CN102229436B - Preparation method of gamma-aluminium oxide (Al2O3) nanofiber - Google Patents
Preparation method of gamma-aluminium oxide (Al2O3) nanofiber Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000002121 nanofiber Substances 0.000 title claims abstract description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title abstract description 8
- 229910052593 corundum Inorganic materials 0.000 title abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 title abstract 2
- 239000012065 filter cake Substances 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 34
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 239000004411 aluminium Substances 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 12
- 238000004062 sedimentation Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- 238000010009 beating Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 2
- 229910003158 γ-Al2O3 Inorganic materials 0.000 abstract 2
- 238000004537 pulping Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000019994 cava Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention discloses a preparation method of gamma-aluminium oxide (Al2O3) nanofiber. The preparation method comprises the following steps of: (a) mixing aluminum-containing inorganic salt solution and alkaline precipitant solution according to the volume ratio of 1:(2-5) and reacting at the temperature of between 30 and 100 DEG C to obtain a suspension; (b) filtering the suspension to obtain a filter cake, and pulping and filtering in deionized water to remove impurities to obtain a filter cake I; (c) treating the filter cake I prepared in the step (b) in an organic solvent, and carrying out filtering and recovering the organic solvent to obtain a filter cake II; and (d) roasting the filter cake II prepared in the step (c) at the temperature of between 300 and 600 DEG C to obtain the gamma-Al2O3 nanofiber material. The preparation method is simple and can be applied to industry. The prepared gamma-Al2O3 has the characteristics of large aperture and large specific surface area.
Description
(1) technical field
The present invention relates to a kind of γ-Al
2O
3The material preparation method relates in particular to a kind of γ-Al
2O
3The preparations of nanomaterials method.
(2) background technology
γ-Al
2O
3Be a kind of support of the catalyst commonly used, be widely used in the various loaded catalysts of preparation.γ-Al
2O
3The character such as the specific surface area of carrier, aperture, pore volume and pattern have important impact to the activity and selectivity of catalyzer.To the pay attention to day by day that the bulky molecular catalysis such as biomass, heavy oil and residual oil transform, need urgently γ-Al along with people
2O
3Carrier has larger specific surface area (improving the dispersity of institute's loaded metal component) and aperture (improving the diffusion of macromolecular cpd in the duct), to improve the reactivity worth of catalyzer.But, γ-Al that existing market is on sale
2O
3Can't have simultaneously high specific surface area and larger aperture.Because for the ordinary oxide material, the raising of its specific surface area can be accompanied by aperture decline (A.Mart í nez, G.Prieto, J.Roll á n, J.Catal.263 (2009) 292-305) usually.Adopt the methods such as organic formwork agent, expanding agent can obtain all larger Al of specific surface area and aperture
2O
3Material, but these preparation process exist the shortcomings such as preparation process complexity, raw material costliness.Simultaneously, easily produce the obnoxious flavour of a large amount of sulfur-bearings, nitrogen in organic removal process of touching plate agent or expanding agent, be unfavorable for environment protection.Above these drawbacks limit these methods in industrial application.
(3) summary of the invention
But the technical problem to be solved in the present invention is to provide a kind of preparation of simple industrial application has wide aperture, bigger serface γ-Al
2O
3Novel method.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of γ-Al
2O
3The preparation method of nanofiber comprises the following steps:
(a) inorganic salt containing aluminium solution and alkaline sedimentation agent solution are mixed according to volume ratio 1: 2～5, in described inorganic salt containing aluminium solution, the mass percent of inorganic salt containing aluminium is 5～40%, in described alkaline sedimentation agent solution, the mass percent of water is 80-95%, reacts after mixing to obtain suspension liquid under 30～100 ℃ of conditions;
(b) the suspension liquid filtration is obtained filter cake, and then remove impurity by making beating, filtration step in deionized water, obtain filter cake I;
(c) will be processed in organic solvent again by the filter cake I that step (b) makes, and then filter, reclaim organic solvent and obtain filter cake II;
(d) will carry out calcination process at 300～600 ℃ by the filter cake II that step (c) makes, obtain γ-Al
2O
3Nano-fiber material.
In step of the present invention (a), we find, the temperature of precipitin reaction and the concentration of raw material have important impact to particle diameter and the structure of controlling precursor particle in this step reaction.By controlling these key factors in step (a), can obtain: (1) has the particle of appropriate particle size, thereby is conducive to filter and washing; (2) between particle, water content is lower, reduces roasting process and caves in because the surface tension phenomenon causes the hole.Therefore, the preferred aluminum nitrate of described inorganic salt containing aluminium and Tai-Ace S 150; In described inorganic salt containing aluminium solution, the mass percent of inorganic salt containing aluminium is 5～40%, is preferably 10～30%, more preferably 10～20%.The preferred aqueous sodium carbonate of described alkaline sedimentation agent solution, aqueous sodium hydroxide solution or ammonia soln, more preferably aqueous sodium carbonate.In preferred steps (a), the temperature of precipitin reaction is 60～100 ℃.
In step of the present invention (b), suspension liquid is filtered obtains filter cake, and then in deionized water by repeatedly pull an oar, the washing step such as filtration to be to remove impurity, can make through the specific surface area of roasting rear oxidation aluminium larger.
In step of the present invention (c), with an organic solvent to carrying out replacement Treatment by the water in step (a) and the precipitated filter cakes that (b) obtains, cause the hole to cave in further reduction roasting process due to the surface tension phenomenon and the phenomenon such as particle aggregation.Described organic solvent can be selected from following a kind of or several combination arbitrarily: methyl alcohol, ethanol, propyl alcohol, butanols.
In step of the present invention (d), preferably with filter cake II at 300-600 ℃ of lower roasting 2-6 hour.Preferred roasting condition was: 400 ℃ of roastings 5 hours.
Described γ-the Al of the concrete recommendation of the present invention
2O
3The preparation method of nanofiber carries out in accordance with the following steps:
(a) inorganic salt containing aluminium solution and alkaline sedimentation agent solution are mixed according to volume ratio 1: 2～5, react under 30～100 ℃ of conditions and obtain suspension liquid; Described inorganic salt containing aluminium solution is aluminum nitrate aqueous solution or aluminum sulfate aqueous solution, and in described inorganic salt containing aluminium solution, the mass percent of inorganic salt is 5～40%; Described alkaline sedimentation agent solution is aqueous sodium carbonate, aqueous sodium hydroxide solution or ammonia soln, and in described alkaline sedimentation agent solution, the mass percent of water is 80-95%;
(b) the suspension liquid filtration is obtained filter cake, and then remove impurity by making beating, filtration step in deionized water, obtain filter cake I;
(c) will be processed in organic solvent again by the filter cake I that step (b) makes, and then filter, reclaim organic solvent and obtain filter cake II; Described organic solvent is selected from following a kind of or several combination arbitrarily: methyl alcohol, ethanol, propyl alcohol, butanols;
The filter cake II that (d) will be made by step (c) obtained γ-Al at 300～600 ℃ of roasting 2-6 hours
2O
3Nano-fiber material.
The Al that the present invention makes
2O
3Material, particle are fibrous particle, and its crystal formation is the γ crystal formation; The material specific surface area is not less than 300m
2g
-1, pore volume is not less than 1.5cm
3g
-1, the aperture is not less than 10nm.
Compared with the prior art, the present invention has the following advantages:
(1) novel method of the present invention report pattern that is conducive to control aluminium oxide particles to form fibrous particle, forms larger aperture, the Al that makes by piling up between these particles
2O
3Material has bigger serface, wide-aperture characteristics.
(2) preparation process of the present invention's report does not need complicated equipment and exacting terms to control, and the raw material that uses is cheap, and the preparation process environmental friendliness is convenient to suitability for industrialized production.
(4) description of drawings
The TEM figure of the aluminum oxide that Fig. 1: embodiment 1 makes.
The XRD figure of the aluminum oxide that Fig. 2: embodiment 1 makes.
(5) embodiment
The below is described further technical scheme of the present invention with specific embodiment, but protection scope of the present invention is not subjected to the restriction of the following example.
Embodiment (1)
With 88 gram Al (NO
3)
39H
2O and 50 gram Na
2CO
3Be dissolved in respectively and be made into 15wt% and 6wt% solution in 250 and 750 ml deionized water, then with Al (NO
3)
3And Na
2CO
3Solution mixes under 95 ℃ of conditions and carries out precipitin reaction.Resulting suspension liquid is filtered obtain filter cake, with deionized water, filter cake is washed, and then filter.Through repeatedly the washing and filtration treatment after, with ethanol, filter cake is processed.After filtration, reclaim ethanol after, resulting filter cake is obtained Al through 400 ℃ of roastings after 5 hours
2O
3Sample.Fig. 1 is TEM figure, shows to exist nanometer fibrous particle.Fig. 2 is XRD figure, shows that this material is γ-Al
2O
3
Embodiment (2)
With 78 gram Al
2(SO
4)
318H
2O and 50 gram Na
2CO
3Be dissolved in respectively and be made into 12wt% and 6wt% solution in 250 and 750 ml deionized water, then with Al
2(SO
4)
3And Na
2CO
3Solution mixes under 95 ℃ of conditions and carries out precipitin reaction.Resulting suspension liquid is filtered obtain filter cake, with deionized water, filter cake is washed, and then filter.After repeatedly washing and filtering, with ethanol, precipitated filter cakes is processed.After filtration, reclaim ethanol after, resulting filter cake is obtained Al through 400 ℃ of roastings after 5 hours
2O
3Sample.
Embodiment (3)
With 17.7 gram Al (NO
3)
39H
2O and 10 gram Na
2CO
3Be dissolved in respectively and be made into 15wt% and 6wt% solution in 50 and 150 ml deionized water, then with Al (NO
3)
3And Na
2CO
3Solution mixes at ambient temperature and carries out precipitin reaction.Resulting suspension liquid is filtered obtain filter cake, with deionized water, filter cake is washed, and then filter.After repeatedly washing and filtering, with ethanol, precipitated filter cakes is processed.After filtration, reclaim ethanol after, resulting filter cake is obtained Al through 400 ℃ of roastings after 5 hours
2O
3Sample.
Embodiment (4)-----F-T building-up reactions
Prepare CoRu/Al take the aluminum oxide of embodiment 1 preparation and commercial aluminum oxide (seeing Table 1) as carrier respectively
2O
3Catalyzer.
Catalyst preparation step: with 4.2 gram Co (NO
3)
26H
2O and 0.14 gram Ru (NO) (NO
3)
3And polyoxyethylene glycol (molecular weight 400 2vol%) joins 120cm under the condition of vigorous stirring
3In methyl alcohol and water mixed solution (the mixed volume ratio is 3: 1).After reaction 2h under 90 ℃, with 3 gram Al
2O
3Carrier joins in formed colloidal sol, and continues vigorous stirring.After evaporating solvent under 100 ℃ of conditions, can make the presoma of cobalt metal and ruthenium load to Al
2O
3On carrier, and obtain the colloidal solid material.The roasting under 400 ℃ of conditions of this colloidal solid material was obtained CoRuO in 4 hours
x/ Al
2O
3Catalyzer.At last, pass through H
2Reduction can prepare CoRu/Al
2O
3Catalyzer (Co=22wt.%, (Ru/Co)
at.=0.03).
By fixed-bed reactor, the synthetic performance of the F-T of catalyzer has been carried out evaluation test.Reaction conditions is 210 ℃, 2000KPa, H
2/ CO=2.With N
2As interior mark, by gas-chromatography to CO, N
2, CH
4, CO
2Carry out online qualitative and quantitative analysis Deng gas-phase product.Test-results shows, under the chemical constitution prerequisite identical with reaction conditions, the aluminum oxide by embodiment 1 preparation is that the catalyzer of carrier preparation has higher CO conversion rate (h than the catalyzer of the preparation take commercial aluminum oxide as carrier
-1).
Table 1: the texture data of alumina material
Table 2:CoRu/Al
2O
3The F-T building-up reactions performance of catalyzer
CO conversion rate (the per hour CO mole number of every mole metal cobalt conversion)
Claims (7)
1. γ-Al
2O
3The preparation method of nanofiber comprises the following steps:
(a) inorganic salt containing aluminium solution and alkaline sedimentation agent solution are mixed according to volume ratio 1:2 ~ 5, in described inorganic salt containing aluminium solution, the mass percent of inorganic salt containing aluminium is 5 ~ 40%, in described alkaline sedimentation agent solution, the mass percent of water is 80 ~ 95%, reacts after mixing to obtain suspension liquid under 30 ~ 100 ℃ of conditions; Described alkaline sedimentation agent solution is aqueous sodium carbonate;
(b) the suspension liquid filtration is obtained filter cake, and then remove impurity by making beating, filtration step in deionized water, obtain filter cake I;
(c) will be processed in organic solvent again by the filter cake I that step (b) makes, and then filter, reclaim organic solvent and obtain filter cake II;
(d) will be carried out calcination process 2-6 hour at 300 ~ 600 ℃ by the filter cake II that step (c) makes, obtain γ-Al
2O
3Nano-fiber material.
2. γ-Al as claimed in claim 1
2O
3The preparation method of nanofiber is characterized in that: the described inorganic salt containing aluminium solution of step (a) is aluminum nitrate aqueous solution or aluminum sulfate aqueous solution.
3. γ-Al as claimed in claim 2
2O
3The preparation method of nanofiber is characterized in that: in the described inorganic salt containing aluminium solution of step (a), the mass percent of inorganic salt containing aluminium is 10 ~ 30%.
4. γ-Al as claimed in claim 1
2O
3The preparation method of nanofiber is characterized in that: the temperature of reaction in step (a) is 60 ~ 100 ℃.
5. γ-Al as claimed in claim 1
2O
3The preparation method of nanofiber is characterized in that: the described organic solvent of step (c) is selected from following a kind of or several combination arbitrarily: methyl alcohol, ethanol, propyl alcohol, butanols.
6. γ-Al as claimed in claim 1
2O
3The preparation method of nanofiber is characterized in that: the described maturing temperature of step (d) is 400 ℃, and roasting time is 5 hours.
7. γ-Al as claimed in claim 1
2O
3The preparation method of nanofiber is characterized in that: described preparation method carries out in accordance with the following steps:
(a) inorganic salt containing aluminium solution and alkaline sedimentation agent solution are mixed according to volume ratio 1:2 ~ 5, react under 30 ~ 100 ℃ of conditions and obtain suspension liquid; Described inorganic salt containing aluminium solution is aluminum nitrate aqueous solution or aluminum sulfate aqueous solution, and in described inorganic salt containing aluminium solution, the mass percent of inorganic salt containing aluminium is 5 ~ 40%; In described alkaline sedimentation agent solution, the mass percent of water is 80-95%;
(b) the suspension liquid filtration is obtained filter cake, and then remove impurity by making beating, filtration step in deionized water, obtain filter cake I;
(c) will be processed in organic solvent again by the filter cake I that step (b) makes, and then filter, reclaim organic solvent and obtain filter cake II; Described organic solution is selected from following a kind of or several combination arbitrarily: methyl alcohol, ethanol, propyl alcohol, butanols;
The filter cake II that (d) will be made by step (c) obtained γ-Al at 300 ~ 600 ℃ of roasting 2-6 hours
2O
3Nano-fiber material.
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| Title |
|---|
| 魏蕾.超细γ-Al2O3的制备、表征及其在羰基硫水解反应中的应用.《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》.2006,(第8期),18-20,24-39,45. * |
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