CN102515145A - Preparation process for high specific surface porous carbon material - Google Patents
Preparation process for high specific surface porous carbon material Download PDFInfo
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- CN102515145A CN102515145A CN2011104444648A CN201110444464A CN102515145A CN 102515145 A CN102515145 A CN 102515145A CN 2011104444648 A CN2011104444648 A CN 2011104444648A CN 201110444464 A CN201110444464 A CN 201110444464A CN 102515145 A CN102515145 A CN 102515145A
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Abstract
The invention discloses a preparation process for a high specific surface porous carbon material. The preparation process comprises the following steps of: (1) removing impurities and drying; (2) preparing an alkaline solution; (3) dispersing; (4) drying at low temperature; (5) performing heat treatment at high temperature; and (6) preparing the high specific surface porous carbon material. By the preparation process for the high specific surface porous carbon material, the specific surface area is accurately controlled when the specific surface area is less than 3,000m<2>/g, and the prepared high specific surface porous carbon material has the specific surface area of 1,500-3,000m<2>/g; meanwhile, raw materials are safe and environment-friendly, a flow is concise and high-efficiency, and the production cost is low.
Description
Technical field
The present invention relates to a kind of raw material of wood-charcoal material, more particularly, relate to a kind of preparation technology of high-ratio surface porous carbon material.
Background technology
Porous carbon material is because its excellent performance is used in foodstuffs industry, chemical industry, medicine industry and other various industry widely.
According to the pore structure of porous charcoal, International Union of Pure and Applied Chemistry(IUPAC) is divided three classes porous charcoal: micropore charcoal (mean pore size < 2 nm), mesopore charcoal (2 nm < mean pore size < 50 nm), macropore carbon (mean pore size>50 nm).Difference according to Application Areas has different performance requirements to porous charcoal.As adsorb organic molecule (like formaldehyde), need to adopt the micropore charcoal; Absorption macromole (like dyestuff) needs to adopt mesopore even macropore carbon; As be applied to energy storage field (like ultracapacitor), and its pore structure there is special requirement equally, the narrow wide straight song in duct with influencing the electrolyte ion diffusive migration of portion within it, thereby influences the energy density and the electrical condenser internal resistance of electrical condenser.
CN 101973542 A disclose the preparation method of a kind of ultracapacitor with porous carbon material, are that raw material, composite alkali metal oxyhydroxide are acvator with refinery coke or pitch coke, through two stage activation prepared porous carbon materials, the porous carbon material that obtains.Though this method can the ratio surface-area, the specific surface area of preparation is only at 1500 ~ 1800m
2Between/the g.
CN101973542A discloses a kind of preparation method of high superficial area porous carbon material.This method is a raw material with Resorcinol and formaldehyde, is catalyzer with Pottasium Hydroxide or sodium hydroxide, uses the charcoal-aero gel method to obtain the porous carbon material of high-specific surface area.But that the Resorcinol of mentioning in this patent, formaldehyde are is poisonous, the inflammableness material of smell with irritating.
Another patent CN102070140A of our company discloses a kind of highly basic that utilizes and has handled the method that obtains the high-specific surface area grapheme material; Use the highly basic activation; Thereby go out the micropore of nanometer scale fast, in large quantity in the Graphene surface corrosion, greatly improve its specific surface area.Though the Graphene specific surface area of this method preparation can reach 3000m
2/ g, but the highly basic that this method is used and the mass ratio of graphite oxide are 1 ~ 50:1, and production cost is high, and contrast table is looked unfamiliar and can not be controlled.
Summary of the invention
In order to remedy the shortcoming of above-mentioned technology, the invention provides a kind of preparation technology of high-ratio surface porous carbon material, realized that specific surface area is at 3000 m
2Accurately controlled when/g is following, prepared high-ratio surface porous carbon material has a large amount of holes, therefore also has sizable specific surface area (1500 ~ 3000 m
2/ g), simultaneously, this preparation technology's materials safety environmental protection, flow process are succinctly efficient, production cost is extremely low.
The preparation technology of high-ratio surface porous carbon material proposed by the invention comprises the steps:
(1) removal of impurities oven dry: one or more the raw material of wood-charcoal material with in gac, carbon nanotube, expanded graphite, graphene oxide, the Graphene, be mixed in the deionized water, dry behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the proportional arrangement corresponding alkali solution of 0.1 ~ 20:1; Said alkaline concentration is 0.1 mol/L ~ 10 mol/L;
(3) dispersion treatment:, join in the alkaline solution that step (2) disposed dispersion treatment 1 hour to 72 hours with step (1) resulting raw material of wood-charcoal material particle or powder; Said dispersion treatment for stir, ultrasonic or leave standstill in one or more arbitrary combination;
(4) cryodrying: with the resulting dispersion soln of step (3), in 20 ℃ ~ 260 ℃ cryodryings to constant weight;
(5) high-temperature heat treatment: the solid particulate or the powder of step (4) gained were carried out 700 ℃ ~ 1200 ℃ high-temperature heat treatment 1 hour to 8 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Particularly, said alkaline solution is one or more the arbitrary combination in Pottasium Hydroxide, sodium hydroxide, yellow soda ash, sodium hydrogencarbonate, salt of wormwood or the saleratus.
Particularly, said cryodrying is one or more the arbitrary combination in vacuum-drying, forced air drying, oil bath drying or the spraying drying.
Particularly, said high-temperature heat treatment is vacuum heat treatment or protection of inert gas thermal treatment.
Particularly, the rare gas element in the said protection of inert gas thermal treatment is one or more the arbitrary combination in nitrogen, helium, neon, argon gas, krypton gas or the xenon.
High-ratio surface porous carbon material proposed by the invention and its preparation method have following beneficial effect:
1. to have realized that specific surface is compared prior art bigger in the present invention, and specific surface area is at 3000 m
2Accurately controlled when/g is following, can be fully prepare the raw material of wood-charcoal material according to the needs of producing, make industrial production purpose, operability stronger.
2. simple and effective, the employed starting material of Production Flow Chart of the present invention all are safety and environmental protections, compare employed raw material in the prior art, and the present invention has fully realized green production, nontoxic; Simultaneously, the present invention is through quantitative alkali adding method, makes the more clear simplification of proportioning raw materials of each Production Flow Chart to have reached the effect of practicing thrift cost, reducing waste liquid.
3. compare the situation of the pore size obvious difference of resulting raw material of wood-charcoal material in the prior art; The high-ratio surface porous carbon material that preparation technology proposed by the invention obtains has the hole of quite a lot of quantity; The aperture stable homogeneous; Its aperture can all be controlled between 2 nm ~ 5 nm, and particularly, the homogeneity in aperture and pore size will embody in following embodiment to some extent.
Description of drawings
Fig. 1 is the figure of the sem of the high-ratio surface porous carbon material that obtains among the embodiment 1.
Embodiment
Below in conjunction with accompanying drawing the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein only is used for explanation and explains the present invention, and be not used in qualification the present invention.
Embodiment 1
The preparation technology of high-ratio surface porous carbon material comprises the steps:
(1) removal of impurities oven dry: graphene oxide is mixed in the deionized water, dries behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the corresponding potassium hydroxide solution of proportional arrangement of 2:1; Said potassium hydroxide solution concentration is 0.1 mol/L;
(3) dispersion treatment: with step (1) resulting raw material of wood-charcoal material particle or powder, join in the alkaline solution that step (2) disposed, stirred 1 hour;
(4) cryodrying: with the resulting dispersion soln of step (3), in 20 ℃ of cryodryings to constant weight;
(5) high-temperature heat treatment: the solid particulate or the powder of step (4) gained were carried out 700 ℃ of high-temperature heat treatment 8 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
As shown in Figure 1, the figure of the sem of the high-ratio surface porous carbon material that Fig. 1 makes for present embodiment can find out on scheming; The structure of high-ratio surface porous carbon material is very even; Pore size is almost consistent, and between 2 nm ~ 5 nm, mean pore size is 3.84 nm.
This technology when the measure solid surface-area, employing be Brunauer-Emmett-Teller (BET) method of using always, BET equation and specific surface area accounting equation are as follows:
1. BET equation:
2. specific surface area accounting equation:
;
Wherein W is the quality of the adsorbed gas when relative pressure P/P0; Wm is the quality that adsorbate forms monolayer surface absorption; Constant C is the sorptive power of relevant first adsorption layer; N is that (6.023 * 1023 molecule/mol), Acs is the molecular cross sectional area of adsorbate to Avogadro constant, and M is the molecular weight of adsorbate.
This process using multiple spot BET method according to equation 1, is made 1/ [W (P0/P-1)] and to the straight line of P/P0, is calculated Wm, substitution equation 2, thus draw specific surface area.
Through measuring gained N
2The specific surface area of absorption is 1500.886 m
2/ g.
Another patent CN102070140A of our company utilizes highly basic to handle the method that obtains the high-specific surface area grapheme material and compares with the present invention; Produce the raw material of wood-charcoal material of same amount; Its cost is 10 times of present embodiment preparation technology production cost; And the generation of specific surface can not be controlled, and structural uniformity is bad, and pore size is heterogeneity also.
Embodiment 2
The preparation technology of high-ratio surface porous carbon material proposed by the invention may further comprise the steps:
(1) removal of impurities oven dry: gac is mixed in the deionized water, dries behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the corresponding sodium hydroxide solution of proportional arrangement of 3:1; Said concentration of sodium hydroxide solution is 1 mol/L;
(3) dispersion treatment:, join in the alkaline solution that step (2) disposed supersound process 4 hours with step (1) resulting raw material of wood-charcoal material particle or powder;
(4) cryodrying: with the resulting dispersion soln of step (3), in 60 ℃ of vacuum-dryings to constant weight;
(5) vacuum heat treatment: the solid particulate or the powder of step (4) gained were carried out 800 ℃ of high-temperature heat treatment 6 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Through detecting the N of gained high-ratio surface porous carbon material
2The specific surface area of absorption is 2027.839 m
2/ g.
Embodiment 3
The preparation technology of high-ratio surface porous carbon material proposed by the invention may further comprise the steps:
(1) removal of impurities oven dry: carbon nanotube, expanded graphite are mixed in the deionized water, dry behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the corresponding yellow soda ash of proportional arrangement of 5:1, the mixing solutions of sodium hydrogencarbonate; Said alkaline concentration is 5 mol/L;
(3) dispersion treatment: with step (1) resulting raw material of wood-charcoal material particle or powder, join in the alkaline solution that step (2) disposed, stir, supersound process 10 hours;
(4) cryodrying:, carry out oil bath drying, forced air drying to constant weight in 100 ℃ with the resulting dispersion soln of step (3);
(5) high-temperature heat treatment: the solid particulate of step (4) gained or powder are carried out 900 ℃ carried out protection of inert gas thermal treatment 4 hours with nitrogen, helium;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Through detecting, the specific surface area of the N2 absorption of gained high-ratio surface porous carbon material is 2443.369 m
2/ g.
Embodiment 4
The preparation technology of high-ratio surface porous carbon material proposed by the invention may further comprise the steps:
(1) removal of impurities oven dry: gac, carbon nanotube, expanded graphite, graphene oxide are mixed in the deionized water, dry behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the corresponding sodium hydroxide of proportional arrangement, yellow soda ash, sodium hydrogencarbonate, the salt of wormwood mixing solutions of 10:1; Said alkaline concentration is 6 mol/L;
(3) dispersion treatment: with step (1) resulting raw material of wood-charcoal material particle or powder, join in the alkaline solution that step (2) disposed, left standstill 30 hours;
(4) cryodrying: with the resulting dispersion soln of step (3), in 200 ℃ of spraying dryings to constant weight;
(5) high-temperature heat treatment: the solid particulate of step (4) gained or powder were carried out 1100 ℃ of neons, argon gas, krypton gas protection of inert gas thermal treatment 2 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Through detecting the N of gained high-ratio surface porous carbon material
2The specific surface area of absorption is 3000 m
2/ g.
Embodiment 5
The preparation technology of high-ratio surface porous carbon material proposed by the invention may further comprise the steps:
(1) removal of impurities oven dry: expanded graphite is placed deionized water, dry behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the corresponding salt of wormwood of proportional arrangement, saleratus, the potassium hydroxide solution of 20:1; Said alkaline concentration is 10 mol/L;
(3) dispersion treatment: with step (1) resulting raw material of wood-charcoal material particle or powder, join in the alkaline solution that step (2) disposed, successively through stir, ultrasonic, the mode of leaving standstill handled 72 hours;
(4) cryodrying:, carry out forced air drying and vacuum-drying to constant weight in 260 ℃ with the resulting dispersion soln of step (3);
(5) high-temperature heat treatment: the solid particulate or the powder of step (4) gained are carried out 1200 ℃ of krypton gas protection of inert gas thermal treatment thermal treatments 1 hour;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Through detecting the N of gained high-ratio surface porous carbon material
2The specific surface area of absorption is 2156.389 m
2/ g.
Embodiment 6
The preparation technology of high-ratio surface porous carbon material proposed by the invention may further comprise the steps:
(1) removal of impurities oven dry:, dry behind the filtering and impurity removing with being mixed in the deionized water in gac, carbon nanotube, expanded graphite, graphene oxide, the Graphene;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is proportional arrangement salt of wormwood, the saleratus of 9:1
The alkali mixing solutions of Pottasium Hydroxide; Said alkaline concentration is 8 mol/L;
(3) dispersion treatment:, join in the alkaline solution that step (2) disposed supersound process 36 hours with step (1) resulting raw material of wood-charcoal material particle or powder;
(4) cryodrying: with the resulting dispersion soln of step (3), dry and vacuum-drying is to constant weight in 140 ℃ of oil baths successively;
(5) high-temperature heat treatment: the solid particulate or the powder of step (4) gained were carried out 1000 ℃ of vacuum heat treatment 4 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
Through detecting the N of gained high-ratio surface porous carbon material
2The specific surface area of absorption is 2365.367 m
2/ g.
What should explain at last is: the above is merely the preferred embodiments of the present invention; Be not limited to the present invention; Although the present invention has been carried out detailed explanation with reference to previous embodiment; For a person skilled in the art, it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the preparation technology of a high-ratio surface porous carbon material comprises the steps:
(1) removal of impurities oven dry: one or more the raw material of wood-charcoal material with in gac, carbon nanotube, expanded graphite, graphene oxide, the Graphene, be mixed in the deionized water, dry behind the filtering and impurity removing;
(2) alkaline solution preparation: the weight ratio according to alkali content and raw material of wood-charcoal material is the proportional arrangement corresponding alkali solution of 0.1 ~ 20:1; Said alkaline concentration is 0.1 mol/L ~ 10 mol/L;
(3) dispersion treatment:, join in the alkaline solution that step (2) disposed dispersion treatment 1 hour to 72 hours with step (1) resulting raw material of wood-charcoal material particle or powder; Said dispersion treatment for stir, ultrasonic or leave standstill in one or more arbitrary combination;
(4) cryodrying: with the resulting dispersion soln of step (3), in 20 ℃ ~ 260 ℃ cryodryings to constant weight;
(5) high-temperature heat treatment: the solid particulate or the powder of step (4) gained were carried out 700 ℃ ~ 1200 ℃ high-temperature heat treatment 1 hour to 8 hours;
(6) making of high-ratio surface porous carbon material: the elementary product of the resulting porous charcoal of step (5) is washed, filtered and drying, remove remaining alkali impurity, obtain the high-ratio surface porous carbon material.
2. the preparation technology of high-ratio surface porous carbon material according to claim 1, said alkaline solution is one or more the arbitrary combination in Pottasium Hydroxide, sodium hydroxide, yellow soda ash, sodium hydrogencarbonate, salt of wormwood or the saleratus.
3. the preparation technology of high-ratio surface porous carbon material according to claim 1, said cryodrying is one or more the arbitrary combination in vacuum-drying, forced air drying, oil bath drying or the spraying drying.
4. the preparation technology of high-ratio surface porous carbon material according to claim 1, said high-temperature heat treatment are vacuum heat treatment or protection of inert gas thermal treatment.
5. the preparation technology of high-ratio surface porous carbon material according to claim 4, the rare gas element in the said protection of inert gas thermal treatment is one or more the arbitrary combination in nitrogen, helium, neon, argon gas, krypton gas or the xenon.
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