CN112408441A - Method and system for preparing mesoporous alumina - Google Patents
Method and system for preparing mesoporous alumina Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 17
- 239000000956 alloy Substances 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 13
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005266 casting Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 15
- 239000007921 spray Substances 0.000 claims description 14
- 229910000645 Hg alloy Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 8
- 229910052753 mercury Inorganic materials 0.000 claims description 8
- 239000002808 molecular sieve Substances 0.000 claims description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- LBFKBYSVICSFQW-UHFFFAOYSA-N [In][Sn][Pb][Bi] Chemical compound [In][Sn][Pb][Bi] LBFKBYSVICSFQW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- 229910001174 tin-lead alloy Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- DAEJUPKPHRBQHZ-UHFFFAOYSA-N [Sn].[Hg] Chemical compound [Sn].[Hg] DAEJUPKPHRBQHZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 229910000799 K alloy Inorganic materials 0.000 claims description 3
- 229910000733 Li alloy Inorganic materials 0.000 claims description 3
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 3
- NDXSUDIGSOJBLQ-UHFFFAOYSA-N [In][Bi][Zn][Sn] Chemical compound [In][Bi][Zn][Sn] NDXSUDIGSOJBLQ-UHFFFAOYSA-N 0.000 claims description 3
- YPQJHZKJHIBJAP-UHFFFAOYSA-N [K].[Bi] Chemical compound [K].[Bi] YPQJHZKJHIBJAP-UHFFFAOYSA-N 0.000 claims description 3
- JYPVGDJNZGAXBB-UHFFFAOYSA-N bismuth lithium Chemical compound [Li].[Bi] JYPVGDJNZGAXBB-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000001989 lithium alloy Substances 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000002893 slag Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- FXZZORURDDBOIW-UHFFFAOYSA-N [Hg].[In].[Bi] Chemical compound [Hg].[In].[Bi] FXZZORURDDBOIW-UHFFFAOYSA-N 0.000 claims description 2
- ZMTYNJDMTGBHAH-UHFFFAOYSA-N [Hg].[Sn].[Bi] Chemical compound [Hg].[Sn].[Bi] ZMTYNJDMTGBHAH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- YVUZUKYBUMROPQ-UHFFFAOYSA-N mercury zinc Chemical compound [Zn].[Hg] YVUZUKYBUMROPQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000009616 inductively coupled plasma Methods 0.000 description 8
- 239000011148 porous material Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 238000004611 spectroscopical analysis Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000802 evaporation-induced self-assembly Methods 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Images
Classifications
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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
- C01F7/42—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation
- C01F7/428—Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation by oxidation in an aqueous solution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/08—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents with metals
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/12—Surface area
-
- 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
- C01P2006/16—Pore diameter
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a method and a system for preparing mesoporous alumina, wherein the method comprises the following steps: 1) melting an aluminum ingot, adding a catalyst, and casting molten alloy liquid into an aluminum alloy block; 2) reacting the obtained aluminum alloy block with water, hydrolyzing the aluminum alloy to generate hydrated alumina and hydrogen, and deslagging and separating slurry obtained by the reaction; 3) filtering and concentrating the slurry after deslagging, and drying the concentrated slurry to obtain pseudo-boehmite dry powder; 4) calcining the pseudo-boehmite dry powder at the temperature of 300-600 ℃. The invention provides a method for preparing mesoporous alumina by aluminum alloy hydrolysis, which can be produced in a pilot plant test or industrial scale and has industrial practicability.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a preparation method and a preparation system of a mesoporous material.
Background
According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), a pore with a pore diameter of 2 to 50nm is called mesoporous (or called mesopore). The mesoporous material has huge specific surface area and three-dimensional pore structure, and is applied to the fields of electrode materials and catalytic reaction. Among them, mesoporous alumina can provide high catalytic activity, strong mechanical properties and hydrothermal stability, and has attracted much attention in the fields of novel catalysts, adsorbents, catalyst carriers, and the like.
The existing methods for preparing mesoporous alumina include sol-gel method, hydrothermal synthesis method, evaporation-induced self-assembly method (research progress of ordered mesoporous alumina preparation, liuhongxia et al, aging and application of synthetic materials, 2014), precipitation method (strong in brown, Beijing university of chemical industry 2010), etc. Wherein the evaporation-induced self-assembly method is a further improvement of the sol-gel method. The aperture of the ordered mesoporous alumina in the precipitation method can be adjusted by changing the polymerization degree of the template. The reaction raw materials of the sol-gel method and the hydrothermal synthesis method comprise a template agent, so the cost is high; in addition, in the face of the production requirement of the mesoporous alumina in industrial scale, the sol-gel method, the hydrothermal synthesis method, the precipitation method and the like have the characteristics of complex procedures and low controllability.
Under appropriate conditions, the aluminum alloy can be subjected to hydrolysis reaction with water to generate hydrated alumina and hydrogen. The hydrated alumina-pseudo-boehmite with the mesoporous structure can be obtained by controlling the reaction temperature and the reaction time, and the gamma-alumina powder with the mesoporous structure can be obtained by high-temperature calcination, has higher purity, less impurity types and low impurity content, and is suitable for large-scale industrial production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing mesoporous alumina, which can realize the production of the mesoporous alumina on a pilot scale and an industrial scale.
It is yet another object of the present invention to provide a system for preparing mesoporous alumina.
The technical scheme for realizing the above purpose of the invention is as follows:
a method of preparing mesoporous alumina comprising the steps of:
1) melting an aluminum ingot and a catalyst together, and casting molten alloy liquid into an aluminum alloy block; the catalyst is an alloy consisting of, or a compound containing, one or more of the following low melting point metals: tin, bismuth, mercury, indium, lead, bismuth, zinc, potassium, lithium and antimony, wherein the mass of the catalyst is 0.05-1.5% of that of the aluminum alloy (the total mass of the aluminum ingot and the catalyst);
2) reacting the obtained aluminum alloy block with water, hydrolyzing the aluminum alloy to generate hydrated alumina and hydrogen, and deslagging and separating slurry obtained by the reaction;
3) filtering and concentrating the slurry after deslagging, and drying the concentrated slurry to obtain pseudo-boehmite dry powder;
4) calcining the pseudo-boehmite dry powder at the temperature of 300-600 ℃.
The catalyst is one of pure mercury, pure bismuth, pure indium, indium-tin alloy, bismuth indium-tin-zinc alloy, bismuth indium-tin-lead alloy, bismuth potassium alloy, bismuth lithium alloy, zinc-mercury alloy, tin-mercury alloy, bismuth indium-mercury or bismuth tin-mercury alloy.
Wherein the indium tin alloy may be InSn49.2The bismuth indium tin zinc alloy can be Bi35In48.6Sn16Zn0.4The bismuth indium tin lead alloy can be BiIn21Sn12Pb18The bismuth-potassium alloy may be BiK2.5The bismuth-lithium alloy may be BiLi14The mercury alloy comprises 5-45% of mercury, the tin-mercury alloy can be composed of 34-69% of mercury, 0.5-5% of antimony and the balance of mercury.
According to a preferable technical scheme, in the step 1), aluminum ingots are placed into a medium-frequency smelting furnace to be melted, and the temperature is controlled to be 680-750 ℃.
In the step 1), after all the metal aluminum is melted, 0.3-1.2% of the catalyst is added, the mixture is stirred for 10-30 min, and an aluminum alloy block is cast after filter residues are filtered.
Further, nitrogen protection is adopted in the process of the step 1).
Wherein in the step 2), aluminum alloy and deionized water are added into a reaction kettle according to the proportion (wt) of 1: 20-1: 50,
more preferably, in the step 2), the temperature of the reaction kettle is controlled to be 50-150 ℃, the pressure is controlled to be 0-0.5 Mpa, and the aluminum alloy is gradually hydrolyzed to generate hydrated alumina and hydrogen. A preferable scheme of the method is that the temperature of the reaction kettle is controlled to be 100-120 ℃, and the pressure is controlled to be 0.1-0.2 Mpa.
Wherein, in the step 3), the concentrated slurry is subjected to spray drying; preferably, the inlet temperature of the spraying equipment is 200-250 ℃, and the outlet temperature is 100-130 ℃. In the step 4), the pseudo-boehmite dry powder is calcined for 2-4 hours at the temperature of 300-600 ℃.
The invention also provides a system for preparing the mesoporous alumina, which comprises a medium-frequency smelting furnace, an alloy forming die, a reaction kettle, a cyclone separator, a filter, a buffer tank, a spray tower and a rotary kiln,
a molten liquid outlet of the intermediate frequency smelting furnace is connected with the alloy forming die;
the reaction kettle is connected with the cyclone separator through a pipeline, the filter is connected with an upper outlet of the cyclone separator, and a lower outlet of the cyclone separator is used for discharging slag; the filter outlet is connected with the buffer tank, the buffer tank is connected with the material inlet of the spray tower, and the material outlet of the spray tower is connected with the rotary kiln.
Wherein the intermediate frequency smelting furnace and the alloy forming die are filled with protective gas; the protective gas is one or more of nitrogen, helium or argon; and/or
The reaction kettle is provided with a hydrogen outlet, the hydrogen outlet is connected with a gas condenser, the outlet of the gas condenser is connected with a molecular sieve dryer, and the molecular sieve dryer is connected with a hydrogen storage tank.
Wherein, the mesh size of the filter screen in the filter can be about 0.05-0.2 mm.
The invention has the beneficial effects that:
the invention provides a method for preparing mesoporous alumina by aluminum alloy hydrolysis, which can be produced in a pilot plant test or industrial scale and has industrial practicability; meanwhile, the mesoporous alumina has the advantages of few impurity types, low impurity content and high purity.
The method does not use organic compounds as reaction raw materials, adopts catalysts with small addition proportion, can recycle the catalysts, and reduces the production cost; meanwhile, deionized water for production can be recycled, no sewage is discharged, and the method is environment-friendly and reliable.
Drawings
FIG. 1 is a flow chart of the present invention for preparing mesoporous alumina.
FIG. 2 is a schematic diagram of the connection of a reaction kettle, a cyclone separator, a filter, a buffer tank and a spray tower in a system for preparing mesoporous alumina.
In the figure, 1 is a reaction kettle, 2 is a cyclone separator, 3 is a filter, 4 is a buffer tank, 5 is a spray tower, 6 is a molecular sieve dryer, 7 is a hydrogen storage tank, 8 is a rotary kiln, and 9 is a gas condenser.
Detailed Description
Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical means used in the invention are all the technical means existing in the field except for special description.
EXAMPLE 1 System for preparing mesoporous alumina
A system for preparing mesoporous alumina comprises a medium-frequency smelting furnace, an alloy forming die, a reaction kettle, a cyclone separator, a filter, a buffer tank, a spray tower and a rotary kiln,
a molten liquid outlet of the intermediate frequency smelting furnace is connected with the alloy forming die;
referring to fig. 2, a reaction kettle 1 is connected with a cyclone separator 2 through a pipeline, a filter 3 is connected with an upper outlet of the cyclone separator 2, and a lower outlet of the cyclone separator 2 is used for discharging slag; the outlet of the filter 3 is connected with the buffer tank 4, the buffer tank 4 is connected with the material inlet of the spray tower 5, and the material outlet of the spray tower 5 is connected with the rotary kiln 8.
In the system, nitrogen is introduced into the intermediate frequency smelting furnace and the alloy forming die. The reaction kettle 1 is provided with a hydrogen outlet, the hydrogen outlet is connected with a gas condenser 9, the outlet of the gas condenser 9 is connected with a molecular sieve dryer 6, and the molecular sieve dryer 6 is connected with a hydrogen storage tank 7.
In the system, the mesh size of a filter screen in the filter is 100 meshes. A material dispersing device is arranged in the spraying tower, the inlet temperature of the spraying tower is 200-250 ℃, and the outlet temperature of the spraying tower is 100-130 ℃.
Example 2 method for preparing mesoporous alumina
This example provides a method for preparing mesoporous alumina, the flow chart referring to fig. 1, using the system of example 1, comprising the following steps:
1) putting an aluminum ingot into a medium-frequency smelting furnace to melt the aluminum ingot, and controlling the temperature to be 680-750 ℃; after the metal aluminum is completely melted,
casting the molten alloy liquid into an aluminum alloy block; the catalyst is a tin-mercury alloy (the weight percentage of each component is 45% of mercury, 50% of tin and 5% of antimony), and the mass of the catalyst accounts for 0.5% of that of the aluminum alloy; adding catalyst, stirring for 30min, filtering, and casting to obtain aluminum alloy block.
2) Reacting the obtained aluminum alloy block with water, adding aluminum alloy and deionized water into a reaction kettle 1 according to the proportion of 1:30(wt), controlling the temperature of the reaction kettle to be 60-70 ℃ and the pressure to be 0 (gauge pressure), hydrolyzing the aluminum alloy to generate hydrated alumina and hydrogen, and deslagging and separating slurry obtained by the reaction by using a cyclone separator 2;
the hydrogen is discharged from the top of the reaction kettle, condensed, dried in a molecular sieve dryer 6 and finally stored in a hydrogen storage tank 7.
3) Filtering and concentrating the slurry after deslagging, and drying the concentrated slurry in a spray tower 5 to obtain pseudo-boehmite dry powder; the inlet temperature of the spray tower was 230 ℃ and the outlet temperature was 110 ℃.
4) The pseudo-boehmite dry powder is transferred into a rotary kiln and calcined for 3h at the temperature of 500 ℃. The median particle diameter D of the product obtained5015.47 μm, pore diameter of 5.73nm, and specific surface area of 238m2/g。5.114Kg of mesoporous alumina can be obtained with a yield of 90.67% (relative to the theoretical value) by 3Kg of blocks of aluminium alloy. The purity of the mesoporous alumina is measured to be more than 99.8 percent by ICP (inductively coupled plasma spectrometry).
Example 3 method for preparing mesoporous alumina
This example provides a method for preparing mesoporous alumina using the system of example 1, comprising the steps of:
1) putting an aluminum ingot into a medium-frequency smelting furnace to melt the aluminum ingot, and controlling the temperature to be 680-750 ℃; after the metal aluminum is completely melted,
casting the molten alloy liquid into an aluminum alloy block; the catalyst is bismuth indium tin lead alloy (BiIn)21Sn12Pb18) The mass of the catalyst accounts for 0.5 percent of that of the aluminum alloy; adding catalyst, stirring for 30min, filtering, and casting to obtain aluminum alloy block.
2) Reacting the obtained aluminum alloy block with water, adding aluminum alloy and deionized water into a reaction kettle 1 according to the proportion of 1:40(wt), controlling the temperature of the reaction kettle at 110 ℃ and the pressure at 0.15Mpa (gauge pressure), hydrolyzing the aluminum alloy to generate hydrated alumina and hydrogen, and deslagging and separating slurry obtained by the reaction by using a cyclone separator 2; the hydrogen was collected as in example 2;
3) filtering and concentrating the slurry after deslagging, and drying the concentrated slurry in a spray tower 5 to obtain pseudo-boehmite dry powder;
4) the pseudo-boehmite dry powder is calcined for 3 hours at the temperature of 500 ℃.
The median particle diameter D of the product obtained5017.18 μm, pore diameter of 6.09nm, and specific surface area of 259m2(ii) in terms of/g. The yield was 92.5%. The purity of the mesoporous alumina is measured to be more than 99.8 percent by ICP (inductively coupled plasma spectrometry).
Example 4 method for preparing mesoporous alumina
This example provides a method for preparing mesoporous alumina using the system of example 1, comprising the steps of:
1) putting an aluminum ingot into a medium-frequency smelting furnace to melt the aluminum ingot, and controlling the temperature to be 680-750 ℃; after the metal aluminum is completely melted,
melt and mixCasting molten gold into an aluminum alloy block; the catalyst is bismuth indium tin lead alloy (BiIn)21Sn12Pb18) The mass of the catalyst is 0.7 percent of that of the aluminum ingot; adding catalyst, stirring for 30min, filtering, and casting to obtain aluminum alloy block.
Steps 2) to 4) were the same as in example 3.
The median particle diameter D of the product obtained5019.68 μm, pore diameter of 7.43nm, and specific surface area of 222.8m2In terms of/g, the yield is 93.7%. The purity of the mesoporous alumina is measured to be more than 99.8 percent by ICP (inductively coupled plasma spectrometry).
Example 5 method for preparing mesoporous alumina
This example provides a method for preparing mesoporous alumina using the system of example 1, comprising the steps of:
1) putting an aluminum ingot into a medium-frequency smelting furnace to melt the aluminum ingot, and controlling the temperature to be 680-750 ℃; after the metal aluminum is completely melted,
casting the molten alloy liquid into an aluminum alloy block; the catalyst is bismuth indium tin lead alloy (BiIn)21Sn12Pb18) The mass of the catalyst is 1 percent of that of the aluminum ingot; adding catalyst, stirring for 30min, filtering, and casting to obtain aluminum alloy block.
Steps 2) to 4) were the same as in example 3.
The median particle diameter D of the product obtained5017.53 μm, pore diameter of 6.28nm, and specific surface area of 232.7m2In terms of a/g yield, 91.6%. The purity of the mesoporous alumina is measured to be more than 99.8 percent by ICP (inductively coupled plasma spectrometry).
Although the present invention has been described with reference to the above embodiments, those skilled in the art will appreciate that various modifications, substitutions and alterations can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method of preparing mesoporous alumina, comprising the steps of:
1) melting an aluminum ingot, adding a catalyst, and casting molten alloy liquid into an aluminum alloy block; the catalyst is an alloy consisting of one or more of the following low melting point metals, or a compound containing one or more of the following low melting point metals: the catalyst comprises tin, bismuth, mercury, indium, lead, bismuth, zinc, potassium, lithium and antimony, wherein the mass of the catalyst accounts for 0.05-1.5% of the total mass of the raw materials;
2) reacting the obtained aluminum alloy block with water, hydrolyzing the aluminum alloy to generate hydrated alumina and hydrogen, and deslagging and separating slurry obtained by the reaction;
3) filtering and concentrating the slurry after deslagging, and drying the concentrated slurry to obtain pseudo-boehmite dry powder;
4) calcining the pseudo-boehmite dry powder at the temperature of 300-600 ℃.
2. The method of claim 1, wherein the catalyst is one of pure mercury, pure bismuth, pure indium, indium-tin alloy, bismuth indium-tin-zinc alloy, bismuth indium-tin-lead alloy, bismuth potassium alloy, bismuth lithium alloy, zinc-mercury alloy, tin-mercury alloy, bismuth indium-mercury, or bismuth tin-mercury alloy.
3. The method for preparing mesoporous alumina according to claim 1, wherein in the step 1), the aluminum ingot is put into a medium-frequency smelting furnace to be melted, and the temperature is controlled to be 680-750 ℃.
4. The method for preparing mesoporous alumina according to claim 1, wherein in the step 1), after all the metal aluminum is melted, 0.3-1.2% of the catalyst is added, the mixture is stirred for 10-30 min, and the aluminum alloy block is cast after filter residue is filtered.
5. The method for preparing mesoporous alumina according to claim 1, wherein in the step 2), the aluminum alloy and the deionized water are added into the reaction kettle according to a weight ratio of 1: 20-1: 50.
6. The method for preparing mesoporous alumina according to any one of claims 1 to 5, wherein in the step 2), the temperature of the reaction kettle is controlled to be 50-150 ℃, the pressure is controlled to be 0-0.5 Mpa, and the aluminum alloy is gradually hydrolyzed to generate hydrated alumina and hydrogen.
7. The method for preparing mesoporous alumina according to any one of claims 1 to 5, wherein in step 3), the concentrated slurry is spray-dried; preferably, the inlet temperature of the spraying equipment is 200-250 ℃, and the outlet temperature is 100-130 ℃.
8. The method for preparing mesoporous alumina according to claim 1, wherein in the step 4), the pseudoboehmite dry powder is calcined at the temperature of 300-600 ℃ for 2-4 h.
9. A system for preparing mesoporous alumina is characterized by comprising a medium-frequency smelting furnace, an alloy forming die, a reaction kettle, a cyclone separator, a filter, a buffer tank, a spray tower and a rotary kiln,
a molten liquid outlet of the intermediate frequency smelting furnace is connected with the alloy forming die;
the reaction kettle is connected with the cyclone separator through a pipeline, the filter is connected with an upper outlet of the cyclone separator, and a lower outlet of the cyclone separator is used for discharging slag; the filter outlet is connected with the buffer tank, the buffer tank is connected with the material inlet of the spray tower, and the material outlet of the spray tower is connected with the rotary kiln.
10. The system for preparing mesoporous alumina according to claim 9, wherein the intermediate frequency smelting furnace and the alloy forming die are both filled with a protective gas, and the protective gas is one or more of nitrogen, helium or argon; and/or
The reaction kettle is provided with a hydrogen outlet, the hydrogen outlet is connected with a condenser, the outlet of the condenser is connected with a molecular sieve dryer, and the molecular sieve dryer is connected with a hydrogen storage tank.
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| CN113371746A (en) * | 2021-07-14 | 2021-09-10 | 中氢能源科技发展(内蒙古)有限公司 | Method for preparing superfine mesoporous alumina and obtained product |
| WO2022105228A1 (en) * | 2020-11-23 | 2022-05-27 | 中氢能源科技发展(内蒙古)有限公司 | Method and system for preparing mesoporous aluminum oxide |
| WO2022134509A1 (en) * | 2020-12-21 | 2022-06-30 | 中氢能源科技发展(内蒙古)有限公司 | Preparation method for pseudo-boehmite |
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