CN110590362A - Preparation method of pore structure-controllable high-strength grade pore carbon monolithic column - Google Patents
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- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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Abstract
The invention relates to a preparation method of a pore structure-controllable high-strength grade pore carbon monolithic column. The method uses resorcinol (R) and formaldehyde (F) as reaction monomers, uses water (H) as a solvent, and regulates and controls the micro-pore structure of the carbon monolithic column by changing the mass ratio of water, formaldehyde solute and resorcinol and the water bath gel temperature. Specifically, water, formaldehyde solute and resorcinol are mixed according to a certain mass ratio to obtain sol, gel aging is carried out at a certain temperature, and the sol is dried under normal pressure and then carbonized under a vacuum condition to obtain the carbon monolithic column. The carbon monolithic column preparation system and the preparation process provided by the invention are simple and rapid, have low equipment requirements, can be used for preparing high-strength graded porous carbon monolithic columns, and are a method beneficial to industrial production of carbon monolithic columns.
Description
The technical field is as follows:
the invention belongs to the technical field of material preparation, and particularly relates to a preparation method of a pore structure-controllable high-strength grade pore carbon monolithic column.
Background art:
since Pekala synthesized carbon monolith materials for the first time at the end of the 80 s of the 20 th century [ r.w.pekala, j.mater.sci.,1989,24,3221], carbon monolith materials have been widely studied and used in capacitor electrode materials, heat insulating materials, adsorption and catalyst supports, etc. Because the preparation and removal of carbon monoliths is simple relative to silica monoliths, it is also suitable for use as a hard template to prepare other monoliths that are not easily prepared by similar methods [ t.kubo, n.tsujioka, n.tanaka and k.hosoya, mater.lett.,2010,64,177 ].
The main methods for preparing the carbon monolithic column include a sol-gel method and a hard template method, wherein the raw materials comprise resorcinol, phenol, melamine and the like, and the sol-gel method taking resorcinol as the raw material can conveniently realize the control of the pore structure of the carbon monolithic column and is more emphasized. However, some of the problems faced by this method also severely restrict its practical application. For example, it has been reported that the pH of a reaction precursor is adjusted by adding an acidic or basic catalyst, and drying is performed by a method such as supercritical drying or freeze drying after solvent substitution, thereby achieving the purpose of controlling the microscopic pore structure of a carbon monolith column [ s.a.alcumhtaseb and j.a.ritter, adv.mater.,2003,15,101 ]. Obviously, the process is complex, long in period and high in cost, and is not beneficial to large-scale industrial production. In addition, according to literature reports, the strength of the Carbon monolith column currently prepared is not high, such as 5MPa [ x.f.jia, b.w.dai, z.x.zhu, j.t.wang, w.m.qiao, d.h.long and dl.c.link, Carbon,2016,108,551] reported by Jia et al, 3.75MPa [ c.s.ye, r.b.zhang, z.m.an and b.l.wang, adv.appl.ceram, 2018,117,468] reported by Ye et al, which limits its practical application.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provide a preparation method of a pore-structure-controllable high-strength-grade pore carbon monolithic column.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a pore structure-controllable high-strength grade pore carbon monolithic column comprises the following steps:
(1) mixing water, formaldehyde solution and resorcinol according to a ratio to obtain uniform sol; wherein, according to the mass ratio, the water (H): formaldehyde solute (F): resorcinol (R) ═ 1.2-3.9 (0.2-0.7):1, preferably in the range of (1.99-2.32): 0.45-0.52):1, and water comprises water in the formaldehyde solution;
(2) sealing and aging the sol under a heating condition to obtain wet gel, wherein the heating temperature is 35-100 ℃, and the aging time is 4-36 h;
(3) drying the wet gel to obtain a resin monolithic column, and carbonizing at high temperature to obtain a carbon monolithic column, wherein the carbonization temperature is 700-900 ℃, and the heat preservation time is 2-3 h.
In the step (1), the mass fraction of the formaldehyde solution is 38%.
In the step (2), the heating mode is water bath heating, and the preferable water bath heating temperature is 35-85 ℃.
In the step (3), the wet gel drying mode is as follows: drying at room temperature for 10-24h, and drying in oven at 40-60 deg.C for 8-36 h.
In the step (3), the resin monolithic column has complete column body and no crack, and the micro-pore structure is controllable and regular.
In the step (3), the strength of the carbon monolithic column reaches 14.31-24.6 MPa.
In the step (3), the carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.26-1.85cm3.g-1Wherein the pore volume of the micropores is 0.15-0.26cm3.g-1The average pore diameter of the macropores is 0.28-4.49 μm, and the specific surface area is 363-567m2.g-1。
According to the invention, researches show that the mass ratio of H/F/R and the water bath gel temperature have decisive influence on the regulation and control of the micro-pore structure of the carbon monolithic column. When the mass ratio of H/F/R is 2.32:0.45:1, the carbon monolithic column prepared under the condition of water bath gel at 85 ℃ not only has a better three-dimensional network interconnection structure, but also has higher strength.
The patent provides a novel method for simply, conveniently and controllably preparing a high-strength grade porous carbon monolithic column. The method comprises the steps of obtaining a reactant precursor by simply regulating and controlling the mass ratio of resorcinol to formaldehyde to water, gelling under a proper condition, and drying and carbonizing at normal pressure to obtain the hierarchical porous carbon monolithic column interconnected by a three-dimensional network.
The invention has the beneficial effects that:
(1) the preparation system used by the method is a ternary simple system: only resorcinol, formaldehyde solution and deionized water are needed;
(2) the continuous adjustment of the pore structure can be realized by simply changing the mass ratio of reactants and the temperature of water bath gel;
(3) the prepared carbon monolithic column is of a hierarchical pore structure, and has good three-dimensional interconnectivity and uniform pore size distribution;
(4) drying at normal pressure to obtain a carbon monolithic column with complete macro and micro structures;
(5) the strength of the carbon monolithic column can reach 24.6MPa at most.
Description of the drawings:
fig. 1 is a scanning electron micrograph, a mechanical property compression curve, a nitrogen adsorption and desorption curve, and a pore size distribution diagram of the high strength carbon monolith H2.32F0.45R1 prepared in example 1; wherein, fig. 1(a1) and fig. 1(a2) are scanning electron micrographs with different multiples, fig. 1(A3) is a mechanical property compression curve, fig. 1(a4) is a nitrogen adsorption and desorption curve, fig. 1(a5) is a micropore size distribution diagram, and fig. 1(a6) is a macropore size distribution diagram;
fig. 2 is a scanning electron micrograph, a mechanical property compression curve, a nitrogen adsorption and desorption curve, and a pore size distribution diagram of the high strength carbon monolith H2.32F0.52R1 prepared in example 2; wherein, fig. 2(a1) and fig. 2(a2) are scanning electron micrographs with different multiples, fig. 2(A3) is a mechanical property compression curve, fig. 2(a4) is a nitrogen adsorption and desorption curve, and fig. 2(a5) is a micropore size distribution diagram;
fig. 3 is a scanning electron micrograph, nitrogen adsorption and desorption curves, and pore size distribution of the high strength carbon monolith H2.15F0.45R1 prepared in example 3; wherein, fig. 3(a1) and fig. 3(a2) are scanning electron micrographs with different multiples, fig. 3(A3) is a nitrogen adsorption and desorption curve, and fig. 3(a4) is a micropore size distribution diagram;
fig. 4 is a scanning electron micrograph, nitrogen adsorption and desorption curves, and pore size distribution of the high strength carbon monolith H1.99F0.45R1 prepared in example 4; wherein, fig. 4(a1) and fig. 4(a2) are scanning electron micrographs with different multiples, fig. 4(A3) is a nitrogen adsorption and desorption curve, and fig. 4(a4) is a micropore size distribution diagram;
FIG. 5 is a scanning electron micrograph, nitrogen adsorption and desorption curves, and pore size distribution plot of the high strength carbon monolith H2.32F0.45R1-95 prepared in example 5; wherein, fig. 5(a1) and fig. 5(a2) are scanning electron micrographs with different multiples, fig. 5(A3) is a nitrogen adsorption and desorption curve, and fig. 5(a4) is a micropore size distribution diagram;
FIG. 6 is a scanning electron micrograph, nitrogen adsorption and desorption curves, and pore size distribution plot of the high strength carbon monolith H2.32F0.45R1-55 prepared in example 6; wherein, fig. 6(a1) and fig. 6(a2) are scanning electron micrographs with different multiples, fig. 6(A3) is a nitrogen adsorption and desorption curve, and fig. 6(a4) is a micropore size distribution diagram;
FIG. 7 is a scanning electron micrograph of a carbon monolith prepared by substituting 20 wt.% resorcinol with phenol.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The starting reagents used in the following examples are all commercially available.
A preparation method of a pore structure-controllable high-strength grade pore carbon monolithic column comprises the following steps:
(1) water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing resorcinol (R) ((1.2-3.9): 0.2-0.7):1 with water, formaldehyde solution and resorcinol, and stirring for 20 min to obtain sol; wherein the mass fraction of the formaldehyde solution is 38 percent;
(2) sealing and aging the sol at a certain water bath temperature to obtain wet gel, wherein the water bath temperature is 35-100 ℃, and the aging time is 4-36 h;
(3) drying the wet gel for 10-24h at room temperature, and drying in an oven at 40-60 ℃ for 8-36h to obtain a resin monolithic column, wherein the resin monolithic column has a complete column body, no cracks and a controllable and regular micro-pore structure, and a carbon monolithic column is obtained through high-temperature carbonization at the carbonization temperature of 700-900 ℃ and the heat preservation time of 2-3h, the strength of the carbon monolithic column reaches 14.31-24.6MPa, the carbon monolithic column contains two-stage pores of micro-pores and macro-pores, and the total pore volume is 1.26-1.85cm3.g-1Wherein the pore volume of the micropores is 0.15-0.26cm3.g-1The average pore diameter of the macropores is 0.28-4.49 μm, and the specific surface area is 363-567m2.g-1。
Example 1:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, stirring for 20 min to obtain sol, and heating in 85 deg.C water bathAnd aging the lower seal for 24h to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, drying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column at 700 ℃ for 2h to obtain the high-strength carbon monolithic column (named H2.32F0.45R1). Scanning electron micrographs of the carbon monolith H2.32F0.45R1 in different multiples are shown in fig. 1(a1) and fig. 1(a2), a mechanical property compression curve is shown in fig. 1(A3), and a nitrogen adsorption and desorption curve is shown in fig. 1(a 4); H2.32F0.45R1 the skeleton is a three-dimensional network interconnection structure with a strength of 24.6 MPa. The carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.85cm3.g-1Wherein the pore volume of the micropores is 0.26cm3.g-1The average pore diameter of the macropores is 1.91 mu m, and the specific surface area is 567m2.g-1. The microporous pore size distribution of the carbon monolith H2.32F0.45R1 is shown in fig. 1(a5), and the macroporous pore size distribution is shown in fig. 1(a 6).
On the basis of the same process parameters in this example, carbon monolithic columns were prepared, except that 20% of the mass of resorcinol was replaced with phenol, and carbon monolithic columns were finally prepared, and the scanning electron micrograph thereof is shown in fig. 7, from which it was found that phenol could not be used to replace resorcinol in order to obtain carbon monolithic columns of the same structure.
Example 2:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, continuously stirring for 20 minutes to obtain sol, and then sealing and aging for 24 hours under the condition of water bath at 85 ℃ to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, drying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column at 700 ℃ for 2h to obtain a carbon monolithic column (named as H2.32F0.52R1). Scanning electron micrographs of the carbon monolith H2.32F0.52R1 in different multiples are shown in fig. 2(a1) and fig. 2(a2), a mechanical property compression curve is shown in fig. 2(A3), and a nitrogen adsorption and desorption curve is shown in fig. 2(a 4); H2.32F0.52R1 the skeleton is a three-dimensional network interconnection structure with strength of 16.83 MPa. The carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.68cm3.g-1Wherein the pore volume of the micropores is 0.15cm3.g-1The average pore diameter of the macropores is 0.68 mu m, and the specific surface area is 404m2.g-1. The pore size distribution of the carbon monolith H2.32F0.52R1 is shown in FIG. 2 (A5).
Example 3:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, continuously stirring for 20 minutes to obtain sol, and then sealing and aging for 24 hours under the condition of water bath at the temperature of 85 ℃ to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, drying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column at 700 ℃ for 2h to obtain a carbon monolithic column (named as H2.15F0.45R1). H2.15F0.45R1 the skeleton is a three-dimensional network interconnection structure with a strength of 20.20 MPa. Scanning electron micrographs of the carbon monolith H2.15F0.45R1 at different multiples are shown in fig. 3(a1) and fig. 3(a2), and a nitrogen adsorption and desorption curve is shown in fig. 3 (A3); the carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.46cm3.g-1Wherein the pore volume of the micropores is 0.2cm3.g-1The average pore diameter of the macropores is 0.78 mu m, and the specific surface area is 448m2.g-1. The pore size distribution of the carbon monolith H2.15F0.45R1 is shown in FIG. 3 (A4).
Example 4:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, continuously stirring for 20 minutes to obtain sol, and then sealing and aging for 24 hours under the condition of water bath at the temperature of 85 ℃ to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, drying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column at 700 ℃ for 2h to obtain a carbon monolithic column (named as H1.99F0.45R1). H1.99F0.45R1 the skeleton is a three-dimensional network interconnection structure with the strength of 15.38 MPa. The scanning electron micrographs of the carbon monolith H1.99F0.45R1 at different multiples are shown in FIG. 4(A1) and FIG. 4(A2), and the adsorption and desorption curves of nitrogen are shown in FIG. 4 (A)3) Shown; the carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.26m3.g-1Wherein the pore volume of the micropores is 0.22cm3.g-1The average pore diameter of the macropores is 0.28 mu m, and the specific surface area is 485m2.g-1. The prepared monolithic column has smaller pore diameter, if the monolithic column is directly dried in a higher-temperature oven, the pores can collapse due to the action of stress, so that the monolithic column is dried at room temperature and then at elevated temperature, the obtained column is complete and has no crack, and the micro-pore structure is intact. The pore size distribution of the carbon monolith H1.99F0.45R1 is shown in FIG. 4 (A4).
Example 5:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, continuously stirring for 20 minutes to obtain sol, and then sealing and aging for 24 hours under the condition of a water bath at 95 ℃ to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, drying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column at 700 ℃ for 2h to obtain a carbon monolithic column which is named as H2.32F0.45R1-95. H2.32F0.45R1-95 has a three-dimensional network interconnection structure and a strength of 22.01 MPa. Scanning electron micrographs of the carbon monolith H2.32F0.45R1-95 at different multiples are shown in fig. 5(a1) and fig. 5(a2), and a nitrogen adsorption and desorption curve is shown in fig. 5 (A3); the carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.77cm3.g-1Wherein the pore volume of the micropores is 0.17cm3.g-1The average pore diameter of the macropore is 4.49 mu m, and the specific surface area is 363m2.g-1. The pore size distribution of the carbon monolith H2.32F0.45R1-95 micropores is shown in FIG. 5 (A4).
Example 6:
water (H, including water in formaldehyde solution): formaldehyde solute (F): mixing water, formaldehyde solution and resorcinol at the mass fraction of 38%, continuously stirring for 20 minutes to obtain sol, and then sealing and aging for 24 hours under the condition of water bath at 55 ℃ to obtain wet gel. Drying the obtained wet gel at room temperature for 12h, and dryingDrying in a 50 ℃ oven for 24h to obtain a resin monolithic column, and carbonizing the resin monolithic column for 2h at 700 ℃ to obtain a carbon monolithic column which is named as H2.32F0.45R1-55. H2.32F0.45R1-55 has a three-dimensional network interconnection structure and a strength of 14.31 MPa. Scanning electron micrographs of the carbon monolith H2.32F0.45R1-55 at different multiples are shown in fig. 6(a1) and fig. 6(a2), and a nitrogen adsorption and desorption curve is shown in fig. 6 (A3); the carbon monolithic column contains two-stage pores of micro-pore and macro-pore, and the total pore volume is 1.41cm3.g-1Wherein the pore volume of the micropores is 0.21cm3.g-1The average pore diameter of the macropores is 0.98 mu m, and the specific surface area is 456m2.g-1. The pore size distribution of the carbon monolith H2.32F0.45R1-55 is shown in FIG. 6 (A4).
Claims (7)
1. A preparation method of a pore structure-controllable high-strength grade pore carbon monolithic column is characterized by comprising the following steps:
(1) mixing water, formaldehyde solution and resorcinol according to a ratio to obtain uniform sol; wherein, according to the mass ratio, water: formaldehyde solute: resorcinol (1.2-3.9): 0.2-0.7):1, and water comprises water in formaldehyde solution;
(2) sealing and aging the sol under the heating condition to obtain wet gel, wherein the heating temperature is 35-100 ℃, and the aging time is 4-36 h;
(3) drying the wet gel to obtain a resin monolithic column, and carrying out high-temperature carbonization to obtain a carbon monolithic column, wherein the carbonization temperature is 700-900 ℃, and the heat preservation time is 2-3 h.
2. The method for preparing the pore structure controllable high-strength grade pore carbon monolithic column as claimed in claim 1, wherein in the step (1), the mass ratio of water: formaldehyde solute: resorcinol (1.99-2.32): 0.45-0.52): 1.
3. The method for preparing the pore structure controllable high-strength grade pore carbon monolithic column as claimed in claim 1, wherein in the step (2), the heating mode is water bath heating, and the heating temperature is 35-85 ℃.
4. The method for preparing a pore structure controllable high-strength grade pore carbon monolithic column as claimed in claim 1, wherein in the step (3), the wet gel drying mode is as follows: drying at room temperature for 10-24h, and drying in oven at 40-60 deg.C for 8-36 h.
5. The method for preparing the pore structure controllable high-strength grade pore carbon monolithic column as claimed in claim 1, wherein in the step (3), the resin monolithic column is complete and has no cracks.
6. The method for preparing the pore structure controllable high-strength grade pore carbon monolithic column as claimed in claim 1, wherein in the step (3), the strength of the carbon monolithic column reaches 14.31-24.6 MPa.
7. The method for preparing a pore structure-controllable high-strength graded pore carbon monolithic column according to claim 1, wherein in the step (3), the carbon monolithic column contains two-stage pores of micro-pores and macro-pores, and the total pore volume is 1.26-1.85cm3.g-1Wherein the pore volume of the micropores is 0.15-0.26cm3.g-1The average pore diameter of the macropores is 0.28-4.49 μm, and the specific surface area is 363-567m2.g-1。
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