JPS62132717A - Manufacture of bonded carbonaceous product - Google Patents
Manufacture of bonded carbonaceous productInfo
- Publication number
- JPS62132717A JPS62132717A JP60272611A JP27261185A JPS62132717A JP S62132717 A JPS62132717 A JP S62132717A JP 60272611 A JP60272611 A JP 60272611A JP 27261185 A JP27261185 A JP 27261185A JP S62132717 A JPS62132717 A JP S62132717A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- bonded
- adhesive
- product
- prepolymer
- 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
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- Carbon And Carbon Compounds (AREA)
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は複数の炭素質製品の接合方法に関し、とくに炭
素質製品間の接着力が大きく、かつ、複雑形状もしくは
大型形状の炭素質製品を簡単に製造する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for joining a plurality of carbonaceous products, and in particular, the present invention relates to a method for joining a plurality of carbonaceous products, and in particular, a method for bonding carbonaceous products with a large adhesion force between the carbonaceous products and a complicated or large shape. Concerning an easy manufacturing method.
熱硬化性樹脂の成形品を原料にして炭素質製品を製造す
る技術は知られている。すなわち特公昭４９１９９９９
、特開昭５９−１６２１１２、特開昭５９−３５０１
１ 、特開昭５７−５１１０９の各公報には、熱硬化性
樹脂の１種であるフェノール樹脂を原料成分の１部とし
て用いた成形品を焼成し、炭素質製品を製造する技術が
示されている。Techniques for manufacturing carbonaceous products using thermosetting resin molded articles as raw materials are known. In other words, Special Publick Showa 4919999
, JP-A-59-162112, JP-A-59-3501
1. Japanese Unexamined Patent Publication No. 57-51109 discloses a technology for producing carbonaceous products by firing molded products using phenolic resin, which is a type of thermosetting resin, as part of the raw material components. ing.
また米国特許３１２１０５０ 、特開昭５９−１４６９
１７、特開昭６０−３６３１６の各公報には、フェノー
ル樹脂発泡体を焼成し、炭素質製品を製造する技術が示
されている。Also, U.S. Patent No. 3121050, JP 59-1469
17 and Japanese Patent Application Laid-Open No. 60-36316 disclose a technique for producing a carbonaceous product by firing a phenolic resin foam.
ところで、従来から知られているこれらの製造方法によ
って得られる炭素質製品は、その高耐熱性を生かして航
空機や宇宙船の外装材、内装材あるいは高温炉の外装材
、内装材に利用されようとしている。これらの用途に利
用される場合、その形状は大型でしかも複雑な形のもの
を要求されることがしばしば発生する。比較的小さな形
状であれば、複雑な形であっても、熱硬化性樹脂を原料
とする限り、樹脂の成形技術を応用して予め所望形状に
成形し焼成、炭素化することにより、目的とする形状の
炭素質製品を得ることは可能である。By the way, the carbonaceous products obtained by these conventionally known manufacturing methods can be used as exterior and interior materials for aircraft and spacecraft, as well as exterior and interior materials for high-temperature furnaces, by taking advantage of their high heat resistance. It is said that When used for these purposes, the shape is often required to be large and complex. Even if the shape is relatively small or complex, as long as thermosetting resin is used as the raw material, it can be molded into the desired shape in advance using resin molding technology, fired, and carbonized. It is possible to obtain carbonaceous products in the form of
しかし、大型形状であると、実質的に成形が難しく、こ
のような方法を採用することはできない。However, if the shape is large, molding is substantially difficult, and such a method cannot be adopted.
そこで、従来は炭素質製品の複数を接着剤にて接合し、
所望形状となしたのち、再度焼成して接着層を炭素化し
て大型、複雑形状品を得ていた。しかし、この方法によ
ると接着層の接着力が弱くて本体となる炭素質製品同志
が強固に一体化したものが得られなかったり、焼成時に
接着層部分と炭素質製品部分の収縮度合が異なるためク
ラックが生じたり、ひどい場合には割れてしまうという
ことが頻繁に生じていた。Therefore, in the past, multiple carbon products were bonded together using an adhesive.
After forming the desired shape, the adhesive layer was carbonized by firing again to obtain a large, complex-shaped product. However, with this method, the adhesive strength of the adhesive layer is weak and the carbonaceous product that forms the main body cannot be firmly integrated, and the degree of shrinkage between the adhesive layer and the carbonaceous product differs during firing. Cracks often occurred, or in severe cases, they broke.
本発明者らは、かかる現状に鑑み、強固に一体化した炭
素質製品を簡単かつ生産性よく製造する方法につき研究
を重ねた結果、以下に示すような製法によれば目的を達
成できることを見出した。In view of the current situation, the inventors of the present invention have conducted repeated research on a method for manufacturing a strongly integrated carbonaceous product easily and with high productivity, and have found that the purpose can be achieved by the manufacturing method shown below. Ta.
すなわち、本発明は実質的に同一の熱硬化性樹脂からな
る樹脂成形品および／または発泡樹脂成形品の複数を、
（ｉｌ＋ 該熱硬化性樹脂の原料であるプレポリマー
と本質的に同一のプレポリマー、
（ｂｌ ン容媒、
（Ｃ１硬化剤、
とからなる接着剤で接合し、次いで該接合品を非酸化性
雰囲気で焼成、炭素化することを特徴とする接合された
炭素質製品の製造方法である。That is, the present invention provides a plurality of resin molded articles and/or foamed resin molded articles made of substantially the same thermosetting resin, (il+) a plurality of resin molded articles and/or foamed resin molded articles made of substantially the same thermosetting resin. Production of a bonded carbonaceous product characterized by bonding with an adhesive consisting of a polymer, (Bln container, (C1 hardening agent), and then firing and carbonizing the bonded product in a non-oxidizing atmosphere. It's a method.
本発明の製造方法で用いる熱硬化性樹脂成形品および／
または熱硬化性樹脂発泡成形品の複数は、いずれも実質
的に同一の熱硬化性樹脂よりなる。Thermosetting resin molded product and/or used in the manufacturing method of the present invention
Alternatively, the plurality of thermosetting resin foam molded products are all made of substantially the same thermosetting resin.
このとき熱硬化性樹脂発泡成形品を選択すれば、焼成後
に得られる炭素質製品は多孔質となるので、軽量で断熱
性にぼれたものとなる。一方、発泡体ではない熱硬化性
樹脂成形品を選択すれば。高強度の炭素質製品を得るこ
とができる。If a thermosetting resin foam molded product is selected at this time, the carbonaceous product obtained after firing will be porous, making it lightweight and with excellent heat insulation properties. On the other hand, if you choose a thermosetting resin molded product instead of a foam. High strength carbonaceous products can be obtained.
熱硬化性樹脂としては、如何なるものも利用でき、たと
えばポリウレタン、ポリイソシアネ−１・、ポリイミド
、フェノール樹脂、フルフラール樹脂、ユリア樹脂、エ
ポキシ樹脂、アクリル樹脂、ピラニル樹脂、フラン樹脂
あるいはこれらの各種変性物たとえばエポキシ変性フェ
ノール樹脂、メラミン変性ユリア樹脂、エポキシ変性ピ
ラニル樹脂、ウレタン変性ピラニル樹脂などを例示する
ことができる。Any thermosetting resin can be used, such as polyurethane, polyisocyanate-1, polyimide, phenol resin, furfural resin, urea resin, epoxy resin, acrylic resin, pyranyl resin, furan resin, or various modified products thereof, such as Examples include epoxy-modified phenol resin, melamine-modified urea resin, epoxy-modified pyranyl resin, and urethane-modified pyranyl resin.
前記熱硬化性樹脂成形品、発泡成形品から選ばれる複数
の成形品を所望形状に接合するために用いられる接着剤
は、前述のｔａ）、［ｂ）および（Ｃ）よりなる。The adhesive used to join a plurality of molded products selected from the thermosetting resin molded products and foamed molded products into a desired shape consists of the above-mentioned ta), [b) and (C).
すなわち、（ａ）のプレポリマーは、たとえば熱硬化性
樹脂の成形品（発泡成形品）がフェノール樹脂の場合に
はレゾール型フェノール樹脂あるいはノボラック型フェ
ノール樹脂を用い、フラン樹脂の成形品の場合にはフル
フリルアルコール縮合物あるいはフルフリルアルコール
とホルマリンの縮合物を用いるように、成形品を構成す
る熱硬化性樹脂の原料であるプレポリマーと実質的に同
一のプレポリマーを用いる。That is, for the prepolymer (a), for example, if the thermosetting resin molded article (foamed molded article) is a phenolic resin, a resol type phenolic resin or a novolak type phenolic resin is used, and in the case of a furan resin molded article, a resol type phenolic resin or a novolac type phenolic resin is used. uses substantially the same prepolymer as the raw material of the thermosetting resin constituting the molded article, such as using a furfuryl alcohol condensate or a condensate of furfuryl alcohol and formalin.
（ｂｌの溶媒は、プレポリマーを熔解もしくは分散せし
める能力を有し、かつ、揮発性の高いものが好ましく、
たとえばメタノール、エタノール、プロパツール、イソ
プロパツール等のアルコール類、エチレングリコール等
のグリコール類、アセトン、メチルエチルケトン等のケ
トン類、酢酸エステル等のエステル類、ジメチルエーテ
ル等のエーテル類、ベンゼン、ｌ・ルエン、キシレン、
ヘキサン等の炭化水素類、四塩化炭素等のハロゲン化炭
化水素類、水あるいはこれらの混合物を例示することが
できる。これらは、（実用するプレポリマーのン容解度
指数にあわせて適宜選択されるが、とくに好ましくは、
成形品への漏れをよくするためつまり成形品表面に接着
剤が均一に塗布できるように、メタノールやエタノール
等のアルコール類を単独または他の溶媒と混合して用い
る。(The solvent for bl is preferably one that has the ability to melt or disperse the prepolymer and has high volatility,
For example, alcohols such as methanol, ethanol, propatool, isopropanol, glycols such as ethylene glycol, ketones such as acetone, methyl ethyl ketone, esters such as acetate, ethers such as dimethyl ether, benzene, l-toluene, xylene,
Examples include hydrocarbons such as hexane, halogenated hydrocarbons such as carbon tetrachloride, water, and mixtures thereof. These are selected as appropriate depending on the solubility index of the prepolymer to be used, but are particularly preferably:
In order to improve leakage into the molded product, that is, so that the adhesive can be applied uniformly to the surface of the molded product, alcohols such as methanol and ethanol are used alone or in combination with other solvents.
硬化剤ＦＣ）は、プレポリマー成分＋ａ）を硬化せしめ
るのに使用されるものであれば如何なるものでもよ（、
たとえばプレポリマーがレゾール型フェノール樹脂−や
フルフリルアルコール縮合物の場合には硫酸、塩酸、硝
酸、リン酸、酢酸、フェノールスルホン酸、ベンゼンス
ルポン酸、１−ルエンスルポン酸等の酸、ノボラック型
フェノール樹脂の場合にはへキサメチルテトラミン、ジ
エチレントリアミン等を１吏用する。The curing agent FC) can be any used for curing the prepolymer component +a).
For example, when the prepolymer is a resol type phenolic resin or a furfuryl alcohol condensate, acids such as sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, acetic acid, phenolsulfonic acid, benzenesulfonic acid, and 1-luenesulfonic acid, novolac type phenol, etc. In the case of a resin, one portion of hexamethyltetramine, diethylenetriamine, etc. is used.
接着剤は上記（ａｌ〜（Ｃ）成分より構成されるが、そ
の割合は硬化剤（Ｃ）成分に関してはｔａ＋成分成分１
単０ｆｂｌ成分はとくに配合割合はないものの、接着剤
全体としての粘度が１〜１００００ｃｐｓ好ましくは５
０〜１０００ｃｐｓの範囲になるように調整するのが好
ましい。この粘度範囲に調整されると、成形品が発泡体
の場合、発泡体への吸収が適度であるため接着強度が高
く、成形品への塗布時に均一にかつタレを生じずに高速
で塗布することができる。The adhesive is composed of the above components (al to (C)), but the ratio is ta + component 1 for the curing agent (C) component.
Although there is no particular blending ratio for the single 0fbl component, the viscosity of the adhesive as a whole is 1 to 10,000 cps, preferably 5
It is preferable to adjust to a range of 0 to 1000 cps. When the viscosity is adjusted to this range, if the molded product is a foam, the adhesion strength is high because the absorption into the foam is moderate, and the coating can be applied uniformly to the molded product at high speed without causing any sagging. be able to.
本発明の製造方法においては、上述してきた熱硬化性樹
脂の成形品および／または発泡成形品の複数を接着剤で
もって接合し、接着層部分が乾燥硬化後に非酸化性雰囲
気で焼成し、炭素化する。In the manufacturing method of the present invention, a plurality of thermosetting resin molded products and/or foamed molded products described above are bonded together with an adhesive, and after the adhesive layer portion is dried and hardened, it is fired in a non-oxidizing atmosphere, and carbon become
接着層は好ましくは０．１〜１０００μとくに１００〜
５００μの厚みになるように形成される。非酸化性雰囲
気での焼成は、たとえば減圧下や＾ｒガス、Ｉｌｅガス
、Ｎ２ガス、ハロゲンガス等の中で、好ましくは６００
°Ｃ以上、とくに８００°Ｃ以上で焼成する。The adhesive layer preferably has a thickness of 0.1 to 1000 μm, particularly 100 μm to 100 μm.
It is formed to have a thickness of 500μ. Firing in a non-oxidizing atmosphere is preferably carried out under reduced pressure or in ^r gas, He gas, N2 gas, halogen gas, etc.
Calculate at a temperature of 800°C or higher, especially 800°C or higher.
焼成時の昇温速度は制限ないものの、一般に樹脂の分解
が開始される３００〜６００°Ｃ付近にかけては徐々に
行うほうがよい。この間に、たとえばフェアノール樹脂
であれば５０％程度の重量；成少、３０％程度の寸法減
少が生ずる。故にこの！益度間における昇温を、急激に
行うと、分解ガスが急激に発生、炭化収縮するので、ｉ
−フられる炭素質製品にはしばしばクラックの入ったも
のが生しる。また焼成温度が６００°Ｃ未満であると、
十分に炭素化されずに、着火温度が低くかつ実用的に再
度寸法変化を生じるような炭素質製品が得られることが
多い。Although there is no limit to the rate of temperature increase during firing, it is generally better to increase the temperature gradually around 300 to 600°C, at which point decomposition of the resin begins. During this time, for example, in the case of phenol resin, weight growth occurs by about 50%, and size decreases by about 30%. Therefore this! If the temperature is raised rapidly between temperatures, cracked gas will be rapidly generated and carbonization will shrink.
- Carbonaceous products that are blown often have cracks. Moreover, when the firing temperature is less than 600°C,
A carbonaceous product is often obtained which is not sufficiently carbonized, has a low ignition temperature and undergoes dimensional changes for practical purposes.
本発明の方法における炭素化において、意図的に黒鉛化
まで進めるには、焼成温度を１８００°Ｃ以上にするこ
とで可能である。In carbonization in the method of the present invention, it is possible to intentionally advance graphitization by setting the firing temperature to 1800°C or higher.
以上に述べてきた本発明の製造方法の最も好ましい態様
は、成形品の熱硬化性樹脂としてフェノール樹脂を用い
、接着剤を構成するプレポリマーとしてレゾール型フェ
ノール樹脂を用いる場合である。ここで、接着剤のプレ
ポリマーは前述のように成形品の熱硬化性樹脂原料のプ
レポリマーと実質的に同一であればよいので、当然のこ
とながら成形品のフェノール樹脂はレゾール型のほかに
ノボラック型フェレノール）３１詣でもよい。接着剤を
構成するレゾール型フェノール樹脂は、好ましくはメチ
ロール指数６０〜１１０、とくに７０〜１００の範囲の
ものであり、ホムルアルデヒト／フェノール（モル比）
の割合が１．１〜１．８とくに１．１〜１．５の範囲の
もの、常温での粘度が１００〜１００００ｃｐｓのもの
が好ましく用いられる。The most preferred embodiment of the manufacturing method of the present invention described above is the case where a phenolic resin is used as the thermosetting resin of the molded article and a resol type phenolic resin is used as the prepolymer constituting the adhesive. Here, as mentioned above, the prepolymer of the adhesive only needs to be substantially the same as the prepolymer of the thermosetting resin raw material of the molded product, so naturally the phenolic resin of the molded product can be used in addition to the resol type. Novolak-type phelenol) 31 visits may be sufficient. The resol type phenolic resin constituting the adhesive preferably has a methylol index in the range of 60 to 110, particularly 70 to 100, and has a homraldehyde/phenol (molar ratio)
Those having a ratio of 1.1 to 1.8, particularly 1.1 to 1.5, and those having a viscosity of 100 to 10,000 cps at room temperature are preferably used.
本発明の製造方法によれば、熱硬化性樹脂からなる成形
品を複数接合したのち焼成炭素化するので、従来のすで
に焼成された炭素質製品を接合後再度焼成する方法に比
べて、最も時間ど手間のかかる焼成作業が一度ですみ、
経済的かつ工程が簡単で、生産性に優れる。また、成形
品を構成する熱硬化性樹脂の原料と実質的に同一のプレ
ポリマーを接着剤として使用するので接着力に優れ、得
られる炭素質製品も強固に−体化している。さらにこの
ような接合成形品を同時に焼成するので、焼成時におけ
る成形品と接着部の炭化収縮力僧なってクラックが生じ
たり割れたりすることはない。また、接着力に優れるの
で接着層を薄くできるといった（憂れた効果を発揮する
。その他、つぼ状、箱状の異型製品も本発明の製造方法
を応用して容易に作ることができる。According to the manufacturing method of the present invention, a plurality of molded products made of thermosetting resin are bonded together and then fired and carbonized, which takes the longest time compared to the conventional method of joining already fired carbonaceous products and firing them again. The time-consuming firing process is done only once.
It is economical, has a simple process, and has excellent productivity. Furthermore, since a prepolymer that is substantially the same as the raw material for the thermosetting resin constituting the molded article is used as an adhesive, it has excellent adhesive strength, and the resulting carbonaceous product is also strongly solidified. Furthermore, since such bonded molded products are fired at the same time, there is no possibility of cracking or splitting due to the carbonization shrinkage force between the molded product and the bonded portion during firing. In addition, since it has excellent adhesive strength, the adhesive layer can be made thinner, which is an advantageous effect. In addition, irregularly shaped products such as pot-shaped and box-shaped products can be easily manufactured by applying the manufacturing method of the present invention.
以下に本発明の内容を好ましい例でもって詳述するが、
本発明はとくにことわりのない限り何らこれらの例に制
限されるものではない。The content of the present invention will be explained in detail below with preferred examples.
The present invention is not limited to these examples unless otherwise specified.
実施例１
密度０．２０ ｇ ／ Ｃｔａ、縦２５０＋ｍ、横２０
０ｍ、厚さ１０關のレゾール型フェノール樹脂発泡体の
角板に（ａ＋レゾール型ラフエノール樹脂プレポリマー
２０℃での粘度３０００ｃｐｓ ） １００重量部、
（ｂ）エタノール２０ｆｆｉｕｓ、（Ｃｌパラトルエン
スルホン酸１０重量部とからなる接着剤組成物を３００
ｇ ／ ｎ？の厚さで塗布後、５分間放置した。次い
でその上に密度０．１０ ｇ ／ ｃｒａ、Ｇ＆ ２５
０ｍｍ、横２５０龍、厚さ３０龍のレゾール型フェノー
ル樹脂発泡体の角板を重ねて２ｋｇの重りを載せて１時
間放置することにより厚さ４０龍の積層体を得た。Example 1 Density 0.20 g/Cta, length 250+m, width 20
100 parts by weight of (a + resol type rough phenol resin prepolymer viscosity 3000 cps at 20°C),
(b) 300 g of an adhesive composition consisting of 20 ffius of ethanol and 10 parts by weight of Cl para-toluenesulfonic acid.
g/n? After coating to a thickness of , it was left for 5 minutes. Then on top of that density 0.10 g/cra, G&25
Square plates of resol-type phenolic resin foam measuring 0 mm, 250 mm in width, and 30 mm in thickness were stacked, a 2 kg weight was placed on top of the square plates, and the plates were left to stand for 1 hour to obtain a laminate with a thickness of 40 mm.
この積層体をマツフル炉に入れＮ２雰囲気下昇温速度１
００℃／ｈｒで１０００°Ｃまで昇温し、この温度で１
時間放置した後冷却し、！１１８（ｈｍ、横１８０１■
、厚さ２９關の多孔質炭素積層体をｉ−７た。This laminate was placed in a Matsufuru furnace at a temperature increase rate of 1 in an N2 atmosphere.
The temperature is raised to 1000°C at a rate of 00°C/hr, and at this temperature 1
Let stand for an hour and then cool! 118 (hm, width 1801■
A porous carbon laminate with a thickness of 29 mm was prepared as i-7.
この炭素積層板の層間は十分に接着しており、接着層付
近にはクラックや剥離を認めなかった。There was sufficient adhesion between the layers of this carbon laminate, and no cracks or peeling was observed near the adhesive layer.
この板を曲げ試験を行ったところ、母材破壊であった。When this plate was subjected to a bending test, it was found that the base material was destroyed.
実施例２
密度０．２０ ｇ ／ ｃｔａのレゾール型フェノール
樹脂発泡体から直径１５０ｍｍ、高さ２００１１１、内
厚２０龍の内筒を切り出した。一方、上記レゾール型フ
ェノール樹脂発泡体から直径１５（１＋ｍ、内厚２０ｓ
ｎの円板を切り出した。前記した円筒と円板とを実施例
１で用いた接着剤及び接着方法で接合しるつぼを作製し
た。このフェノール樹脂発泡体のるつぼを雰囲気炉に入
れ、Ｎ２雰囲気で６０℃／分の昇温速度で昇温し、次い
で、１０００℃で１時間放置後冷却し、取り出した。こ
うして、密度０．２１ｇ／ｃｎｆ、直径１１（ｌｎ、高
さ１４０關、厚さ１４．５ｍｍの多孔質炭素材料からな
るるつぼを得た。Example 2 An inner cylinder with a diameter of 150 mm, a height of 200111 mm, and an inner thickness of 20 mm was cut from a resol type phenolic resin foam having a density of 0.20 g/cta. On the other hand, from the resol type phenolic resin foam, a diameter of 15 (1+ m, inner thickness of 20 s) was obtained.
N discs were cut out. A crucible was prepared by joining the cylinder and disk described above using the adhesive and bonding method used in Example 1. This crucible of phenolic resin foam was placed in an atmospheric furnace and heated at a rate of 60° C./min in a N2 atmosphere, then left at 1000° C. for 1 hour, cooled, and taken out. In this way, a crucible made of a porous carbon material having a density of 0.21 g/cnf, a diameter of 11 mm, a height of 140 mm, and a thickness of 14.5 mm was obtained.
このるつぼの接着はしつかりしており、１０回以上２０
００℃のＮ２雰囲気炉内で使用しても、何ら剥離、亀裂
を生じなかった。The adhesive of this crucible is strong and can be applied more than 10 times 20 times.
Even when used in a N2 atmosphere furnace at 00°C, no peeling or cracking occurred.
実施例３
２００龍×３００鶴×２５鶴、嵩密度０．２５ｇ／ｃＪ
の発泡フェノール樹脂板３枚と同じ材質の２００鶴Ｘ
２００ｍｍ ｘ ２５ｍｍの板２枚の端部を加工後、実
施例１に記載した接着剤を用いて、５枚の板の端部を接
着し、外径２００ ｍＩＩＸ ２００ ａｍ Ｘ ３０
０ ａｍ内径１５０Ｘ １７５Ｘ ２５０關の箱を作っ
た。Example 3 200 dragons x 300 cranes x 25 cranes, bulk density 0.25 g/cJ
200 Tsuru X made of the same material as 3 foamed phenolic resin boards
After processing the edges of two 200 mm x 25 mm plates, the edges of the five plates were glued together using the adhesive described in Example 1 to obtain an outer diameter of 200 m IIX 200 am x 30
0 am I made a box with an inner diameter of 150 x 175 x 250 mm.
このフェノール樹脂発泡体の箱を雰囲気炉に入れＮ２雰
囲気中４０°Ｃ／ｈｒの昇温速度で１２００℃まで昇温
し、次いで同温度に１時間保持した後、冷却した。こう
して、外径１４０ｍｍ Ｘ １４０ｍｍＸ ２１０ｍｍ
、厚さ１７■■、嵩密度０．２１ｇ／Ｃｎ！の多孔質炭
素の箱を得た。この箱の接着面は強固に接合していた。This box of phenolic resin foam was placed in an atmospheric furnace and heated to 1200°C at a rate of 40°C/hr in a N2 atmosphere, then maintained at the same temperature for 1 hour, and then cooled. In this way, outer diameter 140mm x 140mm x 210mm
, thickness 17■■, bulk density 0.21g/Cn! A porous carbon box was obtained. The adhesive surfaces of this box were firmly bonded.
またＮ２雰囲気で１５００℃で１０回以上使用しても、
何ら問題を生じなかった。Moreover, even if used more than 10 times at 1500℃ in N2 atmosphere,
No problems occurred.
比較例１
実施例１で用いたレゾール型フェノール樹脂の角板の各
々を予め、Ｎ２雰囲気で１０００℃で焼成して、嵩密度
０．１１ｇ／ａ＋１、縦１８０ｍｍ横１８０■ｌ厚さ２
１ｍｍの多孔質炭素板と嵩密度０．２１ ｇ ／ｃれ縦
１８０ｍｍ、横１８０鶴、厚さ７ ｗの多孔質炭素板を
得た。この２枚の多孔質炭素板を実施例１で用いた接着
剤で積層貼着後、実施例１と同様な条件で再度焼成した
が、両炭素仮界面の剥離したものしか得られなかった。Comparative Example 1 Each of the square plates of the resol type phenolic resin used in Example 1 was fired in advance at 1000°C in an N2 atmosphere to give a bulk density of 0.11 g/a+1, a length of 180 mm and a width of 180 μl and a thickness of 2.
A 1 mm porous carbon plate with a bulk density of 0.21 g/c, a length of 180 mm, a width of 180 mm, and a thickness of 7 W was obtained. These two porous carbon plates were laminated together using the adhesive used in Example 1, and then fired again under the same conditions as in Example 1, but only the two carbon temporary interfaces were obtained.
比較例２
実施例２で用いた接着剤の代りに、ポリエステルボ）ノ
オールとトリレンジイソシアネートからなるポリウレタ
ン系接着剤を用いて、実施例２と同様にしてフェノール
樹脂発泡体のるつぼを作製した。このるつぼを実施例２
と同じ条件で焼成したところ、底部の剥離したるつぼし
か得られなかった。Comparative Example 2 A phenolic resin foam crucible was produced in the same manner as in Example 2, except that instead of the adhesive used in Example 2, a polyurethane adhesive consisting of polyesterbonol and tolylene diisocyanate was used. Example 2 of this crucible
When the crucible was fired under the same conditions as above, only a crucible with a peeled bottom was obtained.
比較例３
実施例１に於て、用いた接着剤の代りに（ａｊレヅール
型ラフエノール樹脂プレポリマー粘度３０００ｃｐｓ
） １ひＯ型口部、ｆｂ）エタノール５０重口部、（
Ｃ）パラトルエンスルホン酸１０重量部（ｄｌ黒鉛粉末
１００重量部とからなる接着剤を用いる以外は実施例１
と同様にして炭素材料積層物の作製を試みたが、眉間の
接着性が劣り、容易に剥離を生じた。Comparative Example 3 In place of the adhesive used in Example 1, (aj Resul type rough henol resin prepolymer viscosity 3000 cps)
) 1 O-shaped mouth part, fb) 50 heavy mouth part of ethanol, (
C) Example 1 except that an adhesive consisting of 10 parts by weight of paratoluenesulfonic acid (100 parts by weight of dl graphite powder) was used.
An attempt was made to produce a carbon material laminate in the same manner as above, but the adhesion between the eyebrows was poor and it easily peeled off.
Claims (6)
および／または発泡樹脂成形品の複数を、 （ａ）該熱硬化性樹脂の原料であるプレポリマーと本質
的に同一のプレポリマー、 （ｂ）溶媒、 （ｃ）硬化剤、 とからなる接着剤で接合し、次いで該接合品を非酸化性
雰囲気で焼成、炭素化することを特徴とする接合された
炭素質製品の製造方法。(1) A plurality of resin molded articles and/or foamed resin molded articles made of substantially the same thermosetting resin, (a) a prepolymer essentially the same as the prepolymer that is the raw material for the thermosetting resin; (b) a solvent; and (c) a curing agent. .
範囲第１項記載の製造方法。(2) The manufacturing method according to claim 1, wherein the thermosetting resin is a phenolic resin.
特許請求の範囲第２項記載の製造方法。(3) The manufacturing method according to claim 2, wherein the prepolymer is a resol type phenolic resin.
ないし第３項のいずれかに記載の製造方法。(4) The manufacturing method according to any one of claims 1 to 3, wherein the solvent is an alcohol.
る特許請求の範囲第４項記載の製造方法。(5) The manufacturing method according to claim 4, wherein the alcohol is methanol or ethanol.
ｐｓである特許請求の範囲第１項に記載の製造方法。(6) Adhesive viscosity (20℃) is 50 to 1000c
The manufacturing method according to claim 1, which is ps.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60272611A JPS62132717A (en) | 1985-12-05 | 1985-12-05 | Manufacture of bonded carbonaceous product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60272611A JPS62132717A (en) | 1985-12-05 | 1985-12-05 | Manufacture of bonded carbonaceous product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62132717A true JPS62132717A (en) | 1987-06-16 |
Family
ID=17516342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60272611A Pending JPS62132717A (en) | 1985-12-05 | 1985-12-05 | Manufacture of bonded carbonaceous product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62132717A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011517650A (en) * | 2008-03-26 | 2011-06-16 | ハッチンソン | Carbon-based materials derived from latex |
| WO2019069570A1 (en) * | 2017-10-05 | 2019-04-11 | 旭化成株式会社 | Carbon foam, layered carbon foam, and production method for layered carbon foam |
| CN112585104A (en) * | 2018-08-31 | 2021-03-30 | 旭化成株式会社 | Carbon foam, composite and method of manufacture |
-
1985
- 1985-12-05 JP JP60272611A patent/JPS62132717A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011517650A (en) * | 2008-03-26 | 2011-06-16 | ハッチンソン | Carbon-based materials derived from latex |
| WO2019069570A1 (en) * | 2017-10-05 | 2019-04-11 | 旭化成株式会社 | Carbon foam, layered carbon foam, and production method for layered carbon foam |
| JPWO2019069570A1 (en) * | 2017-10-05 | 2020-04-02 | 旭化成株式会社 | Carbon foam, laminated carbon foam, and method for producing laminated carbon foam |
| CN111051266A (en) * | 2017-10-05 | 2020-04-21 | 旭化成株式会社 | Carbon foam, laminated carbon foam, and method for producing laminated carbon foam |
| US11450856B2 (en) | 2017-10-05 | 2022-09-20 | Asahi Kasei Kabushiki Kaisha | Carbon foam, stack carbon foam, and method of manufacturing stack carbon foam |
| CN112585104A (en) * | 2018-08-31 | 2021-03-30 | 旭化成株式会社 | Carbon foam, composite and method of manufacture |
| US11820714B2 (en) | 2018-08-31 | 2023-11-21 | Asahi Kasei Kabushiki Kaisha | Carbon foam, assembly and manufacturing method |
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