JP2004182568A - Porous material - Google Patents

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JP2004182568A
JP2004182568A JP2002354061A JP2002354061A JP2004182568A JP 2004182568 A JP2004182568 A JP 2004182568A JP 2002354061 A JP2002354061 A JP 2002354061A JP 2002354061 A JP2002354061 A JP 2002354061A JP 2004182568 A JP2004182568 A JP 2004182568A
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Japan
Prior art keywords
porous material
peak
carbon material
carbon
cm
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Pending
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JP2002354061A
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Japanese (ja)
Inventor
Tetsuo Kasai
Toshikatsu Maeda
敏勝 前田
鉄夫 笠井
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Frontier Carbon Corp
フロンティアカーボン株式会社
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Priority to JP2002354061A priority Critical patent/JP2004182568A/en
Publication of JP2004182568A publication Critical patent/JP2004182568A/en
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Abstract

An object of the present invention is to provide a porous material which is a novel porous material and characteristically has a high resistance value, a large total pore volume, and a high micropore volume ratio.
A porous material obtained by activating a carbon material, the carbon material having a diffraction angle of 3 to 30 ° in an X-ray diffraction measurement result using CuKα radiation (wavelength = 1.54 °). A porous material having a strongest peak in the range of 10 to 18 ° within the range and being insoluble in an organic solvent.
[Selection diagram] None

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a novel porous material using a novel carbon material as a raw material, and can be made porous without any particular pretreatment, and the obtained porous body has a large electric resistance and a The present invention relates to a porous material having a large specific volume and a high micropore volume ratio.
[0002]
[Prior art]
Activated carbon, a porous carbon material, has been used extensively in the purification of refined sugar, brewing, medicines, oils and fats, and has been used in large quantities as an agent for controlling pollution such as air pollution, water pollution and odor. It occupies the most important position as an adsorbent for use. Further, in recent years, activated carbon has attracted attention as a functional material, and has also attracted attention in advanced water treatment using the adsorption function, air purification, deodorization, and solvent recovery. These functions are understood by the micropores derived from the micrographite structure, which is the basic structure of conventional carbon materials, and the specific surface area thereof. The relationship between the micrographite structure and the micropores is described in Non-Patent Document 1, for example. In the present application, pores smaller than 20 mm are defined as “micropores”, 20 mm to 500 mm are defined as “mesopores”, and 500 mm or more are defined as “macropores” in accordance with IUPAC recommendations.
[0003]
In particular, application to the field of battery materials and electronic component materials, which focuses on high specific surface areas, has been receiving new attention. Use of an ion removing device provided in a water supply path as a conductive coating on the surface of a porous electrode plate (for example, see Patent Document 1), and use of an ion generating electrode in a charging device using an ion generating device (for example, And Patent Document 2). As is apparent from these uses, the conventional activated carbon has a relatively small electric resistance.
[0004]
On the other hand, a heat-generating panel utilizing heat generated by electric resistance of activated carbon particles is disclosed (for example, see Patent Document 3). However, since conventional activated carbon is used, the upper limit of the heat generation temperature is 60 ° C., and to obtain a higher temperature, activated carbon having higher resistance is required. Further, as an insulator having excellent thermal and electrical properties for use in semiconductors, a heat-resistant insulator resin composition in which activated carbon is combined has been disclosed (for example, see Patent Document 4). However, since the conventional activated carbon is also conductive, the amount of addition is at most 20 wt%. Further, in this application, since it is used as a low dielectric constant material, it is expected that not only the electrical resistance but also the pores must have a sufficient total pore volume.
[0005]
Furthermore, there is a demand for various carbon porous materials suitable for a wide variety of applications. Specifically, it can be easily produced, has few impurities, has a large resistance value, has a large pore volume, and has a micropore volume. There has been a demand for a carbon material having a high ratio.
[0006]
[Non-patent document 1]
Carbon, no. 160, pp. 283-289
[Patent Document 1]
JP 2001-162283 A
[Patent Document 2]
JP 2001-125346 A
[Patent Document 3]
JP-A-2001-176643
[Patent Document 4]
JP-A-2002-245855
[0007]
[Problems to be solved by the invention]
An object of the present invention is to produce a novel porous material by using a novel carbon material as a raw material. This porous material can be easily produced, has few impurities, has a large resistance value, and has a high resistance. It has the property that the pore volume is large and the micropore volume ratio is high.
[0008]
[Means for Solving the Problems]
That is, the gist of the present invention is a porous material obtained by activating a carbon material, wherein the carbon material has a diffraction angle of 3 in X-ray diffraction measurement results using CuKα radiation (wavelength = 1.54 °). The porous material is characterized in that the strongest peak exists in the range of 1830 ° and in the range of 101818 ° and is insoluble in an organic solvent.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, the present invention will be described in detail.
[Description of carbon material]
The carbon material used as a raw material of the porous material of the present invention has a carbon content by elemental analysis of usually 90% by weight or more, preferably 95% by weight or more, more preferably 98% by weight or more. May contain small amounts of functional groups.
[0010]
The carbon material used as a raw material of the porous material of the present invention is insoluble in an organic solvent. In this case, the organic solvent is a liquid having a normal temperature and a boiling point of 100 to 300 ° C., especially 120 to 250 ° C. Specifically, for example, benzene, toluene, xylene, mesitylene, 1-methylnaphthalene, 1,2 And aromatic hydrocarbons such as 3,3,5-tetramethylbenzene, 1,2,4-trimethylbenzene and tetralin. Also, as an insoluble property, at room temperature, 100 volume times of 1,2,4-trimethylbenzene is added to the carbon material, the mixture is stirred, filtered, and then dried at 150 ° C. under vacuum to obtain a weight difference of the carbon material. Is preferably 1% or less.
[0011]
The carbon material used as a raw material of the porous material of the present invention has a completely new internal structure, which is not known in conventional carbon materials. This structure is supported by the fact that the strongest peak exists in the range of 10 to 18 ° in the range of the diffraction angle of 3 to 30 ° in the result of X-ray diffraction measurement using CuKα ray (wavelength = 1.54 °). . The diffraction angle of 10 to 18 ° in the above-mentioned wide-angle X-ray analysis (range of diffraction angle of 3 to 30 °) corresponds to 5 to 9 ° in terms of the lattice spacing d calculated by the following equation (1).
[0012]
(Equation 1)
d = λ / 2 sin θ (λ: X-ray wavelength θ: Bragg angle) (Equation 1)
In the case of a carbon material typified by general carbon black or the like, a diffraction peak due to 002 reflection (lattice plane distance 3.4 °) is observed at a diffraction angle of 26 to 27 ° with the development of a graphite structure. In the carbon material used as the raw material of the present invention, a peak corresponding to the carbon material does not exist, or very little, if any. That is, in the carbon material used as the raw material of the porous material of the present invention, the graphite structure does not exist or very little exists. In this respect, the carbon material used as the raw material of the porous material of the present invention has a structure completely different from a carbon material such as ordinary carbon black.
[0013]
Further, in the carbon material used as a raw material of the porous material of the present invention, even when observed by a transmission electron microscope (TEM), a micro graphite structure confirmed by ordinary carbon black is not substantially observed, and an amorphous structure and a Only a small amount of onion structure is observed. This corresponds to the fact that no peak is observed at 26 to 27 ° in the X-ray diffraction measurement results.
[0014]
Normally, the graphite structure is hardly activated, and the absence of the structure means that pores can be easily formed. Furthermore, the absence of a graphite structure is expected to have the effect of low electrical and thermal conductivity.In fact, a composite in which the carbon material is dispersed in a resin is a general resin composite in which carbon black is dispersed. It shows remarkably low conductivity as compared with.
[0015]
The carbon material used as the raw material of the porous material of the present invention has a band G1590 ± 20 cm in Raman spectrum results at an excitation wavelength of 5145 °. -1 And band D1340 ± 40cm -1 When the peak intensities of the respective bands are I (G) and I (D), the peak intensity ratio I (D) / I (G) is 0.4 to 1.0, particularly 0. It is preferably in the range of 0.4 to 0.8.
[0016]
Here, band G1590 ± 20cm -1 And band G1590 ± 20cm -1 And the peak intensity ratio I (D) / I (G) is in the range of 0.4 to 1.0, which means that a regular graphite material has a relatively regular micro graphite structure. It is understood that there are many. In the case of a conventionally known carbon material, when there are many micrographite structures, 002 reflection is always observed at a diffraction angle of 26 to 27 ° in X-ray diffraction measurement results.
[0017]
However, in the case of the carbon material used as the raw material of the porous material of the present invention, the peak intensity ratio I (D) / I (G) is in the range of 0.4 to 1.0 as described above. Has a specific property that a diffraction peak due to 002 reflection does not exist at a diffraction angle of 26 to 27 ° or is very slight even if present.
Considering this together with the peak at a diffraction angle of 10 to 18 ° in the X-ray diffraction measurement result, it suggests that an ordered structure other than a micro graphite structure exists. If the structure of the carbon material is completely disordered, the structure becomes extremely weak, and it becomes difficult to control not only the pore size distribution but also the activation treatment. However, the existence of some ordered structure is considered to be reflected in the pore distribution and the like.
[0018]
From these facts, by using the carbon material having the above characteristics as a raw material of the porous material of the present invention, the activation treatment can be easily performed, the total pore volume is large, the micropore volume ratio is high, and the conductivity is high. It is believed that a less volatile structure is achieved.
The carbon material used as a raw material of the porous material of the present invention has a specific surface area of 200 m as measured by a nitrogen adsorption method (BET method). 2 / G, and the ratio of the pore volume of 10 ° or less to the pore volume of 300 ° or less (pore volume distribution) is less than 10%, preferably 5% or less. It is suitable as a raw material for obtaining a porous material having a specific pore structure reflecting its internal structure. The lower limit of the specific surface area of the raw material carbon material used for the porous material of the present invention is usually 10 m 2 / G, and the lower limit of the pore volume ratio is usually 0.1%.
[0019]
The porous material of the present invention produced from a novel carbon material having these characteristics as a raw material also has a completely novel internal structure that is not known in conventional carbon materials, reflecting the structure of the raw material. This structure has no peak at a diffraction angle of 26 to 27 ° in the result of X-ray diffraction measurement using CuKα ray (wavelength = 1.54 °), and shows the band G1590 ± in the Raman spectrum result at an excitation wavelength of 5145 °. 20cm -1 And band D1340 ± 40cm -1 When the peak intensities of the respective bands are I (G) and I (D), the peak intensity ratio I (D) / I (G) is 0.4 to 1.0, particularly 0. It is preferably in the range of 0.5 to 0.9.
[0020]
In addition, band G1590 ± 20cm -1 The half width of is 40 ~ 110cm -1 , (Especially 50-100 cm -1 ) Is preferable. The meanings of the I (D) / (G) and the half width are described in, for example, Non-Patent Document 1, page 310, but it should be noted that these also require a graphite structure.
As described above, even in the porous material aimed at by the present invention, the absence of a peak at a diffraction angle of 26 to 27 ° in the X-ray diffraction angle measurement result means that the micrographite structure does not exist or exists. Also means that the micrographite structure is not generated by heating during the activation treatment. That is, since a micrographite structure that is difficult to gasify is not formed in the activation treatment, it is considered that the structure is easy to leave holes, and the structure is low in conductivity.
[0021]
On the other hand, in the Raman spectrum measurement, the peak intensity ratio I (D) / I (G) is 1.0 or less, and the band G1590 ± 20 cm -1 Is usually a result suggesting the existence of a micrographite structure, but the result of X-ray diffraction measurement denies the existence of the micrographite structure. Usually, the two bands in the Raman spectrum measurement are recognized as the micrographite structure (I (G)) and the disorder of the structure (I (D)), while the Raman spectrum of various polycyclic aromatic compounds is recognized. Interpretation of superposition is also proposed. (Carbon, 12 , P266) In particular, when interpreting that the half width is small from this viewpoint, it can be understood that the composition of the specific structure is large. That is, it is conceivable that regularity also appears in the pore structure in order to make the structural components uniform.
[0022]
In the porous material of the present invention, the lower limit of the total pore volume measured by the nitrogen adsorption method is 0.2 cc / g or more, preferably 0.3 cc / g or more, and the upper limit of the total pore volume is 3.0 cc. / G or less, preferably 2.0 cc / g or less, and the specific surface area is 200 to 3000 m 2 / G, preferably 400-2000 m 2 / G, more preferably 600-1700 m 2 / G. If the total pore volume or the specific surface area is too small, the function of utilizing the pores and the surface tends to be insufficient. Conversely, if it is too large, it will lead to a decrease in the overall bulk density, a decrease in the strength as a powder, and the filling rate per volume when actually filling the container and using it, or when compounding with other materials It is not preferable because it leads to a decrease.
[0023]
In the porous material of the present invention, the ratio of micropores measured at a relative pressure of 0.2 corresponding to an approximate pore diameter of 20 ° or less in the pore volume measured by the nitrogen adsorption method is from 0.990 to a relative pressure of 0.990. It is at least 20%, preferably at least 30%, of the total pore volume measured at 0.995. If the ratio of the micropore volume is small, the function of utilizing the pores and the surface tends to be insufficient. The porous material of the present invention is expected to exhibit various functions due to the synergistic effect of the function of the micropores and the special internal structure of the matrix.
[0024]
(Method for producing carbon material)
The carbon material used as a raw material of the porous material of the present invention can be produced by a method generally called a combustion method. That is, the carbon-containing compound is burned in a flame, and the obtained raw material soot is collected from the end of the flame, the inside of the flame, or the inner surface of the burner chamber adhered during the combustion, and subsequently, the collected raw material soot is collected. It can be obtained by extracting and removing the organic solvent-soluble components contained therein, filtering and drying.
[0025]
In this combustion method, it is important to burn under the following specific flame conditions. As a specific device, for example, a (water-cooled) burner for realizing a premixed laminar flame and diffusion flame of a carbon raw material compound such as benzene and an oxidizing gas is installed in a decompression chamber, and the system is evacuated by a vacuum pump. In addition, a device or the like that can continue combustion stably is used.
[0026]
In producing a carbon material used as a raw material of the porous material of the present invention using these devices, it is necessary to appropriately select conditions such as a C / O ratio, a combustion chamber pressure, a diluent concentration, and a gas velocity. is there. Preferred conditions for each are that the C / O ratio is greater than 0.5, substantially in the range of 0.72 to 1.07, and the combustion chamber pressure is substantially 1.60 to 13.35 kPa. And the diluent concentration is in the range of 0-40 mol%. Further, the gas velocity can be further increased on an industrial scale, but is preferably substantially in the range of 14 to 75 cm / sec. As a diluent, a general inert gas can be used, but usually, argon is used.
[0027]
The raw material soot thus obtained contains a novel carbon material used as a raw material of the porous material of the present invention, as well as impurities such as a low-molecular-weight aromatic condensed ring compound. Therefore, it is necessary to perform extraction and washing with an organic solvent as a next step to remove these impurities. The organic solvent used here is not particularly limited as long as it is a solvent in which a low-molecular-weight aromatic condensed ring compound or the like is dissolved, but in general, aromatic hydrocarbons are preferable, and aliphatic hydrocarbons and chlorine are more preferable. Organic solvents such as chlorinated hydrocarbons may be used alone or two or more of them may be used in any ratio.
[0028]
Among them, from the industrial viewpoint, among organic solvents, those having a boiling point of 100 to 300 ° C., particularly 120 to 250 ° C., are suitable as the soluble component extraction and removal solvent among liquids at room temperature. Specifically, for example, aromatic hydrocarbons such as benzene, toluene, xylene, methicylene, 1-methylnaphthalene, 1,2,3,5-tetramethylbenzene, 1,2,4-trimethylbenzene, and tetralin are used. Preferably, 1,2,4-trimethylbenzene is more preferable. These can be used alone or as a mixed solvent of two or more.
[0029]
As the extraction device, a stirring and mixing tank can be suitably used, but basically any device can be used. At the time of extraction, the pressure in the vessel is not particularly limited, and may be carried out at normal pressure. The temperature at the time of extraction is, for example, in the range of 1 to 90 ° C., preferably 15 to 40 ° C., and particularly preferably 25 to 35 ° C., from the viewpoint of improving the extraction efficiency. Therefore, it is advantageous to carry out at about room temperature in terms of energy cost. The extraction time may be 1 to 60 minutes, preferably 20 to 40 minutes, but it does not need to be long, and the extraction time has little effect on the extraction efficiency. Further, if necessary, it is preferable to perform extraction while irradiating the extract with ultrasonic waves or the like, because the extraction time is shortened.
[0030]
In addition, the number of extractions can be appropriately selected so that impurities are extracted. Although the amount of the organic solvent can be selected as appropriate, it is preferable that the volume of the organic solvent and the weight of the raw material soot before extraction satisfy the following formula.
The raw material soot weight / organic solvent volume is preferably from 2 to 133 [mg / mL], and more preferably from 33 to 133 [mg / mL]. If the volume of the organic solvent is too large, only the cost is increased. Conversely, if the volume of the organic solvent is too small, the contact between the raw material soot and the organic solvent is not sufficient, and the extraction may not be performed sufficiently.
[0031]
The carbon material which is the raw material of the porous material of the present invention produced by the above method is usually subjected to an activation treatment as it is. 2 Such pressure molding may be performed, and a heat treatment may be performed under the condition of 300 to 1500 ° C., or a pretreatment combining these may be performed. As the activation condition, any method usually used for activated carbon may be used.
[0032]
For example, when zinc chloride is used, a raw material and a high-concentration zinc chloride solution having a specific gravity of about 1.8 are mixed at a ratio of 1: 2 to 1: 3, and then heated to perform an activation treatment. As other chemical activation methods, potassium sulfide, phosphoric acid, alkali metal hydroxide and the like can be used. When the gas activation method is used, an activation treatment under a stream of nitrogen containing 30 to 80%, preferably 40 to 60% of water vapor, or an activation treatment with a carbon dioxide gas, a combustion gas or the like is performed. When used for applications where the contamination of impurities is a problem, the gas activation method, particularly the activation of water vapor and the activation of carbon dioxide gas, are usually preferred. The pressure at the time of activation is usually normal pressure, but it is also possible to carry out pressurization or decompression.
[0033]
In the case of the chemical activation method, a rotary kiln is mainly used as the activation furnace. In the case of the gas activation method, a rotary kiln, a vertical furnace, a multi-stage furnace, a fluidized-bed furnace, or the like is used, but is not limited thereto as long as the furnace can perform uniform treatment.
The activation temperature can be usually from 600 to 1500 ° C, preferably from 700 to 1200 ° C, and more preferably from 800 to 1100 ° C. If the temperature is too low, the reaction time tends to be prolonged. Conversely, if the temperature is too high, the reaction tends to proceed too much and the yield tends to decrease significantly. The reaction time is 5 minutes to 5 hours, preferably 10 minutes to 3 hours, and can be arbitrarily selected depending on the desired degree of the activation treatment.
Further, after the activation treatment, heat treatment may be performed at 600 to 1500 ° C. to remove the remaining functional groups.
[0034]
〔function〕
The porous material of the present invention is expected to have functions such as low conductivity, low heat transfer coefficient, etc. due to its unique internal structure, which does not have a micrographite structure, and has a larger volume and a higher micropore volume. By having a ratio, the possibility of application to electronic component materials as well as ordinary adsorbents is expanded.
[0035]
【Example】
Hereinafter, the present invention will be described specifically with reference to examples. It should be noted that the present invention is not limited to the following examples unless it exceeds the gist. In addition, evaluation of the obtained carbon material and measurement of physical properties were performed as follows.
(1) X-ray diffraction measurement: Philips device PW1700, radiation source: CuKα, output: 40 kV, 30 mA, scanning axis: θ / 2θ, measurement mode: Continuous, measurement range: 2θ = 3 ° to 90 °, capture width: 0.05, scanning speed: 3.0 ° / min.
(2) Raman spectrum: Detected by + Photometrics CCD (512 channels) using an apparatus of NR1800 manufactured by JASCO Corporation. The conditions were as follows: excitation wavelength: 5145 °, excitation output: 5 mW or less, slit width: 400 μm, peak intensity: 1730 to 1165 cm after smoothing (11-point correction) using OMNIC software -1 A linear base line was drawn within the range, and the height to the peak top was defined as the peak intensity. The half-width of the G band peak used the width of the peak at half the height from the baseline to the peak,
(3) Surface area and pore volume: The surface area was determined from a nitrogen adsorption isotherm at a relative pressure of 0.10 to 0.28 using a BET method model using Autosorb 3B manufactured by Canterchrome. The meso-macro pore volume was obtained by analyzing the adsorption isotherm data by the BARRETT-JOYNER-HALENDA method (BJH method), and the micropore was analyzed by the HORVATH-KAWAZOE method (HK method).
(4) Particle Size Measurement by Dynamic Light Scattering: The powder was made into a 0.5 wt% ethanol dispersion, treated with an ultrasonic cleaner for 30 minutes, and then the average dispersed particle size was measured using an Otsuka Electronics FPAH-1000. I asked.
(5) Volume resistance: A sample of a porous material having a thickness of about 1 mm was left in a room at 25 ° C. and 50% RH all day and night, stylus was applied from both sides, and five points were measured.
[0036]
Reference example
Using a device in which a premixed water-cooled burner was installed in a decompression chamber, the inside of the system was evacuated with a vacuum pump, and benzene was premixed with oxygen as a raw material and supplied to the burner to generate a stable laminar flame. The combustion was performed under the conditions of a C / O ratio of 0.995, a combustion chamber pressure of 20 torr, a gas flow rate of 49 cm / sec, and a diluted argon concentration of 10 mol%, and the resulting soot was collected from the top and the wall of the combustion chamber.
[0037]
10.3 g of the collected soot was weighed into a 1-liter volumetric flask, 286.16 g of tetralin was added, and extraction was performed while applying ultrasonic waves at room temperature for 30 minutes with stirring. Thereafter, filtration under reduced pressure was performed with a 0.45 μm filter. After repeating washing and filtration three times with tetralin, drying under reduced pressure at 100 ° C. was carried out all day and night to obtain 9.6 g of a black powder (raw material carbon material). The carbon material was washed with 1 liter of 1,2,4-tetramethylbenzene and dried, but the change in weight was 0.1% or less, and the carbon material was substantially insoluble in the organic solvent. The elemental analysis value of the carbon material was a carbon content of 96 wt% and an oxygen content of 2.6 wt%. Metal impurities were measured for Li, Na, Mg, Si, k, Ca, and Fe, and were all 0.03% or less.
[0038]
In the X-ray diffraction of the carbon material, there is a peak only around the diffraction angle of 14 °, and the graphite peak at 26 ° is very weak, indicating that it is substantially amorphous (see FIG. 1). In the Raman spectrum (see FIG. 2), 1590 cm -1 And 1340cm -1 Large peak at 1460cm -1 There was a small peak. 1590cm -1 Peak intensity I (G) of 10.4, 1340 cm -1 Has a peak intensity I (D) of 6.8 and I (D) / I (G) of 0.65.
[0039]
The surface area of the carbon material is 99 m. 2 / G, the micropore volume at 300 ° or less was about 0.16 cc / g, the micropore volume at 10 ° or less was about 0.002 cc / g, and the true specific gravity was about 1.6 g / cc.
Further, 5 g of BYK182 dispersant and 45 g of propylene glycol methoxy acetate manufactured by BYK Chemie were added to 10 g of the sample, and a dispersion ink was prepared using a zirconia bead using a paint shaker. 15 g of an acrylic acid-based photosensitive resin was added to this ink, mixed well, coated on a glass plate with a doctor knife having a gap of 200 μm, dried, exposed, and measured with a surface resistance measuring instrument. 10 Thirteen Ω · cm.
[0040]
Example 1
0.9 g of the carbon material obtained in Production Reference Example was charged into a mold having a bottom surface of 20 mmφ, and 1 t / cm. 2 Into tablets. The tablets are pulverized in an agate mortar into particles having a diameter of 0.8 to 2 mm, placed in a rotary kiln, heated to 950 ° C. in a nitrogen stream, and then supplied with steam in a nitrogen stream so as to be 55 vol% of steam. For 30 minutes. Yield was 22%.
[0041]
In the X-ray diffraction of the obtained material, broad peaks exist around the diffraction angles of 5.5 ° and 20 °, and no peak is observed around 26 °, indicating that the material is substantially amorphous ( (See FIG. 3). In the Raman spectrum (see FIG. 5), 1590 cm -1 And 1340cm -1 There was a large peak. 1590cm -1 Has a peak intensity I (G) of 3.3, 1340 cm -1 Has a peak intensity I (D) of 2.6, I (D) / I (G) of 0.79, and a half-width of G band of 68 cm. -1 Met.
[0042]
The surface area of the carbon material is 856 m. 2 / G, the total pore volume was 1.03 cc / g, the micropore volume at a nitrogen relative pressure of 0.2 was 0.42 cc / g, and the micropore volume ratio was 41%. The average particle size after the ultrasonic dispersion treatment in ethanol was 220 nm.
When the resistance value of this sample was measured, it was 100 Ω / mm.
[0043]
Example 2
A porous material was produced in the same manner as in Example 1 except that the activation reaction was performed for 45 minutes. The yield was 7%.
In the X-ray diffraction of the porous material, a clear peak exists at a diffraction angle of 5.5 °, a broad peak exists at around 20 °, and no peak is observed at around 26 °. It can be seen that there is (see FIG. 3). In the Raman spectrum (see FIG. 5), 1590 cm -1 And 1340cm -1 There was a large peak. 1590cm -1 Peak intensity I (G) of 2.0, 1340 cm -1 Has a peak intensity I (D) of 1.4, I (D) / I (G) of 0.72, and a half-width of G band of 63 cm. -1 Met.
[0044]
The surface area of the porous material is 431 m. 2 / G, the total pore volume was 0.53 cc / g, the micropore volume at a nitrogen relative pressure of 0.2 was 0.21 cc / g, and the micropore ratio was 40%. The average particle size after the ultrasonic dispersion treatment in ethanol was 174 nm.
Comparative Example 1
FIG. 1 shows an X-ray diffraction measurement result of commercially available carbon black (CF9, manufactured by Mitsubishi Chemical Corporation), and FIG. 2 shows a Raman spectrum result.
[0045]
Comparative Example 2
FIG. 3 shows the results of X-ray diffraction measurement of a commercially available coal-based activated carbon (DIAHOPE008, manufactured by Mitsubishi Chemical Corporation).
Comparative Example 3
When the resistance value of a commercially available coconut shell activated carbon (Diasorb, manufactured by Carbon Tech) was measured, it was 10 Ω · mm.
[0046]
【The invention's effect】
The porous material of the present invention is a novel carbon material, a characteristically high resistance value, a large total pore volume, a carbon material having the property of a high micropore volume ratio, a functional adsorbent, It can be used for various uses such as use for electronic device members, and is extremely useful.
[Brief description of the drawings]
FIG. 1 is an X-ray diffraction chart of Reference Example 1 and Comparative Example 1.
FIG. 2 shows Raman scattering spectra of Reference Example 1 and Comparative Example 1.
FIG. 3 is an X-ray diffraction chart of Examples 1 and 2.
FIG. 4 is an X-ray diffraction chart of Comparative Example 2.
FIG. 5 shows Raman scattering spectra of Examples 1 and 2.
FIG. 6 is a nitrogen adsorption / desorption isotherm of Examples 1 and 2.
FIG. 7 shows mesopore distribution curves obtained by the BJH method in Examples 1 and 2.
FIG. 8 shows a micropore distribution curve by the HK method in Examples 1 and 2.

Claims (7)

  1. A porous material obtained by activating a carbon material, wherein the carbon material has a diffraction angle of 3 to 30 ° in X-ray diffraction measurement results using CuKα radiation (wavelength = 1.54 °). A porous material having a strongest peak in the range of 10 to 18 ° and being insoluble in an organic solvent.
  2. The porous material according to claim 1, which is obtained by activating a carbon material having no peak at a diffraction angle of 26 to 27 °.
  3. The Raman spectrum results at an excitation wavelength of 5145 ° have peaks in band G1590 ± 20 cm −1 and band D1340 ± 40 cm −1 , and the peak intensities of the respective bands are I (G) and I (D). The porous material according to claim 1 or 2, obtained by activating a carbon material having an intensity ratio I (D) / I (G) in a range of 0.4 to 1.0.
  4. Activating a carbon material having a specific surface area measured by a nitrogen adsorption method of less than 200 m 2 / g and a ratio of a pore volume of a diameter of 10 ° or less to a pore volume of a diameter of 300 ° or less less than 10%. The obtained porous material according to any one of claims 1 to 3.
  5. The porous material has no peak at a diffraction angle of 26 ° to 27 ° in the result of X-ray diffraction measurement using CuKα ray (wavelength = 1.54 °), and the Raman spectrum result at an excitation wavelength of 5145 ° indicates band G1590 ±. It has a peak at 20 cm −1 and a band D1340 ± 40 cm −1 , and when the peak intensities of the respective bands are I (G) and I (D), the peak intensity ratio I (D) / I (G) is 0. The porous material according to any one of claims 1 to 4, which has a range of 0.4 to 1.0.
  6. Porous material, in the Raman spectrum result of an excitation wavelength 5145 Å, the half-width of the band G1590 ± 20cm -1 is 40~110Cm -1, porous material according to any one of claims 1 to 5.
  7. Porous material, the total pore volume as measured by nitrogen adsorption method is 0.2cc / g~3.0cc / g, specific surface area of 200~3000M 2, to any one of claims 1 to 6 A porous material as described.
JP2002354061A 2002-12-05 2002-12-05 Porous material Pending JP2004182568A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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GB2410023A (en) * 2004-01-14 2005-07-20 Frontier Carbon Corp Carbon material and process for producing the same
JP2005347517A (en) * 2004-06-03 2005-12-15 Nisshinbo Ind Inc Method of manufacturing activated charcoal for electric double layer capacitor electrode
JPWO2006022329A1 (en) * 2004-08-26 2008-05-08 クラレケミカル株式会社 Transpiration fuel gas adsorbent, transpiration fuel gas collector, activated carbon and method for producing the same
JP2008181950A (en) * 2007-01-23 2008-08-07 Hitachi Chem Co Ltd Electrode material for electric double-layer capacitor, production process and electric double-layer capacitor therefor
WO2016013619A1 (en) * 2014-07-25 2016-01-28 関西熱化学株式会社 Activated carbon with excellent adsorption performance and process for producing same

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2410023A (en) * 2004-01-14 2005-07-20 Frontier Carbon Corp Carbon material and process for producing the same
GB2410023B (en) * 2004-01-14 2008-11-19 Frontier Carbon Corp Carbon material and process for producing the same
JP2005347517A (en) * 2004-06-03 2005-12-15 Nisshinbo Ind Inc Method of manufacturing activated charcoal for electric double layer capacitor electrode
JPWO2006022329A1 (en) * 2004-08-26 2008-05-08 クラレケミカル株式会社 Transpiration fuel gas adsorbent, transpiration fuel gas collector, activated carbon and method for producing the same
JP2008181950A (en) * 2007-01-23 2008-08-07 Hitachi Chem Co Ltd Electrode material for electric double-layer capacitor, production process and electric double-layer capacitor therefor
WO2016013619A1 (en) * 2014-07-25 2016-01-28 関西熱化学株式会社 Activated carbon with excellent adsorption performance and process for producing same
US10105680B2 (en) 2014-07-25 2018-10-23 Kansai Coke And Chemicals Co., Ltd. Activated carbon with excellent adsorption performance and process for producing same

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