CN101486941A - Process for preparing iron based oxygen carrier - Google Patents

Process for preparing iron based oxygen carrier Download PDF

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Publication number
CN101486941A
CN101486941A CNA200910060787XA CN200910060787A CN101486941A CN 101486941 A CN101486941 A CN 101486941A CN A200910060787X A CNA200910060787X A CN A200910060787XA CN 200910060787 A CN200910060787 A CN 200910060787A CN 101486941 A CN101486941 A CN 101486941A
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oxygen carrier
carrier
oxygen
preparation
nitrate
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王保文
丁宁
郑瑛
郑楚光
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Huazhong University of Science and Technology
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Huazhong University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L10/00—Use of additives to fuels or fires for particular purposes
    • C10L10/02—Use of additives to fuels or fires for particular purposes for reducing smoke development

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Abstract

The invention provides an iron-based oxygen carrier preparation method which takes iron and aluminium nitrate as raw materials and urea as fuel, and combines the sol-gel method organically with combustion compound method to prepare nanometer-class Fe2O3/Al2O3 oxygen carrier with excellent anti-sintering performance. The iron-based oxygen carrier preparation method fully uses the mixing evenness between a plurality of components in the sol-gel method and the reaction process self-maintenance, quickness and low energy-consumption characteristics in the combustion compound method, easily obtains the used oxygen carrier preparation raw material, has the advantages of low price, simple preparation technology and easy operation, and is suitable for scaled mass production of the oxygen carrier.

Description

A kind of preparation method of iron based oxygen carrier
Technical field
The present invention relates to the nano material preparation technical field, especially relate to a kind of preparation method of iron based oxygen carrier.
Background technology
Recently, in the many environmental problems of the earth, greenhouse effects and global warming have caused great concern.Fossil oil such as coal, oil and natural gas has also produced a large amount of CO in the combustion of fossil fuel process when providing the world more than 85% with energy 2, be the CO that mankind's activity produces 2A main source.Therefore, reduce the CO that is discharged in the combustion of fossil fuel process 2Has important effect for control Greenhouse effect and Global warming.
Chemical chain burning technology is as a kind of novel fossil fuel CO 2Emission-reduction technology is with existing all kinds of CO 2Emission-reduction technology is compared, and has outstanding feature and advantage, and main manifestations is: when the carrier of oxygen and fuel fully react, need not other extra CO 2Separator can access the high concentration CO near 100% 2Simultaneously, can effectively suppress NO in the fuel projection process xFormation and discharging; Further, because fuel and not mixing of air in this technology so can effectively reduce the irreversible loss of fuel combustion under traditional fuel and the direct catalytic combustion mode of air, can effectively improve the fuel combustion thermal efficiency.
The principle of chemical chain burning technology is: the metal oxygen carrier and the fuel that at first contain lattice oxygen react in the fuel reaction device, the metal oxide of the lower valency that is reduced elemental metals alive is passed in the air reactor, carries out oxidizing reaction with air and makes the metal oxide that is reduced carry out manipulation of regeneration.When said process repeatedly repeats, just formed whole burning chemistry chains process.As seen, cheap, dependable performance, the simple oxygen carrier of preparation play important effect for the enforcement and the use of chemical chain burning technology.
Oxygen carrier mainly is made of active metal oxide and inert support.With regard to the reactive metal oxides that consists of the carrier of oxygen, with NiO, CuO, Fe 2O 3In the carrier of oxygen that these several reactive metal oxides consist of, the general NiO base carrier of oxygen has higher reactivity, but has strong carcinogenicity and thermodynamic limitation, is difficult to reach CH 4Fully conversion Deng gaseous fuel; The CuO base carrier of oxygen has satisfied reactivity, and be exothermic reaction with the reduction reaction of various fuel, thereby highly beneficial for the energy balance in the burning chemistry chains system, but because the fusing point of CuO is lower, thereby the easy sintering of the CuO base carrier of oxygen, reunion, cause fluid bed to take off fluidization; Compare Fe with above-mentioned NiO with the CuO base carrier of oxygen 2O 3Although base carrier of oxygen reactivity worth is lower, the oxygen transfer capacity is little, and low price, raw material are easy to get, environmental friendliness and non-secondary pollution, are very competitive as the active material in the carrier of oxygen.And with regard to the inert support material that consists of the carrier of oxygen, many inert materials of current usefulness comprise Al 2O 3, SiO 2, ZrO 2, MgAl 2O 4, TiO 2, MgO etc., but consider that in chemical chain burning technology the carrier of oxygen is not only the Transfer Medium of Lattice Oxygen, simultaneously or energy carrier.In order to guarantee abundant reaction and the conversion of fossil fuel, no matter from Al 2O 3Fusing point, mechanical performance and in keeping fuel and carrier of oxygen course of reaction aspect the maintenance of fuel reaction actuator temperature, Al 2O 3It all is proper inert carrier.Therefore, when the selection of the carrier of oxygen, reactive metal oxides and inert carrier adopt respectively Fe 2O 3And Al 2O 3
Nano particle Fe 2O 3Stable chemical nature, catalytic activity height, have good light resistance and to ultraviolet shielding properties, and ultra-fine Al 2O 3Then have higher hardness, mechanical stress, good heat transmission and thermal shock resistance properties, make it to have a very wide range of applications in fields such as pottery, catalyst.Citrate-nitrate combustion is owing to be self propagating high temperature synthetic method (SHS) and the combination of sol-gal process, has the product uniform component distribution of certainly keeping characteristic and preparation of preparation process once igniting, thereby at Fe 2O 3, Al 2O 3Preparation process in obtained certain application.But Fe 2O 3/ Al 2O 3The preparation method of compounding ingredients is then relatively considerably less, and the people such as Pu Lietuo are take ferric nitrate, aluminum nitrate as raw material, NH 3/ (NH 4) 2CO 3For adopting coprecipitation, precipitating reagent prepared the Fe of Different Weight share 2O 3(0～100wt%) Fe 2O 3/ Al 2O 3Composite metal oxide, this people such as grade of bayonet socket has prepared the Fe of weight quota as 5wt% take boehmite and ferric nitrate as raw material adopts sol-gal process 2O 3/ Al 2O 3, the so-called liquid phase water in suspension of the employings such as Te Taizi solution (aerosol hydrolysis) has prepared the Fe of similar weight quota 2O 3/ Al 2O 3, the people such as Liu have prepared the Fe of weight quota as 30wt% take iron, aluminium nitrate and hexamethylenetetramine solution for raw material adopts sol-gal process 2O 3/ Al 2O 3Composite metal oxide.
Up to the present, adopt the citrate-nitrate combustion preparation to have independently Fe take iron, aluminium nitrate and organic-fuel as raw material 2O 3With Al 2O 3The complex oxide of phase does not have bibliographical information so far.
Summary of the invention
The invention provides a kind of preparation method of iron based oxygen carrier, take iron, aluminium nitrate with as raw material, take urea as fuel, sol-gel processing and combustion synthesis method combination, prepare the nanoscale Fe with superior anti-sintering property 2O 3/ Al 2O 3The carrier of oxygen.
A kind of preparation method of iron based oxygen carrier, carry out according to following steps:
(1) metal nitrate is mixed with urea, add deionized water after mixing, uniform stirring obtains mixed solution, and the stoichiometric coefficient of metal nitrate and urea is 1, metal nitrate is made of ferric nitrate and aluminum nitrate, and the Fe2O3 that it comprises and the mass ratio of Al2O3 are 6:4～8:2;
(2) adopt magnetic stirring apparatus that the mixing solutions that step (1) makes is stirred, obtain heavy-gravity colloidal sol;
(3) colloidal sol is carried out drying treatment and obtain xerogel;
(4) to the xerogel igniting, made the xerogel auto-combustion 10～15 minutes;
(5) products of combustion that step (4) is formed is made sintering processes, obtains the Fe2O3/Al2O3 iron based oxygen carrier.
Beneficial effect of the present invention is embodied in:
Generally, the present invention has overcome long shortcoming of Prepared by Sol Gel Method time, having remedied also that the prepared powder granularity of self propagating high temperature synthesis method is thick, the deficiency of process controllability difference, is a kind of novel preparation technology of synthetic high-purity nm body, has an extraordinary application prospect.
Be that organic-fuel is used for above-mentioned collosol and gel combustion synthesis method with urea among the present invention, urea plays dual parts complexing agent and reductive agent (fuel just).Specifically, when urea during as complexing agent, urea and iron and aluminum ions complexing, increased the solubility of above-mentioned nitrate in the aqueous solution, prevented from forming iron, aluminum ions selective precipitation and segregation in gel and the water evaporation process; Simultaneously, in the spontaneous combustion process of xerogel through igniting, nitrate ion discharges a large amount of gas and heat as oxidant and urea generation redox reaction, thereby so that the prepared carrier of oxygen has bigger porosity and the pore-size distribution of optimization.Further, when adopting urea to act as a fuel preparation quality than being the Fe of 6:4～8:2 2O 3/ Al 2O 3During the carrier of oxygen, urea prepares Al 2O 3Security and urea with specific adaptability and preparation process is easy to get, cheap, nontoxic, thereby take urea as the raw material preparation quality than the Fe as 6:4～8:2 2O 3/ Al 2O 3The carrier of oxygen has good competitive advantage and great application prospect.
Further, with regard to technical process and the used utensil of preparation, this method technology is simple, has preferably repeatable; Institute's using appliance is fewer, thereby is easy to realize suitability for industrialized production.
In a word, to adopt above-mentioned preparation method to synthesize Fe 2O 3/ Al 2O 3The carrier of oxygen also is used for the chemical chain technology of fossil fuel, thereby should effectively reclaim and reduce CO in the combustion of fossil fuel process for the improvement of the economic performance of this technology and the popularization of this technology 2Discharging of great advantage.
Description of drawings
Fig. 1 is the change curve synoptic diagram that the differential pore size distribution of the oxygen carrier of different mass ratio distributes with mean pore size;
Fig. 2 is the Fe of different quality ratio 2O 3/ Al 2O 3Weight-loss curve schematic diagram when the carrier of oxygen and hydrogen reducing reaction.
Embodiment
Embodiment 1
(1) preparation of metal nitrate, urea mixing solutions
According to Fe 2O 3/ Al 2O 3Mass ratio is that the stoichiometric coefficient of 6:4 and metal nitrate and urea is 1, takes by weighing quantitative ferric nitrate, aluminum nitrate and urea, adds an amount of deionized water, uniform stirring, the solution that obtain dissolving fully, mixes.
(2) preparation of wet gel
Then, above-mentioned solution moved as temperature be set in 75 ℃ the magnetic stirring apparatus that has the constant temperature function, and at the uniform velocity stir, making that the moisture content in the mixing solutions constantly evaporates, iron nitrate, aluminum nitrate and urea uniform mixing, hydrolysis complexing form heavy-gravity colloidal sol.
(3) drying of wet gel
Under 80 ℃ and 120 ℃, carry out respectively stage by stage dry in the wet gel immigration Muffle furnace with above-mentioned formation.
(4) ignition process of xerogel
To in retort furnace stage by stage the exsiccant xerogel under 600 ℃, carry out ignition process, make the xerogel auto-combustion, the time remained on 15 minutes.
(5) Fe 2O 3/ Al 2O 3Synthesizing of the carrier of oxygen
The fluffy cellular-shaped products of combustion that forms through lighting up procedure is continued to carry out sintering processes in retort furnace, and sintering temperature remains on 950 ℃, and sintering time is 2 hours.
Use Fe 6Al 4The expression mass ratio is the Fe of 6:4 2O 3/ Al 2O 3The carrier of oxygen, its surface area are 1.65m 2/ g, average pore size is 8.1nm, and the parameter of other phases sees Table 1.Fe as can be seen from Table I 2O 3/ Al 2O 3When mass ratio was 6:4～8:2, surface area and size of microcrystal were littler, are suitable as the carrier of oxygen.Phase in the table one represents Fe 2O 3With Al 2O 3Mass ratio, Fe for example 8Al 2Expression Fe 2O 3With Al 2O 3Mass ratio be 8:2.
The Fe of table 1 different quality ratio 2O 3/ Al 2O 3The structural parameters of the carrier of oxygen
Figure A200910060787D00091
Fig. 1 is the change curve that the differential pore-size distribution of the carrier of oxygen of different quality ratio distributes with average pore size, as seen from the figure, generally, the Fe of different quality ratio 2O 3/ Al 2O 3The pore-size distribution of the carrier of oxygen is normal distribution curve, and along with Fe 2O 3The increase of content, the intensity of variation of liquid nitrogen hole adsorption volume is gradually littler, and the adsorption volume amount also reduces gradually, but with respect to disastrously assorted inert carrier Al 2O 3Fe 2O 3Even at 950 ℃ of sintering after 2 hours, still have bigger hole adsorption volume and anti-caking power preferably.
Fig. 2 is the Fe of different quality ratio 2O 3/ Al 2O 3Weight-loss curve when the carrier of oxygen and hydrogen reducing reaction, curve is unimodal curve, and Fe is described 2O 3/ Al 2O 3The reaction of the carrier of oxygen and hydrogen is mainly Fe 2O 3With a step reduction reaction of hydrogen, and mass ratio is the Fe of 8:2 2O 3/ Al 2O 3When the igniting product that the carrier of oxygen is processed without oversintering and hydrogen reaction and the reaction of hydrogen be still three-step reaction, even reduction temperature reaches 900 ℃ of times, also do not finish with the reduction reaction of hydrogen, specifically react suc as formula (1) (2) (3).This also illustrates the Fe for the different quality ratio 2O 3/ Al 2O 3The carrier of oxygen for the transfer rate of the Lattice Oxygen that improves the carrier of oxygen, carries out sintering processes or necessary.
3Fe 2O 3+H 2→2Fe 3O 4+H 2O (1)
Fe 3O 4+H 2→3Fe+4H 2O (2)
FeAl 2O4+H 2→Fe+Al 2O 3+H 2O (3)

Claims (2)

1, a kind of preparation method of iron based oxygen carrier, carry out according to following steps:
(1) metal nitrate is mixed with urea, add deionized water after mixing, uniform stirring obtains mixed solution, and the stoichiometric coefficient of metal nitrate and urea is 1, and metal nitrate is made of ferric nitrate and aluminum nitrate, the Fe that it comprises 2O 3With Al 2O 3Mass ratio be 6:4～8:2;
(2) adopt magnetic stirring apparatus that the mixing solutions that step (1) makes is stirred, obtain heavy-gravity colloidal sol;
(3) colloidal sol is carried out drying treatment and obtain xerogel;
(4) to the xerogel igniting, made the xerogel auto-combustion 10～15 minutes;
(5) combustion product that step (4) is formed is made sintering processes, obtains Fe 2O 3/ Al 2O 3Iron based oxygen carrier.
2, the preparation method of a kind of iron based oxygen carrier according to claim 1 is characterized in that, described step (3) is carried out drying stage by stage.
CNA200910060787XA 2009-02-17 2009-02-17 Process for preparing iron based oxygen carrier Pending CN101486941A (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260570A (en) * 2011-06-30 2011-11-30 华北电力大学 Mesoporous silica base molecular sieve based iron-base oxygen carrier and preparation method thereof
CN102382706A (en) * 2011-08-30 2012-03-21 华北电力大学 Cavity structure TiO2 based Fe-based oxygen carrier and its preparation method
CN102410530A (en) * 2011-10-26 2012-04-11 昆明理工大学 Method for preparing oxygen carrier for chemical-looping combustion by utilizing copper residues
CN102862959A (en) * 2011-07-07 2013-01-09 中国石油化工股份有限公司 Applications and preparation of high-activity oxygen carrier in chemical looping circulation hydrogen production
CN103113955A (en) * 2013-02-01 2013-05-22 东南大学 Preparation method of nano porous iron-base oxygen carrier for biological oil chemical-looping hydrogen production
CN103361146A (en) * 2012-04-01 2013-10-23 清华大学 Preparation method of high performance oxygen-carrying particles
CN105197884A (en) * 2015-09-16 2015-12-30 昆明理工大学 Method for preparing oxygen carrier of chemical-looping hydrogen production by means of titanomagnetite
CN107090323A (en) * 2017-03-03 2017-08-25 中国科学院青岛生物能源与过程研究所 It is a kind of that there is composite oxygen carrier of control oxidative function and preparation method thereof
CN109054754A (en) * 2018-06-21 2018-12-21 昆明理工大学 A kind of core-shell structure Fe2O3-Al2O3The preparation method of/(Al@C) the high temperature composite phase-change heat-storage carrier of oxygen
CN109054756A (en) * 2018-06-21 2018-12-21 昆明理工大学 A kind of core-shell structure Fe2O3-CeO2The preparation method of/(Al@C) the high temperature composite phase-change heat-storage carrier of oxygen
CN109092374A (en) * 2018-09-14 2018-12-28 昆明理工大学 A kind of preparation method of the honeycomb carrier of oxygen
CN111378511A (en) * 2018-12-28 2020-07-07 中国石油化工股份有限公司 Biomass microwave gasification utilization method and system
CN114887583A (en) * 2022-04-27 2022-08-12 北京科技大学 Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent

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刘杨先等: "化学链燃烧技术中载氧体的最新研究进展", 《现代化工》 *
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Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102260570A (en) * 2011-06-30 2011-11-30 华北电力大学 Mesoporous silica base molecular sieve based iron-base oxygen carrier and preparation method thereof
CN102862959A (en) * 2011-07-07 2013-01-09 中国石油化工股份有限公司 Applications and preparation of high-activity oxygen carrier in chemical looping circulation hydrogen production
CN102862959B (en) * 2011-07-07 2014-07-23 中国石油化工股份有限公司 Applications and preparation of high-activity oxygen carrier in chemical looping circulation hydrogen production
CN102382706A (en) * 2011-08-30 2012-03-21 华北电力大学 Cavity structure TiO2 based Fe-based oxygen carrier and its preparation method
CN102410530A (en) * 2011-10-26 2012-04-11 昆明理工大学 Method for preparing oxygen carrier for chemical-looping combustion by utilizing copper residues
CN102410530B (en) * 2011-10-26 2014-11-05 昆明理工大学 Method for preparing oxygen carrier for chemical-looping combustion by utilizing copper residues
CN103361146A (en) * 2012-04-01 2013-10-23 清华大学 Preparation method of high performance oxygen-carrying particles
CN103361146B (en) * 2012-04-01 2016-06-22 清华大学 A kind of preparation method of high-performance oxygen carrier granule
CN103113955A (en) * 2013-02-01 2013-05-22 东南大学 Preparation method of nano porous iron-base oxygen carrier for biological oil chemical-looping hydrogen production
CN105197884A (en) * 2015-09-16 2015-12-30 昆明理工大学 Method for preparing oxygen carrier of chemical-looping hydrogen production by means of titanomagnetite
CN107090323A (en) * 2017-03-03 2017-08-25 中国科学院青岛生物能源与过程研究所 It is a kind of that there is composite oxygen carrier of control oxidative function and preparation method thereof
CN107090323B (en) * 2017-03-03 2019-09-17 中国科学院青岛生物能源与过程研究所 A kind of composite oxygen carrier and preparation method thereof with control oxidative function
CN109054754A (en) * 2018-06-21 2018-12-21 昆明理工大学 A kind of core-shell structure Fe2O3-Al2O3The preparation method of/(Al@C) the high temperature composite phase-change heat-storage carrier of oxygen
CN109054756A (en) * 2018-06-21 2018-12-21 昆明理工大学 A kind of core-shell structure Fe2O3-CeO2The preparation method of/(Al@C) the high temperature composite phase-change heat-storage carrier of oxygen
CN109054754B (en) * 2018-06-21 2020-10-27 昆明理工大学 Core-shell structure Fe2O3-Al2O3Preparation method of (Al @ C) high-temperature composite phase-change heat-storage oxygen carrier
CN109054756B (en) * 2018-06-21 2020-10-27 昆明理工大学 Core-shell structure Fe2O3-CeO2Preparation method of (Al @ C) high-temperature composite phase-change heat-storage oxygen carrier
CN109092374A (en) * 2018-09-14 2018-12-28 昆明理工大学 A kind of preparation method of the honeycomb carrier of oxygen
CN111378511A (en) * 2018-12-28 2020-07-07 中国石油化工股份有限公司 Biomass microwave gasification utilization method and system
CN111378511B (en) * 2018-12-28 2021-05-04 中国石油化工股份有限公司 Biomass microwave gasification utilization method and system
CN114887583A (en) * 2022-04-27 2022-08-12 北京科技大学 Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent
CN114887583B (en) * 2022-04-27 2023-10-31 北京科技大学 Mesoporous alumina loaded Cu 2 Preparation method of O adsorbent

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Application publication date: 20090722