CN109317063B - Carbon aerogel and preparation method thereof - Google Patents
Carbon aerogel and preparation method thereof Download PDFInfo
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- CN109317063B CN109317063B CN201811522335.4A CN201811522335A CN109317063B CN 109317063 B CN109317063 B CN 109317063B CN 201811522335 A CN201811522335 A CN 201811522335A CN 109317063 B CN109317063 B CN 109317063B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
Abstract
The invention discloses a carbon aerogel and a preparation method thereof, relating to the field of carbon material preparation, wherein the preparation method of the carbon aerogel comprises the following steps: dissolving resorcinol and formaldehyde in water, and reacting under the condition of an alkaline catalyst to form a resorcinol-formaldehyde solution; standing the resorcinol-formaldehyde solution to form a resorcinol-formaldehyde gel system; freezing the resorcinol-formaldehyde gel system at-120 to-170 ℃ to form a resorcinol-formaldehyde gel system; performing vacuum drying on the resorcinol-formaldehyde gel system, and then placing the resorcinol-formaldehyde gel system in a graphite mold; and placing the graphite mold into a discharge plasma sintering furnace, sintering under a vacuum condition, and cooling to obtain the carbon aerogel. According to the preparation method of the carbon aerogel, the microstructure in the carbon aerogel material is slightly damaged in the preparation process, and the prepared carbon aerogel material has a pore structure which is distributed in a continuous gradient state.
Description
Technical Field
The invention relates to the field of carbon material preparation, and particularly relates to a carbon aerogel and a preparation method thereof.
Background
The carbon aerogel has low density, high specific surface area, continuous pore structure and good high temperature resistance and corrosion resistance, so that the carbon aerogel has wide application prospect in the fields of adsorption and catalysis, and the potential application value of the carbon aerogel arouses great interest of researchers. At present, the existing methods for preparing carbon aerogel mainly focus on high-temperature carbonization methods, and organic precursors are heated and carbonized in a high-temperature furnace under the protection of inert gas or under a vacuum condition to prepare carbon aerogel materials; however, the carbon aerogel prepared by the preparation method has irregular pore structure, and the adsorption and filtration characteristics of the carbon aerogel material are seriously restricted.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In order to solve the technical defects, the invention adopts the technical scheme that the preparation method of the carbon aerogel comprises the following steps:
dissolving resorcinol and formaldehyde in water, and reacting under the condition of an alkaline catalyst to form a resorcinol-formaldehyde solution;
standing the resorcinol-formaldehyde solution to form a resorcinol-formaldehyde gel system;
freezing the resorcinol-formaldehyde gel system at-120 to-170 ℃ to form a resorcinol-formaldehyde gel system;
performing vacuum drying on the resorcinol-formaldehyde gel system, and then placing the resorcinol-formaldehyde gel system in a graphite mold;
and placing the graphite mold into a discharge plasma sintering furnace, sintering under a vacuum condition, and cooling to obtain the carbon aerogel.
Alternatively, the reaction of resorcinol and formaldehyde in water under basic catalyst conditions comprises:
dissolving 2-10g of resorcinol and 8-16ml of formaldehyde in 20-100ml of distilled water, and adjusting the pH value to 7-11 to form a mixed solution;
adding 0.04-1g of sodium carbonate into the mixed solution, and stirring and reacting for 1-2h at room temperature.
Optionally, said allowing the resorcinol-formaldehyde solution to stand comprises: the resorcinol-formaldehyde solution is allowed to stand at 50 ℃ and then at 80 ℃.
Optionally, the resorcinol-formaldehyde solution is allowed to stand at 50 ℃ for 2-4h and at 80 ℃.
Optionally, the freezing time of the resorcinol-formaldehyde gel system at-120 ℃ to-170 ℃ is 1-2 h.
Optionally, the vacuum drying the resorcinol-formaldehyde jelly system comprises: and (3) carrying out vacuum drying on the resorcinol-formaldehyde gel system at the temperature of between 40 ℃ below zero and 120 ℃ below zero, and then carrying out vacuum drying at the temperature of between 150 ℃ and 200 ℃.
Optionally, the resorcinol-formaldehyde gel system is dried under vacuum at-40 ℃ to-120 ℃ for 4-6h, and at 150 ℃ to 200 ℃ for 2-6 h.
Optionally, the step of placing the graphite mold into a spark plasma sintering furnace for sintering under vacuum conditions includes: and (3) putting the graphite mold into a discharge plasma sintering furnace, heating to 800-1200 ℃ at the speed of 50-150 ℃/min, and preserving heat for 5-10 minutes.
Another object of the present invention is to provide a carbon aerogel, which is prepared by the above method for preparing a carbon aerogel.
Optionally, the carbon aerogel has a gradient pore structure.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method of the carbon aerogel provided by the invention has the advantages of simple preparation process, low energy consumption, short preparation period and small damage to the microstructure of the pores in the carbon aerogel material in the preparation process, and the prepared carbon aerogel material has a pore structure which is complete and regular and is distributed in a continuous gradient state.
2, the carbon aerogel material prepared by the invention has a complete and regular pore structure which is distributed in a continuous gradient state.
3, when the carbon aerogel material with the continuous gradient pore structure is used for adsorption and filtration, the effect of layer-by-layer filtration can be achieved, namely large-particle substances can be filtered firstly, small-particle substances can be filtered, and micron-sized particles are adsorbed by the microporous structure, so that the adsorption and filtration characteristics of the carbon aerogel material can be improved, and the application range of the carbon aerogel material is greatly expanded.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below.
FIG. 1 is an SEM image of a carbon aerogel material prepared according to the present invention;
FIG. 2 is a schematic illustration of the freezing of a resorcinol-formaldehyde gel system according to the present invention;
FIG. 3 is a flow diagram of a carbon aerogel material prepared according to the present invention.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
In order to solve the problem that the microstructure of a carbon aerogel material is greatly damaged by the existing preparation method of the carbon aerogel, so that the adsorption and filtration characteristics of the prepared carbon aerogel material are restricted, the invention provides the preparation method of the carbon aerogel. The carbon aerogel prepared by the method has a pore structure with continuous gradient, so that the pore structure of the carbon aerogel prepared by the method is regular and ordered, and the adsorption and filtration characteristics of the carbon aerogel material can be improved.
Referring to fig. 3, the preparation method of the carbon aerogel provided by the invention specifically comprises the following steps:
dissolving resorcinol and formaldehyde in water, and reacting under the condition of an alkaline catalyst to form a resorcinol-formaldehyde solution;
standing the resorcinol-formaldehyde solution to form a resorcinol-formaldehyde gel system;
freezing the resorcinol-formaldehyde gel system at-120 to-170 ℃ to form a resorcinol-formaldehyde gel system;
performing vacuum drying on the resorcinol-formaldehyde gel system, and then placing the resorcinol-formaldehyde gel system in a graphite mold;
and (3) placing the graphite mold into a discharge plasma sintering furnace, sintering under a vacuum condition, and cooling to obtain the carbon aerogel.
In the preparation method, resorcinol and formaldehyde are mixed under the condition of an alkaline catalyst, the resorcinol and the formaldehyde are subjected to polycondensation reaction to form a resorcinol-formaldehyde (RF) solution, the prepared resorcinol-formaldehyde solution is further kept stand, chemical bonds in adjacent polycondensation products are combined in the standing process, and the polycondensation reaction is continued; along with the progress of the polycondensation reaction, the molecular weight of the product is larger and larger, and the viscosity of the resorcinol-formaldehyde solution is gradually increased until the product loses fluidity to form a resorcinol-formaldehyde gel system; wherein water molecules in the solution, byproducts generated in the reaction process, impurities in the raw materials and other small molecular substances are uniformly settled in the resorcinol-formaldehyde gel system along with the reaction.
Wherein, the resorcinol and the formaldehyde are dissolved in water and react under the condition of an alkaline catalyst, and the reaction comprises the following steps:
dissolving 2g-10g of resorcinol and 8ml-16ml of formaldehyde in 20ml-100ml of distilled water, and adjusting the pH value to 7-11 to form a mixed solution;
adding 0.04g-1g of basic catalyst into the mixed solution, and stirring for reaction at room temperature for 1-2 h.
The method for adjusting the pH value can be a pH value adjusting method commonly used in the chemical field, and the pH value is preferably adjusted by using 0.1mol/L NaOH solution.
The alkaline catalyst in the invention is sodium carbonate or potassium carbonate, and the alkaline catalyst is preferably sodium carbonate in the invention. In order to ensure that the reactants can be uniformly mixed and fully react, the catalyst is added into the mixed solution and then stirred so as to improve the conversion rate of the reactants.
In order to convert the prepared resorcinol-formaldehyde solution into a gel system, the resorcinol-formaldehyde solution is kept stand for a certain time to promote the polycondensation reaction to finally form the gel system. Because the reaction speed of the polycondensation reaction and the molecular weight of the polycondensation product are different at different temperatures, in order to reduce the defect of a pore structure generated in the formation process of a gel system and avoid damaging the microstructure of the pore structure, the carbon aerogel preparation method provided by the invention comprises the following steps of standing the resorcinol-formaldehyde solution: and standing the resorcinol-formaldehyde solution at 50 ℃ and then at 80 ℃, wherein the standing time of the resorcinol-formaldehyde solution at 50 ℃ and the standing time at 80 ℃ are both 2-4 h.
The prepared resorcinol-formaldehyde gel system is deeply frozen at the temperature of-120 ℃ to-170 ℃, adjacent molecules in the resorcinol-formaldehyde gel system are combined through van der Waals force due to rapid temperature reduction to form a space network structure, and water molecules and other impurity small molecular substances are dispersed in gaps of the network structure to form the resorcinol-formaldehyde gel system. In the freezing process, the freezing speed is gradually reduced from the surface to the inside of the resorcinol-formaldehyde gel system, so that the freezing degree is gradually reduced from the surface to the inside of the resorcinol-formaldehyde gel system, and the gaps of a space network structure formed in the system are gradually reduced from the surface to the inside and are distributed in a continuous gradient manner. The invention preferably freezes the resorcinol-formaldehyde gel system at-120 ℃ to-170 ℃ for 1-2 h.
The deep freezing can be performed by putting the resorcinol-formaldehyde gel system into a container with a cold source, and then freezing the container in a low-temperature environment, as shown in fig. 2.
Further carrying out vacuum drying on the prepared resorcinol-formaldehyde gel system, removing water molecules and impurity small molecules, placing the resorcinol-formaldehyde gel system in a graphite mold, and sintering in a discharge plasma sintering furnace under a vacuum condition; in the sintering process, the conductive characteristic of graphite is utilized, and a plasma heating mode is adopted to heat the resorcinol-formaldehyde gel system to instantly generate high temperature and excite the reaction activity, so that the resorcinol-formaldehyde gel system is instantly carbonized to form a space network structure, and meanwhile, byproducts are volatilized at high temperature; after cooling, a carbon aerogel material was obtained.
Because the gaps of the space network structure formed in the resorcinol-formaldehyde jelly system are gradually reduced from the surface to the inside and are distributed in a continuous gradient manner, the gaps in the resorcinol-formaldehyde jelly system form a porous structure during sintering, and the formed porous structure maintains the structural characteristic that the gaps in the jelly system are distributed in a continuous gradient manner, so that the prepared carbon aerogel material has a continuous gradient pore structure.
Specifically, after the resorcinol-formaldehyde gel system is frozen for 1-2 hours at-120 to-170 ℃ to prepare the resorcinol-formaldehyde gel system, the vacuum drying of the resorcinol-formaldehyde gel system comprises the following steps: carrying out vacuum drying on the resorcinol-formaldehyde gel system at the temperature of-40 to-120 ℃, and then carrying out vacuum drying at the temperature of 150 to 200 ℃; the invention preferably selects the resorcinol-formaldehyde jelly system to be dried in vacuum for 4-6h at-40 ℃ to-120 ℃ and 2-6h at 150 ℃ to 200 ℃.
Because water molecules and other small molecular impurities exist in the resorcinol-formaldehyde gel system, the vacuum drying process of the resorcinol-formaldehyde gel system is divided into two steps, firstly, the resorcinol-formaldehyde gel system is vacuum dried at the temperature of minus 40 ℃ to minus 120 ℃, so that the water molecules in the gel system are directly sublimated, and the water molecules are removed; and then vacuum drying at 150-200 ℃ to remove other impurity small molecules except water in the jelly glue system so as to reduce the impurity content in the carbon aerogel material and improve the performance of the carbon aerogel material, and simultaneously, after the impurities in the gaps of the jelly glue system are removed, a pore structure is formed so that the carbon aerogel material formed after further sintering has a continuous gradient distribution pore structure.
The graphite mold is placed into a discharge plasma sintering furnace to be sintered under the vacuum condition, and the sintering process comprises the following steps: and (3) putting the graphite mold into a discharge plasma sintering furnace, heating to 800-1200 ℃ at the speed of 50-150 ℃/min under the vacuum condition, and preserving the heat for 5-10 minutes.
In the sintering process, the temperature is raised in a step heating mode to control the heating speed, so that all components in the resorcinol-formaldehyde gel system can fully react, and the occurrence of side reactions is reduced.
The preparation method of the carbon aerogel provided by the invention has the advantages of low energy consumption and short production period, and the prepared carbon aerogel material has a complete and regular pore structure and is distributed in a continuous gradient manner, so that the adsorption and filtration characteristics of the carbon aerogel material can be improved.
When the carbon aerogel material with the continuous gradient pore structure is used for adsorption and filtration, the effect of layer-by-layer filtration can be achieved, namely large-particle substances can be filtered firstly, small-particle substances can be filtered, and micron-sized particles are adsorbed by the microporous structure, so that the application range of the carbon aerogel material is greatly expanded.
Example one
The embodiment provides a preparation method of carbon aerogel, which specifically comprises the following steps:
s1: dissolving 2g of resorcinol and 8ml of formaldehyde in 20ml of distilled water, and adjusting the pH value to 7 to obtain a mixed solution;
s2: adding 0.04g of sodium carbonate into the mixed solution, and stirring and reacting for 1h at room temperature to obtain a resorcinol-formaldehyde solution;
s3: standing the resorcinol-formaldehyde solution at 50 ℃ for 2h, and then standing at 80 ℃ for 2h to form a resorcinol-formaldehyde gel system;
s4: freezing the resorcinol-formaldehyde gel system at-120 ℃ for 1h to form a resorcinol-formaldehyde gel system;
s5: carrying out vacuum drying on the resorcinol-formaldehyde gel system at the temperature of-40 ℃ for 4h, and then carrying out vacuum drying at the temperature of 150 ℃ for 2h to obtain a dried resorcinol-formaldehyde gel system;
s6: and (3) placing the dried resorcinol-formaldehyde gel system in a graphite mold, placing the graphite mold in a discharge plasma sintering furnace, heating to 800 ℃ at the speed of 50 ℃/min under a vacuum condition, preserving the temperature for 5 minutes, and cooling to obtain the carbon aerogel.
In the preparation method of the carbon aerogel provided by the embodiment, a resorcinol-formaldehyde gel system is generated by resorcinol and formaldehyde in the presence of an alkaline catalyst, and a resorcinol-formaldehyde gel system is formed after deep freezing; and (3) further drying the resorcinol-formaldehyde gel system in vacuum, and sintering the resorcinol-formaldehyde gel system in a discharge plasma sintering furnace to obtain the carbon aerogel material.
Fig. 1 is a Scanning Electron Microscope (SEM) photograph of the carbon aerogel material prepared in this embodiment, in fig. 1, a dark portion is a pore structure, and a light portion is a carbon aerogel skeleton, and it can be seen from the drawing that a dark stripe-shaped pore structure is tapered from top to bottom, which proves that the pore diameter of the pore structure in the carbon aerogel material prepared in this embodiment is gradually reduced from top to bottom, and the pore structure is distributed in a continuous gradient state.
The preparation method of the carbon aerogel provided by the embodiment has the advantages of simple preparation process, low energy consumption, short preparation period and small damage to the microstructure of the pores in the carbon aerogel material in the preparation process, and the prepared carbon aerogel material has a pore structure which is complete and regular and is distributed in a continuous gradient state.
When the carbon aerogel material with the continuous gradient pore structure is used for adsorption and filtration, the effect of layer-by-layer filtration can be achieved, namely large-particle substances can be filtered firstly, small-particle substances can be filtered, and micron-sized particles are adsorbed by the microporous structure, so that the adsorption and filtration characteristics of the carbon aerogel material can be improved, and the application range of the carbon aerogel material is greatly expanded.
Example two
Different from the first embodiment, the preparation method of the carbon aerogel in the present embodiment includes the following steps:
s1: dissolving 6g of resorcinol and 12ml of formaldehyde in 60ml of distilled water, and adjusting the pH value to 9 to obtain a mixed solution;
s2: adding 0.7g of sodium carbonate into the mixed solution, and stirring and reacting for 1.5h at room temperature to obtain a resorcinol-formaldehyde solution;
s3: standing the resorcinol-formaldehyde solution at 50 ℃ for 3h, and then standing at 80 ℃ for 3h to form a resorcinol-formaldehyde gel system;
s4: freezing the resorcinol-formaldehyde gel system at-150 ℃ for 1.5h to form a resorcinol-formaldehyde gel system;
s5: carrying out vacuum drying on the resorcinol-formaldehyde gel system at-80 ℃ for 5h, and then carrying out vacuum drying at 180 ℃ for 4h to obtain a dried resorcinol-formaldehyde gel system;
s6: and (3) placing the dried resorcinol-formaldehyde gel system in a graphite mold, placing the graphite mold in a discharge plasma sintering furnace, heating to 1000 ℃ at the speed of 100 ℃/min under a vacuum condition, preserving the temperature for 8 minutes, and cooling to obtain the carbon aerogel.
The preparation method of the carbon aerogel provided by the embodiment has the advantages of simple preparation process, low energy consumption, short preparation period and small damage to the microstructure of the pores in the carbon aerogel material in the preparation process, and the prepared carbon aerogel material has a pore structure which is complete and regular and is distributed in a continuous gradient state.
An SEM image of the carbon aerogel material prepared in this example is shown in fig. 1, and a detailed analysis process refers to relevant contents of some examples, which are not described herein again.
EXAMPLE III
Different from the first embodiment, the preparation method of the carbon aerogel in the present embodiment includes the following steps:
s1: dissolving 10g of resorcinol and 16ml of formaldehyde in 100ml of distilled water, and adjusting the pH value to 11 to obtain a mixed solution;
s2: adding 1g of sodium carbonate into the mixed solution, and stirring and reacting for 2 hours at room temperature to obtain a resorcinol-formaldehyde solution;
s3: standing the resorcinol-formaldehyde solution at 50 ℃ for 4h, and then standing at 80 ℃ for 4h to form a resorcinol-formaldehyde gel system;
s4: freezing the resorcinol-formaldehyde gel system at-170 ℃ for 2h to form a resorcinol-formaldehyde gel system;
s5: carrying out vacuum drying on the resorcinol-formaldehyde gel system at-120 ℃ for 6h, and then carrying out vacuum drying at 200 ℃ for 6h to obtain a dried resorcinol-formaldehyde gel system;
s6: and (3) placing the dried resorcinol-formaldehyde gel system in a graphite mold, placing the graphite mold in a discharge plasma sintering furnace, heating to 1200 ℃ at the speed of 150 ℃/min under a vacuum condition, preserving the temperature for 10 minutes, and cooling to obtain the carbon aerogel.
The preparation method of the carbon aerogel provided by the embodiment has the advantages of simple preparation process, low energy consumption, short preparation period and small damage to the microstructure of the pores in the carbon aerogel material in the preparation process, and the prepared carbon aerogel material has a pore structure which is complete and regular and is distributed in a continuous gradient state.
An SEM image of the carbon aerogel material prepared in this example is shown in fig. 1, and a detailed analysis process refers to relevant contents of some examples, which are not described herein again.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. A preparation method of carbon aerogel with a gradient pore structure is characterized by comprising the following steps:
dissolving 2-10g of resorcinol and 8-16ml of formaldehyde in 20-100ml of distilled water, and adjusting the pH value to 7-11 to form a mixed solution;
adding 0.04-1g of sodium carbonate into the mixed solution, and stirring and reacting for 1-2h at room temperature to form a resorcinol-formaldehyde solution;
standing the resorcinol-formaldehyde solution to form a resorcinol-formaldehyde gel system;
freezing the resorcinol-formaldehyde gel system at-120 to-170 ℃ to form a resorcinol-formaldehyde gel system;
the resorcinol-formaldehyde jelly system is dried in vacuum at the temperature of-40 ℃ to-120 ℃, then dried in vacuum at the temperature of 150 ℃ to 200 ℃, and then placed in a graphite mold;
and (3) putting the graphite mold into a discharge plasma sintering furnace, heating to 800-1200 ℃ at the speed of 50-150 ℃/min under the vacuum condition, preserving the temperature for 5-10 minutes, and cooling to obtain the carbon aerogel with the gradient pore structure.
2. The method of preparing a carbon aerogel having a gradient pore structure according to claim 1, wherein said allowing the resorcinol-formaldehyde solution to stand comprises: the resorcinol-formaldehyde solution is allowed to stand at 50 ℃ and then at 80 ℃.
3. The method for preparing a carbon aerogel having a gradient pore structure according to claim 2, wherein the time for allowing the resorcinol-formaldehyde solution to stand at 50 ℃ and the time for allowing the resorcinol-formaldehyde solution to stand at 80 ℃ are both 2 to 4 hours.
4. The method for preparing carbon aerogel having gradient pore structure according to claim 1, wherein the time for freezing the resorcinol-formaldehyde gel system at-120 ℃ to-170 ℃ is 1-2 h.
5. The method for preparing carbon aerogel with gradient pore structure according to claim 1, wherein the resorcinol-formaldehyde gel system is dried under vacuum at-40 ℃ to-120 ℃ for 4-6h, and at 150 ℃ to 200 ℃ for 2-6 h.
6. A carbon aerogel having a gradient pore structure, which is prepared by the method for preparing a carbon aerogel having a gradient pore structure according to any one of claims 1 to 5.
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