CN106186014B - 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 PDF

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CN106186014B
CN106186014B CN201610578868.9A CN201610578868A CN106186014B CN 106186014 B CN106186014 B CN 106186014B CN 201610578868 A CN201610578868 A CN 201610578868A CN 106186014 B CN106186014 B CN 106186014B
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mesoporous
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naalo
molar ratio
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CN106186014A (en
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白鹏
庄洪庆
吴萍萍
邢伟
阎子峰
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China University of Petroleum East China
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • 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
    • 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
    • C01P2006/12—Surface area
    • 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
    • C01P2006/14—Pore volume
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract

The present invention provides a kind of synthesising mesoporous γ-Al2O3Method, with inorganic cation aluminium salt and NaAlO2Pass through Al at room temperature using triblock polymer Pluronic P123 as structure directing agent for silicon source3+And AlO2 ‑The hydrolysis itself carried out prepares mesoporous γ-Al2O3, short and operating procedure is simple the time required to reaction.Mesoporous γ-the Al that this method synthesizes2O3, specific surface area is up to 452m2/ g, Kong Rong is up to 1.55cm3/ g, aperture is in 10nm or so, and meso-hole structure is being able to maintain stabilization greater than 550 DEG C of roasting temperatures, and gained mesoporous aluminum oxide material mechanical strength is big, is suitable as catalyst carrier.

Description

A kind of mesoporous γ-Al of function admirable2O3Synthetic method
Technical field
The present invention relates to a kind of mesoporous γ-Al2O3Preparation method.It more specifically, is one kind with inorganic cation aluminium Salt and NaAlO2For silicon source, mesoporous γ-Al is prepared as structure directing agent using Pluronic P1232O3Method.
Background technique
The crystal form of aluminium oxide enriches (amorphous, α phase, β phase, γ phase, δ are equal), cheap and easy to get, has good physico It learns property (thermal stability, chemical stability, mechanical stability), is a kind of important catalyst carrier and adsorbent, in industry On be used widely.Meso-porous alumina, as a kind of novel alumina material, except the physics with common alumina material Except chemical characteristic, also there is bigger serface, macropore holds, excellent cellular structure, has in catalysis, adsorbing domain important Application value.
1996, Pinnavaia et al. is reported for the first time successfully synthesized heat-staple meso-porous alumina.It respectively grinds in the whole world Study carefully the study on the synthesis that group has carried out meso-porous alumina extensively.On the whole, common meso-porous alumina synthetic method has following several Kind:
(1) solvent-thermal process method: aluminium isopropoxide is dissolved in the in the mixed solvent of isopropanol or isopropanol and water by Gan etc., It is added after toluene in stainless steel autoclave, 150~190 DEG C of reaction 20h obtain meso-porous alumina.Solvent-thermal process method behaviour Make simply, it is time-consuming short, it is reproducible, but need to use organic solvent, environment is unfriendly, higher cost.Meanwhile synthesis condition compared with Harshness, there are some potential safety problemss.
(2) sol-gel method: by surfactant dissolution form vitreosol in a solvent, be sequentially added silicon source and its His reagent is aged after stirring and dissolving.Colloidal sol is changed into gel after being sufficiently aged, and is post-processed to gel and obtains mesoporous oxygen Change aluminium.Sol-gel method method is easy safely, but manufacturing cycle is relatively long, less reproducible.
(3) precipitation method: the precipitation method, which are reacted using silicon source with precipitating reagent, generates colloidal sol or gel to prepare meso-porous alumina.It is heavy Shallow lake method is faster than sol-gel method, safe operation, is easy to industrial amplification, but obtained meso-porous alumina specific surface area is relatively small, Structural behaviour is relatively poor.
Although in the latest 20 years, the synthesis of meso-porous alumina makes great progress.But most of synthetic method is general It needs to use expensive and toxic alkyl aluminum as silicon source, producing cost is high, big to operator's actual bodily harm.Some are needed Time-consuming, complicated hydrolysis and pH value adjustment process, so that the production cycle is long, severe reaction conditions.
In method disclosed in 101993102 A of CN, researcher does template with methylcellulose, with sodium metasilicate and chlorination Aluminium prepares siliceous meso-porous alumina, and gained precipitating will be aged by constant temperature.In method disclosed in 102219242 A of CN, Researcher does template with P123, prepares meso-porous alumina using inorganic aluminate and ammonium hydroxide or ammonium salt, and P123 is initially and aluminium salt Solution is dissolved in together, rear that ammonium hydroxide or ammonium salt solution is added to adjust pH value generation precipitating.The above method comes using inorganic silicon source Meso-porous alumina is prepared, avoids the use of alkyl silicon source, but the Kong Rong of obtained meso-porous alumina is smaller, specific surface area is not It is high.
Summary of the invention
That present invention aim to address the prior arts is at high cost, operating procedure is complicated and the mesoporous γ-Al of gained2O3Kong Rong little The problem of, develop a kind of at low cost, the easy high-specific surface area of preparation method, the mesoporous γ-Al of macropore appearance2O3Synthetic method.
The present invention provides a kind of synthesising mesoporous γ-Al2O3Method, with inorganic cation aluminium salt and NaAlO2For silicon source, with Pluronic P123 is structure directing agent, passes through Al at room temperature3+And AlO2 -The hydrolysis itself carried out prepares mesoporous γ- Al2O3, short and operating procedure is simple the time required to reaction.Mesoporous γ-the Al that this method synthesizes2O3, specific surface area is reachable 452m2The high specific surface area of/g, Kong Rong is up to 1.55cm3/ g, aperture are being greater than 550 DEG C of temperature in 10nm or so, meso-hole structure Lower roasting is able to maintain stabilization, and gained mesoporous aluminum oxide material mechanical strength is big, is suitable as catalyst carrier.
Typical synthesis step are as follows: respectively by AlCl3·6H2O and NaAlO2It is dissolved in appropriate amount of deionized water, and stirs 1h, P123 is added in appropriate amount of deionized water simultaneously and stirs 1h, forms P123 solution.Cocurrent mixes AlCl at room temperature3With NaAlO2Solution controls AlO2 -And Al3+Molar ratio adjust the pH value of mixed system, stir 2h.Cocurrent is mixed to get Precipitating is filtered, is washed, and obtains clean aluminum hydroxide precipitation.Aluminum hydroxide precipitation is redispersed in P123 solution, mechanical stirring 2h.Uniformly mixed aluminum hydroxide precipitation and the solution combined object of P123 are placed in baking oven dry 12h.Compound after drying exists Certain temperature is warming up to the heating rate of 2 DEG C/min in Muffle furnace, constant temperature calcining for a period of time, it is mesoporous to obtain purpose product γ-Al2O3.Compared with pervious preparation method, the present invention has the advantage that
(1) present invention carries out at room temperature in alumina precursor synthesis phase, and low energy consumption.
(2) present invention uses cheap, nontoxic inorganic aluminate AlCl3And NaAlO2, avoid the higher and toxic alkane of price The use of base aluminium.
(3) present invention passes through Al in control precipitation reaction3+And AlO2 -Molar ratio control pH value, pH value adjustment process Simply, and precipitation reaction speed is fast.
Detailed description of the invention
The 1 mesoporous γ-Al of gained of Fig. 1 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Fig. 2 embodiment 1 roasts2O3XRD wide-angle diffraction figure.
The 2 mesoporous γ-Al of gained of Fig. 3 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Fig. 4 embodiment 2 roasts2O3XRD wide-angle diffraction figure.
The 3 mesoporous γ-Al of gained of Fig. 5 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Fig. 6 embodiment 3 roasts2O3XRD wide-angle diffraction figure.
The 4 mesoporous γ-Al of gained of Fig. 7 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Fig. 8 embodiment 4 roasts2O3XRD wide-angle diffraction figure.
The 5 mesoporous γ-Al of gained of Fig. 9 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Figure 10 embodiment 5 roasts2O3XRD wide-angle diffraction figure.
The 6 mesoporous γ-Al of gained of Figure 11 embodiment2O3N2Adsorption and desorption isotherms and pore size distribution curve figure；
Mesoporous γ-the Al of gained after Figure 12 embodiment 6 roasts2O3XRD wide-angle diffraction figure.
Specific embodiment
It is described in conjunction with the embodiments a specific embodiment of the invention, but is not limited only to this, P123 used in the present embodiment It is the product of SIGMA-ALDRICH company, molecular weight 5800.
Embodiment 1:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 2.78 cocurrents.Mixture is filtered, Washing, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 29, mechanical stirring 2 are small When.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, it is dry after compound be transferred in Muffle furnace, with 2 DEG C/ The heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Fig. 12Adsorption and desorption isotherms and pore-size distribution This γ-Al known to curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 400.9m2/ g, Kong Rongwei 1.43cm3/ g, aperture concentrate on 10.8nm.The material prepared known to the XRD spectra in Fig. 2 is γ-Al2O3Crystal phase.
Embodiment 2:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 2.78 cocurrents.Mixture is filtered, Washing, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 22.7, mechanical stirring 2 Hour.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, the compound after drying is transferred in Muffle furnace, with 2 DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Fig. 32Adsorption and desorption isotherms and aperture This γ-Al known to distribution curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 421.9m2/ g, Kong Rongwei 1.56cm3/ g, aperture concentrate on 9.4nm.The material prepared known to the XRD spectra in Fig. 4 is γ-Al2O3Crystal phase.
Embodiment 3:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 2.56 cocurrents.Mixture is filtered, Washing, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 38.7, mechanical stirring 2 Hour.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, the compound after drying is transferred in Muffle furnace, with 2 DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Fig. 52Adsorption and desorption isotherms and aperture This γ-Al known to distribution curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 400.3m2/ g, Kong Rongwei 1.38cm3/ g, aperture concentrate on 9.7nm.The material prepared known to the XRD spectra in Fig. 6 is γ-Al2O3Crystal phase.
Embodiment 4:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 2.56 cocurrents.Mixture is filtered, Washing, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 23.2, mechanical stirring 2 Hour.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, the compound after drying is transferred in Muffle furnace, with 2 DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Fig. 72Adsorption and desorption isotherms and aperture This γ-Al known to distribution curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 438.3m2/ g, Kong Rongwei 1.44cm3/ g, aperture concentrate on 9.5nm.The material prepared known to the XRD spectra in Fig. 8 is γ-Al2O3Crystal phase.
Embodiment 5:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 2.56 cocurrents.Mixture is filtered, Washing, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 23.2, mechanical stirring 2 Hour.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, the compound after drying is transferred in Muffle furnace, with 2 DEG C/heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Fig. 92Adsorption and desorption isotherms and aperture This γ-Al known to distribution curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 452.3m2/ g, Kong Rongwei 1.39cm3/ g, aperture concentrate on 9.2nm.The material prepared known to the XRD spectra in Figure 10 is γ-Al2O3Crystal phase.
Embodiment 6:
At room temperature, NaAlO will be contained2Solution and contain AlCl3·6H2The solution of O, according to AlO2 -And Al3+Rub You generate white precipitate, gained mixture is stirred at room temperature 2 hours than mixing in 3 cocurrents.Mixture is filtered, is washed It washs, obtains aluminum hydroxide precipitation, precipitating is redispersed in Al3+The P123 solution that/P123 molar ratio is 23.2, mechanical stirring 2 are small When.The compound stirred evenly is placed in 100 DEG C of baking ovens dry 12h, it is dry after compound be transferred in Muffle furnace, with 2 DEG C/ The heating rate of min is warming up to 550 DEG C, 550 DEG C constant temperature calcining 2 hours.By the N in Figure 112Adsorption and desorption isotherms and aperture point This γ-Al known to cloth curve2O3For mesoporous material, resulting mesoporous γ-Al2O3Specific surface area is 401.2m2/ g, Kong Rongwei 1.20cm3/ g, aperture concentrate on 8.8nm.The material prepared known to the XRD spectra in Figure 12 is γ-Al2O3Crystal phase.

Claims (6)

1. a kind of mesoporous γ-Al of function admirable2O3Synthetic method has follow steps:
(1) respectively by cationic aluminium salt and NaAlO2It is dissolved in appropriate amount of deionized water, and stirs 1h；P123 is added to and is gone in right amount 1h is stirred in ionized water, forms P123 solution；
(2) cocurrent mixed-cation aluminium salt and NaAlO at room temperature2Solution controls the molar ratio of zwitterion silicon source to adjust mixing The pH value of liquid, stirs 2h later；
(3) precipitated product for obtaining step (2) is filtered, is washed, and clean aluminum hydroxide precipitation is obtained, by aluminum hydroxide precipitation It is redispersed in P123 solution, mechanical stirring 2h；
(4) uniformly mixed aluminum hydroxide precipitation and the solution combined object of P123 are placed in baking oven dry 12h；
(5) when the compound after drying is warming up to 550 DEG C, one section of constant temperature calcining in Muffle furnace with the heating rate of 2 DEG C/min Between, obtain the mesoporous γ-Al of purpose product2O3。
2. mesoporous γ-Al according to claim 12O3Synthetic method, it is characterised in that: cation described in step (1) Aluminium salt is aluminum nitrate, aluminium chloride, aluminum sulfate, one or more of aluminum aluminum sulfate.
3. mesoporous γ-Al according to claim 12O3Synthetic method, it is characterised in that: step (2) described AlO2-With Al3+Molar ratio in 2.56~3 ranges, carry out cocurrent hybrid reaction.
4. mesoporous γ-Al according to claim 12O3Synthetic method, it is characterised in that: P123 solution in step (3), Al3+Molar ratio with P123 is in 22.7~38.7 ranges.
5. mesoporous γ-Al according to claim 12O3Synthetic method, it is characterised in that: step (4) is will be containing certain The compound for measuring deionized water carries out moisture evaporation drying in 80~140 DEG C of baking oven.
6. mesoporous γ-Al according to claim 12O3Synthetic method, it is characterised in that: roasting 2 in step (5)~ 48h。
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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
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
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

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