CN106186014A - A kind of mesoporous γ Al2O3 synthetic method of function admirable - Google Patents
A kind of mesoporous γ Al2O3 synthetic method of function admirable Download PDFInfo
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- CN106186014A CN106186014A CN201610578868.9A CN201610578868A CN106186014A CN 106186014 A CN106186014 A CN 106186014A CN 201610578868 A CN201610578868 A CN 201610578868A CN 106186014 A CN106186014 A CN 106186014A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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Abstract
The present invention provides a kind of synthesising mesoporous γ Al2O3Method, with inorganic cation aluminium salt and NaAlO2For aluminum source, with triblock polymer Pluronic P123 as structure directing agent, under room temperature, pass through Al3+And AlO2 ‑The hydrolysis self carried out is to prepare mesoporous γ Al2O3, reaction required time is short and operating procedure is simple.The mesoporous γ Al that this method synthesizes2O3, specific surface area is up to 452m2/ g, pore volume is up to 1.55cm3/ g, aperture is at about 10nm, and meso-hole structure can keep stable more than 550 DEG C of roasting temperatures, and gained mesoporous aluminum oxide material mechanical strength is big, is suitable as catalyst carrier.
Description
Technical field
The present invention relates to a kind of mesoporous γ-Al2O3Preparation method.More specifically, it is a kind of with inorganic cation aluminum
Salt and NaAlO2For aluminum source, prepare mesoporous γ-Al with Pluronic P123 for structure directing agent2O3Method.
Background technology
The crystal formation of aluminium oxide abundant (amorphous, α phase, β phase, γ phase, δ are equal), cheap and easy to get, have good physico
Learn character (heat stability, chemical stability, mechanical stability), be a kind of important catalyst carrier and adsorbent, in industry
On be used widely.Meso-porous alumina, as the alumina material that a class is novel, except the physics with common alumina material
Outside chemical characteristic, also there is bigger serface, big pore volume, excellent pore passage structure, have important in catalysis, adsorbing domain
Using value.
1996, Pinnavaia et al. reported first successfully synthesized heat-staple meso-porous alumina.The whole world is respectively ground
Study carefully group and extensively carry out the study on the synthesis of meso-porous alumina.On the whole, conventional meso-porous alumina synthetic method has following several
Kind:
(1) aluminum isopropylate. is dissolved in the mixed solvent of isopropanol or isopropanol and water by solvent-thermal process method: Gan etc.,
After addition toluene in rustless steel autoclave, 150～190 DEG C of reaction 20h obtain meso-porous alumina.Solvent-thermal process method is grasped
Make simple, the shortest, reproducible, but need to use organic solvent, environment is unfriendly, relatively costly.Meanwhile, synthesis condition is relatively
, there is certain potential safety hazard in harshness.
(2) sol-gel process: by surfactant dissolve form vitreosol in a solvent, be sequentially added aluminum source and
His reagent, is aged after stirring and dissolving.Colloidal sol is changed into gel after fully ageing, gel is carried out post processing and i.e. obtains mesoporous oxygen
Change aluminum.Sol-gel process method safety is easy, but manufacturing cycle is relatively long, and repeatability is poor.
(3) sedimentation method: the sedimentation method use aluminum source and precipitant to react generation colloidal sol or gel to prepare meso-porous alumina.Heavy
Shallow lake method is faster than sol-gel process, operates safety, it is easy to industry is amplified, but the meso-porous alumina specific surface area obtained is relatively small,
Structural behaviour is relatively poor.
Although recent two decades comes, the synthesis of meso-porous alumina achieves bigger progress.But major part synthetic method is general
Needing to use expensive and poisonous alkyl aluminum as aluminum source, producing cost is high, big to operator's actual bodily harm.Some needs
Time-consumingly, complicated hydrolysis and pH value regulation process so that the production cycle is long, severe reaction conditions.
In method disclosed in CN 101993102 A, researcher does template with methylcellulose, with sodium silicate and chlorination
Aluminum prepares siliceous meso-porous alumina, and gained precipitation to be aged through constant temperature.In method disclosed in CN 102219242 A,
Researcher does template with P123, utilizes inorganic aluminate and ammonia or ammonium salt to prepare meso-porous alumina, and P123 is initially and aluminium salt
Solution is dissolved in together, and rear addition ammonia or ammonium salt solution regulate pH value and produce precipitation.Said method have employed inorganic aluminum source
Preparing meso-porous alumina, it is to avoid the use in alkyl aluminum source, but the pore volume of obtained meso-porous alumina is less, specific surface area is not
High.
Summary of the invention
Present invention aim to address that prior art cost is high, operating procedure is complicated and gained mesoporous γ-Al2O3Pore volume is little
Problem, develop a kind of low cost, the easy high-specific surface area of preparation method, big pore volume mesoporous γ-Al2O3Synthetic method.
The present invention provides a kind of synthesising mesoporous γ-Al2O3Method, with inorganic cation aluminium salt and NaAlO2For aluminum source, with
Pluronic P123 is to pass through Al under structure directing agent, room temperature3+And AlO2 -The hydrolysis self carried out to prepare mesoporous γ-
Al2O3, reaction required time is short and operating procedure is simple.Mesoporous γ-the Al that this method synthesizes2O3, specific surface area up to
452m2The high specific surface area of/g, pore volume is up to 1.55cm3/ g, aperture is at about 10nm, and meso-hole structure is more than 550 DEG C of temperature
Lower roasting can keep stable, and gained mesoporous aluminum oxide material mechanical strength is big, is suitable as catalyst carrier.
Typical synthesis step is: respectively by AlCl3·6H2O and NaAlO2It is dissolved in appropriate amount of deionized water, and stirs 1h,
P123 is joined stirring 1h in appropriate amount of deionized water simultaneously, forms P123 solution.At room temperature and flow mixing AlCl3With
NaAlO2Solution, controls AlO2 -And Al3+Mol ratio regulate the pH value of mixed system, stir 2h.Also stream is mixed to get
Precipitation sucking filtration, washing, obtain the aluminum hydroxide precipitation cleaned.Aluminum hydroxide precipitation is redispersed in P123 solution, mechanical agitation
2h.It is dried 12h in the aluminum hydroxide precipitation of mix homogeneously and the solution combined thing of P123 are placed on baking oven.Dried complex exists
Muffle furnace is warming up to uniform temperature, constant temperature calcining a period of time with the heating rate of 2 DEG C/min, obtains purpose product mesoporous
γ-Al2O3.Compared with former preparation method, present invention have the advantage that
(1) present invention is at room temperature carried out at alumina precursor synthesis phase, and energy consumption is low.
(2) present invention uses cheap, nontoxic inorganic aluminate AlCl3And NaAlO2, avoid the alkane that price is higher and poisonous
The use of base aluminum.
(3) present invention is by controlling Al in precipitation3+And AlO2 -Mol ratio carry out control ph, pH value regulation process
Simply, and precipitation speed is fast.
Accompanying drawing explanation
Fig. 1 embodiment 1 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Fig. 2 embodiment 1 roasting2O3XRD wide-angle diffraction figure.
Fig. 3 embodiment 2 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Fig. 4 embodiment 2 roasting2O3XRD wide-angle diffraction figure.
Fig. 5 embodiment 3 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Fig. 6 embodiment 3 roasting2O3XRD wide-angle diffraction figure.
Fig. 7 embodiment 4 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Fig. 8 embodiment 4 roasting2O3XRD wide-angle diffraction figure.
Fig. 9 embodiment 5 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Figure 10 embodiment 5 roasting2O3XRD wide-angle diffraction figure.
Figure 11 embodiment 6 gained mesoporous γ-Al2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Gained mesoporous γ-Al after Figure 12 embodiment 6 roasting2O3XRD wide-angle diffraction figure.
Detailed description of the invention
It is described in conjunction with the embodiments the detailed description of the invention of the present invention, but is not limited only to this, the P123 used in the present embodiment
Being the product of SIGMA-ALDRICH company, molecular weight is 5800.
Embodiment 1:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 2.78 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration,
Washing, obtains aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 29, and mechanical agitation 2 is little
Time.Being placed in by the complex stirred in 100 DEG C of baking ovens and be dried 12h, dried complex proceeds in Muffle furnace, with 2 DEG C/
The heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Fig. 12Adsorption and desorption isotherms and pore-size distribution
Curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 400.9m2/ g, pore volume is
1.43cm3/ g, aperture concentrates on 10.8nm.The material being understood preparation by the XRD spectra in Fig. 2 is γ-Al2O3Crystalline phase.
Embodiment 2:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 2.78 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration,
Washing, obtains aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 22.7, mechanical agitation 2
Hour.Being dried 12h in the complex stirred is placed in 100 DEG C of baking ovens, dried complex proceeds in Muffle furnace, with 2
DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Fig. 32Adsorption and desorption isotherms and aperture
Distribution curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 421.9m2/ g, pore volume is
1.56cm3/ g, aperture concentrates on 9.4nm.The material being understood preparation by the XRD spectra in Fig. 4 is γ-Al2O3Crystalline phase.
Embodiment 3:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 2.56 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration,
Washing, obtains aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 38.7, mechanical agitation 2
Hour.Being dried 12h in the complex stirred is placed in 100 DEG C of baking ovens, dried complex proceeds in Muffle furnace, with 2
DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Fig. 52Adsorption and desorption isotherms and aperture
Distribution curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 400.3m2/ g, pore volume is
1.38cm3/ g, aperture concentrates on 9.7nm.The material being understood preparation by the XRD spectra in Fig. 6 is γ-Al2O3Crystalline phase.
Embodiment 4:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 2.56 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration,
Washing, obtains aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 23.2, mechanical agitation 2
Hour.Being dried 12h in the complex stirred is placed in 100 DEG C of baking ovens, dried complex proceeds in Muffle furnace, with 2
DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Fig. 72Adsorption and desorption isotherms and aperture
Distribution curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 438.3m2/ g, pore volume is
1.44cm3/ g, aperture concentrates on 9.5nm.The material being understood preparation by the XRD spectra in Fig. 8 is γ-Al2O3Crystalline phase.
Embodiment 5:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 2.56 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration,
Washing, obtains aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 23.2, mechanical agitation 2
Hour.Being dried 12h in the complex stirred is placed in 100 DEG C of baking ovens, dried complex proceeds in Muffle furnace, with 2
DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Fig. 92Adsorption and desorption isotherms and aperture
Distribution curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 452.3m2/ g, pore volume is
1.39cm3/ g, aperture concentrates on 9.2nm.The material being understood preparation by the XRD spectra in Figure 10 is γ-Al2O3Crystalline phase.
Embodiment 6:
At room temperature, will be containing NaAlO2Solution with containing AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub
You 3 and flow mixing by ratio, produce white precipitate, and gained mixture is stirred at room temperature 2 hours.Mixture is carried out sucking filtration, washes
Wash, obtain aluminum hydroxide precipitation, precipitation is redispersed in Al3+/ P123 mol ratio is the P123 solution of 23.2, and mechanical agitation 2 is little
Time.Being placed in by the complex stirred in 100 DEG C of baking ovens and be dried 12h, dried complex proceeds in Muffle furnace, with 2 DEG C/
The heating rate of min is warming up to 550 DEG C, 550 DEG C of constant temperature calcinings 2 hours.By the N in Figure 112Adsorption and desorption isotherms divides with aperture
Cloth curve understands this γ-Al2O3For mesoporous material, the mesoporous γ-Al of gained2O3Specific surface area is 401.2m2/ g, pore volume is
1.20cm3/ g, aperture concentrates on 8.8nm.The material being understood preparation by the XRD spectra in Figure 12 is γ-Al2O3Crystalline phase.
Claims (8)
1. the mesoporous γ-Al of a function admirable2O3Synthetic method, has steps of:
(1) respectively by cation aluminium salt and NaAlO2It is dissolved in appropriate amount of deionized water, and stirs 1h；P123 is joined and goes in right amount
Ionized water stirs 1h, forms P123 solution；
(2) under room temperature and flow mixed-cation aluminium salt and NaAlO2Solution, the mol ratio controlling zwitterion aluminum source regulates mixing
The pH value of liquid, stirs 2h afterwards；
(3) the precipitated product sucking filtration that step (2) obtained, washing, obtain the aluminum hydroxide precipitation cleaned, by aluminum hydroxide precipitation
It is redispersed in P123 solution, mechanical agitation 2h；
(4) it is dried 12h in the aluminum hydroxide precipitation of mix homogeneously and the solution combined thing of P123 are placed on baking oven；
(5) dried complex is warming up to uniform temperature, constant temperature calcining one section with the heating rate of 2 DEG C/min in Muffle furnace
Time, obtain purpose product mesoporous γ-Al2O3。
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: the cation described in step (1)
Aluminium salt is aluminum nitrate, aluminum chloride, aluminum sulfate, one or more in aluminium potassium sulfate etc..
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: step (2) described AlO2 -With
Al3+Mol ratio in 2.56～3 scopes, carry out and flow hybrid reaction.
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: P123 solution in step (3),
Al3+With the mol ratio of P123 in the range of 22.7～38.7.
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: step (3) is at aluminium hydroxide
After precipitation sucking filtration, washing, it is redispersed in P123 solution, carries out mechanical agitation.
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: step (4) is will be containing certain
The complex of amount deionized water, carries out moisture evaporation drying in the baking oven of 80～140 DEG C.
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: the roasting employed in step (5)
Burning temperature is 400～700 DEG C, roasting 2～48h.
Mesoporous γ-Al the most according to claim 12O3Synthetic method, it is characterised in that: the spy of step (5) products obtained therefrom
Levy for: specific surface area is up to 452m2/ g, pore volume is up to 1.55cm3/ g, aperture is at about 10nm, and the mechanical strength of material is big.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107715872A (en) * | 2017-10-31 | 2018-02-23 | 中国石油大学(华东) | A kind of super high-specific-surface mesoporous alumina load gold nano catalyst（Au/γ‑Al2O3）Synthetic method |
| CN111943242A (en) * | 2019-05-17 | 2020-11-17 | 国家能源投资集团有限责任公司 | Mesoporous gamma-Al2O3Preparation method of carrier and mesoporous gamma-Al2O3Carrier |
| CN114506870A (en) * | 2022-03-15 | 2022-05-17 | 昆明理工大学 | Production of NaAlO by using high-alumina fly ash2/γ-Al2O3Method for preparing nano mesoporous material |
| CN115722195A (en) * | 2022-12-05 | 2023-03-03 | 广东邦普循环科技有限公司 | Preparation method of fluoride ion adsorbent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107715872A (en) * | 2017-10-31 | 2018-02-23 | 中国石油大学(华东) | A kind of super high-specific-surface mesoporous alumina load gold nano catalyst（Au/γ‑Al2O3）Synthetic method |
| CN111943242A (en) * | 2019-05-17 | 2020-11-17 | 国家能源投资集团有限责任公司 | Mesoporous gamma-Al2O3Preparation method of carrier and mesoporous gamma-Al2O3Carrier |
| CN111943242B (en) * | 2019-05-17 | 2022-12-23 | 国家能源投资集团有限责任公司 | Mesoporous gamma-Al 2 O 3 Preparation method of carrier and mesoporous gamma-Al 2 O 3 Carrier |
| CN114506870A (en) * | 2022-03-15 | 2022-05-17 | 昆明理工大学 | Production of NaAlO by using high-alumina fly ash2/γ-Al2O3Method for preparing nano mesoporous material |
| CN115722195A (en) * | 2022-12-05 | 2023-03-03 | 广东邦普循环科技有限公司 | Preparation method of fluoride ion adsorbent |
| CN115722195B (en) * | 2022-12-05 | 2023-12-12 | 广东邦普循环科技有限公司 | Preparation method of fluoride ion adsorbent |
| WO2024119629A1 (en) * | 2022-12-05 | 2024-06-13 | 广东邦普循环科技有限公司 | Preparation method for fluoride ion adsorbent |
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