Carbon material and method for production thereof

FIELD: chemistry.

SUBSTANCE: invention can be used in making catalyst supports, sorbents, electrochemical catalysts and lithium-ion batteries. The method includes reacting, at 700-900°C, a calcium salt, e.g., calcium tartrate or calcium tartrate doped with a transition metal, which is a template precursor, and liquid or gaseous carbon-containing compounds or mixtures thereof as a carbon source. The obtained product is treated with hydrochloric acid. Concentration of the doped transition metal is not more than 1 at%.

EFFECT: obtaining a homogeneous mesoporous carbon material characterised by specific surface area of 850-930 m2/g, pore volume of 2,9-3,3 cm3/g and average pore diameter of 10-30 nm.

4 cl, 3 dwg, 9 ex

 

The invention relates to nanotechnology and relates to the field of carbon materials, including porous materials and the synthesis of these carbon materials.

Most of the carbon materials obtained in the industry, have a porous structure (pore size less than 2 nm), which imposes restrictions on their use. The development of techniques for obtaining mesoporous carbon (pore size of more than 2 nm and less than 50 nm) with predetermined structural characteristics due to the need to improve material properties for use as a carrier of catalysts, sorbents, in Biomedicine, dolnoslaski electrochemical capacitors, lithium-ion batteries and other engineering fields.

Currently there are a number of methods of synthesis of mesoporous carbon. Thus it is necessary to determine that the mesoporous carbon materials can be divided into two groups: materials with a wide distribution of pore diameters and materials having similar size and ordered pores.

Among the traditional methods of creating porous carbon material and a material with disordered pores there are several ways:

Catalytic activation using metal-containing compounds [A. OOI et al. Formation of mesopores in phenolic resin-derived carbon fiber by catalytic activation using cobalt. Carbon. 1995, 33, pp1085-1090]. Adding metal catalyzes the formation of the structure of mesopores with a size of several tens nm (presence of micropores is still significantly), the maximum specific surface area of 170 m2/year

- Carbonization of the copolymer or carbon precursor consisting of a thermosetting component and a thermally unstable component [J. Ozaki et al. Novel preparation method for the production of mesoporous carbon fiber from a polymer blend. Carbon. 1997, 35, pp.1031-1033]. The pore size was 4 nm by carbonization of a mixture of phenolic resin is polyvinyl butyral.

- Carbonization of organic aerogels [Y.N. Feng. Fabrication of carbon aerogels. Advanced Materials Research. 2006, 11-12, pp.19-22]. The obtained mesoporous material (pore size is in the region of 2.5 to 6.1 nm) with high porosity (>80%) and relatively high surface area (>400 m2/g).

- Template synthesis using such inorganic compounds as, for example, silicon oxide [Z. Tang et al. Properties of mesoporous carbon prepared from different carbon precursors using nanosize silica as a template. New carbon materials. 2010, 25, pp.465-469]. The carbon material has a very high value of pore volume (4 cm3/g) and developed specific surface (1000 m2/g). The distribution of pores is quite wide - from 10 to 100 nm.

Methods of creating a mesoporous carbon material with similar pore size are: synthesis-replication using restrategising template PU is eat impregnation, carbonization and removal of the template (the porous structure is determined by the structure of the template) and self-Assembly using destructible of templates by condensation and carbonization (porous structure is determined by the synthesis conditions such as the ratio of the reagents, solvents and temperature). Example destructible template is the use of amphiphilic triblock copolymers [F. Zhang et al. An aqueous cooperative assembly route to synthesize ordered mesoporous carbons with controlled structures and morphology. Chemistry Materials. 2006, 18, pp.5279-5288]. The material obtained by the proposed method has a pore size 4.1-6.8 nm, which can be varied in the millimeter or micrometer scale. The main disadvantage of the proposed method is the relatively high cost of pure starting compounds for the synthesis of porous carbon.

It is known that the pyrolysis of the carbon aerogel at a temperature above 1000°C, containing a small amount of ions of metals such as Cr, Fe, Co, Ni, catalyzes graphitization carbon material, affect the values of specific surface area and volume and pore size [F. J. Maldonado-Hodar et al. Catalytic Graphitization of Carbon Aerogels by Transition Metals. Langmuir. 2000, 16, pp.4367-4373]. The disadvantage of the proposed method of synthesis and the resulting material is a significant amount of graphitized carbon layers in the particles of a porous material, which leads to the formation of macropores in the structure is round and relatively low specific surface area (300-400 m 2/g).

A method of obtaining nanostructured carbon containing micro - and mesopores, which includes mixing particles of the precursor template (calcium carbonate) and predecessor carbon (formaldehyde resin), followed by pressing into a tablet, by heating the tablet to 900°C, resulting in carbonization of the carbon precursor on the surface of the nanoparticles of the template, the nanoparticles of the template are removed from the resulting product solution of hydrochloric acid - the prototype of the invention. [Chunrong Zhao et al. Nano-CaC03 as template for preparation of large disordered mesoporous carbon with hierarchical porosities. Jornal of Materials Chemistry. 2010, 20, pp.976-980]. Thus obtained samples of the material depending on the ratio of initial reagents are characterized by values of specific surface and pore volume in the range 503-1215 m2/g and 1.8-9.0 cm3/g, respectively, i.e., the material is characterized by a large variation in porosity and contains micro-and mesopores. The disadvantage of this method is the use of toxic compounds as a carbon source.

The objective of the invention is to develop a technologically simple and inexpensive method of obtaining a carbon material, the technical result is to obtain a carbon material having a uniform mesoporous structure with a high specific surface

The problem is solved in that the carbon material of the nanostructure which is formed by carbon atoms having porosity with a developed specific surface is homogeneous mesoporous carbon material and is characterized by a specific surface 850-930 m2/g, pore volume 2.9-3.3 cm3/g and an average pore diameter of 10-30 nm.

The task according to the method is solved in that a method of obtaining a carbon material including the interaction between calcium salts, which is the predecessor of the template, and a carbon source at 700-900°C followed by treatment of the resulting product with hydrochloric acid, as a precursor to a template use the tartrate of calcium or calcium tartrate-doped transition metal, and as a source of carbon use liquid or gaseous carbon-containing compounds or mixtures thereof, the concentration of subsidized transition metals is not more than at.% and use diluted hydrochloric acid.

Distinctive features of the invention material are:

carbon material is homogeneous mesoporous material

the material is characterized by a specific surface 850-930 m2/g

pore volume 2.9-3.3 cm3/g and an average pore diameter of 10-30 nm.

Distinctive features of the invention according to the method are the SJ: as a precursor to a template use the tartrate of calcium or calcium tartrate, doped transition metal; carbon source is liquid or gaseous carbon-containing compounds or their mixtures; the concentration of the doped transition metal is less than 1 at.%; use of diluted hydrochloric acid.

In the proposed method uses inexpensive, easily available starting reagents. The calcium tartrate is an inexpensive reagent, it can use without additional purification, fully mixed with the receiving calcium oxide, which is a carrier for carbon and well soluble in dilute less aggressive acids. Getting the doped calcium tartrate is also straightforward. The doped transition metal is less than 1 at.% is sufficient for catalysis of the decomposition of carbon-containing compounds with the formation of nanostructured carbon sufficiently that affects the increase in the yield of the finished product, but also on the degree of graphitization of the carbon layers in the resulting product. Trace amounts of transition metal atoms can also easily be dissolved with dilute acid during the removal of the template particles. As a carbon source using liquid or gaseous carbon-containing substances or mixtures liable to undergo Razlog the tion in a given temperature range.

Scheme of the proposed method are shown in Fig.1.

Examples of making mesoporous carbon material

Example 1. A portion of the calcium tartrate (~300 mg)containing 1 at.% iron, placed in a ceramic boat and enter into the chamber of the reactor, heating the reactor up to 800°C. thermal decomposition of the original substance is carried out in an inert atmosphere for 10 minutes During this time, the original connection is decomposed with the formation of calcium oxide with distributed therein atoms of the transition metal. Further, at a temperature of 800°C is injected into the reactor vapors of ethyl alcohol (C2H5IT within hours. When interacting molecules of alcohol obtained by the template particles on the surface is the deposition of carbon. After cooling to room temperature from the reactor goes to the boat with a black substance. The resulting material is placed in a glass container and filled with a solution of diluted hydrochloric acid (1:1) under stirring to obtain a fine mist of black substance in solution. The obtained suspension is filtered on a membrane filter and washed repeatedly with small portions of distilled water until neutral pH. The precipitate is dried in air or in a drying Cabinet with a temperature of 100°C to constant weight.

Typical carbon material obtained by the proposed method represents the FDS is th black powder (TEM image in figure 2). Determination of textural characteristics is performed on an automated instrument ASAP-2400 of the company Micromeritics. Before measurements the investigated sample Tegaserod in dynamic vacuum at 150°C for 4 hours. Carbon material is characterized by a high specific surface area (854 m2/g). The pore distribution of typical and presented on Fig.3. The study of the porous structure showed that the resulting material mainly contains mesopores in the range of 10-30 nm (micropores ~1.5% of the total). Total pore volume calculated by the point of maximum filling of the sample adsorbed nitrogen at the maximum partial pressure is 2.9 cm3/year

Example 2. Obtaining mesoporous carbon material are similar to example 1, but as a liquid carbon source using acetonitrile. The resulting material is characterized by a high specific surface (905 m2/g), the predominant content of pores in the range of 15-25 nm and pore volume 3.0 cm3/year

Example 3. A portion of the calcium tartrate (~50 mg) was placed in a ceramic boat and enter into the chamber of the reactor, the reactor is heated to 800°C. thermal decomposition of the original substance is carried out in an inert atmosphere for 10 minutes During this time, the original connection is decomposed with the formation of oxide. Next, at 800°C in the reactor hearth is raised a carbon source (ethylene) for one hour. After cooling to room temperature from the reactor goes to the boat with the black substance. The resulting material is placed in a glass container and filled with a solution of diluted hydrochloric acid (1:1) under stirring to obtain a fine mist of black substance in solution. The obtained suspension is filtered on a membrane filter and washed repeatedly with small portions of distilled water until neutral pH. The precipitate is dried in air or in a drying Cabinet with a temperature of 100°C to constant weight. The obtained carbon material is characterized by a high specific surface area of 870 m2/g, a pore distribution of 10-30 nm and pore volume 3.1 cm3/year

Example 4. A portion of the calcium tartrate (~100 mg)containing 0.5% cobalt, placed in a ceramic boat in the center of the reactor and the rector heated to 900°C. thermal decomposition of the parent compound is carried out in an inert atmosphere for 10 minutes During this time, the original connection is decomposed with the formation of calcium oxide with distributed therein atoms of the transition metal, the surface of which is the deposition of carbon. When interacting molecules of methane obtained with particles of the template on the surface is the deposition of carbon. After cooling to room temperature from the reactor goes to the boat with a black substance. Receiving the hydrated material is placed in a glass container and filled with a solution of diluted hydrochloric acid (1:1) under stirring to obtain a fine mist of black substance in solution. The obtained suspension is filtered on a membrane filter and washed repeatedly with small portions of distilled water until neutral pH. The precipitate is dried in air or in a drying Cabinet with a temperature of 100°C to constant weight. The obtained carbon material is characterized by a high specific surface 923 m2/g, a pore distribution of 10-30 nm and pore volume 3.3 cm3/year

Example 5. Obtaining mesoporous carbon material with the use of other gaseous carbon source - acetylene - lead analogously to example 3. The obtained carbon material is characterized by a high specific surface 903 m2/g, a pore distribution of 10-25 nm and pore volume 3.1 cm3/year

Example 6. A portion of the calcium tartrate (~100 mg)containing 0.5 at.% Nickel is placed in a ceramic boat and enter into the chamber of the reactor, heating the reactor up to 700°C. thermal decomposition of the original substance is carried out in an inert atmosphere for 10 minutes During this time the original compound decomposes to form calcium oxide distributed therein atoms of the transition metal. Further, at a temperature of 700°C is injected into the reactor vapors of a mixture of ethanol and acetonitrile (50:50) for one hour. After cooling to room temperature from the reactor goes to the boat with a black substance. The resulting material is placed in a glass the second container and is filled with a solution of diluted hydrochloric acid (1:1) under stirring to obtain a fine mist of black substance in solution. The obtained suspension is filtered on a membrane filter and washed repeatedly with small portions of distilled water until neutral pH. The precipitate is dried in air or in a drying Cabinet with a temperature of 100°C to constant weight. The obtained carbon material is characterized by a high specific surface 930 m2/g, a pore distribution of 10-30 nm and pore volume 3.3 cm3/year

Example 7. Obtaining mesoporous carbon material using a mixture of liquid carbon sources - toluene-acetonitrile (70:30), while the ratio in the mixture may be any, as they are well mixed, and does not affect the textural characteristics of the material, obtaining lead analogously to example 6. The obtained carbon material is characterized by a high specific surface 917 m2/g, a pore distribution of 10-20 nm and a pore volume 3.1 cm3/year

Example 8. A portion of the calcium tartrate (~100 mg)containing 0.2 at.% iron, placed in a ceramic boat and enter into the chamber of the reactor, the reactor is heated to 800°C. thermal decomposition of the original substance is carried out in an inert atmosphere for 10 minutes During this time, the original connection is decomposed with the formation of oxide. Next, at 800°C in the reactor serves a gaseous source of carbon - ethylene, is passed through the vessel with liquid carbon source - ethanol during the hour. After cooling to room temperature from the reactor goes to the boat with the black substance. The resulting material is further processed analogously to example 3. The obtained carbon material is characterized by a specific surface 901 m2/g, a pore distribution of 15-30 nm and pore volume 3.2 cm3/year

Example 9. Obtaining mesoporous carbon material using a mixture of the carbon source is methane-acetonitrile - lead analogously to example 8. The obtained carbon material is characterized by a specific surface area of 927 m2/g, a pore distribution of 10-20 nm and a pore volume 3.2 cm3/year

Thus, the experimental data show that the use of the proposed method to obtain porous carbon with the given parameters. Carbon porous material tested as electrode material for supercapacitors (Cbeats=230 f/g at a scan rate of potential 10 mV/s for the carbon material obtained on the basis of tartrate of calcium doped 0.8%Fe), and lithium-ion battery (capacity lithium intercalation carbon material obtained using tartrate-doped 0.2% Fe, is about 550 mAh/g at a current charge-discharge 50 mA/g). The data obtained demonstrate the prospects of use of this product in the electrochemical the industry.

1. The carbon material of the nanostructure which is formed by carbon atoms having porosity with a developed specific surface, characterized in that it is homogeneous mesoporous carbon material and is characterized by a specific surface 850-930 m2/g, pore volume 2.9-3.3 cm3/g and an average pore diameter of 10-30 nm.

2. A method of obtaining a carbon material including the interaction between calcium salts, which is the predecessor of the template, and a carbon source at 700-900°C followed by treatment of the resulting product with hydrochloric acid, characterized in that as the predecessor of the template using the tartrate of calcium or calcium tartrate-doped transition metal, and as a source of carbon use liquid or gaseous carbon-containing compounds or mixtures thereof.

3. The method of receiving according to claim 2, characterized in that the concentration of the doped transition metal is less than 1 at.%

4. The method of receiving according to claim 2, characterized in that the use of dilute hydrochloric acid.



 

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