CN1425606A - Ordered nano mesoporous carbon material of two-way connection and 3-D cubic structure and its preparing method - Google Patents
Ordered nano mesoporous carbon material of two-way connection and 3-D cubic structure and its preparing method Download PDFInfo
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Abstract
Macroporous ordered nano mescoporous carbon material with spatial symmetry of Ia3d is prepared through the process of: mixing carbon source and solvent homogeneously with SiO2 mesoporous material with 3D connection and double continuous pore canal as template agent; heat treatment to evaporate solvent; high temperature roasting under protective nitrogen to carbonate carbon source completely; eliminating SiO2 template agent, filtering, washing and drying. The material has two-way connecting and 3D ordered pore and canal structure, large pore diameter, great specific surface area and great pore volume, and is powder, sheet or film.
Description
Technical field
The invention belongs to technical field of inorganic material, be specifically related to ordered nano meso-porous carbon material of a kind of wide aperture, high-specific surface area, diconnected, three-dimensional cubic structure and preparation method thereof.
Technical background
Flourish along with mesoporous nano material field, the carbon material of mesoporous nano also more and more receives scientist and investigator's concern.This mainly is because this class material all has self special advantages at aspects such as electronics, catalysis and hydrogen storage.Orderly mesoporous nano carbon material then because having the duct of rule arranges, shows more special nature, thereby is attracting many scientific workers to carry out the synthetic work of this class material.At present existing people adopts porous material as the synthesizing ordered mesoporous nano carbon material of hard template.Ordered porous material is because have the duct of particular arrangement, thereby has the space constraint effect, so carbon is grown in the duct, plays the effect of hard template.Currently used porous material comprises micro-pore zeolite, aluminum oxide film etc.; SiO 2 mesoporous materials also is used gradually recently.Because the inorganic wall of Metaporous silicon dioxide material is made up of unformed silicon-dioxide, the surface has abundant hydroxyl, interacts with the precursor that contains the carbon that enriches hydroxyl easily; Because the aperture of carbon nanomaterial will be subjected to the restriction of former hard template wall size, the aperture of the synthetic ordered nano meso-porous carbon material that obtains is usually all less than 5nm at present again.In addition, for three-dimensional successive meso-porous carbon material, still there is not relevant report.
Recently, the contriver has become out the thicker earth silicon material FDU-5 of wall (spatial symmetry is a cube Ia3d), it also has the co-continuous pore passage structure of three-dimensional communication, the aperture maximum can reach 9.5nm (Chinese patent application number: 02151024.5), adopt it as the synthetic hard template, be expected to synthesize have big aperture, the mesoporous nano carbon material of high specific surface area, diconnected, three-dimensional cubic structure.
Summary of the invention
The objective of the invention is to propose a kind of orderly mesoporous nano carbon material and preparation method thereof, require this material to have wide aperture, high-specific surface area, diconnected, three-dimensional cubic structure, to satisfy the needs of industrial application and research.
The ordered nano meso-porous carbon material that the present invention proposes, be with after corresponding solvent is mixed by carbon source, the SiO 2 mesoporous materials (spacer is Ia3d, is designated as FDU-5, sees CN02151024.5) that employing has three-dimensional communication, co-continuous duct prepares for template.This material has orderly diconnected, three-dimensional cubic structure, and the material aperture is 3-8nm, and specific surface area is 500-1700m
2/ g.Preferable aperture is 6-8nm, and specific surface area is 1000-1700m
2/ g.This material is the ordered nano material of a kind of wide aperture, high-specific surface area, diconnected, three-dimensional side's square structure.
Among the present invention, as the SiO 2 mesoporous materials FDU-5 of template, can be powder, also can be single piece of material or thin-film material.Corresponding, mesoporous nano carbon material shape also is powder, single piece of material or thin-film material.If single piece of material, its size generally can be (0.5-5) * (0.5-5) cm
2, thickness is 0.2-2cm.If thin-film material, its size generally can be (0.5-5) * (0.5-5) cm
2, thickness is 0.1-1000 μ m.Above-mentioned materials, the electric conductivity that is calculated by volt-ampere curve is 5-100s/m.
Among the present invention, can adopt sucrose, also can adopt furfuryl alcohol, perhaps mixture of phenol and formaldehyde etc. in carbon source (being the precursor of carbon).Correspondingly, the solvent of use is respectively sulfuric acid and water, ethanol etc.
The preparation method of the above-mentioned ordered nano meso-porous carbon material that the present invention proposes is as follows: at first that carbon source and solvent is even, above-mentioned SiO 2 mesoporous materials with three-dimensional communication, co-continuous duct is joined in this solution; Through Overheating Treatment, make solvent evaporates, obtain the black solid thing; Roasting under nitrogen protection again makes the carbon source carbonization, obtains the mixture of carbon and silicon-dioxide; Last removed template method also carries out aftertreatment, can obtain the ordered nano meso-porous carbon material of wide aperture that spatial symmetry is Ia3d, high-specific surface area, diconnected, three-dimensional cubic structure, and its appearance can be powder, film or monolithic.
Among the above-mentioned preparation method, the consumption (quality) of carbon source and template SiO 2 mesoporous materials is than generally can be 1: 0.5-2.The general segmentation of thermal treatment is carried out: in 50-100 ℃ of scope, kept 2-10 hour earlier, in 100-200 ℃ of scope, kept 2-10 hour.Maturing temperature is generally 800-1100 ℃, and roasting time is 4-20 hour.
Among the above-mentioned preparation method, original silicon dioxide hard template can adopt sodium hydroxide solution to remove, and the concentration of using is 1-3molL
-1Also can adopt hydrofluoric acid dissolution to remove, the concentration of use is generally 8-15%.
Among the above-mentioned preparation method, the reagent that is used as the carbon precursor can be to contain the sucrose that enriches hydroxyl, also can be furfuryl alcohol, perhaps the mixture of phenol and formaldehyde.
Among the present invention, carbon source is by the hydroxyl effect of hydroxyl with mesoporous silicon oxide template internal surface, and then enters the duct of Metaporous silicon dioxide material by the capillary condensation effect.
Adopting sucrose with carbon source below is example, further introduces its preparation process:
1, form sucrose and the mixed uniformly solution of sulfuric acid: take by weighing sucrose, add the entry and the vitriol oil, mix the back and stir on magnetic stirring apparatus, churning time is 0.5-4 hour, thereby forms sucrose homodisperse solution in sulfuric acid.The mass ratio of used sucrose, the vitriol oil, water can be 1: (0.05-0.4): (2-50);
2, formation contains Metaporous silicon dioxide material, sucrose, vitriolic suspension liquid: the macroporous silica material FDU-5 (spatial symmetry Ia3d) that will have the co-continuous pore passage structure of three-dimensional communication joins in the prepared clear solution of step 1, and continues to stir 4-12 hour; The mass ratio of mesoporous material FDU-5 and sucrose can be 1: 0.5-2;
3, thermal treatment makes solvent evaporates: will be transferred in the baking oven by the prepared mixture of step 2 and place, keeping temperature earlier is 50-100 ℃, heats 2-10 hour; Again temperature is heightened in 120-200 ℃, heated 2-10 hour;
4, double-steeping: 1-3 comes again with step, so that fill fully in the duct;
5, form the mixture of carbon and silicon-dioxide: by the resulting material of step 4 under nitrogen protection in 800-1100 ℃ of roasting 4-20 hour;
6, removing and the aftertreatment of material of template: place sodium hydroxide solution or hydrofluoric acid to stir for some time the resulting mixture of step 5, make original silica template dissolving, churning time is 10-100 hour; Then after filtration, washing, drying, can obtain spatial symmetry is the large aperture ordered mesoporous nano carbon material of Ia3d.
Among the present invention, what the preparation of mesoporous nano carbon material is play the guiding role as hard template is that wall is thick, the macroporous silica material FDU-5 of co-continuous pore passage structure with three-dimensional communication, and its duct spatial symmetry is a cube Ia3d; Used FDU-5 can be a powdered material, also can be single piece of material and thin-film material.
Among the present invention, hard template FDU-5 can obtain by different surfaces promoting agent guiding is synthetic.Used tensio-active agent comprises polyoxy olefin block copolymers Pluronic P123 (EO
20PO
70EO
20), Pluronic P103 (EO
17PO
85EO
17), Pluronic L121 (EO
5PO
70EO
5), Pluronic P85 (EO
26PO
39EO
26), Pluronic P65 (EO
20PO
30EO
20), Brij 30 (C
12EO
4), Brij 35 (C
12EO
23), Brij 56 (C
16EO
10), Brij 58 (C
16EO
20) and Brij 76 (C
18EO
10).Can use single surfactant when synthetic, the mixed surfactant that also can use two or more segmented copolymer to form.
Embodiment
Embodiment 1, when adopting sucrose as carbon source, is the large aperture ordered mesoporous nano carbon material of Ia3d for the spatial symmetry of powdery, and its synthesis step is as follows: with the 2.5g sucrose dissolved in the solution that forms by the 0.28g vitriol oil and 12g water; After powerful stirring for some time, add 2g FDU-5 powder, continue to stir 8 hours; Again this mixture is placed 70 ℃ of baking ovens to place 7 hours, transfer to then in 150 ℃ of baking ovens and placed 7 hours; When carrying out filling the second time, the amount of the sucrose of use, the vitriol oil and water is respectively 1.5g, 0.16g and 12g.Subsequently with the black solid substance transfer that obtains in tube furnace, roasting is 7 hours in 1000 ℃ of nitrogen atmospheres, promptly obtains the mixture of carbon and silicon-dioxide.This mixture is used 10%HF solution soaking 24 hours, filter then, wash and drying, promptly obtain very light black powder, be desired mesoporous nano carbon material.The aperture of this mesoporous nano carbon material is 6.4nm, and pore volume is 0.74cm
3/ g, specific surface area is 852m
2/ g.
Embodiment 2, when adopting furfuryl alcohol as carbon source, are the large aperture ordered mesoporous nano carbon material of Ia3d for pulverous spatial symmetry, and its synthesis step is as follows: the 1.6g furfuryl alcohol is evenly dispersed in the 10g ethanol; Add the 2gFDU-5 powder afterwards, continue to stir 8 hours; Again this mixture is placed 70 ℃ of baking ovens to place 7 hours, transfer to then in 150 ℃ of baking ovens and placed 7 hours; Subsequently with the black solid powder transfer that obtains in tube furnace, roasting is 7 hours in 1000 ℃ of nitrogen atmospheres, promptly obtains the mixture of carbon and silicon-dioxide.The sodium hydroxide solution of this mixture with 1.5mol/L soaked 24 hours, filter then, wash and drying, promptly obtain very light black powder, be desired mesoporous nano carbon material.The aperture of this material is 5.7nm, and pore volume is 0.91cm
3/ g, specific surface area is 915m
2/ g.
Embodiment 3, and another kind of phenol and the formaldehyde blended space symmetry of adopting is that the concrete steps of large aperture ordered mesoporous nano carbon material of Ia3d are as follows: the FDU-5 powder of 1g being mixed aluminium 5% joins in the 1.7ml phenol, stirs; Under vacuum condition, be heated to 130 ℃ again, make phenol enter in the duct of mesoporous silicon oxide fertile material; In above-mentioned system, add 1.5ml formaldehyde afterwards, place 130 ℃ of baking oven reactions 30 hours, form the mixture of phenolic resin and silicon-dioxide; Then with the substance transfer that obtains in tube furnace, roasting is 6 hours in 900 ℃ of nitrogen atmospheres, promptly obtains the mixture of carbon and silicon-dioxide.After this mixture soaked 48 hours with the sodium hydroxide solution of 2mol/L, after filtration, washing and dry, promptly obtain the mesoporous nano carbon material.Its aperture is 5.9nm, and pore volume is 1.39cm
3/ g, specific surface area is 957m
2/ g.
Embodiment 4, are the large aperture ordered mesoporous nano carbon film material of Ia3d for spatial symmetry, and its synthesis step is as described below: with the 1.2g sucrose dissolved in the solution that forms by the 0.14g vitriol oil and 6g water; After powerful stirring for some time, add the FDU-5 film of 1.2g circle, continue to soak 8 hours; Again this mixture is placed 70 ℃ of baking ovens to place 7 hours, transfer to then in 150 ℃ of baking ovens and placed 7 hours; When carrying out filling the second time, the amount of the sucrose of use, the vitriol oil and water is respectively 0.8g, 0.08g and 6g.Subsequently with the black solid substance transfer that obtains in tube furnace, roasting is 7 hours in 1000 ℃ of nitrogen atmospheres, promptly obtains the mixture of carbon and silicon-dioxide.This mixture is used 10%HF solution static immersing 24 hours, filter then, wash and drying, promptly obtain very light black powder, be desired mesoporous nano carbon film material.The diameter of the carbon film material of this sharp circle is 5cm, and thickness is 10 μ m.The aperture of this mesoporous nano carbon material is 4.9nm, and pore volume is 0.85cm
3/ g, specific surface area is 1154m
2/ g.
Embodiment 5, are the large aperture ordered mesoporous nano carbon single piece of material of Ia3d for spatial symmetry, and its synthesis step is as described below: with the 2.0g sucrose dissolved in the solution that forms by the 0.20g vitriol oil and 15g water; Add the silicon-dioxide monolithic that 1.5g has the co-continuous cubic structure at the powerful 30min that stirs on the magnetic stirring apparatus after time, soaked 6 hours; Again this mixture is placed 80 ℃ of baking ovens to place 6 hours, transfer to then in 160 ℃ of baking ovens and placed 6 hours; When carrying out filling the second time, the amount of the sucrose of use, the vitriol oil and water is respectively 1.5g, 0.10g and 10g.Subsequently the black solid monolithic that obtains is transferred in the tube furnace, roasting is 6 hours in 950 ℃ of nitrogen atmospheres, promptly obtains the mixture of carbon and silicon-dioxide.After this mixture soaked 48 hours with 10% hydrogen fluoride solution, through filtration, washing and dry, promptly obtain mesoporous nano carbon single piece of material.The diameter of this mesoporous carbon single piece of material is 2.1cm, and thickness is 0.3cm, and the aperture is 4.6nm, and pore volume is 1.9cm
3/ g, specific surface area is 1530m
2/ g.
Claims (10)
1, a kind of ordered nano meso-porous carbon material, it is characterized in that by carbon source with after coordinative solvent mixes, the SiO 2 mesoporous materials that employing has three-dimensional communication, co-continuous duct prepares as template, have orderly diconnected, three-dimensional cubic structure, the material aperture is 3-8nm, and specific surface area is 500-1700m
2/ g.
2, ordered nano meso-porous carbon material according to claim 1 is characterized in that being shaped as powder, or single piece of material, or thin-film material, and the size of single piece of material is (0.5-5) * (0.5-5) cm
2, thickness is 0.2-2cm; The size of thin-film material is (0.5-5) * (0.5-5) cm
2, thickness is 0.1-1000 μ m.
3, a kind of preparation method of ordered nano meso-porous carbon material as claimed in claim 1 is characterized in that at first that carbon source and solvent is evenly, and the SiO 2 mesoporous materials that will have three-dimensional communication, co-continuous duct joins in this solution; Through Overheating Treatment, make solvent evaporates, obtain the black solid thing; Roasting under nitrogen protection again makes the carbon source carbonization, obtains the mixture of carbon and silicon-dioxide; Last removed template method also carries out aftertreatment.
4, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that the mass ratio of the consumption of carbon source and template SiO 2 mesoporous materials is: 1: 0.5-2.
5, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that the thermal treatment segmentation carries out: kept 2-4 hour in 50-100 ℃ of scope earlier; In 120-200 ℃ of scope, kept 2-10 hour again.
6, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that maturing temperature is 800-1100 ℃, roasting time 4-20 hour.
7, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that removed template method can adopt sodium hydroxide solution or hydrofluoric acid.
8, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that the SiO 2 mesoporous materials that adopts is a powder, or single piece of material, or thin-film material.
9, the preparation method of ordered nano meso-porous carbon material according to claim 3 is characterized in that carbon source adopts sucrose, or furfuryl alcohol, or the mixture of phenol and formaldehyde.
10, the preparation method of ordered nano meso-porous carbon material according to claim 9 is characterized in that the synthesis step when carbon source adopts sucrose is as follows:
(1) forms sucrose and the mixed uniformly solution of sulfuric acid: take by weighing sucrose, add the entry and the vitriol oil, mix the back and stirred 0.5-4 hour on magnetic stirring apparatus, form sucrose homodisperse solution in sulfuric acid, the mass ratio of used sucrose, the vitriol oil, water is 1: (0.05-0.4): (2-50);
(2) formation contains Metaporous silicon dioxide material, sucrose, vitriolic suspension liquid: the macroporous silica material FDU-5 that will have the co-continuous pore passage structure of three-dimensional communication joins in the prepared clear solution of step 1, and continues to stir 4-12 hour; The mass ratio of mesoporous material and sucrose is 1: 0.5-2;
(3) thermal treatment makes solvent evaporates: will be transferred in the baking oven by the prepared mixture of step 2 and place, keeping temperature earlier is 50-100 ℃, heats 2-10 hour; Again temperature is heightened in 120-200 ℃, heated 2-10 hour;
(4) double-steeping: 1-3 comes again with step, so that fill fully in the duct;
(5) form the mixture of carbon and silicon-dioxide: by the resulting material of step 4 under nitrogen protection in 800-1100 ℃ of roasting 4-20 hour;
(6) removing and the aftertreatment of material of template: place sodium hydroxide solution or hydrofluoric acid to stir 10-100 hour the resulting mixture of step 5, make original silica template dissolving; Then after filtration, washing, drying, promptly obtaining spatial symmetry is the large aperture ordered mesoporous nano carbon material of Ia3d.
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