JP5118388B2 - Production method of carbon black - Google Patents

Description

  The present invention relates to a method for producing carbon black using coal as a raw material.

  Conventionally, carbon black has been widely used in various fields, for example, as a reinforcing material for tires and rubbers, black pigments for printing inks and paints, resin adhesives, dry battery materials, conductive materials, etc. Mainly used as a reinforcing material.

  Such carbon black production methods include an oil furnace method, a thermal method, a channel method, and the like. Currently, the oil furnace method accounts for 90% or more of the production amount. Coal-based creosote oil, petroleum-based ethylene bottom oil, FCC cracked oil, etc. are used as raw materials for the oil furnace process, but all are by-products in the refining process and are greatly influenced by trends in coke production and petroleum refining. There is a problem of being influenced.

Therefore, various methods for producing carbon black using coal as a raw material have been studied from the viewpoint of stably securing raw materials used for the production of carbon black and from the viewpoint of reducing production costs.
Examples of a method for producing carbon black using such coal as a raw material include a method of pulverizing and using coal, a method of thermally decomposing coal, and the like.

  For example, in Patent Document 1, as a method of using finely pulverized coal, the raw material coal is pulverized to an appropriate particle size and subjected to dry distillation treatment, and the dry-distilled coal powder is treated with a surface treatment agent. A method for obtaining carbon black modified with an agent is disclosed.

  In Patent Document 2, as a method for thermally decomposing coal, in a method for producing carbon black containing less than about 1% ash from a carbonaceous material, the carbonaceous material is mixed with oxygen and 2,200 ° F. to 3,000. A method for producing carbon black that is reacted at a temperature of ° F (about 1,204 ° C to 1,649 ° C) is disclosed. Further, Patent Document 3 discloses carbon obtained by separating oil from tar obtained by rapid thermal decomposition of coal to 600 to 1000 ° C. in a time of 10 seconds or less, and using this as a carbon black feedstock. A method for producing black feedstock is disclosed.

  Further, Patent Document 4 discloses a method of pulverizing raw material coal to an appropriate particle size, mixing with water to form a slurry, and introducing the slurry into a reaction furnace to obtain carbon black by thermal decomposition. ing.

JP-A-2-202958 (page 3, upper left column, line 2 to lower left column, line 11) JP-A-61-275362 (page 2, lower left column, line 10 to page 3, upper left column, line 18) Japanese Patent No. 2745653 (page 2, left column, line 7 to page 2, right column, line 7) Japanese Examined Patent Publication No. 4-14147 (page 6, right column, line 6 to page 3, left column, line 3)

However, the conventional method for producing carbon black has the following problems.
In the production method using finely pulverized coal as the raw material, it is difficult to separate ash in the coal, and the ash contained in the carbon black cannot be reduced, so that it cannot be used for the production of high-quality carbon black. There was a problem.
Further, in the method of producing carbon black by pyrolyzing coal, there are problems that it is difficult to control pyrolysis and that the yield of carbon black is low. Furthermore, in the method of performing pyrolysis using coal particles as they are, the reaction temperature, pressure, residence time, coal particle size, etc. must be controlled, and precise operation condition control is required. It was.

  This invention is made | formed in view of the said problem, The objective is to provide the manufacturing method of carbon black which can obtain carbon black provided with the outstanding quality with high efficiency.

The method for producing carbon black according to claim 1 of the present invention includes a slurry preparation step, an extraction step, a separation step, an extracted coal acquisition step, a remelted extracted coal solution acquisition step, and a pyrolysis step. It is characterized by that.

According to such a procedure, in a slurry preparation process, a solvent and coal which is a raw material of carbon black are mixed to prepare a slurry. Moreover, in the extraction process, the coal component extracted into the solvent is extracted into the solvent with high efficiency by heat-treating the slurry obtained in the slurry preparation process. Furthermore, in the separation step, the slurry obtained in the extraction step is an extracted coal solution that is a solution containing coal components extracted in a solvent, and a non-extracted coal concentrate that is a slurry containing coal components that are insoluble in the solvent. To be separated. And in an extraction charcoal acquisition process, a solvent is isolate | separated from the extraction charcoal solution isolate | separated at the isolation | separation process, and an extraction charcoal is manufactured. Further, in the re-dissolved extracted coal solution acquisition step, the extracted coal obtained in the extracted coal acquisition step is dissolved in a solvent separated from one or more of the extracted coal solution and the non-extracted coal concentrate. Furthermore, in the thermal decomposition step, the extracted coal contained in the redissolved extracted coal solution obtained in the redissolved extracted coal solution obtaining step is pyrolyzed to produce carbon black.

  According to the carbon black production method of the present invention, coal is heated and extracted using a solvent to obtain a solvent extract material such as extracted coal, and the obtained solvent extract material is used as a raw material. The ash content in carbon black can be reduced. Therefore, high-quality carbon black can be produced from coal easily and with high efficiency. Moreover, since solvent extraction substances, such as extraction charcoal, are excellent in softening meltability, carbon black can be manufactured with a high yield. Furthermore, even if cheap coal is used, high-quality carbon black can be produced with a high yield, so that economic efficiency can be improved.

Next, the method for producing carbon black 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 method for producing carbon black according to the first embodiment of the present invention, and FIG. 2 is a method for producing carbon black according to the second embodiment of the present invention. FIG. 3 is a flowchart for explaining the steps of the method for producing carbon black according to the third embodiment of the present invention, and FIG. 4 is a method for producing carbon black according to the fourth embodiment of the present invention. A flowchart illustrating the process of
FIG. 5 is a flowchart for explaining the steps of the carbon black production method according to the fifth embodiment of the present invention, and FIG. 6 uses a gravity sedimentation method as a method for separating the extracted coal solution and the non-extracted coal concentrate. FIG. 7 is a schematic diagram showing an outline of a process for producing a raw material for carbon black to be supplied into a reaction furnace.

[First Embodiment]
First, a first embodiment of the method for producing carbon black according to the present invention will be described.
As shown in FIG. 1, the method for producing carbon black includes a slurry preparation step (S1), an extraction step (S2), a separation step (S3), and a thermal decomposition step (S4).
Hereinafter, each step will be described.

<Slurry preparation step (S1)>
The slurry preparation step (S1) is a step of preparing a slurry by mixing a solvent and coal.

As the solvent for dissolving coal, it is preferable to use a non-hydrogen donating solvent mainly composed of a bicyclic aromatic.
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. Since this non-hydrogen donating solvent is stable even in a heated state and has excellent affinity with coal, the proportion of coal components extracted into the solvent (hereinafter also referred to as “extraction rate”) is high. It is a solvent that can be easily recovered by methods such as distillation. The recovered solvent can be recycled for improving economic efficiency.
The main components of the non-hydrogen-donating solvent include bicyclic aromatic naphthalene, methylnaphthalene, dimethylnaphthalene, trimethylnaphthalene and the like, other naphthalenes having an aliphatic side chain, biphenyl and long chain Alkylbenzenes with aliphatic side chains are included.

  The non-hydrogen donating solvent preferably has a boiling point of 180 to 330 ° C. When the boiling point is less than 180 ° C., the required pressure in the extraction step (S2) and the separation step (S3) increases, and the loss due to volatilization increases in the step of recovering the solvent, and the solvent recovery rate decreases. . Furthermore, the extraction rate in the extraction step (S2) decreases. On the other hand, when it exceeds 330 ° C., it becomes difficult to separate the solvent from the extracted coal solution and the non-extracted coal concentrate described later, and the solvent recovery rate is lowered.

  Moreover, as a solvent which dissolves coal, in addition to the non-hydrogen donating solvent, a monocyclic aromatic compound such as benzene, toluene and xylene, a polar solvent such as N-methylpyrrolidone (NMP) and pyridine, and the like are used. You can also.

  Coal used as a raw material for carbon black (hereinafter also referred to as “raw coal”) includes non-slightly caking coal that has little softening and melting properties, and low-grade coal such as lignite and sub-bituminous coal. It is preferable to use it. By using inexpensive coal such as these, carbon black can be manufactured at low cost, so that economic efficiency can be improved. However, the coal used is not limited to these inferior coals, 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.). Further, the low-grade coal is coal that contains 20% or more moisture and is desired to be dehydrated. Examples of such low-grade coal include lignite, lignite, and sub-bituminous coal. For example, lignite coal includes Victoria coal, North Dakota coal, Belga coal, etc., and sub-bituminous coal includes West Banco coal, Binungan 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 moisture and desired to be dehydrated is included in the low-grade coal referred to in the present invention.

  Although the coal density | concentration with respect to a solvent is based also on the kind of raw material coal, the range of 10-30 mass% is preferable on a dry coal basis, and the range of 15-25 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, but if it exceeds 30% by mass, the viscosity of the prepared slurry becomes high, and the separation of the extracted coal solution and the non-extracted coal concentrate in the slurry transfer and separation step (S3) It tends to be difficult.

<Extraction process (S2)>
The extraction step (S2) is a step in which the extraction process is performed by heating the slurry obtained in the slurry preparation step (S1). By this extraction process, the coal component is extracted into the solvent.
By extracting the coal component into a solvent, high-quality carbon black can be obtained with high efficiency.

  The heating temperature of the slurry in the extraction step (S2) is preferably in the range of 300 to 420 ° C. When the heating temperature is less than 300 ° C., it is insufficient to weaken the bonds between the molecules constituting the coal, and when inferior coal is used as the raw coal, the resolidification temperature of the resulting ashless coal is strongly coagulated. It tends to be difficult to raise the charcoal resolidification temperature to the same level. On the other hand, if it exceeds 420 ° C., the pyrolysis reaction of coal becomes very active and recombination of the generated pyrolysis radicals occurs, so that the extraction rate tends to decrease.

  The heating time of the slurry in the extraction step (S2) is preferably in the range of 3 to 60 minutes. If the heating time is less than 3 minutes, the extraction process may be insufficient and the extraction rate tends to decrease. On the other hand, when the heating time exceeds 60 minutes, the thermal decomposition reaction proceeds too much, the radical polymerization reaction proceeds, and the extraction rate tends to decrease.

  In addition, during extraction in this extraction step (S2), aromatic-rich components mainly having an average boiling point (Tb50: 50% distillation temperature) of 200 to 300 ° C. are generated by thermal decomposition of coal. It can be used as a part of the solvent.

The extraction step (S2) is preferably performed in the presence of an inert gas.
This is because contact with oxygen in the extraction step (S2) is dangerous because it may ignite, and the cost increases when hydrogen is used.
As the inert gas used in the extraction step (S2), inexpensive nitrogen is preferably used, but is not particularly limited. The pressure in the extraction step (S2) 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.

<Separation step (S3)>
The separation step (S3) is a step of separating the slurry obtained in the extraction step (S2) into an extracted coal solution and a non-extracted coal concentrate.
Here, the extracted coal solution refers to a solution containing a coal component extracted into a solvent, and the non-extracted coal concentrate is a slurry containing a coal component insoluble in the solvent (coal containing ash, that is, ash coal). Say.

The method for separating the slurry into the extracted coal solution and the non-extracted coal concentrate in the separation step (S3) is not particularly limited, but it is preferable to use a gravity sedimentation method (the gravity sedimentation method will be described later). To do).
As a method for separating the slurry into the extracted charcoal solution and the non-extracted charcoal concentrate, various filtration methods and centrifugal separation methods are generally known, and these methods may be used. However, the filtration method requires frequent replacement of the filter, and the centrifugation method has a problem that clogging with undissolved coal components is likely to occur. 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, the extracted coal solution, which is a solution containing coal components extracted into the solvent, is concentrated from the lower part of the gravity sedimentation tank, which is a slurry containing coal components insoluble in the solvent. A liquid can be obtained.

  The extracted coal dissolved in the extracted coal solution contains almost no ash, has no moisture, and exhibits a higher calorific value than the raw coal. Furthermore, the softening and melting property, which is a particularly important quality as a raw material for carbon black, is greatly improved, and shows a performance (fluidity) far superior to that of raw material coal. Therefore, this extracted coal is suitable as a carbon black raw coal, and an extracted coal solution in which the extracted coal is dissolved can be used as a raw material as it is.

  The extracted coal contained in the extracted coal solution has an ash concentration as low as 1/10 to 1/100 that of coal, and can be 0.1% by mass (based on dry coal mass) or less (JP 2005-2005). 120185), ash content in carbon black can be reduced. Further, according to NMR (nuclear magnetic resonance) analysis, about 90% of the extracted coal is aromatic carbon and, on average, about 4 to 6 aromatic rings are condensed. Becomes higher.

  Then, as will be described later, the extracted coal without ash can be obtained from the extracted coal solution by separating and collecting the solvent from the extracted coal solution and the non-extracted coal concentrate using a distillation method or the like. Moreover, the non-extracted charcoal with which the ash content was concentrated can be obtained from the non-extracted charcoal concentrate as needed.

<Pyrolysis step (S4)>
The pyrolysis step (S4) is a step of supplying the extracted coal solution obtained in the separation step (S3) into the reaction furnace and producing carbon black by pyrolysis.

  In the pyrolysis step (S4), first, fuel oil (or gas) and air are introduced into the reactor, and the fuel oil (or gas) is completely burned, and high temperature combustion at 1300 to 1700 ° C. is performed in the reactor. A gas atmosphere is formed. Next, the extracted charcoal solution is supplied into the reaction furnace by spraying from, for example, a spray nozzle, whereby the extracted charcoal contained in the extracted charcoal solution is pyrolyzed to generate carbon black.

  If the temperature in the reaction furnace is less than 1300 ° C., thermal decomposition is not promoted and the yield of carbon black tends to decrease. On the other hand, if it exceeds 1700 ° C., control of thermal decomposition is difficult and the fuel cost is high. Therefore, productivity tends to decrease.

  Then, the gas containing carbon black is rapidly cooled to 400 ° C. or lower by water injection or the like in the latter stage of the reaction furnace, and the carbon black generated by the bag filter or the like is recovered.

By using the extracted charcoal solution as it is, it can be easily sprayed and uniformly reacted when supplied into the reaction furnace. In addition, handling is improved.
As described above, the extracted coal solution can be used as it is, but as described later, the solvent may be separated and recovered from the extracted coal solution, and the solvent may be recycled.

[Second Embodiment]
Next, a second embodiment of the method for producing carbon black according to the present invention will be described.
As shown in FIG. 2, the carbon black manufacturing method includes a slurry preparation step (S21), an extraction step (S22), a separation step (S23), an extracted coal acquisition step (S24), and a pyrolysis step (S25). ) And.
Hereinafter, each step will be described.

  Since the slurry preparation step (S21), the extraction step (S22), and the separation step (S23) are the same as those in the first embodiment (S1, S2, S3), description thereof is omitted here. The pyrolysis step (S25) is the same as in the first embodiment (S4) except that the extracted coal is supplied in the reaction furnace instead of the extracted coal solution. Is omitted.

<Extracted charcoal acquisition process (S24)>
The extracted charcoal acquisition step (S24) is a step of obtaining extracted charcoal by separating the solvent from the extracted charcoal solution separated in the separation step (S23).

  As a method for separating the solvent from the extracted charcoal solution, a general distillation method, an evaporation method (spray drying method or the like) or the like can be used, and the separated and recovered solvent is, for example, a solvent supply tank (see FIG. 6). ) And can be used repeatedly. Extracted coal substantially free of ash can be obtained from the extracted coal solution by separating and collecting the solvent.

  As described above, this extracted coal contains almost no ash, has no moisture, and exhibits a higher calorific value than raw coal. And since it shows the performance (fluidity) far superior to raw material coal, it is suitable as raw material coal of carbon black.

  The extracted coal thus obtained is supplied into the reactor, but the extracted coal exhibits softening and melting properties at 200 to 300 ° C. (see Japanese Patent Application Laid-Open No. 2006-070182). The extracted coal immediately after is recovered is in a molten state. Therefore, as in the conventional oil furnace method, liquid supply into the reaction furnace is possible.

  By using the extracted charcoal, the standard product as carbon black raw coal can be used as it is, and the solvent can be reused.

  If necessary, in the extracted coal acquisition step (S24), in addition to obtaining extracted coal, the solvent is separated from the non-extracted coal concentrate separated in the separation step (S23) to obtain non-extracted coal. You may manufacture (non-extracted charcoal acquisition process).

  The method for separating the solvent from the non-extracted charcoal concentrate can use a general distillation method, evaporation method or the like, as in the above-described extracted charcoal acquisition step (S24). For example, it can circulate to a solvent supply tank (refer FIG. 6), and can be used repeatedly. By separating and collecting the solvent, non-extracted charcoal in which ash is concentrated can be obtained from the non-extracted charcoal concentrate.

Although this non-extracted coal contains ash, it has no water and has a sufficient calorific value. This is not shown for softening and melting properties, but since the oxygen-containing functional group is eliminated, it can be used for various fuels.
Only the extracted coal without ash from the extracted coal solution is produced for carbon black raw coal, only the solvent is recovered from the non-extracted coal concentrate, Similarly, it can be used as fuel.

[Third Embodiment]
Next, a third embodiment of the method for producing carbon black according to the present invention will be described.
As shown in FIG. 3, the method for producing carbon black includes a slurry preparation step (S31), an extraction step (S32), a separation step (S33), an extracted coal concentrate acquisition step (S34), and a thermal decomposition step. (S35).
Hereinafter, each step will be described.

  The slurry preparation step (S31), the extraction step (S32), and the separation step (S33) are the same as those in the first embodiment (S1, S2, S3), and thus the description thereof is omitted here. The pyrolysis step (S35) is the same as that in the first embodiment (S4) except that the extracted coal solution is supplied into the reaction furnace instead of the extracted coal solution. The description is omitted.

<Extracted charcoal concentrate acquisition step (S34)>
The extracted charcoal concentrate obtaining step (S34) is a step of obtaining an extracted charcoal concentrate by separating a part of the solvent from the extracted charcoal solution separated in the separation step (S33).

In the extracted coal acquisition step (S24) in the second embodiment, all of the solvent is separated and recovered from the extracted coal solution, and the recovered solvent is circulated and used as necessary. It is not necessary to separate and collect all, and only a part may be separated and collected. By separating and recovering a part of the solvent, the recovered solvent can be recycled.
Further, by using the extracted charcoal concentrate, it is easy to spray and uniformly react when supplied into the reaction furnace.

  Here, the part of the solvent is not particularly limited, and may be appropriately adjusted in accordance with the performance of the solvent recovery device or the like, the environment in the actual production process of carbon black, the equipment, the production status, and the like.

[Fourth Embodiment]
Next, a fourth embodiment of the carbon black production method according to the present invention will be described.
As shown in FIG. 4, the method for producing carbon black includes a slurry preparation step (S41), an extraction step (S42), a separation step (S43), an extracted coal acquisition step (S44), and a remelted extracted coal solution. An acquisition process (S45) and a thermal decomposition process (S46) are included.
Hereinafter, each step will be described.

  In addition, about slurry preparation process (S41), extraction process (S42), and separation process (S43), it is said 2nd implementation about said 1st embodiment (S1, S2, S3), and extraction charcoal acquisition process (S44). Since it is the same as that of form (S24), description is abbreviate | omitted here. The pyrolysis step (S46) is the same as the first embodiment (S4) except that the remelted extracted coal solution is supplied into the reaction furnace instead of the extracted coal solution. Then, explanation is omitted.

<Remelting extraction charcoal solution acquisition process (S45)>
The remelted extracted charcoal solution acquisition step (S45) is a step of dissolving the extracted charcoal obtained in the extracted charcoal acquisition step (S44) in a solvent to obtain a remelted extracted charcoal solution.

  The solvent for dissolving the extracted charcoal is the same as the solvent described in the slurry preparation step (S1) of the first embodiment. Moreover, an unused solvent may be used, and a solvent separated and recovered from an extracted coal solution or a non-extracted coal concentrate may be recycled.

  The remelted extracted coal solution thus obtained is supplied into the reaction furnace as described above. However, if the extracted coal is dissolved in a solvent and used, handling is further improved. In addition, standard products as carbon black raw coal can be used, and further, when supplied to the reaction furnace, it is easy to spray and make uniform reaction easy.

[Fifth Embodiment]
Next, a fifth embodiment of the carbon black production method according to the present invention will be described.
As shown in FIG. 5, the carbon black manufacturing method includes a slurry preparation step (S51), an extraction step (S52), a separation step (S53), an extracted coal acquisition step (S54), and a finely pulverized extracted coal acquisition. A process (S55) and a thermal decomposition process (S56) are included.
Hereinafter, each step will be described.

  In addition, about the slurry preparation process (S51), the extraction process (S52), and the separation process (S53), the first embodiment (S1, S2, S3) and the extracted charcoal acquisition process (S54) are the second implementation. Since it is the same as the form (S24), the description is omitted here. The pyrolysis step (S56) is the same as that in the first embodiment (S4) except that not the extracted coal solution but the pulverized extracted coal is supplied into the reaction furnace. The description is omitted.

<Pulverized extracted charcoal acquisition step (S55)>
The finely pulverized extracted coal acquisition step (S55) is a step of pulverizing the extracted coal obtained in the extracted coal acquisition step (S54) to obtain finely pulverized extracted coal.

The extracted coal has a hard glove index (HGI) of 100 or more (ordinary coal is around 50) and is very pulverized. Here, the hard glove index (HGI) is an index representing grindability, and the larger this value, the better the grindability. Therefore, since the extracted coal is excellent in pulverization, the extracted coal obtained in the extracted coal acquisition step (S54) is pulverized and pulverized, and the differentiated extracted coal (pulverized extracted coal) is supplied into the reaction furnace. It is also possible to do. By using finely pulverized extracted coal, the extracted coal is easily pyrolyzed, and carbon black can be efficiently generated. Further, a standard product as carbon black raw coal can be used, and further, the operation is easy at the time of supply to the reactor.
The supply to the reaction furnace can be performed, for example, by blowing pulverized coal.

  The average particle size of the finely pulverized extracted coal is not particularly limited, and may be appropriately adjusted depending on the type of the reactor, the heating temperature, the amount of components in the extracted coal, etc., but is usually about 100 μm or less, preferably It adjusts so that it may become 70 micrometers or less, More preferably, it is 20 micrometers or less. By adjusting the particle size in this way, the thermal decomposition reaction can be performed uniformly.

  As a method for pulverizing the extracted charcoal, a conventionally known method may be used. For example, an impact pulverizer such as a screen mill, a jet pulverizer such as a micronizer, and a ball mill pulverizer such as a tube mill or a pot mill may be used alone. Or it can use combining suitably.

  In carrying out the present invention, other steps may be included between or before and after each step as long as they do not adversely affect each step. For example, the surface of the carbon black obtained as described above is further removed by using a vibratory wet classifier, a wind separator, etc., to remove foreign substances present in the carbon black, or by using a commonly used oxidizing agent. A step of performing a treatment for reforming may be included.

  Next, with reference to FIG. 6, an example of the process of the carbon black production method will be described using a gravity sedimentation method as an example of a method for separating an extracted coal solution and a non-extracted coal concentrate.

  As shown in FIG. 6, first, in the solid-liquid separator 100, predetermined amounts of coal and solvent are respectively supplied from the coal supply tank 1 and the solvent supply tank 2 to the slurry preparation tank 3 to prepare a coal / solvent slurry. Next, a predetermined amount of this slurry is supplied from the slurry preparation tank 3 to the preheater 4 by a pump (not shown), and is heated to a predetermined temperature by the preheater 4. Then, a predetermined amount of the heated slurry is supplied to the extraction tank 5 heated to 300 to 420 ° C., the extraction treatment is performed for a predetermined residence time, and then the extracted slurry is supplied to the settling tank 6 for extraction. Separate into charcoal solution and unextracted charcoal concentrate.

  The non-extracted charcoal concentrate is discharged from the lower part of the settling tank 6 to the non-extracted charcoal concentrate receiver 7, and then the solvent is separated and collected by the non-extracted charcoal concentrate solvent recovery device 8 as necessary. Unextracted charcoal is obtained from the charcoal concentrate. The extracted charcoal solution is extracted from the upper part of the settling tank 6 and supplied to the extracted charcoal solution receiver 9, and then the solvent is separated and recovered by the extracted charcoal solution solvent recovery device 10 to obtain the extracted charcoal from the extracted charcoal solution. . Note that the extracted coal is in a molten state in the extracted coal solution solvent recovery device 10 maintained at about 200 to 300 ° C., and is supplied to the reaction furnace 20 as it is.

  In the reaction furnace 20, fuel oil (or gas) is combusted and heated to 1300 to 1700 ° C., and the extracted coal is thermally decomposed in the reaction furnace 20 to generate carbon black. And the gas containing carbon black is rapidly cooled by injecting cooling water in the latter stage in the reaction furnace 20, and the carbon black produced | generated by the bag filter 21 is collect | recovered.

  Here, the solvent separated and recovered by the non-extracted charcoal concentrated liquid solvent recovery device 8 and the extracted charcoal solution solvent recovery device 10 is circulated to the solvent supply tank 2 and reused as necessary.

  Here, the case where the extracted coal is supplied into the reaction furnace 20 is shown as an example (the second embodiment), but as the solvent extraction material supplied into the reaction furnace 20 as a raw material of carbon black, It is not limited to extracted coal. Hereinafter, the raw material of carbon black supplied into the reaction furnace will be described with reference to FIGS.

  As shown in FIG. 7, after the coal as a raw material is heated and extracted, it is subjected to solid-liquid separation, and the solvent is recovered from the extracted coal solution to obtain the extracted coal, and the solvent is recovered from the non-extracted coal concentrate to Extracted coal is obtained. Here, examples of the solvent extraction substance supplied into the reaction furnace 20 as a raw material for carbon black include the following.

  (A) Extracted coal solution (raw material 1) obtained by solid-liquid separation after heat extraction of coal and before solvent recovery, that is, the extracted coal solution supplied to the extracted coal solution receiver 9 is used as it is. You may supply in the reaction furnace 20 (the said 1st Embodiment).

  (B) Extracted charcoal in the molten state immediately after all the solvent in the extracted charcoal solution is recovered (raw material 2), that is, extracted charcoal obtained by separating and recovering all the solvent in the extracted charcoal solution solvent recovery device 10 Alternatively, it may be supplied into the reaction furnace 20 (the second embodiment).

  (C) Extracted charcoal concentrate (raw material 3) obtained by partially recovering the solvent in the extracted charcoal solution, that is, in the extracted charcoal solution solvent recovery device 10, only a part of the solvent is separated. -The extracted charcoal concentrate which is recovered and mixed with the extracted charcoal and the solvent may be supplied into the reaction furnace 20 (the third embodiment).

  (D) A re-dissolved extracted charcoal solution (raw material 4) obtained by adding a solvent to the extracted charcoal, that is, the extracted charcoal obtained by separating and recovering all of the solvent in the extracted charcoal solution solvent recovery apparatus 10 The redissolved and extracted charcoal solution obtained by dissolving in the reactor may be supplied into the reaction furnace 20 (the fourth embodiment).

  (E) Finely extracted coal obtained by pulverizing extracted coal (raw material 5), that is, fine coal obtained by finely pulverizing extracted coal obtained by separating and recovering the solvent in the extracted coal solution solvent recovery device 10 The pulverized and extracted charcoal may be supplied into the reaction furnace 20 (the fifth embodiment).

  As described above, in the present invention, as the raw material of carbon black supplied into the reaction furnace 20, the raw material in the above-described first to fifth embodiments according to the environment, equipment, manufacturing status, etc. in the actual manufacturing process. 1 to 5 (see FIG. 7) can be appropriately selected.

  As mentioned above, although the best embodiment was shown and demonstrated in detail about the manufacturing method of carbon black concerning the present invention, the meaning of the present invention is not limited to the above-mentioned contents. 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 black which concerns on 1st Embodiment of this invention. It is a flowchart explaining the process of the manufacturing method of the carbon black which concerns on 2nd Embodiment of this invention. It is a flowchart explaining the process of the manufacturing method of the carbon black which concerns on 3rd Embodiment of this invention. It is a flowchart explaining the process of the manufacturing method of the carbon black which concerns on 4th Embodiment of this invention. It is a flowchart explaining the process of the manufacturing method of the carbon black which concerns on 5th Embodiment of this invention. It is a schematic diagram explaining the process of the manufacturing method of carbon black at the time of using a gravity sedimentation method as a method of isolate | separating into an extracted charcoal solution and a non-extracted charcoal concentrate. It is a schematic diagram which shows the outline about the manufacturing process of the solvent extraction material supplied in a reaction furnace as a raw material of carbon black.

Explanation of symbols

S1, S21, S31, S41, S51 Slurry preparation step S2, S22, S32, S42, S52 Extraction step S3, S23, S33, S43, S53 Separation step S4, S25, S35, S46, S56 Thermal decomposition step S24, S44, S54 Extracted coal acquisition process S34 Extracted coal concentrate acquisition process S45 Remelted extraction coal solution acquisition process S55 Finely ground extracted coal acquisition process 1 Coal supply tank 2 Solvent supply tank 3 Slurry preparation tank 4 Preheater 5 Extraction tank 6 Settling tank 7 Non Extracted coal concentrate receiver 8 Non-extracted coal concentrate solvent recovery device 9 Extracted coal solution receiver 10 Extracted coal solution solvent recovery device 20 Reactor 21 Bag filter 100 Solid-liquid separator

Claims (1)

A slurry preparation step of preparing a slurry by mixing a solvent and coal;
An extraction step of performing an extraction treatment by heating the slurry obtained in the slurry preparation step;
A separation step of separating the slurry obtained in the extraction step into an extracted coal solution and a non-extracted coal concentrate using a gravity sedimentation method;
Extracted coal acquisition step of obtaining the extracted coal by separating the solvent from the extracted coal solution separated in the separation step;
Re-dissolved extracted charcoal solution obtaining step for dissolving the extracted charcoal obtained in the extracted charcoal obtaining step in a solvent and obtaining a re-dissolved extracted charcoal solution;
Supplying the re-dissolved extracted charcoal solution obtained in the re-dissolved extracted charcoal solution obtaining step into a reaction furnace, and producing a carbon black by pyrolysis;
Only including,
In the re-dissolved extracted charcoal solution obtaining step, as a solvent for dissolving the extracted charcoal, a solvent separated from one or more of the extracted charcoal solution and the non-extracted charcoal concentrate is used . Production method.

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