KR102073155B1 - A production method of binderless carbon block using reformation of mesocarbon microbeads - Google Patents

Abstract

The present invention relates to a method for producing a carbon block by producing and mesocarbon microbeads from coal tar pitch, and to a carbon block produced by such a method, more specifically mesocarbon micro prepared from coal tar pitch Through the oxidation stabilization process of the beads, to increase the aromatic carbon content to suppress the expansion phenomenon, to control the volatilization rate of low molecular weight of the carbonization process to produce an isotropic carbon block improved mechanical properties and It relates to a high-density and high-strength carbon block produced by this manufacturing method.

Description

A production method of binderless carbon block using reformation of mesocarbon microbeads}

The present invention relates to a method for producing a high density carbon block without a polymer binder, and more particularly, to a method for producing a high density and high strength binderless carbon block through the production of mesocarbon microbeads from the coal tar pitch and oxidation stabilization. .

High-density, high-strength isotropic carbon blocks are materials of high utility in modern high-tech industries because of their low electrical resistance and good mechanical properties at high temperatures (K. Miyazaki, et al., Journal of Materials Science, 16 (1981) 752-762; And H. Marsh, et al., Introduction to carbon technologies, in, Universidad de Alicante, Alicante: 1997). In particular, high-density, high-strength isotropic carbon blocks are used as excellent materials in nuclear reactors, electrical contacting, electrodes, refractory materials, crucibles for chemicals and semiconductors. (MR Delport, et al., Journal of Materials Science, 51 (2016) 6309-6318; K. Shen, et al., Carbon, 90 (2015) 197-206; and Y.-G. Wang, et al. , Carbon, 37 (1999) 1049-1057).

A general method for producing high density isotropic carbon blocks is to pulverize, knead and shape coke and binder pitch as fillers and repeat firing and impregnation. Another method is to form and calcinate the self-sintering coke or mesoface pitch through cold isostatic pressing without binder (W. Boenigk, et al., Google Patents, 1994; A. Grint, et al., Google Patents, 1989; S.-M. Lee, et al., Carbon letters, 16 (2015) 135-146; Q. Lin, et al., Journal of Analytical and Applied Pyrolysis, 71 (2004) 817-826; and M.-D. Fang, et al., Carbon, 50 (2012) 906-913). Another method is isothermal pressure molding and mesocarbon microbeads (MCMBs) is calcined. As such, the improved manufacturing methods have the advantage of lower process costs and labor than conventional methods. In particular, since 1973, MCMBs have been reported by many researchers as precursors of high density high strength carbon blocks and rechargeable Li-ion batteries (Y. Yamada, et al., Carbon, 12 (1974). 307-319; LM Manocha, et al., Carbon, 39 (2001) 663-671; M.-D. Fang, et al., Materials Chemistry and Physics, 149-150 (2015) 400-404; Y. Cheng, et al., Engineering, 47 (2013) 290-297; Y. Song, et al., Carbon, 42 (2004) 1427-1433; M. Broussely, et al., Electrochimica Acta, 45 (1999) 3 -22; M. Endo, et al., Carbon, 38 (2000) 183-197; and I. Mochida, et al., Carbon, 38 (2000) 305-328).

The effects and mechanisms of oxidation stabilization on mesophase pitch and carbon fiber have been reported several times (J. Drbohlav, et al., Carbon, 33 (1995) 693-711; SM Zeng, et al. , Carbon, 31 (1993) 413-419; I. Mochida, et al., Carbon, 28 (1990) 311-319; and Y. Korai, et al. Carbon, 29 (1991) 561-567). The mechanism of reported oxidative stabilization is divided into three steps. Initially, methylene hydrogens are reduced. Thereafter, aldehyde ketone / carboxylic acid functionality is produced, and ester and anhydride functionality is increased (J. Drbohlav, et al., Carbon, 33 (1995) 693 -711).

This oxidation mechanism is used for different purposes in each application. Oxidative stabilization of the carbon fiber manufacturing process increases carbonization yield and has good mechanical properties (SM Zeng, et al., Carbon, 31 (1993) 413-419; and A. Bismarck, et al., Applied Science and Manufacturing, 30 (1999) 1351-1366). In addition, when producing an excellent isotropic pitch, when increasing the aromatic carbon content, air blowing is used by applying an oxidation mechanism (J. Drbohlav, et al., Carbon , 33 (1995) 693-711; I. Mochida, et al., Carbon, 28 (1990) 311-319; LE Jones, et al., Carbon, 29 (1991) 251-269; and VJ Mimeault, et al Fiber Science and Technology, 3 (1971) 273-283). An oxidation process is also used in the graphene manufacturing method developed by Hummers (WS Hummers, et al., Journal of the American Chemical Society, 80 (1958) 1339-1339; J. Chen, et al., Carbon, 64 (2013) 225-229; and J. Shen, et al., Chemistry of Materials, 21 (2009) 3514-3520). Graphite oxide (GO) is prepared by increasing the oxygen content of graphite by using KMnO ₄ , NaNO ₃ and H ₂ SO ₄ . Thereafter, graphene is prepared through exfoliation and reduction (WS Hummers, et al., Journal of the American Chemical Society, 80 (1958) 1339-1339; J. Chen, et al., Carbon, 64 (2013) 225-229; and H. Bai, et al., Advanced Materials, 23 (2011) 1089-1115). The oxidation process is processed for smooth exfoliation but has the disadvantage of recovering during reduction at about 900 ° C. (H. Bai, et al., Advanced Materials, 23 (2011) 1089-1115; G. Wang, et al., Small, 8 (2012) 452-459; and C.-Y. Su, et al., ACS Nano, 4 (2010) 5285-5292). In addition, research to address restacking has been reported continuously (X. Yang, et al., Advanced Materials, 23 (2011) 2833-2838; J. Li, et al. Crystals, 3 (2013) 163; and JH Lee, et al., ACS Nano, 7 (2013) 9366-9374).

Accordingly, the present inventors have developed a high density and high strength isotropic carbon block through the oxidation stabilization process of mesocarbon microbeads (MCMBs) prepared from coal tar pitch, and by increasing the aromatic carbon content (aromatic carbon content) The present invention has been completed by suppressing the swelling phenomenon and establishing an optimum condition for adjusting the low molecular weight volatilization rate in the carbonization process to improve mechanical properties.

It is an object of the present invention to provide a method for producing high density and high strength isotropic carbon blocks using oxidative stabilization of mesocarbon microbeads prepared from coal tar pitch.

It is another object of the present invention to provide a method for improving the mechanical properties of carbon blocks through oxidation stabilization of mesocarbon microbeads prepared from coal tar pitch.

It is another object of the present invention to provide a high density and high strength isotropic carbon block produced through oxidation stabilization of mesocarbon microbeads prepared from the coal tar pitch.

In order to achieve the above object, the present invention

* 1) heat treating coal tar pitch (CTP) to prepare mesocarbon microbeads (MCMBs);

2) oxidatively stabilizing the mesocarbon microbeads of step 1); And

3) carbonizing the oxidation stabilized mesocarbon microbeads of step 2) to produce a carbonized carbon block (CCB).

The present invention also provides a high-density and high-strength carbon block produced by the manufacturing method according to the present invention.

The present invention can produce an isotropic carbon block of high density and high strength through the oxidation stabilization process of mesocarbon microbeads prepared from coal tar pitch.

The present invention improves the mechanical properties of the carbonized carbon block by controlling the volatilization rate of the low molecular weight in the carbonization process by increasing the aromatic carbon content (aromatic carbon content) by using the oxidation stabilization process of mesocarbon microbeads You can.

1 is a graph showing a TG weight loss curve of coal tar pitch (CTP).
2 is a diagram illustrating a production flow of carbon blocks from MCMB.
3 is a schematic diagram of an apparatus for heat treatment and oxidation stabilization: (1) an air gas system; (2) nitrogen gas systems; (3) a gas injection line; (4) gas discharge lines; (5) water traps; (6) effluent storage; (7) thermocouples; (8) temperature controllers; (9) coal tar pitch; (10) heating coils; (11) reactor.
4 is a diagram showing the results of polarized light microscopy analysis of coal tar pitch (CTP) heat treated at different temperatures: (a) 400 ° C .; (b) 430 ° C .; (c) 450 ° C .; (d) 480 ° C .; (d) 500 ° C.
5 is a graph showing the particle diameter of the MCMB prepared at 430 ℃.
6 is a diagram showing an SEM image of MCMB after the extraction process.
7 is a graph showing XPS spectra of Raw MCMB, S-MCMB-200, S-MCMB-250, and S-MCMB-300, respectively.
8 is a graph showing the results of thermogravimetric analysis of raw and stabilized MCMB at 5 ° C./min heating rate and nitrogen atmosphere.
9 is a diagram showing a SEM image of carbon blocks of MCMB treated under different stabilization conditions: (a) Raw MCMBs; (b) 150 ° C .; (c) 200 ° C .; (d) 250 ° C .; (e) 300 ° C.
10 is a diagram showing a model of the sintering mechanism of carbon blocks from MCMB during the carbonization process.

Hereinafter, the present invention will be described in detail.

The present invention provides a process for producing carbon blocks from the production of mesocarbon microbeads from coal tar pitch and through oxidation stabilization.

Specifically, the present invention

1) heat treating coal tar pitch (CTP) to prepare mesocarbon microbeads (MCMBs);

2) oxidatively stabilizing the mesocarbon microbeads of step 1); And

3) carbonizing the oxidatively stabilized mesocarbon microbeads of step 2) to produce a carbonized carbon block (CCB).

In the manufacturing method, the heat treatment of step 1) is preferably heated to 400 ~ 500 ℃, and more preferably to 400 ~ 450 ℃ in a nitrogen atmosphere. This is because the heating temperature is a suitable condition for producing mesocarbon microbeads from heat treated coal tar pitch, and especially for producing uniform micro grains of 75 um or less for producing high density and high strength carbon blocks. . At this time, in the case of the upper limit of the proposed heat treatment range, uniform ultrafine particles of uniform 75 um or less become larger as shown in FIG. 4 to form a single mesoface structure, and in the case of the lower limit of the heat treatment range, the isotropic pitch or the soft pitch is Generated and no ultrafine particles are generated.

In the above method, after the heat treated coal tar pitch of step 1) is mixed with an organic solvent, mesocarbon microbeads may be extracted through vacuum filtration. Here, the organic solvent is preferably tetrahydrofurane (THF), but is not limited thereto. In addition, the extracted mesocarbon microbeads can be washed with toluene or the like.

In the above production method, the oxidation stabilization of the step 2) is preferably heated at 150 ~ 300 ℃, more preferably at 150 ~ 250 ℃ mesocarbon microbeads in an air atmosphere. The heating conditions for the oxidation stabilization are suitable conditions for increasing the aromatic carbon content, suppressing the expansion phenomenon, and reducing the volatilization rate of the low molecular weight of the carbonization process for producing high density and high strength carbon blocks. At this time, in the case of the upper limit of the stabilization conditions presented, as shown in Fig. 9, small cracks are generated on the surface of the carbon block and the mechanical properties are reduced.

In the manufacturing method, the heat treatment and oxidation stabilization of step 1) and step 2), the air gas system for supplying air to the reactor; A nitrogen gas system for supplying nitrogen to the reactor; A gas injection line connected to each reactor from the supply gas system and the nitrogen gas system to inject gas into the reactor; A gas discharge line connected to the effluent reservoir from the reactor to discharge gas of the reactor; And a reactor capable of heating.

The heat treatment and oxidation stabilization device is connected to the gas discharge line effluent storage unit for storing the effluent discharged; A water trap connected to the effluent reservoir to capture gas; A thermocouple connected to the reactor for measuring temperature; And a temperature controller connected to the reactor and the thermocouple to control the temperature.

In the manufacturing method, after step 2) may further comprise the step of sorting or molding the oxidized stabilized mesocarbon microbeads.

In the production method, the carbonization of the step 3) is preferably heated at 850 ~ 1200 ℃ in a nitrogen atmosphere, it is more preferable to carbonize by increasing the heating temperature step by step.

In one embodiment of the present invention, mesocarbon microbeads were prepared from coal tar pitch and subjected to oxidation stabilization at different temperatures, and then the oxygen content of the mesocarbon microbeads was analyzed by elemental analysis (EA) and X-ray photoelectron spectroscopy (XPS). The carbon blocks carbonized at 1200 ° C. were analyzed for morphological and mechanical properties. As a result, it was confirmed that as the temperature of oxidative stabilization increased, the oxygen content increased and the physical properties of the carbonized carbon blocks were significantly improved through oxidative stabilization. In particular, as the oxygen content increased, small cracks were observed between mesocarbon microbead particles, and the expansion phenomenon was dependent on the weight loss from 30 ° C to 600 ° C when carbonizing, and the flexural strength was from 30 ° C to 600 ° C during carbonization. It was confirmed that the weight loss of the affected by. Thus, it was confirmed that carbonized carbon blocks derived from mesocarbon microbeads which were oxidatively stabilized at about 200 ° C. for 1 hour exhibited optimum mechanical properties and high density.

The present invention also provides a high-density and high-strength carbon block produced by the manufacturing method according to the present invention.

The carbon block preferably has a density of 1.3 to 1.6 g / cm ³ , a Shore hardness of 85 to 95 HS, and a flexural strength of 40 to 120 Mpa.

Hereinafter, the present invention will be described in detail by Examples and Comparative Examples.

However, the following Examples and Comparative Examples are merely illustrative of the present invention, the contents of the present invention is not limited to the following Examples and Comparative Examples.

Example 1 Preparation of Mesocarbon Microbeads from Coal Tar Pitch

Coal tar pitch (CTP) (OCI Company Ltd.) was used as the raw material. The characteristics of the coal tar pitch used are shown in Table 1 below. The composition of coal tar pitch was analyzed using elemental analysis (EA, TruSpec, LECO Corp., USA), and toluene insoluble (TI) and quinolinol insoluble (QI) were determined in ASTM D-4072 and ASTM D-2318 standards. Decided accordingly. Thermal behavior of CTP was performed at 900 ° C. at a heating rate of 5 ° C./min in nitrogen flow using a thermal flow assay (TGA, STA 409 PC, Netzsch Corp., Germany). Elemental analysis of coal tar pitch (EA) showed 93.50% carbon, 4.49% hydrogen, 1.34% nitrogen, 0.46% sulfur, and solubility analysis showed 9.7% quinoline insoluble (QI) and 32.1% toluene insoluble (TI). The carbon yield of CTP was 44.9% at 900 ° C. as shown in FIG. 1.

Characteristics of Coal Tar Pitch Elemental Analysis (wt%) Insolubility Analysis (%) C H N S C / H TI QI 93.5 4.49 1.34 0.46 1.74 32.1 9.7

Coal tar pitch was heated at 400-500 ° C. (performed at 400 ° C., 430 ° C., 450 ° C., 480 ° C. and 500 ° C., respectively) under a nitrogen atmosphere using the reactor shown in FIG. 3. 10 g of heated coal tar pitch was mixed with 100 ml of tetrahydrofurane (THF) at 50 ° C. for 12 hours and extracted by vacuum filtration. In addition, the extracted MCMB was washed twice with toluene at 80 ° C.

Example 2 Oxidation Stabilization of Mesocarbon Microbeads

The oxidation stabilization process of mesocarbon microbeads was performed in the apparatus shown in FIG. 3. In the prepared mesocarbon microbead air atmosphere was heated for 1 hour at 150 ~ 300 ℃ to increase the oxygen content. According to the stabilization process, four kinds of mesocarbon microbeads were prepared at 150 ° C., 200 ° C., 250 ° C. and 300 ° C., respectively, and S-MCMB-150, S-MCMB-200, S-MCMB-250 and S-MCMB-, respectively. It was specified as 300.

Example 3 Preparation of Carbon Blocks from Mesocarbon Microbeads

Raw mesocarbon microbeads and stabilized mesocarbon microbeads were classified into sieves of 75 um (200 mesh) or less, respectively. In addition, untreated mesocarbon microbeads and stabilized mesocarbon microbeads were molded without binder below 28 Mpa by cold compression into two disks of 15 x 15 x 3 mm and 60 x 10 x 3 mm. The green carbon block was carbonized at 1200 ° C. for 1 hour at a heating rate of 1 ° C./min in a nitrogen atmosphere. Thus, two kinds of carbonized carbon blocks (CCBs) were produced from mesocarbon microbeads.

Experimental Example 1 Surface and Particle Size Analysis of the Prepared MCMB

Polarization microscopy analysis was performed using polarization microscopy (PLM, BX51M, Olympus Corp., Japan) on coal tar pitch heat treated at five different temperatures.

As a result, as shown in FIG. 4, the heat treated coal tar pitch formed mesophase. As the heat treatment temperature rose, the mesophase shape was clearly seen. Mesophase initiation started from coal tar pitch heat-treated at 400 ° C and complete mesophase at temperatures above 480 ° C. In particular, mesocarbon microbeads were observed for the coal tar pitch heat-treated between 400 and 450 ° C. To produce high density and high strength carbon blocks, uniform micro grains of 75 μm or less appeared under heat treatment conditions of 430 ° C. (FIG. 4).

In addition, particle diameters were investigated using polarized light microscopes for coal tar pitches heat treated at five different temperatures. To analyze the average particle diameter, about 400 mesophase spherules prepared at 430 ° C. were measured using a polarization microscope.

As a result, as shown in Figure 5, all mesophase globules were 40 um or less in size, the average particle size was found to be 13.53 um (Fig. 5).

In addition, surface images were observed using a scanning electron microscope (SEM, JSM-6700F, JEOL Ltd., Japan) for mesocarbon microbeads extracted from coal tar pitch heat-treated at 430 ° C.

As a result, as shown in FIG. 6, the mesocarbon microbeads were reconfirmed to have a rough surface and a uniform size of about 14 um (FIG. 6).

Experimental Example 2 Characterization of MCMB According to Oxidation Stabilization

Compositions were analyzed using elemental analysis (EA, TruSpec, LECO Corp., USA) for raw mesocarbon microbeads and stabilized mesocarbon microbeads.

Elemental Analysis of MCMB According to Stabilization Conditions Sample Elemental Analysis (wt%) Element ratio C H N Other C / H Raw MCMB 96.15 2.17 1.32 0.36 3.69 S-MCMB-150 95.17 3.13 1.05 0.65 2.53 S-MCMB-200 94.10 3.34 0.78 1.78 2.35 S-MCMB-250 92.80 2.79 0.84 3.57 2.77 S-MCMB-300 91.83 2.59 1.14 4.44 2.95

As a result, as the stabilization temperature increased, the carbon ratio decreased and the Others ratio increased. And since the other element of the ratio is the oxygen content, the oxygen content also increased as the stabilization temperature increased. The hydrogen ratio was shown to decrease rapidly from the stabilization temperature above 200 ℃. The C / H ratios of Raw MCMBs, S-MCMBs-200, and S-MCMBs-300 were 3.69, 2.35, and 2.95, respectively. This means that the aromaticity rate is lowered and increased from the stabilization temperature of 200 ° C.

In addition, the oxygen content according to the oxidation stabilization temperature was analyzed by X-ray photoelectron spectroscopy (XPS, AXIS-NOVA, Kratos Inc., Japan).

As a result, as shown in FIG. 7, the five functional groups analyzed were 530.6, 532.4, 533.8, 534.3, 563.3, and C = O, CO, OC = O, C-OH, H ₂ O, respectively. (Chemosorbed O ₂ or adsorbed H ₂ O) were analyzed. As the temperature of oxidative stabilization increased, the functional groups of C═O and OC═O increased and H ₂ O was removed. The content of C-OH was high in S-MCMBs-200. Through this, it is determined that the hydrogen ratio of Table 2 increases and decreases from the stabilization temperature of 200 ° C as the -OH functional group is generated.

Experimental Example 3 Analysis of Morphology and Mechanical Properties of Carbonized Carbon Blocks

Thermogravimetric analysis was performed under a nitrogen atmosphere at a heating rate of 5 ° C./min for Raw mesocarbon microbeads and stabilized mesocarbon microbeads.

As a result, as shown in FIG. 8, three sections are shown based on the point where the weight loss ratio changes. The fixed carbon of S-MCMBs-150 and S-MCMBs-200 is about 0.3%, and the fixed carbon of S-MCMBs-250 and S-MCMBs-300 is about 1.6% than raw MCMB. Increased. The weight loss ratios of the three sections are shown in Table 3 below.

Weight reduction ratio of carbonized carbon blocks derived from mesocarbon microbeads Sample % Weight loss Overall weight reduction At 30 ℃
Up to 600 ℃ At 600 ℃
Up to 850 ℃ At 850 ℃
Up to 1200 ℃ Raw MCMB 10.35 7.23 2.47 0.65 S-MCMB-150 10.31 7.43 2.39 0.4 S-MCMB-200 10.33 5.93 3.68 0.72 S-MCMB-250 11.17 5.07 3.65 2.45 S-MCMB-300 11.76 4.05 4.52 3.20

In the volatile materials corresponding to the weight loss of 30 ° C to 600 ° C, raw MCMBs and S-MCMBs-150 showed the largest values. The volatile material corresponding to the weight loss of 850 ° C. to 1200 ° C. showed the largest value of S-MCMBs-300. In addition, morphological analysis of carbonized carbon blocks according to stabilization process conditions was performed by observing the surface image of the carbonized carbon blocks using a scanning electron microscope (SEM, JSM-6700F, JEOL Ltd., Japan). It was.

As a result, as shown in Fig. 9 (a, b), a swelling phenomenon was observed. As such, it is judged to be a major factor in the weight loss expansion phenomenon of 30 ° C to 600 ° C. As shown in FIG. 9 (d, e), borderlines were clearly observed between mesocarbon microbead particles. The weight loss from 850 ° C. to 1200 ° C. is reported as the section with the smallest volume shrinkage. Therefore, weight loss of 850 ° C to 1200 ° C is considered to be a major cause of generating small cracks between mesocarbon microbead particles, and is considered to be a major factor for reducing mechanical properties.

In addition, the mechanical properties of the carbonized carbon block according to the stabilization process conditions were analyzed. The density of the carbonized carbon blocks was investigated by Archimedes drainage method. Shore hardness test (SH, Type-D, Kobunshi Keiki, Japan) was measured according to ASTM D-2240 standard. Bending strength was tested using a Universal Testing Machine (UTM, WL2100, WITHLAB Ltd., Korea) according to ASTM C-1161 standard.

Mechanical Properties of Carbonized Carbon Blocks Derived from Mesocarbon Microbeads Sample Shore hardness
(HS) Flexural strength
(Mpa) Volume shrinkage
(%) Bulk density
(g / cm ³ ) S-MCMB-150 90 - 20.22 1.35 S-MCMB-200 94 116 31.51 1.57 S-MCMB-250 85 43 29.78 1.48 S-MCMB-300 85 14 29.54 1.42

As a result, evaluation of the mechanical properties of the carbonized carbon block derived from Raw MCBM was impossible due to the expansion phenomenon as shown in FIG. 9 (a). The flexural strength of S-MCMBs-200 was 116 Mpa and the volume shrinkage was 31.51%. In addition, the density was 1.57 g / cm ³ and S-MCMBs-200 showed the highest value. From these results, the sintering mechanism of the carbonization process is shown in three steps in FIG. The step before carbonization Oxygen contents were indicated according to XPS results. The second step indicated that the volatilization and volumetric contraction of the volatiles was the largest. And the expansion phenomenon of the carbonized carbon block derived from Raw MCBM. The final step was a period of low volume shrinkage, indicating that a weight loss of 850 ° C. to 1200 ° C. produced small cracks.

Claims (11)

1) heat treating and extracting coal tar pitch (CTP) to prepare mesocarbon microbeads (MCMBs);
2) oxidatively stabilizing the mesocarbon microbeads of step 1); And
3) carbonizing the oxidatively stabilized mesocarbon microbeads of step 2) to produce a carbonized carbon block (CCB);
here
The heat treatment of step 1) is heated to 400 ~ 500 ℃ in a nitrogen atmosphere,
In the extraction of step 1), the heat treated coal tar pitch is mixed with an organic solvent, and then MCMBs are extracted through vacuum filtration.
Oxidation stabilization of step 2) is characterized in that to increase the oxygen content by heating the mesocarbon microbead at 150 ~ 250 ℃ in air atmosphere
Carbon block manufacturing method.
delete delete delete delete The method of claim 1,
The heat treatment and oxidation stabilization of step 1) and step 2)
An air gas system for supplying air to the reactor;
A nitrogen gas system for supplying nitrogen to the reactor;
A gas injection line connected to each reactor from the supply gas system and the nitrogen gas system to inject gas into the reactor;
A gas discharge line connected to the effluent reservoir from the reactor to discharge gas of the reactor; And
Method for producing a carbon block, characterized in that carried out using a device comprising a reactor capable of heating.
The method of claim 6,
The device is
An effluent storage unit connected to the gas discharge line to store the effluent discharged;
A water trap connected to the effluent reservoir to capture gas;
A thermocouple connected to the reactor for measuring temperature; And
And a temperature controller connected to the reactor and the thermocouple to adjust the temperature.
The method of claim 1,
After the step 2) further comprises the step of screening or molding the oxidatively stabilized mesocarbon microbeads.
Claim 9 was abandoned upon payment of a set-up fee. The method of claim 1,
The carbonization of step 3) is a carbon block manufacturing method characterized in that the heating at 850 ~ 1200 ℃ in a nitrogen atmosphere.
Made by the manufacturing method of any one of claims 1 and 6 to 9,
Density is 1.3 ~ 1.6 g / cm ³ , Shore hardness is 85 ~ 95 HS, Flexural strength is characterized in that 40 to 120 Mpa
Carbon blocks.
delete

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