JP2009173540A - Porous carbon material powder and method of manufacturing the same - Google Patents
Porous carbon material powder and method of manufacturing the same Download PDFInfo
- Publication number
- JP2009173540A JP2009173540A JP2009080665A JP2009080665A JP2009173540A JP 2009173540 A JP2009173540 A JP 2009173540A JP 2009080665 A JP2009080665 A JP 2009080665A JP 2009080665 A JP2009080665 A JP 2009080665A JP 2009173540 A JP2009173540 A JP 2009173540A
- Authority
- JP
- Japan
- Prior art keywords
- porous carbon
- carbon material
- temperature
- moss
- material powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/0675—Vegetable refuse; Cellulosic materials, e.g. wood chips, cork, peat, paper
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62204—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse
- C04B35/62213—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products using waste materials or refuse using rice material, e.g. bran or hulls or husks
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/009—Porous or hollow ceramic granular materials, e.g. microballoons
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
この発明は、それまで利用価値が低いとされてきていた麩糠類を、有望な工業用資源である多孔性炭素材とすることにより、高機能製品用の素材として広範に応用しようとするものであり、特にその技術分野については特定されるものではなく、あらゆる分野をその技術分野とするものであって、したがって、麩糠類を生産する農業や麩糠類を消費する人々に係わる技術分野をはじめとし、麩糠類から油性分等を精製する技術分野、その分野に必要な製造機械や試験機械、施設設備等各種機械を製造、販売する分野、それらに必要な資材、部品を提供する分野、それら資材、部品の加工に必要な機械、工具類を提供する分野、またそれら資材や機械装置、部品類に必要な素材、例えば木材、合板、プラスチック、各種金属材料を提供する分野、それらに組み込まれる電子分品やそれらを集積した制御機器の分野、各種計測器の分野、当該設備、器具を動かす動力機械の分野、そのエネルギーとなる電力やエネルギー源である電気、オイルの分野といった一般的に産業機械として総称されるような分野、更には、それら設備、器具類を試験、研究したり、それらの修理、展示、販売、輸出入、ならびに使用する分野、将又、麩糠類を原材料として得られるこの発明の新素材やそれを使った粉末を応用する全ての分野、この発明に包含されている製造方法を実施するために必要となる農業、機械、電気、化学その他あらゆる技術分野、この発明の製造方法を実施する過程で発生するゴミ屑を回収、運搬する回収、輸送の分野、ゴミ屑を効率的に再生利用するリサイクル分野、そして現時点で想定できないが、新たに加わってくる未知の分野の果てまでと、関係しない技術分野はない程である。 This invention is intended to be widely applied as a material for high-performance products by using porous carbon material, which is a promising industrial resource, for moss that had been considered to have low utility value until then. In particular, the technical field is not specified, and all fields are used as the technical field. Therefore, technical fields related to agriculture that produces moss and people who consume moss. In addition, the technical field for refining oily components from moss, the field for manufacturing and selling various machines such as manufacturing and testing machines and facility equipment necessary for the field, and the materials and parts necessary for them Fields, fields that provide machines and tools necessary for processing these materials and parts, and fields that provide materials, machinery, and parts necessary for materials such as wood, plywood, plastics, and various metal materials The field of electronic components incorporated in them, the field of control equipment that integrates them, the field of various measuring instruments, the field of power equipment that moves the equipment and instruments, the field of electricity and energy that is the energy and the field of oil, etc. Fields generally referred to as industrial machines, as well as fields that test, research, repair, display, sell, import / export, and use of those facilities and instruments All fields of application of the new material of the present invention obtained from the raw materials and powders using the same, agriculture, machinery, electricity, chemistry and all other technologies required to carry out the manufacturing method included in the present invention The field, the collection and transportation of garbage waste generated in the process of carrying out the manufacturing method of the present invention, the field of transportation, the recycling field that efficiently recycles garbage waste, and the present It can not be assumed in it, and to the ends of the unknown in the art to which the coming new addition, it is enough not the technical field that is not related.
（視 点）
我が国の主要穀物である米からは、副産物として大量の籾殻や糠が発生する。また、同様に、麦や蕎麦、大豆等の穀類からも大量の殻や麩（フスマ）を生じさせ、それら殻や麩糠類等、穀類からの副産物の多くは、邪魔者として焼却処分に回されてしまうか、あるいは、米糠は搾油して米糠油を製造したり、殻（特に籾殻）の極一部が暗渠用資材や燻炭等として利用される外、その製炭過程で留出された乾留気化物が、凝縮されて防虫剤や動物忌避剤、土壌改良剤、水虫治療薬等として利用されることもある。
(point of view)
A large amount of rice husks and straw is produced as a by-product from rice, which is the main grain in Japan. Similarly, a large amount of husks and straws are produced from grains such as wheat, buckwheat, and soybeans, and many of the by-products from cereals such as husks and straws are disposed of by incineration as an obstacle. Or the rice bran is squeezed to produce rice bran oil, or a very small part of the shell (especially rice husk) is used as a material for culvert or charcoal, and is distilled during the coal making process. In some cases, the evaporated carbonized product is condensed and used as an insect repellent, animal repellent, soil conditioner, athlete's foot therapeutic agent, and the like.
しかし、脱脂糠を含む麩糠類は、大部分が飼料化あるいは茸培地化されたり、肥料化される等して農業用資材に活用される程度の利用に止まっていることから、これら麩糠類の工業用資材としての有効利用が模索され続けてきている。
その一つが、麩糠類を炭素化する技術である。この麩糠類の炭素化は、小規模には、バッチ式で蒸し焼きする方法で、また、大規模には、ロータリーキルンや多段流動床炉等で連続的に焼成する方法等で実施されることとなるが、麩糠類が非常に微細な粉末体であって、通気性や熱伝導性が悪い上、僅かとはいえ油脂分を含有していることにも災いされ、燃え尽きて灰化してしまう割合も多く、効率的且つ完全な炭素化が難しいという経済効率上の大きな難点と、加えて、製造された炭化物は、細かくて飛散し易い性状のものとなってしまい、取り扱い上の不便さが伴うといった問題等から、あまり積極的な事業化が成されてきた実績もなく、したがって、麩糠類から形成した炭化物、所謂「炭（すみ）」は、その質、量からして、農業用土壌改良材として利用されることはあっても、工業用材料として有効活用されることはなかったのが実情である。
However, most of the cocoons containing defatted cocoons have been used only for agricultural materials such as feed or potato medium or fertilizer. The effective use of these as industrial materials continues to be sought.
One of them is the technology to carbonize moss. This carbonization of moss is carried out by a batch-type steaming method on a small scale, and by a continuous firing method in a rotary kiln, a multistage fluidized bed furnace, etc. on a large scale. However, moss is a very fine powder, poor air permeability and heat conductivity, and even though it contains a small amount of fats and oils, it burns out and becomes ashed. The ratio is high, and it is difficult to achieve efficient and complete carbonization. In addition, the produced carbide is fine and easily scattered, which is inconvenient to handle. There is no track record of aggressive commercialization due to the problems involved, and therefore, the so-called “char” formed from moss is used for agriculture in terms of quality and quantity. Although it may be used as a soil conditioner, Is the reality of never be effectively used as a use material.
（従来の技術）
そこで、米糠油製造業に係わるものとして、脱脂糠の有効利用に関して極めて強い関心を抱いていたことから、逸早くその技術開発、研究に取り組み、山形大学工学部および山形県工業技術センター双方の指導も得て、既に特開平１０−１０１４５３号公報に掲載されているとおり、「多孔性炭素材製品の製造方法」として、遂に脱脂糠を始めとし、粉砕した籾殻や、小麦をひいて粉にしたときに皮屑として出る麩（フスマ）や、場合によっては、蕎麦殻、大豆殻等も加えた麩糠類を原材料として、例えば、外壁材等の建材や家具、梱包用素材といった極めて身近な素材をはじめ、軸受け部品その他の機械部品等に、更には、電解精製して導電材料、発熱体、電子部品等といった高機能製品を成形するようにした麩糠類の有効利用に関する技術を完成するに至った。
(Conventional technology)
Therefore, as it was related to the rice bran oil manufacturing industry, it had a very strong interest in the effective use of defatted rice bran, so it quickly worked on its technology development and research, and received guidance from both Yamagata University's Faculty of Engineering and Yamagata Prefectural Industrial Technology Center. As already described in Japanese Patent Application Laid-Open No. 10-101453, as “a method for producing a porous carbon material product”, when defatted rice bran and finally crushed rice husk and wheat are ground into powder The raw material is husks that appear as leather scraps, and, in some cases, cocoons that include buckwheat husks and soybean husks. For example, building materials such as exterior wall materials, furniture, and packaging materials. Technology for effective use of cages that have been refined electrolytically to form high-performance products such as conductive materials, heating elements, electronic parts, etc. The has been completed.
そうして、この完成した「多孔性炭素材製品の製造方法」に従って各種高機能製品の製造を開始し、資源の有効活用という観点からは勿論のこと、品質上、機能上からも十分過ぎる有用性を再確認している中、この製造方法による場合、その製造工程上の特徴から、高機能製品が特定されて初めてその高機能製品に合わせた金型作りに取り掛かり、その完成を待って目的とする所定の高機能製品の製造をこの発明の工程に従って準じ開始し、製品を提供するという手順とならざるを得ないことになる。
（問題意識）
上述のような事情から、製品が決定されない限り、換言すれば形状・構造の特定された高機能製品についての受注をしない限り、当然のことながらこの発明の実施ができず、その間、製造ラインは停止したままとなってしまい、採算効率上において不都合を来してしまうことになる上、受注してからその都度全ての工程を最初から順次実施していくことになるため、受注後、製品供給までに要する時間の短縮は殆ど不可能となって迅速な対応をすることができなくなり、需要者からの要望に応え切れなくしてしまう虞れもあり得るといった問題があることを初めて認識するに至った。
(Awareness of problems)
Under the circumstances as described above, unless the product is determined, in other words, unless an order is received for a highly functional product with a specified shape and structure, the present invention cannot be practiced. Since it will remain stopped, it will cause inconvenience in profitability, and all the processes will be performed sequentially from the beginning each time an order is received. It is almost impossible to shorten the time required to complete the process, making it impossible to respond promptly, and for the first time to recognize that there is a possibility that it may become impossible to respond to demands from consumers. It was.
（発明の目的）
この発明は、それら新たな課題へ対処するために引き続き開発、研究を進めてきたところ、ようやくそれら高機能製品を迅速且つ確実に得られるようにするための有効な手段となり得る新規な多孔性炭素材粉末およびその製造方法を完成することに成功したものであり、以下では、その構成の詳細を、幾つかの実施例と共に説示していくこととする。
(Object of invention)
The present invention has been continuously developed and researched to cope with these new problems. Finally, a novel porous carbon that can be an effective means for obtaining these highly functional products quickly and reliably. The material powder and the manufacturing method thereof have been successfully completed, and in the following, the details of the configuration will be explained together with some examples.
（発明の構成）
先ず、この発明の基をなす多孔性炭素材は、基本的に次のとおりの構成から成り立っている。 即ち、２０メッシュアンダーの米糠や麩等の麩糠類に、熱硬化性樹脂、および適量の糊料入り水溶液または水を加えてなる混練状麩糠類を乾燥、造粒し、４メッシュアンダーに篩分け、選別して麩糠類粒状素材にした上、それら麩糠類粒状素材を、不活性ガス雰囲気中または真空中で焼成、炭化してなる多孔性炭素材とし、それらを粉砕、粉末化して所望粒度のものとした構成を要旨とする多孔性炭素材粉末である。
(Structure of the invention)
First, the porous carbon material forming the basis of the present invention basically consists of the following configurations. That is, kneaded rice cakes made by adding a thermosetting resin and an appropriate amount of an aqueous solution containing paste or water to rice cakes such as rice bran and rice cakes of 20 mesh under are dried, granulated, and made into 4 mesh under. After sieving and sorting to make moss granular materials, these moss granular materials are baked and carbonized in an inert gas atmosphere or in vacuum to form porous carbon materials, which are pulverized and powdered. Thus, a porous carbon material powder having a desired particle size as a gist.
（関連する発明１）
上記したこの発明の多孔性炭素材粉末に関連し、この発明には、この多孔性炭素材粉末の製造方法からなるが包含されている。
即ち、２０メッシュアンダーの米糠や麩等の麩糠類に、熱硬化性樹脂、および適量の糊料入り水溶液または水を加えて混練する工程、それら混練状麩糠類を、６０ないし８０℃まで加温して揮発性物質を除去しながら乾燥して造粒した上、４メッシュアンダーに篩分け、選別して麩糠類粒状素材にする工程、それら麩糠類粒状素材を、不活性ガス雰囲気中または真空中で焼成、炭化する工程、それら炭化粒状麩糠類を最終焼成温度から所定降温速度で常温まで冷却して多孔性炭素材とする工程、それら工程で得られた冷却済みの多孔性炭素材を粉砕して所望粒度に粉末化する工程、以上の各工程を順次経過させていくようにした構成を要旨とする多孔性炭素材粉末の製造方法が、それである。
(Related invention 1)
In relation to the porous carbon material powder of the present invention described above, the present invention includes a method comprising the method for producing the porous carbon material powder.
That is, a step of adding a thermosetting resin and an appropriate amount of an aqueous solution containing paste or water to kneads such as rice bran and koji with 20 mesh under, and kneading kneaded pork to 60 to 80 ° C. Drying and granulating while removing volatile substances by heating, sieving into 4 mesh under, selecting to make moss granular material, these moss granular material in inert gas atmosphere A process of firing and carbonizing in a medium or vacuum, a process of cooling these carbonized particulates from the final firing temperature to room temperature at a predetermined temperature drop rate to a porous carbon material, and the cooled porous material obtained in these processes This is a method for producing a porous carbon material powder, which includes a step of pulverizing a carbon material to obtain a powder having a desired particle size and a structure in which the above steps are sequentially performed.
これを、より具体的な構成のものとして示せば、２０メッシュアンダーの米糠や麩等の麩糠類に、熱硬化性樹脂、および適量の糊料入り水溶液または水を加えて混練する工程、それら混練状麩糠類を、６０ないし８０℃まで加温して揮発性物質を除去しながら乾燥して造粒した上、４メッシュアンダーに篩分け、選別して麩糠類粒状素材にする工程、それら麩糠類粒状素材を、不活性ガス雰囲気中または真空中で所定の昇温速度に従って昇温させていき、最終焼成温度で７００℃以上の温度で焼成、炭化する工程、それら炭化粒状麩糠類を最終焼成温度から所定降温速度で常温まで冷却する工程、それら工程で得られた冷却済みの多孔性炭素材を粉砕して所望粒度に粉末化する工程、以上の各工程を順次経過させていくようにした多孔性炭素材粉末の製造方法ということができる。 If this is shown as having a more specific structure, a process of adding a thermosetting resin and an appropriate amount of an aqueous solution containing paste or water to kneads such as rice bran or koji with a 20 mesh under, kneading them, A step of heating and kneading the kneaded rice cake to 60 to 80 ° C. while removing volatile substances and granulating it, and sieving into 4 mesh under and selecting to make a rice cake granular material; A step of raising the temperature of these granular materials in an inert gas atmosphere or in a vacuum according to a predetermined rate of temperature increase, and firing and carbonizing at a final firing temperature of 700 ° C. or higher; The process of cooling the product from the final firing temperature to room temperature at a predetermined temperature drop rate, the process of pulverizing the cooled porous carbon material obtained in those processes and pulverizing it to the desired particle size, and passing each of the above processes sequentially Porous carbon made to go It can be said that the production method of the powder.
以上のとおりの構成を要旨として実現されるこの発明の多孔性炭素材粉末、およびその製造方法によれば、需要者から求められることになるであろうと予測される高機能製品の性状に適したサイズの多孔性炭素材粉末を、多孔性炭素材から効率的にその都度作り出すか、予め十分な量を用意しておき、需要者からの高機能製品の特定後は、単に特定された高機能製品の性状に適合した最適な粒度のこの発明の多孔性炭素材粉末を選択し、それら多孔性炭素材粉末に、これまた対象とする高機能製品の性状を勘案した最適割合となるよう熱硬化性樹脂を混合して混練物とする工程から直ちに多孔性炭素材製品の製造を開始することができることになり、従前までの場合のように、高機能製品が特定されない限り所定の高機能製品の製造をすることができず、その間、製造ラインは停止したままとして採算効率を落したり、製品供給までに時間を要することになるといった不都合は完全に払拭され、需要者からの要望に迅速に対応可能にして需要者への利便性改善されるようにすると共に、廃棄物扱いされてきた麩糠類を、付加価値の高い多種多様な機能（構造強度や摩擦係数・膨脹係数等の物理的機能の外、吸着性や断熱性、耐熱性、耐薬品性、耐候性、通電性、電磁シールド性等といった作用的機能）を有する高機能製品へと効率的且つ確実に製品化するようにするという秀れた特徴が得られるものとなる。 According to the porous carbon material powder of the present invention that is realized based on the configuration as described above and the manufacturing method thereof, it is suitable for the properties of high-function products that are expected to be demanded by consumers. A porous carbon material powder of the size is efficiently produced from the porous carbon material each time, or a sufficient amount is prepared in advance, and after the high-performance product is identified from the consumer, the specified high-function Select the porous carbon material powder of the present invention with the optimal particle size suitable for the properties of the product, and heat cure so that the porous carbon material powder has the optimum ratio in consideration of the properties of the target high-performance product. As a result, the production of porous carbon material products can be started immediately from the step of mixing the functional resin into a kneaded product. Manufacturing In the meantime, inconveniences such as reducing the profitability and maintaining the production line while stopping the production line and taking time to supply the product are completely eliminated, and it is possible to respond quickly to demands from customers and demand. In addition to improving the convenience to the user, it is also possible to adsorb moss that has been treated as waste by adding a wide variety of high-value-added functions (in addition to physical functions such as structural strength, friction coefficient, and expansion coefficient) Excellent features such as efficient and reliable commercialization of high-functional products with functional properties such as heat resistance, heat insulation, heat resistance, chemical resistance, weather resistance, electrical conductivity, and electromagnetic shielding properties) Is obtained.
上記したとおりの構成からなるこの発明の実施に際し、その最良もしくは望ましい形態について説明を加えることにする。 先ず、麩糠類としては、米糠油を搾油した後に大量に残る脱脂糠を始めとし、小麦をひいて粉にしたときに皮屑として出る麩、更には、籾殻や蕎麦殻、大豆殻、グルテンフィード（トウモロコシの皮や実の滓、即ちコーンスターチを製造したときの残滓）等、穀類を加工処理する過程で発生する粉末状の、あるいは粉砕処理した皮殻を包含しており、それらは、望ましくは、その粒度が一定以下（例えば、脱脂後の糠の場合、脱脂過程で焦げたり、固形化した大粒なものを除くために、１２メッシュアンダー、最適には２０メッシュアンダー）に揃うよう、篩に掛けたものが採用されるようにし、その後の成形性や素材構造の均質化等に有利なものとすべきである。 In implementing the present invention having the above-described configuration, the best or desirable mode will be described. First of all, cocoons include defatted rice bran that remains in large quantities after squeezing rice bran oil, rice cakes that appear as waste when wheat is ground and powdered, and rice husk, buckwheat husk, soybean husk, gluten Includes powdered or crushed shells generated during the processing of cereals, such as feed (corn husks and cocoons, ie, residues from the manufacture of corn starch), which are preferably Sieving so that the particle size is equal to or less than a certain level (for example, in the case of defatted soot, to remove large particles that have been burned or solidified during the degreasing process, 12 mesh under, optimally 20 mesh under) Should be adopted, which should be advantageous for subsequent formability and homogenization of the material structure.
熱硬化性樹脂としては、代表的なフェノール樹脂を、例えば、約１０〜６０重量パーセント程度に希釈したものを採用することによって、麩糠類への混合、攪拌作業を円滑にすることができて望ましく、また、その混合割合は、麩糠類の種類によっても異なるが、例えば脱脂後の糠の場合であれば約５〜８０重量パーセント程度、麩（ふすま）であれば約５〜７０重量パーセント程度、また、グルテンフィードであれば約５〜６０重量パーセント程度、（但し、何れの場合にも、麩糠類の粒度や含水率、素材温度等の条件によって変更される。）といった具合に、麩糠類に対応した最適な割合で採用され、それら麩糠類への浸透率を調整する必要のある場合には、混合、撹拌作業環境や混合、撹拌後の放置時間の設定等の各種条件が検討されるようにする。 なお、上記熱硬化性樹脂、糊料入り水溶液、又は水は、麩糠類と混合させた場合、麩糠類に対し糊剤として機能するものであり、糊料入り水溶液の糊料としては、海草糊料やコラーゲン、澱粉、リグニン等を用いることができる。 As a thermosetting resin, a typical phenolic resin diluted to about 10 to 60 weight percent, for example, can be used for smooth mixing and agitation to moss. Desirably, the mixing ratio varies depending on the kind of cocoons, but for example, about 5 to 80% by weight in the case of cocoon after degreasing, and about 5 to 70% by weight in the case of cocoon (bran). If it is a gluten feed, it is about 5 to 60 weight percent (however, in any case, it is changed depending on conditions such as grain size, moisture content, material temperature, etc.) Various conditions such as setting of mixing, stirring work environment and mixing, and leaving time after stirring are adopted when it is necessary to adjust the permeation rate to these moss by adopting the optimum ratio corresponding to moss. Is considered So as to. The thermosetting resin, the aqueous solution containing paste, or water, when mixed with moss, functions as a sizing agent for potatoes. Seaweed paste, collagen, starch, lignin and the like can be used.
麩糠類粒状素材は、焼成、炭化後の品質にばらつきをなくすようにする必要から、乾燥、造粒した後の混練状麩糠類を、４メッシュアンダーに予め篩分け、選別した麩糠類粒状素材が採用されるようにすべきであり、こうして粒度を調整した麩糠類粒状素材は、品質にばらつきを生じさせないものとして焼成、炭化された後、最終的に、需要者から求められることになるであろうと予測される各種高機能製品の性状、即ち、製品形状の複雑さ、それに起因した型詰めの難易度、構造強度、外観の緻密さ加減等の差異に対し、自在に対応可能とするような粒度、例えば２５０ないし１００μｍ、１５０ないし１００μｍ、１５０μｍ以下、１００μｍ以下、５０ないし１０μｍ、１０μｍ以下等といった段階別のものとして用意ができるよう、適宜粉砕機（アトマイザー）によって一旦粉砕した後、振盪篩によって選別してこの発明の多孔性炭素材粉末とするものである。 In order to eliminate unevenness in the quality after baking and carbonization, the dried granular material is pre-screened and screened into 4 mesh under the kneaded dried dried and granulated powder. The granular material should be adopted, and the moss granular material thus adjusted in particle size should be finally demanded by consumers after being fired and carbonized so as not to cause variations in quality. It is possible to respond freely to the characteristics of various high-function products that are expected to become, that is, the complexity of the product shape, the difficulty of mold filling caused by it, the structural strength, the fineness of appearance, etc. As appropriate, the particle size can be prepared in stages such as 250 to 100 μm, 150 to 100 μm, 150 μm or less, 100 μm or less, 50 to 10 μm, 10 μm or less. After once crushed by crusher (atomizer), and screened by shaking sieve is to a porous carbon material powder of the present invention.
関連する発明２および３における熱硬化性樹脂は、既述した如く、麩糠類への混合、攪拌作業を円滑にする上で、例えば、代表的なフェノール樹脂を約１０〜６０重量パーセント程度に希釈したものを採用するようにする等、その混合割合は、麩糠類の種類によっても異なり、例えば脱脂後の糠の場合であれば約５〜８０重量パーセント程度、麩（ふすま）であれば約５〜７０重量パーセント程度、また、グルテンフィードであれば約５〜６０重量パーセント程度、（但し、何れの場合にも、麩糠類の粒度や含水率、素材温度等の条件によって変更される。）といった具合に、麩糠類に対応した最適な割合で採用され、それら麩糠類への浸透率を調整する必要のある場合には、混合、撹拌作業環境や混合、撹拌後の放置時間の設定等の各種条件が検討されるようにする。 As described above, the thermosetting resin in the related inventions 2 and 3 is, for example, about 10 to 60% by weight of a typical phenolic resin in order to facilitate mixing and stirring into moss. The mixing ratio varies depending on the type of potato, such as using a diluted one. For example, about 5 to 80% by weight in the case of cocoon after degreasing, About 5 to 70 percent by weight, or about 5 to 60 percent by weight for gluten feed (in any case, depending on conditions such as grain size, moisture content, material temperature, etc.) )), Etc., and in cases where it is necessary to adjust the penetration rate into the moss, mixing, stirring work environment, mixing, and standing time after stirring Various conditions such as setting There is to be considered.
この熱硬化性樹脂の混合、含浸工程では、熱硬化性樹脂の麩糠類への浸透率の吟味し、所定濃度の熱硬化性樹脂の混入に並行して、適量の水を加えたり、あるいは、各種動植物糊料（例えば海草糊料やコラーゲン、澱粉、リグニン等）や澱粉、各種糖液等の繋ぎ剤を適量（例えば、脱脂後の糠の場合であれば約５〜３０重量パーセント程度）混合した水溶液を加えて実施されるようにしたり、あるいは、予め、成形性を良くするための水や繋ぎ剤混合液を、所定濃度の熱硬化性樹脂に混入したものとした上で麩糠類への混合、撹拌作業を実施して混練状麩糠類となるようにすべきである。 In the mixing and impregnation process of the thermosetting resin, the penetration rate of the thermosetting resin into moss is examined, and an appropriate amount of water is added in parallel with the mixing of the thermosetting resin of a predetermined concentration, or Appropriate amounts of various animal and plant pastes (for example, seaweed paste, collagen, starch, lignin, etc.) and starch, various sugar solutions, etc. (for example, about 5 to 30% by weight in the case of defatted koji) It can be carried out by adding a mixed aqueous solution, or pre-mixed with water or a binder solution for improving moldability mixed in a thermosetting resin of a predetermined concentration. Mixing and stirring operations should be carried out to obtain kneaded potatoes.
所定の割合まで熱硬化性樹脂を混合させた混練状麩糠類は、例えば、平面型造粒機や筒型造粒機等の公知の造粒機を使って造粒しながら、６０〜８０℃程度まで加温して揮発分を抜いて乾燥させた上、焼成段階でのガス抜けを円滑なものとして極力均質な炭化が実現されるようにする配慮から、それら造粒物を篩に掛けて所定サイズ、望ましくは４メッシュアンダー程度、より好ましくは５メッシュアンダー程度のものに揃えてしまう、麩糠類粒状素材にする工程を必要としている。 The kneaded rice cake in which the thermosetting resin is mixed to a predetermined ratio is, for example, 60 to 80 while granulating using a known granulator such as a flat granulator or a cylindrical granulator. In order to achieve uniform carbonization as much as possible by smoothing out the gas at the firing stage after drying up by heating up to about ℃ and removing volatile matter, these granulated products are sieved In other words, it is necessary to have a process for forming a moss-like granular material that has a predetermined size, desirably about 4 mesh under, more preferably about 5 mesh under.
こうして用意された麩糠類粒状素材、特に４メッシュアンダーの麩糠類粒状素材は、次に、不活性ガス雰囲気中または真空中で焼成、炭化する工程に移されるが、上記した熱硬化性樹脂を含む麩糠類粒状素材が燃焼してしまわないよう、窒素ガス等の不活性ガス雰囲気中、または真空下等といった無酸素状態を維持して実施されることを要し、また、それら麩糠類粒状素材が崩壊してしまわないよう急激な温度上昇を避けるよう注意すべきである。特に、２００〜４００℃付近では、分解に伴う大量のガスが発生するため、この間の昇温速度には十分な配慮がなされるべきであり、例えば、麩糠類が脱脂糠の場合を例にすれば、５００℃辺りまでは、毎分１．０〜５．０℃程度（樹脂の割合や粒度等の条件に応じて決定される。）の昇温速度とすべきである。 The moss particulate material prepared in this way, particularly the moss granule material of 4 mesh under, is then transferred to a step of firing and carbonizing in an inert gas atmosphere or in vacuum. It is necessary to maintain an oxygen-free condition such as in an inert gas atmosphere such as nitrogen gas or under vacuum so that the moss-containing granular material does not burn. Care should be taken to avoid sudden temperature rises so that the granular material does not collapse. In particular, in the vicinity of 200 to 400 ° C., a large amount of gas is generated due to decomposition. Therefore, sufficient consideration should be given to the rate of temperature increase during this period. In this case, the temperature increase rate should be about 1.0 to 5.0 ° C. per minute (determined depending on conditions such as the ratio of resin and particle size) up to around 500 ° C.
なお、焼成温度としては、この発明の多孔性炭素材粉末に必要とされる特性、例えば硬度や純度、多孔性や絶縁性、加工性や構造強度等々に応じ、略２００℃程度の温度から千数百度の範囲内の最適な温度が選択されることとなり、多孔性炭素材粉末の強度や密度等を左右する焼成具合に繋がる各種要素を勘案した上、最適な時間に渡って焼成が実施されるようにしなければならない。 The firing temperature ranges from about 200 ° C. to 1000 ° C. depending on the properties required for the porous carbon material powder of the present invention, such as hardness, purity, porosity, insulation, workability, structural strength, etc. An optimum temperature within the range of several hundred degrees will be selected, and firing will be carried out over the optimum time, taking into account various factors that lead to the degree of firing that affects the strength and density of the porous carbon material powder. I have to do so.
引き続き実施される炭化粒状麩糠類の冷却工程は、最終焼成温度から所定降温速度、例えば１．５℃／分程度の割合で常温まで冷却するものとし、それら常温に戻した炭化粒状麩糠類は、適宜粉砕機（アトマイザー）を使って粉砕する工程を経てから、振盪篩によって各段階毎の粒度のもの、例えば２５０ないし１００μｍ、１５０ないし１００μｍ、１５０μｍ以下、１００μｍ以下、５０ないし１０μｍ、１０μｍ以下等といった段階別のものに選別するようにし、需要者から求められることになるであろうと予測される各種高機能製品の性状、即ち、製品形状の複雑さ、それに起因した型詰めの難易度、構造強度、外観の緻密さ加減等の差異に対し、自在に対応可能とするこの発明の多孔性炭素材粉末が得られるようにするものである。 The subsequent cooling step of the carbonized granular rice cake is performed by cooling from the final firing temperature to room temperature at a predetermined rate of temperature reduction, for example, at a rate of about 1.5 ° C./min. Is appropriately pulverized using a pulverizer (atomizer), and then has a particle size of each stage by a shaking sieve, for example, 250 to 100 μm, 150 to 100 μm, 150 μm or less, 100 μm or less, 50 to 10 μm, 10 μm or less Etc., and the characteristics of various high-function products that are expected to be demanded by consumers, that is, the complexity of the product shape, the difficulty of mold filling caused by it, It is intended to obtain the porous carbon material powder of the present invention that can freely cope with differences such as structural strength and fineness of appearance.
また、関連する発明４の場合の製造方法における熱硬化性樹脂は、先の多孔性炭素材粉末を製造する際のものと変らないが、その混合割合は、先のものと異なり、主に所望の高機能製品とするために選択された所定粒度の多孔性炭素材粉末に、金型による成形性を付与する繋ぎ材として機能させ、合わせて焼成工程においてそれらを炭化してこの発明の多孔性炭素材の組成の一部に組み入れてしまうものであり、多孔性炭素材粉末９０ないし４０ｗ％に対し、熱硬化性樹脂が１０ないし４０ｗ％の割合の中から、多孔性炭素材粉末の粒度や含水率、素材温度等の条件に対応した最適な混合割合のものとして選択され、多孔性炭素材粉末と熱硬化性樹脂とによる混練物とするものである。 Further, the thermosetting resin in the production method in the case of the related invention 4 is not different from that in the previous production of the porous carbon material powder, but the mixing ratio is different from the previous one and mainly desired. The porous carbon material powder of a predetermined particle size selected to be a high-functional product of the present invention functions as a binder that imparts moldability with a mold, and carbonizes them in the firing step together to make the porosity of this invention It is incorporated into a part of the composition of the carbon material, and the particle size of the porous carbon material powder from the ratio of 10 to 40 w% of the thermosetting resin with respect to 90 to 40 w% of the porous carbon material powder. It is selected as an optimal mixing ratio corresponding to conditions such as moisture content and material temperature, and is a kneaded product of porous carbon material powder and thermosetting resin.
なお、この熱硬化性樹脂の混合工程において混練物とする際には、多孔性炭素材粉末への浸透率を吟味し、所定濃度の熱硬化性樹脂の混入に並行して適量の水を加えたり、あるいは、各種動植物糊料や澱粉、各種糖液等の繋ぎ剤を適量混合した水溶液を加えて実施されるようにしたり、あるいは、予め、成形性を良くするための水や繋ぎ剤混合液を、所定濃度の熱硬化性樹脂に混入したものとした上で混合、撹拌作業を実施して混練物となるようにする、先の混練状麩糠類とする際の熱硬化性樹脂の場合と同様の手段が排除されている訳ではなく、必要に応じて適宜採用することができるは言うまでもない。 In addition, when preparing a kneaded product in the mixing step of the thermosetting resin, the permeation rate into the porous carbon material powder is examined, and an appropriate amount of water is added in parallel with the mixing of the thermosetting resin of a predetermined concentration. Or by adding an aqueous solution in which an appropriate amount of binders such as various animal and vegetable pastes, starches, and various sugar solutions are mixed, or in advance, water or binder mixture for improving moldability. In the case of the thermosetting resin used in the above kneaded porcelain, which is mixed with the thermosetting resin of a predetermined concentration and then mixed and stirred to form a kneaded product Needless to say, the same means as in the above are not excluded and can be appropriately adopted as necessary.
金型内に充填した混練物は、成形品単位面積当り４０ないし４５０ｋｇ／ｃｍ２の圧力で加圧、成形するようにすべきであり、そして、それら成形品の焼成、炭化工程は、先の麩糠類粒状素材の場合の焼成、炭化工程のように、麩糠類の燃焼を配慮する必要がないことから、不活性ガス雰囲気中または真空中に限定されている訳ではなく、空気中であっても可能になる。 The kneaded material filled in the mold should be pressed and molded at a pressure of 40 to 450 kg / cm 2 per unit area of the molded product. Since it is not necessary to consider the burning of moss as in the firing and carbonization process of moss-like granular materials, it is not limited to an inert gas atmosphere or vacuum, but in the air. But it will be possible.
この工程における昇温速度は、最終焼成温度が５００℃以下の場合、室温から２５０℃までは１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分の実施されるものとし、その最終焼成温度で３時間保持した後、冷却工程では、１．５℃／分の降温速度で常温まで冷却されるようにし、最終焼成温度が５００℃を越える場合には、室温から２５０℃までは１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分、５００℃で１時間保持した上、５００℃から目的とする最終焼成温度まで２℃／分の昇温速度で昇温され、最終焼成温度で２時間保持した後、冷却工程では、１．５℃／分の降温速度で常温まで冷却されるようにしたものとするのが望ましい。 以下、上記したこの発明の多孔性炭素材粉末、およびその製造方法、ならびにそれら多孔性炭素材粉末を使った多孔性炭素材製品の製造方法が、更に具体的に把握できるようにするため、幾つかの実施例および関連実施例などを説示してみることにする。 In this step, when the final baking temperature is 500 ° C. or less, the temperature rise rate is 1.2 ° C./min from room temperature to 250 ° C., 1 ° C./min from 250 ° C. to 350 ° C., 1. After being held at the final firing temperature for 3 hours at the final firing temperature, the cooling step is performed to cool to room temperature at a temperature drop rate of 1.5 ° C./minute, and the final firing temperature is 500 ° C. In the case of exceeding 250 ° C., 1.2 ° C./min, from 250 ° C. to 350 ° C., 1 ° C./min, from 350 ° C. to 500 ° C., 1.2 ° C./min, and held at 500 ° C. for 1 hour. Above, the temperature is raised from 500 ° C. to the target final firing temperature at a rate of 2 ° C./minute, held at the final firing temperature for 2 hours, and then cooled at room temperature at a temperature drop rate of 1.5 ° C./minute. It is desirable that the cooling is performed. The porous carbon material powder of the present invention, the manufacturing method thereof, and the manufacturing method of the porous carbon material product using these porous carbon material powders will be described below in order to make it more concretely understood. Such an embodiment and related embodiments will be explained.
この事例は、麩糠類中で最も代表的な素材の一つである脱脂糠を採用し、特に硬質の多孔性炭素材粉末を製造する方法の代表的な実施例である。
「混合工程」
油を抽出した脱脂糠を５０メッシュの篩に掛け通過したものを用い、この脱脂糠７５ｗ％に、フェノ−ル樹脂［（株）ホ−ネンコ−ポレ−ション製 豊年レジングル−ｐｘ−１６００（商品名）］を熱硬化性樹脂として２５ｗ％になるように添加し、充分混合する。
「造粒工程」
揮発分を除去するため、８０℃に加熱しながら造粒し、４メッシュのフルイを通過したものを麩糠類粒状素材とする。
This case is a typical example of a method for producing a hard porous carbon material powder using a defatted soot, which is one of the most typical materials among moss.
"Mixing process"
The oil-extracted defatted rice cake was passed through a 50-mesh sieve, and 75% by weight of this defatted rice cake was added to phenol resin [Honen Resingle-px-1600, manufactured by Honenko-Poration Co., Ltd. (product) Name)] is added as a thermosetting resin so as to be 25% by weight and mixed well.
"Granulation process"
In order to remove volatile matter, the mixture is granulated while being heated to 80 ° C., and passed through a 4-mesh sieve to obtain a moss-like granular material.
「焼成工程」
焼成炉内で窒素ガスを流しながら焼成する。その際の昇温速度は、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃までを１℃／分、３５０℃から５００℃まで１．２℃／分、５００℃で１時間保持、５００℃から目的とする温度まで２℃／分、目的温度で２時間保持する。冷却は、１．５℃／分の割合で行う。
「粉砕工程」
常温にまで戻した炭化済みの麩糠類粒状素材は、粉砕機（アトマイザー）によって一旦粉砕した後、振盪篩によって選別して１００μｍ以下のこの発明の多孔性炭素材粉末を得る。
"Baking process"
Baking while flowing nitrogen gas in the baking furnace. In this case, the heating rate was 1.2 ° C./min from room temperature to 250 ° C., 1 ° C./min from 250 ° C. to 350 ° C., 1.2 ° C./min from 350 ° C. to 500 ° C., 1 hour at 500 ° C. Hold, hold from 500 ° C. to the target temperature at 2 ° C./min, at the target temperature for 2 hours. Cooling is performed at a rate of 1.5 ° C./min.
"Crushing process"
The carbonized porcelain granular material that has been returned to room temperature is once pulverized by a pulverizer (atomizer) and then selected by a shaking sieve to obtain a porous carbon material powder of the present invention having a thickness of 100 μm or less.
［関連実施例１］
次は、上記実施例１の製造方法によって得られた多孔性炭素材粉末を使って平板状の多孔性炭素材製品を製造する代表的な製造方法である。
「混合工程」
多孔性炭素材粉末７５ｗ％に、フェノ−ル樹脂［（株）ホ−ネンコ−ポレ−ション製豊年レジングル−ｐｘ−１６００（商品名）］を熱硬化性樹脂として２５ｗ％になるように添加し、充分混合して混練物とする。
[Related Example 1]
The following is a typical production method for producing a flat porous carbon material product using the porous carbon material powder obtained by the production method of Example 1 above.
"Mixing process"
Add a phenolic resin [Bonen Resin-plux-1600 (trade name) manufactured by Honen-Co., Ltd.] as a thermosetting resin to 75w% of the porous carbon material powder so as to be 25w%. Mix well to obtain a kneaded product.
「金型成形工程」
１４０〜１７０℃の温度範囲に設定した平板製品用の金型（７５×１５０×６ｍｍ）内に、混練物１００ｇを充填した上、ゲージ圧力５０ｋｇ／ｃｍ２で２分間加圧した後、解圧してガス抜きをする。ガス抜き後、再びゲージ圧力５０ｋｇ／ｃｍ２で３分間加圧して平板状成形品を得た。 なお、当該成形品の物性強化のため、さらに１５０〜２５０℃の温度範囲で加熱器による空中加熱処理を実施した。
"Mold molding process"
A flat plate mold (75 × 150 × 6 mm) set in a temperature range of 140 to 170 ° C. was filled with 100 g of the kneaded material, pressurized at a gauge pressure of 50 kg / cm 2 for 2 minutes, and then depressurized. Degas. After degassing, pressurization was again performed at a gauge pressure of 50 kg / cm 2 for 3 minutes to obtain a flat plate-shaped product. In addition, in order to reinforce the physical properties of the molded product, air heat treatment with a heater was further performed in a temperature range of 150 to 250 ° C.
「焼成工程」
焼成炉で窒素ガスを流し、無酸素状態にした上、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃までを１℃／分、３５０℃から５００℃まで１．２℃／分の割合で昇温させる昇温速度で焼成した上、５００℃状態を１時間保持し続けた後、再び５００℃から９００℃までを２℃／分で昇温させ、９００℃に達したところでその温度を２時間保持し続け、その後、１．５℃／分の割合で常温まで冷却する。
以上の工程を順次実施して、この発明の多孔性炭素材製品を製造することができる。
"Baking process"
Nitrogen gas was allowed to flow in the firing furnace to make it oxygen-free, and then 1.2 ° C / min from room temperature to 250 ° C, 1 ° C / min from 250 ° C to 350 ° C, 1.2 ° C / min from 350 ° C to 500 ° C. After firing at a rate of temperature rising at a rate of minutes and holding at 500 ° C. for 1 hour, the temperature was raised again from 500 ° C. to 900 ° C. at a rate of 2 ° C./minute, and reached 900 ° C. The temperature is kept for 2 hours and then cooled to room temperature at a rate of 1.5 ° C./min.
The porous carbon material product of the present invention can be manufactured by sequentially performing the above steps.
［関連実施例２］
上記実施例１の製造方法によって得た多孔性炭素材粉末を使って平板状の多孔性炭素材製品を製造する代表的な製造方法である。
「混合工程」
実施例１で得た多孔性炭素材粉末７５重量部と、ノボラック型粉体フェノ−ル樹脂［ＤＩＫ社製、フェノライト５５１０（商品名）］２５重量部とを充分混合して混練物とする。
[Related Example 2]
This is a typical production method for producing a flat porous carbon material product using the porous carbon material powder obtained by the production method of Example 1 above.
"Mixing process"
75 parts by weight of the porous carbon material powder obtained in Example 1 and 25 parts by weight of a novolac powder phenolic resin [manufactured by DIK, Phenolite 5510 (trade name)] are sufficiently mixed to obtain a kneaded product. .
「金型圧縮成型工程」
１４０〜１７０℃の温度範囲に設定した平板製品用の金型（厚さは材料の量、圧力によって変動することができる；７５×１５０×ｔｍｍ）内に、混練物１００ｇを充填した上、ゲージ圧５０ｋｇ／ｃｍ２で２分間加圧してから解圧してガス抜きをし、その後、再びゲージ圧５０ｋｇ／ｃｍ２で３分間加圧して平板状成形品とする。
"Mold compression molding process"
A mold for flat plate products set in a temperature range of 140 to 170 ° C. (thickness can vary depending on the amount of material and pressure; 75 × 150 × tmm) is filled with 100 g of the kneaded material, and a gauge After pressurizing at a pressure of 50 kg / cm 2 for 2 minutes, depressurizing and degassing, and then pressurizing again at a gauge pressure of 50 kg / cm 2 for 3 minutes to obtain a flat molded product.
「焼成工程」
焼成炉（外熱式、東海高熱社製）内で窒素ガスを流し、無酸素状態にした上、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分の昇温速度で焼成した上、５００℃の状態を１時間保持し続けた後、再び５００℃から９００℃までを２℃／分の昇温速度で焼成し、９００℃に達したところでその温度を２時間保持し続け、その後、６００℃までは１．２℃／分の速度で、６００℃から室温までは１．５℃／分の降温速度で降温し、常温まで冷却する。
以上の工程を順次実施して、この発明の多孔性炭素材製品を製造することができる。
"Baking process"
Nitrogen gas was allowed to flow in a firing furnace (external heat type, manufactured by Tokai Koyo Co., Ltd.) to make it oxygen-free, and then 1.2 ° C / min from room temperature to 250 ° C, 1 ° C / min from 250 ° C to 350 ° C, 350 After firing at a temperature increase rate of 1.2 ° C./minute from 500 ° C. to 500 ° C. and keeping the state of 500 ° C. for 1 hour, again from 500 ° C. to 900 ° C. at a temperature increase rate of 2 ° C./minute. When the temperature reaches 900 ° C., the temperature is maintained for 2 hours, and then the temperature is decreased to 600 ° C. at a rate of 1.2 ° C./min, and from 600 ° C. to room temperature at a rate of 1.5 ° C./min. Cool down to room temperature.
The porous carbon material product of the present invention can be manufactured by sequentially performing the above steps.
［関連実施例３］
上記実施例１の製造方法によって得た多孔性炭素材粉末を使って平板状（６０×１５×２ｍｍ）の多孔性炭素材製品を製造ようにした、この発明の他の例による製造方法である。
「混合工程」
実施例１で得た多孔性炭素材粉末７５重量部と、ノボラック型粉体フェノ−ル樹脂［ＤＩＫ社製、フェノライト５５１０（商品名）］２５重量部とをミキシング熱ロールで加熱混練し、得られた混練物をパワーミルで粉砕して、４ｍｍ×４ｍｍ×４ｍｍ以下の顆粒状成形材料を製造する。
[Related Example 3]
It is a manufacturing method according to another example of the present invention in which a porous carbon material product having a flat plate shape (60 × 15 × 2 mm) is manufactured using the porous carbon material powder obtained by the manufacturing method of Example 1 above. .
"Mixing process"
75 parts by weight of the porous carbon material powder obtained in Example 1 and 25 parts by weight of a novolac powder phenolic resin [manufactured by DIK, Phenolite 5510 (trade name)] were heated and kneaded with a mixing heat roll, The obtained kneaded material is pulverized with a power mill to produce a granular molding material of 4 mm × 4 mm × 4 mm or less.
「射出成型工程」
スクリュウ式射出成形機（松田製作所、７５Ｆ−３６Ｋ型）を用い、射出温度は入口８０℃、中間１００℃、出口ノズル１２０℃に設定し、また、金型温度は１８０℃に設定し、１１０ｋｇ／ｃｍ２の圧力を掛けて射出成形を実施する。
そして、射出成形品の製造サイクルは９０秒／１回として平板状成形品（１３×６４×３ｔ）とする。
"Injection molding process"
Using a screw type injection molding machine (Matsuda Seisakusho, 75F-36K type), the injection temperature was set to 80 ° C at the inlet, 100 ° C in the middle, and 120 ° C at the outlet nozzle, and the mold temperature was set to 180 ° C and 110 kg / Injection molding is performed with a pressure of cm2.
The production cycle of the injection-molded product is 90 seconds / one time to obtain a flat plate-shaped product (13 × 64 × 3t).
「焼成工程」
上記で得られた成形品をバッチ式焼成炉を用い、窒素ガス雰囲気中で、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分の昇温速度で焼成した上、５００℃の状態を１時間保持し続けた後、再び５００℃から９００℃までを２℃／分の昇温速度で焼成し、９００℃に達したところでその温度を２時間保持した。その後、６００℃までは１．２℃／分の速度で、６００℃から室温までは１．５℃／分の降温速度で降温し、常温まで冷却する。 以上の工程を順次実施して、この発明の多孔性炭素材製品を製造することができる。
"Baking process"
Using the batch-type firing furnace, the molded product obtained above is 1.2 ° C / min from room temperature to 250 ° C, 1 ° C / min from 250 ° C to 350 ° C, from 350 ° C to 500 ° C. After baking at a heating rate of 1.2 ° C./min and keeping the state at 500 ° C. for 1 hour, the baking is again performed from 500 ° C. to 900 ° C. at a heating rate of 2 ° C./min. The temperature was maintained for 2 hours. Thereafter, the temperature is lowered to 600 ° C. at a rate of 1.2 ° C./min, and from 600 ° C. to room temperature at a rate of 1.5 ° C./min. The porous carbon material product of the present invention can be manufactured by sequentially performing the above steps.
「焼成工程」
上記で得られた成形品をバッチ式焼成炉を用い、窒素ガス雰囲気中で、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分の昇温速度で焼成した上、５００℃の状態を１時間保持し続けた後、再び５００℃から９００℃までを２℃／分の昇温速度で焼成し、９００℃に達したところでその温度を２時間保持した。その後、６００℃までは１．２℃／分の速度で、６００℃から室温までは１．５℃／分の降温速度で降温し、常温まで冷却する。 以上の工程を順次実施して、この発明の多孔性炭素材製品を製造することができる。
"Baking process"
Using the batch-type firing furnace, the molded product obtained above is 1.2 ° C / min from room temperature to 250 ° C, 1 ° C / min from 250 ° C to 350 ° C, from 350 ° C to 500 ° C. After baking at a heating rate of 1.2 ° C./min and keeping the state at 500 ° C. for 1 hour, the baking is again performed from 500 ° C. to 900 ° C. at a heating rate of 2 ° C./min. The temperature was maintained for 2 hours. Thereafter, the temperature is lowered to 600 ° C. at a rate of 1.2 ° C./min, and from 600 ° C. to room temperature at a rate of 1.5 ° C./min. The porous carbon material product of the present invention can be manufactured by sequentially performing the above steps.
［関連実施例４］
この実施例は、上記実施例１の製造方法によって得た多孔性炭素材粉末を使った更に他の例による製造方法である。
「混合工程」
実施例１で得た多孔性炭素材粉末５５重量部と、ノボラック型粉体フェノ−ル樹脂［ＤＩＫ社製、フェノライト５５１０（商品名）］２５重量部と、炭素繊維（ドナカーボ Ｓ−２４２、ドナック（株）製）２０重量部とをミキサーで混練して成形材料とする。
[Related Example 4]
This example is a manufacturing method according to still another example using the porous carbon material powder obtained by the manufacturing method of Example 1 above.
"Mixing process"
55 parts by weight of the porous carbon material powder obtained in Example 1, 25 parts by weight of a novolac-type powder phenol resin [manufactured by DIK, Phenolite 5510 (trade name)], and carbon fiber (Donna Carbo S-242, 20 parts by weight of Donac Co., Ltd.) is kneaded with a mixer to obtain a molding material.
「加圧成型工程」
金型温度１５０℃に設定した金型（７５×１５０×ｔｍｍ）に、１００ｇの上記成形材料を充填し、ゲージ圧４０ｋｇ／ｃｍ２で２分間加圧してから解圧してガス抜きをする。その後、ゲージ圧４０ｋｇ／ｃｍ２で２分間加圧し、更にその後１分解圧、再度ゲージ圧６０ｋｇ／ｃｍ２で２分間加圧することによって成形品となし、該成形品を２００℃の加熱器に５時間放置し熱処理（アフターキュア）を行い、この発明の多孔性炭素材製品を製造するものである。
"Pressure molding process"
A mold (75 × 150 × tmm) set at a mold temperature of 150 ° C. is filled with 100 g of the molding material, pressurized at a gauge pressure of 40 kg / cm 2 for 2 minutes, and then depressurized and degassed. Thereafter, pressurization was performed at a gauge pressure of 40 kg / cm 2 for 2 minutes, and after that, a molded product was formed by pressurizing at 1 decomposition pressure and again at a gauge pressure of 60 kg / cm 2 for 2 minutes, and the molded product was left in a 200 ° C. heater for 5 hours. Heat treatment (after cure) is performed to produce the porous carbon material product of the present invention.
「加圧成型工程」
金型温度１５０℃に設定した金型（７５×１５０×ｔｍｍ）に、１００ｇの上記成形材料を充填し、ゲージ圧４０ｋｇ／ｃｍ２で２分間加圧してから解圧してガス抜きをする。その後、ゲージ圧４０ｋｇ／ｃｍ２で２分間加圧し、更にその後１分解圧、再度ゲージ圧６０ｋｇ／ｃｍ２で２分間加圧することによって成形品となし、該成形品を２００℃の加熱器に５時間放置し熱処理（アフターキュア）を行い、この発明の多孔性炭素材製品を製造するものである。
"Pressure molding process"
A mold (75 × 150 × tmm) set at a mold temperature of 150 ° C. is filled with 100 g of the molding material, pressurized at a gauge pressure of 40 kg / cm 2 for 2 minutes, and then depressurized and degassed. Thereafter, pressurization was performed at a gauge pressure of 40 kg / cm 2 for 2 minutes, and after that, a molded product was formed by pressurizing at 1 decomposition pressure and again at a gauge pressure of 60 kg / cm 2 for 2 minutes, and the molded product was left in a 200 ° C. heater for 5 hours. Heat treatment (after cure) is performed to produce the porous carbon material product of the present invention.
実施例１において、フェノール樹脂を以下のようにコラーゲン入り水溶液に変えて麩糠類粒状素材を作製するようにした外は、実施例１と同様の工程を経て多孔性炭素材粉末を得るようにした上、麩糠類９５重量部に対し、１重量％の濃度のコラーゲン入り水溶液５重量部を散布して攪拌した後、デスクペレッター（ダルトン社製Ｆ−２０／１２−３３０型）でペレット直径φ５×Ｌ１０のペレットを製造する。 In Example 1, a porous carbon material powder is obtained through the same steps as in Example 1 except that the phenol resin is changed to an aqueous solution containing collagen as described below to produce a moss-like granular material. In addition, 95 parts by weight of moss was sprayed with 5 parts by weight of a collagen-containing aqueous solution having a concentration of 1% by weight and stirred, and then pelleted with a desk pelleter (F-20 / 12-330 type manufactured by Dalton). A pellet having a diameter of φ5 × L10 is manufactured.
（実施例などの作用）
以上のとおりの工程によって構成されるこの発明の多孔性炭素材は、多孔性炭素材粉末の原材料として機能するもので、この発明の多孔性炭素材を製造する者がその製造をする傍ら、所望の多孔性炭素材粉末とするために予め所定量をストックして、需要者から求められることになるであろうと予測される高機能製品の性状に拘わらず、予め炭化粒状麩糠類を適宜粉砕機（アトマイザー）で粉砕し、振盪篩によって各段階毎の粒度のもの、例えば２５０ないし１００μｍ、１５０ないし１００μｍ、１５０μｍ以下、１００μｍ以下、５０ないし１０μｍ、１０μｍ以下等といった段階別のものに選別、用意しておき、高機能製品が特定された後、直ちにその性状、即ち、製品形状の複雑さ、それに起因した型詰めの難易度、構造強度、外観の緻密さ加減等に適合した最適な粒度のこの発明の多孔性炭素材粉末を選択した上、それら多孔性炭素材粉末に対する熱硬化性樹脂の混合割合（９０〜４０ｗ％）：（１０〜６０ｗ％）の範囲から、これまた対象とする高機能製品の性状を勘案した最適割合となるよう熱硬化性樹脂を混合して混練物とし、金型成形工程を経て成形物を得て焼成、炭化工程を実施し、この発明による多孔性炭素材製品を製造するようにするか、あるいはそれ自体が商取引きの対象とされ、この発明の多孔性炭素材を購入した者が、それを原材料として自らの高機能製品に最適な粒度の多孔性炭素材粉末にするような用い方をすることもできる。
(Effects of Examples etc.)
The porous carbon material of the present invention constituted by the steps as described above functions as a raw material of the porous carbon material powder. While the person who manufactures the porous carbon material of the present invention manufactures the porous carbon material, it is desired. In order to obtain a porous carbon material powder, a predetermined amount is stocked in advance, and carbonized granular rice cake is appropriately crushed in advance, regardless of the properties of high-function products that are expected to be demanded by consumers. Pulverized by a machine (atomizer), and classified by stage using a shaking sieve, such as 250 to 100 μm, 150 to 100 μm, 150 μm or less, 100 μm or less, 50 to 10 μm, 10 μm or less, etc. In addition, immediately after a high-performance product is identified, its properties, that is, the complexity of the product shape, the difficulty of mold filling resulting from it, the structural strength, and the fineness of the appearance. After selecting the porous carbon material powder of the present invention having an optimum particle size suitable for the degree of adjustment, the mixing ratio of the thermosetting resin to the porous carbon material powder (90 to 40 w%): (10 to 60 w%) From this range, a thermosetting resin is mixed into a kneaded product so as to obtain an optimum ratio considering the properties of the target high-functional product, and a molded product is obtained through a mold forming process, followed by firing and carbonizing processes. To implement a porous carbon material product according to the present invention, or as such is subject to commerce, and a person who has purchased the porous carbon material of the present invention uses it as a raw material for It can also be used in the form of a porous carbon material powder having the optimum particle size for functional products.
多孔性炭素材の製造方法では、主原料となる麩糠類に熱硬化性樹脂、および適量の糊料入り水溶液または水をを加えて混練した混練状麩糠類は、焼成工程における円滑なガス抜きを実現し得るよう、予め５メッシュアンダーに粒度調整、造粒する工程を不可欠とし、焼成工程における焼失防止等のため、不活性ガス雰囲気中または真空中で、所定の昇温速度に従って所望する最終焼成温度にまで達しさせて焼成、炭化する焼成工程と、最終焼成温度から所定降温速度で常温まで冷却する工程とを必須の構成要件と、また、多孔性炭素材粉末の製造方法では、どのような性状の高機能製品の製造も可能にする粉末化工程とを必須の構成要件としており、こうして各種サイズの多孔性炭素材粉末を予め十分に製造、ストックすることになる結果、この発明が包含する多孔性炭素材製品製造への移行が円滑になし得るものとなる。 In the method for producing a porous carbon material, a kneaded cake obtained by adding a thermosetting resin and an appropriate amount of a paste-containing aqueous solution or water to a koji as a main raw material is a smooth gas in the firing step. In order to achieve removal, it is essential to adjust the particle size to 5 mesh under and granulate in advance, and in order to prevent burnout in the firing process, etc., in an inert gas atmosphere or in vacuum, according to a predetermined rate of temperature increase In the manufacturing method of the porous carbon material powder, which is an essential constituent requirement for the firing step of reaching the final firing temperature and firing and carbonizing, and the step of cooling from the final firing temperature to room temperature at a predetermined temperature-decreasing rate, As a result of the fact that the powdering process that enables the production of high-performance products with such properties is an essential constituent requirement, porous carbon material powders of various sizes are sufficiently produced and stocked in advance, Invention the transition to encompass the porous carbon material product manufactured becomes to be made smoothly in.
なお、以下には、この発明の技術的思想に基づく上記した実施例および関連実施例によって得られた多孔性炭素材製品の物性を、次の参考例のもののそれと比較して示すことにより、後述するこの発明の効果がより明確なものとなるようにする。
《参考例１》
５０メッシュの篩に掛け通過した脱脂糠７５重量部と、フェノ−ル樹脂［（株）ホ−ネンコ−ポレ−ション製 豊年レジングル−ｐｘ−１６００（商品名）］２５重量部とを充分混合して混練物を得た上、揮発分を除去するため、８０℃に加熱しながら造粒し、１２メッシュの篩を通過したものを原材料となし、該原材料１５ｇをヒーター付金型（内径４２ｍｍ、長さ６０ｍｍ）に充填した上、ハイプレッシャージャッキー（シリンダー内径２１ｍｍ）によってゲージ圧３００ｋｇ／ｃｍ２、温度１８０℃まで加熱しながら成形、製造する。途中、数回ガス抜きのため、ゲージ圧７０ｋｇ／ｃｍ２程度まで圧力を下げて水分や分解ガスを抜いている。
In the following, the physical properties of the porous carbon material products obtained by the above-described examples and related examples based on the technical idea of the present invention will be described later by comparing with those of the following reference examples. The effect of the present invention is made clearer.
<< Reference Example 1 >>
75 parts by weight of defatted rice cake passed through a 50 mesh sieve and 25 parts by weight of phenol resin [Honen Resin-px-1600 (trade name) manufactured by Honenco Corporation] are mixed thoroughly. In order to remove the volatile matter, the mixture was granulated while being heated to 80 ° C., and passed through a 12 mesh sieve as a raw material, and 15 g of the raw material was heated to a die with a heater (inner diameter 42 mm, And is molded and manufactured while being heated to a gauge pressure of 300 kg / cm 2 and a temperature of 180 ° C. by a high pressure jacky (cylinder inner diameter of 21 mm). On the way, in order to degas several times, the pressure is lowered to a gauge pressure of about 70 kg / cm 2 and water and decomposition gas are extracted.
焼成炉に窒素ガスを流しながら、室温から２５０℃まで１．２℃／分、２５０℃から３５０℃まで１℃／分、３５０℃から５００℃まで１．２℃／分の昇温速度で焼成した上、５００℃の状態を１時間保持し続けた後、再び５００℃から９００℃までを２℃／分の昇温速度で焼成し、９００℃に達したところでその温度を２時間保持し続けた後、１．５℃／分の降温速度で６００℃まで冷却し、その後常温までは自然冷却して多孔性炭素材製品としたものである。 Firing at a rate of 1.2 ° C / min from room temperature to 250 ° C, 1 ° C / min from 250 ° C to 350 ° C, and 1.2 ° C / min from 350 ° C to 500 ° C while flowing nitrogen gas through the firing furnace In addition, after maintaining the state of 500 ° C. for 1 hour, it was fired again from 500 ° C. to 900 ° C. at a rate of 2 ° C./min. When the temperature reached 900 ° C., the temperature was maintained for 2 hours. After that, it is cooled to 600 ° C. at a temperature lowering rate of 1.5 ° C./min, and then naturally cooled to room temperature to obtain a porous carbon material product.
《試験例１》
上記で得た実施例３、４、および参考例１の多孔性炭素材製品について物性を評価した結果が表１に示され、また、実施例５の成形品についてもその物性を評価した結果が表２に示されている。なお、表中、各項目は以下のようにして評価している。
嵩 比 重 ： 一定重量（１００ｇ）の試料をメスシリンダーに採り、その容量を読 んで重量／容量を計算。
真 比 重 ： ＪＩＳ Ｒ１６２０（ピクノメーター法）に従った測定。
曲げ応力 ： ＪＩＳ Ｒ１６０１（３点法）に従い、インストロン型材料試験機を 用い、２０℃、６５％ＲＨの環境下で測定。
圧縮応力 ： ＪＩＳ Ｒ１６０８に従った測定。
熱膨張係数 ： ＪＩＳ Ｐ１６１８に従った測定。
焼成収縮率 ： 焼成前後の成形品をスケールで計測した上、焼成後／焼成前の比率を 計算。
摩擦係数 ： 往復摩擦試験装置（新東洋科学（株）製、ピンオンデスクＨＥＩＤＯ Ｎ−２２型）を用いた測定。
耐摩耗性 ： 往復摩擦試験装置（新東洋科学（株）製、ピンオンデスクＨＥＩＤＯ Ｎ−２２型）を用い、触針式表面粗さ計を使って摩擦方向に垂直に摩耗 痕の断面曲線を５ケ所測定し、これを基に摩耗体積を求めた上で、以下 の式（１）に従って比摩耗量を算出。ここで、Ｗｓは比摩耗量、Ｖは摩 耗体積、Ｗは垂直荷重、Ｌはすべり距離を示す。
<< Test Example 1 >>
The results of evaluating the physical properties of the porous carbon material products of Examples 3 and 4 and Reference Example 1 obtained above are shown in Table 1, and the results of evaluating the physical properties of the molded product of Example 5 are also shown. It is shown in Table 2. In the table, each item is evaluated as follows.
Bulk specific gravity: Take a sample of a constant weight (100 g) in a graduated cylinder, read the volume, and calculate the weight / volume.
True specific gravity: Measurement according to JIS R1620 (Pycnometer method).
Bending stress: Measured in an environment of 20 ° C. and 65% RH using an Instron type material testing machine according to JIS R1601 (3-point method).
Compressive stress: Measurement according to JIS R1608.
Thermal expansion coefficient: Measurement according to JIS P1618.
Firing shrinkage ratio: After measuring the molded product before and after firing on a scale, the ratio after firing / before firing is calculated.
Friction coefficient: Measurement using a reciprocating friction test apparatus (manufactured by Shin-Toyo Kagaku Co., Ltd., pin-on-desk HEIDO N-22 type).
Abrasion resistance: Using a reciprocating friction test device (manufactured by Shin-Toyo Kagaku Co., Ltd., pin-on-desk HEIDO N-22 type), using a stylus type surface roughness tester, the cross-sectional curve of the wear scar is perpendicular to the friction direction. After measuring the five locations and determining the wear volume based on this measurement, the specific wear amount was calculated according to the following equation (1). Here, Ws is the specific wear amount, V is the wear volume, W is the vertical load, and L is the slip distance.
気孔面積率は、試料表面を走査型レーザー顕微鏡（レーザーテック製）１ＬＭ２１を用いて観察し、プリンターに出力された写真をもとに、以下の式（２）に従って算出している。ここで、Ａｐは気孔面積、Ａａは全面積を示す。 The pore area ratio is calculated according to the following formula (2) based on a photograph output to a printer by observing the sample surface using a scanning laser microscope (manufactured by Lasertec) 1LM21. Here, Ap represents the pore area, and Aa represents the total area.
次に、加工性は、ドリリング加工、フライス加工、旋削加工、及び研削加工の各加工面における試料の加工のし易さを、専門家が判断した結果で評価し、次の表１にそれを示してある。
そして、電気抵抗値と体積固有抵抗値とについて比較したデータは、以下の表２に示すとおりである。
なお、電気抵抗値は、１×１×１ｔの試験片を作製し、デジタルマルチメーターカスタム（ＣＤＭ−２７Ｄ）で測定し、体積固有抵抗値についは、東亜電波工業製（ＳＭ−８００１）で、１００×１００×２ｔの試験片を作製することによって測定した。
In addition, an electrical resistance value produced a test piece of 1 × 1 × 1t, measured with a digital multimeter custom (CDM-27D), and a volume specific resistance value was manufactured by Toa Denpa Kogyo (SM-8001), Measurements were made by making 100 x 100 x 2t test specimens.
（実施例などの効果）
以上、各実験結果から明らかにされているとおり、関連実施例２等で得られる本願発明の多孔性炭素材製品は、焼成収縮率、曲げ応力、圧縮応力、耐摩耗性等が向上する外、加工性能に秀れたものとなり、また、関連実施例１で得られる多孔性炭素材は、多孔性炭素材製品製造の基をなす多孔性炭素材粉末の原材料として有効に使用し得ることが確認されたことから、この発明の効果として既述してあるとおり、需要者から要求された最終製品（高機能製品）の性状、例えば、製品形状の複雑さ、それに起因した型詰めの難易度、構造強度、外観の緻密さに応じ、その最終製品の製造に最適な粒径を有する多孔性炭素材粉末を適格に選択、採用可能にすることが裏付けられ、そして、この原材料を予め用意しておきさえすれば、どのような性状の高機能製品の製造も適格に対応可能にする多孔性炭素材粉末が得られ、また、最適な多孔性炭素材粉末を用い、次の工程である多孔性炭素材粉末と樹脂とを混合し、成形、焼成するという工程を経ることによって最終製品の製造を開始することができ、多孔性炭素材製品を迅速に製造することができるという効果を奏するものとなる。
(Effects of Examples etc.)
As described above, as clarified from the results of each experiment, the porous carbon material product of the present invention obtained in Related Example 2 and the like is improved in firing shrinkage rate, bending stress, compressive stress, wear resistance, etc. It was confirmed that the porous carbon material obtained in the related example 1 can be effectively used as a raw material for the porous carbon material powder that forms the basis of the production of the porous carbon material product. Therefore, as already described as the effect of the present invention, the properties of the final product (high-function product) requested by the customer, for example, the complexity of the product shape, the difficulty of mold filling caused by it, It is proved that the porous carbon material powder having the optimum particle size for the production of the final product can be selected and adopted according to the structural strength and the fineness of the appearance, and this raw material is prepared in advance. What kind of sex Porous carbon material powder that enables the production of high-functional products in a qualified manner can be obtained, and the optimal porous carbon material powder is used to mix the porous carbon material powder, which is the next step, and resin. The final product can be manufactured through the steps of molding and firing, and the porous carbon material product can be rapidly manufactured.
（結 び）
叙上の如く、この発明は、既に開発、実用化済みとなっているの多孔性炭素材粉末の製造方法の弱点を完全に補填し、脱脂糠を始めとし、小麦をひいて粉にしたときに皮屑として出る麩、更には、籾殻や蕎麦殻、大豆殻、グルテンフィード等、穀類を加工処理する過程で発生する微細な粉末状あるいは粉砕処理した皮殻等といった、これまでは主として農業用資材としてしか利用方法のなかった麩糠類を、極めて応用範囲の広い工業用資材、特に高機能製品として効率的且つ経済的に有効活用可能にするものであって、先の発明共々、セラミックス素材を必要とする広い範囲の分野への進出を確実なものとして、その普及、拡大が図られるものと予想されることから、麩糠類処理加工業者にとっては職域の拡大の引き金として期待が高まるだけではなく、各種工業製品製造業者や一般ユーザー、ひいては麩糠類の取り扱いに苦慮してきた農業生産業者からもその有用性が高く評価されるものになると予想される。
(Conclusion)
As mentioned above, the present invention completely compensates for the weakness of the production method of porous carbon material powder that has already been developed and put to practical use. In the past, mainly rice for agriculture, such as fine powdered or crushed shells produced during the processing of cereals such as rice husk, buckwheat husk, soybean husk, gluten feed, etc. It is possible to effectively use moss that has been used only as a material for industrial materials with a very wide range of application, especially as high-performance products, in an efficient and economical manner. As a certainty, it is expected that it will spread and expand into a wide range of fields that require food, so expectation will increase as a trigger for the expansion of the occupational area for slaughter processing processors Rather, various industrial products manufacturers and general users, is expected to be those that are also highly evaluated its usefulness from agricultural producers, which has been struggling in the handling of the thus Fusumanukarui.
Claims (3)
A step of adding a thermosetting resin and an appropriate amount of an aqueous solution containing glue or water to kneads such as rice bran and koji under 20 mesh, and kneading these kneaded rice cakes to 60 to 80 ° C. Then, after drying and granulating while removing volatile substances, sieving into 4 mesh under and selecting to make moss granular material, these moss granular material in inert gas atmosphere or The temperature is raised in vacuum according to a predetermined temperature increase rate, and the final baking temperature is calcined and carbonized at a temperature of 700 ° C. or higher, and the carbonized particulates are cooled from the final baking temperature to room temperature at a predetermined temperature decrease rate. 2. The process, the process of pulverizing the cooled porous carbon material obtained in these processes and pulverizing it to a desired particle size, and the above-mentioned processes are sequentially passed. Of porous carbon material powder Law.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009080665A JP2009173540A (en) | 2002-09-27 | 2009-03-27 | Porous carbon material powder and method of manufacturing the same |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002283666 | 2002-09-27 | ||
| JP2009080665A JP2009173540A (en) | 2002-09-27 | 2009-03-27 | Porous carbon material powder and method of manufacturing the same |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2003320344A Division JP4328591B2 (en) | 2002-09-27 | 2003-09-11 | Porous carbon material, method for producing the same, and method for producing a porous carbon material product using the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2009173540A true JP2009173540A (en) | 2009-08-06 |
Family
ID=34260178
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2009080665A Pending JP2009173540A (en) | 2002-09-27 | 2009-03-27 | Porous carbon material powder and method of manufacturing the same |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP2009173540A (en) |
| KR (1) | KR20040027447A (en) |
| CN (1) | CN1496957A (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101000955B (en) * | 2006-01-09 | 2010-11-03 | 英耐时有限公司 | Negative electrode carbon material for lithium ion secondary battery and its manufacturing method |
| JP2009538811A (en) * | 2006-05-31 | 2009-11-12 | マックス−プランク−ゲゼルシャフト ツア フェルデルンク デア ヴィッセンシャフテン エー．ファウ． | Method for producing porous carbon casting |
| KR100934386B1 (en) * | 2008-04-17 | 2009-12-30 | 김은경 | Manufacturing method of carbon composite panel |
| CN102164851A (en) * | 2008-09-29 | 2011-08-24 | 日清奥利友集团株式会社 | Burned plant material and electromagnetic shielding member |
| KR101123586B1 (en) * | 2010-07-08 | 2012-03-21 | 한서대학교 산학협력단 | A production method of high porosity carbon |
| CN103647082B (en) * | 2013-12-24 | 2016-05-04 | 中国船舶重工集团公司第七一二研究所 | The preparation method of the hard carbon microsphere cathode material of a kind of lithium rechargeable battery |
| DK2954951T3 (en) * | 2014-06-11 | 2023-09-18 | Heraeus Deutschland Gmbh & Co Kg | SUPPORTED CATALYST AND METHOD FOR PRODUCING A POROUS GRAPHITIZED CARBON MATERIAL COATED WITH METAL NANOPARTICLES |
| CN109384454A (en) * | 2018-10-26 | 2019-02-26 | 陕西科技大学 | A kind of environment-friendly type anion porous brick and its preparation method and application |
| KR20230113864A (en) | 2022-01-24 | 2023-08-01 | 동의대학교 산학협력단 | Manufacturing method of high-purity carbon material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04328591A (en) * | 1991-04-30 | 1992-11-17 | Minolta Camera Co Ltd | Laser printer |
| JPH10101453A (en) * | 1996-10-01 | 1998-04-21 | Sanwa Yushi Kk | Production of porous carbon material product and hard porous carbon material product |
| JP2002187774A (en) * | 2000-12-15 | 2002-07-05 | Minebea Co Ltd | Material for bearing rolling element |
-
2003
- 2003-09-26 CN CNA031514863A patent/CN1496957A/en active Pending
- 2003-09-26 KR KR1020030066868A patent/KR20040027447A/en not_active Application Discontinuation
-
2009
- 2009-03-27 JP JP2009080665A patent/JP2009173540A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04328591A (en) * | 1991-04-30 | 1992-11-17 | Minolta Camera Co Ltd | Laser printer |
| JPH10101453A (en) * | 1996-10-01 | 1998-04-21 | Sanwa Yushi Kk | Production of porous carbon material product and hard porous carbon material product |
| JP2002187774A (en) * | 2000-12-15 | 2002-07-05 | Minebea Co Ltd | Material for bearing rolling element |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1496957A (en) | 2004-05-19 |
| KR20040027447A (en) | 2004-04-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP2009173540A (en) | Porous carbon material powder and method of manufacturing the same | |
| JP4328591B2 (en) | Porous carbon material, method for producing the same, and method for producing a porous carbon material product using the same | |
| JP3530329B2 (en) | Method for manufacturing porous carbon material product | |
| JP6224678B2 (en) | Grinding expanded graphite agglomerate, method for producing the same, and use thereof | |
| Nida et al. | 3D printing of grinding and milling fractions of rice husk | |
| Ghasemi et al. | Optimization of pelleting and infrared-convection drying processes of food and agricultural waste using response surface methodology (RSM) | |
| CN105800610B (en) | A kind of preparation method of binder free coal base agglomerated activated carbon | |
| Puspasari et al. | Drying kinetics of oil palm frond particles in an agitated fluidized bed dryer | |
| JPS6223642B2 (en) | ||
| AU2019257750A1 (en) | High temperature bio-char carbonization, micron grinding and classification | |
| Zhang et al. | Ultrasonic vibration-assisted pelleting of cellulosic biomass for ethanol manufacturing: An investigation on pelleting temperature | |
| CN101168677A (en) | Method for producing high-strength post-forming biomass charcoal | |
| Wojdalski et al. | Production and Properties of Apple Pomace Pellets and their Suitability for Energy Generation | |
| JP3060389U (en) | Porous carbon material products formed from fusarium | |
| Jubu et al. | Determination of the thermal properties of groundnut shell particles reinforced polymer composite | |
| JP2007016072A (en) | Method for producing porous carbon material | |
| CN105754360B (en) | A kind of straw base wood moulding heating floor and based on fluorine processing under floor processing method | |
| Tumuluru et al. | Binding Mechanism, Densification Systems, Process Variables, and Quality Attributes | |
| JP3127308B2 (en) | Granulation method of organic fertilizer | |
| Arul Kumar et al. | Mechanical, physical and chemical properties of saw dust briquette | |
| KR100521653B1 (en) | Preparation of sweet potato pulp anthracite blended briquettes | |
| Dalimunthe et al. | Physical Properties of Varied Composition of Peanut Shell and Palm Oil Shell’s Briquettes | |
| WO2023175934A1 (en) | Method for producing solid biomass fuel | |
| Van Quyen et al. | DEVELOPMENT OF SINGLE PELLETIZER UNIT FOR MODELLING FLAT DIE PELLETIZER | |
| Witdarko et al. | The Effect of Compacting Pressure on the Quality of Rice Husk Charcoal Briquettes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20100615 |
|
| A02 | Decision of refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A02 Effective date: 20110510 |