CN119143497A - Magnesium-aluminum composite oxide and preparation method thereof - Google Patents
Magnesium-aluminum composite oxide and preparation method thereof Download PDFInfo
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- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 102
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims abstract description 82
- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 64
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims abstract description 64
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 50
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 47
- 239000011777 magnesium Substances 0.000 claims abstract description 47
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000000126 substance Substances 0.000 claims abstract description 32
- 230000000977 initiatory effect Effects 0.000 claims abstract description 27
- -1 aluminum alkoxide Chemical class 0.000 claims abstract description 25
- 230000035484 reaction time Effects 0.000 claims abstract description 19
- 230000007062 hydrolysis Effects 0.000 claims abstract description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 10
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000009835 boiling Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 9
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 7
- 229910052740 iodine Inorganic materials 0.000 claims description 7
- 239000011630 iodine Substances 0.000 claims description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 2
- 229960002523 mercuric chloride Drugs 0.000 claims description 2
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 2
- 238000000746 purification Methods 0.000 abstract description 6
- 239000002002 slurry Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 239000012535 impurity Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 238000009616 inductively coupled plasma Methods 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229910052596 spinel Inorganic materials 0.000 description 7
- 239000011029 spinel Substances 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- RJZNFXWQRHAVBP-UHFFFAOYSA-I aluminum;magnesium;pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Al+3] RJZNFXWQRHAVBP-UHFFFAOYSA-I 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 2
- 244000046052 Phaseolus vulgaris Species 0.000 description 2
- 150000001449 anionic compounds Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229910001412 inorganic anion Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002891 organic anions Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- TURPNXCLLLFJAP-UHFFFAOYSA-N 2-[2-(2-hydroxyethoxy)ethoxy]ethyl hydrogen sulfate Chemical compound OCCOCCOCCOS(O)(=O)=O TURPNXCLLLFJAP-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- OIPWQYPOWLBLMR-UHFFFAOYSA-N hexylalumane Chemical compound CCCCCC[AlH2] OIPWQYPOWLBLMR-UHFFFAOYSA-N 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000013460 polyoxometalate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
- C04B35/443—Magnesium aluminate spinel
-
- 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
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
-
- 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
-
- 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
- C01F7/021—After-treatment of oxides or hydroxides
-
- 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
- C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
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- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/54—Particle size related information
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to the field of preparation of magnesium-aluminum composite oxides and discloses a magnesium-aluminum composite oxide and a preparation method thereof. The method comprises the steps of (1) carrying out a first reaction on an aluminum simple substance and a first fatty alcohol under anhydrous conditions to obtain a material containing aluminum alkoxide, (2) carrying out a second reaction on the material containing aluminum alkoxide, a magnesium simple substance and a second fatty alcohol obtained in the step (1) under anhydrous conditions under the action of a catalyst, and (3) carrying out hydrolysis on a reaction product obtained in the step (2) to obtain a magnesium aluminum bimetallic alkoxide, and then optionally drying and roasting to obtain a magnesium aluminum composite oxide, wherein the first fatty alcohol and the second fatty alcohol respectively independently comprise n-amyl alcohol and optionally n-hexyl alcohol. The preparation method of the magnesium-aluminum composite oxide provided by the invention can obtain the high-purity magnesium-aluminum composite oxide without subsequent purification treatment, and has the advantages of short initiation time and short reaction time.
Description
Technical Field
The invention relates to the field of preparation of magnesium-aluminum composite oxides, in particular to a magnesium-aluminum composite oxide and a preparation method thereof.
Background
The high-purity superfine magnesia-alumina spinel powder (magnesia-alumina composite oxide) is synthesized artificially, and has purity over 99.99% and granularity of submicron-nanometer level. The magnesia-alumina spinel powder is mainly used in refractory material, wear-resistant material, fine ceramic and pigment industry before, and is gradually expanded to the high technical fields of light performance materials, catalysts, carrier materials thereof and the like in recent years. With the development of laser crystal materials and functional materials, higher requirements are put on the purity, granularity and chemical uniformity of magnesia-alumina spinel powder. Therefore, the prepared magnesia-alumina spinel powder with high purity, superfine and good chemical uniformity has important significance for application.
At present, many researches are carried out on the preparation method of the magnesia-alumina spinel at home and abroad, and mainly adopted methods include a solid phase method, a precipitation method, a sol-gel method, an aluminum-magnesium bimetallic alkoxide hydrolysis method, a hydrothermal synthesis method, a combustion synthesis method, a solution evaporation method and the like. The aluminum-magnesium bi-metal alkoxide hydrolysis method has the advantages that metal aluminum, metal magnesium and fatty alcohol are used as raw materials, impurity ions are not introduced in the reaction process, and the aluminum-magnesium bi-metal alkoxide hydrolysis method can be further purified by reduced pressure distillation or recrystallization, so that the purity of the obtained magnesium-aluminum spinel powder is higher.
US6514473B2, US6517795B1, US20010001653A1, CN1109576C and CN1171979a disclose a process for preparing high purity hydrotalcite by reacting an alcohol or alcohol mixture with at least one or more divalent metals and at least one or more trivalent metals and hydrolyzing the obtained alkoxide mixture with water, the corresponding metal oxides being prepared by calcination. However, in the whole preparation process, the required reaction temperature of fatty alcohol and metallic aluminum and metallic magnesium is far higher than the boiling point of fatty alcohol, the reaction can be carried out only by a special reaction device, the reaction condition is harsh, the volatilization loss of alcohol is more, the reaction can be completed only by adding alcohol for many times, the operation is complex, the cost is increased, the industrial application is not favored, and the water-soluble organic or inorganic anions are added in the hydrolysis process so as to introduce new impurities, thus the purity of the obtained product is lower, and the subsequent filtering and purifying treatment is needed.
Therefore, there is a need to develop a process for preparing high purity magnesia-alumina spinel powder with simple operation.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a magnesium-aluminum composite oxide and a preparation method thereof. The preparation method of the magnesium-aluminum composite oxide provided by the invention can obtain the high-purity magnesium-aluminum composite oxide without subsequent purification treatment, and has the advantages of short initiation time and short reaction time.
In order to achieve the above object, an aspect of the present invention provides a method for preparing a magnesium aluminum composite oxide, the method comprising the steps of:
(1) Under the anhydrous condition, carrying out a first reaction on an aluminum simple substance and first fatty alcohol to obtain a material containing aluminum alkoxide;
(2) Under the action of a catalyst, carrying out a second reaction on the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1) under the anhydrous condition;
(3) Hydrolyzing the reaction product in the step (2) to obtain magnesium-aluminum bimetallic alkoxide, and then optionally drying and roasting to obtain magnesium-aluminum composite oxide;
Wherein the first fatty alcohol and the second fatty alcohol each independently comprise n-amyl alcohol and optionally n-hexyl alcohol, and the molar dosage ratio of the n-amyl alcohol to the n-hexyl alcohol is 1:0-10.
In the art, the higher the carbon number of the n-alcohol, the faster the reaction rate, but the more severe the reaction and the difficult to control, and at the same time, the higher the viscosity of the n-alcohol along with the increase of the carbon chain, which is unfavorable for the synthesis reaction, and the magnesium-aluminum composite oxide is generally prepared by adopting C2-C4 fatty alcohols such as ethanol, isopropanol, n-butanol and the like. In addition, in the reaction of magnesium and fatty alcohol, the initiation of the reaction of metal magnesium and fatty alcohol is difficult, the reaction of fatty alcohol of C2-C4 and metal magnesium is usually carried out under the condition of taking a catalyst and/or an organic solvent as a dispersing agent, the initiation time is long, and new impurities are introduced. The inventor finds that the magnesium-aluminum composite oxide can be prepared by adopting n-alcohol comprising n-amyl alcohol and optionally n-hexyl alcohol under the anhydrous condition through a specific two-step reaction, and the magnesium-aluminum composite oxide with high purity can be obtained without subsequent purification treatment (such as reduced pressure distillation, recrystallization and the like), and meanwhile, the initiation time can be shortened when the specific alcohol is adopted to participate in the reaction, so that the overall reaction time of a reaction system is shortened.
In a second aspect, the present invention provides a magnesium-aluminum composite oxide obtained by the preparation method of the first aspect.
Through the technical scheme, the beneficial effects of the invention include:
The preparation method provided by the invention can obtain the high-purity magnesium-aluminum composite oxide without subsequent purification treatment, the purity is more than 99.99%, and meanwhile, the magnesium-aluminum ratio in the magnesium-aluminum composite oxide can be flexibly adjusted so as to meet the actual needs.
Preferably, the preparation method provided by the invention has the advantages of short initiation time, high reaction rate, mild reaction conditions and no introduction of other impurities except impurities carried by the metal magnesium aluminum. The preparation method provided by the invention has the advantages of less catalyst consumption and low preparation cost.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, the "first" and "second" do not limit each substance and operation, but only distinguish substances introduced in different steps from each other, and perform operations in different stages.
In one aspect, the present invention provides a method for preparing a magnesium aluminum composite oxide, the method comprising the steps of:
(1) Under the anhydrous condition, carrying out a first reaction on an aluminum simple substance and first fatty alcohol to obtain a material containing aluminum alkoxide;
(2) Under the action of a catalyst, carrying out a second reaction on the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1) under the anhydrous condition;
(3) Hydrolyzing the reaction product in the step (2) to obtain magnesium-aluminum bimetallic alkoxide, and then optionally drying and roasting to obtain magnesium-aluminum composite oxide;
Wherein the first fatty alcohol and the second fatty alcohol each independently comprise n-amyl alcohol and optionally n-hexyl alcohol, and the molar dosage ratio of the n-amyl alcohol to the n-hexyl alcohol is 1:0-10.
In the preparation method, the reactions in the step (1) and the step (2) are carried out under anhydrous conditions, so that the problem that the reaction cannot be carried out continuously due to the fact that aluminum alkoxide generated in the step (1) and magnesium aluminum alkoxide generated in the step (2) are hydrolyzed to generate hydroxide is avoided.
The mode for realizing the anhydrous condition is not particularly limited, and can be carried out by adopting the technical means conventional in the art. For example, the reaction can be carried out in a three-neck flask, and the three-neck flask can be cleaned and dried in advance or put into an oven for drying before the reaction, so that the three-neck flask is clean and anhydrous.
The anhydrous condition according to the present invention does not require control of complete absence of water, but means that no additional water is introduced, but that a very small amount of water adsorbed in the air in the raw material and/or the catalyst is not excluded.
In the present invention, the term "optionally" means with or without, with or without addition, with or without, unless otherwise specified. Specifically, n-hexanol may be added to the first fatty alcohol and the second fatty alcohol, or n-hexanol may not be added.
According to the present invention, preferably, the first fatty alcohol comprises n-pentanol and n-hexanol, and the molar usage ratio of n-pentanol to n-hexanol is 1:0.1-1;
the second fatty alcohol is n-amyl alcohol.
In the present invention, the molar ratio of n-pentanol to n-hexanol is 1:0.1-1, for example, 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1:0.5, 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1, and any value in the range consisting of any two of these values. With the adoption of the preferred embodiment, the magnesium-aluminum composite oxide with high purity is obtained, and the reaction initiation time is shortened. When the molar ratio of n-pentanol to n-hexanol is higher than the above range, the first reaction initiation time is significantly increased, thereby extending the overall reaction time of the reaction system, and when the molar ratio of n-pentanol to n-hexanol is lower than the above range, the purity of the magnesium-aluminum composite oxide is reduced.
According to the present invention, the temperature of the first reaction is preferably 20 ℃ below the boiling point of the first fatty alcohol to the boiling point of the first fatty alcohol, preferably 20 ℃ below the boiling point of the first fatty alcohol to 2 ℃ below the boiling point of the first fatty alcohol. With the preferred embodiment, the higher reaction rate can be maintained, and incomplete reaction caused by volatilization loss of the first fatty alcohol at too high a temperature can be avoided.
When the first fatty alcohol comprises n-pentanol and n-hexanol, the temperature of the first reaction is based on the boiling point of n-pentanol.
The initiation time in the present invention means a time from the initiation of the temperature rise to the reaction temperature until the generation of a continuous large amount of bubbles (or the generation of strings of bubbles) in the solution is observed. The preparation method provided by the invention can obviously shorten the initiation time of the first reaction. According to the invention, the initiation time of the first reaction is preferably from 0.2 to 4.5 hours, preferably from 0.2 to 0.5 hours.
The reaction time as used herein refers to the time from when a continuous mass of bubbles (or strings of bubbles) are observed in the solution to when no significant bubbles are observed in the solution. The preparation method provided by the invention can obviously shorten the reaction time of the first reaction. Preferably, the reaction time of the first reaction is 0.4 to 4 hours, preferably 0.5 to 2 hours.
According to the invention, the molar ratio of the elemental aluminum to the first fatty alcohol is preferably from 1:3 to 5, preferably from 1:3.1 to 4.5. With this preferred embodiment, complete reaction of the elemental aluminum is facilitated.
According to the present invention, preferably, the purity of the elemental aluminum is not less than 99.9 mass%. With this preferred embodiment, it is advantageous to obtain a magnesium aluminum composite oxide with high purity.
The present invention is not particularly limited in the form of the aluminum element, and may be selected as usual in the art. Preferably, the aluminum simple substance is selected from at least one of aluminum blocks, aluminum beans, aluminum sheets, aluminum wires and aluminum scraps.
The aluminum blocks, beans, flakes, filaments, and scraps of the present invention are well known to those skilled in the art and the present invention is not described in detail herein.
According to one embodiment of the invention, the aluminum alkoxide-containing material obtained in step (1) is cooled to 80-100 ℃ and then subjected to a second reaction. With such preferred embodiments, volatilization of the alcohol can be effectively reduced.
According to the present invention, the temperature of the second reaction is preferably 20 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol, preferably 10 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol. With this preferred embodiment, the second reaction temperature is lower than the above range, the reaction initiation is difficult and the reaction rate is slow, and the second reaction temperature is higher than the above range, the fatty alcohol is liable to be volatilized and lost to result in incomplete reaction.
The initiation time definition of the second reaction is the same as that of the first reaction.
The preparation method provided by the invention can obviously shorten the initiation time of the second reaction. Preferably, the initiation time of the second reaction is from 0.25 to 5 hours, preferably from 0.25 to 0.5 hours.
The reaction time definition of the second reaction is the same as that of the first reaction.
The preparation method provided by the invention can obviously shorten the reaction time of the second reaction. Preferably, the reaction time of the second reaction is 0.4 to 4 hours, preferably 0.6 to 3 hours.
According to the invention, preferably, the molar ratio of the elemental magnesium to the second fatty alcohol is from 1:2 to 7, preferably from 1:2 to 4. By adopting the preferred embodiment, the reaction can be completed rapidly and fully, and meanwhile, excessive fatty alcohol waste can be avoided, so that the cost can be saved.
Preferably, the molar ratio of the magnesium simple substance to the aluminum simple substance is 1:0.3-3, preferably 1:0.5-2. By adopting the preferred embodiment, the aluminum magnesium alkoxide can be fully dispersed and generated, and the smooth reaction is ensured.
Preferably, the mass ratio of the catalyst to the total reactant in the step (2) is 1:100-300, preferably 1:100-200, wherein the total reactant is the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1). By adopting the preferred mode, the catalyst consumption is greatly reduced while the reaction rate is improved, and the cost can be reduced.
The invention has a wide selection range of the types of the catalysts, and can be a routine choice in the field. Preferably, the catalyst is at least one selected from elemental iodine, mercury dichloride and aluminum trichloride, and is preferably elemental iodine in order to further increase the reaction rate without introducing other impurities.
According to the present invention, preferably, the purity of the elemental magnesium is not less than 99.9 mass%. With this preferred embodiment, it is advantageous to obtain a magnesium aluminum composite oxide with high purity.
The present invention is not particularly limited in the form of existence of the magnesium element, and may be selected conventionally in the art. Preferably, the magnesium simple substance is at least one selected from magnesium blocks, magnesium sheets, magnesium wires, magnesium scraps, magnesium grains, magnesium strips and magnesium powder.
The magnesium blocks, magnesium flakes, magnesium filaments, magnesium chips, magnesium particles, magnesium strips and magnesium powder according to the present invention are well known to those skilled in the art, and the present invention is not described in detail herein.
According to the present invention, preferably, the first reaction and/or the second reaction is/are carried out under condensed reflux conditions.
Preferably, the reaction mass is purged with an inert gas to displace air therein prior to being fed into the reactors of the first and second reactions. With the adoption of the preferred embodiment, the surface oxidation of the elemental aluminum and the elemental magnesium can be prevented while the interior of the reactor is dried.
The invention has wider selection range of the inert gas types, and can be used without influencing the reaction. The inert gas of the present invention is preferably nitrogen.
In the hydrolysis process, any additive such as hydroxide anions, organic anions (especially alkoxide ions, alkoxide ether sulfate, aryloxide ether sulfate, glycol ether sulfate) and inorganic anions (carbonate, bicarbonate, chloride, nitrate, sulfate and polyoxometalate anions) are not added, so that the purpose of full hydrolysis can be achieved, new impurities are not introduced, and subsequent impurity removal treatment is not needed. In the hydrolysis process in the step (3), the hydrolysis temperature and the water adding amount are controlled within the following ranges, so that the full hydrolysis of the alkoxy magnesium aluminum is facilitated, the water consumption is reduced, and the cost is saved.
According to the invention, the hydrolysis in step (3) is preferably carried out at a temperature of 60-100 ℃, preferably 85-95 ℃.
The time of the hydrolysis is not particularly limited, provided that the slurry after the hydrolysis has good fluidity and does not adhere to the wall.
According to the invention, the reaction product of step (2) is preferably used in a mass ratio to water of from 1:1 to 5, preferably from 1:1.1 to 3.5.
According to the present invention, preferably, the method further comprises separating the material obtained by the hydrolysis in the step (3), and then optionally drying and calcining to obtain the magnesium-aluminum composite oxide.
The separation method is not particularly limited, and may be performed by a method conventionally used in the art.
In the present invention, the term "optionally" means with or without, with or without addition, with or without, unless otherwise specified. Specifically, the step (3) of the present invention may be performed with or without drying.
The specific conditions for the drying are not particularly limited in the present invention, and can be carried out by referring to a conventional method in the art.
According to the present invention, preferably, the conditions of the calcination in the step (3) include a temperature of 550 to 850 ℃ for 4 to 8 hours. The calcination is typically carried out in an air atmosphere, which may include a flowing atmosphere or a stationary atmosphere.
According to a particularly preferred embodiment of the present invention, a method for producing a magnesium aluminum composite oxide, the method comprising the steps of:
(1) Under the anhydrous condition, carrying out a first reaction on an aluminum simple substance and first fatty alcohol to obtain a material containing aluminum alkoxide;
(2) Under the action of a catalyst, carrying out a second reaction on the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1) under the anhydrous condition;
(3) Hydrolyzing the reaction product in the step (2) to obtain magnesium-aluminum bimetallic alkoxide, and then optionally drying and roasting to obtain magnesium-aluminum composite oxide;
The first fatty alcohol comprises n-amyl alcohol and n-hexyl alcohol, the molar use ratio of the n-amyl alcohol to the n-hexyl alcohol is 1:0.1-1, and the second fatty alcohol is n-amyl alcohol;
the temperature of the second reaction is 20 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol, preferably 10 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol;
the initiation time of the second reaction is 0.25-0.5h;
The reaction time of the second reaction is 0.6-3h;
the molar ratio of the magnesium simple substance to the second fatty alcohol is 1:2-4;
the molar ratio of the magnesium simple substance to the aluminum simple substance is 1:0.5-2.
The specific preparation method can obtain the high-purity magnesium-aluminum composite oxide without subsequent purification treatment, and the purity is higher than 99.99 percent, and meanwhile, the preparation method provided by the invention has the advantages of mild reaction condition, short initiation time, high reaction rate and no introduction of other impurities except impurities carried by metal magnesium aluminum. Preferably, the preparation method provided by the invention has the advantages that the catalyst consumption is small, and the preparation cost can be reduced.
In a second aspect, the present invention provides a magnesium-aluminum composite oxide obtained by the preparation method of the first aspect.
The high-purity magnesium-aluminum composite oxide prepared by the method has wide application, and can be applied to catalyst preparation. According to the present invention, preferably, the purity of the magnesium aluminum composite oxide is greater than 99.99%.
The present invention will be described in detail by examples.
In the following examples, the magnesium-aluminum ratio of the magnesium-aluminum composite oxide, the product purity, was measured by Inductively Coupled Plasma (ICP);
In the following examples, all reagents used were commercially available and were analytically pure.
Example 1
(1) The three-neck flask is cleaned in advance, put into an oven for drying, the three-neck flask is guaranteed to be clean and anhydrous, nitrogen is used for sweeping the three-neck flask before the test, 6.76g of aluminum wires with the purity of 99.996 mass percent are added into the three-neck flask with a heating and condensing system, 86.85g of n-amyl alcohol is taken, and the aluminum wires are immersed into the three-neck flask. Gradually heating to 135 ℃ (the boiling point of n-amyl alcohol is 137.8 ℃), and keeping condensing reflux until no obvious bubbles are generated in the solution, and cooling to 100 ℃ after no aluminum wires are generated in the solution. The initiation time and reaction time of the reaction are shown in Table 1.
(2) Adding 3.01g of magnesium scraps with the purity of 99.9 mass percent into 92.86g of n-amyl alcohol solution of n-amyl aluminum obtained by the reaction, adding 0.67g of iodine simple substance with the purity of 99.8 mass percent into a three-neck flask, gradually heating to 135 ℃ and keeping condensing reflux until no obvious bubbles are generated in the solution and no magnesium scraps remain in the solution, and finishing the reaction. The initiation time and reaction time of the reaction are shown in Table 1.
(3) 131.04G of the n-amyl alcohol solution of the n-pentyloxymethylaluminum obtained in the step (2) is transferred to a 1000mL beaker at 90 ℃, and 90 ℃ deionized water is added for hydrolysis until the solution is layered and the fluidity of the lower slurry is good, the slurry is not adhered, and 350g of deionized water is used. And (3) obtaining a magnesium hydroxide aluminum slurry phase and an n-amyl alcohol phase, separating the n-amyl alcohol phase at the upper layer, placing the magnesium hydroxide aluminum slurry in a blast constant temperature drying oven, drying at 120 ℃ for 12 hours, and then placing in a muffle furnace for roasting at 600 ℃ for 6 hours to obtain the magnesium aluminum composite oxide. The magnesium-aluminum ratio and the product purity are shown in Table 2 by Inductively Coupled Plasma (ICP) analysis.
Example 2
(1) The three-necked flask was cleaned in advance, put in an oven for drying, the three-necked flask was kept clean and anhydrous, the three-necked flask was purged with nitrogen before the test, 2.69g of the aluminum wire used in example 1 was added to the three-necked flask with a heating and condensing system, and 28.30g of n-pentanol and 10.22g of n-hexanol were taken and added to the three-necked flask to submerge the aluminum wire. Gradually heating to 135 ℃, keeping condensing reflux until no obvious bubbles are generated in the solution, and cooling to 100 ℃ after no aluminum wires are generated in the solution. The initiation time and reaction time of the reaction are shown in Table 1.
(2) 2.40G of magnesium chips adopted in the example 1 are added into 39.06g of the solution obtained by the reaction, 0.50g of iodine simple substance with the purity of 99.8 mass percent is added into 27.24g of n-amyl alcohol to a three-neck flask, the temperature is gradually increased to 130 ℃, and the condensation reflux is maintained until no obvious bubbles are generated in the solution and no magnesium chips remain in the solution, and the reaction is finished. The initiation time and reaction time of the reaction are shown in Table 1.
(3) 68.5G of the n-amyl alcohol solution of the alkoxy magnesium aluminum obtained in the step (2) is transferred to a 1000mL beaker at 90 ℃, and 90 ℃ deionized water is added for hydrolysis until the solution is layered and the fluidity of the lower slurry is good, the slurry is not adhered to the wall, and 210g of deionized water is used. The magnesium aluminum slurry phase and the n-amyl alcohol phase are obtained, the upper n-amyl alcohol phase is separated, the magnesium aluminum slurry is placed in a blast constant temperature drying oven, dried for 12 hours at 120 ℃, then placed in a muffle furnace for roasting for 6 hours at 600 ℃ to obtain a magnesium aluminum composite oxide, and the magnesium aluminum proportion and the product purity are obtained through Inductively Coupled Plasma (ICP) analysis, wherein the magnesium aluminum proportion and the product purity are shown in Table 2.
Example 3
The procedure of example 1 was followed, except that the n-pentanol in step (1) was replaced with 44.08g of n-pentanol and 49.56g of n-hexanol, to obtain a magnesium-aluminum composite oxide. The magnesium-aluminum ratio and the product purity are shown in Table 2 by Inductively Coupled Plasma (ICP) analysis.
Example 4
The procedure of example 1 was followed, except that the temperature of the first and second reactions was 137 ℃. After the first reaction is finished, aluminum scraps still do not react, the n-amyl alcohol solution needs to be supplemented until the reaction is complete, magnesium scraps still do not react, the n-amyl alcohol solution needs to be supplemented until the reaction is complete, the operation is complex, the cost is increased, and the industrial application is not facilitated.
The magnesium-aluminum composite oxide is obtained, and the magnesium-aluminum ratio and the product purity are obtained through Inductively Coupled Plasma (ICP) analysis and are shown in Table 2.
Comparative example 1
High purity aluminum magnesium alkoxide was prepared as in example 1, except that 6.78g of the aluminum flake used in example 1, 3.01g of the magnesium flake used in example 1, and 0.60g of the elemental iodine used in example 1 were simultaneously added to a three-necked flask, and reacted with 106.27g of n-pentanol at 135℃for 36 hours, and a large amount of aluminum flake and magnesium flake (about 9.02 g) remained, and the reaction was not completed.
The magnesium-aluminum composite oxide is obtained, and the magnesium-aluminum ratio and the product purity are obtained through Inductively Coupled Plasma (ICP) analysis and are shown in Table 2.
Comparative example 2
In a three-necked flask with heating and condensing system, 3.42g of the magnesium turnings used in example 1 were initially introduced, and then 33.50g of n-amyl alcohol were added to immerse the magnesium turnings. Gradually heating to 135 ℃ and keeping condensing reflux, wherein the generated alkoxy magnesium adheres to the bottom of the three-neck flask, so that the reaction cannot be continued, and the magnesium-aluminum composite oxide cannot be obtained.
Comparative example 3
The procedure of example 1 was followed, except that n-pentanol in the reactions of step (1) and step (2) was replaced with an equimolar amount of n-butanol, the reaction temperature was 115℃and the boiling point of n-butanol was 117.25 ℃to obtain a magnesium-aluminum composite oxide, and the magnesium-aluminum ratio and the product purity thereof were obtained by Inductively Coupled Plasma (ICP) analysis and are shown in Table 2.
Comparative example 4
The procedure of example 2 was followed, except that the n-pentanol and n-hexanol in the reaction of step (1) were replaced with 43.02g of n-hexanol, and the reaction temperature was 150℃to obtain a magnesium-aluminum composite oxide, and the magnesium-aluminum ratio and the product purity thereof were obtained by Inductively Coupled Plasma (ICP) analysis and are shown in Table 2.
Comparative example 5
(1) The three-necked flask was put in an oven to be dried in advance to ensure that the three-necked flask was clean and anhydrous, the three-necked flask was purged with nitrogen before the test, 6.77g of the aluminum wire used in example 1 was added to the three-necked flask with a heating and condensing system, and 106.33g of n-hexanol was added to the three-necked flask to immerse metallic aluminum. Gradually heating to 150 ℃ (the boiling point of the n-hexanol is 157 ℃), enabling the n-hexanol to react with the high-purity aluminum wires, keeping condensing reflux until no obvious bubbles are generated in the solution, and cooling to 100 ℃ after no high-purity aluminum wires are generated in the solution. The initiation time and reaction time of the reaction are shown in Table 1.
(2) Adding 6.01g of magnesium chips adopted in the example 1 into 112.35g of n-hexanol solution of n-hexylaluminum obtained by the reaction in the step (1), adding 1.22g of iodine simple substance with the purity of 99.8 mass percent into a three-neck flask, gradually heating to 150 ℃ to enable the n-hexanol to react with the high-purity magnesium chips, keeping condensing reflux until no obvious bubbles are generated in the solution and no magnesium chips remain in the solution, and finishing the reaction. The initiation time and reaction time of the reaction are shown in Table 1.
(3) 218.86G of n-hexanol solution of n-hexyloxymagnesium aluminum was transferred to a 1000mL beaker at 90℃and added with deionized water at 90℃for hydrolysis until the solution was layered and the fluidity of the lower slurry was good, 315g of deionized water was used. And (3) generating a magnesium hydroxide aluminum slurry phase and a normal hexanol phase, separating the upper normal hexanol phase, placing the magnesium hydroxide aluminum slurry in a blast constant temperature drying oven, and drying at 120 ℃ for 12 hours to obtain the high-purity magnesium hydroxide aluminum compound. The magnesium-aluminum composite is placed in a muffle furnace for roasting at 600 ℃ for 6 hours to obtain a high-purity magnesium-aluminum composite oxide, and the magnesium-aluminum ratio and the product purity of the magnesium-aluminum composite oxide are obtained through Inductively Coupled Plasma (ICP) analysis and are shown in Table 2.
TABLE 1
TABLE 2
As can be seen from the results in Table 2, the specific preparation method provided by the invention can be used for obtaining the high-purity magnesium-aluminum composite oxide with the purity of more than 99.99% without subsequent purification treatment. Meanwhile, the ratio of magnesium to aluminum in the magnesium-aluminum composite oxide can be flexibly adjusted so as to meet the actual needs.
As can be seen from the results in Table 1, the preparation method provided by the invention has the advantages of short initiation time and high reaction rate.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A method for preparing a magnesium aluminum composite oxide, the method comprising the steps of:
(1) Under the anhydrous condition, carrying out a first reaction on an aluminum simple substance and first fatty alcohol to obtain a material containing aluminum alkoxide;
(2) Under the action of a catalyst, carrying out a second reaction on the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1) under the anhydrous condition;
(3) Hydrolyzing the reaction product in the step (2) to obtain magnesium-aluminum bimetallic alkoxide, and then optionally drying and roasting to obtain magnesium-aluminum composite oxide;
Wherein the first fatty alcohol and the second fatty alcohol each independently comprise n-amyl alcohol and optionally n-hexyl alcohol, and the molar dosage ratio of the n-amyl alcohol to the n-hexyl alcohol is 1:0-10.
2. The method of claim 1, wherein,
The first fatty alcohol comprises n-amyl alcohol and n-hexanol, and the molar dosage ratio of the n-amyl alcohol to the n-hexanol is 1:0.1-1;
the second fatty alcohol is n-amyl alcohol.
3. The method of claim 1, wherein,
The temperature of the first reaction is 20 ℃ below the boiling point of the first fatty alcohol to the boiling point of the first fatty alcohol, preferably 20 ℃ below the boiling point of the first fatty alcohol to 2 ℃ below the boiling point of the first fatty alcohol;
preferably, the initiation time of the first reaction is from 0.2 to 4.5 hours, preferably from 0.2 to 0.5 hours;
Preferably, the reaction time of the first reaction is 0.4 to 4 hours, preferably 0.5 to 2 hours;
Preferably, the molar ratio of the aluminum simple substance to the first fatty alcohol is 1:3-5, preferably 1:3.1-4.5;
preferably, the purity of the elemental aluminum is not less than 99.9 mass%.
4. A method according to any one of claim 1 to 3, wherein,
The temperature of the second reaction is 20 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol, preferably 10 ℃ below the boiling point of the second fatty alcohol to 2 ℃ below the boiling point of the second fatty alcohol;
preferably, the initiation time of the second reaction is from 0.25 to 5 hours, preferably from 0.25 to 0.5 hours;
preferably, the reaction time of the second reaction is 0.4 to 4 hours, preferably 0.6 to 3 hours.
5. The method according to any one of claims 1 to 4, wherein,
The molar ratio of the magnesium simple substance to the second fatty alcohol is 1:2-7, preferably 1:2-4;
Preferably, the molar ratio of the magnesium simple substance to the aluminum simple substance is 1:0.3-3, preferably 1:0.5-2;
preferably, the mass ratio of the catalyst to the total reactant in the step (2) is 1:100-300, preferably 1:100-200, wherein the total reactant is the material containing aluminum alkoxide, magnesium simple substance and second fatty alcohol obtained in the step (1).
6. The method according to any one of claims 1 to 5, wherein,
The catalyst is at least one of iodine simple substance, mercury dichloride and aluminum trichloride, and is preferably iodine simple substance;
preferably, the purity of the elemental magnesium is not less than 99.9 mass%.
7. The method according to any one of claims 1-6, wherein,
The first reaction and/or the second reaction is/are carried out under condensing reflux conditions.
8. The method according to any one of claims 1-7, wherein,
The temperature of the hydrolysis in step (3) is 60-100 ℃, preferably 85-95 ℃;
preferably, the mass ratio of the reaction product of step (2) to water is 1:1-5, preferably 1:1.1-3.5.
9. The method according to any one of claims 1-8, wherein,
The roasting condition in the step (3) comprises the temperature of 550-850 ℃ and the time of 4-8h.
10. A magnesium aluminum composite oxide produced by the production method according to any one of claims 1 to 9;
Preferably, the purity of the magnesium aluminum composite oxide is greater than 99.99%.
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