CN1762810A - One-step baking method for preparing magnetic microspheric alumina - Google Patents
One-step baking method for preparing magnetic microspheric alumina Download PDFInfo
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- CN1762810A CN1762810A CN 200510102791 CN200510102791A CN1762810A CN 1762810 A CN1762810 A CN 1762810A CN 200510102791 CN200510102791 CN 200510102791 CN 200510102791 A CN200510102791 A CN 200510102791A CN 1762810 A CN1762810 A CN 1762810A
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Abstract
The present invention provides process of preparing magnetic microspherical alumina. The prepared magnetic Me2+-Fe2+-Fe3+-LDHs core precursor is dispersed directly into aluminum sol and formed through oil column forming process, and through further washing, drying and once roasting, the magnetic microspherical alumina is prepared. The present invention has simplified operation, saving in power and lowered cost. The magnetic Me2+-Fe2+-Fe3+-LDHs core precursor may be well dispersed in aluminum sol, and after post treatment, especially high temperature roasting, the obtained magnetic microspherical alumina has well continuous magnetic domain structure and high magnetic performance. The magnetic microspherical alumina may be used as magnetic catalyst or magnetic catalyst carrier.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic microsphere aluminum oxide, be specifically related to prepare the method for magnetic microsphere aluminum oxide through an one-step baking.This magnetic microsphere aluminum oxide can be used as magnetic catalyst or magnetic catalyst carrier.
Background technology
Catalyzed reaction can be divided into fixed-bed process and fluidized-bed process by the technology type of implementing.The particle of used catalyzer is less in the fluidized-bed process, generally is to make after powder or the carrier loaded active ingredient of fine particle shape.Catalyzer is dispersed under the continuous disturbance of reactant in the fluidized-bed reactor and plays katalysis in fluidized-bed process, wearing and tearing that catalyzer causes because of collision and relative movement and to penetrate the loss that strainer causes with Flow of Goods and Materials be inevitable.In order to address the above problem, people have expected giving catalyzer magnetic, under the constraint of magnetic field force, make catalyzer in fluidized-bed evenly, arrange along the magnetic line of force direction in an orderly manner, increase the chance that reactant contacts with catalyzer, the raising catalytic efficiency.In addition, the position of granules of catalyst relative fixed in reaction bed, thus reduce or avoided collision, wearing and tearing and the loss of catalyzer.
Chemical industry progress .2002,21 (8), P536-539; Chemical reaction engineering and technology .2002,18 (1), P26-30; Refining of petroleum and chemical industry .2003,34 (11), P44-48 has reported the result of study of nickel base amorphous alloy magnetic powder catalyzer a plurality of reaction systems of catalytic hydrogenation in magnetic stablizing bed technology, but because of used catalyzer is an amorphous alloy, pore structure is bad, so activity is lower, can not realize the coordination and the unification of magnetic and catalyst activity.
Process engineering journal .2002,4 (2), P319-324 has reported with Fe
3O
4Magnetic nanoparticle is a magnetic nuclear, adopts the forming oil column legal system to be equipped with the result of study of the spherical alumina supporter of magnetic.Its weak point is Fe
3O
4Be hard magnetic material, have bigger coercive force after core prepares magnetic alumina carrier and then makes catalyzer, catalyzer has the magnetic by self to produce the autohemagglutination phenomenon, has caused difficulty for its homodisperse.
The inventor provides a kind of magnetic high-dispersion load metal catalyst and its production and use in application number is 200410048063.0 patent application.Wherein the preparation method of the magnetic microsphere aluminum oxide of Jie Shaoing at first prepares Me by the stratiform precursor process
2+-Fe
2+-Fe
3+-LDHs (hydrotalcite, Me
2+Be divalent-metal ion), then, it is distributed in the aluminium colloidal sol through grinding again after the surface coats, adopt oil-drop method to carry out the aluminum oxide that moulding, aging, washing, drying and roasting get microspheroidal, have magnetic at last.But the process of this preparation magnetic microsphere aluminum oxide is more loaded down with trivial details, need carry out twice high-temperature roasting and just can obtain sample.At first, need be with the Me of preparation
2+-Fe
2+-Fe
3+-LDHs roasting at high temperature then,, is carried out high-temperature roasting for the second time and is made peripheral hydrated aluminum oxide have good pore structure behind the peripheral generation of magnetic nuclear aqua oxidation aluminium lamination through oil-drop method to be transformed into ferrospinel magnetic nuclear.Zhi Bei magnetic microsphere aluminum oxide cost is higher like this, and the magnetic ferrite particle after mechanical mill that is equipped with through the high temperature roasting is bigger, the particle size distribution range broad, the content in each magnetic microsphere aluminum oxide particle has nothing in common with each other, and therefore has influence on the magnetic of microspheroidal aluminum oxide.
Summary of the invention
The method that only prepares magnetic microsphere aluminum oxide that the purpose of this invention is to provide a kind of simplification by bakes to burn the article, and the more original re-baking method of the magnetic of sample is improved to some extent.
Result of study shows, with Me
2+-Fe
2+-Fe
3+-LDHs is with hydrated aluminum oxide (boehmite) roasting, except the aluminum oxide that is transformed into ferrospinel and corresponding crystal formation respectively mutually, there is no the generation of cenotype, illustrate to exist directly with Me
2+-Fe
2+-Fe
3+-LDHs is applied to oil-drop method technology prepares magnetic microsphere aluminum oxide by bakes to burn the article possibility.The present invention directly examines precursor Me with the magnetic of preparation
2+-Fe
2+-Fe
3+-LDHs is distributed in the aluminium colloidal sol, adopts oil-drop method to carry out moulding, obtains magnetic microsphere aluminum oxide through washing, drying and roasting again.This method has been saved elder generation magnetic has been examined precursor Me
2+-Fe
2+-Fe
3+-LDHs carries out roasting makes its roasting process that changes into magnetic ferrite, and the magnetic of the microspheroidal aluminum oxide that obtains is compared with the sample in application number 200410048063.0 patent applications and is improved to some extent.
Concrete preparation method is as follows:
A. according to Fe
2++ Fe
3+=2Me
2+(Me
2++ Fe
2+)/Fe
3+=2～4 mol ratio preparation contains divalent-metal ion Me
2+And Fe
2+, Fe
3+The ionic mixing salt solution, wherein the volumetric molar concentration of each metal ion species is 0.1-0.6M; With NaOH and solubility weak acid sodium salt preparation mixed ammonium/alkali solutions, wherein NaOH concentration is 1.0-2.5M, and weak acid sodium salt concentration is 0-1.7M; At N
2Under the condition of protection, mixed ammonium/alkali solutions slowly is added drop-wise in the mixing salt solution, when the pH value in the system reaches 7-12, stops to drip, at N
2Protection in 20-65 ℃ of water-bath crystallization 5-25 hour down, after filtration, washing obtains the filter cake that solid content is 10-30%, its solids component is hydrotalcite type magnetic nuclear precursor Me
2+-Fe
2+-Fe
3+-LDHs.
Negatively charged ion in the mixing salt solution is Cl
-, NO
3 -Or SO
4 2-In any one or a few; Me
2+Be ionic radius and Fe
2+Close divalent-metal ion Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+Or Co
2+In any one or a few, be preferably Mn
2+, Co
2+, Ni
2+, Mg
2+In any one or two kinds; Solubility weak acid sodium salt is yellow soda ash, sodium bicarbonate or sodium-acetate.
B. aluminium powder is dissolved in the soluble aluminum salts solution of 0.1-2M and prepares Al
3+/ Cl
-Weight ratio is the aluminium colloidal sol of 0.9-1.5, is 3-25% by magnetic ferrite spinel shared weight percentage in the magnetic microsphere aluminum oxide that finally obtains again, with the Me of steps A preparation
2+-Fe
2+-Fe
3+-LDHs adds in the aluminium colloidal sol, thorough mixing and dispersion; In the mol ratio of Al and organic amine is that the ratio of 2-10 adds the organic amine solution that concentration is 1-5M in said mixture, and mixing the back, to spray into temperature by decollator be moulding in 50-105 ℃ the moulding oil, obtains the miniature bead of gel of 5-500 μ m; From oil, isolate bead,, through washing, drying, obtain the magnetic microsphere aluminum oxide presoma again in 100-180 ℃ of aging 5-20 hour.The iron level of aluminium powder should be less than 0.1%, its size range when 20-150 μ m its in aluminum soluble salt, be easier to the dissolving ℃
Employed aluminum soluble salt is Al (NO in the process
3)
39H
2O, AlCl
36H
2O, Al
2(SO
4)
318H
2A kind of among the O; Organic amine is a kind of in hexamethylenetetramine, the urea or the mixture of the two.
C. with the resulting microspheroidal alumina precursor of drying, rise to 700 ℃-1000 ℃, and kept 3-8 hour, obtain the magnetic microsphere aluminum oxide that granularity is 2-200 μ m with 10-20 ℃/minute temperature rise rate.
Measure the prepared magnetic microsphere aluminum oxide of the present invention with vibrating sample magnetometer, its specific saturation magnetization is greater than 3.8emu/g.
Unusual effect of the present invention is: omitted Me
2+-Fe
2+-Fe
3+-LDHs magnetic nuclear precursor carries out the process that roasting changes into magnetic ferrite, the step that can not only simplify the operation, save energy reduces cost, and directly steps A is obtained contain Me
2+-Fe
2+-Fe
3+The filter cake of-LDHs is distributed in the aluminium colloidal sol, can improve the dispersity of magnetic nuclear presoma in aluminium colloidal sol, and the domain structure that obtains magnetic microsphere aluminum oxide after subsequent disposal especially high-temperature roasting is more continuous, thereby its magnetic performance is further improved.
Embodiment
Embodiment 1:
A. in container with taking off CO
2Deionized water configuration Ni (NO
3)
26H
2O, Fe (NO
3)
39H
2O and FeCl
24H
2The mixing salt solution of O, and to make GOLD FROM PLATING SOLUTION belong to ionic concentration be respectively Ni
2+Be 0.2M, Fe
2+Be 0.2M, Fe
3+Be 0.2M.At N
2Under the condition of protection, slowly add mixed ammonium/alkali solutions in mixing salt solution, wherein NaOH concentration is 1.5M, Na
2CO
3Concentration is 0.5M.When the pH value in the system reaches 7, stop to drip mixed ammonium/alkali solutions, at N
2Under the protective condition in 20 ℃ of water-baths, crystallization 8 hours.Filter the back with taking off CO
2Frozen water washing, obtain hydrotalcite structure magnetic ferrite precursor Ni
2+-Fe
2+-Fe
3+-CO
3 2-LDHs.
B. size range is dissolved in the AlCl of 1M at 70-110 μ m aluminium powder
36H
2Prepare Al in the O solution
3+/ Cl
-Weight ratio is 1.35 aluminium colloidal sol, is 10% ratio in the quality percentage composition of ferrospinel in the magnetic microsphere aluminum oxide that finally obtains, and adds Ni
2+-Fe
2+-Fe
3+-CO
3 2-LDHs fully disperses back preparation suspended substance in aluminium colloidal sol; Hexamethylenetetramine is dissolved in the solution that deionized water is made into 3M, in the mol ratio of Al and hexamethylenetetramine in the aluminium colloidal sol is that 9 ratio adds hexamethylenetetramine solution in above-mentioned suspended substance, it is in 95 ℃ the moulding oil that mixture sprays into temperature by decollator, separate behind the moulding bead in 170 ℃ aging 10 hours, again through washing, dry magnetic microsphere aluminum oxide presoma.
C. with dried microballoon in 700 ℃ of roasting temperatures 4 hours, obtain the magnetic microsphere gamma-alumina of size range at 60-120 μ m.Recording specific saturation magnetization with vibrating sample magnetometer is 3.8emu/g.
Embodiment 2:
Keeping other preparation condition among the embodiment 1 constant, is 15% adding Ni by the part by weight of ferrospinel in the magnetic microsphere aluminum oxide that finally obtains
2+-Fe
2+-Fe
3+-CO
3 2-LDHs is in aluminium colloidal sol; The specific saturation magnetization that records magnetic microsphere aluminum oxide is 4.4emu/g, and crystal formation is the γ type.
Embodiment 3:
Keep other preparation condition among the embodiment 1 constant, hexamethylenetetramine during with the preparation magnetic alumina carrier is substituted by urea, aging temperature and digestion time become 130 ℃ and 18 hours respectively, rise to 900 ℃ with 15/ minute temperature rise rate, kept 6 hours, the specific saturation magnetization of gained magnetic microsphere aluminum oxide is 4.1emu/g, and crystal formation is the δ type.
Embodiment 4:
Keep other preparation condition among the embodiment 1 constant, the Ni (NO in the time of will preparing hydrotalcite (LDHs)
3)
26H
2O is by Co (Cl)
26H
2O substitutes; By the part by weight of ferrospinel in the magnetic microsphere aluminum oxide that finally obtains is the prepared Co of 10% adding
2+-Fe
2+-Fe
3+-CO
3 2-LDHs is in aluminium colloidal sol; The specific saturation magnetization that records magnetic microsphere aluminum oxide is 4.8emu/g, and crystal formation is the γ type.
Embodiment 5:
Keep other preparation condition among the embodiment 1 constant, dried microballoon in 1000 ℃ of roasting temperatures 4 hours, is obtained size range at the magnetic microsphere θ of 55-110 μ m aluminum oxide.Recording specific saturation magnetization with vibrating sample magnetometer is 4.4emu/g.
Embodiment 6:
Keep other preparation condition among the embodiment 1 constant, particle size range is dissolved in the Al (NO of 1.5M at the aluminium powder of 40-100 μ m
3)
39H
2O prepares aluminium colloidal sol, obtains the magnetic microsphere gamma-alumina of size range at 65-118 μ m.Recording specific saturation magnetization with vibrating sample magnetometer is 3.9emu/g.
Embodiment 7:
Keep other preparation condition among the embodiment 1 constant, with the Na of preparation magnetic nuclear presoma
2CO
3Replace to NaHCO
3, its concentration in mixed ammonium/alkali solutions is 0.8M.At first prepare Ni
2+-Fe
2+-Fe
3+-CO
3 2-Behind the LDHs magnetic nuclear presoma, finally prepare the magnetic microsphere gamma-alumina of size range at 58-130 μ m.Recording specific saturation magnetization with vibrating sample magnetometer is 4.0emu/g.
Claims (2)
1. one kind prepares the method for magnetic microsphere aluminum oxide through an one-step baking, and concrete steps are as follows:
A. according to Fe
2++ Fe
3+=2Me
2+(Me
2++ Fe
2+)/Fe
3+=2～4 mol ratio preparation contains divalent-metal ion Me
2+And Fe
2+, Fe
3+The ionic mixing salt solution, wherein the volumetric molar concentration of each metal ion species is 0.1-0.6M; With NaOH and solubility weak acid sodium salt preparation mixed ammonium/alkali solutions, wherein NaOH concentration is 1.0-2.5M, and weak acid sodium salt concentration is 0-1.7M; At N
2Under the condition of protection, mixed ammonium/alkali solutions slowly is added drop-wise in the mixing salt solution, when the pH value in the system reaches 7-12, stops to drip, at N
2Protection in 20-65 ℃ of water-bath crystallization 5-25 hour down, after filtration, washing obtains the filter cake that solid content is 10-30%, its solids component is hydrotalcite type magnetic nuclear precursor Me
2+-Fe
2+-Fe
3+-LDHs;
Me
2+Be ionic radius and Fe
2+Close divalent-metal ion: Mn
2+, Zn
2+, Cu
2+, Ni
2+, Mg
2+Or Co
2+In any one or a few;
B. aluminium powder is dissolved in the soluble aluminum salts solution of 0.1-2M and prepares Al
3+/ Cl
-Weight ratio is the aluminium colloidal sol of 0.9-1.5, is 3-25% by magnetic ferrite spinel shared weight percentage in the magnetic microsphere aluminum oxide that finally obtains again, with the Me of steps A preparation
2+-Fe
2+-Fe
3+-LDHs adds in the aluminium colloidal sol, thorough mixing and dispersion; In the mol ratio of Al and organic amine is that the ratio of 2-10 adds the organic amine solution that concentration is 1-5M in said mixture, and mixing the back, to spray into temperature by decollator be moulding in 50-105 ℃ the moulding oil, obtains the miniature bead of gel of 5-500 μ m; From oil, isolate bead,, through washing, drying, obtain the magnetic microsphere aluminum oxide presoma again in 100-180 ℃ of aging 5-20 hour;
C. with the resulting microspheroidal alumina precursor of drying, rise to 700 ℃-1000 ℃, and kept 3-8 hour, obtain the magnetic microsphere aluminum oxide that granularity is 2-200 μ m with 10-20 ℃/minute temperature rise rate.
2. according to claim 1ly prepare the method for magnetic microsphere aluminum oxide, it is characterized in that the negatively charged ion in the described mixing salt solution of steps A is Cl through an one-step baking
-, NO
3-Or SO
4 2-In any one or a few; Me
2+Be Mn
2+, Co
2+, Ni
2+, Mg
2+In any one or two kinds; Solubility weak acid sodium salt is yellow soda ash, sodium bicarbonate or sodium-acetate;
The described aluminum soluble salt of step B is Al (NO
3)
39H
2O, AlCl
36H
2O, Al
2(SO
4)
318H
2A kind of among the O; Organic amine is a kind of in hexamethylenetetramine, the urea or the mixture of the two.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100463715C (en) * | 2007-06-08 | 2009-02-25 | 北京化工大学 | Core-shell structure magnetic microsphere aluminum oxide and method for preparing the same |
| CN100479921C (en) * | 2006-06-30 | 2009-04-22 | 北京化工大学 | Sphericity spinel material with cage construction and method for preparing the same |
| CN101279295B (en) * | 2007-04-03 | 2010-12-08 | 中国科学院过程工程研究所 | Preparation method of spherical magnetic nano alumina supporting material |
| CN101172255B (en) * | 2006-10-31 | 2011-04-20 | 中国石油化工股份有限公司 | Method for preparing magnetic microspheric alumina support |
| CN114438324A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Valuable metal enrichment method for waste FCC catalyst |
Family Cites Families (7)
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| US4804796A (en) * | 1984-04-23 | 1989-02-14 | California Institute Of Technology | Catalytic, hollow, refractory spheres, conversions with them |
| US6676783B1 (en) * | 1998-03-27 | 2004-01-13 | Siemens Westinghouse Power Corporation | High temperature insulation for ceramic matrix composites |
| CN1100040C (en) * | 1999-04-29 | 2003-01-29 | 中国石油化工集团公司 | Hydrofinishing method of caprolactam |
| CN1119333C (en) * | 2000-06-28 | 2003-08-27 | 中国石油化工股份有限公司 | Process for hydrorefining caprolactam |
| CN1180881C (en) * | 2002-07-23 | 2004-12-22 | 北京化工大学 | Magnetic nano solid base catalyst and its preparnig method |
| CN1226088C (en) * | 2002-09-19 | 2005-11-09 | 北京化工大学 | High Dispersing palladium catalyst prepared by lamellar precursor and preparation method thererof |
| CN100372610C (en) * | 2004-06-14 | 2008-03-05 | 北京化工大学 | Magnetic microspheric high-dispersion loaded metal catalyst, preparing method and use |
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2005
- 2005-09-19 CN CNB200510102791XA patent/CN100345758C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100479921C (en) * | 2006-06-30 | 2009-04-22 | 北京化工大学 | Sphericity spinel material with cage construction and method for preparing the same |
| CN101172255B (en) * | 2006-10-31 | 2011-04-20 | 中国石油化工股份有限公司 | Method for preparing magnetic microspheric alumina support |
| CN101279295B (en) * | 2007-04-03 | 2010-12-08 | 中国科学院过程工程研究所 | Preparation method of spherical magnetic nano alumina supporting material |
| CN100463715C (en) * | 2007-06-08 | 2009-02-25 | 北京化工大学 | Core-shell structure magnetic microsphere aluminum oxide and method for preparing the same |
| CN114438324A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Valuable metal enrichment method for waste FCC catalyst |
| CN114438324B (en) * | 2020-10-20 | 2024-02-13 | 中国石油化工股份有限公司 | Valuable metal enrichment method for waste FCC catalyst |
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