CN103736442A - Method for preparing porous alumina composite material through biological template method - Google Patents
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Abstract
The invention relates to a method for preparing a porous alumina composite material through a biological template method. The method comprises the following steps: duplicating a macro-pore tubular structure of a plant leaf, which is used as a biological template, through alumina in a material preparation process to obtain biomorphic alumina with a macro-pore fiber tubular structure; growing an LDHs (layered double hydroxides) nanosheet in a macro-pore channel of the biomorphic alumina in situ through an in-situ growth technology to obtain a porous LDHs/alumina composite material; roasting the porous LDHs/alumina composite material at the temperature of 500-800 DEG C to obtain the porous alumina composite material. The LDHs nanosheet is grown in the macro-pore channel of the biomorphic alumina, so that the specific surface area of the biomorphic alumina can be remarkably increased, and the pore structure of the biomorphic alumina is diversified. The porous alumina composite material can be widely applied to the fields of adsorption, catalysis and the like.
Description
Technical field
The present invention relates to the method for a kind of biological template legal system for porous oxidation aluminium composite material, belong to the preparing technical field of porous material.
Background technology
Organism, through long-term natural selection and evolution, mostly has fine hiberarchy and special function, and the biomorphic materials that utilizes bionics techniques preparation to have fine structure is focus and the difficult point of studying in field of functional materials.Bionical synthesizing is mainly the generation that utilizes biomaterial induction inorganic material, controls the pattern of inorganic material by copying the structure of biomaterial.At present, many biomaterials have been used as template carrys out the porous material of synthesizing inorganic structure, these biological templates comprise blade, pollen grain, shell membrane, spider's thread fiber and the silk etc. of bone, pilose antler, corner, feather, hair, insect wing, bacterium, fungi, virus, string, plant, but these biomimetic materials are mainly accurately copying biological structure, and take the biomorphic materials after copying as basis, prepare the material of new structure still in the preliminary research stage.
Plant leaf blade is subject to extensive concern in recent years owing to having unique micro-nano structure, on plant leaf blade, there is a large amount of fiber state structures, this structure stems from the needs of plant growth, by long-term evolution and differentiation, the unique fiber tubular structure that has formed Multi hiberarchy and multi scale, common this structure is difficult to obtain by artificial means.Plant leaf blade is due to wide material sources and have reproducibility, and therefore adopting plant leaf blade is that biological template is prepared biomorphic materials and had good development prospect.But, after blade construction copies, the specific area of material mainly concentrates on the tube wall of material, and the fiber tubular structure (macroporous structure) of micron-scale is difficult to the specific area that provides higher, if can be in the material of some function nano sizes " filling " inorfil pipe, or " growth " is at fibre pipe inner surface, build high specific surface area porous material and there is larger using value, function nano material can effectively increase or improve the function of biomorphic materials on the one hand, on the other hand, nano material " filling " or " growth " are in fibre pipe, the specific area and the pore structure of having enriched material of material have been increased, material after structure can be micropore-mesopore material, micropore-large pore material and mesopore-macropore material, the duct of this multilevel hierarchy is conducive to the diffusion of adsorption molecule, absorption and transmission, mesoporous and macropore in material can allow the adsorbate that volume is larger to pass through better, and micropore and mesoporous material can provide high-specific surface area and large pore volume, the absorption of the molecule that corresponding volume is less is more favourable.
Therefore, the present invention is directed to the distinctive structural form of plant leaf blade, using plant leaf blade as a kind of biological template, utilize aluminium oxide accurately to copy plant leaf structure, the doughnut structure that form aluminium oxide after utilization copies exists, layered double-hydroxide (LDHs) nanometer sheet is grown in macropore fiber conduit, to increase alumina composite material specific area and to enrich material hole structure, has invented a kind of preparation method of biological template legal system for porous oxidation aluminium composite material that utilize.
Summary of the invention
Technical problem: the object of the invention is to provide the method for a kind of biological template legal system for porous oxidation aluminium composite material, unique macroporous structure that the method utilizes biomorphic materials to exist, in material duct growth in situ LDHs nanometer sheet, the specific area and the pore structure of enriching aluminium oxide that can effectively increase alumina composite material, expansion biomimetic material is in the application of absorption and catalytic field.
Technical scheme: the present invention utilizes the special structure of plant leaf blade, using plant leaf blade as a kind of biological template, utilize aluminium oxide to copy plant leaf blade to obtain form aluminium oxide, utilize the macroporous structure that has hollow in form aluminium oxide, the LDHs of surface in situ growth therein nanometer sheet, by controlling LDHs growth course, control the pore structure of material, utilize biological template legal system for porous oxidation aluminium composite material.
Biological template legal system is for a method for porous oxidation aluminium composite material, and this preparation method is:
A) by adding 2～5g biological template in every 100mL absolute ethyl alcohol, biological template is washed in absolute ethyl alcohol 3～5 times, by every 100mL hydrochloric acid solution, add 2～5g biological template again, biological template after ethanol washing is immersed in the aqueous hydrochloric acid solution of 3wt%～6wt%, dipping 4～6h, filter, with after distilled water washing 2～4 times, biological template is immersed in 6～12h in the fresh aqueous hydrochloric acid solution of same volume 3wt%～6wt% again, filter, with the pH that distilled water is washed till filtrate, be neutral, dry 6～12h at 50～80 ℃, obtains pretreatment biological template.
B) by every 100mL aluminum saline solution, add 0.2～2g pretreatment biological template, the pretreatment biological template that step a) is obtained is immersed in the aluminum saline solution of 0.1～0.5mol/L, after dipping 2～6h, take out, distilled water washing 1～3 time, dry 6～12h at 50～80 ℃, 500～800 ℃ of roasting 2～6h, obtain biomorph aluminium oxide.
C) by divalent metal M salt and step b) in the mol ratio of biomorph aluminium oxide of preparation be 1:6～1:1, the mol ratio of organic amine and biomorph aluminium oxide is 6:1～1:1 meter, by the divalent metal M saline solution of 0.005～0.05mol/L, organic amine and biomorph aluminium oxide join in the autoclave of inner liner polytetrafluoroethylene, mix, 80～160 ℃ of hydro-thermal reaction 5～15h, cooling, filter, distilled water washing 3～6 times, dry 12～24h at 50～80 ℃, obtain porous LDHs/ alumina composite material, 500～800 ℃ of roasting 2～6h, obtain porous oxidation aluminium composite material.
For the method step of porous oxidation aluminium composite material, the biological template described in a) is ginkgo leaf to above-mentioned a kind of biological template legal system, Poplar leaves, maize leaves, the combination of one or more in Folium sophorae, aluminium salt described in step b) is aluminum nitrate, aluminum sulfate, the combination of one or several in aluminium chloride, organic amine described in step c) is dimethylamine, ethylenediamine, triethylamine, the combination of one or several in hexa, divalent metal M salt is zinc nitrate, magnesium nitrate, nickel nitrate, magnesium sulfate, magnesium chloride, zinc acetate, zinc chloride, the combination of one or several in nickelous sulfate.
Beneficial effect: the present invention utilizes plant leaf blade for biological template, biological template legal system is for porous oxidation aluminium composite material, utilize aluminium oxide to copy plant leaf blade macropore tubular structure, acquisition has the biomorph aluminium oxide of macropore fiber tubular structure, utilize in-situ growth technology, in biomorph aluminium oxide macropore, growth in situ LDHs nanometer sheet, can obtain porous oxidation aluminium composite material by high-temperature roasting.
The present invention, at the basic engineering porous material of biological structure, utilizes the structure of organism uniqueness to prepare porous oxidation aluminium composite material, is different from physical-chemical process and prepares Woelm Alumina.Compared with prior art, the invention has the advantages that:
(1), the present invention utilizes in-situ growth technology, and LDHs nanometer sheet growth in situ, at biological oxidation aluminum fiber pipe interior, is significantly increased to the specific area of biomorph aluminium oxide, the specific area of the porous material of preparation can be from 70～90m
2/ g(biomorph aluminium oxide) be increased to 200m
2/ g above (porous oxidation aluminium composite material).In addition, the pore structure of composite alumina presents diversity, has multilevel hierarchy, can have macropore and meso-hole structure, and pore structure has adjustability in composite simultaneously.
(2), biological template used in the present invention is plant leaf blade, plant leaf blade wide material sources and there is reproducibility, adopting plant leaf blade is that biological template is prepared porous material and had inexpensive, environmental friendliness.
(3), the present invention introduces function nano material in form aluminium oxide macroporous structure, prepares porous oxidation aluminium composite material, its performance is better than single alumina material.
The specific embodiment
Embodiment 1:
Choose 2g ginkgo leaf as biological template, ginkgo leaf is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that ginkgo leaf after cleaning is joined to 100mL concentration, dipping 6h, taking-up is with after distilled water washing 3 times, it is in the fresh hydrochloric acid solution of 6wt% that ginkgo leaf is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment ginkgo leaf template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 0.5g ginkgo leaf is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the magnesium nitrate solution that 30mL concentration is 0.03mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 120 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 2:
Choose 3g Poplar leaves as biological template, Poplar leaves is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that Poplar leaves after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that Poplar leaves is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment Poplar leaves template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 1g Poplar leaves is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the magnesium nitrate solution that 30mL concentration is 0.03mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 120 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 3:
Choose 2g ginkgo leaf as biological template, ginkgo leaf is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that ginkgo leaf after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that ginkgo leaf is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment ginkgo leaf template.
Get the aluminum sulfate solution that 200mL concentration is 0.1mol/L, pretreated 1g ginkgo leaf is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the magnesium nitrate solution that 30mL concentration is 0.03mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 120 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 500 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 4:
Choose 3g Poplar leaves as biological template, Poplar leaves is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that Poplar leaves after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that Poplar leaves is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment Poplar leaves template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 1g Poplar leaves is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the nickel sulfate solution that 30mL concentration is 0.02mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 120 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 5:
Choose 3g Poplar leaves as biological template, Poplar leaves is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that Poplar leaves after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that Poplar leaves is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment Poplar leaves template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 1g Poplar leaves is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the zinc nitrate solution that 30mL concentration is 0.02mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 80 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 6:
Choose 2g ginkgo leaf as biological template, ginkgo leaf is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that ginkgo leaf after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that ginkgo leaf is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment ginkgo leaf template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 0.5g ginkgo leaf is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and ethylenediamine 0.005mol are joined in the magnesium nitrate solution that 30mL concentration is 0.03mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 120 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Embodiment 7:
Choose 3g Folium sophorae as biological template, Folium sophorae is washed 3 times in 100mL absolute ethyl alcohol.It is in 6wt% hydrochloric acid solution that Folium sophorae after cleaning is joined to 100mL concentration, dipping 6h, taking out distilled water washs after 3 times, it is in the fresh hydrochloric acid solution of 6wt% that Folium sophorae is immersed in to 100mL concentration again, dipping 12h filters, with the pH that distilled water is washed till filtrate, be neutral, dry 12h at 80 ℃, obtains pretreatment Folium sophorae template.
Get the aluminum nitrate solution that 200mL concentration is 0.1mol/L, pretreated 1g Folium sophorae is immersed in aluminum nitrate solution, after dip time 4h, take out, distilled water washing 3 times, dry 12h at 80 ℃, at 500～800 ℃ of roasting 4h, obtains biomorph aluminium oxide.
Biomorph aluminium oxide 0.001mol and hexa 0.004mol are joined in the zinc acetate solution that 30mL concentration is 0.01mol/L, after mixing, transfer in the autoclave of inner liner polytetrafluoroethylene, hydro-thermal reaction 12h at 80 ℃, cooling, filtration, distilled water washing obtain porous LDHs/ alumina composite material.Porous LDHs/ alumina composite material, at 550 ℃ of roasting 4h, is obtained to porous oxidation aluminium composite material.
Claims (3)
1. biological template legal system, for a method for porous oxidation aluminium composite material, is characterized in that the method is:
A) by adding 2～5g biological template in every 100mL absolute ethyl alcohol, biological template is washed in absolute ethyl alcohol 3～5 times, by every 100mL hydrochloric acid solution, add 2～5g biological template again, biological template after ethanol washing is immersed in the aqueous hydrochloric acid solution of 3wt%～6wt%, dipping 4～6h, filter, with after distilled water washing 2～4 times, biological template is immersed in 6～12h in the fresh aqueous hydrochloric acid solution of same volume 3wt%～6wt% again, filter, with the pH that distilled water is washed till filtrate, be neutral, dry 6～12h at 50～80 ℃, obtains pretreatment biological template;
B) by every 100mL aluminum saline solution, add 0.2～2g pretreatment biological template, the pretreatment biological template that step a) is obtained is immersed in the aluminum saline solution of 0.1～0.5mol/L, after dipping 2～6h, take out, distilled water washing 1～3 time, dry 6～12h at 50～80 ℃, 500～800 ℃ of roasting 2～6h, obtain biomorph aluminium oxide.
C) by divalent metal M salt and step b) in the mol ratio of biomorph aluminium oxide of preparation be 1:6～1:1, the mol ratio of organic amine and biomorph aluminium oxide is 6:1～1:1 meter, by the divalent metal M saline solution of 0.005～0.05mol/L, organic amine and biomorph aluminium oxide join in the autoclave of inner liner polytetrafluoroethylene, mix, 80～160 ℃ of hydro-thermal reaction 5～15h, cooling, filter, distilled water washing 3～6 times, dry 12～24h at 50～80 ℃, obtain porous LDHs/ alumina composite material, 500～800 ℃ of roasting 2～6h, obtain porous oxidation aluminium composite material.
2. a kind of biological template legal system according to claim 1 is for the method for porous oxidation aluminium composite material, it is characterized in that the biological template described in step a) is one or more the combination in ginkgo leaf, Poplar leaves, maize leaves or Folium sophorae.
3. a kind of biological template legal system according to claim 1 is for the method for porous oxidation aluminium composite material, it is characterized in that the aluminium salt described in step b) is one or several the combination in aluminum nitrate, aluminum sulfate, aluminium chloride; Organic amine described in step c) is one or several the combination in dimethylamine, ethylenediamine, triethylamine, hexa, and divalent metal M salt is one or several the combination in zinc nitrate, magnesium nitrate, nickel nitrate, magnesium sulfate, magnesium chloride, zinc acetate, zinc chloride, nickelous sulfate.
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| CN103736442B (en) | 2015-10-07 |
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