JPH0273881A - Production of sealing material - Google Patents

Production of sealing material

Info

Publication number
JPH0273881A
JPH0273881A JP63224407A JP22440788A JPH0273881A JP H0273881 A JPH0273881 A JP H0273881A JP 63224407 A JP63224407 A JP 63224407A JP 22440788 A JP22440788 A JP 22440788A JP H0273881 A JPH0273881 A JP H0273881A
Authority
JP
Japan
Prior art keywords
sealing material
carbon fiber
expanded graphite
graphite powder
carbon
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.)
Granted
Application number
JP63224407A
Other languages
Japanese (ja)
Other versions
JPH0553190B2 (en
Inventor
Hiroshi Shirata
白田 寛
Junichi Aizawa
淳一 相沢
Takeshi Ishikawa
猛 石川
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.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
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 Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP63224407A priority Critical patent/JPH0273881A/en
Publication of JPH0273881A publication Critical patent/JPH0273881A/en
Publication of JPH0553190B2 publication Critical patent/JPH0553190B2/ja
Granted legal-status Critical Current

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  • Ceramic Products (AREA)
  • Sealing Material Composition (AREA)

Abstract

PURPOSE:To obtain a sealing material having excellent tensile strength, compression restoration and heat-resistance in high workability by mixing expanded graphite powder with carbon fibers coated with a binder, forming the mixture and calcining the product. CONSTITUTION:The objective sealing material can be produced by (1) mixing (A) expanded graphite powder (e.g., graphite expanded to a bulk expansion ratio of >=10 by immersing natural graphite in a strong oxidizing agent such as concentrated sulfuric acid, washing with water, dewatering and quickly heating at 600-1300 deg.C) with (B) carbon fiber coated with a binder (preferably phenolic resin or furan resin) (preferably a carbon fiber having a length of 0.5-50mm and produced by coating a carbon fiber with thermally cracked carbon and subjecting to expansion treatment), (2) forming the mixture and (3) calcining the formed article preferably in a non-oxidizing atmosphere at 1000 deg.C.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は原子力等に使用され、引張り強度、圧縮復元性
及び耐熱性に優れたシール材の製造法に関する。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for manufacturing a sealing material that is used in nuclear power plants and has excellent tensile strength, compression recovery properties, and heat resistance.

(従来の技術) 従来、密封装置等に使用されるパラギン等のシール材は
1石綿繊維基材に潤滑剤笹の補助材を組安定性、耐食性
、耐熱性!に問題がわシ、使用範囲が限定されていた。
(Conventional technology) Conventionally, sealing materials such as paragin used in sealing devices, etc. are made by combining an asbestos fiber base material with a lubricant bamboo as an auxiliary material.It has stability, corrosion resistance, and heat resistance! The problem was that the range of use was limited.

この間1lllを解決すべく近年可撓性を有し、不浸透
性、耐食性、耐熱性、化学的安定性等にすぐれた膨張黒
鉛製のシール材が用いられるようになってきた。
Recently, in order to solve this problem, sealing materials made of expanded graphite, which are flexible, have excellent impermeability, corrosion resistance, heat resistance, chemical stability, etc., have come into use.

(発明が解決しようとする1111) 前記、Il膨張黒鉛粉みを圧縮成形して得たシート材料
を所望の形状と厚さに積層したパツキン勢のシール材は
1粒子間結合が小さく脆いため、変形破損しやす<、*
に折り曲げに対して弱く、取扱いに注意を要するので作
業性が殊いなど種々の欠点があった。
(1111 to be solved by the invention) The above-mentioned sealing material of Packkin type, which is made by laminating sheet materials obtained by compression molding Il expanded graphite powder in a desired shape and thickness, has small interparticle bonds and is brittle. Easily deformed and damaged <, *
It has various drawbacks, such as being weak against bending and requiring careful handling, resulting in poor workability.

本発明はこれらの欠点を除去し、化学的安定性。The present invention eliminates these drawbacks and improves chemical stability.

耐熱性にすぐれ、従来の膨張黒鉛材よシも引張り強度及
び圧縮復元性を向上せしめると共に、シール性を保持す
るシール材の製造法を提供するものである。
The present invention provides a method for producing a sealing material that has excellent heat resistance, improves tensile strength and compressive recovery properties compared to conventional expanded graphite materials, and maintains sealing properties.

CSaを解決するための手段) 本発明は膨張黒鉛粉に結合材11−被着させた炭素繊維
を加えて混合して成形し2次いで焼成するシール材の製
造法に関する。
Means for Solving CSa) The present invention relates to a method for manufacturing a sealing material in which carbon fiber coated with a binder 11 is added to expanded graphite powder, mixed, molded, and then fired.

本発明において使用する膨張黒鉛粉としては。The expanded graphite powder used in the present invention includes:

公知の方法によって得られるものが使用される。Those obtained by known methods are used.

例えば天然黒鉛、熱分解黒鉛、キッシュ黒鉛等を濃硫酸
、濃硝酸、退散化水素水等の強酸化剤又はこれらの混合
液中に浸漬した後、水洗、脱水を行い、その後600〜
1300℃の温度に急熱して膨張処理を行う事によシ原
料黒鉛粉との嵩密度比で10倍以上の倍率に膨張した膨
張黒鉛粉を用いる。
For example, natural graphite, pyrolytic graphite, quiche graphite, etc. are immersed in a strong oxidizing agent such as concentrated sulfuric acid, concentrated nitric acid, and dehydrogenated water, or a mixture thereof, and then washed with water and dehydrated.
Expanded graphite powder is used which has been expanded to a bulk density ratio of 10 times or more compared to the raw material graphite powder by rapidly heating it to a temperature of 1300° C. and carrying out an expansion treatment.

炭素繊維は、シール材の引張り強度を増大するために添
加するものであシ、公知のものを用い。
The carbon fiber is added to increase the tensile strength of the sealing material, and a known carbon fiber is used.

表面に結合材を被着させる。A bonding material is applied to the surface.

炭素繊維の形態は短繊維、連続繊維、織布、フェルト状
、マット状の不織布等のいずれでもよいが、短繊維が好
ましい。膨張黒鉛に短繊維を加えるとシール材の異方性
が小さくなり復元特性、摺動特性が向上する。さらに繊
維長は0.5〜50■とした方が好ましい。繊維長が短
かすぎると強度向上の効果がなく、長すぎると成形性が
悪くなる。
The carbon fibers may be in the form of short fibers, continuous fibers, woven fabrics, felt-like, mat-like nonwoven fabrics, etc., but short fibers are preferred. Adding short fibers to expanded graphite reduces the anisotropy of the sealing material and improves its restoring properties and sliding properties. Furthermore, it is preferable that the fiber length is 0.5 to 50 cm. If the fiber length is too short, there will be no effect of improving strength, and if the fiber length is too long, moldability will deteriorate.

膨張黒鉛粉と混合する炭素繊維のシール材中の含有量は
0.5〜20重量%が好ましい。少々いと強度を向上す
る効果が与られず、多すぎるとシール性が低下する。
The content of carbon fiber mixed with expanded graphite powder in the sealing material is preferably 0.5 to 20% by weight. If it is too small, the effect of improving the strength will not be imparted, and if it is too large, the sealing performance will deteriorate.

結合材は、熱硬化性樹脂、タールピッチ等の高分子有機
化合物が用いられ特に制限はないが、炭化収率の高いフ
ェノール樹脂、フラン樹脂等が好ましい。
As the binder, a thermosetting resin, a high-molecular organic compound such as tar pitch can be used, and there is no particular limitation, but phenol resin, furan resin, etc., which have a high carbonization yield, are preferable.

炭素繊維に結合材を被着させ、膨張黒鉛粉との結合をよ
くするには、炭素繊維と例えばノボラック型フェノール
樹脂の粉末を混合してもよいが。
In order to coat the carbon fibers with a binder and improve their bonding with the expanded graphite powder, the carbon fibers may be mixed with powder of, for example, a novolac type phenol resin.

炭素繊維の表面に充分に被着させるためには1例えば樹
脂フェノのような液状にした結合材を塗布。
In order to sufficiently adhere to the surface of the carbon fiber, 1. For example, apply a liquid binding material such as resin phenol.

含浸する。炭素繊維を該結合材中に浸漬する。炭素繊維
と該結合材とを混合するのが好ましい。このあと、その
まま、低温で加熱して溶剤を除去する。又は樹脂を半硬
化状態にした後、膨張黒鉛粉と混合する。
Impregnate. Carbon fibers are dipped into the binder. Preferably, the carbon fibers and the binder are mixed. Thereafter, the solvent is removed by heating at a low temperature. Alternatively, after the resin is semi-cured, it is mixed with expanded graphite powder.

膨張黒鉛粉と炭素繊維との混合は公知の混合機を用いて
行い9次いで公知の圧縮プレス、静水圧プレス等を用い
て成形する。好ましくは熱圧成形して結合材を硬化させ
る。最後に非酸化性の雰囲気で約1000℃で焼成して
結合材を炭化して。
The expanded graphite powder and carbon fibers are mixed using a known mixer, and then molded using a known compression press, isostatic press, or the like. Preferably, the bonding material is cured by hot pressing. Finally, the binder is carbonized by firing at approximately 1000°C in a non-oxidizing atmosphere.

シール材とされる。It is used as a sealing material.

結合材の添加量は、シール材中の結合材の炭化物が0.
5〜15重量%となる量が好ましい。結合材が少ないと
膨張黒鉛粉と炭素繊維を結合する効果が弱く、多すぎる
と結合材が膨張黒鉛粉中に浸透して圧縮復元性(シール
材の可撓性)が低下する。
The amount of binder added is such that the amount of carbide in the binder in the sealant is 0.
An amount of 5 to 15% by weight is preferred. If the binding material is too small, the effect of binding the expanded graphite powder and carbon fibers will be weak, and if it is too large, the binding material will penetrate into the expanded graphite powder, reducing compression recovery properties (flexibility of the sealing material).

更に膨張黒鉛粉と炭素繊維との接着力を増すために2例
えばCVDにより熱分解炭素を被覆したPAN系炭素炭
素質繊維膨張黒鉛粉の製法と同じ方法で膨張化処理し、
熱分解炭素だけを膨張させた材料を前記炭素繊維と同様
にして使用してもよい。
Furthermore, in order to increase the adhesive strength between the expanded graphite powder and the carbon fibers, the expanded graphite powder is expanded using the same method as the manufacturing method of the expanded graphite powder, which is a PAN-based carbonaceous fiber coated with pyrolytic carbon, for example, by CVD.
A material obtained by expanding only pyrolytic carbon may be used in the same manner as the carbon fiber.

(実施例) 以下本発明の詳細な説明する。(Example) The present invention will be explained in detail below.

実施例1 一 鱗状黒鉛を濃硫酸と濃硝酸との混合液に浸漬し水洗し乾
燥した後、1200℃の急熱して高密度が0002g/
am3の膨張黒鉛粉を得た。一方、7μmφの炭素連続
繊維(東邦ベスロン製、ベスファイト)をフェノール樹
脂ワニス(日立化成工業製、VPIIN)中に3時間浸
漬後取出し、50℃で減圧乾燥して溶剤(メタノール)
を除去し。
Example 1 Graphite scales were immersed in a mixture of concentrated sulfuric acid and concentrated nitric acid, washed with water, dried, and then rapidly heated to 1200°C to achieve a high density of 0002g/
An am3 expanded graphite powder was obtained. On the other hand, carbon continuous fibers with a diameter of 7 μm (Besphite, manufactured by Toho Veslon) were immersed in phenolic resin varnish (VPIIN, manufactured by Hitachi Chemical Co., Ltd.) for 3 hours, taken out, dried under reduced pressure at 50°C, and then treated with a solvent (methanol).
Remove.

長さ25謳に切断した。この樹脂被着炭素繊維10重量
部及び前記膨張黒鉛粉80重量部を■型混合機で混合し
た混合粉を金型に入れ、160℃で熱圧成形して樹脂を
硬化させた。この成形体を窒素ガス雰囲気下徐々に昇温
し、1000℃で1時間焼成し、密度が1.5 g/c
m”のシール材を得た。
It was cut into 25 lengths. A mixed powder prepared by mixing 10 parts by weight of this resin-coated carbon fiber and 80 parts by weight of the expanded graphite powder using a type 2 mixer was placed in a mold, and hot-press molded at 160° C. to harden the resin. The temperature of this compact was gradually raised in a nitrogen gas atmosphere and baked at 1000°C for 1 hour, resulting in a density of 1.5 g/c.
A sealing material having a size of 1.5 m was obtained.

尚シール材中の樹脂炭化物の含有量は0,8重量%でち
った。
The content of resin carbide in the sealing material was 0.8% by weight.

実施例2 結合材にフルフリルアルコール初期給金物(日立化成工
業製、VF303)に硬化剤としてパラトルエンスルホ
ン酸メチルエステルヲ1 li量% 添加したものを用
いた以外は実施例1と同様にして。
Example 2 The same procedure as in Example 1 was carried out except that the binder was a furfuryl alcohol initial charge (manufactured by Hitachi Chemical Co., Ltd., VF303) and 1 li% of para-toluenesulfonic acid methyl ester was added as a hardening agent. .

密度1.491011”のシール材を得た。尚シール材
中の樹脂炭化物の含有量はα6重量%であった。
A sealing material having a density of 1.491011'' was obtained.The content of resin carbide in the sealing material was α6% by weight.

実施例3 実施例1における樹脂被着前の炭素繊維をCVD処理し
た。即ち1100℃で窒素ガス稀釈のベンゼンガス(混
合ガス中のベンゼン含有量446体積チ)を600時間
供給し、炭素繊維に熱分解炭素を被覆し九。次いでこの
炭素繊維を実施例1における膨張黒鉛粉の製造と同じ方
法で膨張化処理し。
Example 3 The carbon fibers in Example 1 before being coated with resin were subjected to CVD treatment. That is, benzene gas diluted with nitrogen gas (benzene content in the mixed gas: 446 vol. h) was supplied at 1100° C. for 600 hours to coat the carbon fibers with pyrolytic carbon. Next, this carbon fiber was subjected to expansion treatment in the same manner as in the production of expanded graphite powder in Example 1.

表面の熱分解炭素を膨張させた後、実施何重と同様にし
て樹脂を被着し、以下実施例1と同様にして膨張黒鉛粉
と混合、成形、焼成して、密度L5G/cffl”のシ
ール材を得た。
After expanding the pyrolytic carbon on the surface, resin was applied in the same manner as in the previous example, and then mixed with expanded graphite powder, molded, and fired in the same manner as in Example 1 to obtain a material with a density of L5G/cffl''. A sealing material was obtained.

比較例 実施例1で用いた膨張黒鉛粉だけを成形し、密度14g
/ca”のシール材を得た。
Comparative Example Only the expanded graphite powder used in Example 1 was molded, and the density was 14g.
/ca'' sealing material was obtained.

実施例で得られた3種類のシール材及び比較例で得られ
た炭素繊維及び結合材を含まないシール材について特性
を測定した結果を第1表に示す。
Table 1 shows the results of measuring the characteristics of the three types of sealing materials obtained in the Examples and the sealing materials containing no carbon fiber and binder obtained in the Comparative Examples.

第1表 注)圧縮率、復元率は人8TM  F−36−G(荷重
a 52 kg/an”)によった。
Table 1 Note) The compression rate and recovery rate were based on Human 8TM F-36-G (load a 52 kg/an'').

第1表から、実施例のシール材は比較例のシール材に比
べて引張シ強度が著しく増大し、圧縮率が適度であシ、
復元率も向上していることが明らかである。
From Table 1, it can be seen that the sealing material of the example has significantly increased tensile strength and moderate compression ratio compared to the sealing material of the comparative example.
It is clear that the recovery rate has also improved.

(発明の効果) 本発明によれば、炭素繊維の補強によシ引張ル強度は膨
張黒鉛単体に比して格段に大きく、従って取扱いが容易
となシ2作業性が一段と向上すると共に圧縮復元性及び
耐熱性にもすぐれたシール材が得られる。
(Effects of the Invention) According to the present invention, the tensile strength is much higher than that of expanded graphite alone due to reinforcement of carbon fiber, and therefore handling is easy.2 Workability is further improved, and compression and recovery are achieved. A sealing material with excellent properties and heat resistance can be obtained.

特許出願人 工業技術院長 飯塚幸=Patent applicant Yuki Iizuka, Director of the Agency of Industrial Science and Technology

Claims (3)

【特許請求の範囲】[Claims] 1.膨張黒鉛粉に結合材を被着させた炭素繊維を加えて
混合して成形し,次いで焼成することを特徴とするシー
ル材の製造法。
1. A method for manufacturing a sealing material, characterized by adding carbon fiber coated with a binder to expanded graphite powder, mixing and shaping, and then firing.
2.炭素繊維の長さが0.5〜50mmである請求項1
に記載のシール材の製造法。
2. Claim 1: The carbon fiber has a length of 0.5 to 50 mm.
The manufacturing method of the sealing material described in .
3.炭素繊維が熱分解炭素を被覆した後,膨張化処理を
施した炭素繊維である請求項1又は2に記載のシール材
の製造法。
3. 3. The method for manufacturing a sealing material according to claim 1, wherein the carbon fiber is a carbon fiber coated with pyrolytic carbon and then subjected to an expansion treatment.
JP63224407A 1988-09-09 1988-09-09 Production of sealing material Granted JPH0273881A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63224407A JPH0273881A (en) 1988-09-09 1988-09-09 Production of sealing material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63224407A JPH0273881A (en) 1988-09-09 1988-09-09 Production of sealing material

Publications (2)

Publication Number Publication Date
JPH0273881A true JPH0273881A (en) 1990-03-13
JPH0553190B2 JPH0553190B2 (en) 1993-08-09

Family

ID=16813281

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63224407A Granted JPH0273881A (en) 1988-09-09 1988-09-09 Production of sealing material

Country Status (1)

Country Link
JP (1) JPH0273881A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604594A (en) * 2012-02-08 2012-07-25 太原市小店区志达机械加工厂 Preparation method of high-temperature composite sealing material
JP2013516374A (en) * 2009-12-31 2013-05-13 エスゲーエル カーボン ソシエタス ヨーロピア Graphite-containing molded body and method for producing the same
EP1440955B1 (en) * 2003-01-24 2017-04-05 Eagle Industry Co., Ltd. A seal assembly containing a sliding element and the use of a sliding element for seals

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5292216A (en) * 1976-01-30 1977-08-03 Nippon Carbon Co Ltd Flexible graphite sheet materials
JPS63280787A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280789A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280788A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280786A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5292216A (en) * 1976-01-30 1977-08-03 Nippon Carbon Co Ltd Flexible graphite sheet materials
JPS63280787A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280789A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280788A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket
JPS63280786A (en) * 1987-05-13 1988-11-17 Asahi Chem Ind Co Ltd Composition for gasket

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1440955B1 (en) * 2003-01-24 2017-04-05 Eagle Industry Co., Ltd. A seal assembly containing a sliding element and the use of a sliding element for seals
JP2013516374A (en) * 2009-12-31 2013-05-13 エスゲーエル カーボン ソシエタス ヨーロピア Graphite-containing molded body and method for producing the same
CN102604594A (en) * 2012-02-08 2012-07-25 太原市小店区志达机械加工厂 Preparation method of high-temperature composite sealing material

Also Published As

Publication number Publication date
JPH0553190B2 (en) 1993-08-09

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