JPH0415397A - Carbon fiber heat insulating material - Google Patents

Carbon fiber heat insulating material

Info

Publication number
JPH0415397A
JPH0415397A JP2117624A JP11762490A JPH0415397A JP H0415397 A JPH0415397 A JP H0415397A JP 2117624 A JP2117624 A JP 2117624A JP 11762490 A JP11762490 A JP 11762490A JP H0415397 A JPH0415397 A JP H0415397A
Authority
JP
Japan
Prior art keywords
carbon fiber
heat insulating
insulating material
fiber heat
crashed
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
Application number
JP2117624A
Other languages
Japanese (ja)
Inventor
Tetsuo Ito
哲夫 伊藤
Yasuhiko Yumitate
恭彦 弓立
Mamoru Kameda
亀田 守
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DIC Corp
Original Assignee
Dainippon Ink and Chemicals Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Dainippon Ink and Chemicals Co Ltd filed Critical Dainippon Ink and Chemicals Co Ltd
Priority to JP2117624A priority Critical patent/JPH0415397A/en
Publication of JPH0415397A publication Critical patent/JPH0415397A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce new heat insulating material at a low cost by utilizing the cut parts, defective articles, etc. of the carbon fiber heat insulating members which are generated in a variety of processes by molding a mixture of the crashed articles of the carbon fiber heat insulating material and the thermosetting resin and further carrying out baking. CONSTITUTION:A carbon fiber heat insulating material is crashed by utilizing the device which is commonly used widely such as a press, crasher, mill, and a mixer. The crashed article of the carbon fiber heat insulating material is commonly formed into powder, milled or chop form. The crashed article is mixed with the thermosetting resin, and poured into a metal mold having an aimed shape, and after heat molding, baking at an aimed temperature is carried out, and a molded heat insulating material is formed. Accordingly, the defective articles formed in the manufacturing process, transport, etc. of the carbon fiber heat insulating material or the waste articles after cutting work can be utilized again.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は炭素繊維断熱材を簡易なりラッシャープレス等
により破砕して得られる破砕物と熱硬化性樹脂との混合
物を成形し、更に焼成することにより得られる炭素繊維
断熱材に関する。
Detailed Description of the Invention (Field of Industrial Application) The present invention involves crushing a carbon fiber insulation material using a simple lasher press or the like, molding a mixture of the crushed material and a thermosetting resin, and then firing the mixture. The present invention relates to a carbon fiber heat insulating material obtained by the above method.

(従来の技術) 炭素繊維断熱材は炭素繊維フェルトあるいはチョンブ等
の素材にフェノール樹脂等を含浸させ、平板、円筒等目
的形状に成形した後焼成することにより得られる。
(Prior Art) A carbon fiber heat insulating material is obtained by impregnating a material such as carbon fiber felt or chimney with a phenol resin, forming the material into a desired shape such as a flat plate or cylinder, and then firing the material.

(発明が解決しようとする課題) 焼成後の断熱材は所定の寸法、形状物とする為に更に加
工することが不可欠である。このため、この工程で相当
程度の切りしろ等の断片が生じる。
(Problems to be Solved by the Invention) After firing, it is essential to further process the heat insulating material in order to make it into a predetermined size and shape. Therefore, a considerable amount of fragments such as cutting margins are generated in this process.

一方、焼成品は強度的に脆く、傷つき易く、焼成、加工
、運送等の諸工程において破損などの不良品を生じるこ
とも多い。この様な断片や不良品等は通常再使用される
ことなく廃棄され、結果的に製品コストにかなりの程度
影響を及ぼすことにつながる。
On the other hand, fired products are fragile and easily damaged, and often result in defective products such as breakage during various processes such as firing, processing, and transportation. Such fragments and defective products are usually discarded without being reused, resulting in a considerable impact on product costs.

本発明は、上記のような種々の段階で生ずる炭素繊維断
熱材の切りしろ、不良品等を再利用して安価な断熱材を
新たに生産すること、更には目的とする断熱材そのもの
のコストダウンを計ることを目的とする。
The present invention aims to reuse the cutting margins and defective products of carbon fiber insulation materials generated at various stages as described above to produce new inexpensive insulation materials, and further reduce the cost of the intended insulation material itself. The purpose is to measure down.

(課題を解決するための手段) 本発明者らは、かかる目的を達成すべく鋭意研究した結
果、以下のことを知見した。
(Means for Solving the Problem) The present inventors have made the following findings as a result of intensive research to achieve the above object.

即ち、炭素繊維断熱材は強度的にそれ程強くなく、広く
工業的に用いられている粉砕機、クラッシャー、プレス
等を用いることで、例えば粉砕機を用いた場合、歯の形
状、すき間を選択することにより、またプレスにおいて
は圧力を調節することにより種々な長さの破砕物とする
ことができることが判った。一方炭素繊維断熱材は既に
フェノール樹脂等を含浸させた炭素繊維を2000°C
前後で焼成、黒鉛化させたものであり、炭素繊維ミルド
あるいはチョップ等を出発原料とすることよりも樹脂と
の含浸、分散等の工程でなじみが良く、且つ破砕物と熱
硬化性樹脂との混合物を成形して得られたものを再度焼
成する際は樹脂を炭化するに足る温度域で焼成するだけ
でも十分断熱特性等において満足できる炭素繊維断熱材
とすることも可能であった。そしてこのような知見に基
づき、遂に本発明を完成させるに至った。
In other words, carbon fiber insulation materials are not very strong, and by using a crusher, crusher, press, etc. that are widely used industrially, for example, if a crusher is used, the shape of the teeth and the gap can be selected. It has also been found that by adjusting the pressure in the press, it is possible to produce crushed products of various lengths. On the other hand, carbon fiber insulation materials are made by heating carbon fibers already impregnated with phenolic resin at 2000°C.
It is calcined and graphitized before and after, and is more compatible with the resin during the impregnation and dispersion process than using milled or chopped carbon fiber as a starting material, and the combination of the crushed material and thermosetting resin is better. When re-firing the mixture obtained by molding, it was possible to obtain a carbon fiber heat insulating material with satisfactory heat insulation properties by simply firing at a temperature range sufficient to carbonize the resin. Based on this knowledge, we have finally completed the present invention.

即ち、本発明は炭素繊維断熱材の破砕物と熱硬化性樹脂
との混合物を成形し、更に焼成することを特徴とする炭
素繊維断熱材にある。
That is, the present invention resides in a carbon fiber insulation material characterized by molding a mixture of a crushed carbon fiber insulation material and a thermosetting resin and then firing the mixture.

本発明で用いる炭素繊維断熱材とは、ピッチ系、PAN
系炭素繊維にかかわらず、それのフェルト、ミルド、チ
ョップ等にフェノール等の熱硬化性樹脂を含浸させ、所
定形状に成形させた後、焼成あるいは未焼成のものを含
めた広義の炭素繊維断熱材を意味する。それを破砕した
ものを本発明においては再利用する。又、上記したフェ
ルトとは炭素繊維そのものから得られたものに限らず、
パイロメノクスやカイノールの様な耐熱繊維との混繊フ
ェルトも含んでいる。
The carbon fiber insulation material used in the present invention is pitch-based, PAN
Regardless of the type of carbon fiber, it is a carbon fiber insulation material in a broad sense, including felt, milled, chopped, etc., impregnated with thermosetting resin such as phenol, molded into a specified shape, and then fired or unfired. means. The crushed material is reused in the present invention. In addition, the above-mentioned felt is not limited to that obtained from carbon fiber itself.
It also includes felts mixed with heat-resistant fibers such as pyromenox and kynor.

炭素繊維断熱材の破砕物を得る為の炭素繊維断熱材は前
述した通りであるが、焼成温度は必ずしも2000°C
前後で黒鉛化されたものに限定されるものではなく、使
用したマトリックス樹脂が炭化されるに足る温度で焼成
されたものでも何ら本目的に不都合ではない。しかしな
がら好ましくは600℃以上で炭化したものを用いるこ
とが望ましい。
The carbon fiber insulation material used to obtain the crushed carbon fiber insulation material is as described above, but the firing temperature is not necessarily 2000°C.
The material is not limited to those that are graphitized at the front and rear, and even those that are fired at a temperature sufficient to carbonize the matrix resin used are not inconvenient for this purpose. However, it is preferable to use one that has been carbonized at 600° C. or higher.

炭素繊維断熱材の破砕方法としては、プレス、クランシ
ャー ミル、ミキサー等の広<−船釣に用いられる装置
を利用することで足る。即ち圧力により押しつぶす、あ
るいは切断により破砕する原理の装置であれば特に制限
なく用いることができる。また使用する装置は、目的と
する破砕物の粒度、糸長等に応じて選択すれば艮(、且
つ同一装置でも圧力や回転速度、歯の形状等を選ぶこと
により種々の大きさの破砕物とすることが可能である。
As a method for crushing the carbon fiber insulation material, it is sufficient to use equipment used for fishing on boats, such as a press, crusher mill, or mixer. That is, any device based on the principle of crushing by pressure or crushing by cutting can be used without any particular restrictions. In addition, the equipment to be used can be selected depending on the particle size, thread length, etc. of the target crushed material (and even the same equipment can be used to process crushed materials of various sizes by selecting the pressure, rotation speed, tooth shape, etc.). It is possible to do so.

またプレスを利用する場合はアルミハニカム等の補助具
を使用し、大きさを調節することなども可能である。
Furthermore, when using a press, it is also possible to use an auxiliary tool such as an aluminum honeycomb to adjust the size.

そして、上記方法により得られた炭素繊維断熱材の破砕
物は通常、粉状、ミルドないしはチョンプ状になる。
The crushed material of the carbon fiber heat insulating material obtained by the above method is usually in the form of powder, milled or chomped.

これらの破砕物は熱硬化性樹脂と混合し、目的とする形
状金型に充てんし、加熱成形後目的とする温度で焼成す
ることにより本発明の成形断熱材となす。
These crushed materials are mixed with a thermosetting resin, filled into a mold having the desired shape, heated and then fired at the desired temperature to form the molded heat insulating material of the present invention.

ここで熱硬化性樹脂とはレゾール、ノボラックタイプの
フェノール樹脂、ビニルエステル樹脂、フラン樹脂、ビ
スマレイミド系樹脂など一般的に入手できるものを選べ
ば良くまた2種以上の樹脂混合物を用いることも何ら不
都合ではない。しかしながら安価で種々のグレードが揃
い且つ炭化率が高く種々の溶剤に可溶であるなどの点か
らフェノール樹脂が望ましい。
Here, the thermosetting resin can be selected from commonly available resins such as resol, novolak type phenolic resin, vinyl ester resin, furan resin, and bismaleimide resin, and it is also possible to use a mixture of two or more resins. It's not an inconvenience. However, phenolic resins are desirable because they are inexpensive, available in various grades, have a high carbonization rate, and are soluble in various solvents.

破砕物と熱硬化性樹脂との混合比率は混合方法、例えば
湿式か乾式か、破砕物の粒度、成形物の大きさ、成形物
の嵩密度等々により影響され一概に規定できないが、樹
脂比率として10〜80重量%、好ましくは15〜40
%の範囲が望ましい。
The mixing ratio of the crushed material and the thermosetting resin is influenced by the mixing method, such as wet or dry, the particle size of the crushed material, the size of the molded product, the bulk density of the molded product, etc., and cannot be unconditionally defined, but the resin ratio 10-80% by weight, preferably 15-40%
A range of % is desirable.

(実施例) 次いで、本発明を実施例によりさらに説明する。(Example) Next, the present invention will be further explained by examples.

尚、例中の部及び%は重量基準である。Note that parts and percentages in the examples are based on weight.

実施例1 ■ドナツク製のピッチ系炭素繊維フェルトにフェノール
樹脂を含浸させ、所定量のプリプレグを積層し、150
°Cにて1時間圧縮成形することにより30閣厚の焼成
曲平板を得た。得られた平板を真空下2000°Cにて
焼成することで30III11厚さ、嵩密度0.16g
/c1i1の炭素繊維断熱材を得た。
Example 1 ■ Pitch-based carbon fiber felt made by Donutku was impregnated with phenol resin, and a predetermined amount of prepreg was laminated to form a 150
By compression molding at °C for 1 hour, a fired curved plate with a thickness of 30 mm was obtained. By firing the obtained flat plate at 2000°C under vacuum, it has a thickness of 30III11 and a bulk density of 0.16g.
/c1i1 carbon fiber insulation material was obtained.

カッターにて四方パリ取りした。パリを更に3〜4c1
11長に折り袋に入れ、袋のままプレス盤面にfl、3
0kg/ctll加圧、圧縮することにより断熱材ミル
ド繊維を得た。得られた破砕物の嵩密度は0.35〜0
.40g/cdであった。
I cut off the edges on all sides with a cutter. 3~4 c1 more in Paris
Fold it into a 11-length bag and place it on the press board with the bag intact, fl, 3
A heat insulating milled fiber was obtained by pressurizing and compressing at 0 kg/ctll. The bulk density of the obtained crushed material is 0.35 to 0.
.. It was 40g/cd.

得られた破砕物とノボラックタイプの発泡性フェノール
(住人ディレズ■製)樹脂とを各々60対40の比で混
合した。十分均質に混合したものの嵩密度は約0.43
g/cdであった。混合物を円筒金型に充てんし、10
0〜120℃乾燥機内にて30分間加熱することで発泡
成形体を得た。更にこのものを150℃、30分間ポス
トキュアし、次いで脱型後真空雰囲気下1000℃迄昇
温させ焼成した。昇温速度は1〜b 且つ1000℃迄昇温すれば完全に炭化が終了していた
。焼成後得られた円筒状断熱材の嵩密度は約0.17g
/cjであった。
The obtained crushed material and a novolac type foamable phenol resin (manufactured by Jumi Direz ■) were mixed in a ratio of 60:40. The bulk density of a sufficiently homogeneous mixture is approximately 0.43
g/cd. Fill the mixture into a cylindrical mold,
A foamed molded product was obtained by heating in a dryer at 0 to 120°C for 30 minutes. Further, this product was post-cured at 150°C for 30 minutes, and then, after demolding, the temperature was raised to 1000°C in a vacuum atmosphere and fired. The heating rate was 1-b, and carbonization was completely completed when the temperature was raised to 1000°C. The bulk density of the cylindrical insulation material obtained after firing is approximately 0.17g.
/cj.

また上記方法と同様にして10m厚の平板を作成−・h
r・℃であった。
In addition, a 10m thick flat plate was made in the same manner as above.
It was r.℃.

注1)試験片は100LX20”X 10T(mm)。Note 1) The test piece is 100L x 20” x 10T (mm).

H,S、=10寵/分、スパン70鶴3点曲げ。H, S, = 10 strokes/min, span 70 crane 3-point bending.

注2)窒素中において非定常法により測定。Note 2) Measured using an unsteady method in nitrogen.

実施例2 予め2000℃にて焼成された炭素繊維断熱材を鋸にて
粗切りし、このものを樹脂粉砕用ミルに投入、粉砕する
ことにより嵩密度0.2〜0.8g/ciのミルドを得
た。嵩密度はミルの歯の大きさを変えることで調節可能
であった。
Example 2 A carbon fiber insulation material pre-fired at 2000° C. is roughly cut with a saw, and this material is put into a resin pulverizing mill and pulverized to produce a milled material with a bulk density of 0.2 to 0.8 g/ci. I got it. The bulk density could be adjusted by changing the size of the mill teeth.

嵩密度約0.65g/−の破砕物と大日本インキ化学工
業■製の水溶性レゾールタイプの発泡性フェノール樹脂
を各々60対40の比で混合し、均質なスラリーを得た
。スラリーを金型に充てんし、80℃X30分次いで1
50℃×60分加熱することで均質な発泡成形体を得た
。脱型後、真空下2000℃迄焼成することにより炭素
繊維断熱材を得た。得られた断熱材の嵩密度、曲げ強度
、熱伝導率(1200℃)は各々、0.2g/a+I、
7〜8 kg / cal、1、2 kcal/w−h
r ・’Cであった。
The crushed material having a bulk density of about 0.65 g/- and a water-soluble resol type foamable phenolic resin manufactured by Dainippon Ink & Chemicals Ltd. were mixed in a ratio of 60:40 to obtain a homogeneous slurry. Fill the mold with the slurry, and then
A homogeneous foam molded product was obtained by heating at 50° C. for 60 minutes. After demolding, the carbon fiber insulation material was obtained by firing at 2000° C. under vacuum. The bulk density, bending strength, and thermal conductivity (1200°C) of the obtained heat insulating material were 0.2 g/a+I, respectively.
7-8 kg/cal, 1,2 kcal/w-h
It was r・'C.

(測定方法は実施例1記載と同じ) 実施例3 ■ドナツク製の炭素繊維ドナカーボSとパイロメノクス
を各々70対30の比率で混ぜて混繊フェルト(嵩密度
0.08g/cJl、厚さLow)を得、このものにフ
ェノール樹脂を含浸させ成形、真空下2000℃迄焼成
することで炭素繊維断熱材を得た。
(Measurement method is the same as described in Example 1) Example 3 ■ Mixed fiber felt (bulk density 0.08 g/cJl, thickness Low) by mixing carbon fiber Dona Carbo S manufactured by Donatsu and Pyromenox at a ratio of 70:30. This material was impregnated with phenol resin, molded, and fired under vacuum to 2000°C to obtain a carbon fiber heat insulating material.

得られた断熱材のパリ部を実施例1と同様プレス圧縮す
ることで嵩密度0.3 g/c++lのミルド状破砕物
とした。このものに不揮発分40%のエタノール溶液の
フェノール樹脂をミルドに対し25%分含浸させ、乾燥
しエタノールを除去した。このものを0.2g/−とな
る様所定量をとり、所定金型に充てんし、加圧成形した
。脱型後1200℃迄真空下焼成した。得られた断熱材
は嵩密度約0.18g/c!lであった。更にこのもの
を真空下2200℃迄昇温(200℃/時で昇温)し、
真空度を計測することによりガス発生の有無を測ったら
昇温開始前真空度1. OX 10−”Torrが22
00℃到達時においては9 X 10−”Torrであ
り、且つ昇温途中もほとんど110 X 10−”To
rrでありガスの発生は認められなかった。
The resulting heat insulating material was press-compressed in the same manner as in Example 1 to obtain a milled crushed product having a bulk density of 0.3 g/c++l. This product was impregnated with a 25% phenol resin solution in ethanol with a non-volatile content of 40% based on the milled material, and dried to remove the ethanol. A predetermined amount of this product was taken to give a weight of 0.2 g/-, filled into a predetermined mold, and pressure-molded. After demolding, it was fired under vacuum to 1200°C. The obtained insulation material has a bulk density of approximately 0.18 g/c! It was l. Furthermore, this material was heated to 2200°C under vacuum (temperature raised at 200°C/hour),
By measuring the degree of vacuum, the presence or absence of gas generation was determined and the degree of vacuum was 1. OX 10-” Torr is 22
When the temperature reaches 00℃, the temperature is 9 X 10-"Torr, and during the temperature rise, it is almost 110 X 10-"Torr.
rr, and no gas generation was observed.

即ち破砕物が予め2000℃焼成されている為、120
0℃程度に焼成すればその後に使用した樹脂は完全に炭
化されており、発生ガス、断熱特性等において問題はな
く焼成費用の削減になった。
In other words, since the crushed material has been pre-fired at 2000°C,
When fired to about 0°C, the resin used thereafter was completely carbonized, and there were no problems with gas generation or heat insulation properties, resulting in a reduction in firing costs.

(発明の効果) 本発明の炭素繊維断熱材は、炭素繊維断熱材の製造工程
上、運送途上等に発生する不良品あるいは切削加工後の
廃棄物を再利用することにより、本来製品に上乗せされ
ていたこれら不良重分の価格を下げることが可能となり
、且つ安価な高温用断熱材を提供しうる。また既に焼成
されたものを用いる為に未焼成の炭素繊維そのものを使
用するより樹脂とのなじみが良く且つ焼成温度も必ずし
も2000℃前後にする必要がなく樹脂を炭化するに足
る温度域で十分な場合も多く、この点でも安価な断熱材
を作ることが可能である。
(Effects of the Invention) The carbon fiber insulation material of the present invention can be manufactured by reusing defective products or cutting waste generated during the manufacturing process of carbon fiber insulation materials or during transportation. This makes it possible to reduce the price of these defective materials, and to provide an inexpensive high-temperature heat insulating material. In addition, since carbon fibers that have already been fired are used, they are more compatible with the resin than using unfired carbon fibers themselves, and the firing temperature does not necessarily have to be around 2000°C; a temperature range sufficient to carbonize the resin is sufficient. In many cases, it is possible to make inexpensive insulation materials in this respect as well.

代理人 弁理士 高 橋 勝 利Agent: Patent Attorney Katsutoshi Takahashi

Claims (1)

【特許請求の範囲】[Claims] 1.炭素繊維断熱材の破砕物と熱硬化性樹脂との混合物
を成形し、更に焼成することを特徴とする炭素繊維断熱
材。
1. A carbon fiber insulation material characterized in that a mixture of a crushed carbon fiber insulation material and a thermosetting resin is molded and then fired.
JP2117624A 1990-05-09 1990-05-09 Carbon fiber heat insulating material Pending JPH0415397A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2117624A JPH0415397A (en) 1990-05-09 1990-05-09 Carbon fiber heat insulating material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2117624A JPH0415397A (en) 1990-05-09 1990-05-09 Carbon fiber heat insulating material

Publications (1)

Publication Number Publication Date
JPH0415397A true JPH0415397A (en) 1992-01-20

Family

ID=14716350

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2117624A Pending JPH0415397A (en) 1990-05-09 1990-05-09 Carbon fiber heat insulating material

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04139013A (en) * 1990-10-01 1992-05-13 Yazaki Corp Production of superfine carbonaceous powder
EP3279175A1 (en) * 2016-08-05 2018-02-07 Honeywell International Inc. Vibration assisted densification of a fiber preform

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04139013A (en) * 1990-10-01 1992-05-13 Yazaki Corp Production of superfine carbonaceous powder
EP3279175A1 (en) * 2016-08-05 2018-02-07 Honeywell International Inc. Vibration assisted densification of a fiber preform
CN107685456A (en) * 2016-08-05 2018-02-13 霍尼韦尔国际公司 The vibration auxiliary of carbon fiber preforms is fine and close
US10151026B2 (en) 2016-08-05 2018-12-11 Honeywell International Inc. Vibration assisted densification of a carbon fiber preform

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