is on the vesicular structure of porous ceramic film, supported active composition Fe
2O
3And constitute; Wherein, in the load-type iron-based oxygen carrier of described embedding, Fe
2O
3The quality percentage composition shared separately with porous ceramic film is respectively 5-50% and 50-95%.
2. the iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 1 is characterized in that, the effect owing to whipping agent in making processes of described porous ceramic film produces vesicular structure.
3. preparation method based on the iron-based oxygen carrier of fly ash base porous ceramic film is characterized in that possessing following steps:
Step (1): with main component is SiO
2, Al
2O
3, CaO, MgO, TiO
2, K
2O, Na
2The cinder of O grinds evenly, and adding mass content is the whipping agent of flyash quality 0%-30%, and adopting semidrying on pressing machine is the condition dip mold moulding of 30MPa in forming pressure, is pressed into the thin slice of φ 10 * 5mm;
Step (2): with the thin slice of compacting in retort furnace under 1100 ℃ of-1300 ℃ of temperature condition calcining 2h promptly obtain the fly ash base porous ceramics piece;
Step (3): measure molysite and be dissolved in the distilled water of capacity; With the preparation porous ceramics piece put into above-mentioned solution, with the strong aqua volumetric soiutions to PH be 9.0, leave standstill after the ultrasonication, filter and collect filter residue then;
Step (4): measure the distilled water of capacity, the filter residue that obtains in the step (3) is put into wherein and used ultrasonic wave to handle once more, filter and collect filter residue then;
Step (5): the filter residue that obtains in the step (4) is carried out drying, roasting, promptly obtain iron-based oxygen carrier based on the flyash porous ceramic film, and in the load-type iron-based oxygen carrier that obtains, Fe
2O
3The quality percentage composition shared separately with porous ceramic film is respectively 5-50% and 50-95%.
4. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that the ultrasonic treatment time in the described step (3) is 1-10h, and time of repose is 2-20h.
5. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that the ultrasonic treatment time in the described step (4) is 30s-60s.
6. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that the drying in the described step (5) is common air dry oven drying, and drying temperature is 120 ℃, and be 10h time of drying.
7. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that the maturing temperature in the described step (5) is 550 ℃, and roasting time is 5h.
8. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that described molysite is iron nitrate or iron(ic) chloride.
9. the preparation method of a kind of iron-based oxygen carrier based on the fly ash base porous ceramic film according to claim 3 is characterized in that described whipping agent is the wood chip that particle diameter is not more than 0.1mm.
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Cited By (10)
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|---|---|---|---|---|
| CN102533388A (en) * | 2011-12-05 | 2012-07-04 | 华北电力大学 | Application method of nickel (Ni)-loaded mesoporous silicon dioxide hollow sphere iron-based oxygen carrier |
| CN102585969A (en) * | 2012-02-16 | 2012-07-18 | 华北电力大学 | Novel iron-based oxygen carrier of nuclear-free cavity structure and preparation method thereof |
| CN102728339A (en) * | 2012-06-21 | 2012-10-17 | 华北电力大学 | Porous inorganic ceramic membrane-graphene-TiO2 photocatalyst composite material and its preparation method |
| CN102728346A (en) * | 2012-06-21 | 2012-10-17 | 华北电力大学 | MnO2-TiO2 carbon nanotube-porous inorganic ceramic membrane low-temperature catalytic denitrification self-cleaning material and its preparation method |
| CN103113954A (en) * | 2013-01-18 | 2013-05-22 | 东南大学 | Method for preparing bio-oil chemical-looping hydrogen recycled F2O3/Al2O3 oxygen carrier through ultrasonic method |
| CN103464166A (en) * | 2013-09-10 | 2013-12-25 | 合肥工业大学 | Preparation method of supported transition metal catalyst utilizing iron tailings as carrier and method for degrading organic pollutants |
| CN104059714A (en) * | 2014-07-03 | 2014-09-24 | 安徽工业大学 | Method for preparing Fe2O3/Al2O3 oxygen carrier by taking ferrous metallurgy dust mud as main raw materials |
| CN106867624A (en) * | 2017-03-07 | 2017-06-20 | 东南大学 | A kind of CuO and quasi- east coal ash modify oxygen carrier of iron ore and preparation method thereof jointly |
| CN110054225A (en) * | 2019-05-09 | 2019-07-26 | 新奥科技发展有限公司 | A kind of preparation method of oxygen carrier |
| CN110342864A (en) * | 2019-06-28 | 2019-10-18 | 新奥科技发展有限公司 | A kind of coal ash for manufacturing for the carrier of oxygen method |
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| CN102533388A (en) * | 2011-12-05 | 2012-07-04 | 华北电力大学 | Application method of nickel (Ni)-loaded mesoporous silicon dioxide hollow sphere iron-based oxygen carrier |
| CN102533388B (en) * | 2011-12-05 | 2014-01-15 | 华北电力大学 | Application method of nickel (Ni)-loaded mesoporous silicon dioxide hollow sphere iron-based oxygen carrier |
| CN102585969A (en) * | 2012-02-16 | 2012-07-18 | 华北电力大学 | Novel iron-based oxygen carrier of nuclear-free cavity structure and preparation method thereof |
| CN102728346A (en) * | 2012-06-21 | 2012-10-17 | 华北电力大学 | MnO2-TiO2 carbon nanotube-porous inorganic ceramic membrane low-temperature catalytic denitrification self-cleaning material and its preparation method |
| CN102728339A (en) * | 2012-06-21 | 2012-10-17 | 华北电力大学 | Porous inorganic ceramic membrane-graphene-TiO2 photocatalyst composite material and its preparation method |
| CN102728339B (en) * | 2012-06-21 | 2014-06-25 | 华北电力大学 | Porous inorganic ceramic membrane-graphene-TiO2 photocatalyst composite material and its preparation method |
| CN103113954A (en) * | 2013-01-18 | 2013-05-22 | 东南大学 | Method for preparing bio-oil chemical-looping hydrogen recycled F2O3/Al2O3 oxygen carrier through ultrasonic method |
| CN103464166A (en) * | 2013-09-10 | 2013-12-25 | 合肥工业大学 | Preparation method of supported transition metal catalyst utilizing iron tailings as carrier and method for degrading organic pollutants |
| CN103464166B (en) * | 2013-09-10 | 2015-07-22 | 合肥工业大学 | Preparation method of supported transition metal catalyst utilizing iron tailings as carrier and method for degrading organic pollutants |
| CN104059714A (en) * | 2014-07-03 | 2014-09-24 | 安徽工业大学 | Method for preparing Fe2O3/Al2O3 oxygen carrier by taking ferrous metallurgy dust mud as main raw materials |
| CN106867624A (en) * | 2017-03-07 | 2017-06-20 | 东南大学 | A kind of CuO and quasi- east coal ash modify oxygen carrier of iron ore and preparation method thereof jointly |
| CN110054225A (en) * | 2019-05-09 | 2019-07-26 | 新奥科技发展有限公司 | A kind of preparation method of oxygen carrier |
| CN110342864A (en) * | 2019-06-28 | 2019-10-18 | 新奥科技发展有限公司 | A kind of coal ash for manufacturing for the carrier of oxygen method |
| CN110342864B (en) * | 2019-06-28 | 2022-01-07 | 新奥科技发展有限公司 | Method for preparing oxygen carrier from fly ash |
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Application publication date: 20111130 |