JP2009120464A - Method for producing carbon material - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a carbon material capable of economically obtaining in a high yield a high-purity carbon material having ≤60% in porosity and having a significantly low ash concentration using an ashless coal as a material, and to provide a method for producing a carbon material capable of economically obtaining in a high yield a high-purity carbon material having a densely and significantly low ash concentration and capable of obtaining the carbon material while keeping a predetermined shape. <P>SOLUTION: The method for producing a carbon material comprises an ashless coal producing step (S1) for producing an ashless coal, a carbonizing raw material producing step (S2) comprising mixing an ashless coal with an organic solvent to extract a component soluble in the organic solvent from the ashless coal and then separating the resulting material into a liquid part containing a soluble component and a non-liquid part containing a component insoluble in an organic solvent to make the non-liquid part as a carbonizing raw material, a molding step (S3) for molding the carbonizing raw material into agglomerates, and a carbonization step (S4) for carbonizing the carbonizing raw material by heat-treating in an inert atmosphere, in which the ratio of the produced carbonizing raw material is defined to a predetermined ratio. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a carbon material production method for producing a carbon-based material with a very low ash content using coal as a raw material.

  Carbon products are excellent in heat resistance, chemical stability, mechanical strength, etc., and also have electrical conductivity, so structural materials, reducing agents for metallurgical industry including coke for iron making, conductive materials Or widely used as industrial machine parts materials. The carbon material for producing this carbon product is produced by forming an organic raw material (carbon material raw material) into a lump shape, and heat-treating this formed body at a high temperature to carbonize it. Here, although the characteristics required for the carbon material raw material for producing the carbon material are slightly different depending on the application, generally, it can be formed into a lump and formed into a molded body (however, it is carbonized as a powder) And when it is not used as powdered carbon), the carbon yield is high, and the properties of the resulting carbon material are excellent.

  Here, as a method for producing the carbon material, it is conceivable to use coal as a raw material. However, among coals, non-caking coals are brittle and difficult to form, and even if formed, they will be pulverized when heat-treated. Conversely, caking coal is easy to mold, but expands, melts or deforms during the heat treatment. Therefore, unless the coal is processed by any method, it cannot be used as a carbon material raw material.

  Therefore, coke powder (coal coke or petroleum coke) as an aggregate and tar or pitch as a molding binder are used as a carbon material raw material. Coke is produced by dry distillation of petroleum, characterized by having a low volatile content of 1% by mass, carbonizing without melting, and a high fixed carbon (carbon yield) of about 90% by mass. Tar and pitch are auxiliary materials in the carbonization process, and fixed carbon is not as high as coke, but has a property of melting when heated, and plays a role of connecting coke particles (role of binder).

  However, if the raw material is coke alone, it cannot be formed into a lump, but if it is only tar or pitch, it can be formed but melts and loses its shape when heated for carbonization. For this reason, it is typical for carbon materials to be formed by kneading coke and binder (pitch and / or tar) and then heat-treating them at a high temperature of 1000 ° C. or higher in an inert gas atmosphere to carbonize and graphitize them. It is a manufacturing process.

  Here, for example, coal coke is an unused component when producing iron-making coke, petroleum coke is a by-product of the oil refining process, and tar and pitch are also used in coal and oil refining industry. Is a by-product of As described above, since any of these raw materials is an unused component or a by-product of another manufacturing process, it contains ash in the component (for example, coke contains about 10% by mass of ash). It is inevitable that the carbon material produced using ash also contains ash. However, since this ash content deteriorates the characteristics of the carbon material, it is not preferable to be contained in the component. In addition, since carbonization is a process of heat treatment at a high temperature of 1000 ° C. or higher, a large amount of energy is required, and in the carbon production process, heat treatment at 1000 ° C. or higher is performed again. And is inefficient.

  As other carbon material raw materials, solvent-extracted coal and coal liquefaction products are known. However, the former has a problem of containing ash equivalent to coal, and the latter has a problem of low carbon yield, and the production process itself has not been put into practical use.

  As described above, it is preferable that the ash content in the carbon material is low. However, as long as the raw material is a natural product such as coal or petroleum, it is unavoidable to contain a certain amount of ash. % To more than 10% by mass of ash). Therefore, when an extremely high-purity carbon material is required, heat treatment is performed on the carbon material with a halogen gas such as chlorine to convert ash to volatile metal halides and remove the ash. However, this process is expensive and uneconomical.

Here, as a new coal reforming method, a technique for extracting coal using a non-hydrogen-donating solvent is disclosed (for example, see Patent Documents 1 and 2). This reforming method uses a non-hydrogen-donating aromatic compound as a solvent, and is treated at a relatively mild condition of, for example, 400 ° C. and 1 MPa, so that it is treated as compared with conventional solvent-extracted charcoal and liquefied products. Costs and equipment costs are much smaller. And the characteristic of the modified coal (ashless coal, ie, hyper coal) obtained in this way is that the ash concentration is as low as 0.3% by mass or less and a relatively low temperature of about 200 to 300 ° C. It is to melt at. Therefore, application development as a binder for coke production has been advanced taking advantage of this characteristic, and in recent years, attempts have been made to produce a carbon material by using this ashless coal as a carbon material raw material. .
JP 2006-70183 A JP 2007-161926 A

So-called ashless coal, which is produced by solvent extraction of coal and removing ash and non-soluble coal components, is a bituminous material derived from coal, but does not substantially contain ash. It is considered suitable as a carbon material raw material. However, since this ashless coal foams violently in the carbonization process in which the carbon material raw material is heat treated, the porosity (porosity content) is 80% or more, and it is not suitable as an iron-making coke. There is a problem that only a carbon material can be obtained, and a problem that the carbon yield is not necessarily as high as about 60% by mass or less.
Further, in recent years, when obtaining a carbon material as a massive molded body, development of a technique that can obtain a carbonized material while maintaining a predetermined shape without the molded body expanding due to a heat treatment for carbonization. The demand for is also growing. Furthermore, there is a demand for obtaining carbon materials more economically.

The present invention has been made in view of the above problems, and its purpose is to produce a high-purity carbon material having a porosity of 60% or less and an extremely low ash concentration using ashless coal as a raw material. It is to provide a method for producing a carbon material that can be obtained economically at a high rate.
In addition, a carbon material capable of obtaining a dense and highly pure carbon material having a very low ash concentration in a high yield and economically, and capable of obtaining a carbon material in a state in which a predetermined shape is maintained. It is in providing the manufacturing method of.

  As a result of various studies by the present inventors, problems when using ashless coal as a carbon material raw material, that is, foaming vigorously in the carbonization process, low porosity, it is difficult to obtain a dense and strong carbon material, and It has been found that the reason why the carbon yield is not necessarily as high as about 60% by mass or less is due to a relatively light component (hereinafter referred to as a light component as appropriate) contained in ashless coal. Such a light component volatilizes or decomposes in the initial stage of the carbonization treatment, so that it easily causes foaming and dissipates out of the system in the carbonization step, resulting in a decrease in carbon yield. Therefore, in order to effectively remove such light components, the present inventors mixed ashless coal and an organic solvent to extract a component soluble in the organic solvent (light component), The present inventors have found that the above problems can be solved and have reached the present invention. Furthermore, it has been found that the removal of the light components can increase the softening temperature of the carbon material raw material, and the carbon material can be obtained in a state in which the predetermined shape is maintained, and the present invention has been reached.

  That is, the 1st form of the manufacturing method of the carbon material which concerns on this invention includes an ashless coal manufacturing process, a carbonization raw material manufacturing process, and a carbonization process, and is manufactured at the said carbonization raw material manufacturing process. The ratio of a carbonized raw material is 40-90 mass% with respect to the ashless coal mixed at the said carbonized raw material manufacturing process, It is characterized by the above-mentioned.

According to such a manufacturing method, ashless coal which is reformed coal is manufactured by modifying coal in the ashless coal manufacturing process. In the carbonization raw material production process, first, the ashless coal produced in the ashless coal production process and the organic solvent are mixed to form a mixture, and the soluble component soluble in the organic solvent from the ashless coal Is extracted. Next, the mixture after extraction is separated into a liquid part containing the soluble component and a non-liquid part containing a component insoluble in the organic solvent, and the non-liquid part becomes a carbonization raw material. And in the carbonization process, the carbonization raw material manufactured at the said carbonization raw material manufacturing process is heat-processed by inert atmosphere, and is carbonized. Further, by defining the ratio of the carbonized raw material produced in the carbonized raw material production process within a predetermined range, foaming in the heat treatment in the carbonization process is suppressed, the porosity is approximately 60% or less, and the apparent specific gravity is A carbon material of approximately 0.6 g / cm ³ or more can be obtained, and the carbon yield and economy can be improved, and the moldability does not deteriorate.

Moreover, in the 1st form of the manufacturing method of the carbon material which concerns on this invention, after the said carbonization raw material manufacturing process, the shaping | molding process which shape | molds the carbonization raw material manufactured at the said carbonization raw material manufacturing process in the lump form, In the carbonization step, the molded body molded in the molding step may be carbonized by heat treatment in an inert atmosphere.
According to such a manufacturing method, it can obtain as a molded object which shape | molded the carbonization raw material in the lump shape.

  The 2nd form of the manufacturing method of the carbon material which concerns on this invention includes an ashless-coal manufacturing process, a carbonization raw material manufacturing process, a formation process, and a carbonization process, and is manufactured by the said carbonization raw material manufacturing process. The ratio of the carbonized raw material to be produced is 40 to 90% by mass with respect to the ashless coal mixed in the carbonized raw material production process, and the softening temperature of the carbonized raw material is 350 ° C. or higher, and the molding process is performed. The ratio of the carbonized raw material in the formed body is 80% by mass or more.

According to such a manufacturing method, ashless coal which is reformed coal is manufactured by modifying coal in the ashless coal manufacturing process. In the carbonization raw material production process, first, the ashless coal produced in the ashless coal production process and the organic solvent are mixed to form a mixture, and the soluble component soluble in the organic solvent from the ashless coal Is extracted. Next, the mixture after extraction is separated into a liquid part containing the soluble component and a non-liquid part containing a component insoluble in the organic solvent, and the non-liquid part becomes a carbonization raw material. Furthermore, in the forming step, the carbonized raw material manufactured in the carbonized raw material manufacturing step is formed into a lump as the main component of the forming raw material. In the carbonization step, the molded body molded in the molding step is heat-treated in an inert atmosphere and carbonized. In addition, by prescribing the ratio and softening temperature of the carbonized raw material produced in the carbonized raw material production process to a predetermined level, the effect of suppressing foaming in the heat treatment in the carbonization process and the effect of improving the carbon yield are further improved. It can be made high, and the moldability does not deteriorate. Furthermore, by defining the ratio of the carbonized raw material in the molded body within a predetermined range, molding becomes easy, and the molded body does not expand or pores are not generated by the heat treatment in the carbonization process. Thereby, a carbon material having a porosity of about 30% or less and an apparent specific gravity of about 1.0 g / cm ³ or more can be obtained.

In the method for producing a carbon material according to the present invention, it is preferable to use an oxygen-containing organic solvent as the organic solvent.
According to such a manufacturing method, polar components are efficiently removed among light components contained in ashless coal.

  According to the method for producing a carbon material according to the present invention, it is possible to economically produce a carbon material having a low porosity in a high yield by removing a relatively light component contained in ashless coal. it can. Moreover, since ashless coal obtained by reforming coal is used as a raw material, the produced carbon material has a high purity with a very low ash concentration.

  According to the method for producing another carbon material according to the present invention, a relatively light component contained in ashless coal is removed to produce a relatively dense carbon material economically with a high yield. be able to. Moreover, since ashless coal obtained by reforming coal is used as a raw material, the produced carbon material has a high purity with a very low ash concentration. Furthermore, the carbon material made into a molded body can be obtained in a state where a predetermined shape is maintained.

  In addition, the carbon material obtained by the method for producing a carbon material according to the present invention has a porosity of 60% or less, unlike a porous and brittle carbon material obtained by carbonizing a conventional ashless coal as it is. Therefore, it is also suitable as coke for metallurgy such as iron making. Furthermore, in the present invention, since the coal is processed by two-stage solvent fractionation, a carbon material corresponding to iron-making coke can be produced using inferior coal such as lignite as a raw material. Inferior coals such as lignite and sub-bituminous coal have low thermal fluidity and cannot be hardened even if carbonized as they are.

  Next, a method for producing a carbon material according to the present invention will be described in detail with reference to the drawings. In the drawings to be referred to, FIG. 1 is a flowchart for explaining the steps of the carbon material manufacturing method according to the first embodiment of the present invention, and FIG. 2 is the carbon material manufacturing method according to the second embodiment of the present invention. It is a flowchart explaining the process of.

[First Embodiment]
First, 1st Embodiment about the manufacturing method of the carbon material which concerns on this invention is described.
As shown in FIG. 1, the manufacturing method of a carbon material includes an ashless coal manufacturing process (S1), a carbonized raw material manufacturing process (S2), and a carbonization process (S4). Moreover, you may include a shaping | molding process (S3) after a carbonization raw material manufacturing process (S2) as needed.
Hereinafter, each step will be described.

<Ashless coal manufacturing process (S1)>
The ashless coal production step (S1) is a step of reforming coal to produce ashless coal that is a modified coal.
In addition, the ashless coal as used in the field of this invention is what is called hyper coal, and is manufactured by solvent-extracting coal and removing ash and an insoluble coal component. This ashless coal has very little ash (ash content of 0.3% by mass or less), and water content is generally 0.5% by mass or less.

  A publicly known method can be used as a method for obtaining ashless coal, and the solvent species and production conditions are appropriately selected in view of the properties of coal and the design of the carbon material raw material. However, in order to obtain ashless coal more efficiently and inexpensively, for example, it is preferable to produce ashless coal by the following method. In the method, first, a mixture (slurry) in which coal and a non-hydrogen donating solvent are mixed is heated to extract coal components that are soluble in the non-hydrogen donating solvent. Next, the slurry after extraction is separated into a liquid part and a non-liquid part, and the non-hydrogen donating solvent is separated from the liquid part to produce ashless coal.

  The coal used as the raw material for ashless coal (hereinafter also referred to as raw material coal) is preferably inferior quality coal. By using inexpensive inferior coal, ashless coal can be produced at a lower cost, so that the economy can be further improved. However, the coal used is not limited to inferior coal, and caking coal may be used as necessary.

In addition, inferior coal here means coal, such as a non-slightly caking coal, a general coal, a low grade coal (brown coal, subbituminous coal, etc.). Examples of the low-grade coal include lignite, lignite, and sub-bituminous coal. Further, for example, lignite coal includes Victoria coal, North Dakota coal, Berga coal, and sub-bituminous coal includes West Banco coal, Vinungan coal, Samarangau coal, and the like. The low-grade coal is not limited to those exemplified above, and any coal containing a large amount of water and desired to be dehydrated is included in the low-grade coal referred to in the present invention.
The coal is preferably pulverized into as small particles as possible, and preferably has a particle size of 1 mm or less.

  The non-hydrogen donating solvent is a coal derivative which is a solvent mainly composed of a bicyclic aromatic and purified mainly from a coal carbonization product. This non-hydrogen-donating solvent is stable even in a heated state and has excellent affinity with coal. Therefore, the proportion of soluble components (herein, coal components) extracted into the solvent (hereinafter also referred to as extraction rate) In addition, it is a solvent that can be easily recovered by a method such as distillation. The main components of the non-hydrogen donating solvent include bicyclic aromatic naphthalene, methyl naphthalene, dimethyl naphthalene, trimethyl naphthalene and the like, and the other components of the non-hydrogen donating solvent have an aliphatic side chain. Naphthalenes, anthracenes, fluorenes, and also include biphenyl and alkylbenzenes with long-chain aliphatic side chains.

  The extraction rate of coal can be increased by heat extraction using a non-hydrogen-donating solvent. In addition, unlike polar solvents, the solvent can be easily recovered, so that it is easy to circulate the solvent. Furthermore, since it is not necessary to use expensive hydrogen, a catalyst, or the like, coal can be solubilized at low cost to obtain ashless coal, and economic efficiency can be improved.

  Although the coal density | concentration with respect to a solvent is based also on the kind of raw material coal, the range of 10-50 mass% is preferable on a dry coal basis, and the range of 20-35 mass% is more preferable. When the coal concentration with respect to the solvent is less than 10% by mass, the proportion of the coal component extracted into the solvent decreases with respect to the amount of the solvent, which is not economical. On the other hand, the higher the coal concentration, the better. However, when it exceeds 50% by mass, the viscosity of the prepared slurry becomes high, and it becomes difficult to move the slurry and separate the liquid part and the non-liquid part described later.

  The heating temperature of the slurry is preferably in the range of 300 to 450 ° C. By setting the heating temperature within this range, the bonds between the molecules constituting the coal are loosened, mild thermal decomposition occurs, and the extraction rate becomes the highest. When the heating temperature is less than 300 ° C., it tends to be insufficient to weaken the bonds between the molecules constituting the coal, and the extraction rate is difficult to improve. On the other hand, when the temperature exceeds 450 ° C., the pyrolysis reaction of coal becomes very active and recombination of the generated pyrolysis radicals occurs, so that the extraction rate is hardly improved and the alteration of coal is difficult to occur. In addition, Preferably, it is 300-400 degreeC.

  The heating time (extraction time) is a criterion for reaching the dissolution equilibrium, but it is economically disadvantageous to realize it. Therefore, since it varies depending on conditions such as the particle diameter of coal and the type of solvent, it cannot be generally stated, but it is usually about 10 to 60 minutes. If the heating time is less than 10 minutes, the extraction of the coal component tends to be insufficient, while if it exceeds 60 minutes, the extraction does not proceed any further, which is not economical.

The extraction of the coal component soluble in the non-hydrogen donating solvent is preferably performed in the presence of an inert gas. This is because contact with oxygen is dangerous because it may ignite, and when hydrogen is used, the cost increases.
As the inert gas to be used, inexpensive nitrogen is preferably used, but is not particularly limited. The pressure is preferably 1.0 to 2.0 MPa, although it depends on the temperature at the time of extraction and the vapor pressure of the solvent used. When the pressure is lower than the vapor pressure of the solvent, the solvent is volatilized and is not trapped in the liquid phase and cannot be extracted. In order to confine the solvent in the liquid phase, a pressure higher than the vapor pressure of the solvent is required. On the other hand, if the pressure is too high, the cost of the equipment and the operating cost increase, which is not economical.

Thus, the slurry after extracting a coal component is isolate | separated into a liquid part and a non-liquid part.
Here, the liquid part means a solution containing a coal component extracted into a solvent, and the non-liquid part means a solute containing a coal component insoluble in the solvent (coal containing ash, that is, ash coal).

  As a method for separating the slurry into a liquid part and a non-liquid part, various filtration methods and centrifugal separation methods are generally known. However, the filtration method requires frequent replacement of the filter, and the centrifugation method tends to cause clogging with undissolved coal components, making it difficult to implement these methods industrially. Therefore, it is preferable to use a gravity sedimentation method that allows continuous operation of fluid and is suitable for a large amount of processing at low cost. Thereby, from the upper part of the gravity sedimentation tank, a liquid part (hereinafter also referred to as a supernatant liquid) containing a coal component extracted into the solvent is contained, and from the lower part of the gravity sedimentation tank, a coal component insoluble in the solvent is contained. A non-liquid part (hereinafter also referred to as a solid content concentrate) which is a solute can be obtained.

And ashless coal is obtained by isolate | separating a non-hydrogen donating solvent from this liquid part.
As a method for separating the solvent from the supernatant liquid (liquid part), a general distillation method or evaporation method (spray drying method, etc.) can be used. From the supernatant liquid, ashless coal substantially free of ash Can be obtained. This ashless coal has an ash content of 0.3% by mass or less, almost no ash, moisture content of approximately 0.5% by mass or less, and a higher calorific value than raw coal. Therefore, by carbonizing this ashless coal, a high-purity carbon material having an extremely low ash concentration can be obtained.

<Carbonization raw material manufacturing process (S2)>
In the carbonization raw material production step (S2), the ashless coal produced in the ashless coal production step (S1) and an organic solvent are mixed to form a mixture, which is soluble in the organic solvent from the ashless coal. A soluble component is extracted, and the mixture after extraction is separated into a liquid part containing the soluble component and a non-liquid part containing a component insoluble in the organic solvent, and the non-liquid part is used as a carbonization raw material. It is a process.

  The purpose of this carbonized raw material manufacturing step (S2) is to remove only light components soluble in organic solvents contained in ashless coal and obtain only carbonized raw materials that are insoluble in organic solvents. . As described above, this light component prevents the carbon material from being densified, and also causes the carbon yield to decrease. Therefore, the light component contained in ashless coal is removed by this carbonization raw material manufacturing process (S2).

  The point of setting the conditions in the carbonized raw material production step (S2) is how much light components (solvent soluble components) are removed. Since this ratio varies depending on the characteristics of the raw ashless coal and the requirements required for the carbon material and its manufacturing process, it cannot be determined uniquely. However, assuming a typical ashless coal, carbon material, and production process, the light component removal rate (hereinafter also referred to as the removal rate) is 10 to 60% by mass, that is, the carbonized raw material to be produced (insoluble) The ratio of the component (hereinafter also referred to as the acquisition rate) is 40 to 90% by mass ((mass of carbonization raw material) with respect to the ashless coal supplied to the process (the ashless coal mixed in the process). / Massed ashless coal mass = 40-90 mass%)). The removal rate is preferably 20 to 40% by mass (acquisition rate: 60 to 80% by mass).

When the acquisition rate exceeds 90% by mass, the effect of suppressing foaming and the effect of improving the carbon yield become insufficient. In addition, the porosity is large (generally over 60%) and the apparent specific gravity is low (generally less than 0.6 g / cm ³ ). On the other hand, if the acquisition rate is less than 40% by mass, the yield of the active ingredient (carbonized raw material) decreases and the product becomes high, which causes the problem that in addition to being uneconomical, the moldability decreases. . However, if the decrease in yield is acceptable, the decrease in moldability can be avoided by adding an appropriate amount of an appropriate binder.

  In addition, adjustment of an acquisition rate can be performed by adjusting suitably the kind of solvent, the ratio of a solvent and ashless coal, temperature, pressure, processing time, etc. As a general guideline, light components dissolve at a higher rate depending on conditions such as high boiling point aromatic solvent, ashless coal, large amount of solvent, high temperature, long time treatment, etc. Small value. However, the effect varies depending on the nature of the raw coal and the production conditions of ashless coal, and cannot be pointed out in general.

In the carbonized raw material production step (S2), first, ashless coal and an organic solvent are mixed to form a mixture (slurry), and soluble components soluble in the organic solvent are extracted from the ashless coal.
Here, the extraction rate of coals is greatly influenced by the type of solvent, that is, the dissolving power of the solvent. Therefore, when the solvent is selected, it is generally determined how much light components can be removed.

  The organic solvent used in the carbonized raw material production step (S2) may be selected from those often used for coal extraction, such as benzene, N-methyl-2-pyrrolidinone, pyridine, quinoline, anthracene oil, creosote oil, tetrahydrofuran, Acetone, methyl ethyl ketone, dioxane, methanol, phenol (hydrous), cresol, methylnaphthalene (may be an isomer mixture), dimethylnaphthalene (may be an isomer mixture) and the like are preferable. In addition, you may mix and use 2 or more types among these.

  Among the above organic solvents, it is particularly preferable to use an oxygen-containing organic solvent such as tetrahydrofuran, acetone, methyl ethyl ketone, dioxane, methanol, phenol (containing water), cresol and the like. When these oxygen-containing organic solvents are used, it is considered that polar components can be efficiently removed even among light components in ashless coal. Since the polar component is generally composed of a hetero element such as an oxygen-containing functional group, it is considered that the polar component decomposes at a relatively low temperature to cause foaming and may cause a low carbon yield.

  As described above, when the solvent is selected, it is generally determined how much light component can be removed, but the extraction rate (removal rate) (here, the proportion of the light component extracted into the solvent). Can be greatly changed by changing the extraction temperature. That is, the extraction rate can be changed by utilizing the phenomenon that the dissolving power decreases as the temperature decreases, and the dissolving power increases as the temperature increases.

The extraction rate can also be changed by changing the mixing ratio of the solvent and ashless coal or the extraction time. For example, the amount of dissolution can be reduced by using a relatively small amount of a solvent having a high dissolving power with respect to ashless coal, or the amount of dissolution can be reduced by shortening the extraction time. However, such a method is less preferred because it reduces the selectivity of extraction.
In other words, mass transfer rather than dissolving relatively easily dissolved components (generally components with relatively low molecular weight (light) or having many side chains such as alkyl groups) among ashless coal components. This is because the extraction is limited by this limitation. That is, when the amount of the solvent is too small, the solubility reaches saturation while molecules on the particle surface in contact with the solvent preferentially dissolve (only the surface of the particle dissolves and reaches a dissolution equilibrium), so it is originally extracted. Such a light component remains in a relatively large amount. The same thing happens when the extraction time is too short.

  As an example of the extraction method, as the simplest method, there is a method in which ashless coal powder and an organic solvent are put in a container to form a slurry and stirred for a predetermined time. You may heat as needed. The atmosphere is preferably an inert atmosphere in order to avoid oxidation, combustion and explosion of ashless coal. In addition, as described in the ashless coal production step (S1), nitrogen is preferably used as the inert gas, but is not particularly limited. Further, the extraction may be performed at normal pressure, but when the temperature is higher than the boiling point of the solvent, the extraction is performed under pressure. The extraction method is not particularly limited as long as a component soluble in a solvent can be extracted and a light component can be removed.

  The extraction time is appropriately selected according to the extraction speed, but is usually about 5 to 120 minutes, more preferably 20 to 60 minutes. If the extraction time is less than 5 minutes, extraction of light components tends to be insufficient. On the other hand, if the extraction time exceeds 120 minutes, the extraction does not proceed any further, which is not economical.

  The ratio of ashless charcoal to organic solvent is preferably 3 to 20 (organic solvent / ashless charcoal (mass ratio)). If the ratio is less than 3, it tends to be difficult to form a slurry. On the other hand, if it exceeds 20, there is no inconvenience in characteristics, but a large amount of solvent is used, which is not economical.

Next, the mixture (slurry) after extracting the light components in this way is separated into a liquid part containing the soluble component and a non-liquid part containing a component insoluble in the organic solvent.
Here, a liquid part means the solution containing the light component extracted by the solvent, and a non-liquid part means the solute containing the component (carbonization raw material) insoluble in the solvent.

As a method for separating the mixture (slurry) into a liquid part and a non-liquid part, various filtration methods and centrifugal separation methods are generally known, but are not particularly limited.
Moreover, in order to remove the solvent remaining in the non-liquid part, a drying process for drying the obtained non-liquid part (carbonized raw material) may be further performed. Drying can be carried out by holding in a nitrogen atmosphere or under reduced pressure while heating if necessary.
By such a method, a carbonized raw material powder from which light components have been removed is obtained.

The carbonized raw material powder thus obtained may be carbonized as it is when producing a powdered carbon material, but if necessary, it is molded into a lump before being carbonized. It may be a body.
<Molding step (S3)>
The forming step (S3) is a step of forming the carbonized raw material powder produced in the carbonized raw material production step (S2) into a lump after the carbonized raw material production step (S2).
The carbonization raw material powder can be formed by a known method. For example, compression molding, two-roll tablet molding, or the like. A compact can be obtained relatively easily by pulverizing and high-pressure pressing. Moreover, you may use a suitable binder compound. As the binder, known materials such as tar, pitch, ashless coal itself, and resin can be used. Of these, ashless coal itself is most preferred because of its low ash content. The ratio of the binder compound in the molded body is preferably less than 20% by mass. Further, an appropriate filler such as carbon fiber, or a trait or by-product charcoal produced as a by-product in the ashless coal manufacturing step (S1) may be added and mixed.

<Carbonization process (S4)>
The carbonization step (S4) is a step of carbonizing the carbonized raw material manufactured in the carbonized raw material manufacturing step (S2) or the molded body molded in the molding step (S3) by heat treatment in an inert atmosphere. It is.
The method and conditions for the carbonization treatment are not particularly limited, and can be performed using a known technique. Typically, heat treatment is performed at 1000 ° C. or higher and, if necessary, 2000 ° C. or higher in an inert atmosphere such as nitrogen or argon. Moreover, a temperature increase rate shall be about 0.1-5 degreeC / min. This carbonization treatment may be performed under pressure using a hot isostatic pressing apparatus or the like.

[Second Embodiment]
Next, a second embodiment of the carbon material manufacturing method according to the present invention will be described.
In the carbonization step (S1), when the molded body is heat-treated, the molded body may expand and the shape of the carbonized raw material may be damaged. However, according to the second embodiment of the present invention, it is possible to obtain a high-purity carbon material that is dense and has an extremely low ash concentration, and that the molded body does not expand due to heat treatment. The carbon material can be obtained while maintaining a predetermined shape. In this case, the molded body is slightly shrunk by heat treatment and becomes dense.

As shown in FIG. 2, the carbon material manufacturing method includes an ashless coal manufacturing process (S11), a carbonized raw material manufacturing process (S12), a molding process (S13), and a carbonization process (S14). Is included.
Hereinafter, each step will be described.
Note that the ashless coal production step (S11) and the carbonization step (S14) are the same as those in the first embodiment (S1, S4), and thus the description thereof is omitted here.

<Carbonization raw material manufacturing process (S12)>
In the carbonization raw material production step (S12), the ashless coal produced in the ashless coal production step (S11) and an organic solvent are mixed to form a mixture, and the ashless coal is soluble in the organic solvent. A soluble component is extracted, and the mixture after extraction is separated into a liquid part containing the soluble component and a non-liquid part containing a component insoluble in the organic solvent, and the non-liquid part is used as a carbonization raw material. It is a process.

  As described below, the carbonization raw material is the same as the carbonization raw material manufacturing step (S2) of the first embodiment except that the softening temperature of the carbonization raw material is 350 ° C. or higher. The softening temperature of the chemical raw material will be described.

In the second embodiment, as described above, the obtained carbon material is molded into a lump shape, and the molded shape is maintained even if heat treatment is performed in the carbonization step (S14).
The ashless coal produced and recovered in the ashless coal production step (S11) is obtained by removing residual coal and ash from the coal, and is usually softened and melted at a temperature of 300 ° C or lower, sometimes 200 ° C or lower. With such a property of softening at a low temperature, the heat treatment by the carbonization step (S14) may cause softening and melting, and the shape of the molded body may be damaged.

Here, the elimination of the alkyl group and the dehydrogenation reaction, which are the initial reactions of the carbonization reaction, generally start around 400 ° C. Therefore, if the softening temperature is 350 ° C. or higher, preferably higher than 400 ° C., the molded body is carbonized without being softened and melted by heating at a rate controlled in the carbonization step (S14). Can do. Thereby, a molded object can be converted into carbon, maintaining the shape. A carbon material having a porosity of approximately 30% or less and an apparent specific gravity of approximately 1.0 g / cm ³ or more can be obtained.
Therefore, the carbonization raw material needs to have a softening temperature of 350 ° C. or higher. More preferably, it is 400 ° C. or higher, more preferably 450 ° C. or higher, or a property that does not soften. When the softening temperature is less than 350 ° C., the molded body is softened and melted, and a carbon material cannot be obtained in a state where a predetermined shape is maintained, the porosity is increased, and the apparent specific gravity is slightly decreased.

  In addition, adjustment of softening temperature is performed by changing the removal rate of a low molecular weight component in solvent fractionation. Furthermore, the removal ratio of the low molecular weight component can be performed by appropriately adjusting the type of solvent, the ratio of solvent to ashless coal, temperature, pressure, treatment time, etc. in solvent fractionation. As a general guideline, light components dissolve at a higher rate depending on conditions such as high boiling point aromatic solvent, ashless coal, large amount of solvent, high temperature, long time treatment, etc., so the softening temperature is A big rise. However, the effect varies depending on the nature of the raw coal and the production conditions of ashless coal, and cannot be pointed out in general.

In the present invention, the softening temperature is adjusted by removing soluble components with an organic solvent (solvent fractionation). The purpose of solvent fractionation here is to remove the low molecular weight components (light components) that are responsible for the low softening temperature. Examples of the solvent suitable for this purpose include the organic solvents described in the carbonization raw material manufacturing step (S2) of the first embodiment. By extracting with these organic solvents, components soluble in the solvent are removed.
In addition, as for solvent fractionation for adjusting softening temperature, as the carbonization raw material manufacturing process (S2) of the said 1st Embodiment demonstrated, the acquisition rate of a carbonization raw material should also satisfy | fill the range of 40-90 mass% simultaneously. Adjust to.

  Next, an example of a method for measuring the softening temperature will be described. First, the sample is pulverized so that the whole amount passes through a sieve having an opening of 1.19 mm. The crushed sample is put in a suitable container, and the temperature is increased at 20 ° C./min in an inert atmosphere. Go. Then, the state of the sample is observed with a microscope having a magnification of 100 times, and the temperature at which the sample particles begin to deform is defined as a softening temperature.

<Molding step (S13)>
In the molding step (S13), after the carbonized raw material manufacturing step (S12), the carbonized raw material manufactured in the carbonized raw material manufacturing step (S12) is used as a main component of the molding raw material, and the carbonized raw material is agglomerated. This is a molding step.

  As described below, the proportion of the carbonized raw material (here, the carbonized raw material manufactured in the carbonized raw material manufacturing step (S12) according to the present invention) in the molded body is 80% by mass or more. Since it is the same as that of the shaping | molding process (S3) of the said 1st Embodiment except making it, here, the ratio of a carbonization raw material is demonstrated.

  In the molding step (S13), as described in the first embodiment, the obtained carbonized raw material itself may be molded, or an appropriate binder compound may be mixed. However, if the ratio of the carbonized raw material in the molded body is less than 80% by mass, it is difficult to mold the carbonized raw material. Even if the molded body is molded, the molded body may expand due to the heat treatment in the carbonization step (S14). Since pores are generated, it is difficult to obtain carbon with a low porosity in a high yield. Furthermore, the apparent specific gravity tends to be low.

  Therefore, it mix | blends so that the ratio of the carbonization raw material in a molded object may occupy 80 mass% or more, and it is set as a shaping | molding raw material. More preferably, it is 90% by mass or more, more preferably 100% by mass, that is, the obtained carbonized raw material is molded as it is without adding a binder compound.

  As described above, the method for producing a carbon material of the present invention includes an ashless coal production process, a carbonized raw material production process, a molding process, and a carbonization process in both the first embodiment and the second embodiment. In one embodiment, the molding process is included as needed). However, in carrying out the present invention, within a range that does not adversely affect the respective steps, for example, a coal pulverization step for pulverizing raw coal, or a removal step for removing unnecessary substances such as dust, before or after each step. Alternatively, other steps such as a carbonized raw material drying step for drying the carbonized raw material may be included.

Next, the manufacturing method of the carbon material according to the present invention will be specifically described with reference to examples and comparative examples.
<First embodiment>
In the first example, the apparent specific gravity, porosity, carbon yield, and ash concentration of the carbon material were examined.
First, ashless coal was produced by the following method.
Sub-bituminous coal was used as raw material coal, and 4 times the amount (20 kg) of solvent (1-methylnaphthalene (manufactured by Nippon Steel Chemical Co., Ltd.)) was mixed with 5 kg of this raw material coal to prepare a slurry. This slurry was pressurized with 1.2 MPa of nitrogen and extracted in an autoclave with an internal volume of 30 L at 370 ° C. for 1 hour. This slurry was separated into a supernatant and a solid concentrate in a gravity sedimentation tank maintained at the same temperature and pressure, and the solvent was separated and recovered from the supernatant by a distillation method to obtain ashless coal.
The following tests were conducted using the ashless coal thus obtained. In addition, since it can be carbonized without shaping | molding that it can shape | mold and carbonize, it heat-processed after forming into a molded object here.

[Example 1]
After mixing with 1 part by weight of ashless coal pulverized so that the whole amount passes through a sieve with an opening of 0.149 mm and mixing with 10 parts by weight of methyl ethyl ketone and stirring for 1 hour, use a nominal 0.5 μm filter. Insoluble matter (carbonized raw material) was collected by filtration. When this carbonized raw material was dried at 100 ° C. under reduced pressure, the carbonized raw material acquisition rate (carbonized raw material mass / charged ashless coal mass) was 78% by mass.
Next, this carbonized raw material is pulverized so that the entire amount passes through a sieve having an opening of 0.149 mm, and 5 g is filled in a mold having a cylindrical cavity with a diameter of 30 mm, and 0.1 ton / cm ² Press-molded with pressure. As a result, a molded body having a thickness of 6.4 mm and an apparent specific gravity of 1.1 g / cm ³ was obtained. This molded body was heated at a rate of 5 ° C./min in a nitrogen atmosphere and carbonized at 1000 ° C.

[Example 2]
A carbonized raw material was obtained under the same conditions as in Example 1 except that tetrahydrofuran was used instead of methyl ethyl ketone as the solvent. The yield of the carbonized raw material was 71% by mass. This carbonized raw material was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 6.4 mm and an apparent specific gravity of 1.1 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

[Example 3]
The mixture is mixed at a ratio of 5 parts by mass of 2-methylnaphthalene to 1 part by mass of ashless coal pulverized so that the whole amount passes through a sieve having a mesh opening of 0.149 mm, and heated to 360 ° C. under 1 MPa nitrogen pressure. The whole amount of ashless coal was dissolved by stirring for 1 hour. This was cooled to room temperature and left for 5 hours. The precipitated solid component (carbonized raw material) was collected by filtration with a nominal 0.5 μm filter. When dried under reduced pressure at 100 ° C., the acquisition rate of the carbonized raw material was 63% by mass.
This carbonized raw material was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 11.8 mm and an apparent specific gravity of 1.08 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

[Comparative Example 1]
The ashless coal was used as a carbonized raw material without solvent extraction, and the carbonized raw material was molded under the same conditions as in Example 1. A molded body having a thickness of 6.4 mm and an apparent specific gravity of 1.1 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

[Comparative Example 2]
A carbonized raw material was obtained under the same conditions as in Example 1 except that toluene was used instead of methyl ethyl ketone as the solvent. The acquisition rate of the carbon material was 97% by mass.
This carbon material was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 6.7 mm and an apparent specific gravity of 1.05 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

[Comparative Example 3]
A carbonized raw material was obtained under the same conditions as in Example 3 except that n-hexane was used instead of methyl ethyl ketone as the solvent. The acquisition rate of the carbonized raw material was 98% by mass.
This carbonized raw material was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 6.2 mm and an apparent specific gravity of 1.15 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

[Comparative Example 4]
The mixture is mixed at a ratio of 10 parts by mass of 2-methylnaphthalene to 1 part by mass of ashless coal pulverized so that the whole amount passes through a sieve having a mesh opening of 0.149 mm, and heated to 200 ° C. under nitrogen pressure of 1 MPa. Stir for 1 hour. While maintaining this temperature and pressure, insoluble matter (carbonized raw material) was collected by filtration using a nominal 0.5 μm filter. When dried under reduced pressure at 100 ° C., the acquisition rate of the carbonized raw material was 38% by mass.
This carbonized raw material was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 7.4 mm and an apparent specific gravity of 0.95 g / cm ³ was obtained. In addition, this molded object was a fragile thing which was broken when a little force was applied. This molded body was carbonized under the same conditions as in Example 1.

[Reference Example 1]
It mixed in the ratio of 1 mass part of ashless coal with respect to 10 mass parts of carbonization raw materials prepared by the comparative example 4, and it grind | pulverized so that the whole quantity might pass the sieve with an opening of 0.149 mm.
This mixture was molded under the same conditions as in Example 1. As a result, a molded body having a thickness of 12.3 mm and an apparent specific gravity of 1.04 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 1.

The apparent specific gravity, porosity, carbon yield (carbon material mass / charged ashless coal mass), and ash concentration of the carbon material obtained as described above were measured.
Here, the apparent specific gravity and the porosity were calculated according to JIS K2151 (testing method for cokes), and the ash concentration was measured according to JIS M8812 (industrial analysis method for coals and cokes).
The apparent specific gravity was judged to be good if it was 0.6 g / cm ³ or more and poor if it was less than 0.6 g / cm ³ . A porosity of 60% or less was judged good and a porosity exceeding 60% was judged bad. As for the carbon yield, those having 65% by mass or more were judged to have high carbon yield, and those having less than 65% by mass were judged to have low carbon yield. An ash concentration of less than 0.3% by mass was judged to be low.
These test results are shown in Table 1.

  In Table 1, Examples 1-3 satisfy | fill the structure of this invention. Therefore, it was possible to obtain a carbon molded body having a low porosity by being carbonized without significant foaming in the carbonization step. Moreover, as shown in Table 1, the carbon yield was high. The ash concentration in carbon was a high-purity quality with a very low ash concentration.

On the other hand, since Comparative Examples 1-4 did not satisfy the configuration of the present invention, they had the following problems.
Since the ashless coal was not solvent-extracted in the comparative example 1, it was not able to obtain a carbon molded object by foaming violently at a carbonization process. Moreover, the apparent specific gravity was low, the porosity was large, and the carbon yield was as low as 56% by mass. In Comparative Example 2, the acquisition rate of the carbonized raw material exceeded the upper limit value, so that the carbon molded body could not be obtained by vigorously foaming in the carbonization step. Further, the apparent specific gravity was low, the porosity was high, and the carbon yield was as low as 57% by mass.

  In Comparative Example 3, since the acquisition rate of the carbonized raw material exceeded the upper limit, foaming was severe and a carbon molded body having a small porosity could not be obtained. Moreover, the apparent specific gravity was low and the carbon yield was as low as 59% by mass. In Comparative Example 4, since the acquisition rate of the carbonized raw material was less than the lower limit value, a crack occurred in the molded body in the carbonization step, and the moldability decreased. Moreover, although the comparative example 4 had a high carbon yield, since the acquisition rate of the carbonization raw material was low, it was uneconomical.

  In Reference Example 1, it was possible to obtain a carbon molded body that was carbonized without foaming vigorously in the carbonization step, had a high apparent specific gravity, and a low porosity. That is, even if the acquisition rate of the carbonized raw material is less than the lower limit, it was found that a decrease in formability can be avoided by adding an appropriate amount of ashless coal as a binder.

<Second embodiment>
In the second example, the shape (thickness) of the molded body before and after the carbonization step was examined in addition to the apparent specific gravity, porosity, carbon yield, and ash concentration of the carbon material.
First, ashless coal was produced by the same method as in the first example. The softening temperature of ashless coal was 290 ° C. and the ash content was 0.2% by mass.

[Example 4]
The mixture was mixed at a ratio of 10 parts by mass of pyridine to 1 part by mass of ashless coal pulverized so that the whole amount passed through a sieve having an opening of 0.149 mm, and stirred at 50 ° C. for 1 hour. Insoluble matter (carbonized raw material) was collected by filtration using a nominal 0.5 μm filter. When dried under reduced pressure at 150 ° C., the acquisition rate of the carbonized raw material was 68% by mass, and the softening temperature was 355 ° C.
Next, 300 g of a carbonized raw material pulverized so as to pass through a sieve having an opening of 0.149 mm is filled in a cylindrical mold having a diameter of 100 mm, and compressed by applying a pressure of 0.3 ton / cm ² at room temperature. Molded. As a result, a molded body having a thickness of 3.8 cm and an apparent specific gravity of 1.02 g / cm ³ was obtained. The molded body was heated from room temperature to 380 ° C. at a temperature increase rate of 30 ° C./h in a nitrogen atmosphere, held at that temperature for 1 hour, and subsequently heated to 1500 ° C. at a temperature increase rate of 30 ° C./h. And it carbonized by hold | maintaining at this temperature for 30 minutes.

[Example 5]
The carbonized raw material was collected by filtration under the same conditions as in Example 6 except that quinoline was used instead of pyridine as the solvent. The acquisition rate of the carbonized raw material was 42% by mass, and the softening temperature was 450 ° C.
It mixed in the ratio of 15 mass parts of ashless coal with respect to 85 mass parts of this carbonization raw material, and it grind | pulverized so that the whole quantity might pass the sieve with an opening of 0.149 mm. This was molded in the same manner as in Example 4. A molded body having a thickness of 3.7 cm and an apparent specific gravity of 1.04 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 4.

[Comparative Example 5]
The ashless coal was used as a carbonized raw material without solvent extraction, and this carbonized raw material was molded under the same conditions as in Example 4. As a result, a molded body having a thickness of 3.9 cm and an apparent specific gravity of 0.99 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 4.

[Comparative Example 6]
A carbonized raw material was collected by filtration in the same manner as in Example 4 except that xylene was used instead of pyridine. When dried under reduced pressure at 150 ° C., the acquisition rate of the carbonized raw material was 79% by mass, and the softening temperature was 340 ° C.
Next, the carbonized element was molded in the same manner as in Example 4. As a result, a molded body having a thickness of 3.8 cm and an apparent specific gravity of 1.02 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 4.

[Comparative Example 7]
The carbonization raw material was collected by filtration under the same conditions as in Example 4 except that quinoline was used instead of pyridine as the solvent. The acquisition rate of the carbonized raw material was 42% by mass, and the softening temperature was 450.
The mixture was mixed at a ratio of 25 parts by mass of the ashless coal with respect to 75 parts by mass of the carbonized raw material, and pulverized so that the entire amount passed through a sieve having an opening of 0.149 mm. This was molded in the same manner as in Example 4. A molded body having a thickness of 3.8 cm and an apparent specific gravity of 1.02 g / cm ³ was obtained. This molded body was carbonized under the same conditions as in Example 4.

The apparent specific gravity, porosity, carbon yield (carbon material mass / charged ashless coal mass), and ash concentration of the carbon material obtained as described above were measured. Moreover, it investigated about the shape (thickness) of the molded object before and behind the carbonization process.
An apparent specific gravity of 1.0 g / cm ³ or more was judged to be good, and an apparent specific gravity of less than 1.0 g / cm ³ was judged to be poor. A porosity of 30% or less was judged good and a porosity exceeding 30% was judged bad. As for the carbon yield, those having 65% by mass or more were judged to have high carbon yield, and those having less than 65% by mass were judged to have low carbon yield. An ash concentration of less than 0.3% by mass was judged to be low. The shape of the molded body after the carbonization step is a predetermined one in which the thickness of the molded body is contracted, a carbon material obtained in a state where the predetermined shape is maintained, and a case in which the thickness of the molded body is expanded. It was judged that the carbon material could not be obtained in the state where the shape was maintained.
These test results are shown in Table 2. In Table 2, “-” indicates that a carbon molded body could not be obtained.

  In Table 2, Examples 4 and 5 satisfy the configuration of the present invention. Therefore, as shown in Table 2, the carbon molded body had an apparent specific gravity of 1.0 or more. The carbon yield was high. Furthermore, the ash concentration in the carbon was a high-purity quality with a very low ash concentration. Moreover, the porosity was as low as 30% or less, and the molded body after carbonization maintained a predetermined shape.

On the other hand, Comparative Examples 5 to 7 did not satisfy the configuration of the present invention, and thus had the following problems.
In Comparative Example 5, since ashless coal was not subjected to solvent extraction, it was not possible to obtain a carbon molded body by foaming vigorously in the carbonization step. Further, the apparent specific gravity was low, and the carbon yield was as low as 56% by mass. Furthermore, since the softening temperature of the carbonized raw material was too low (ashless coal: 290 ° C.), the porosity was as high as 89%.

  In Comparative Example 6, since the softening temperature of the carbonized raw material was too low, the thickness of the molded body expanded to 4.1 cm, and a carbon material having a predetermined shape was not obtained. Moreover, although apparent specific gravity was also favorable, it was somewhat low and the porosity exceeded 30%. In Comparative Example 7, the apparent specific gravity was low and the porosity exceeded 30% because the ratio of the carbonized raw material in the molded body in the molding step was less than the lower limit. The carbon yield was as low as 58% by mass. Although the thickness of the molded body is reduced after carbonization, the carbonization process causes expansion and contraction of the molded body at the same time. It is thought to be happening.

  The carbon material production method according to the present invention has been described in detail with reference to the best embodiment and examples. However, the gist of the present invention is not limited to the above-described contents, and the scope of rights is claimed. It should be interpreted broadly based on the description of the scope. Needless to say, the contents of the present invention can be widely modified and changed based on the above description.

It is a flowchart explaining the process of the manufacturing method of the carbon material which concerns on 1st Embodiment of this invention. It is a flowchart explaining the process of the manufacturing method of the carbon material which concerns on 2nd Embodiment of this invention.

Explanation of symbols

S1, S11 Ashless coal production process S2, S12 Carbonized raw material production process S3, S13 Molding process S4, S14 Carbonization process

Claims (4)

An ashless coal manufacturing process for reforming coal to produce ashless coal, which is a modified coal,
The ashless coal produced in the ashless coal production step is mixed with an organic solvent to extract a soluble component soluble in the organic solvent from the ashless coal. Separating into a liquid part containing a soluble component and a non-liquid part containing a component insoluble in the organic solvent, and a carbonized raw material production process using the non-liquid part as a carbonized raw material;
A carbonization step in which the carbonized raw material produced in the carbonized raw material production step is carbonized by heat treatment in an inert atmosphere,
The method for producing a carbon material, wherein a ratio of the carbonized raw material produced in the carbonized raw material production step is 40 to 90% by mass with respect to ashless coal mixed in the carbonized raw material production step. After the carbonized raw material manufacturing step, including a molding step of molding the carbonized raw material manufactured in the carbonized raw material manufacturing step into a lump shape,
2. The method for producing a carbon material according to claim 1, wherein in the carbonization step, the molded body molded in the molding step is heat-treated in an inert atmosphere to be carbonized. An ashless coal manufacturing process for reforming coal to produce ashless coal, which is a modified coal,
The ashless coal produced in the ashless coal production step is mixed with an organic solvent to extract a soluble component soluble in the organic solvent from the ashless coal. Separating into a liquid part containing a soluble component and a non-liquid part containing a component insoluble in the organic solvent, and a carbonized raw material production process using the non-liquid part as a carbonized raw material;
With the carbonized raw material produced in the carbonized raw material production step as a main component of the molding raw material, a molding step for molding the carbonized raw material into a lump,
A carbonization step of carbonizing the molded body molded in the molding step by heat treatment in an inert atmosphere,
The ratio of the carbonized raw material manufactured in the carbonized raw material manufacturing step is 40 to 90% by mass with respect to the ashless coal mixed in the carbonized raw material manufacturing step, and the softening temperature of the carbonized raw material is 350 ° C. or higher. And
The method for producing a carbon material, wherein a ratio of the carbonized raw material in the molded body molded in the molding step is 80% by mass or more.   The method for producing a carbon material according to any one of claims 1 to 3, wherein the organic solvent is an oxygen-containing organic solvent.

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