CN103112878A - Method for preparing aluminum oxide with large specific surface area - Google Patents
Method for preparing aluminum oxide with large specific surface area Download PDFInfo
- Publication number
- CN103112878A CN103112878A CN2012105876624A CN201210587662A CN103112878A CN 103112878 A CN103112878 A CN 103112878A CN 2012105876624 A CN2012105876624 A CN 2012105876624A CN 201210587662 A CN201210587662 A CN 201210587662A CN 103112878 A CN103112878 A CN 103112878A
- Authority
- CN
- China
- Prior art keywords
- aluminum oxide
- liquor
- crystallization
- solution
- ammoniacal liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a method for preparing aluminum oxide. The method is characterized by comprising the following steps of: dissolving aluminum oxide solid in 0.1-0.5mol/L lauroyl sodium glutamate aqueous liquor to obtain 1-5mol/L aluminum chloride liquor; adding ammonia water or mixed liquor of ammonia water and organic amine into the aluminum chloride liquor, and adjusting pH value to 7-8 so as to obtain Al<3+>:OH<-> in the liquid; standing the liquor for 3-5hours at 20-50 DEG C by lauroyl glutamate ions, wherein the molar ratio is 1: (0.05-3): (1.5-7.5); crystallizing the liquor after standing in a reaction kettle at 100-140 DEG C for 24-96hours; and filtering and washing the crystallizing liquid and roasting in a muffle furnace at 500-700 DEG C for 4-6 hours to obtain solid aluminum oxide. The specific surface area of gamma-aluminum oxide can reach 240-400<m2>/g.
Description
Technical field
The present invention relates to inorganic synthetic and Application Areas, specifically, the present invention relates to a kind of preparation method of aluminum oxide of high-specific surface area.
Background technology
Aluminum oxide is widely used in the every field such as machinery, metallurgy, oil, chemical industry, electronics, optics, aerospace owing to possessing excellent physical and chemical performance.Aspect Industrial Catalysis, aluminum oxide is a kind of good support of the catalyst especially, but, the shortcoming such as pore volume little, mean pore size larger little due to specific surface area makes it seriously restrict it as the catalytic effect of carrier.
At present, the preparation method of aluminum oxide mainly contains following several: sol-gel method; Carbonic acid decomposition method and neutralisation.Patent CN 102515232A discloses a kind of preparation method of aluminum oxide, the method utilizes sol-gel method to prepare the aluminium hydroxide superfine crystal powder of bigger serface, obtain the spherical powder of ultra-fine a-aluminum oxide after calcining, but because the aluminium source of using is the organo-aluminium alcoholates such as aluminum ethylate, price is comparatively expensive, so production cost is higher.Patent CN 101774618A discloses the preparation method of another aluminum oxide, and the method is utilized using sodium bicarbonate to decompose sodium aluminate solution, and the aluminum oxide specific surface area that makes is up to 201m
2/ g, pore volume are 0.32cm
3/ g, mean pore size is 3.27nm; The method technique is simple, and is easy to operate, but that shortcoming is specific surface area is less than normal, and raw material sodium metaaluminate price is higher, and cost is high.Patent CN 101993102A discloses the preparation method of another aluminum oxide, and the method adopts the acid-base neutralisation method of sodium metaaluminate and aluminum chloride, and the aluminum oxide specific surface area that makes is up to 315.9m
2/ g, pore volume are 0.29cm
3/ g, the aperture is 3.95nm, but that shortcoming is sodium metaaluminate is expensive, production cost is higher.
Summary of the invention
In order to solve the problem of prior art, it is the aluminium source that the present invention adopts inorganic aluminate aluminum chloride, adopts the preparation of sol-gel and hydrothermal method to have the alumina supporter of high-specific surface area.
The inventive method comprises the steps:
A) under 20-50 ℃, aluminum chloride solids is dissolved in the sodium lauroyl glutamate aqueous solution that concentration is 0.1-0.5mol/L, obtain the liquor alumini chloridi of 1-5mol/L;
B) add the mixing solutions of ammoniacal liquor or ammoniacal liquor and organic amine in liquor alumini chloridi, the adjusting pH value is 7-8, makes Al in solution
3+: OH
-: the mol ratio of lauroyl glutamate radical ion is 1:0.05-3:1.5-7.5; Under 20-50 ℃ with the standing 3-5h of mentioned solution;
C) with the crystallization in reactor of the solution after standing, crystallization temperature is 100-140 ℃, and crystallization time is 24-96h;
D) the gained crystallization liquid is filtered, washs, roasting in the retort furnace of 500-700 ℃, roasting time is 4-6h, obtains solid alumina.
In the methods of the invention, in step a), the concentration of the sodium lauroyl glutamate aqueous solution is preferably 0.276-0.414mol/L, and the concentration of liquor alumini chloridi is preferably 1-2mol/L.
In step b), preferably at the mixing solutions that continues to add under stirring ammoniacal liquor or ammoniacal liquor and organic amine, churning time is preferably 1-2h;
Wherein, the massfraction of described ammoniacal liquor is 10%-25%; Organic amine can be ethamine, quadrol, propylamine, one or more in oxammonium hydrochloride;
Wherein, Al in solution
3+: OH
-: the mol ratio of lauroyl glutamate radical ion is preferably 1:0.5-1:1.5-2.0, more preferably 1:0.58:1.75.
In step c), described reactor preferably adopts the tetrafluoroethylene reactor, and crystallization temperature is preferably 100-120 ℃, and crystallization time is preferably 48-72 hour.
In step d), maturing temperature is preferably 550 ℃, and roasting time is preferably 4 hours.
The aluminum oxide specific surface area that makes by the inventive method can reach 240-400m
2/ g.
The inventive method has following beneficial effect: the advantages such as employing collosol and gel and hydrothermal synthesis method prepare aluminum oxide, possess technique simple, and be easy to operate, and production cost is low, and above-mentioned steps all obtains the aluminum oxide of bigger serface, and pore volume reaches 0.4-0.6cm
3/ g; The amino acid type surfactant sodium lauroyl glutamate that adopts belongs to environmentally friendly catalyzer, has the characteristics such as degraded is rapid, safety.
The method for preparing the large specific surface aluminum oxide provided by the invention has significant advantage than prior art, and the aluminum oxide that makes is with a wide range of applications in catalytic field, fractionation by adsorption field.
Embodiment
Following examples will help further to explain the present invention, but be not used in restriction content of the present invention.
In the present invention, agents useful for same is the commercially available prod.
Embodiment one
Take the 11.64g sodium lauroyl glutamate under 35 ℃, be dissolved in the 120ml deionized water and form micella, slowly add 4.6g aluminum chloride.Be that 25wt.% ammoniacal liquor regulator solution PH is 7 with massfraction, under 35 ℃ aging 5 hours, in its crystallization still of packing into, 100 ℃ of crystallization 72 hours, product was after suction filtration, washing, drying, 600 ℃ of lower roastings 4 hours, obtain aluminum oxide, specific surface area is 280m
2/ g, pore volume are 0.47cm
3/ g, mean pore size is 4.2nm.
Embodiment two
Take the 11.64g sodium lauroyl glutamate under 25 ℃, be dissolved in the 80ml deionized water and form micella, slowly add 4.6g aluminum chloride.Be that 25wt.% ammoniacal liquor regulator solution PH is 7 with massfraction, under 25 ℃ aging 3 hours, in its crystallization still of packing into, 100 ℃ of crystallization 72 hours, product was after suction filtration, washing, drying, 550 ℃ of lower roastings 4 hours, obtain aluminum oxide, specific surface area is 240m
2/ g, pore volume are 0.4cm
3/ g, mean pore size is 3.7nm.
Embodiment three
Take the 11.64g sodium lauroyl glutamate under 40 ℃, be dissolved in the 120ml deionized water and form micella, slowly add 4.6g aluminum chloride.The mixing solutions regulator solution PH that is 10wt.% ammoniacal liquor and oxammonium hydrochloride with massfraction is 7, under 40 ℃ aging 4 hours, in its reactor of packing into, 120 ℃ of crystallization 48 hours, product is after suction filtration, washing, drying, and 600 ℃ of lower roastings 4 hours, obtaining the aluminum oxide specific surface area was 285m
2/ g, pore volume are 0.48cm
3/ g, mean pore size is 4.4nm.
Embodiment four
Take the 11.64g sodium lauroyl glutamate under 30 ℃, be dissolved in the 80ml deionized water and form micella, slowly add 4.6g aluminum chloride.Mixing solutions regulator solution PH with massfraction 10wt.% ammoniacal liquor and diethylamine is 7, under 30 ℃ aging 5 hours, in its reactor of packing into, 120 ℃ of crystallization 48 hours, product was after suction filtration, washing, drying, 550 ℃ of lower roastings 4 hours, obtain aluminum oxide, specific surface area is 310m
2/ g, pore volume are 0.51cm
3/ g, mean pore size is 3.86nm.
Comparative Examples one
Under 70 ° of C, 400rpm continue to stir, to the NaAlO of the 4.0mol/L of 30ml
2(contain CTAB, i.e. cetyl trimethylammonium bromide 21.6g) in solution, add the NaHCO of 1.2mol/L
3Solution 330ml controls NaHCO
3: NaAlO
2Mass ratio is 1.1:1.Constant temperature stirs 6h, filters and washs, and the gained solid is calcined 3h in 650 ° of C retort furnaces, make aluminum oxide, and specific surface area is 201.1m
2/ g, pore volume are 0.32cm
3/ g, mean pore size is 3.27nm.
Comparative Examples two
Under 60 ° of C, 600rpm continue to stir, to the NaAlO of the 0.5mol/L of 150ml
2In solution, slowly add the AlCl of 60ml0.5mol/L
3Solution, the molecular ratio of controlling two kinds of aluminium salt is 2.5:1, when PH=11, add 4.2g template methylcellulose gum powder (concentration is 20g/L), constant temperature stirs 1h, 80 ° of C ageing 1h, vacuum filtration, washing, 150 ° of dry 6h of C, at 500 ° of C calcining 4h, obtain aluminum oxide, specific surface area is 212.1m
2/ g, pore volume are 0.29cm
3/ g, mean pore size is 363nm.
Claims (10)
1. a method for preparing aluminum oxide, is characterized in that, comprises the steps:
A) under 20-50 ℃, aluminum chloride solids is dissolved in the sodium lauroyl glutamate aqueous solution that concentration is 0.1-0.5mol/L, obtain the liquor alumini chloridi of 1-5mol/L;
B) add the mixing solutions of ammoniacal liquor or ammoniacal liquor and organic amine in liquor alumini chloridi, the adjusting pH value is 7-8, makes Al in solution
3+: OH
-: the mol ratio of lauroyl glutamate radical ion is 1:0.05-3:1.5-7.5; Under 20-50 ℃ with the standing 3-5h of mentioned solution;
C) with the crystallization in reactor of the solution after standing, crystallization temperature is 100-140 ℃, and crystallization time is 24-96h;
D) the gained crystallization liquid is filtered, washs, roasting in the retort furnace of 500-700 ℃, roasting time is 4-6h, obtains solid alumina.
2. method according to claim 1, is characterized in that, in step a), the concentration of the sodium lauroyl glutamate aqueous solution is 0.276-0.414mol/L.
3. method according to claim 2, is characterized in that, the concentration of step a) liquor alumini chloridi is 1-2mol/L.
4. method according to claim 1, is characterized in that, in step b), at the mixing solutions that continues to add under stirring ammoniacal liquor or ammoniacal liquor and organic amine, churning time is 1-2h.
5. method according to claim 4, is characterized in that, in step b), the massfraction of described ammoniacal liquor is 10%-25%.
6. method according to claim 5, is characterized in that, in step b), organic amine is ethamine, quadrol, propylamine, one or more in oxammonium hydrochloride.
7. method according to claim 6, is characterized in that, Al in the solution of step b)
3+: OH
-: the mol ratio of lauroyl glutamate radical ion is 1:0.5-1:1.5-2.0.
8. method according to claim 1, is characterized in that, in step c), described reactor adopts the tetrafluoroethylene reactor, and crystallization temperature is 100-120 ℃, and crystallization time is 48-72 hour.
9. method according to claim 1, is characterized in that, in step d), maturing temperature is 550 ℃, and roasting time is 4 hours.
10. according to claim 1-9 described methods of any one, is characterized in that, prepared aluminum oxide specific surface area is 240-400m
2/ g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105876624A CN103112878A (en) | 2012-12-28 | 2012-12-28 | Method for preparing aluminum oxide with large specific surface area |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105876624A CN103112878A (en) | 2012-12-28 | 2012-12-28 | Method for preparing aluminum oxide with large specific surface area |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103112878A true CN103112878A (en) | 2013-05-22 |
Family
ID=48411287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105876624A Pending CN103112878A (en) | 2012-12-28 | 2012-12-28 | Method for preparing aluminum oxide with large specific surface area |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103112878A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289229A (en) * | 2014-10-27 | 2015-01-21 | 北京碧水源环境工程有限公司 | Preparation method for load transition metal catalyst for ozone oxidation as well as load transition metal catalyst and application thereof |
| CN107540007A (en) * | 2016-06-29 | 2018-01-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of nano-sheet meso-porous alumina |
| CN111589449A (en) * | 2020-06-18 | 2020-08-28 | 南京工业大学 | Cobalt-based catalyst for propane dehydrogenation, preparation method and application |
| CN112707420A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Alumina material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597077A (en) * | 2009-07-09 | 2009-12-09 | 南开大学 | A kind of synthetic method of meso-porous alumina |
| CN101863501A (en) * | 2010-04-27 | 2010-10-20 | 中国神华能源股份有限公司 | Method for producing superfine aluminum hydroxide and aluminum oxide by using solution of aluminum chloride |
-
2012
- 2012-12-28 CN CN2012105876624A patent/CN103112878A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597077A (en) * | 2009-07-09 | 2009-12-09 | 南开大学 | A kind of synthetic method of meso-porous alumina |
| CN101863501A (en) * | 2010-04-27 | 2010-10-20 | 中国神华能源股份有限公司 | Method for producing superfine aluminum hydroxide and aluminum oxide by using solution of aluminum chloride |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104289229A (en) * | 2014-10-27 | 2015-01-21 | 北京碧水源环境工程有限公司 | Preparation method for load transition metal catalyst for ozone oxidation as well as load transition metal catalyst and application thereof |
| CN107540007A (en) * | 2016-06-29 | 2018-01-05 | 中国科学院大连化学物理研究所 | A kind of preparation method of nano-sheet meso-porous alumina |
| CN112707420A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Alumina material and preparation method thereof |
| CN111589449A (en) * | 2020-06-18 | 2020-08-28 | 南京工业大学 | Cobalt-based catalyst for propane dehydrogenation, preparation method and application |
| CN111589449B (en) * | 2020-06-18 | 2022-05-03 | 南京工业大学 | Cobalt-based catalyst for propane dehydrogenation, preparation method and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6276257B2 (en) | Y-type zeolite containing rare earth and method for producing the same | |
| CN101704538B (en) | Hydrothermal method for preparing series of special-shaped graded pseudo-boehmite | |
| CN102583467B (en) | Method for using hydrotalcite-like substance with low zinc-aluminum molar ratio as precursor to manufacture zinc-aluminum spinel | |
| CN1666956A (en) | Method for synthesizing nanometer size mordenite | |
| CN107758715B (en) | Method for preparing high-crystallinity high-purity pseudo-boehmite | |
| CN103466669B (en) | Method of using aluminium hydroxide to make pseudo-boehmite in hydrothermal synthesis mode | |
| CN102698785A (en) | Preparation method of diatomite-loaded nitrogen-doped nanometer TiO2 photocatalysis material | |
| CN103112878A (en) | Method for preparing aluminum oxide with large specific surface area | |
| CN104043477A (en) | ZSM-5/MCM-48 composite molecular sieve, preparation method and application thereof | |
| CN101993102A (en) | Method for inorganically synthesizing organized mesoporous alumina | |
| CN102910654A (en) | Preparation method of fibrous boehmite with large specific surface area and large pore area | |
| CN102464326B (en) | Method for synthesizing high-silicon mordenite | |
| CN106186014B (en) | A kind of mesoporous γ-Al2O3 synthetic method of function admirable | |
| CN112642427B (en) | Metal M doped titanium dioxide photocatalyst and application thereof in photocatalytic nitrogen fixation | |
| JP5802124B2 (en) | Method for producing mesoporous alumina | |
| CN101269829B (en) | Gamma-AL2O3 material with large specific surface area and preparing method thereof | |
| CN106276992A (en) | A kind of preparation method of foliaceous nanometer gama-alumina | |
| CN102674390A (en) | Method for directly synthesizing heteroatom substituted multistage ordered mesoporous molecular sieve | |
| CN109179429B (en) | Method for preparing mesoporous nano-silica from chlorosilane residual liquid | |
| JP2021151942A (en) | Porous silica alumina particles and method for producing the same | |
| CN102963925A (en) | Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor | |
| CN106219582B (en) | A kind of preparation method for holding γ-Al2O3 with super large mesoporous hole | |
| CN104891541A (en) | Method for preparing flaky alpha alumina with ammonium aluminum carbonate hydroxide pyrolysis method | |
| CN105217677B (en) | A kind of method preparing titanium nanotube for template with attapulgite clay | |
| CN103288114A (en) | Preparation method of high-purity aluminum oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130522 |