CN109420529A - A kind of preparation method of alumina support - Google Patents
A kind of preparation method of alumina support Download PDFInfo
- Publication number
- CN109420529A CN109420529A CN201710771943.8A CN201710771943A CN109420529A CN 109420529 A CN109420529 A CN 109420529A CN 201710771943 A CN201710771943 A CN 201710771943A CN 109420529 A CN109420529 A CN 109420529A
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- Prior art keywords
- temperature
- preparation
- acid
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- boehmite
- Prior art date
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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 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 34
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 26
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000012545 processing Methods 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004927 clay Substances 0.000 claims abstract description 14
- 229910017464 nitrogen compound Inorganic materials 0.000 claims abstract description 13
- 150000002830 nitrogen compounds Chemical class 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 150000007524 organic acids Chemical class 0.000 claims abstract description 8
- 238000004898 kneading Methods 0.000 claims abstract description 6
- 238000010009 beating Methods 0.000 claims abstract description 3
- 238000002791 soaking Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 239000004411 aluminium Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- 125000002723 alicyclic group Chemical group 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 150000001408 amides Chemical group 0.000 claims description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- -1 amides compound Chemical class 0.000 claims description 2
- DNSISZSEWVHGLH-UHFFFAOYSA-N butanamide Chemical compound CCCC(N)=O DNSISZSEWVHGLH-UHFFFAOYSA-N 0.000 claims description 2
- 210000002700 urine Anatomy 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 22
- 239000011148 porous material Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 14
- 239000003795 chemical substances by application Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 239000006229 carbon black Substances 0.000 description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052901 montmorillonite Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 241000772415 Neovison vison Species 0.000 description 2
- 241000219782 Sesbania Species 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005360 mashing Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007324 demetalation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 229910001648 diaspore Inorganic materials 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- FYSNRPHRLRVCSW-UHFFFAOYSA-N dodecasodium;tetraborate Chemical class [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-].[O-]B([O-])[O-] FYSNRPHRLRVCSW-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000000415 inactivating effect Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001935 peptisation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/883—Molybdenum and nickel
-
- 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
- B01J35/635—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
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of alumina support.This method comprises: boehmite and water are mixed with beating by (1), the mixed acid solution of organic acid and inorganic acid is added into slurries, the pH value for controlling slurries is 2-5, carries out being heated to reflux processing；(2) basic nitrogen compound is added into step (1), is then sealed hydro-thermal process, the slurries after hydro-thermal process are washed, dry, obtain treated boehmite；(3) the treated boehmite kneading and compacting for obtaining the clay after high-temperature process with step (2), molding is through drying, low-temperature bake；(4) material that is obtained with aqueous slkali soaking step (3) simultaneously seals heat treatment, and material is washed after processing, dry and roasting, and alumina support is made.The alumina support has large hole appearance and aperture, pore distribution concentration, and duct has the uniformity inside good connectivity and duct, is suitable for preparation weight, residuum hydrogenating and metal-eliminating catalyst.
Description
Technical field
The present invention relates to a kind of preparation methods of alumina support, relate in particular to a kind of suitable for preparation weight, residual oil
The preparation method of the alumina support of Hydrodemetalation catalyst.
Background technique
Currently, in the production process of mink cell focus hydrodemetallization, since feedstock oil contains a certain amount of vanadium, sulphur, arsenic, nickel
Equal impurity, easily form deposition, so that the duct of blocking catalyst, causes catalyst activity to decline rapidly, or even inactivation, influence
Industrial application.Hold with large hole and the catalyst of larger bore dia holds metal and appearance coke formation is strong, catalyst can be slowed down
The operation cycle for inactivating, making catalyst extends.The pore structure of catalyst is determined that therefore, preparation has by the carrier for constituting catalyst
Large hole is held and the carrier of larger bore dia is prepared for the higher decompression residuum of residual oil, especially tenor, adds hydrogen
The key of catalyst for demetalation.
CN1160602A disclose a kind of macropore alumina supporter for being suitable as Hydrodemetalation catalyst carrier and its
Preparation method.The preparation method of the macropore alumina supporter includes that boehmite dry glue powder is mixed with water or aqueous solution,
It is kneaded into plastic, obtained plastic is extruded into bar on banded extruder, drying simultaneously roasts to obtain product, its main feature is that,
It is additionally added carbon black powder in above process as physics expanding agent and chemical action can occur with boehmite or aluminium oxide
The chemical enlargement agent of phosphorous, silicon or boron compound.Wherein carbon black powder dosage is 3-10wt%(on the basis of the weight of aluminium oxide).
Alumina support obtained can be used for preparing mink cell focus especially residuum hydrogenating and metal-eliminating and/or Hydrobon catalyst.
Alumina support disclosed in US4448896 be using carbon black as expanding agent, process is as follows: by expanding agent with intend it is thin
Diaspore dry glue powder is uniformly mixed, and aqueous solution of nitric acid kneading 30 minutes that mass fraction is 4.3% are added into said mixture,
Then ammonia spirit kneading 25 minutes that mass fraction is 2.1% are added, uniformly rear extruded moulding, carrier after molding pass through kneading
Final alumina support is made in roasting.Wherein the additional amount of carbon black powder is preferably greater than activated alumina or its precursor weight
20%。
CN102441436A discloses a kind of preparation method of alumina support.This method prepares the step of alumina support such as
Under: (1) boehmite dry glue powder and extrusion aid be uniformly mixed, and is then added and has dissolved physics expanding agent and chemical enlargement agent
Aqueous solution；(2) step (1) resulting material is uniformly mixed, the extruded moulding on banded extruder；(3) step (2) resulting material is dry
Final alumina support is made in dry, roasting.
In conclusion would generally be increased using physics expanding agent during prior art preparation macropore alumina supporter big
The accounting in hole.But the method cannot be guaranteed there is good connectivity between the alumina support duct prepared, cannot guarantee that
Uniformity inside the duct of the alumina support of preparation.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of preparation methods of alumina support.This method does not use
Physics expanding agent, the pore size distribution with biggish aperture and concentration while the alumina support of preparation holds with large hole, and
And duct has the uniformity inside good connectivity and duct.The carrier is suitable for preparation weight, residuum hydrogenating and metal-eliminating
Catalyst, hydrodemetallization activity and stability with higher.
The present invention provides a kind of preparation methods of alumina support, comprising:
(1) boehmite and water are mixed with beating, the mixed acid solution of organic acid and inorganic acid, control is added into gained slurries
The pH value of slurrying liquid is 2-5, carries out being heated to reflux processing；
(2) basic nitrogen compound is added into step (1), is then sealed hydro-thermal process, the slurries warp after hydro-thermal process
Washing, drying, obtain treated boehmite；
(3) the treated boehmite kneading and compacting for obtaining the clay after high-temperature process with step (2), molding
Through drying, low-temperature bake；
(4) material that is obtained with aqueous slkali soaking step (3) simultaneously seals heat treatment, and material is washed after processing, dry and roasting,
Alumina support is made.
In the method for the present invention, in step (1), the organic acid is one or more of acetic acid, oxalic acid and citric acid
Mixing, the inorganic acid are the mixing of one or more of sulfuric acid, nitric acid and hydrochloric acid；Organic acid and nothing in mixed acid solution
The molar ratio of machine acid is 1:3-1:6, and the inorganic acid molar concentration in the mixed acid solution is 3-6mol/L.
In the method for the present invention, boehmite described in step (1) add water pulping process using conventional method in that art into
The mass ratio of row, boehmite and water is preferably 1:3-1:10, wherein water is preferably deionized water.Described is heated to reflux
Treatment temperature is 30-60 DEG C, and being heated to reflux the time is 1-5 hours.
In the method for the present invention, basic nitrogen compound described in step (2) are as follows: urea, amides and alicyclic ring amine chemical combination
The mixing of one or more of object, the amides compound can be with are as follows: formamide, acetamide, propionamide, in butyramide
One or more mixing, the alicyclic ring aminated compounds can be with are as follows: triethylenediamine, diethylenetriamines, hexa-methylene
The mixing of one or more of tetramine；Preferably, the basic nitrogen compound is one of urea and acetamide or two
Kind mixing；The additional amount of the basic nitrogen compound and intend thin aluminium stone with Al2O3The mass ratio of meter is 1:5-1:10.
In the method for the present invention, preferably, borate is added while basic nitrogen compound is added in step (2), described
Borate can be the mixing of one or more of metaborate, ortho-borate and multi-borate, the additional amount of borate with
Boron oxide meter and boehmite are with Al2O3The mass ratio of meter is 0.5:100-1.5:100.
In the method for the present invention, sealing hydro-thermal process described in step (2) is the heat under the self-generated pressure of autoclave
Processing, treatment temperature are 120-160 DEG C, and the processing time is 4-8 hours.
In the method for the present invention, drying temperature described in step (2) is 100-120 DEG C, and drying time is 6-10 hours.
In the method for the present invention, clay described in step (3) is one in kaolin, montmorillonite, diatomite and concavo-convex rod soil
Kind or several mixing.The clay is as follows through the condition of high-temperature process: temperature is 950-1100 DEG C, and the processing time is that 5-10 is small
When.Clay through high-temperature process and intend thin aluminium stone with Al2O3The mass ratio of meter is 5:100-15:100.
In the method for the present invention, molding described in step (3), drying can be carried out using conventional method in that art.It formed
Cheng Zhong can according to need and one of conventional shaping assistant, such as peptizing agent, extrusion aid etc. or a variety of is added.Described
Peptizing agent is one or more in hydrochloric acid, nitric acid, sulfuric acid, acetic acid and oxalic acid etc., and the extrusion aid, which refers to, to be conducive to be squeezed into
One of substance of type, such as sesbania powder, carbon black, graphite powder and citric acid are a variety of.The drying condition are as follows: dry temperature
60-130 DEG C of degree, drying time are 1-10 hours.
In the method for the present invention, low-temperature bake temperature described in step (3) is 250-350 DEG C, preferably 280-320 DEG C, is roasted
Time is 3-6 hours.
In the method for the present invention, aqueous slkali described in step (4) is the solution of sodium hydroxide and/or potassium hydroxide, aqueous slkali
Molar concentration with OH-It is calculated as 3-5mol/L, the dosage of aqueous slkali and the mass ratio of the clay after high-temperature process are 40:1-60:
1。
In the method for the present invention, the heat treatment of sealing described in step (4) carries out in autoclave, heat treatment temperature 70-100
DEG C, the processing time is 3-5 hours.The drying temperature is 100-120 DEG C, and drying time is 2-10 hours.The maturing temperature
It is 550-700 DEG C, calcining time is 6-10 hours.
Compared with prior art, the invention has the following advantages that
The mixed acid that 1. a certain amount of organic acid and inorganic acid are added preparation method of the invention into the boehmite of mashing
Solution is heated to reflux processing, makes part boehmite peptization, while dissolving amorphous phase hydrated alumina therein, and keep away
Exempt from the destruction to boehmite crystal phase, in the sealing hydrothermal treatment process after subsequent addition basic nitrogen compound, is easy
Formation monocrystalline granularity is larger, crystal phase is uniform, intercrystalline moderately bonds, and clay is forming after being conducive to the high-temperature process being added in this way
It is more easily dispersed in the outer surface in duct in the process, desilication reaction occurs for clay when being then heat-treated in alkaline solution,
Not only make the aperture of carrier outer surface relatively large, while under the action of alkaline solution, also increases each hole in shaping carrier
The uniformity of connectivity and pore distribution between road.Load using alumina support of the invention as Hydrodemetalation catalyst
When body, appearance metal and volume carbon ability with higher has using the Hydrodemetalation catalyst that the aluminium oxide is prepared as carrier
Higher activity and activity stability.
2. borate is added while basic nitrogen compound is added in preparation method of the invention, make borate and aluminium
Double hydrolysis occur for salt, and the boron oxide precipitating load of formation is in oxidation aluminium surface, modulation carrier while improving carrier aperture
Surface nature.
Specific embodiment
Below with reference to embodiment to further illustrate the technical scheme of the present invention, but it is not limited to following embodiment.This
In invention, wt% is mass fraction.
Using N2Physics suction-desorption method characterization embodiment and comparative example carrier pore structure, concrete operations are as follows: using
ASAP-2420 type N2Physics is inhaled-is desorbed instrument and characterizes to sample pore structure.A small amount of sample is taken to be vacuum-treated 3 ~ 4 at 300 DEG C
Hour, finally product is placed under the conditions of liquid nitrogen cryogenics (- 200 DEG C) and carries out nitrogen suction-desorption test.Wherein specific surface area according to
BET equation obtains, and pore-size distribution and Kong Rong are obtained according to BJH model.
Embodiment 1
Weigh 200g boehmite dry glue powder (production of Wenzhou essence crystal alumina Co., Ltd, aluminium oxide contents on dry basis 70wt%)
It sets in a round bottom flask, 600 grams of deionized water mashing is added into flask, the mixing of nitric acid and acetic acid is added in Xiang Shangshu slurries
Acid solution (in mixed acid solution, nitric acid molar concentration is 3mol/L, and the molar concentration of acetic acid is 1mol/L), controls the pH of slurries
Value is 3 and is heated to reflux 3 hours in 40 DEG C.Above-mentioned slurries are transferred in autoclave, 15 grams of urea are added simultaneously into mixed material
It is heat-treated 6 hours after autoclave is sealed in 140 DEG C.Mixed serum is filtered after being cooled to room temperature, is washed, 120 DEG C of dryings 8 are small
When treated boehmite is made.
Weigh 200 grams of 7.5 grams of montmorillonite and the treated boehmite of 950 DEG C of roastings 5 hours, sesbania powder 6
Gram be uniformly mixed, be added into mixed material in right amount dissolved with the aqueous solution of 5 grams of acetic acid, extruded moulding, molding is in 120 DEG C of dryings
5 hours, dried object roasted 5 hours in 300 DEG C.Boehmite after roasting is placed in autoclave polytetrafluoroethyllining lining,
The sodium hydroxide solution that 400 grams of concentration are 4 mol/L is added simultaneously, the autoclave after sealing is heat-treated 4 hours in 90 DEG C, processing
Material afterwards is through filtering, deionized water washing, 110 DEG C drying 6 hours, 600 DEG C of roastings, 8 hours obtained alumina supports of the present invention
The property of A1, carrier are shown in Table 1.
Embodiment 2
With embodiment 1, only the additional amount of deionized water is 1400 grams.In mixed acid solution, sulfuric acid molar concentration is 4mol/L,
The molar concentration of oxalic acid is 1mol/L, and the pH value for controlling slurries is 2, and the temperature being heated to reflux is 30 DEG C, is flowed back 5 hours.Urea
Additional amount be 21 grams, hydro-thermal process temperature be 120 DEG C, hydro-thermal process 8 hours.Montmorillonite is changed to diatomite, and maturing temperature is
1100 DEG C, the additional amount of diatomite is 21 grams.Low-temperature bake temperature is 250 DEG C, and calcining time is 10 hours.Aqueous slkali is concentration
For the potassium hydroxide solution of 3 mol/L, solution usage is 1500 grams.Mixture heat treatment temperature is 100 DEG C, and the processing time is 3
Hour, alumina support A2 is made, the property of carrier is shown in Table 1.
Embodiment 3
With embodiment 1,1.0 grams of sodium tetraborates are added into mixed material while urea is only added.Montmorillonite is changed to quality
Than the diatomite and kaolinic mixture for 1:1, alumina support A3 of the present invention is made, the property of carrier is shown in Table 1.
Embodiment 4
With embodiment 1, only the additional amount of deionized water is 2000 grams.In mixed acid solution, the molar concentration of sulfuric acid is 6mol/
L, the molar concentration of citric acid are 1mol/L, and the pH value for controlling slurries is 5, and being heated to reflux temperature is 60 DEG C, and return time 1 is small
When.Urea is changed to acetamide, and additional amount is 28 grams, and 160 DEG C of hydro-thermal process temperature, hydrothermal conditions are 4 hours.Montmorillonite changes
For kaolin, maturing temperature is 1000 DEG C, and kaolinic additional amount is 14 grams.Low-temperature bake temperature is 350 DEG C, and calcining time is
7 hours.Aqueous slkali is that concentration is 5mol/L, and solution usage is 1200 grams.Mixture heat treatment temperature be 70 DEG C, processing the time be
4 hours, alumina support A4 of the present invention is made, the property of carrier is shown in Table 1.
Comparative example 1
With embodiment 1, only boehmite is handled without acid, and comparative example alumina support A5 is made, and the property of carrier is shown in Table
1。
Comparative example 2
With embodiment 1, only the unmixed acid processing of boehmite and urea liquid seal hydro-thermal process, and comparative example oxygen is made
Change alumina supporter A6, the property of carrier is shown in Table 1.
Comparative example 3
With embodiment 1, clay is not only added in carrier, comparative example alumina support A7 is made, the property of carrier is shown in Table 1.
1 carrying alumina volume property of table
Note: * pore size distribution refers to that the Kong Rong of certain diameter range inner hole in carrier accounts for the percentage of total pore volume.
Table 1 the result shows that, using the method for the present invention prepare alumina support, while with larger aperture with compared with
Big Kong Rong, pore distribution concentration is in 10-20nm.The alumina support of this method preparation is suitable for weight, residuum hydrogenating and metal-eliminating neck
Domain.
Embodiment 6
The present embodiment prepares Hydrodemetalation catalyst using aluminium oxide obtained by above-mentioned embodiment and comparative example as carrier.
Each 100 grams of alumina support prepared by embodiment 1-4 and comparative example 1-3 are weighed, 150mL Mo- is separately added into
Ni-NH3Solution (contains MoO by final catalyst312.0wt%, NiO3.0 wt%) dipping 2 hours, filter off redundant solution, 120 DEG C of bakings
It is dry, then 550 DEG C roasting temperature 5 hours, correspondence obtains Hydrodemetalation catalyst C1-C7.
Embodiment 7
The following examples illustrate be by carrier and comparative example aluminium oxide of aluminium oxide of the present invention carrier preparation hydrodemetallization
The catalytic performance of catalyst.
Using feedstock oil listed by table 2 as residual oil raw material, the catalytic of C1-C7 is evaluated on fixed bed residual hydrogenation reaction unit
Can, the item that catalyst be long 2 ~ 3 millimeters, reaction temperature is 375 DEG C, hydrogen partial pressure 13MPa, and volume space velocity is small for 1.0 when liquid
When-1, hydrogen to oil volume ratio 1000, measurement generates the content of each impurity in oil after reaction 3000 hours, calculates impurity removal percentage, comments
Valence the results are shown in Table 3.
2 raw material oil nature of table
3 catalyst hydrogenation performance comparison of table
| C1 | C2 | C3 | C4 | C5 | C6 | C7 | |
| De- V+Ni rate, wt% | 62.2 | 65.2 | 63.4 | 63.1 | 51.9 | 50.6 | 49.4 |
| Desulfurization degree, wt% | 40.4 | 37.3 | 40.7 | 41.8 | 30.4 | 29.0 | 28.6 |
It can be seen from 3 data of table compared with comparing alumina support, have using the catalyst that aluminium oxide of the present invention is prepared as carrier
There are higher hydrodemetallization activity and stability.
Claims (10)
1. a kind of preparation method of alumina support, it is characterised in that the following steps are included:
(1) boehmite and water are mixed with beating, the mixed acid solution of organic acid and inorganic acid, control is added into gained slurries
The pH value of slurrying liquid is 2-5, carries out being heated to reflux processing；
(2) basic nitrogen compound is added into step (1), is then sealed hydro-thermal process, the slurries warp after hydro-thermal process
Washing, drying, obtain treated boehmite；
(3) the treated boehmite kneading and compacting for obtaining the clay after high-temperature process with step (2), molding
Through drying, low-temperature bake；
(4) material that is obtained with aqueous slkali soaking step (3) simultaneously seals heat treatment, and material is washed after processing, dry and roasting,
Alumina support is made.
2. according to right want 1 described in preparation method, it is characterised in that: in step (1), the organic acid be acetic acid, oxalic acid
One or more of with citric acid, the inorganic acid is one or more of sulfuric acid, nitric acid and hydrochloric acid；Mixed acid solution
In organic acid and the molar ratio of inorganic acid be 1:3-1:6, the inorganic acid molar concentration in the mixed acid solution is 3-6mol/
L。
3. according to right want 1 described in preparation method, it is characterised in that: in step (1), the mass ratio of boehmite and water is
1:3-1:10, wherein water is preferably deionized water；The described treatment temperature that is heated to reflux is 30-60 DEG C, is heated to reflux the time and is
1-5 hours.
4. according to right want 1 described in preparation method, it is characterised in that: in step (2), the basic nitrogen compound be urine
One or more of element, amides and alicyclic ring aminated compounds, the amides compound are formamide, acetamide, third
One or more of amide and butyramide, the alicyclic ring aminated compounds be triethylenediamine, diethylenetriamines and
One or more of hexa；Preferably, the basic nitrogen compound is one of urea and acetamide
Or two kinds；The additional amount of the basic nitrogen compound and intend thin aluminium stone with Al2O3The mass ratio of meter is 1:5-1:10.
5. according to right want 1 described in preparation method, it is characterised in that: in step (2), be added basic nitrogen compound it is same
When be added borate, the borate is one or more of metaborate, ortho-borate and multi-borate, borate
Additional amount is in terms of boron oxide and boehmite is with Al2O3The mass ratio of meter is 0.5:100-1.5:100.
6. according to right want 1 described in preparation method, it is characterised in that: in step (2), the sealing hydro-thermal process be in height
The heat treatment under the self-generated pressure of reaction kettle is pressed, treatment temperature is 120-160 DEG C, and the processing time is 4-8 hours；The drying
Temperature is 100-120 DEG C, and drying time is 6-10 hours.
7. according to right want 1 described in preparation method, it is characterised in that: in step (3), the clay be kaolin, cover it is de-
One or more of soil, diatomite and concavo-convex rod soil, the clay is as follows through the condition of high-temperature process: temperature 950-1100
DEG C, the processing time is 5-10 hours；Clay through high-temperature process and intend thin aluminium stone with Al2O3The mass ratio of meter is 5:100-15:
100。
8. according to right want 1 described in preparation method, it is characterised in that: in step (3), the drying condition are as follows: dry temperature
Degree is 60-130 DEG C, and drying time is 1-10 hours；The low-temperature bake temperature be 250-350 DEG C, preferably 280-320 DEG C,
Calcining time is 3-6 hours.
9. according to right want 1 described in preparation method, it is characterised in that: in step (4), the aqueous slkali be sodium hydroxide
And/or the solution of potassium hydroxide, the molar concentration of aqueous slkali is with OH-It is calculated as 3-5mol/L, the dosage and high-temperature process of aqueous slkali
The mass ratio of clay afterwards is 40:1-60:1.
10. according to right want 1 described in preparation method, it is characterised in that: in step (4), the sealing is heat-treated in high pressure
It is carried out in kettle, heat treatment temperature is 70-100 DEG C, and the processing time is 3-5 hours；The drying temperature is 100-120 DEG C, dry
Time is 2-10 hours, and the maturing temperature is 550-700 DEG C, and calcining time is 6-10 hours.
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Effective date of registration: 20230914 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |