CN114560482A - Pseudo-boehmite powder, forming carrier and preparation method thereof - Google Patents
Pseudo-boehmite powder, forming carrier and preparation method thereof Download PDFInfo
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- CN114560482A CN114560482A CN202210117285.1A CN202210117285A CN114560482A CN 114560482 A CN114560482 A CN 114560482A CN 202210117285 A CN202210117285 A CN 202210117285A CN 114560482 A CN114560482 A CN 114560482A
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- 239000000843 powder Substances 0.000 title claims abstract description 80
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002002 slurry Substances 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 50
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011148 porous material Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 238000006703 hydration reaction Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 20
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 5
- 230000000996 additive effect Effects 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 230000036571 hydration Effects 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 239000007790 solid phase Substances 0.000 claims description 5
- 239000012266 salt solution Substances 0.000 claims description 4
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 150000007529 inorganic bases Chemical class 0.000 claims description 2
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 2
- 150000007530 organic bases Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000001125 extrusion Methods 0.000 abstract description 2
- 238000005096 rolling process Methods 0.000 abstract description 2
- 238000010411 cooking Methods 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 16
- 239000002994 raw material Substances 0.000 description 10
- 239000002243 precursor Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000003213 activating effect Effects 0.000 description 6
- 230000005484 gravity Effects 0.000 description 6
- 239000008188 pellet Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 229910006636 γ-AlOOH Inorganic materials 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 241000219782 Sesbania Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- -1 aluminum alkoxide Chemical class 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Images
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/633—Pore volume less than 0.5 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- 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
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- 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
- C01P2006/14—Pore volume
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention particularly relates to a pseudo-boehmite powder, a forming carrier and a preparation method thereof, belonging to the technical field of pseudo-boehmite preparation, and the method comprises the following steps: will be rho-Al2O3Mixing the slurry with a solvent, and then grinding to obtain first slurry; mixing the first slurry with a conversion additive to obtain second slurry; carrying out hydration reaction on the second slurry to obtain third slurry; carrying out solid-liquid separation, washing and drying on the third slurry to obtain pseudo-boehmite powder; mixing the obtained pseudo-boehmite powder with a binder, a pore-expanding agent and a forming agent, and obtaining spherical or strip-shaped particles by adopting a rolling forming or extrusion forming mode; cooking the granulesAnd (4) melting and roasting to obtain the formed carrier. Using low cost rho-Al2O3The material is used for hydration reaction, and the key indexes of the pseudo-boehmite powder such as pore volume, specific surface area and the like can be effectively improved.
Description
Technical Field
The invention belongs to the technical field of preparation of pseudo-boehmite, and particularly relates to a pseudo-boehmite powder, a forming carrier and a preparation method thereof.
Background
The pseudo-boehmite is an alumina crystal containing 1.8-2.5 crystal waters, and has incomplete crystallinity and a crystal form mostly in a sheet-layered structure with wrinkles. Pseudoboehmite has a spatial network structure, large voids and a developed specific surface area, and thus is often used as a precursor for preparing an active alumina-based catalyst.
At present, the traditional process for preparing the pseudoboehmite in China mainly comprises a sodium metaaluminate-carbon dioxide method, an aluminum alkoxide hydrolysis method, an ammonia water-aluminum salt reaction method and the like, wherein the methods all need the steps of gelatinizing, aging, washing, drying and the like, the preparation process is long, a plurality of influencing factors exist, and the control of reaction process parameters is difficult. Meanwhile, the prepared product has the pore volume of 0.4-1.5 mL/g and the specific surface area of 200-400 m2Between/g, although can satisfy the requirements of high-end catalyst and absorption at home and abroadThe auxiliary agent is required in the market, but the product cost is high, the production process relates to high-concentration acid-base and organic solution, waste water and waste residue are generated, and the process environment-friendliness is poor. The production of strip and spherical carriers is limited by raw material indexes, and product cost and product indexes cannot be considered, so that the conventional quick-release live aluminum ball has low cost but poorer indexes, and the strip quasi-thin water carrier has good indexes but high cost, and the contradiction is more prominent particularly for a mesoporous carrier.
Disclosure of Invention
The application aims to provide a pseudo-boehmite powder, a forming carrier and a preparation method thereof, and aims to solve the problem that the pseudo-boehmite powder prepared by the existing method is low in product index.
The embodiment of the invention provides a preparation method of pseudo-boehmite powder, which comprises the following steps:
will be rho-Al2O3Mixing the slurry with a solvent, and then grinding to obtain first slurry;
mixing the first slurry with a conversion additive to obtain second slurry;
carrying out hydration reaction on the second slurry to obtain third slurry;
and carrying out solid-liquid separation, washing and drying on the third slurry to obtain the pseudo-boehmite powder.
Optionally, the step of mixing rho-Al2O3Mixing with a solvent, and grinding to obtain the rho-Al in a first slurry2O3And the mass ratio of the solvent is 1: (2-10).
Optionally, the particles in the first slurry have a particle size of 1 μm to 30 μm.
Optionally, the conversion aid comprises at least one of inorganic acid, organic acid, inorganic base, organic base, inorganic salt solution and organic surfactant, and the addition mass of the conversion aid is less than or equal to 10%.
Optionally, the liquid-solid ratio of the second slurry is (2-10): 1.
Optionally, the pH of the second slurry is: 2-13
Optionally, the temperature of the hydration reaction is 0-120 ℃, the time of the hydration reaction is 1-24 h, and stirring is carried out during the hydration reaction.
Based on the same inventive concept, the embodiment of the invention also provides the pseudo-boehmite powder, and the powder is prepared by the preparation method of the pseudo-boehmite powder.
Based on the same inventive concept, the embodiment of the invention also provides a preparation method of the molded carrier, which comprises the following steps:
obtaining the pseudo-boehmite powder, wherein the pseudo-boehmite powder is the pseudo-boehmite powder;
mixing the pseudo-boehmite powder, the solid-phase binder, the pore-expanding aid and the forming aid to obtain a mixture;
and carrying out molding, hydration treatment and activation roasting on the mixture to obtain a molded carrier.
Based on the same inventive concept, the embodiment of the invention also provides a molded carrier, and the carrier is prepared by the preparation method of the molded carrier.
Optionally, the pore volume of the carrier is 0.5mL/g-0.7mL/g, and the proportion of pores with the diameter of more than 75nm in the pores of the carrier is more than 10%.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
the preparation method of the pseudo-boehmite powder provided by the embodiment of the invention adopts low-cost rho-Al2O3The material is subjected to hydration reaction, and key indexes such as pore volume, specific surface area and the like of the pseudo-boehmite powder can be effectively improved.
The above description is only an overview of the technical solutions of the present invention, and the present invention can be implemented in accordance with the content of the description so as to make the technical means of the present invention more clearly understood, and the above and other objects, features, and advantages of the present invention will be more clearly understood.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a first flowchart of a method provided by an embodiment of the invention;
fig. 2 is a flowchart of a method according to an embodiment of the present invention.
Detailed Description
The present invention will be specifically explained below in conjunction with specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly presented thereby. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the general idea of the embodiment of the application is as follows:
according to an exemplary embodiment of the present invention, there is provided a method for preparing a pseudo-boehmite powder, the method including:
s1, mixing rho-Al2O3Mixing the slurry with a solvent, and then grinding to obtain first slurry;
In some embodiments, p-Al2O3The preparation method comprises the step of carrying out flash roasting on the aluminum hydroxide in a fast-removing furnace.
Specifically, rho-Al is obtained by flash roasting aluminum hydroxide in a fast-removing furnace2O3And deionized water according to the ratio of 2: 1-10: 1, and feeding the slurry into a grinder to a certain granularity.
To make rho-Al2O3The slurry has good fluidity and controlled rho-Al2O3And a solvent in a mass ratio of 1: 2-1: 10, the solution is very viscous due to the overlarge value of the ratio, and the solid content of the reaction system is too small and the yield is reduced if the ratio is too small.
In this example, the particle size of the particles in the first slurry is 1 μm to 30 μm.
The reason for controlling the particle size of the particles in the first slurry to be 1 μm to 30 μm is that controlling the appropriate particle size facilitates completion of the conversion reaction, and too large a particle size results in incomplete reaction, while too small a particle size results in excessively viscous solution and increased water demand.
S2, mixing the first slurry with a conversion additive to obtain second slurry;
in particular, for controlling rho-Al2O3The degree and speed of hydration reaction can be adjusted by adding a proper amount of conversion auxiliary agent into the obtained slurry and adjusting the liquid-solid ratio rho-Al2O3And solvent to 1: 2-1: 10.
to make rho-Al2O3Fully dispersing in the solution, and controlling the liquid-solid ratio of the second slurry to be 1: 2-1: 10, the solid-liquid ratio is too large, so that the solution is too viscous, the conversion reaction is not thorough, and if the solid ratio is too small, the solid content of the reaction system is too small, and the yield is reduced.
Specifically, the conversion aid may be an inorganic or organic acid, a base, a salt solution, wherein the acid includes but is not limited to one of nitric acid, sulfuric acid, hydrochloric acid, formic acid, acetic acid, and citric acid, wherein the base includes but is not limited to one of ammonia, sodium hydroxide, and potassium hydroxide, wherein the salt solution includes but is not limited to one of sodium carbonate and sodium bicarbonate, and the surfactant is selected from one or more of a cationic dispersant, an anionic dispersant, and a nonionic dispersant, including but not limited to dodecyltrimethylammonium bromide, sodium dodecylsulfate, polyethylene glycol, and the like. The addition mass of the transformation aid is 0-1%.
The reason for controlling the addition amount of the conversion aid to be 0-1% is that rho-Al is added under the action of the aid with proper concentration compared with the addition of no aid2O3Can be fully converted.
S3, carrying out hydration reaction on the second slurry to obtain third slurry;
specifically, the hydration reaction is carried out at the temperature of 0-120 ℃, the reaction process is accompanied by stirring, and the reaction time is 1-24 h.
The hydration reaction temperature is controlled to be 0-120 ℃, the reaction time is controlled to be 1-24h, so that the reaction is thorough, the output efficiency is reduced due to overlong time when the value is overlarge, and the reaction is incomplete due to undersize.
And S4, carrying out solid-liquid separation, washing and drying on the third slurry to obtain the pseudo-boehmite powder.
Specifically, after the hydration reaction is finished, the obtained slurry is subjected to suction filtration, washing and drying to obtain the pseudoboehmite product with large pore volume, high specific surface area, high purity and high crystallinity.
The method has simple and short process, and only needs to add rho-Al into a grinder and a high-temperature reaction tank according to a certain proportion in the preparation process of the molding precursor2O3Adding a small amount of conversion auxiliary agent into pure water if necessary, and stirring for a certain time at constant temperature. Low equipment investment, low raw material investment cost, short reaction time and low total investment cost. In addition, as the key indexes such as pore volume, specific surface area and the like are obviously improved, the novel product has high catalysis and adsorption efficiency and small dosage when being used in the fields of downstream catalysts, adsorbents and the like, reduces the use cost for downstream manufacturers and has wide application prospect.
According to another exemplary embodiment of the present invention, a pseudo-boehmite powder is provided, which is prepared by the method for preparing the pseudo-boehmite powder provided above.
The pore volume of the pseudo-boehmite powder is 0.3-0.8 mL/g, and the specific surface area of the pseudo-boehmite powder is 200-450 m 2The purity of the pseudo-boehmite powder is 90.00-99.99%, and the crystallinity of the pseudo-boehmite powder is 30-95%.
The main phase of the pseudo-boehmite powder contains gamma-AlOOH and a trace amount of beta-Al (OH)3The high-resolution transmission electron microscope characterization shows that gamma-AlOOH is uniformly distributed with a large number of pores with the pore diameter of 2-5 nm, and primary particles are within 50nm, so that the material has the characteristics of large pore volume, high specific surface area and concentrated pore diameter distribution.
According to another exemplary embodiment of the present invention, there is provided a method of manufacturing a shaped carrier, the method including:
s1, mixing rho-Al2O3Mixing the slurry with a solvent, and then grinding to obtain first slurry;
s2, mixing the first slurry with a conversion additive to obtain second slurry;
s3, carrying out hydration reaction on the second slurry to obtain third slurry;
s4, carrying out solid-liquid separation, washing and drying on the third slurry to obtain a pseudo-boehmite powder;
s5, mixing the pseudo-boehmite powder, the solid-phase binder, the pore-expanding aid and the forming aid to obtain a mixture;
in some embodiments, the pseudo-boehmite powder, the solid-phase binder, the pore-enlarging aid and the forming aid are added in a mass ratio of 1: 1: 0.1: 0.1, in particular, the solid phase binder may be chosen from rho-Al 2O3Common pseudo-boehmite, alumina sol, silica sol, etc.; the pore-enlarging assistant may be selected from macroporous quasi-thin water, macroporous alumina silica gel, etc.; the forming aid can be selected from sesbania powder, starch and the like.
And S6, forming, hydrating and activating roasting the mixture to obtain a formed carrier.
In the embodiment, the main process parameters of hydration treatment are 0-120 ℃, the PH value is 2-13, the time is 1-24h, and the main process parameters of activation roasting are 300-700 ℃.
Low cost rho-Al produced by the Pair fast strip Process2O3The material is prepared by controlling the normal pressure hydration condition to obtain the pseudo-boehmite product of the active alumina precursor, thereby effectively improving the rho-Al content of the material2O3The pore volume, the specific surface area and other key indexes are obtained, the precursor is taken as a main raw material, other components are added, the physical and chemical properties of the product are adjusted, the purity and the strength of the product are improved, and a mesoporous carrier series product with the pore volume of 0.3-0.8mlL/g is finally obtained by adopting an appropriate forming and processing mode, so that the catalytic efficiency and the adsorption efficiency in the downstream application process are effectively improved, and a brand new active alumina carrier series product with high added value is formed.
According to another exemplary embodiment of the present invention, there is provided a shaped carrier, which is produced by the method for producing a shaped carrier as provided above. Specifically, the pore volume of the carrier is 0.5mL/g-0.7mL/g, the ratio of pores with the diameter of more than 75nm in the pores of the carrier is more than 10%, and the specific surface area of the carrier can be adjusted according to the activation temperature.
In practice, the molding process of the molded carrier includes two types:
(1) mixing the obtained pseudoboehmite powder and the traditional pseudoboehmite according to the proportion of 1: 1-5: 1, adding 2-10% of sesbania powder, uniformly mixing, adding a proper amount of dilute nitric acid according to the water-powder ratio of 30-80%, kneading, extruding, activating and roasting the obtained product to obtain the strip-shaped active alumina-based catalyst carrier, wherein the pore volume of the obtained product can be kept above 0.45mL/g, and the specific surface area can be kept to 320m2More than g.
(2) Mixing the obtained pseudoboehmite powder with high-quality rho-Al2O3Mixing the raw powder, pore-expanding agent, forming assistant, etc. and rolling to form the spherical active alumina carrier. The pore volume of the product reaches between 0.5 and 0.70mL/g, and the specific surface area can reach 280-340m at most2The content of macropores with the diameter of more than 75nm is more than 10 percent between the concentration of the active carbon and the concentration of the macropores per gram, and the catalyst is very suitable for catalytic oxidation reaction of organic matters in the fields of coal chemical industry and wastewater treatment.
The pseudo-boehmite powder, the molded carrier and the production method thereof according to the present application will be described in detail below with reference to examples, comparative examples and experimental data.
Example 1
A preparation method of pseudo-boehmite powder comprises the following steps:
To 100g of rho-Al2O3Adding 1000ml of deionized water, grinding the mixture in a grinder until the D50 particle size is 5 microns, taking out the slurry, pouring the slurry into a beaker, adding a small amount of acetic acid to adjust the pH value of the solution to 6.0, placing a baked cake in a constant-temperature water bath kettle, heating the baked cake to 90 ℃, keeping the stirring speed and the temperature constant, controlling the reaction time to be 4 hours, and filtering, washing and drying the slurry after the reaction is finished to obtain the molded precursor powder.
Example 2
A preparation method of pseudo-boehmite powder comprises the following steps:
to 100g of rho-Al2O3Adding 1000ml of deionized water, grinding the mixture in a grinder until the D50 particle size is 3 microns, taking out the slurry, pouring the slurry into a beaker, adding a small amount of sodium bicarbonate to adjust the pH value of the solution to 7.5, placing a baked cake in a constant-temperature water bath kettle, heating the baked cake to 90 ℃, keeping the stirring speed and the temperature constant, controlling the reaction time for 3 hours, and filtering, washing and drying the slurry after the reaction is finished to obtain the molded precursor powder.
Example 3
A method of making a shaped support, the method comprising:
mixing the pseudo-boehmite raw powder obtained in the embodiment 1 according to the proportion of 30% and the low-sodium pseudo-boehmite according to the proportion of 70%, adding 2-10% of sesbania powder, uniformly mixing, adding a proper amount of dilute nitric acid solution according to the proportion of 30-80% of the water powder, kneading, extruding, and performing activated roasting on the obtained product to obtain the active alumina-based catalyst.
Example 4
A method of making a shaped support, the method comprising:
70 percent of pseudo-boehmite raw powder and 30 percent of rho-alumina raw powder obtained in the embodiment 2 are mixed for 0.5h, granulation with a diameter of 2-4mm is carried out by adopting a turntable, the bulk specific gravity of green pellets is controlled to be 1.0g/ml, hydration treatment is carried out for 36h, and activation is carried out in a vertical furnace at 500 ℃, thus obtaining the active alumina-based catalyst.
Example 5
A method of making a shaped support, the method comprising:
the pseudo-boehmite raw powder obtained in the embodiment 1, rho-alumina raw powder 50% and silicon-aluminum dry glue powder 15% are mixed for 1h, the raw materials are granulated into particles with phi of 2-4mm by adopting a turntable, the bulk specific gravity of green pellets is controlled to be 1.01g/ml, hydration treatment is carried out for 36h, and the active alumina-based catalyst can be obtained by activating in a vertical furnace at 500 ℃.
Example 6
A method of making a shaped support, the method comprising:
the pseudo-boehmite raw powder obtained in the embodiment 2, rho-alumina raw powder 45% and silicon-aluminum dry glue powder 5% are mixed for 1h, the raw materials are granulated into particles with the diameter of 2-4mm by adopting a turntable, the bulk specific gravity of green pellets is controlled to be 1.0g/ml, hydration treatment is carried out for 24h, and the active alumina-based catalyst can be obtained by activating in a vertical furnace at the temperature of 600 ℃.
Example 7
A method of making a shaped support, the method comprising:
the pseudo-boehmite raw powder obtained in the embodiment 1, rho-alumina raw powder 50% and silicon-aluminum dry glue powder 20% are mixed for 1h, the raw materials are granulated into particles with phi of 2-4mm by adopting a turntable, the bulk specific gravity of green pellets is controlled to be 0.99g/ml, hydration treatment is carried out for 36h, and the active alumina-based catalyst can be obtained by activating in a vertical furnace at 550 ℃.
Example 8
A method of making a shaped support, the method comprising:
the pseudo-boehmite raw powder obtained in the embodiment 2, rho-alumina raw powder and silicon-aluminum dry glue powder are 0, the raw materials are mixed for 0.5h, granulation with a rotating disc is carried out to obtain phi 2-4mm, the bulk specific gravity of green pellets is controlled to be 1.02g/ml, hydration treatment is carried out for 24h, and activation is carried out in a vertical furnace at 500 ℃, so as to obtain the active alumina-based catalyst.
Example 9
A method of making a shaped support, the method comprising:
the pseudo-boehmite raw powder obtained in the embodiment 1, rho-alumina raw powder and silicon-aluminum dry glue powder are 10 percent, the raw materials are mixed for 1h, granulation with phi 2-4mm is carried out by adopting a turntable, the bulk specific gravity of green pellets is controlled to be 1.02g/ml, hydration treatment is carried out for 24h, and activation is carried out in a vertical furnace at 400 ℃, so as to obtain the active alumina-based catalyst.
Comparative example 1
Sodium aluminate solution with certain concentration and acid gasBodies such as CO2Acid liquid such as hydrochloric acid, aluminum sulfate, aluminum chloride and the like, and the neutralization reaction is carried out, the PH of the reaction end point is controlled, and the pore volume is more than 0.39mL/g, the specific surface is 290m2A pseudo-boehmite product per gram. Meanwhile, a production process of the product can generate a large amount of residual mother liquor and washing liquor, the direct discharge of the mother liquor and the washing liquor can bring serious environmental protection problems, and the cost is greatly increased by adopting the treatment processes of neutralization precipitation, crystallization evaporation and the like at present.
Comparative example 2
In the normal rho-Al2O3Directly adding water as a binder to produce an active alumina spherical product with the pore volume of 0.41ml/g and the specific surface of 295m2The volume/g is lower than the pore volume and the specific surface of the product formed by the method.
Comparative example 3
Adding peptizing agent and extrusion aid into a common pseudo-boehmite product, kneading, extruding, curing, activating and the like to obtain an active alumina strip-shaped product, wherein the pore volume of the product is 0.35mL/g, and the specific surface area is 236m2The volume/g is lower than the pore volume and the specific surface of the product formed by the method.
Related experiments:
the precursor powders obtained in examples 1-2 and comparative example 1 were subjected to the test, and the results are shown in the following table.
From the above table, the precursor powder (i.e. pseudo-boehmite powder) prepared by the method provided by the application has a pore volume of 0.3-0.8 ml/g and a specific surface area of 200-450 m2In the case of the comparative example and the example, when a certain parameter is out of the range of the examples, the pore volume and the specific surface index of the product are decreased.
The active alumina-based catalysts obtained in examples 3 to 9 and comparative examples 2 to 3 were subjected to the test, and the results are shown in the following table.
From the above table, the active alumina-based catalyst prepared by the method provided by the embodiment of the present application has a pore volume of 0.45mL/g or more and a specific surface area of 300m 2Above/g, as can be seen from the comparison of the data of the comparative examples and examples, when a certain parameter is out of the range of the examples of the present application, the reduction of the pore volume and specific surface index of the product may occur.
One or more technical solutions in the embodiments of the present invention at least have the following technical effects or advantages:
(1) the method provided by the embodiment of the invention uses rho-Al obtained by quickly removing aluminum hydride2O3As starting material, p-Al2O3Carrying out wet grinding, normal-pressure hydrothermal conversion and auxiliary agent modification to obtain a pseudo-boehmite product with medium and large pore volume and high specific surface area;
(2) the method provided by the embodiment of the invention uses the rho-Al obtained by quickly removing the aluminum hydride2O3As starting material, p-Al2O3Wet grinding, hydrothermal conversion modification under normal pressure or near normal pressure to obtain main phase containing gamma-AlOOH and trace beta-Al (OH) with large pore volume and high specific surface area3The pseudo-boehmite product. High-resolution transmission electron microscope characterization shows that gamma-AlOOH is uniformly distributed with a large number of pores with the pore diameter of 2-5 nm, and primary particles are within 50nm, so that the material has the characteristics of large pore volume, high specific surface area and concentrated pore diameter distribution. The pore volume of the obtained product is between 0.4 and 0.8mL/g, and the specific surface area is between 200 and 450m2Between/g;
(3) The method provided by the embodiment of the invention is simple and short in process, and only rho-Al needs to be added into a grinder and a high-temperature reaction tank according to a certain proportion in the preparation process of the molding precursor2O3Adding a small amount of conversion auxiliary agent into pure water if necessary, and stirring for a certain time at constant temperature. Low equipment investment, low raw material investment cost, short reaction time and low total investment cost. In addition, as the key indexes such as pore volume, specific surface area and the like are obviously improved, the novel product is used in the fields of downstream catalysts, adsorbents and the likeThe catalyst has high catalytic and adsorption efficiency and small dosage, reduces the use cost for downstream manufacturers, and has wide application prospect;
(4) the maximum pore volume of the formed carrier provided by the embodiment of the invention reaches 0.5-0.70ml/g, the specific surface area can be adjusted according to the activation temperature, the carrier has the outstanding characteristic that the content of macropores with the diameter of more than 75nm is more than 10%, and the mass transfer efficiency in the catalytic process is greatly improved.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including the preferred embodiment and all changes and modifications that fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A preparation method of pseudo-boehmite powder is characterized by comprising the following steps:
will rho-Al2O3Mixing the slurry with a solvent, and then grinding to obtain first slurry;
mixing the first slurry with a conversion additive to obtain second slurry;
carrying out hydration reaction on the second slurry to obtain third slurry;
and carrying out solid-liquid separation, washing and drying on the third slurry to obtain the pseudo-boehmite powder.
2. The method for preparing pseudo-boehmite powder according to claim 1, characterized in that p-Al is mixed 2O3Mixing with a solvent, and grinding to obtain rho-Al in the first slurry2O3And the mass ratio of the solvent is 1: (2-10).
3. The method for preparing pseudo-boehmite powder according to claim 1, characterized in that the particle size of the particles in the first slurry is 1 μm to 30 μm.
4. The method for preparing pseudo-boehmite powder according to claim 1, characterized in that the solvent is deionized water or a solution of deionized water and a conversion aid, the conversion aid comprises at least one of inorganic acid, organic acid, inorganic base, organic base, inorganic salt solution and organic surfactant, and the addition mass of the conversion aid is less than or equal to 10%; the pH value of the second slurry is 2-13.
5. The method for preparing pseudo-boehmite powder according to claim 1, characterized in that the liquid-solid ratio of the second slurry is (2-10): 1.
6. the method for preparing pseudo-boehmite powder according to claim 1, characterized in that the temperature of the hydration reaction is 0 ℃ to 120 ℃, the time of the hydration reaction is 1h to 24h, and stirring is carried out during the hydration reaction.
7. A pseudo-boehmite powder characterized in that the powder is prepared by the method for preparing the pseudo-boehmite powder according to any one of claims 1 to 6.
8. A method of making a shaped support, the method comprising:
obtaining pseudo-boehmite powder, wherein the pseudo-boehmite powder is the pseudo-boehmite powder in claim 7;
mixing the pseudo-boehmite powder, the solid-phase binder, the pore-expanding aid and the forming aid to obtain a mixture;
and carrying out molding, hydration treatment and activation roasting on the mixture to obtain a molded carrier.
9. A shaped carrier, characterized in that it is produced by the process for the production of a shaped carrier according to claim 8.
10. The shaped support according to claim 9, wherein the support has a pore volume of 0.5mL/g to 0.7mL/g, and the proportion of pores having a diameter of 75nm or more among the pores of the support is more than 10%.
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