JP2017081799A - Porous carbon and organic halogen compound removal device using same - Google Patents
Porous carbon and organic halogen compound removal device using same Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
Abstract
Description
本発明は、多孔質炭素、及びそれを用いた有機ハロゲン化合物除去装置に関する。 The present invention relates to porous carbon and an organic halogen compound removing apparatus using the same.
活性炭に代表される多孔質炭素は、吸着性能に優れているため従来から悪臭の除去、液中の不純物除去、溶剤蒸気の回収、除去などの各種用途に広く使用されている。特に、水を浄化するための浄水器には、活性炭が使用されている（例えば、特許文献１及び２参照）。
しかし、一般的に使用されるヤシ殻活性炭では、有機ハロゲン化合物等の低分子量化合物を十分に吸着させることは困難であった。
また、このような従来の浄水器にあっては、通液倍率が大きいと、即ち、浄水器中を流れる水の総量が大きくなると、浄水機能を十分に発揮できない場合があるといった問題があった。
そこで、有機ハロゲン化合物等の低分子量化合物の吸着性能に優れ、かつ通液倍率が大きい場合でも吸着性能の低下が生じにくい浄水器に使用可能な多孔質炭素の提供が望まれていた。
Since porous carbon typified by activated carbon is excellent in adsorption performance, it has been widely used for various purposes such as removal of malodor, removal of impurities in liquid, recovery and removal of solvent vapor, and the like. In particular, activated carbon is used in a water purifier for purifying water (see, for example, Patent Documents 1 and 2).
However, generally used coconut shell activated carbon is difficult to sufficiently adsorb low molecular weight compounds such as organic halogen compounds.
In addition, in such a conventional water purifier, there is a problem that when the liquid passing ratio is large, that is, when the total amount of water flowing in the water purifier increases, the water purifying function may not be sufficiently exhibited. .
Therefore, it has been desired to provide porous carbon that can be used in a water purifier that is excellent in the adsorption performance of low molecular weight compounds such as organic halogen compounds and that does not easily deteriorate the adsorption performance even when the liquid flow rate is large.
本発明は、従来における前記諸問題を解決し、以下の目的を達成することを課題とする。
即ち、本発明は、有機ハロゲン化合物等の低分子量化合物の吸着性能に優れ、かつ通液倍率が大きい場合でも吸着性能の低下が生じにくい多孔質炭素を提供することを目的とする。
An object of the present invention is to solve the above-described problems and achieve the following objects.
That is, an object of the present invention is to provide porous carbon that is excellent in the adsorption performance of a low molecular weight compound such as an organic halogen compound, and that hardly deteriorates the adsorption performance even when the liquid passing ratio is large.
前記課題を解決するための手段としては、以下の通りである。即ち、
＜１＞ メソ孔容積が０．０７（ｃｍ３／ｇ）以上で、細孔径０．４ｎｍ〜０．６ｎｍの最大微分容積値が１．６以上であることを特徴とする多孔質炭素である。
＜２＞ 前記多孔質炭素の窒素ＢＥＴ法による比表面積が１０（ｍ２／ｇ）以上である前記＜１＞に記載の多孔質炭素である。
＜３＞ 前記多孔質炭素の全細孔容積が０．５（ｃｍ３／ｇ）以上である前記＜１＞から＜２＞のいずれかに記載の多孔質炭素である。
＜４＞ 前記多孔質炭素の一次粒子の粒子径が０．４２５（ｍｍ）以下である前記＜１＞から＜３＞のいずれかに記載の多孔質炭素である。
＜５＞ 前記多孔質炭素のマイクロ孔容積が０．５（ｃｍ３／ｇ）以上である前記＜１＞から＜４＞のいずれかに記載の多孔質炭素である。
＜６＞ 前記多孔質炭素の一次粒子の粒子径が０．１（ｍｍ）以下である前記＜４＞から＜５＞のいずれかに記載の多孔質炭素である。
＜７＞ 前記多孔質炭素の原材料が植物由来の材料からなる前記＜１＞から＜６＞のいずれかに記載の多孔質炭素である。
＜８＞ 前記植物由来の材料がイネ科タケ類由来の材料である前記＜７＞に記載の多孔質炭素である。
＜９＞ 前記イネ科タケ類が孟宗竹である前記＜８＞に記載の多孔質炭素である。
＜１０＞ 前記＜１＞から＜９＞のいずれかに記載の多孔質炭素からなるフィルターを有することを特徴とする、有機ハロゲン化合物除去装置である。
＜１１＞ 有機ハロゲン化合物が濃度０．０６ｍｇ／Ｌで含有された水に対し、通液倍率１，０００倍で有機ハロゲン化合物を除去した場合、有機ハロゲン化合物の除去率が９０％以上である前記＜１０＞に記載の有機ハロゲン化合物除去装置。
＜１２＞ 有機ハロゲン化合物が濃度０．０６ｍｇ／Ｌで含有された水に対し、通液倍率３，０００倍で有機ハロゲン化合物を除去した場合、有機ハロゲン化合物の除去率が６５％以上である前記＜１０＞から＜１１＞のいずれかに記載の有機ハロゲン化合物除去装置である。
＜１３＞ 有機ハロゲン化合物が濃度０．０６ｍｇ／Ｌで含有された水に対し、通液倍率６，０００倍での有機ハロゲン化合物を除去した場合、有機ハロゲン化合物の除去率が５０％以上である前記＜１０＞から＜１２＞のいずれかに記載の有機ハロゲン化合物除去装置である。
＜１４＞ 前記有機ハロゲン化合物がクロロホルムである前記＜１１＞から＜１３＞のいずれかに記載の有機ハロゲン化合物除去装置である。
Means for solving the problems are as follows. That is,
<1> A porous carbon having a mesopore volume of 0.07 (cm 3 / g) or more and a maximum differential volume value of pore diameters of 0.4 nm to 0.6 nm of 1.6 or more. .
<2> The porous carbon according to <1>, wherein the porous carbon has a specific surface area of 10 (m 2 / g) or more according to a nitrogen BET method.
<3> The porous carbon according to any one of <1> to <2>, wherein the total pore volume of the porous carbon is 0.5 (cm 3 / g) or more.
<4> The porous carbon according to any one of <1> to <3>, wherein a particle diameter of primary particles of the porous carbon is 0.425 (mm) or less.
<5> The porous carbon according to any one of <1> to <4>, wherein a micropore volume of the porous carbon is 0.5 (cm 3 / g) or more.
<6> The porous carbon according to any one of <4> to <5>, wherein a particle diameter of primary particles of the porous carbon is 0.1 (mm) or less.
<7> The porous carbon according to any one of <1> to <6>, wherein the raw material of the porous carbon is a plant-derived material.
<8> The porous carbon according to <7>, wherein the plant-derived material is a material derived from a grass family bamboo.
<9> The porous carbon according to the above <8>, wherein the Gramineae bamboo is Miso bamboo.
<10> An organic halogen compound removing device comprising a filter made of the porous carbon according to any one of <1> to <9>.
<11> The removal rate of the organic halogen compound is 90% or more when the organic halogen compound is removed at a flow rate of 1,000 times with respect to water containing the organic halogen compound at a concentration of 0.06 mg / L. <10> The organohalogen compound removing apparatus according to <10>.
<12> When the organic halogen compound is removed at a flow rate of 3,000 times with respect to water containing the organic halogen compound at a concentration of 0.06 mg / L, the removal rate of the organic halogen compound is 65% or more. <10> to <11>. The organic halogen compound removing device according to any one of <11>.
<13> When the organic halogen compound is removed at a flow rate of 6,000 times with respect to water containing the organic halogen compound at a concentration of 0.06 mg / L, the removal rate of the organic halogen compound is 50% or more. The organic halogen compound removing apparatus according to any one of <10> to <12>.
<14> The organic halogen compound removing apparatus according to any one of <11> to <13>, wherein the organic halogen compound is chloroform.
本発明によれば、従来における前記諸問題を解決し、前記目的を達成することができ、有機ハロゲン化合物等の低分子量化合物の吸着性能に優れ、かつ通液倍率が大きい場合でも吸着性能の低下が生じにくい多孔質炭素を提供することができる。 According to the present invention, the conventional problems can be solved, the object can be achieved, the adsorption performance of a low molecular weight compound such as an organic halogen compound is excellent, and the adsorption performance is reduced even when the liquid passing ratio is large. It is possible to provide porous carbon that is less prone to cause the occurrence of carbon dioxide.
（多孔質炭素）
本発明の多孔質炭素は、メソ孔容積が０．０７（ｃｍ３／ｇ）以上で、細孔径０．４ｎｍ〜０．６ｎｍの最大微分容積値が１．６以上である。
本発明者らは、上記特性を有する多孔質炭素が、有機ハロゲン化合物等の低分子量化合物の吸着性能に優れ、かつ通液倍率が大きい場合でも吸着性能の低下が生じにくいことを見出した。
本発明の多孔質炭素は、細孔（ポア）を多く有している。細孔は、メソ孔、マイクロ孔、マクロ孔に分類される。ここで、メソ孔は孔径が２ｎｍ〜５０ｎｍの細孔をいい、マイクロ孔は孔径が２ｎｍよりも小さい細孔をいい、マクロ孔は孔径が５０ｎｍよりも大きい細孔をいう。
マクロ孔は、不純物を含む水や空気等の通り道となってメソ孔・マイクロ孔へ導き、吸着させる機能があるため、ある程度の容積があったほうがよい。しかし多過ぎると低分子量物質の吸着には不利となる。マイクロ孔は、低分子量物質の吸着には有効であるが、特に通液倍率が大きいときには、吸着性能が低下する傾向がある。一方、メソ孔容積が大きいと低分子量物質を効率良く吸着可能であり、かつ通液倍率がある程度大きくても吸着性能力が低下しにくい。さらに、細孔径０．４ｎｍ〜０．６ｎｍの最大微分容積値が１．６以上であると、特に低分子量物質を効率良く吸着可能となる。そこで、上記特性を有する多孔質炭素は、有機ハロゲン化合物等の低分子量化合物の吸着性能に優れ、通液倍率が大きい場合でも吸着性能が低下せず、いずれの効果も満足することができる。
(Porous carbon)
The porous carbon of the present invention has a mesopore volume of 0.07 (cm 3 / g) or more and a maximum differential volume value of pore diameters of 0.4 nm to 0.6 nm of 1.6 or more.
The present inventors have found that porous carbon having the above characteristics is excellent in adsorption performance for low molecular weight compounds such as organic halogen compounds, and that the adsorption performance is hardly lowered even when the liquid flow rate is large.
The porous carbon of the present invention has many pores. The pores are classified into mesopores, micropores, and macropores. Here, the mesopore refers to a pore having a pore diameter of 2 nm to 50 nm, the micropore refers to a pore having a pore diameter smaller than 2 nm, and the macropore refers to a pore having a pore diameter larger than 50 nm.
The macropores should have a certain volume because they have a function to guide and adsorb to the mesopores / micropores as a passage for water or air containing impurities. However, too much is disadvantageous for adsorption of low molecular weight substances. The micropores are effective for the adsorption of a low molecular weight substance, but the adsorption performance tends to decrease particularly when the liquid flow rate is large. On the other hand, when the mesopore volume is large, a low molecular weight substance can be adsorbed efficiently, and the adsorptive capacity is not easily lowered even if the liquid passing ratio is somewhat large. Furthermore, when the maximum differential volume value with a pore diameter of 0.4 nm to 0.6 nm is 1.6 or more, a low molecular weight substance can be adsorbed particularly efficiently. Therefore, porous carbon having the above characteristics is excellent in the adsorption performance of low molecular weight compounds such as organic halogen compounds, and even when the liquid passage ratio is large, the adsorption performance does not decrease, and any effect can be satisfied.
＜本発明の多孔質炭素の特性＞
さらに良好な吸着性能を確保するため、前記多孔質炭素は以下の特性を有することが好ましい。
前記多孔質炭素における窒素ＢＥＴ法による比表面積は、１０（ｍ２／ｇ）以上であることが好ましい。
前記多孔質炭素における全細孔容積は、０．５（ｃｍ３／ｇ）以上であることが好ましい。
前記多孔質炭素の一次粒子の粒子径は、０．４２５（ｍｍ）以下であることが好ましく、０．１（ｍｍ）以下であることがより好ましい。細孔と不純物を含む水や空気等とが接触しやすくするためには、一次粒子の粒子径が０．４２５（ｍｍ）以下であることが望ましい。尚、前記多孔質炭素の一次粒子は、二次凝集されていてもよく、さらに性能を低下させない程度であれば、前記多孔質炭素は顆粒状やチップ状に成型されていてもよい。
さらにマイクロ孔容積が大きいほうが本発明の目的とする低分子物質の吸着には有効であることから、前記多孔質炭素のマイクロ孔容積は、０．５（ｃｍ３／ｇ）以上であることが好ましい。
<Characteristics of porous carbon of the present invention>
In order to secure better adsorption performance, the porous carbon preferably has the following characteristics.
The specific surface area of the porous carbon by the nitrogen BET method is preferably 10 (m 2 / g) or more.
The total pore volume in the porous carbon is preferably 0.5 (cm 3 / g) or more.
The particle diameter of the primary particles of the porous carbon is preferably 0.425 (mm) or less, and more preferably 0.1 (mm) or less. In order to facilitate contact between the pores and water or air containing impurities, it is desirable that the primary particles have a particle size of 0.425 (mm) or less. The primary particles of the porous carbon may be secondary agglomerated, and the porous carbon may be formed into granules or chips as long as the performance is not deteriorated.
Furthermore, since the larger micropore volume is effective for the adsorption of the low-molecular substance targeted by the present invention, the micropore volume of the porous carbon may be 0.5 (cm 3 / g) or more. preferable.
＜特性の測定方法＞
前記多孔質炭素の特性は、例えば、以下の装置を使用して測定することができる。
マイクロメリテックスジャパン合同会社製の３ＦＬＥＸを使用して、窒素吸着等温線を測定し、比表面積はＢＥＴ法で、全細孔容積は一点吸着法で、メソ孔容積はＢＪＨ法で、マイクロ孔容積はＨＫ法で、マイクロ孔領域の細孔分布はＤＦＴ法で、それぞれ算出することができる。またＤＦＴ法によりマイクロ孔領域の細孔分布を求め、細孔径０．４ｎｍ〜０．６ｎｍの最大微分容積値を算出することができる。
［具体的な測定方法］
炭化処理及び賦活処理をした多孔質炭素を３０ｍｇ用意し、相対圧（Ｐ／Ｐ０）０．００００００１から０．９９５の範囲を測定する条件に設定した３ＦＬＥＸを使用して、比表面積、全細孔容積、メソ孔容積、マイクロ孔容積、マイクロ孔領域の細孔分布を測定することができる。
また、前記多孔質炭素の一次粒子の粒子径は、レーザ回折／散乱式粒子径分布測定装置ＬＡ−９５０（ＨＯＲＩＢＡ社製）を使用することにより求めることができる。ＬＡ−９５０を用いて、湿式法により粒子径０．０１μｍ〜３，０００μｍの範囲で粒子径分布を測定する。前記多孔質炭素の一次粒子の粒子径とは、横軸を粒子径、縦軸を個数頻度でプロットした粒子径分布において、分布の中央値に対応した粒子径（メジアン径）をいう。
<Method for measuring characteristics>
The characteristics of the porous carbon can be measured using, for example, the following apparatus.
Nitrogen adsorption isotherm was measured using 3FLEX manufactured by Micromeritex Japan LLC. Specific surface area was BET method, total pore volume was single point adsorption method, mesopore volume was BJH method, micropore volume Can be calculated by the HK method, and the pore distribution in the micropore region can be calculated by the DFT method. Further, the pore distribution in the micropore region can be obtained by the DFT method, and the maximum differential volume value with a pore diameter of 0.4 nm to 0.6 nm can be calculated.
[Specific measurement method]
30 mg of porous carbon that has been carbonized and activated is prepared, and the specific surface area, total pores are measured using 3FLEX set to the conditions for measuring the relative pressure (P / P0) in the range of 0.0000001 to 0.995. The pore distribution in the volume, mesopore volume, micropore volume, and micropore region can be measured.
Moreover, the particle diameter of the primary particle | grains of the said porous carbon can be calculated | required by using the laser diffraction / scattering type particle size distribution measuring apparatus LA-950 (made by HORIBA). Using LA-950, the particle size distribution is measured in the range of particle size 0.01 μm to 3,000 μm by a wet method. The particle diameter of the primary particles of the porous carbon refers to a particle diameter (median diameter) corresponding to a median value of the distribution in a particle diameter distribution in which the horizontal axis represents the particle diameter and the vertical axis represents the number frequency.
＜多孔質炭素の材料＞
前記多孔質炭素の原材料は、植物由来の材料であることが好ましい。植物由来であると、メソ孔やマイクロ孔の容積値を上記所望の値に調整することが容易となる。また、環境負荷が少ない点でも、植物由来とする利点がある。
前記植物由来の材料としては、特に制限はなく、目的に応じて適宜選択することができるが、イネ科タケ類由来の材料であることがより好ましい。
前記イネ科タケ類としては、具体的に、マダケ属（モウソウチク）、オカメザサ属、シホウチク属、ナリヒラダケ属（リクチュウダケ、ナリヒラダケ、クマナリヒラ、メダラナリヒラ、ヒメヤシャダケ、ビゼンナリヒラ、ケナシナリヒラ、ヤシャダケ、ニッコウナリヒラ、アオナリヒラ）、トウチク属（トウチク）、ヤダケ属（ヤクシマダケ、ヤダケ、メンヤダケ、ラッキョウヤダケ）、アズマザサ属（レイコシノ、ジョウボウザサ、ゲンケイチク、ナンブシノ、マエザワザサ、スエコザサ）、クマザサ属（キタミコザサ、ミヤマスズ、ゲイビクマザサ、ロッコウミヤマザサ、ヤマトザサ、ヨナイザサ、クザカイザサ、キンタイザサ、シャコタンチク、フシブトザサ、タナハシザサ、ヤリクマソザサ、ゴテンバザサ、ハツロウザサ、オオシダザサ、ヒメカミザサ、ナンブスズ、フシゲヒメカミザサ、カンサイザサ、ミヤマクマザサ、タンザワザサ、アリマコスズイヌスズ、スズダケ、クマスズハンゲスズ、ケスズ、キンタイチシマ、ネマガリダケ）、カンチク属、メダケ属（リュウキュチク、カンザンチク、タイミンチク、メダケハガワリメダケ、スダレヨシゴキダケ、ボウシュウネザサ、アズマネザサ、ジョウホウジダケ、オロシマチク、ケネザサ）、バンブーサー属（ソルニー・バンブー）、シチク属、ホウライチク属（ホウライチク、シュチク、ダウサンチク）などが挙げられる。
中でも、前記イネ科タケ類がマダケ属のモウソウチク（孟宗竹）であるとより好ましい。
モウソウチクを原材料に使用した多孔質炭素は、特にメソ孔の調整が容易である。
<Porous carbon material>
The raw material of the porous carbon is preferably a plant-derived material. When it is derived from a plant, it becomes easy to adjust the volume value of mesopores and micropores to the desired value. Moreover, there exists an advantage derived from a plant also at a point with little environmental impact.
There is no restriction | limiting in particular as said plant-derived material, Although it can select suitably according to the objective, It is more preferable that it is a material derived from Gramineae bamboo.
Specific examples of the genus Bambooaceae include the genus Mushroom (Mosouchiku), the genus Omezasa, the genus Shihochiku, the Narihirada (Rikuchudake, Narihiratake, Kumanarihira, Medalanahirahira, Himeya-shadake, Bizenarihirahi, Shashinahirahira, Shashinahirahira, Tochiku (Tochiku), Yadatake (Yakushimadake, Yadake, Menyadake, Rakkyo Yadatake), Azumazasa (Reikoshino, Drosophila), Genkichiku, Nambushino, Maezawazaza, Sumazazaza, Sasayamazazamu, Sasayamazaza, Yasami-zazaza, Sami-zasamaza , Yonizasa, Kuzakaizasa, Kintaizasa, Shakotanchiku, Fushibutozasa, Tanahashizasasa, Yarikuma Sozasa, Gotenbazasa, Heronosa, Ooida Sasa, Himekisa, Nambusu, Fushigemememisasa, Kansaizasa, Miyama Kumasa, Tanzawasasa, Arimakosuzu Inuzu, Suzuda, Kumasu Hangesu, Kesu, Kintaichishima, Nemagaridake), Kanchiku, Medusa (Kanziku, Taiminiku, Taiminchi) Examples include Medakehagari Medake, Sudareyoshikida, Bousunezasa, Azuma Nesasa, Bamboo edulis, Oroshimachiku, Kennesa), Bamboo (Sorny Bamboo), Chichiku, Houraichiku (Houraichiku, Schiku, Dausanchiku), etc. .
Especially, it is more preferable in the said Gramineae bamboo being Mosouchiku of the genus Madake (Miso bamboo).
In the case of porous carbon using Moso bamboo as a raw material, the adjustment of mesopores is particularly easy.
＜多孔質炭素の製造方法＞
本発明の多孔質炭素は、炭化処理や賦活処理を経ることにより製造される。
炭化処理は、中温（３００℃から１０００℃）且つ無酸素状態で蒸焼き（乾留）にすることをいい、賦活処理は、炭素材料の細孔構造を発達させ、細孔を付加することをいう。賦活処理は、水蒸気や二酸化炭素等を用いて炭化物を高温（８００℃から１，４００℃）で一定時間乾留することにより、単位質量あたりの表面積を大きくする。
上記炭化処理条件や上記賦活処理条件を適宜調整することにより、所望のメソ孔容積及び細孔径０．４ｎｍ〜０．６ｎｍの最大微分容積値を示す多孔質炭素を得ることができる。
材料が、例えばイネ科タケ類由来の材料である場合、炭化処理に供する竹の粉末の粒径を調整することも、所望の多孔質炭素を得るうえで有効な手段となる。具体的には、粒径が５μｍから３０ｍｍ、より好ましくは５μｍから５ｍｍの竹の微粉末に対し、炭化処理を施すのが好ましい。また、その際の炭化処理及び賦活処理の条件としては、具体的には、４００℃から１０００℃の炭化温度で１時間から１０時間、炭化処理を行うことが好ましい。また、８００℃から１０００℃の賦活温度で０．５時間から１０時間、より好ましくは０．５時間から５時間、さらに好ましくは０．５時間から２時間、水蒸気のよる賦活処理を行うことが好ましい。
<Method for producing porous carbon>
The porous carbon of the present invention is produced by undergoing carbonization treatment or activation treatment.
Carbonization treatment refers to steaming (dry distillation) in an intermediate temperature (300 ° C. to 1000 ° C.) and oxygen-free state, and activation treatment refers to the development of the pore structure of the carbon material and addition of pores. . In the activation treatment, the surface area per unit mass is increased by carbonizing the carbide for a certain time at a high temperature (800 ° C. to 1,400 ° C.) using water vapor, carbon dioxide, or the like.
By appropriately adjusting the carbonization treatment conditions and the activation treatment conditions, porous carbon having a desired mesopore volume and a maximum differential volume value with a pore diameter of 0.4 nm to 0.6 nm can be obtained.
When the material is a material derived from, for example, Gramineae, adjusting the particle size of the bamboo powder to be carbonized is also an effective means for obtaining the desired porous carbon. Specifically, it is preferable to carbonize the fine bamboo powder having a particle size of 5 μm to 30 mm, more preferably 5 μm to 5 mm. Further, as the conditions for the carbonization treatment and activation treatment at that time, specifically, the carbonization treatment is preferably performed at a carbonization temperature of 400 ° C. to 1000 ° C. for 1 hour to 10 hours. Further, the activation treatment with water vapor may be performed at an activation temperature of 800 ° C. to 1000 ° C. for 0.5 hours to 10 hours, more preferably 0.5 hours to 5 hours, and even more preferably 0.5 hours to 2 hours. preferable.
（有機ハロゲン化合物除去装置）
本発明の有機ハロゲン化合物除去装置は、前記多孔質炭素からなるフィルターを有する。
本発明の有機ハロゲン化合物除去方法は、前記有機ハロゲン化合物除去装置用いて有機ハロゲン化合物を前記多孔質炭素に吸着させて除去する方法である。
より具体的には、水浄化用フィルターとして前記多孔質炭素材料を用い、フィルター中に有機ハロゲン化合物の不純物を含む水を通液することにより、有機ハロゲン化合物を除去する。
この際、フィルター内に充填する前記多孔質炭素材料の充填密度としては、０．２ｇ／ｃｍ３以上であることが好ましい。
本発明の有機ハロゲン化合物除去装置によれば、有機ハロゲン化合物の効果的な除去が可能となるため、通液倍率が大きい場合でも高い吸着性能を維持することができる。本発明の有機ハロゲン化合物除去装置を用いると、通液倍率が１，０００倍、より好ましくは通液倍率が３，０００倍、さらに好ましくは通液倍率が６，０００倍の条件下でも有機ハロゲン化合物を高い除去率で除去することができる。
具体的には、本発明の有機ハロゲン化合物除去装置を用いて、有機ハロゲン化合物を濃度０．０６ｍｇ／Ｌで含有する水に対し、通液倍率１，０００倍の条件で有機ハロゲン化合物を除去すると、除去率は９０％以上を示す。通液倍率３，０００倍の条件では、除去率は６５％以上、より好ましくは７０％以上を示す。また、通液倍率６，０００倍の条件では、除去率は５０％以上、より好ましくは６５％以上を示す。
本発明では、除去し得る対象の化合物として、前記有機ハロゲン化合物がクロロホルムであることがより好ましい。本発明の有機ハロゲン化合物除去装置は、クロロホルムの除去効果に優れている。
(Organic halogen compound removal equipment)
The organic halogen compound removing apparatus of the present invention has the filter made of the porous carbon.
The organic halogen compound removing method of the present invention is a method for removing an organic halogen compound by adsorbing the porous carbon using the organic halogen compound removing apparatus.
More specifically, the porous carbon material is used as a water purification filter, and the organic halogen compound is removed by passing water containing impurities of the organic halogen compound through the filter.
At this time, the packing density of the porous carbon material filled in the filter is preferably 0.2 g / cm 3 or more.
According to the organic halogen compound removing apparatus of the present invention, the organic halogen compound can be effectively removed, so that high adsorption performance can be maintained even when the liquid flow rate is large. When the organic halogen compound removing apparatus of the present invention is used, the organic halogen compound is used even under conditions where the liquid passing ratio is 1,000 times, more preferably the liquid passing ratio is 3,000 times, and even more preferably, the liquid passing ratio is 6,000 times. The compound can be removed with a high removal rate.
Specifically, when the organohalogen compound removing apparatus of the present invention is used to remove an organohalogen compound under the condition of a flow rate of 1,000 times with respect to water containing the organohalogen compound at a concentration of 0.06 mg / L. The removal rate is 90% or more. The removal rate is 65% or more, more preferably 70% or more under the condition of a liquid passing ratio of 3,000 times. Further, the removal rate is 50% or more, more preferably 65% or more under the condition of a liquid passing magnification of 6,000 times.
In the present invention, the organic halogen compound is more preferably chloroform as the target compound that can be removed. The organic halogen compound removing apparatus of the present invention is excellent in the effect of removing chloroform.
以下、本発明の実施例を説明するが、本発明は、これらの実施例に何ら限定されるものではない。 Examples of the present invention will be described below, but the present invention is not limited to these examples.
（実施例１）
原材料として籾殻を用いた。炭素化した籾殻（エコー商会製）に対し、酸又はアルカリ処理し、その後、９６０℃で１時間、水蒸気による賦活処理を行ない活性炭１を得た。
活性炭１の製造条件を下記表１に示す。また、３ＦＬＥＸ（マイクロメリテックスジャパン合同会社製）の装置を使用し、上述した測定方法により、活性炭１の各種特性を計測した。その結果を下記表２−１に示す。
＜クロロホルム除去試験＞
試料水は、クロロホルムを０．０６±０．００６ｍｇ／Ｌの濃度に調製した。そして、内径４ｍｍのチューブに活性炭１を１ｍＬ（長さ８０ｍｍ）充填した。試料水を温度２０℃で、通液倍率１，０００倍の条件で活性炭充填カラムに通水した。活性炭充填カラムから流出した試料水を採取し、クロロホルム濃度をガスクロマトグラフィーを用いて定量測定した。カラム通過前の試料水とカラムの活性炭層を通過した試料水を比較し、除去率を求めた。
ここで、通液倍率（倍）とは、一定時間において、活性炭の体積に対し通過した試料水の体積の割合をいう。通液倍率１，０００倍時のクロロホルム除去率とは、空間速度ＳＶ＝２，０００(単位：１／ｈ)で、クロロホルム水溶液を通液倍率（通液体積/活性炭体積）１，０００倍で通過させた時、つまり、活性炭１ｍＬに対し、クロロホルム水溶液を１，０００ｍＬ流した時の除去率をいう。
さらに、通液倍率１，０００倍と同様の方法で、通液倍率３，０００倍、及び６，０００倍における除去率も求めた。結果を下記表２に示す。
Example 1
Rice husk was used as a raw material. Carbonized rice husk (Echo Shokai) was treated with acid or alkali, and then activated with steam at 960 ° C. for 1 hour to obtain activated carbon 1.
The production conditions of the activated carbon 1 are shown in Table 1 below. Moreover, the various characteristics of the activated carbon 1 were measured by the measuring method mentioned above using the apparatus of 3FLEX (made by Micromeritex Japan GK). The results are shown in Table 2-1 below.
<Chloroform removal test>
As the sample water, chloroform was prepared to a concentration of 0.06 ± 0.006 mg / L. Then, 1 mL (80 mm in length) of activated carbon 1 was filled in a tube having an inner diameter of 4 mm. The sample water was passed through the activated carbon packed column at a temperature of 20 ° C. under the condition of a passing rate of 1,000 times. The sample water flowing out from the activated carbon packed column was collected, and the chloroform concentration was quantitatively measured using gas chromatography. The removal rate was determined by comparing the sample water before passing through the column and the sample water passing through the activated carbon layer of the column.
Here, the liquid flow rate (times) refers to the ratio of the volume of sample water that has passed through the volume of activated carbon over a certain period of time. The chloroform removal rate when the flow rate is 1,000 times is the space velocity SV = 2,000 (unit: 1 / h), and the chloroform solution passage rate (flow rate / activated carbon volume) is 1,000 times. It means the removal rate when passing 1,000 mL of chloroform aqueous solution with respect to 1 mL of activated carbon.
Furthermore, the removal rate at the liquid passing magnification of 3,000 times and 6,000 times was also determined in the same manner as the liquid passing ratio of 1,000 times. The results are shown in Table 2 below.
（実施例２）
原材料として中国産の竹を用いた。炭素化した竹のチップ（有限会社綜合製）に対し、９００℃で１時間、水蒸気による賦活処理を行ない活性炭２を得た。
活性炭２の製造条件を下記表１に示す。実施例１と同様の方法により、活性炭２の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−１に示す。
(Example 2)
Chinese bamboo was used as a raw material. An activated carbon 2 was obtained by subjecting the carbonized bamboo chips (manufactured by Kyogo Co., Ltd.) to activation treatment with steam at 900 ° C. for 1 hour.
The production conditions of the activated carbon 2 are shown in Table 1 below. Various characteristics of the activated carbon 2 were measured in the same manner as in Example 1. Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-1 below.
（実施例３）
原材料として九州産の孟宗竹を用いた。竹の微粉末（粒径（公称）：５μｍ〜５００μｍ、バンブーテクノ社製）に対し、６００℃で６時間炭化処理を行ない、その後、９００℃で３時間、水蒸気による賦活処理を行ない活性炭３を得た。
活性炭３の製造条件を下記表１に示す。実施例１と同様の方法により、活性炭３の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−１に示す。
(Example 3)
Kyushu bamboo shoots from Kyushu were used as raw materials. Bamboo fine powder (particle size (nominal): 5 μm to 500 μm, manufactured by Bamboo Techno Co., Ltd.) is carbonized at 600 ° C. for 6 hours, and then activated by steam for 3 hours at 900 ° C. Obtained.
The production conditions of the activated carbon 3 are shown in Table 1 below. Various characteristics of the activated carbon 3 were measured in the same manner as in Example 1. Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-1 below.
（実施例４）
原材料として九州産の孟宗竹を用いた。竹の粉末（粒径（公称）：０．１ｍｍ〜０．４ｍｍ、バンブーテクノ社製）に対し、６００℃で６時間炭化処理を行ない、その後、９００℃で３時間、水蒸気による賦活処理を行ない活性炭４を得た。
活性炭４の製造条件を下記表１に示す。実施例１と同様の方法により、活性炭４の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−１に示す。
Example 4
Kyushu bamboo shoots from Kyushu were used as raw materials. Bamboo powder (particle size (nominal): 0.1 mm to 0.4 mm, manufactured by Bamboo Techno Co., Ltd.) is carbonized at 600 ° C. for 6 hours, and then activated by steam at 900 ° C. for 3 hours. Activated carbon 4 was obtained.
The production conditions for the activated carbon 4 are shown in Table 1 below. Various characteristics of the activated carbon 4 were measured in the same manner as in Example 1. Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-1 below.
（実施例５）
原材料として九州産の孟宗竹を用いた。竹の粉末（粒径（公称）：０．１ｍｍ〜０．４ｍｍ、バンブーテクノ社製）に対し、６００℃で６時間炭化処理を行ない、その後、９００℃で１時間、水蒸気による賦活処理を行ない活性炭５を得た。
活性炭５の製造条件を下記表１に示す。実施例１と同様の方法により、活性炭５の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−２に示す。
(Example 5)
Kyushu bamboo shoots from Kyushu were used as raw materials. Bamboo powder (particle size (nominal): 0.1 mm to 0.4 mm, manufactured by Bamboo Techno Co., Ltd.) is carbonized at 600 ° C. for 6 hours, and then activated by steam at 900 ° C. for 1 hour. Activated carbon 5 was obtained.
The production conditions for the activated carbon 5 are shown in Table 1 below. Various characteristics of the activated carbon 5 were measured in the same manner as in Example 1. Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-2 below.
（実施例６）
原材料として九州産の孟宗竹を用いた。竹の微粉末（粒径（公称）：５μｍ〜５００μｍ、バンブーテクノ社製）に対し、６００℃で６時間炭化処理を行ない、その後、９００℃で１時間、水蒸気による賦活処理を行ない活性炭６を得た。
活性炭６の製造条件を下記表１に示す。実施例１と同様の方法により、活性炭６の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−２に示す。
(Example 6)
Kyushu bamboo shoots from Kyushu were used as raw materials. Bamboo fine powder (particle size (nominal): 5 μm to 500 μm, manufactured by Bamboo Techno Co., Ltd.) is carbonized at 600 ° C. for 6 hours, and then activated by steam at 900 ° C. for 1 hour to obtain activated carbon 6. Obtained.
The production conditions for the activated carbon 6 are shown in Table 1 below. Various characteristics of the activated carbon 6 were measured in the same manner as in Example 1. Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-2 below.
（比較例１）
原材料としてヤシ殻を用いた。ヤシ殻の比較用活性炭１（ＣＮ２４０Ｇ、フタムラ化学社製）を用い、実施例１と同様の方法により、比較用活性炭１の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−２に示す。
(Comparative Example 1)
Coconut shell was used as a raw material. Various characteristics of the activated carbon 1 for comparison were measured by the same method as in Example 1 using the activated carbon 1 for comparison with coconut shell (CN240G, manufactured by Phutamura Chemical Co., Ltd.). Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-2 below.
（比較例２）
原材料としてヤシ殻を用いた。ヤシ殻の比較用活性炭２（クラレコールＧＷ、クラレケミカル株式会社製）を用い、実施例１と同様の方法により、比較用活性炭２の各種特性を計測した。また、クロロホルムの除去率を求めた。結果を下記表２−２に示す。
(Comparative Example 2)
Coconut shell was used as a raw material. Various characteristics of the activated carbon 2 for comparison were measured by the same method as in Example 1 using the activated carbon 2 for comparison of coconut shell (Kuraray Coal GW, manufactured by Kuraray Chemical Co., Ltd.). Moreover, the removal rate of chloroform was calculated | required. The results are shown in Table 2-2 below.
本発明の多孔質炭素は、その高い吸着性能ゆえ、キャパシタの電極材料、各種吸着剤、マスク、吸着シート、触媒用の担体等に使用することができる。 The porous carbon of the present invention can be used for capacitor electrode materials, various adsorbents, masks, adsorption sheets, catalyst carriers and the like because of its high adsorption performance.
Claims (14)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2015213673A JP6426583B2 (en) | 2015-10-30 | 2015-10-30 | Porous carbon and organic halogen compound removing apparatus using the same |
| PCT/JP2016/081778 WO2017073631A1 (en) | 2015-10-30 | 2016-10-26 | Porous carbon and organic halogen compound removal device using same |
| KR1020187012313A KR102622510B1 (en) | 2015-10-30 | 2016-10-26 | Porous carbon and organic halogen compound removal device using the same |
| CN201680063260.0A CN108348890B (en) | 2015-10-30 | 2016-10-26 | Porous carbon and organic halide removal device using same |
| TW105135064A TW201728533A (en) | 2015-10-30 | 2016-10-28 | Porous carbon and organic halogen compound removing device using the same |
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| JP (1) | JP6426583B2 (en) |
| KR (1) | KR102622510B1 (en) |
| CN (1) | CN108348890B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0840713A (en) * | 1994-05-26 | 1996-02-13 | Tousou Sangyo Kk | Activated carbon, its production and water treatment using the activated carbon |
| JPH11217207A (en) * | 1998-01-30 | 1999-08-10 | Kurimoto Ltd | Production of active carbon from unsaturated polyester resin waste material |
| JP2007261918A (en) * | 2006-03-30 | 2007-10-11 | Shiga Pref Gov | Method for manufacture bamboo activated carbon |
| JP2013112572A (en) * | 2011-11-29 | 2013-06-10 | Nagaoka Univ Of Technology | Hydrogen occlusion method, and hydrogen occluding material |
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| JP2950666B2 (en) | 1991-11-15 | 1999-09-20 | クラレケミカル株式会社 | Activated carbon water purifier |
| JPH11140492A (en) * | 1997-11-11 | 1999-05-25 | Ishihara Kk | Charcoal from bamboo |
| JP3693544B2 (en) | 2000-01-31 | 2005-09-07 | 松下電器産業株式会社 | Activated carbon and water purifier provided with the same |
| TWI367125B (en) * | 2008-01-24 | 2012-07-01 | Forestry Bureau Council Of Agriculture Executive Yuan | Heavy metal adsorbent and fabrication method thereof |
| JP6218355B2 (en) * | 2011-02-10 | 2017-10-25 | ソニー株式会社 | Filter media |
| CN103693642B (en) * | 2013-12-23 | 2016-01-06 | 湖南华银能源技术有限公司 | Prepare method and the production equipment thereof of bamboo matrix activated carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0840713A (en) * | 1994-05-26 | 1996-02-13 | Tousou Sangyo Kk | Activated carbon, its production and water treatment using the activated carbon |
| JPH11217207A (en) * | 1998-01-30 | 1999-08-10 | Kurimoto Ltd | Production of active carbon from unsaturated polyester resin waste material |
| JP2007261918A (en) * | 2006-03-30 | 2007-10-11 | Shiga Pref Gov | Method for manufacture bamboo activated carbon |
| JP2013112572A (en) * | 2011-11-29 | 2013-06-10 | Nagaoka Univ Of Technology | Hydrogen occlusion method, and hydrogen occluding material |
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| WO2017073631A1 (en) | 2017-05-04 |
| JP6426583B2 (en) | 2018-11-21 |
| CN108348890B (en) | 2021-06-29 |
| KR102622510B1 (en) | 2024-01-08 |
| TW201728533A (en) | 2017-08-16 |
| CN108348890A (en) | 2018-07-31 |
| KR20180069833A (en) | 2018-06-25 |
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