RU2537306C2 - Processing method of heavy hydrocarbon compounds so that volumetric carbon frame is obtained (versions) - Google Patents

Abstract

FIELD: oil and gas industry.

SUBSTANCE: invention relates to oil processing industry and can be used at processing of oil or heavy hydrocarbon compounds to obtain a volumetric carbon frame for composite materials. In compliance with the proposed method, a formwork is prepared, the cross section of which determines a profile of the carbon frame, and mass of a solid-state melting catalyst - blowing agent is formed inside the formwork by means of individual components having either a regular or irregular geometrical shape; besides, laying of the individual components is performed so that an inter-rib gap forms continuous inter-rib formwork channels along ribs and tops of the laid bodies. A raw mixture is prepared by addition to heavy hydrocarbon compounds of a cocatalyst consisting of a mixture of light hydrocarbons; the inter-rib formwork channels are filled inside the formwork in the body of the mass of the solid-state melting catalyst - blowing agent with the raw mixture; the formwork is fully placed into a melt of a catalytic mixture having the temperature of 200-300°C, and the formwork is exposed in the melt of the catalytic mixture till melting of the mass of the solid-state melting catalyst - blowing agent and formation of a volumetric carbon frame. Then, the formwork is removed together with the obtained volumetric carbon frame and the latter is cleaned from residues of the liquid melt of the catalytic mixture. As a melting catalyst - blowing agent, a mixture of metal chlorides is used, which has a melting temperature of 180-200°C.

EFFECT: simpler production of a carbon frame owing to excluding a carbon fibre production stage.

16 cl, 3 tbl, 4 dwg

Description

The invention relates to the oil refining industry and can be used in oil refining, namely in the processing of heavy hydrocarbon compounds to obtain a bulk carbon frame.

Currently, the manufacture of composite materials using bulk carbon frames is widespread. The unique properties of the new carbon materials and their combination in relation to specific consumer values can significantly increase the range of their practical use, including in civil engineering. High strength characteristics allow the use of carbon frames as reinforcing elements of composite materials; heat resistance in combination with chemical inertness - in the form of finishing products of internal and external coatings (decorative tiles, etc.); heat resistance and chemical inertness - in heat-insulating structures. The only factor restraining the massive use of carbon frames is their high cost, and therefore, significant technological costs for their manufacture.

A technical solution is known in which a three-dimensional frame is made of carbon fiber yarns made by the three-dimensional weaving method in the form of a spatial shell (Application for the grant of a patent of the Russian Federation 2000123974, IPC СВВ 31/00, priority from 09/19/2000). In the known technical solution, dressings are used - Ural N-22. In the tangential direction and along the generatrix of the reinforcing surface, carbon fibers UKN-5000 are used. The dressing threads form angles of 40-50 ° with the threads located in the axial section planes along the generatrix surface. The prepared frame is placed in an oven, the pyrocarbon matrix is precipitated in an isothermal manner. At the same time, the binder is carbonized.

A technical solution is known in which a three-dimensional frame is made by pulling the fibers of the supporting rod through separate channels, followed by winding with a winding bundle (RF Patent 2405092, priority from 12/26/2008, IPC Е04С 5/07). In this technical solution for the manufacture of the carcass, a method for pre-laying carbon fiber in bundles and their subsequent processing is used. So, the bearing rod of the composite reinforcement is made in the form of an array of low-modulus fibers with reinforcement previously and evenly laid in bundles of high-modulus fibers. Low-modulus and high-modulus fibers are evenly distributed over the channels and impregnated with a polymer binder based on synthetic resins that provide the necessary strength properties of the composite matrix.

A technical solution is known in which the volumetric frame is made of separate modules made by pretreatment and bundling carbon fiber filaments, then each module is subsequently impregnated with a carbon-containing composition, protective coatings are applied, followed by carbonization or graphitization, and pyrocarbon is saturated with gaseous or liquid hydrocarbons (Application for the grant of a patent of the Russian Federation 2008136197, priority date 09.09.2008, IPC С04В 35/83). The volumetric frame is assembled by adding the modules in the given order into a single package, followed by cold or hot pressing and / or flashing with thread or rods along one of the workpiece coordinates. Next, the final operations are carried out to saturate the framework with pyrocarbon in the atmosphere of gaseous or liquid hydrocarbons, carbonization, graphitization, thermal oxidation, and the application of protective coatings.

The disadvantages of the known technical solutions is the significant duration of the production process in time, the hardware complexity and the complexity of operations aimed at obtaining the strength characteristics of carbon fiber (carbon). Thus, expensive carbon filaments having significant strength characteristics predetermine the high price level of bulk carbon skeletons and, therefore, hinder their use in the national economy. As noted above, new carbon materials have unique properties, where strength characteristics are one of their types. There are needs where strength characteristics are not critical. For example, decorative tiles for interior or exterior decoration of buildings and premises. At such a positioning angle, the characteristic is the high fire resistance and incombustibility of carbon materials. Products with such characteristics are in high demand on the market (just cite the tragedy at the Lame Horse club as an example). In this case, in order to meet market demand, the product is in need of fragile characteristics of the material of carbon frames, such as chemical inertness, environmental friendliness, color gamut, and heat resistance. Strength characteristics are of secondary importance, exclusively within the framework of the self-supporting frame of the tile structure. Thus, the integrated use of the properties of carbon frames is limited to the prerequisite for paying the imputed cost of technologies for obtaining strength characteristics in carbon fiber, which may be unnecessary for specific needs.

The production of bulk carbon frames directly from heavy hydrocarbon compounds, bypassing the stages of manufacturing yarns having affordable prices for mass use, could contribute to the wide development of production and the introduction of new composite materials in the general civil sector (building materials and structures, furniture plates, a wide range of decorative, finishing non-combustible and environmentally friendly materials, etc.).

Known technical solutions in which using multi-stage processing of raw materials from heavy hydrocarbon compounds receive carbon fibers (Patent GB 1071400, "Method for producing carbon structures from molten baked substances", IPC B65D 85 / 804B priority number JP 19630058942, 1963-11-01 ; Patent GB 1091890, "Production of carbon or graphite filaments", IPC D01F 9/145, priority number JP 19650002928 1965-01-2).

Known technical solutions for the processing of heavy hydrocarbon compounds that describe carbon fiber production processes in which the raw material is pretreated to facilitate spinning and increase the mechanical properties of the fibers (German Patent 1208894 "PROCESS FOR PRODUCING CARBON FILAMENTS", IPC D01F 9/145, D01F 9/15, French patent No. 2052112, IPC D01F 9/145, priority from 1969-07-17). Such auxiliary processes for the preparation of raw materials include, in particular, the processes of incorporation of sulfur, polymers such as polyethylene and polystyrene, the introduction of plasticizers such as castor oil, or alkylated and sulfided derivatives.

Known technical solutions that describe the processes of preliminary preparation and processing of raw materials to facilitate the spinning process and improve the mechanical properties of the fibers by processing the raw materials with a solvent so as to isolate the most volatile products before the fiber spinning operation. Solvents may be, for example, acetone, hexane, toluene or quinoline (UK Patent No. 1208894, French Patent No. 2113351, IPC C01B 31/00, priority number US 19700084883 1970-10-28).

A well-known technical solution for processing raw materials for producing carbon fiber discloses a method of heat treatment and distillation of coal tar pitch, aimed at increasing the average molecular weight of raw materials by polymerization (US Patent No. 3595946, IPC D01F 9/15, 01/31/01, priority number US 19680734257 1968-06 -04). Moreover, to accelerate the process can be used various means aimed at oxidation, dehydrogenation and polymerization. The raw material thus prepared is then used to make a yarn by spinning, which is then carbonized and graphitized.

A technical solution is known, which is taken as a prototype (US Patent No. 4431623, IPC С10С 3/14; D01F 9/14; D01F 9/145, priority number GB 19810017658, 1981-06-09). In a known technical solution, the process of producing carbon fiber from petroleum bitumen resins involves the preparation of raw materials from a heavy steam cracking residue by heat treatment and heat exposure, at which the melting temperature of the processed raw material in step 1 is between 55 and 90 ° C, in step 2 is between 85 ° C and 110 ° C and step 3 - between 350 and 450 ° C. Further, the method includes obtaining fiber by spinning from prepared raw materials at a temperature above its melting point, then, to ensure refractoriness, the obtained fibers are treated with a gas mixture: (a) NO and O ₂ at a temperature not exceeding 200 ° C, or (b) halogens in gaseous form, followed by treatment with O ₂ at a temperature of not more than 250 ° C, or (c) SO ₂ , separately or mixed with O ₂ , at a temperature of not more than 300 ° C, at which the resin content in the fiber body is controlled by the value not above 30% by weight, then the fibers when heated Carbonization and, if desired, graphitization.

The disadvantages of the known technical solutions is the fact that each of the above patents provides for a long and energy-intensive preparation of the hydrocarbon feedstock in order to obtain the necessary plasticity and purity indicators of the prepared feedstock necessary for the fiber spinning process, since, regardless of the method used, the only form of the finished product in the above technical solutions is carbon fiber or carbon. These shortcomings determine, on the one hand, the high cost of carbon fiber obtained, on the other hand, provide for the mandatory subsequent process of obtaining a carbon skeleton, which will further increase the cost of the final product. In aggregate, it can be noted that at present the process for producing bulk carbon skeletons consists of two stages: a) various methods for carrying out the process for producing carbon dioxide or carbon fiber; and b) various methods for the production of carbon fiber (carbon fiber) bulk carbon skeleton.

The objective of the invention is to develop a method for the processing of heavy hydrocarbon compounds, which allows to obtain bulk carbon frames of various shapes in one process, bypassing the process of obtaining coal.

The problem is solved in that in the method of organizing the processing of heavy hydrocarbon compounds to obtain a bulk carbon frame, including the use of heavy hydrocarbon compounds and subsequent processing of the resulting product, the raw material mixture is additionally prepared by introducing into the heavy hydrocarbon compounds a cocatalyst consisting of a mixture of light hydrocarbons, a catalytic mixture is prepared , which is either a mixture of metal chlorides having a melting point of 180-200 ° C and a temp. a boiling point of 600-620 ° C, or a mixture of metal chlorides with the addition of a process intensifier, a formwork is prepared, the cross section of which determines the profile of the carbon skeleton, is formed inside the formwork, from individual elements of the solid-state fusible blowing catalyst having either the correct or irregular geometric shape , an array of solid-state fusible catalyst-blowing agent, laying individual elements in such a way that the intercostal gap forms along the edges and tops of the street Born bodies inextricable intercostal formwork channels. The intercostal formwork channels in the solid solid fusible catalyst-pore former array are filled with the raw material mixture inside the formwork form. Next, the formwork form, together with the solid-state fusible catalyst-pore former massif and the intercostal formwork channels filled with the raw material mixture in the body of the solid-state fusible catalyst-pore former massif, is placed completely in the melt of the catalytic mixture, having a temperature of 200-300 ° C, and kept in the melt of the catalytic mixture until melting an array of solid-state fusible catalyst-blowing agent and the formation of a volumetric carbon skeleton, the formwork is removed together with the obtained volume nym carbon skeleton. After that, the obtained volumetric carbon skeleton is purified from the remnants of the molten liquid of the catalytic mixture. In this case, either heavy native high molecular weight oil compounds, or peaks, or products of heat treatment of lignin, or polyvinyl chloride, or bottoms from the distillation of benzyl chloride, or chlorobenzene, or natural and artificial asphalts, or bitumen, or chemical refining products are used as heavy hydrocarbon compounds. crude oil and petroleum products, or products of extraction of coal with aromatic hydrocarbons, or waste from the oil and coal industries. As an intensifier of the catalytic mixture, complex compounds are used, which are alkyl derivatives of metals of groups I-III of the Periodic system with transition metal halides. As light hydrocarbons, a hydrocarbon fraction with a boiling point below 200 ° C is used; a hollow mesh structure is used as the formwork. Individual elements having the correct or irregular geometric shape of the solid-state fusible catalyst-blowing agent array are made of liquid melt of the catalytic mixture, and either the prism, or the pyramid, or the cylinder, or the cone, or the sphere, or the regular polyhedron are used as the correct geometric shape, either a polyhedron, or a parallelepiped, or a tetrahedron, and crushed chips are used as an irregular geometric shape. On the edges of the individual elements of the correct geometric shape of the array of solid-state fusible catalyst-blowing agent, a chamfer is either rectilinear or curved. Purification of the obtained product is carried out at a temperature equal to or higher than 650 ° C. The resulting bulk carbon frames are subdivided: a) carbon frame - when using the correct form of the elements of the fusible solid-state catalyst-blowing agent and b) foam carbon - when using the irregular shape of the elements of the fusible solid-state catalyst-blowing agent.

In another embodiment, in the method of organizing the processing of heavy hydrocarbon compounds to obtain a bulk carbon frame, including the use of heavy hydrocarbon compounds, the subsequent processing of the resulting product is additionally carried out in the following steps:

additionally, a raw material mixture is prepared by introducing into a heavy hydrocarbon compound a cocatalyst consisting of a mixture of light hydrocarbons, a catalytic mixture is prepared, which is either a mixture of metal chlorides having a melting point of 180-200 ° C and a boiling point of 600-620 ° C, or a mixture of metal chlorides with the addition of a process intensifier;

prepare the formwork, the cross section of which determines the profile of the carbon skeleton, fill the formwork with a raw material mixture and place it on the surface, and then completely into the molten liquid of the catalyst mixture having a temperature of 200-300 ° C, maintain the formwork in the molten catalyst mixture until a bulk carbon skeleton in the form of a non-woven carbon web. Next, the formwork is removed together with the obtained carbon skeleton and the obtained carbon skeleton is purified from the remnants of the molten liquid of the catalytic mixture. In this case, either heavy native high molecular weight oil compounds, or peaks, or products of heat treatment of lignin, or polyvinyl chloride, or bottoms from the distillation of benzyl chloride, or chlorobenzene, or natural and artificial asphalts, or bitumen, or chemical refining products are used as heavy hydrocarbon compounds. crude oil and petroleum products, or products of extraction of coal with aromatic hydrocarbons, or waste from the oil and coal industries. As an intensifier of the catalytic mixture, complex compounds are used, which are alkyl derivatives of metals of groups I-III of the Periodic system with transition metal halides. As light hydrocarbons, a hydrocarbon fraction with a boiling point below 200 ° C is used, and a hollow mesh structure is used as the formwork. While cleaning the resulting product is carried out at a temperature above 650 ° C.

The technical result of the claimed invention consists in simplification by combining the operational stages of obtaining structural material and its shaping, in the possibility of forming a given pattern of the spatial arrangement of the ribs of the obtained frame, in expanding the range of the range of processed raw materials, in reducing energy consumption due to the exclusion of auxiliary operations, including thermal exposure, in reducing the cost of the process. In general, the claimed technical solution provides an expansion of the range of the range of processed raw materials, an increase in speed and a reduction in the production cycle of manufacturing products, and consequently, a reduction in energy consumption and cost of finished products.

In FIG. 1 is a flowchart of the method, where it is indicated: 1 — heavy carbon compounds, 2 — cocatalyst, 3 — raw material mixture, 4 — individual elements of a solid-state fusible catalyst-blowing agent, 5 — formwork form, 6 — an array of solid-state fusible catalyst-blowing agent, 7 - formwork filled with the prepared mixture with an array of solid-state fusible catalyst-blowing agent containing intercostal formwork channels, 8 - catalytic mixture, 9 - intensifier, 10 - filled with raw mixture formwork immersed in the melt of the catalytic mixture, 11 — formed bulk carbon skeleton inside the melt of the catalytic mixture, 12 — extracted bulk carbon skeleton, 13 — bulk carbon skeleton removed from the remains of the catalytic mixture, 14 — carbon skeleton for subsequent processing.

In FIG. 2 shows a diagram of the dimensions and laying in the formwork of elements of a solid-state fusible catalyst-blowing agent, where A is a display of an element of a solid-state fusible catalyst-blowing agent in an orthographic projection, B is a diagram of the laying of elements of a solid-state fusible catalyst-blowing agent in a formwork, C is a display of two laid in the lower row elements of solid-state fusible catalyst-blowing agent in isometric projection, D is the cross section of the stacked elements of solid-state fusible catalyst a-pore former with the display of formwork channels in the intercostal space.

In FIG. 3 presents a diagram of a carbon skeleton obtained as a result of the claimed technical solution using a solid-state fusible solid-state pore-forming catalyst (prism).

In FIG. 4 presents a General technological scheme for producing carbon structures, giving an idea of the organization of the proposed technical solution, where: 1 - a device for preparing the raw mix; 2, 3 — a reactor consisting of a bath with a molten catalyst mixture (2) and a forced gas exhaust hood (3), equipped with pressure rollers (5) and mixers (4); 6 - separation tank; 7 - condensation capacity of light hydrocarbons; 8 - block storage of hydrogen chloride (HCl) and chlorine recovery (Cl); 9 - distillation column; 10 - furnace carbonization products; 11 - graphitization furnace products.

The claimed technical solution for the organization of the processing of heavy hydrocarbon compounds to obtain volumetric carbon frames (item 1) in the form of carbon frames, implemented using elements of a fusible solid-state catalyst-pore former of the correct form (prism) is as follows.

Product positioning according to the claimed technical solution: Finished products. Carbon frame. Due to its versatility, the carbon skeleton can act as a component of composite materials (for example, as reinforcing structural elements: partitions, panels, etc.) or decorative products (for example, three-dimensional wall or ceiling coating). In this example, an element of a decorative wall covering is implemented on a self-supporting frame for indoor or outdoor premises with a size of 200 * 200 * 5 mm with a cell of 10 * 5 mm (Fig. 3). Color - black coal. The main advantages over existing on the market - the material relates to non-combustible building materials and structures for interior decoration. This conclusion can be made on the basis that the temperature regime for obtaining the material, in particular in the carbonization zone (1000-1100 ° C), exceeds the temperature regime for testing the obtained material for combustibility (745-755 ° C) according to GOST 30244-94. Building materials. Combustibility test methods, clause 6.4.3.

Preparation of the raw mix (1 frame). To prepare the raw material mixture, dehydrated heavy hydrocarbon compounds of a fraction of 350-500 ° C, density 889 kg / m ³ (Fig. 1, p. 1) in the amount of 18.59 g, as well as cocatalyst (Fig. 1, p. 2) were used ) a hydrocarbon fraction with a boiling point below 200 ° C in an amount of 1.65 g. The total mixture of raw materials (Fig. 1, p. 3) = 1.65 g + 17.99 g = 20.2 g.

Preparation of the catalytic mixture. By sequential mixing of the components and bringing the mixture to a melt state at t = 200 ° C, a catalytic mixture (Fig. 1, p. 8) of 1634.71 g was prepared. 94.05 g of Ziegler-Natta catalyst (Al ( C ₂ H ₅ ) ₂ Cl + TiCl ₄ ) (Fig. 1, p. 9), as well as metal chlorides: AlCl ₃ - 1076.04 g; FeCl ₃ - 352.8 g; TiCl ₄ - 54.5 g; VCl ₄ - 57.33 g.

The prepared catalyst mixture was used as follows: 1222 g of the prepared catalyst mixture with a temperature of 200 ° C was placed in a reaction bath (Fig. 4, p. 2) and then, the mixture was heated to 200 ° C. This temperature was systemically maintained by a thermostat; the second part in the amount of 412.8 g was directed to the manufacture of elements of the solid-state fusible catalyst-blowing agent (Fig. 4, p. 4).

Preparation of elements of solid-state fusible catalyst blowing agent. In accordance with the accepted form of the carbon frame structure (Fig. 3), the elements of the solid-state fusible catalyst-pore former have the correct geometric shape of the prism, at the top of which lies an isosceles right triangle, and the prism base has a size of 10 * 5 mm with chamfered edges. The dimensions of the solid-state fusible catalyst-blowing agent element (Fig. 2, a, b). The total number of elements of solid-state fusible catalyst 1600 pcs. on one coal frame.

The formwork form (Fig. 1, p. 5) for the elements of the solid-state pore-forming catalyst was made of fluoroplast-4 material. This form has 1600 single shuttering places, each of which fully corresponds to the figure of the element of the solid-state fusible catalyst-blowing agent, located with the top down. 412.8 g of a molten to liquid state of a catalytic mixture with a temperature of 200 ° C were poured into a pre-prepared form. Further, the mold with the melt was cooled to room temperature, as a result of which the molten melt cast into the mold turned into a solid state of aggregation, assuming the given geometric shape of the elements of the solid-state fusible catalyst-blowing agent. The elements of the solid-state fusible catalyst-blowing agent thus prepared were removed from the mold and prepared for the next operation — laying in the array of the solid-state fusible catalyst-blowing agent (Fig. 1, p. 6).

Laying the elements of the solid-state fusible catalyst in the formwork form (Fig. 1, p. 6). The formwork made of fluoroplast-4 follows the contours of the finished frame 200 * 200 * 5 mm with a cell 10 * 5 mm (Fig. 3). The side walls of the formwork mold have a screed mechanism, which allows, after laying and filling the mold with solid-state catalyst elements, to fix the stacked mass in the mold by compression. The shape of the lattice bottom of the shuttering form provides the device with a given chamfer profile, as well as the possible pouring of the raw mix from the shuttering channels when filling. The formwork lid when it is closed after laying the array of solid-state catalysts provides both the possibility of filling the raw material mixture and the formation of the necessary bevel profile. At the time of laying, the elements of the solid-state fusible catalyst-blowing agent were in a solid state of aggregation. The stacking of elements was carried out sequentially in 2 rows. The first row was laid on the edge of the larger face of the element, comprising 10 mm. The elements were stacked tightly to each other, then the stacked array was compressed in the formwork by the screed mechanism. The laying pattern of the lower row (Fig. 2C, B), the upper row (Fig. 2B), taking into account the chamfer along the edges of each individual element, provides in the intercostal space the formation of formwork channels along the edges of the element (Fig. 2D).

Filling an array of solid-state catalyst elements with a raw material mixture. The prepared raw mix (Fig. 1, p. 3) in an amount of 20.2 g was heated to 70 ° C and then poured into the formwork onto the prepared and fixed array of elements of the solid-state pore-forming catalyst. The condition of filling all formwork channels with the mass of the raw mix was monitored. After pouring the raw material mixture, the filled form was aged 3-5 minutes until the end of active gas evolution (Fig. 1, p. 7).

The reaction block. After the cessation of active gas evolution, the formwork, filled with the raw mixture with an array of solid-state catalyst elements, was moved into the bath with the melt of the catalytic mixture and completely immersed in the melt body (Fig. 1, p. 10). At the same time, along with the dissolution of the elements of the solid-state catalyst and the formation of the carbon skeleton, technological flows were carried out (according to Fig. 4, p. "Traffic flows"). The exposure time in the reaction bath is 5 minutes Impregnation conditions - complete dissolution or transition of elements of a solid-state fusible catalyst-blowing agent into a liquid state of aggregation. After dissolution of the solid-state catalyst array, the formwork was removed, and the formed carbon skeleton (Fig. 1, p. 11) was fed to the pinch rollers (Fig. 4, p. 5), through which the catalytic mixture was transported through the melt array to the cleaning and carbonization zone (Fig. 4, p. 10), where it was cleaned (Fig. 1, p. 12).

Cleaning up. Partially, the process of cleaning regime begins even in the reaction bath at the time of shaping of the non-melting body of the future carbon skeleton. In the body of the liquid melt, the initial hydrocarbon feed is purified from mechanical impurities, sulfur, oxygen compounds and other organoelemental compounds. Some of them turn into a solid precipitate, sink to the bottom of the bath and then are removed in the form of sludge; part passes into a gaseous form (СО, СО ₂ ) and is caught by exhaust. In parallel with the cleaning, the formation of a non-fusible spatial framework of a given shape is carried out. The second zone of purification from the remains of the catalytic mixture is provided before the carbonization furnace. Directly in the cleaning zone, the mode provides for a sequential increase in temperature from ~ 200 ° C at the inlet to 650 ° C at a rate of no higher than 200 ° C per hour in argon. Such a regime, on the one hand, ensured an increase in the properties of refractoriness, and, on the other hand, ensured the sublimation of the remains of the catalytic mixture and the released compounds. The presence of active chlorine in the remains of the catalytic mixture contributed to the development of these processes. (Fig. 1, p. 13). Upon completion of the cleaning process, the carbon skeleton (Fig. 1, p. 14) was moved to the carbonization zone (Fig. 4, p. 11), which was carried out at a temperature of 1000 ° C. Upon completion of carbonization, the sample had a weight of 12.56 g, density 1.32 g / cm ³ , porosity 88.38%.

Qualitative characteristics of the carbon frame. After the operation of cleaning and heat treatment at a temperature of more than or equal to 650 ° C, the carbon frame already had a certain strength, providing at least self-supporting properties. The necessary strength characteristics for structural materials can be obtained during subsequent carbonization, graphitization, as well as other operations associated with obtaining a composite material, for example carbidization (deposition and preparation of silicon carbide coating on the surface of the carbon frame).

If in the production of carbon fiber the main task is to obtain the highest possible strength characteristics, the main task of the proposed technical solution is to form a spatial carbon structure in one step, bypassing the stage of production of coal (carbon fiber). Therefore, the main condition is to obtain the frame itself as a product. Defects in the form of gaps in the solid body of the frame can, depending on the degree of their presence, completely or partially destroy the frame. Thus, for this invention is significant characteristic - the level of defectiveness (D _f ). This characteristic is calculated as the ratio of the total area of the product to the area of open defects (%).

The ideal option is D _f → 0. The most optimal mode in actual conditions D _f → min. There is a close relationship between the melt temperature of the catalytic mixture and the value of D _f . Optimization options for this indicator by modeling the main characteristics of the mode are shown in examples 1-4.

Example 1

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 450 ° C. Upon contact of the feed mixture with the melt of the catalytic mixture occurs, including rapid gas evolution. The proportion of the sublimated part of the feed mixture (gas phase) is 80%. The fraction of the condensed carbon-containing part in the formwork is 20%. By removing the carbon skeleton from the melt (Fig. 1, p. 12), D _f is 42%. There are no whole blocks in horizontal and vertical planes. The frame is not self-supporting.

Example 2

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 320 ° C. The fraction of the sublimated part of the feed mixture (gas phase) is 69%. The fraction of the condensed carbon-containing part is 31%. Df is 26%. There are no separate nodes and jumpers in horizontal and vertical planes. The frame is not self-supporting.

Example 3

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. The proportion of the sublimated part of the feed mixture (gas phase) is 54%. The fraction of the condensed carbon-containing part is 46%. Df is 14%. Deep defects on the frame elements in horizontal and vertical planes.

Example 4

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. We introduce 10% of the Ziegler-Natta catalyst ((C ₂ H ₅ ) ₂ AlCl + TiCl ₄ ). The proportion of the sublimated part of the feed mixture (gas phase) is reduced and amounts to 27%. The fraction of the condensed carbon-containing part is 73%. D _f is 5%. Minor defects on the frame elements in horizontal and vertical planes.

Comparative table of the degree of defectiveness of the characteristics and process conditions

Conclusion: The most optimal temperature for processing the raw mixture in the reaction bath is the temperature of sample 4. This temperature regime allows, on the one hand, the necessary reactions to be carried out in the processed mixture, and, on the other hand, the necessary amount of carbon material is formed and used to form a bulk carbon skeleton.

The claimed technical solution for the organization of the processing of heavy hydrocarbon compounds to obtain bulk carbon frames (item 1) in the form of carbon foam, implemented using elements of a fusible solid-state catalyst-blowing agent of irregular shape (crushed chips) is as follows.

Product positioning according to the claimed technical solution: Finished products: Decorative tiles for interior decoration of foam. Due to its versatility, the carbon frame can act as a component of composite materials (for example, as reinforcing structural elements: partitions, panels, etc.) or decorative products (for example, volumetric wall or ceiling coating). In this example, an element of a decorative wall covering is implemented on a self-supporting frame for indoor or outdoor premises with a size of 200 * 200 * 5 mm. Color - black coal. The main advantages over existing on the market - the material relates to non-combustible building materials and structures for interior decoration. This conclusion can be made on the basis that the temperature regime of obtaining the material, in particular, in the carbonization zone (1000-1100 ° C) exceeds the temperature regime of testing the obtained material for combustibility (745-755 ° C) according to GOST 30244-94. Building materials. Combustibility test methods, clause 6.4.3. An additional feature emphasizing market advantage is the noise absorption inherent in any porous saturated structure.

Preparation of the raw mix (1 tile). To prepare the raw material mixture with a volume of 30 cm ³ , dehydrated heavy hydrocarbon compounds of a fraction of 350-500 ° C, density 889 kg / m ³ (Fig. 1, p. 1) in an amount of 24.00 g, and also cocatalyst (Fig. 1) were used , p. 2) a hydrocarbon fraction with a boiling point below 200 ° C in an amount of 2.13 g. The raw material mixture in total (Fig. 1, p. 3) = 2.13 g + 24.0 g = 26.13 g.

Preparation of the catalytic mixture. By sequential mixing of the components and bringing the mixture to a melt state at t = 200 ° C, a catalytic mixture (Fig. 1, p. 8) of 1634.71 g was prepared. 94.05 g of Ziegler-Natta catalyst (Al ( C ₂ H ₅ ) ₂ Cl + TiCl ₄ ) (Fig. 1, item 9), as well as metal chlorides: AlCl ₃ - 1076.04 g. FeCl ₃ - 352.8 g. TiCl ₄ - 54.5 g. VCl ₄ - 57.33 g.

The prepared catalyst mixture was used as follows: 1237.7 g of the prepared catalyst mixture with a temperature of 200 ° C was placed in the reaction bath (Fig. 4, p. 2) and then, the mixture was heated to 200 ° C. This temperature was systemically maintained by a thermostat; the second part in the amount of 397.0 g by cooling was transferred to the solid state of aggregation and was sent to the preparation of the elements of the solid-state fusible catalyst-blowing agent (Fig. 4, p. 4) of irregular shape - crushed crumbs.

Preparation of the elements of the solid-state fusible catalyst-blowing agent of irregular shape (crushed crumbs). The cooled array of the catalytic mixture in a volume of 170 cm ³ and weighing 397 g was crushed in a mill into crumbs with an average grain size of 1-2 mm and then placed into the formwork.

Laying the elements of the solid-state fusible catalyst of irregular shape in the formwork form (Fig. 1, p. 6). The formwork made of fluoroplast-4 follows the contours of the finished frame 200 * 200 * 5 mm. The side walls of the formwork mold have a screed mechanism, which allows, after laying and filling the mold with crushed crumbs of the solid-state pore former, to fix the stacked mass in the mold by compression. The shape of the lattice bottom of the formwork provides contact of the crushed chips with the melt of the catalyst mixture. The lid of the formwork form when it is closed after laying the array of solid-state catalysts provides both the possibility of pouring the raw material mixture and the release of gases. At the time of laying, the elements of the solid-state fusible catalyst-pore former in the form of crushed chips were in a solid state of aggregation. The crushed chips were laid in the formwork, followed by surface leveling.

Filling an array of solid-state catalyst elements with a raw material mixture. The prepared raw mix (Fig. 1, p. 3) in an amount of 26.1 g was heated to 70 ° C, then poured into the formwork onto the prepared array of crushed crumbs of solid-state pore-forming catalyst. The condition of filling all the voids with the mass of the raw mixture was monitored. After pouring the raw material mixture, the filled form was fixed by closing the lid and held for 3-5 minutes until the end of active gas evolution (Fig. 1, p. 7).

The reaction block. After the cessation of active gas evolution, the formwork, filled with the raw mix, with an array of crushed crumbs of the solid-state pore-forming catalyst, was moved into the bath with the catalyst mixture melt and completely immersed in the melt body (Fig. 1, p. 10). At the same time, along with the dissolution of the elements of the solid-state catalyst and the formation of the carbon skeleton, technological flows were carried out (according to Fig. 4, paragraph “transport streams.” The exposure time in the reaction bath was 5 minutes. Impregnation conditions — complete dissolution or transition of the elements of the solid-state fusible catalyst — the pore former in a liquid state of aggregation.After dissolving the solid-state catalyst array, the formwork was removed, and the formed carbon skeleton (Fig. 1, p. 11) was fed to the fixture back focus lock clips (Figs. 4, p. 5), through which is transported through the array molten catalyst mixture in the purification and carbonization zone (Fig. 4, p. 10), where performed its cleaning (Fig. 1, p. 12).

Cleaning up. Partially, the process of cleaning regime begins even in the reaction bath at the time of shaping of the non-melting body of the future carbon skeleton. In the body of the liquid melt, the initial hydrocarbon feed is purified from mechanical impurities, sulfur, oxygen compounds and other organoelemental compounds. Some of them turn into a solid precipitate, sink to the bottom of the bath and then are removed in the form of sludge; part passes into a gaseous form (СО, СО ₂ ) and is caught by exhaust. In parallel with the cleaning, the formation of a non-fusible spatial framework of a given shape is carried out. The second zone of purification from the remains of the catalytic mixture is provided before the carbonization furnace. Directly in the cleaning zone, the mode provides for a sequential increase in temperature from ~ 200 ° C at the inlet to 650 ° C at a rate of no higher than 200 ° C per hour in argon. Such a regime, on the one hand, ensured an increase in the properties of refractoriness, and, on the other hand, ensured the sublimation of the remains of the catalytic mixture and the released compounds. The presence of active chlorine in the residues of the catalytic mixture contributed to the development of these processes (Fig. 1, p. 13). Upon completion of the cleaning process, the sample (Fig. 1, p. 14) was moved to the carbonization zone (Fig. 4, p. 11), which was carried out at a temperature of 1000 ° C. Upon completion of carbonization, the sample had a weight of 16.22 g, a density of 1.32 g / cm ³ , porosity of 85.0%.

Qualitative characteristics of foam tile. After the operation of cleaning and heat treatment at a temperature of more than or equal to 650 ° C, the carbon frame already had a certain strength, providing at least self-supporting properties. The necessary strength characteristics for structural materials can be obtained during subsequent carbonization, graphitization, as well as other operations associated with obtaining a composite material, for example, carbidization (deposition and obtaining a silicon carbide coating on the surface of the carbon frame).

If in the production of carbon fiber the main task is to obtain the highest possible strength characteristics, the main task of the proposed technical solution is to form a spatial carbon structure in one step, bypassing the stage of production of coal (carbon fiber). Therefore, the main condition is to obtain the frame itself as a product. Defects in the form of gaps in the solid body of the frame can, depending on the degree of their presence, completely or partially destroy the frame. Thus, for this invention is significant characteristic - the level of defectiveness (D _f ). This characteristic is calculated as the ratio of the total area of the product to the area of open defects (%).

The ideal option is D _f → 0. The most optimal mode in actual conditions D _f → min. There is a close relationship between the melt temperature of the catalytic mixture and the value of D _f . Optimization options for this indicator by modeling the main characteristics of the mode are shown in examples 1-4.

Example 1

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 450 ° C. Upon contact of the feed mixture with the melt of the catalytic mixture occurs, including rapid gas evolution. The proportion of the sublimated part of the feed mixture (gas phase) is 80%. The fraction of the condensed carbon-containing part in the formwork is 20%. By removing the carbon skeleton from the melt (Fig. 1, p. 12), D _f is 42%. There are no whole blocks in horizontal and vertical planes. The frame is not self-supporting.

Example 2

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 320 ° C. The fraction of the sublimated part of the feed mixture (gas phase) is 69%. The fraction of the condensed carbon-containing part is 31%. D _f is equal to 26%. There are no separate nodes and jumpers in horizontal and vertical planes. The frame is not self-supporting.

Example 3

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. The proportion of the sublimated part of the feed mixture (gas phase) is 54%. The fraction of the condensed carbon-containing part is 46%. D _f is equal to 14%. Deep defects on the frame elements in horizontal and vertical planes.

Example 4

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. We introduce 10% of the Ziegler-Natta catalyst ((C ₂ H ₅ ) ₂ AlCl + TiCl ₄ ). The proportion of the sublimated part of the feed mixture (gas phase) is reduced and amounts to 27%. The fraction of the condensed carbon-containing part is 73%. D _f is 5%. Minor defects on the frame elements in horizontal and vertical planes.

Comparative table of the degree of defectiveness of the characteristics and process conditions

Conclusion: The most optimal temperature for processing the raw mixture in the reaction bath is the temperature of sample 4. This temperature regime allows, on the one hand, the necessary reactions to be carried out in the processed mixture, and, on the other hand, the necessary amount of carbon material is formed and used to form a bulk carbon skeleton.

The claimed technical solution for organizing the processing of heavy hydrocarbon compounds to obtain bulk carbon frames (p. 11) in the form of a carbon web, implemented without the use of a solid fusible catalyst-blowing agent, is as follows.

Product positioning according to the claimed technical solution: Finished products. Non-woven carbon fabric. In this example, we have implemented an example of obtaining a sample of decorative wall coverings for indoor or outdoor premises with a size of 200 * 200 mm, 0.5 mm thick. Color - black coal. The main advantages over existing on the market are incombustibility, a high degree of fire resistance.

Preparation of the raw mix (for 1 sample of non-woven carbon blanket with a size of 200 * 200 * 0.5 mm). To prepare the raw material mixture, dehydrated heavy hydrocarbon compounds of a fraction of 350-500 ° C, density 889 kg / m ³ in an amount of 16.0 g, and a cocatalyst hydrocarbon fraction with a boiling point below 200 ° C in an amount of 1.42 g were used. Raw mixture (total) = 16.0 g + 1.42 g = 17.42 g.

Preparation of the catalytic mixture. By sequential mixing of the components and bringing the mixture to a melt state at t = 200 ° C, a catalytic mixture (Fig. 1, p. 8) of 1634.71 g was prepared. 94.05 g of Ziegler-Natta catalyst (Al ( C ₂ H ₅ ) ₂ Cl + TiCl ₄ ) (Fig. 1, p. 9), as well as metal chlorides: AlCl ₃ - 1076.04 g; FeCl ₃ - 352.8 g; TiCl ₄ - 54.5 g; VCl ₄ - 57.33 g. The prepared catalyst mixture with a temperature of 200 ° C was placed in a reaction bath (Fig. 4, p. 2) and then the mixture was heated to 200 ° C. This temperature was systemically maintained by a thermostat.

The formation of a non-woven carbon web profile. The prepared raw material mixture in the amount of 17.4 g was heated to 70 ° C, then poured into the formwork, mounted and fixed on the melt surface of the reaction bath (Fig. 4, p. 2). The formwork made of fluoroplast-4 follows the contours of the resulting sample of a non-woven carbon strip 200 * 200 mm. The side walls of the formwork form prevent the spread of the feed mixture over the surface of the melt of the catalyst mixture in the reaction bath. The shape of the lattice bottom of the shuttering form ensures the transfer of the condensed solid of the obtained sample to the pressure rollers (Fig. 4, p. 5). After pouring the raw material mixture, the filled form was aged 3-5 minutes (until the end of active gas evolution).

The reaction block. After the cessation of active gas evolution, the formwork was engaged with the pressure rollers and provided direction, as well as the transfer of the obtained condensed solid to the pressure rollers. When applying to the pinch rollers, a geometric profile of the resulting solid was formed in thickness. At the same time, due to compression by the pressure rollers, the obtained sample was stretched in length, the oil fraction was pressed, the condensed solid was homogenized and densified, and its predetermined thickness was adjusted (0.5 mm). Then, with the pressure rollers, the condensed solid was completely immersed in the melt body of the catalytic mixture. Then, together with the formwork, the sample was removed from the reaction bath and transported to the carbonization zone (Fig. 4, p. 10), where it was cleaned. The time of the technological operation (exposure time) - 5 minutes

Cleaning up. The cleaning mode was ensured by a sequential increase in temperature to 650 ° C at a rate of 200 ° C for 1 hour in argon. Such a regime, on the one hand, ensured an increase in the properties of refractoriness, and, on the other hand, ensured the sublimation of the remains of the catalytic mixture and the released compounds. The presence of active chlorine in the remains of the catalytic mixture contributed to the development of these processes. Upon completion of the cleaning process, the carbon sample (Fig. 1, p. 14) was moved to the carbonization zone (Fig. 4, p. 11), which was carried out at a temperature of 1000 ° C. Upon completion of carbonization, the sample had a weight of 10.81 g, density 1.32 g / cm ³ , porosity 40%.

Qualitative characteristics of non-woven carbon web. After the operation of cleaning and heat treatment at a temperature of more than or equal to 650 ° C, the nonwoven carbon strip sample had a certain strength, providing at least self-supporting properties. The necessary strength characteristics for structural materials can be obtained during subsequent carbonization, graphitization, as well as other operations (for example, carbidization). The main objective of the invention is the implementation of spatial carbon construction in one stage, bypassing the stage of production of coal (carbon fiber). Therefore, the main condition is to obtain the frame itself as a product. Defects in the form of gaps on the surface and in the solid body of the non-woven carbon strip sample provide a mismatch between the declared consumer properties and the appearance of the decorative product. Thus, for this invention is significant characteristic - the level of defectiveness (D _f ). This characteristic is calculated as the ratio of the total area of the product to the area of open defects (%).

The ideal option is D _f → 0. The most optimal mode in actual conditions D _f → min. Optimization options for this indicator by modeling the main characteristics of the mode are shown in examples 1-4.

Example 1

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 450 ° C. The proportion of the sublimated part of the feed mixture (gas phase) is 80%. The fraction of the condensed carbon-containing part is 20%. D _f is equal to 42%. The condensed solid is represented by individual pieces, does not have a given geometric dimensions.

Example 2

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 320 ° C. The fraction of the sublimated part of the feed mixture (gas phase) is 69%. The fraction of the condensed carbon-containing part is 31%. D _f is equal to 26%. The resulting sample did not have clear geometric dimensions. On the surface, significant defects were observed in the form of holes with uneven edges.

Example 3

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. The proportion of the sublimated part of the feed mixture (gas phase) is 54%. The fraction of the condensed carbon-containing part is 46%. D _f is equal to 14%. Individual defects on the surface of a nonwoven carbon strip sample in the form of uneven holes.

Example 4

The feedstock is heavy hydrocarbon compounds of a fraction of 350-500 ° C, with a density of 889 kg / m ³ . The melt temperature of the catalyst mixture in the reaction bath is 200 ° C. We introduce 10% of the Ziegler-Natta catalyst ((C ₂ H ₅ ) ₂ AlCl + TiCl ₄ ). The proportion of the sublimated part of the feed mixture (gas phase) is reduced and amounts to 27%. The fraction of the condensed carbon-containing part is 73%. D _f is 5%. Slight defects on the surface of the non-woven carbon web sample.

Comparative table of the degree of defectiveness of the characteristics and process conditions

Conclusion: The most optimal temperature for processing the raw mixture in the reaction bath is the temperature of sample 4. This temperature regime allows, on the one hand, to carry out the necessary reactions in the processed mixture, on the other hand, to obtain and use the necessary amount of carbon material to form a bulk carbon frame in the form carbon nonwoven sample.

The advantage of the proposed variants of the method of organizing the processing of heavy hydrocarbon compounds to obtain a volumetric carbon frame is:

- in combining in one process the operational stages of obtaining structural material and its shaping, which eliminates the stage of producing carbon fiber, and will also provide a significant reduction in cost due to the rejection of a number of auxiliary energy-intensive operations;

- the possibility of changing the type of spatial structure due to the use or non-use of elements of a fusible solid-state catalyst-blowing agent of various shapes, which significantly expands the range of use of the obtained carbon frames in the production of both non-load-bearing structures (for example, decorative finishing coatings) and load-bearing structures: furniture plates , building panel board, structural and molded products;

- in the use of the cleaning, destructive and polycondensation effects of the molten catalyst mixture on heavy hydrocarbon compounds, which significantly expands the range of raw materials used;

- in the aggregate of the positive effects represented by the claimed invention, provided that in comparable units of measure, the added value productivity indicator of the obtained spatial carbon frames is higher than the same indicator of light fuel production, which allows a larger scale to consider an alternative paradigm of oil use. If at present the paradigm of oil use sounds like: “oil into light fuels”, then an alternative paradigm may sound like: “light oil fractions into light fuels, heavy fractions into composite materials and structures”.

Claims (16)

1. The method of organizing the processing of heavy hydrocarbon compounds to obtain a volumetric carbon skeleton, including:
a) the use of heavy hydrocarbon compounds;
b) subsequent processing of the resulting product,
characterized in that
additionally carry out the following steps:
c) prepare the formwork, the cross-section of which is carried out determining the profile of the carbon frame;
d) form inside the formwork form of separate elements having either the correct or irregular geometric shape, an array of solid-state fusible catalyst-blowing agent, stacking the individual elements so that the intercostal gap forms inextricable intercostal formwork channels along the edges and tops of the laid bodies;
d) prepare the raw material mixture by introducing into heavy hydrocarbon compounds a cocatalyst consisting of a mixture of light hydrocarbons;
e) fill the intercostal formwork channels in the solid body of the solid-state fusible catalyst-blowing agent with the raw material mixture inside the formwork form;
g) the formwork form, together with the solid-state fusible catalyst-pore former massif and the intercostal formwork channels filled with the raw material mixture in the body of the solid-state fusible catalyst-pore former massif, is placed completely in the melt of the catalytic mixture at a temperature of 200-300 ° C;
h) either a mixture of metal chlorides having a melting point of 180-200 ° C and a boiling point of 600-620 ° C, or a mixture of metal chlorides with the addition of a process intensifier is used as a catalytic mixture;
i) kept in the melt of the catalytic mixture until the mass of the solid-state fusible catalyst-blowing agent is molten and a bulk carbon frame is formed;
j) the formwork is removed along with the resulting bulk carbon skeleton;
k) carry out the purification of the obtained bulk carbon frame from the remnants of the liquid melt of the catalytic mixture. 2. The method according to claim 1, characterized in that as the heavy hydrocarbon compounds use either isolated native high molecular weight oil compounds, or pecks, or heat treatment products of lignin or polyvinyl chloride, or still bottoms from the distillation of benzyl chloride or chlorobenzene, either natural or artificial asphalts, or bitumen, or products of chemical refining of crude oil and oil products, or products of extraction of coal with aromatic hydrocarbons, or waste from the oil and coal industries. 3. The method according to claim 1, characterized in that as the intensifier use complex compounds, which are alkyl derivatives of metals of groups I-III of the Periodic system with transition metal halides. 4. The method according to claim 1, characterized in that as light hydrocarbons use a hydrocarbon fraction with a boiling point below 200 ° C. 5. The method according to claim 1, characterized in that a hollow mesh structure is used as the formwork. 6. The method according to claim 1, characterized in that the individual elements having the correct or irregular geometric shape of the solid-state solid fusible catalyst-blowing agent array are made of molten catalyst mixture. 7. The method according to any one of claims 1 or 6, characterized in that either a prism or a tetrahedron, or a cylinder, or a cone, or a sphere, or a regular polyhedron, or a polyhedron, or a parallelepiped, or a pyramid is used as the correct geometric shape. 8. The method according to any one of claims 1 or 6, characterized in that crushed chips are used as an irregular geometric shape. 9. The method according to claim 1, characterized in that on the edges of the individual elements of the correct geometric shape of the solid-state fusible catalyst-blowing agent array, a chamfer is made in either a rectilinear or curvilinear shape. 10. The method according to claim 1, characterized in that the purification of the obtained product is carried out at a temperature equal to or higher than 650 ° C. 11. A method of organizing the processing of heavy hydrocarbon compounds to obtain a volumetric carbon skeleton, including:
a) the use of heavy hydrocarbon compounds;
b) subsequent processing of the resulting product,
characterized in that
additionally carry out the following steps:
c) prepare the formwork, the cross-section of which is carried out determining the profile of the carbon frame;
d) preparing a raw mix by introducing into a heavy hydrocarbon compound a cocatalyst consisting of a mixture of light hydrocarbons;
d) fill the formwork with the raw material mixture and place it on the surface, and then completely into the liquid melt of the catalytic mixture at a temperature of 200-300 ° C;
f) either a mixture of metal chlorides having a melting point of 180-200 ° C and a boiling point of 600-620 ° C or a mixture of metal chlorides with the addition of a process intensifier is used as a catalytic mixture;
g) maintain the formwork in the melt of the catalytic mixture until the formation of a volumetric carbon skeleton in the form of a non-woven carbon web;
h) remove the formwork together with the obtained carbon frame;
i) carry out the purification of the obtained carbon frame from the remnants of the molten liquid of the catalytic mixture. 12. The method according to claim 11, characterized in that as the heavy hydrocarbon compounds use either isolated native high molecular weight oil compounds, or pecks, or heat treatment products of lignin, or polyvinyl chloride, or still bottoms during the distillation of benzyl chloride, or chlorobenzene, or natural and artificial asphalts, or bitumens, or products of chemical refining of crude oil and oil products, or products of extraction of coal with aromatic hydrocarbons, or waste from the oil and coal industries . 13. The method according to claim 11, characterized in that as the intensifier use complex compounds, which are alkyl derivatives of metals of groups I-III of the Periodic system with transition metal halides. 14. The method according to claim 11, characterized in that the hydrocarbon fraction with a boiling point below 200 ° C is used as light hydrocarbons. 15. The method according to claim 11, characterized in that a hollow mesh structure is used as the formwork. 16. The method according to claim 11, characterized in that the purification of the obtained product is carried out at a temperature above 650 ° C.

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