CN104445322A - Method for preparing porous alumina particles from aluminum hydroxide extracted from slag - Google Patents

Method for preparing porous alumina particles from aluminum hydroxide extracted from slag Download PDF

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Publication number
CN104445322A
CN104445322A CN201410762330.4A CN201410762330A CN104445322A CN 104445322 A CN104445322 A CN 104445322A CN 201410762330 A CN201410762330 A CN 201410762330A CN 104445322 A CN104445322 A CN 104445322A
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CN
China
Prior art keywords
slag
porous alumina
hours
particles
extracted
Prior art date
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Pending
Application number
CN201410762330.4A
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Chinese (zh)
Inventor
肖秋国
申少华
彭美勋
杨明平
张欣
张飞
张玲玲
李维君
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Hunan University of Science and Technology
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Hunan University of Science and Technology
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Priority to CN201410762330.4A priority Critical patent/CN104445322A/en
Publication of CN104445322A publication Critical patent/CN104445322A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
    • C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention discloses a method for preparing porous alumina particles from aluminum hydroxide extracted from slag. The method comprises the following steps: (1) extracting a white Al(OH)3 flocculent precipitate from aluminum-containing slag, washing and purifying to obtain a water-containing Al(OH)3 precipitate, standing, and airing, so that the moisture content is in a range from 30 to 60 percent; adopting a sol-gel method, adding glacial acetic acid, stirring at normal temperature under the action of a magnetic stirrer until the precipitate disappears to form semi-transparent aluminum acetate basic sol, and standing and aging for 12-24 hours; and (2) performing spray drying to obtain white powder, adding the powder into a muffle furnace, and calcining at the temperature of 1050-1200 DEG C for 2-4 hours, wherein the calcined white powder is the target product. According to the method disclosed by the invention, alumina of which the particles have porous properties is prepared, the porous alumina is not formed by bridging among the particles, the specific surface area is large, loading of the catalyst is promoted, and the porous alumina particles can serve as excellent catalyst carriers.

Description

A kind of aluminium hydroxide extracted from slag prepares the method for porous oxidation aluminum particulate
Technical field
The present invention relates to chemical technology field, particularly a kind of preparation method of porous oxidation aluminum particulate.
Background technology
Along with the development of material technology, porous material due to its excellent physical and chemical performance, and more and more obtains the attention of people.Activated porous alumina, as the one of porous material, due to its have both simultaneously porous material and stupalith performance and become people research new direction.The existing method preparing porous alumina has a lot, comprises the multiple methods such as masterplate method, organic additive method, plasma body spray method and electrochemical process.In general, masterplate method needs multiple step, prepare comparatively loaded down with trivial details, and cost is higher.And the method such as organic additive and ionspray only needs one-step synthesis, preparation is got up relatively easily easy.Existing organic additive process, the hole that organic solvent is formed does not have masterplate method regular, and needs to attempt additive or experiment condition, could obtain the porous material of uniform pore diameter.Although and plasma body spray method than masterplate method and organic additive all simple, need special equipment.Electrochemical process namely what is often called anonizing, actual effect is not fine.
The people such as Tokudome (Yasuaki Tokudome, Koji Fujita, Kazuki Nakanishi, Kiyotaka Miura, et al. Synthesis of Monolithic Al 2o 3with Well-Defined Macropores and Mesostructured Skeletons via the Sol-Gel Process Accompanied by Phase Separation [J]. Chem. 2007,19:3393-3398) with AlCl 36H 2o is as aluminium source, and ethanol is as solvent, and add the propylene oxide of different concns as linking agent, when the concentration of propylene oxide is very low (≤0.04), the particle size of gained aluminum oxide is very little, is almost in nanometer scale; When the concentration of propylene oxide is between 0.05-0.11, what obtain is class circuit board type macroporous structure, and the increase of concentration along with propylene oxide, aperture size becomes large.When can work as concentration >=0.012 of propylene oxide, the macroporous structure of the aluminum oxide prepared disappears, and what obtain is but dispersed particle preferably one by one.
The people such as Liu (Chang Liu, Yongchun Liu, Qingxin Ma, et al. Mesoporous transition alumina with uniform pore structure synthesized by alumisol spray pyrolysis [J]. Chemical Engineering Journal. 2010,136:133 – 142) adopt plasma spraying legal system to be about the porous oxidation aluminum of 3.0-4.7 nm for aperture, prepared aluminum oxide illustrates stronger stability, is expected to obtain potential application in the industrial production.Its plasma body fog system is made up of three major portions, and one is made up of domestic atomizer, and a part is dehumidification system, and a part is high temperature sintering system in addition.The method than masterplate method and organic additive all also simple, not only only need a step to complete experiment, but also not Structure of need linking agent.On time and cost, all save than the two.But prerequisite needs such a set of equipment.
Generally speaking, its particle of porous alumina itself also imporosity prepared by existing method forms hole by the bridging action between particle.
Summary of the invention
The object of the present invention is to provide a kind of aluminium hydroxide extracted from the slag such as coal gangue, ferro-aluminum slag to be that porous oxidation aluminum particulate prepared by raw material, itself there is porous character, instead of form porous by building bridge between particle.
For achieving the above object, embodiment of the present invention are: a kind of method extracted aluminium hydroxide and prepare porous oxidation aluminum particulate from slag, comprises the following steps:
(1) white Al (OH) is extracted from containing aluminium ore slag 3flocks, and carry out washing the moisture Al (OH) of purification acquisition 3precipitation, air-dry through leaving standstill, (density is at 1.25 ~ 1.45g/cm in 30 ~ 60% scopes to control its water content 3scope within), then adopt sol-gel method, filling Al (OH) 3glacial acetic acid is added, stirring at normal temperature under the effect of magnetic stirring apparatus in sedimentary beaker, until precipitation disappears form translucent eston colloidal sol, then still aging 12 ~ 24 hours.The described aluminium ore cinder ladle that contains draws together coal gangue, ferro-aluminum slag.
(2) carry out spraying dry after colloidal sol ageing, the white powder obtained, put into retort furnace in 1050 ~ 1200 DEG C of calcinings 2 ~ 4 hours, the white powder after calcining is target compound.
As optimization, in step (1), described Al (OH) 3the volume ratio of throw out and Glacial acetic acid is 1:10 ~ 40, and in colloidal sol, the concentration of eston controls in the scope of 0.2 ~ 2mol/L.
As optimization, in step (2), spray-dired condition is: air outlet temperature is 100 DEG C, and the cleansing pin time is 2s, blower fan 60.00Hz, and spray pressure is 0.2MPa, and striker pressure is 0.4MPa.Dynamic parameter is: vapo(u)rizing temperature 160 DEG C ~ 240 DEG C, spray velocity is 10r/min ~ 30r/min.
The present invention utilizes the aluminium hydroxide extracted from the slag such as coal gangue, ferro-aluminum slag, obtains aluminum subacetate, obtains aluminum subacetate powder after ageing by spray-dired mode, obtain porous oxidation aluminum particulate finally by quick burning with acetic acid reaction.The present invention has prepared the aluminum oxide that a kind of particle itself has porous character, instead of forms the aluminum oxide of porous by building bridge between particle, and specific surface area is comparatively large, is very beneficial for the load of catalyzer, can as good support of the catalyst.New there is high value-added product for extracting alumina from coal gangue provides one.
Accompanying drawing explanation
What Fig. 1 showed is its particle of existing porous alumina itself and imporosity, is to form hole by the bridging action between particle;
Fig. 2 is porous alumina granule-morphology figure prepared by the present invention, shows itself to have porous character;
Fig. 3 is the comparison diagram of XRD diffraction of the present invention and figure standard diagram, and showing that its thing phase composite is detected by X-ray diffraction (XRD), after obtaining its XRD diffractogram, is α-Al with standard diagram comparative analysis result 2o 3.
Fig. 4 is Technology Roadmap of the present invention.
Embodiment
Embodiment 1:
From slag, extract the method that aluminium hydroxide prepares porous oxidation aluminum particulate, concrete grammar and step as follows:
(1) from coal gangue, white Al (OH) is first extracted 3(aluminium hydroxide) flocks, and carry out washing the moisture Al (OH) of purification acquisition 3precipitation, air-dry through leaving standstill, get the Al (OH) of water content about 30% 3precipitation about 12.5 ~ 14.5g(10mL) put in beaker, then adopt sol-gel method, add the Glacial acetic acid of 100 ~ 400mL, stirring at normal temperature under the effect of magnetic stirring apparatus, until precipitation disappears form translucent eston colloidal sol, then still aging 24 hours;
(2), after colloidal sol ageing, the DC-1500 spray-drier of Shanghai Da Cheng experimental installation company limited is adopted to be carried out spraying dry.The main preset parameter of spray-drier is: air outlet temperature is 100 DEG C, and the cleansing pin time is 2s, blower fan 60.00Hz, and spray pressure is 0.2MPa, and striker pressure is 0.4MPa.Dynamic parameter is: vapo(u)rizing temperature 160 DEG C ~ 240 DEG C, and spray velocity is 10r/min ~ 30r/min;
(3) the white powder 6 ~ 7g obtained after drying.Put into retort furnace in 1100 DEG C of calcinings 3 hours, the white powder after calcining is observed by scanning electronic microscope (SEM), and its pattern as shown in Figure 2.Its thing phase composite is detected by X-ray diffraction (XRD), after obtaining its XRD diffractogram, is α-Al with standard diagram comparative analysis result 2o 3, as shown in Figure 3.
Embodiment 2:
White Al (OH) is extracted from ferro-aluminum slag 3(aluminium hydroxide) flocks, other step and method is identical with embodiment 1.
Embodiment 3: first prepare white Al (OH) with materials such as metallic aluminium and aluminium salt 3flocks, other step and method is identical with embodiment 1.

Claims (3)

1. from slag, extract the method that aluminium hydroxide prepares porous oxidation aluminum particulate, it is characterized in that, comprise the following steps:
(1) white Al (OH) is extracted from containing aluminium ore slag 3flocks, and carry out washing the moisture Al (OH) of purification acquisition 3precipitation, air-dry through leaving standstill, control its water content in 30 ~ 60% scopes, then adopt sol-gel method, fill Al (OH) 3glacial acetic acid is added, stirring at normal temperature under the effect of magnetic stirring apparatus in sedimentary beaker, until precipitation disappears form translucent eston colloidal sol, then still aging 12 ~ 24 hours,
The described aluminium ore cinder ladle that contains draws together coal gangue, ferro-aluminum slag;
(2) carry out spraying dry after colloidal sol ageing, the white powder obtained, put into retort furnace in 1050 ~ 1200 DEG C of calcinings 2 ~ 4 hours, the white powder after calcining is target compound.
2. the method extracted aluminium hydroxide and prepare porous oxidation aluminum particulate from slag according to claim 1, is characterized in that, in step (1), and described Al (OH) 3the volume ratio of throw out and Glacial acetic acid is 1:10 ~ 40, and in colloidal sol, the concentration of eston controls in the scope of 0.2 ~ 2mol/L.
3. the method extracted aluminium hydroxide and prepare porous oxidation aluminum particulate from slag according to claim 1, it is characterized in that, in step (2), spray-dired condition is: air outlet temperature is 100 DEG C, and the cleansing pin time is 2s, blower fan 60.00Hz, spray pressure is 0.2MPa, striker pressure is 0.4MPa, and dynamic parameter is: vapo(u)rizing temperature 160 DEG C ~ 240 DEG C, spray velocity is 10r/min ~ 30r/min.
CN201410762330.4A 2014-12-13 2014-12-13 Method for preparing porous alumina particles from aluminum hydroxide extracted from slag Pending CN104445322A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108336348A (en) * 2018-03-29 2018-07-27 新乡学院 A kind of method of alumina-coated anode material for lithium-ion batteries
CN114471143A (en) * 2021-12-30 2022-05-13 山东中航天业科技有限公司 Defect alumina modified wide-temperature desulfurizer and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070189959A1 (en) * 2006-02-15 2007-08-16 Steven Allen Carlson Methods of preparing separators for electrochemical cells
CN102795647A (en) * 2011-05-26 2012-11-28 中国石油化工股份有限公司 Macro-porous aluminum oxide and preparation method thereof
CN103539173A (en) * 2013-10-06 2014-01-29 太原理工大学 Highly thermostable and ordered mesoporous alumina material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070189959A1 (en) * 2006-02-15 2007-08-16 Steven Allen Carlson Methods of preparing separators for electrochemical cells
CN102795647A (en) * 2011-05-26 2012-11-28 中国石油化工股份有限公司 Macro-porous aluminum oxide and preparation method thereof
CN103539173A (en) * 2013-10-06 2014-01-29 太原理工大学 Highly thermostable and ordered mesoporous alumina material and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
肖秋国等: "从煤矸石中提取氧化铝的影响因素", 《煤炭科学技术》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108336348A (en) * 2018-03-29 2018-07-27 新乡学院 A kind of method of alumina-coated anode material for lithium-ion batteries
CN114471143A (en) * 2021-12-30 2022-05-13 山东中航天业科技有限公司 Defect alumina modified wide-temperature desulfurizer and preparation method and application thereof
CN114471143B (en) * 2021-12-30 2023-02-17 山东中航天业科技有限公司 Defect alumina modified wide-temperature desulfurizer and preparation method and application thereof

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Application publication date: 20150325