CN103359705A - Graded porous carbon material and preparation method thereof - Google Patents
Graded porous carbon material and preparation method thereof Download PDFInfo
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- CN103359705A CN103359705A CN2013102839596A CN201310283959A CN103359705A CN 103359705 A CN103359705 A CN 103359705A CN 2013102839596 A CN2013102839596 A CN 2013102839596A CN 201310283959 A CN201310283959 A CN 201310283959A CN 103359705 A CN103359705 A CN 103359705A
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Abstract
The invention discloses a preparation method of a graded porous carbon material. According to the preparation method, a carbon material with a graded pore structure is prepared by taking wood (bamboo) as a primary template, a surfactant as a secondary template and a linear phenolic resin as a precursor through with limited-range self-assembly and high-temperature carbonization process. The graded porous carbon material is simple in preparation process, rapid and time-saving and low in production cost, biomasses such as wood (bamboo) can be efficiently utilized, and the additional values of the biomasses are increased; the graded porous carbon material prepared by using the preparation method has a large specific surface area and a graded micro-pore, meso-pore and macro-pore ternary nano structure, and has wide application prospects in the fields of catalysis, absorption, separation, energy storage and the like.
Description
Technical field
The present invention relates to Material Field, be specially a kind of grading-hole Carbon Materials and preparation method thereof.
Background technology
The grading-hole Carbon Materials has the aperture can be regulated and control, and the ternary pore structure of micropore, mesoporous and macropore reasonable layout.In catalytic applications, its macropore can provide efficient mass transfer space, can greatly reduce diffusional resistance; Mesoporous transmission path has greatly improved the rate of diffusion of ion, is conducive to the transmission of reactant and product; And micropore can improve the degree of scatter of reactive material, and abundant active centre is provided, and catalytic effect has been played positive promoter action.Thereby the grading-hole Carbon Materials all has in fields such as catalysis, absorption, separation, energy storage widely to be used.At present, the preparation method of grading-hole Carbon Materials mainly contains template, template-activation coupling method, exempts from template, and their raw materials and template mostly are Chemicals.Along with the shortage of the energy and the continuous deterioration of environment, how directly to utilize natural biomass as raw material, and prepare the grading-hole material with particular topology structure by method simply, effectively and cheaply and day by day become most important.
Wood (bamboo) material has the test-tube baby structure (pore structure) of unidirectional array, the test-tube baby tissue of its fibrous tissue from the cell envelope structure of nanometer scale to micron dimension, arrive again the annual ring of millimeter magnitude, formed the biological structure characteristics such as unique multi-level, test-tube baby structure, fibrous and anisotropy.The principal constituent of wood (bamboo) material is xylogen, Mierocrystalline cellulose and hemicellulose, and carbon accounts for 44% in the main component.Thereby wood (bamboo) material not only can be made the synthetic stay in place form of biomimesis, and can be as carbon source and the stay in place form of preparation carbide composite material.In addition, compare with other material that comes from industrial chemicals, the outstanding advantage of wood (bamboo) material is its " renewable " property and " environmental protection ", meets the strategic idea of human social.Undoubtedly, wood (bamboo) material natural anisotropy graded porous structure has in preparation and has the advantageous advantage that other stay in place form can not be compared aspect the matrix material of special microstructure grading-hole.
Compare " soft template method " on the traditional sense, solvent evaporates induces self-assembly method to have: the selection of (1) solvent, precursor is diversity more; (2) precursor and template do not need that phase-splitting is precipitated out from solution, have reduced the control requirement to precursor and the collaborative assembling of template molecule; (3) preparation process simple to operate, save time fast.Therefore, solvent evaporates induces self-assembly method can be widely used in the preparation process of multiple mesoporous material.Obviously, reasonably utilize wood (bamboo) material biological template to induce self assembling process in conjunction with solvent evaporates, will be for our preparation has unique micropore, hierarchical porous structure functional materials mesoporous and macropore provides new approaches.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of grading-hole Carbon Materials.The present invention is take wood (bamboo) material as elementary template, and tensio-active agent is secondary template, and lacquer resins is presoma, prepares the Carbon Materials with hierarchical porous structure by means of confinement self-assembly and high temperature carbonization process.Preparation process of the present invention is simple, save time fast, production cost is low, can efficiently utilize the biological material such as wood (bamboo) material and improve its added value, the grading-hole Carbon Materials of the present invention's preparation has high specific surface area and graduate micropore, mesoporous and macroporous structure.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of preparation method of grading-hole Carbon Materials comprises the steps:
Under (1) 25 ~ 40 ℃, it is 1:(20 ~ 100 that a certain amount of tensio-active agent is dissolved in mass ratio) ethanol in, then add low order resol, fully stir and obtain clear soln.
(2) pretreated wood (bamboo) powder is joined the airtight vacuum pressurized tank, vacuumize, then inject a certain amount of step (1) solution, negative pressure of vacuum dipping 30 ~ 60 minutes.Take out, in 30～60 ℃ of lower volatilization desolventizings, drying, then 100～150 ℃ of lower curing 6～36 hours.
(3) under protective atmosphere, step (2) gained crude product is placed 600 ~ 1200 ℃ of charings of charring furnace 3 ~ 6 hours, temperature rise rate is 3 ~ 8 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Described tensio-active agent is a kind of in the triblock copolymers such as polyethylene oxide-poly(propylene oxide), oxyethane-polybutylene oxide, as being preferably non-ionic surfactant F127.
Described low order resol (M
w＜500) can pass through known technology: prepare such as the base catalyzed reactions between phenolic aldehyde and the formaldehyde.
Described wood (bamboo) powder is that size is 30 ~ 300 orders, and the mass ratio of wood powder and precursor liquid is 1:(1～9).
Described reducing atmosphere is a kind of in nitrogen, the argon gas or both mix, as being preferably argon gas.
Described high temperature carbonization is 600 ~ 1200 ℃.
Beneficial effect:
The present invention compares with existing " template ", " template-activation coupling method ", " exempting from template " etc., have following advantage: (1) is take wood (bamboo) material as first template, the secondary template of tensio-active agent, lacquer resins is presoma, utilizes confinement self-assembly and high temperature carbonization process to prepare to have micropore, the Carbon Materials of the hierarchical porous structure of mesoporous and macropore; (2) preparation process is simple, saves time fast, production cost is low; (3) can effectively utilize the biomass innovative development grading-hole Carbon Materials such as low-quality wood (bamboo) material, wood (bamboo) material residuum, improve its added value.
Description of drawings
Fig. 1 is the little angle x-ray diffraction pattern of the grading-hole Carbon Materials of embodiment 5 preparations.
Fig. 2 is the scanning electron microscope (SEM) photograph of the grading-hole Carbon Materials of embodiment 5 preparations.
Fig. 3 is the transmission electron microscope picture (a) of the grading-hole Carbon Materials of embodiment 5 preparations.
Fig. 4 is the transmission electron microscope picture (b) of the grading-hole Carbon Materials of embodiment 5 preparations.
Fig. 5 is the N of the grading-hole Carbon Materials of embodiment 5 preparations
2Adsorption-desorption curve (a).
Fig. 6 is the pore size distribution curve (b) of the grading-hole Carbon Materials of embodiment 5 preparations.
Embodiment
The below gives an actual example and describes the present invention.
Embodiment 1:
(1) with 6.1g phenol in 40 ~ 42 ℃ of lower meltings, adding the 1.3g mass percent and be 20% the NaOH aqueous solution stirred 10 minutes, splash into fast 10.5 g concentration and be 37% formalin, be warming up to 70 ~ 75 ℃ of reactions 1 hour, be cooled to room temperature, with the pH value of the HCI solution regulator solution of 0.6M near 7.0, in 50 ~ 52 ℃ of vacuum decompressions dehydrations 1 ~ 2 hour.The thick liquid that obtains is dissolved in 80g ethanol, and being made into mass percent is that 40% homogeneous solution is stand-by.
Under (2) 25 ℃, get 6.15g F127 and be dissolved in the 43.1g ethanol, stirred 2 hours, then add the low order phenol resin solution that 30g step (1) is prepared, continue to stir 1 hour, obtain settled solution.
(3) wood after the 10g alligatoring (bamboo) powder is transferred to airtight vacuum pressed tank, be evacuated to 0.09Mpa, then inject the solution of 80g step (2) preparation, negative pressure of vacuum dipping 45 minutes, slowly emptying.Take out wood (bamboo) powder after flooding, place 35 ℃ of lower volatilization desolventizings of unlimited vessel, dryings, then 105 ℃ of lower curing 8 hours.
(4) under argon shield atmosphere, step (3) gained crude product is placed 700 ℃ of charings of charring furnace 4 hours, temperature rise rate is 3 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Embodiment 2:
(1) with 6.1g phenol in 40 ~ 42 ℃ of lower meltings, adding the 1.3g mass percent and be 20% the NaOH aqueous solution under this temperature stirred 10 minutes, add 10.5 g concentration and be 37% formalin, be warming up to 70 ~ 75 ℃ of reactions 1 hour, be cooled to room temperature, with the pH value of 0.6M HCI solution regulator solution near 7.0, in 50 ~ 52 ℃ of vacuum decompressions dehydrations 1 ~ 2 hour.The thick liquid that obtains is dissolved in 80g ethanol, and to be made into mass percent be that 40% homogeneous solution is stand-by.
Under (2) 40 ℃, get 10g F127 and be dissolved in the 70g ethanol, stirred 2 hours, then add the low order resol ethanolic soln that 50g step (1) is prepared, continue to stir 1 hour, obtain clear sol.
(3) wood after the 10g alligatoring (bamboo) powder is transferred to the airtight vacuum pressurized tank, be evacuated to 0.09Mpa, then inject the solution of 130g step (2) preparation, negative pressure of vacuum dipping 60 minutes, slowly emptying.Take out wood (bamboo) powder after flooding, place unlimited vessel in 40 ℃ of lower volatilization desolventizings, dryings, then 150 ℃ of lower curing 6 hours.
(4) under nitrogen protection atmosphere, step (3) gained crude product is placed 900 ℃ of charings of charring furnace 4.5 hours, temperature rise rate is 4 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Embodiment 3:
(1) with 6.1g phenol in 40 ~ 42 ℃ of lower meltings, adding the 1.3g mass percent and be 20% the NaOH aqueous solution under this temperature stirred 10 minutes, add 10.5 g concentration and be 37% formalin, be warming up to 70 ~ 75 ℃ of reactions 1 hour, be cooled to room temperature, with the pH value of 0.6M HCI solution regulator solution near 7.0, in 50 ~ 52 ℃ of vacuum decompressions dehydrations 1 ~ 2 hour.The thick liquid that obtains is dissolved in 80g ethanol, and to be made into mass percent be that 40% homogeneous solution is stand-by.
Under (2) 30 ℃, get 4.62g F127 and be dissolved in the 32.3g ethanol, stirred 1.5 hours, then add the low order resol ethanolic soln that 23.08g step (1) is prepared, continue to stir 1.5 hours, obtain clear sol.
(3) wood after 10 alligatoring (bamboo) powder is transferred to the airtight vacuum pressurized tank, be evacuated to 0.09Mpa, then inject the solution of 60g step (2) preparation, negative pressure of vacuum dipping 30 minutes, slowly emptying.Take out wood (bamboo) powder after flooding, place 45 ℃ of lower volatilization desolventizings of unlimited vessel, dryings, then 100 ℃ of lower curing 10 hours.
(4) under argon shield atmosphere, step (3) gained crude product is placed 700 ℃ of charings of charring furnace 3 hours, temperature rise rate is 6 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Embodiment 4:
(1) with 6.1g phenol in 40 ~ 42 ℃ of lower meltings, adding the 1.3g mass percent and be 20% the NaOH aqueous solution under this temperature stirred 10 minutes, add 10.5 g concentration and be 37% formalin, be warming up to 70 ~ 75 ℃ of reactions 1 hour, be cooled to room temperature, with the pH value of 0.6M HCI solution regulator solution near 7.0, in 50 ~ 52 ℃ of vacuum decompressions dehydrations 1 ~ 2 hour.The thick liquid that obtains is dissolved in 80g ethanol, and to be made into mass percent be that 40% homogeneous solution is stand-by.
Under (2) 30 ℃, get 7.69g F127 and be dissolved in the 53.85g ethanol, stirred 1 hour, then add the low order resol ethanolic soln that 38.46g step (1) is prepared, continue to stir 1.5 hours, obtain settled solution.
(3) wood after 10 alligatoring (bamboo) powder is transferred to the airtight vacuum pressurized tank, be evacuated to 0.09Mpa, then inject the solution of 100g step (2) preparation, negative pressure of vacuum dipping 30 minutes, slowly emptying.Take out wood (bamboo) powder after flooding, place unlimited vessel in 45 ℃ of lower volatilization desolventizings, dryings, then 105 ℃ of lower curing 12 hours.
(4) under nitrogen protection atmosphere, step (3) gained crude product is placed 700 ℃ of charings of charring furnace 3 hours, temperature rise rate is 5 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Embodiment 5:
(1) with 6.1g phenol in 40 ~ 42 ℃ of lower meltings, adding the 1.3g mass percent and be 20% the NaOH aqueous solution under this temperature stirred 10 minutes, add 10.5 g concentration and be 37% formalin, be warming up to 70 ~ 75 ℃ of reactions 1 hour, be cooled to room temperature, with the pH value of 0.6M HCI solution regulator solution near 7.0, in 50 ~ 52 ℃ of vacuum decompressions dehydrations 1 ~ 2 hour.The thick liquid that obtains is dissolved in 80g ethanol, and to be made into mass percent be that 40% homogeneous solution is stand-by.
Under (2) 40 ℃, get 12g F127 and be dissolved in the 84g ethanol, stirred 1 hour, then add the solution of 60g step (1) preparation, continue to stir 1 hour, obtain settled solution.
(3) wood after the 10g alligatoring (bamboo) powder is transferred to the airtight vacuum pressurized tank, be evacuated to 0.095Mpa, then inject the solution that 130g step (2) is prepared, negative pressure of vacuum dipping 60 minutes, slowly emptying.Take out wood (bamboo) powder after flooding, place 40 ℃ of lower volatilization desolventizings of unlimited vessel, dryings, then 120 ℃ of lower curing 24 hours.
(4) under argon shield atmosphere, step (3) gained crude product is placed 900 ℃ of charings of charring furnace 4 hours, temperature rise rate is 3 ℃/min, can obtain a kind of grading-hole Carbon Materials.
Fig. 1 can find out that for this little angle x-ray diffraction pattern of executing the prepared grading-hole Carbon Materials of example this matrix material has obvious mesoscopic structure characteristic diffraction peak.
Fig. 2 is the scanning electron microscope (SEM) photograph of the prepared grading-hole Carbon Materials of this embodiment, can find out the microtexture of this material, has kept the natural micropore structure of first template (timber).
Fig. 3,4 is the transmission electron microscope picture of the prepared grading-hole Carbon Materials of this embodiment, such as figure (a) with (b), has showed clearly micropore and the meso-hole structure of this matrix material.
Fig. 5 and Fig. 6 are the N of the prepared grading-hole Carbon Materials of this embodiment
2Adsorption-desorption curve (a) and corresponding pore size distribution curve (b).Adopt specific surface area, pore volume and the pore size distribution of the ASAP2010 nitrogen adsorption instrument test grading hole Carbon Materials of U.S. Micromeritics company.The result shows that the specific surface area of this material is 568.3m
2/ g, pore volume are 0.35cm
3/ g.From the nitrogen adsorption isothermal curve, can find out to have obvious micropore and mesoporous adsorpting characteristic, consistent with the TEM test result.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (7)
1. the preparation method of a grading-hole Carbon Materials is characterized in that, comprises the steps:
Under (1) 25 ~ 40 ℃, get proper amount of surfactant and be dissolved in a certain amount of ethanol, then add low order resol, fully stir and obtain clear soln;
(2) pretreated wood (bamboo) powder is joined the airtight vacuum pressurized tank, vacuumize, then inject a certain amount of step (1) solution, negative pressure of vacuum dipping 30 ~ 60 minutes, take out, in 30 ~ 60 ℃ of lower volatilization desolventizings, drying, then 100 ~ 150 ℃ of lower curing 6 ~ 36 hours;
(3) under protective atmosphere, step (2) gained crude product was placed the charring furnace high temperature carbonization 3 ~ 6 hours, temperature rise rate is 3 ~ 8 ℃/min, can obtain a kind of grading-hole Carbon Materials.
2. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 is characterized in that, the mass ratio of described tensio-active agent and ethanol is 1:(20 ~ 100); The mass ratio of low order resol and ethanol is 1:(6 ~ 40).
3. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 and 2 is characterized in that, described tensio-active agent is the tensio-active agent (EO such as triblock copolymer such as polyethylene oxide-poly(propylene oxide), oxyethane-polybutylene oxide
nPO
mEO
n, EO
nBO
mEO
n) in one or more mixture, as being preferably EO
106PO
70EO
106(F127).
4. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 and 2 is characterized in that, described resol is low-molecular-weight lacquer resins prepolymer (M
w＜500).
5. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 and 2 is characterized in that, described wood (bamboo) powder is 30 ~ 300 orders, and the mass ratio of the mixed solution of wood (bamboo) powder and step (1) is 1:(1 ~ 9).
6. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 is characterized in that, described protective atmosphere is a kind of or both mixing in nitrogen, the argon gas.
7. the preparation method of a kind of grading-hole Carbon Materials according to claim 1 is characterized in that, the carbonization temperature described in the step (3) is 600 ~ 1200 ℃.
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| CN107381535A (en) * | 2017-09-15 | 2017-11-24 | 青岛科技大学 | A kind of method for preparing order mesoporous carbon microspheres |
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