CN103818938B - A kind of preparation method of high thermal stability modified aluminium oxide supports - Google Patents
A kind of preparation method of high thermal stability modified aluminium oxide supports Download PDFInfo
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- CN103818938B CN103818938B CN201410067575.5A CN201410067575A CN103818938B CN 103818938 B CN103818938 B CN 103818938B CN 201410067575 A CN201410067575 A CN 201410067575A CN 103818938 B CN103818938 B CN 103818938B
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- high thermal
- thermal stability
- aluminium oxide
- isopropyl alcohol
- oxide supports
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 51
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000007062 hydrolysis Effects 0.000 claims abstract description 15
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 15
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910000858 La alloy Inorganic materials 0.000 claims abstract description 8
- 238000004821 distillation Methods 0.000 claims abstract description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 230000006698 induction Effects 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- -1 isopropylAlcohol lanthanide Chemical class 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 229960004592 isopropanol Drugs 0.000 claims 4
- 238000005266 casting Methods 0.000 abstract description 4
- 239000000413 hydrolysate Substances 0.000 abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 239000011148 porous material Substances 0.000 description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 4
- 229910001593 boehmite Inorganic materials 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229910001679 gibbsite Inorganic materials 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 229910002705 Al(C3H7O)3 Inorganic materials 0.000 description 1
- 238000004131 Bayer process Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- QERYCTSHXKAMIS-UHFFFAOYSA-M thiophene-2-carboxylate Chemical compound [O-]C(=O)C1=CC=CS1 QERYCTSHXKAMIS-UHFFFAOYSA-M 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of method of preparing high thermal stability modified aluminium oxide supports, be characterized in using the aluminium ingot of purity >=99.5% and the lanthanide rare metal of purity >=99% according to mass fraction 10:1～200:1, in frequency induction melting furnace, melting obtains Al-La alloy cast ingot in a vacuum, ingot casting makes by pressure processing the strip that thickness is 0.05～0.5mm, cut into 1～50mm long, under the condition that the rectangle strip that 1～50mm is wide and isopropyl alcohol are catalyst at 1～5% aluminum trichloride (anhydrous), 85 ~ 95 DEG C of back flow reaction are after 4 ~ 8 hours, prepare aluminium isopropoxide and isopropyl alcohol group of the lanthanides metal dibasic alkoxide, this dibasic alkoxide is 60 ~ 80 DEG C of not exclusively hydrolysis, be decompressed to after 0.09～0.01MPa at 60 ~ 85 DEG C, through distillation, hydrolysate is 85 ~ 95 DEG C of oven dry, 800～900 DEG C of calcinings, finally prepare the metal-modified high thermal stability aluminum oxide carrier of lanthanide rare powder body material.
Description
Technical field
The present invention relates to a kind of preparation method of high thermal stability modified aluminium oxide supports, particularly one Al-LaAlloy is prepared binary isopropoxide, then by not exclusively hydrolysis, calcining, changes thereby prepare rare earth modified high thermal stabilityThe preparation method of property alumina support.
Background technology
Activated alumina is one of a large amount of inorganic chemical products that use on our times. The main component of activated aluminaFor the aluminium oxide of the crystal formation such as γ, ρ, it is the solid material of a kind of porous, high degree of dispersion. The character feature master of activated aluminaBe: specific area is large, reactivity is strong, absorption property is good. Activated alumina is preparation space flight and aviation, weapons, electronics, special typeThe raw material of the tip materials such as pottery, is the car tail gas purificant of function admirable, in petrochemical industry and chemical industry, is used as and urgesAgent or carrier, in various industries as adsorbent and dehydrating agent.
The at present preparation method of activated alumina, is mainly divided into two kinds: a kind of be gibbsite that Bayer process is produced orIndustrial aluminium hydroxide thermal dehydration makes, but its impurity content is higher, and pass and surface texture are difficult to improve; Another kind method isBy in and aluminium salt or sodium aluminate solution or decompose to obtain aluminium glue, boehmite or boehmite by aluminium alcoholates, thenAt 400-800 DEG C, activation makes, due to the performance requirement difference to product, and raw material difference, corresponding manufacturing process also has very largeDifference.
Chinese patent (CN1202010C) introduced aluminium oxide under the existence of La with after sol-gel process preparationAt the temperature of 1000-1100 DEG C, long-time calcining keeps specific surface at 100m2/ g. The method is under Al (OH) 3 gel statesAdd the metal oxide of the modifications such as rare earth, add inhomogeneous problem but exist.
Summary of the invention
The object of the invention is to overcome the problems such as activated alumina poor high temperature stability that prior art produces, provide onePlant the preparation method of high thermal stability modified aluminium oxide supports, its adopts Al-La alloy to prepare binary isopropoxide, then passes through notComplete hydrolysis, calcining, thus prepare the preparation method of rare earth modified high thermal stability modified aluminium oxide supports.
The present invention realizes by following technical proposal, it is characterized in that comprising following process steps:
A: with the aluminium ingot of purity >=99.5% and the lanthanide rare metal of purity >=99%, by mass fraction 10:1～200:1,In frequency induction melting furnace, preparing Al-La is in a vacuum alloy cast ingot, and alloy cast ingot makes thickness by pressure processingThe strip of 0.05～0.5mm, cutting into length is 1～50mm, the rectangle strip that width is 1～50mm, rectangle strip and isopropylUnder the condition that alcohol is catalyst at 1～5% aluminum trichloride (anhydrous), 85 ~ 95 DEG C of back flow reaction, after 4 ~ 8 hours, prepare isopropyl alcoholAluminium and isopropyl alcohol group of the lanthanides metal dibasic alkoxide;
B: the dibasic alkoxide that steps A is prepared is 60 ~ 80 DEG C of hydrolysis under stirring condition, prepare boehmiteAnd the mixture of lanthanum hydroxide (being), be 0.5～5 to add water according to Al-La alloy cast ingot and the mass fraction ratio of water, make 1%~ 5% dihydroxylic alcohols is not hydrolyzed;
C: step B products therefrom is decompressed to after 0.1～0.02Mpa at 60 ~ 85 DEG C, distills 1～4 hour, distillation water outletSeparate the isopropyl alcohol producing, this isopropyl alcohol because of not moisture can direct reuse; Product after distillation is dried 4 ~ 6 hours at 85 ~ 95 DEG C, obtainsObtain product;
D: product that step C obtains obtains high thermal stability modified aluminium oxide supports powder material 800～900 DEG C of calciningsMaterial.
Raw material A l in described steps A and rare earth lanthanum are the common commercially available material that meets purity requirement; Described backflowReaction adopts common water-bath glass condensing reflux reactor.
The water adopting while hydrolysis in described step B is the pure water that resistivity is not less than 10M Ω, water in hydrolytic process controlAmount, is not exclusively hydrolyzed dibasic alkoxide, remains with 1% ~ 5% unhydrolysed dibasic alkoxide;
Related chemical reaction in process of the present invention
1, reacting of aluminium and isopropyl alcohol
2Al+6C3H7OH=2Al(C3H7O)3+3H2
2, the hydrolysis of aluminium alcoholates
Al(C3H7O)3+3H2O=Al(OH)3+3C3H7OH
3, aluminium is to the overall reaction of aluminium hydroxide
2Al+6C3H7OH+6H2O=3H2+2Al(OH)3+6C3H7OH
4, aluminium hydroxide is to the reaction of aluminium oxide
2Al(OH)3=Al2O3+3H2O
5, the overall reaction from aluminium to aluminium oxide
2Al+6C3H7OH+6H2O=3H2+6C3H7OH+Al2O3+3H2O
Can find out from reaction equation, isopropyl alcohol does not consume in positive reaction process in theory.
This patent innovation is rare earth element to generate dibasic alkoxide in the mode of alloy together with Al, then jointly not completeAll-hydrolytic, final calcining is rare earth oxide, therefore, rare earth oxide distributes more even, finally at 1200 DEG C, within 24 hours, forgesAfter burning, still keep 60m2The specific area of/g and the pore volume of 0.45ml/g, shown superior high-temperature stability. This modification powderAfter body material is aging through 1200 DEG C, still there is higher specific area and pore volume.
Technique of the present invention is succinct, flow process is short, energy consumption is low, environmental friendliness, non-environmental-pollution, can carry out large-scale production,There is obvious novelty, can produce significant economic benefit and social benefit.
Brief description of the drawings
Further illustrate flesh and blood of the present invention below in conjunction with accompanying drawing with example, but content of the present invention is not limited toThis.
Fig. 1 is process flow diagram of the present invention.
Detailed description of the invention
Technical scheme of the present invention realizes by the technological process of Fig. 1:
(1) with the aluminium ingot of purity >=99.5% and the lanthanide rare metal of purity >=99% according to mass fraction 10:1～200:1, frequently in induction melting furnace, prepare Al-La alloy cast ingot in a vacuum;
(2) ingot casting makes the strip of thickness 0.05～0.5mm by pressure processing, cuts into length and is 10～500mm, wideDegree is the strip of 10～500mm;
(3) 85 ~ 95 DEG C of backflows under the condition that the strip of having sheared and isopropyl alcohol are catalyst at 1～5% aluminum trichloride (anhydrous)React after 4 ~ 8 hours, prepare aluminium isopropoxide and isopropyl alcohol group of the lanthanides dibasic alkoxide;
(4) dibasic alkoxide 60 ~ 80 DEG C of hydrolysis under stirring condition, prepare boehmite and lanthanum hydroxide (being)Mixture, is 0.5～5 to add water according to Al-La alloy cast ingot and the mass fraction ratio of water, makes 1% ~ 5% not water of dihydroxylic alcoholsSeparate;
(5) 60 ~ 85 DEG C of products therefroms are decompressed to 0.1～0.02MPa distillation 1～4 hour, distill out the isopropyl that hydrolysis producesAlcohol, this isopropyl alcohol because of not moisture can direct reuse. Product after distillation is dried 4 ~ 6 hours at 85 ~ 95 DEG C;
(6) obtain high thermal stability modified aluminium oxide supports powder body material 800～900 DEG C of calcinings.
It should be noted that:
Metallic aluminium purity >=99.5% described in step (1), lanthanide rare metal purity >=99%, is common commercially available materialMaterial;
Vacuum intermediate-frequency induction melting furnace described in step (1) is industrial common equipment;
Back flow reaction described in step (3) is common water-bath glass condensing reflux reactor;
The water adopting while hydrolysis in step (4) is the pure water that resistivity is not less than 10M Ω.
Embodiment 1
Prepare in the vacuum intermediate-frequency smelting furnace of existing routine techniques by the feeding quantity of mass fraction Al:La=20:1Al-La alloy cast ingot, this ingot casting is after conventional surface treatment, and by the method for pressure processing, being worked into thickness is 0.1mmStrip, after surface clean, cutting into length is 2mm, the rectangle strip that width is 10mm, the 100g getting wherein adds backflowIn reactor, then add 600g industrial isopropanol and 3g aluminum trichloride (anhydrous). Heating water bath to 95 DEG C, reacted complete after 4 hoursGenerate dibasic alkoxide. This dibasic alkoxide adds 190g water to be not exclusively hydrolyzed under 60 DEG C of stirring conditions. Hydrolysate is 85DEG C be decompressed to 0.1Mpa distillation 1 hour, distill out the isopropyl alcohol that hydrolysis produces, this isopropyl alcohol can direct reuse. Product after distillationThing is dried 4 hours at 95 DEG C. The product of having dried prepares high thermal stability modified aluminas for 1 hour 900 DEG C of calcinings. RatioSurface area is not less than 220m2/ g, pore volume is not less than 0.8ml/g. Through 1200 DEG C, 24 o'clock long-pending being not less than of degradation rear surface80m2/ g, pore volume is not less than 0.55ml/g
Embodiment 2
Prepare in the vacuum intermediate-frequency smelting furnace of existing routine techniques by the feeding quantity of mass fraction Al:La=100:1Al-La alloy cast ingot, this ingot casting, after conventional surface treatment, by the method for pressure processing, is worked into thickness and is0.2mm, after surface clean, cutting into length is 2mm, the rectangle strip that width is 3mm, the 100g getting wherein adds backflowIn reactor, then add 600g industrial isopropanol and 3g aluminum trichloride (anhydrous). Heating water bath to 85 DEG C, reacted complete after 8 hoursGenerate dibasic alkoxide. This dibasic alkoxide adds 198g water to be not exclusively hydrolyzed under 80 DEG C of stirring conditions. Hydrolysate is 60DEG C be decompressed to 0.1Mpa distillation 1 hour, distill out the isopropyl alcohol that hydrolysis produces, this isopropyl alcohol can direct reuse. Product after distillationThing is dried 6 hours at 85 DEG C. The product of having dried prepares high thermal stability modified aluminas for 1 hour 900 DEG C of calcinings. RatioSurface area is not less than 150m2/ g, pore volume is not less than 0.7ml/g. Through 1200 DEG C, 24 o'clock long-pending being not less than of degradation rear surface60m2/ g, pore volume is not less than 0.45ml/g.
Claims (3)
1. a preparation method for high thermal stability modified aluminium oxide supports, is characterized in that comprising following process steps:
A: with the aluminium ingot of purity >=99.5% and the lanthanide rare metal of purity >=99%, by mass fraction 10:1～200:1, veryIn empty medium frequency induction melting furnace, preparing Al-La is alloy cast ingot, alloy cast ingot by pressure processing make thickness 0.05～The strip of 0.5mm, cutting into length is 1～50mm, the rectangle strip that width is 1～50mm, rectangle strip and isopropyl alcohol 1～5% aluminum trichloride (anhydrous) is that under the condition of catalyst, 85 ~ 95 DEG C of back flow reaction, after 4 ~ 8 hours, prepare aluminium isopropoxide and isopropylAlcohol lanthanide series metal dibasic alkoxide;
B: the metal dibasic alkoxide that steps A is prepared is 60 ~ 80 DEG C of hydrolysis under stirring condition, prepare boehmiteAnd the mixture of lanthanum hydroxide (being), be 0.5～5 to add water according to Al-La alloy cast ingot and the mass fraction ratio of water, make 1%~ 5% dihydroxylic alcohols is not hydrolyzed;
C: step B products therefrom is decompressed to after 0.1～0.02Mpa at 60 ~ 85 DEG C, distills 1～4 hour, distill out hydrolysis and produceRaw isopropyl alcohol, this isopropyl alcohol because of not moisture can direct reuse; Product after distillation is dried 4 ~ 6 hours at 85 ~ 95 DEG C, obtains and producesThing;
D: product that step C obtains obtains high thermal stability modified aluminium oxide supports powder body material 800～900 DEG C of calcinings.
2. the preparation method of high thermal stability modified aluminium oxide supports according to claim 1, is characterized in that described stepRaw material A l and rare earth lanthanum in rapid A are the common commercially available material that meets purity requirement; Described back flow reaction adopts commonWater-bath glass condensing reflux reactor.
3. the preparation method of high thermal stability modified aluminium oxide supports according to claim 1, is characterized in that described stepThe water adopting while hydrolysis in rapid B is the pure water that resistivity is not less than 10M Ω, and the water yield in controlling in hydrolytic process, makes dibasic alkoxideNot exclusively hydrolysis, remains with 1% ~ 5% unhydrolysed dibasic alkoxide.
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| US5312789A (en) * | 1987-05-27 | 1994-05-17 | Minnesota Mining And Manufacturing Company | Abrasive grits formed of ceramic, impregnation method of making the same and products made therewith |
| CN1202010C (en) * | 2001-09-19 | 2005-05-18 | 川化集团有限责任公司 | Aluminium oxide maintaining high specific surface area under high temperature and its preparing method |
| CN102381722B (en) * | 2011-08-10 | 2013-10-23 | 郭万里 | Preparation method of activated aluminum oxide and product prepared by using same |
| CN103055947B (en) * | 2011-10-21 | 2015-04-15 | 中国石油化工股份有限公司 | Preparation method of alumina support |
| CN103332717A (en) * | 2013-07-18 | 2013-10-02 | 北京世纪地和控股有限公司 | Production method of high-activity aluminium oxide |
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