JPH0686707B2 - 炭素繊維の製造における前駆体繊維の融着防止方法 - Google Patents

炭素繊維の製造における前駆体繊維の融着防止方法

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Publication number
JPH0686707B2
JPH0686707B2 JP59193671A JP19367184A JPH0686707B2 JP H0686707 B2 JPH0686707 B2 JP H0686707B2 JP 59193671 A JP59193671 A JP 59193671A JP 19367184 A JP19367184 A JP 19367184A JP H0686707 B2 JPH0686707 B2 JP H0686707B2
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JP
Japan
Prior art keywords
precursor
fiber
precursor fiber
fibers
amino
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.)
Expired - Lifetime
Application number
JP59193671A
Other languages
English (en)
Other versions
JPS6175881A (ja
Inventor
吏 藤井
淳 磯部
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.)
Takemoto Oil and Fat Co Ltd
Original Assignee
Takemoto Oil and Fat 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 Takemoto Oil and Fat Co Ltd filed Critical Takemoto Oil and Fat Co Ltd
Priority to JP59193671A priority Critical patent/JPH0686707B2/ja
Priority to KR1019850005525A priority patent/KR880000496B1/ko
Priority to EP85306306A priority patent/EP0174806B1/en
Publication of JPS6175881A publication Critical patent/JPS6175881A/ja
Publication of JPH0686707B2 publication Critical patent/JPH0686707B2/ja
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
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    • C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
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    • C08G77/04—Polysiloxanes
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/052—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing nitrogen
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    • C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/053—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing sulfur
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    • C10M2229/04—Siloxanes with specific structure
    • C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
    • C10M2229/054—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing phosphorus
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    • C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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Description

【発明の詳細な説明】 〈産業上の利用分野〉 本発明は炭素繊維の製造における前駆体繊維の融着防止
方法に関し、更に詳しくは、炭素繊維の製造において、
アクリル系の前駆体繊維（プレカーサー）に優れた分繊
性を付与し、とりわけ耐炎化工程での該前駆体繊維相互
間の融着を防止して、優れた物性の炭素繊維を製造する
ことができる、炭素繊維の製造における前駆体繊維の融
着防止方法に関する。
〈従来の技術とその問題点〉 一般に炭素繊維は、前駆体繊維を酸化性雰囲気下に200
〜300℃で加熱焼成する耐炎化工程により耐炎化繊維と
した後、不活性雰囲気下に700℃以上の高温で炭素化す
る炭素化工程を経て製造される。そしてこの際、耐炎化
工程前、通常は前駆体繊維を製造する工程で、該前駆体
繊維に油剤を塗布して、該前駆体繊維に平滑性、帯電防
止性、集束性等の一般的諸性能を付与する他、前述の如
き炭素繊維の製造条件に対応する必要性から、該前駆体
繊維に分繊性を付与し、また耐炎化工程での前駆体繊維
相互間の融着を防止することが行なわれる。
従来一般に、前駆体繊維にホスフェートのアルカリ金属
塩、各種カチオン活性剤、ポリオキシアルキレンエーテ
ル等の油剤を塗布することが行なわれている。ところ
が、これらの方法には、炭素繊維に相応の帯電防止性、
集束性、平滑性を付与することができるものの、塗布す
る油剤がその本来的性質に基づいて熱安定性が悪く、こ
れらが熱分解するため、前駆体繊維の分繊性に劣り、ま
たこれらが耐炎化工程でタールを生じたり或は加熱初期
にその大部分が揮散するため、耐炎化工程で前駆体繊維
相互間に融着が生じるという問題点がある。
そこで従来、改良方法として、前駆体繊維にジメチルポ
リシロキサン、フェニルメチルポリシロキサン、エポキ
シポリシロキサン、ポリエーテルポリシロキサン、モノ
アミノポリシロキサン等の各種のシリコーン系油剤を塗
布することが提案されている（特公昭51−12739、特公
昭52−24136、特開昭52−148227等）。ところが、これ
らの方法にも、それぞれに次のような問題点がある。す
なわち、前駆体繊維にジメチルポリシロキサンやフェニ
ルメチルポリシロキサンを塗布する方法の場合、塗布す
る油剤それ自体は熱安定性が良好である反面、これらが
その分子内に極性基を持たないことにより前駆体繊維に
対する配向性（均一付着性、以下同じ）が不充分である
ためと考えられるが、前駆体繊維の分繊性及び耐炎化工
程での該前駆体繊維相互間の融着防止性に劣り、またこ
れらが非極性であるため、静電気による毛羽立ちや糸切
れ等が発生し易い。前駆体繊維にエポキシポリシロキサ
ンを塗布する方法の場合、その分子内のエポキシ基の開
環重合等により、前駆体繊維相互間を固着し、またそれ
自体をタール化するため、耐炎化工程での前駆体繊維相
互間の融着防止性は全くなく、むしろ弊害になる。前駆
体繊維にポリエーテルポリシロキサンを塗布する方法の
場合、その分子内の柄ー照る結合が熱的に弱く、耐炎化
工程においてそのほとんどが熱分解し、揮散するため、
耐炎化工程での前駆体繊維相互間の融着防止性に著しく
劣り、またその熱分解の際の発熱が前駆体繊維の異常反
応を誘引する。そして前駆体繊維にモノアミノポリシロ
キサンを塗布する方法の場合、これは以上説明した従来
の他のシリコーン性油剤を塗布する方法に比べれば良好
な性能を発揮するが、熱的にはなお弱い面を持ち、前駆
体繊維の分繊性及び耐炎化工程での該前駆体繊維相互間
の融着防止性が依然として充分でなく、また工業的な生
産工程中で毛羽や糸切れ等が発生する。
〈発明が解決しようとする問題点〉 本発明は、叙上の如く従来の問題点を解決するもので、
アクリル系の前駆体繊維の工程通過性を保持しつつ、該
前駆体繊維に優れた分繊性を付与し、とりわけ耐炎化工
程での該前駆体繊維相互間の融着を防止して、高品質の
炭素繊維を安定製造することができる、炭素繊維の製造
における前駆体繊維の融着防止方法を提供するものであ
る。
〈問題点を解決するための手段〉 しかして本発明者らは、上記観点で鋭意研究した結果、
アクリル系の前駆体繊維に特定のオルガノポリシロキサ
ンと特定のアミノ変性基を有するアミノ変性ポリシロキ
サンとがそれぞれ所定割合から成る油剤を所定量塗布し
た後、耐炎化処理することが正しく好適であることを見
出した。
すなわち本発明は、アクリル系の前駆体繊維を200〜300
℃で耐炎化処理し、引き続き炭素化処理して炭素繊維を
製造するに際し、該前駆体繊維に次の一般式（Ｉ）で示
されるオルガノポリシロキサンと一般式（II）で示され
るアミノ変性ポリシロキサンとが該オルガノポリシロキ
サン／該アミノ変性ポリシロキサン＝10/90〜90/10（重
量比）の割合から成る油剤を0.01〜５重量％塗布した
後、耐炎化処理することを特徴とする炭素繊維の製造に
おける前駆体繊維の融着防止方法に係る。
一般式（Ｉ）： ［但し、Ｒはメチル基又はフェニル基。m,nはオルガノ
ポリシロキサンの25℃における粘度が５〜1000センチス
トークスとなる１以上の整数。］ 一般式（II）： ［但し、Ｘは炭素数３〜５のアルキレン基。Ｙは炭素数
２〜６のアルキレン基。p,qはアミノ変性ポリシロキサ
ンの25℃における粘度が10〜10000センチストークスと
なる１以上の整数。］ 一般式（Ｉ）で示されるオルガノポリシロキサンはその
25℃における粘度が５〜1000センチストークス（以下粘
度はいずれも25℃におけるセンチストークスで示す）の
ものである。粘度が５未満であると、分子量不足とな
り、前駆体繊維製造工程や耐炎化工程初期にその殆どが
揮散し、所期の効果が得られない。逆に粘度が1000を超
えると、耐炎化工程での前駆体繊維相互間の融着防止性
が低下する。好ましくは粘度が10〜100のものが良く、
該当するジメチルポリシロキサンは好適例である。
一般式（II）で示されるアミノ変性ポリシロキサンは、
分子内にアミノ変性基１個当たり窒素原子を２個含むも
ので、かかるアミノ変性基によって前駆体繊維に対する
配向性が良好になるためと考えられるが、本発明の目的
に適い極めて有効である。
本発明でアクリル系の前駆体繊維に塗布する油剤は、一
般式（Ｉ）で示されるオルガノポリシロキサンと一般式
（II）で示されるアミノ変性ポリシロキサンとが該オル
ガノポリシロキサン／該アミノ変性ポリシロキサン＝10
/90〜90/10（重量比）の割合から成るものであるが、合
目的的に25/75〜90/10（重量比）の割合から成るものが
好ましい。
上記油剤はアクリル系の前駆体繊維の製造工程又は該製
造工程の後であって耐炎化工程前の段階で前駆体繊維に
塗布する。その塗布形態はエマルジョン、有機溶剤溶液
又はストレート等のいずれでもよく、またその塗布方法
はローラー給油法、スプレー給油法又はガイドオイリン
グ法等のいずれでもよい。この際の油剤付着量は、一方
で本発明の効果を充分に発現させつつ、他方で経済性も
含めて付着量に見合った効果を発現させるため、前駆体
繊維に対し0.01〜５重量％とする。
かくしてアクリル系の前駆体繊維に特定組成の油剤を所
定量塗布した後、該前駆体繊維を200〜300℃で耐炎化処
理し、引き続き炭素化処理して、炭素繊維を製造する。
本発明において肝要な点は、アクリル系の前駆体繊維に
前述した特定組成の油剤を所定量塗布した後、耐炎化処
理する処にある。該油剤はアクリル系の前駆体繊維に対
する配向性が良く、とりわけ200〜300℃の耐炎化工程に
おいても相応に安定であり、加熱所期の段階で不都合に
揮散したり、或は熱分解することは殆どなく、また重合
等の化学反応を起こすこともない。したがって本発明に
よると、アクリル系の前駆体繊維に優れた分繊性を付与
し、とりわけ耐炎化工程での該前駆体繊維相互間の融着
を防止できる。
〈実施例〉 以下、実施例等を挙げて本発明の構成及び効果をより具
体的にするが、本発明がここに挙げる実施例に限定され
るというものではない。
第１表に示した組成の油剤（実施例１〜４、比較例１〜
19）85重量部とポリオキシエチレンノニルフェニルエー
テル15重量部とを含有する水乳化液を調製した。
アクリルフィラメント糸（16000デニール/12000フィラ
メント）に調製した水乳化液をそれぞれ付着量0.5±0.1
重量％（水を除いた成分換算、以下同じ）となるように
浸漬法で塗布した後、乾燥ローラーを用いて115℃×４
秒間乾燥して前駆体繊維束（プレカーサートウ）を作製
し、該前駆体繊維束を試料としてその分繊性を後述の方
法で評価した。
また上記前駆体繊維束を240℃の強制循環式オーブン中
で60分間処理（耐炎化処理）して耐炎化繊維を得、これ
を試料としてその融着防止性を後述の方法で評価した。
更にアクリルフィラメント糸（75デニール/40フィラメ
ント）に前記水乳化液をそれぞれ付着量0.5±0.1重量％
となるようにローラー給油法で塗布した試料糸を作製
し、該試料糸の摩擦係数及び発生電気を後述の方法で評
価した。
結果を第１表にまとめて示した。
・分繊性の評価（表中、分繊で示した） 試料を2cmに切断し、黒紙上で軽く振盪して、分繊状態
を次の基準で評価した。
試料を2cmに切断し、白紙上で軽く振盪して、融着防止
状態を次の基準で評価した。
試料糸を20℃×65％RHの雰囲気下に24時間放置し、同条
件下に初張力20g、糸速100m/分でクロムメッキ梨地加工
ピンと接触走行させて、その摩擦係数をμメーター（エ
イコー測器社製）で測定し、次の基準で評価した。
◎＝摩擦係数0.25未満 ○＝摩擦係数0.25〜0.28未満 △＝摩擦係数0.28〜0.31未満 ×＝摩擦係数0.31以上 ・発生電気の評価（表中、電気で示した） 前記摩擦係数の測定の際に、クロムメッキ梨地加工ピン
との接触後の発生電気を集電式電位測定器（春日電気社
製）で測定し、次の基準で評価した。
○＝発生電気100ボルト未満 △＝発生電気100〜300ボルト ×＝発生電気300ボルトより大 注）第１表において、 DMSはジメチルポリシロキサン、PSはフェニルポリシロ
キサン、PESはポリエーテル変性ポリシロキサン。かっ
こ内の数値は粘度。油剤の右列数値は組成を示す重量
比。ASはアミノ変性ポリシロキサン、CSはカルボキシ変
性ポリシロキサンで、それぞれ次の通り。
AS−Ａ（アミノ変性率2.6） AS−Ｂ（アミノ変性率2.7） AS−Ｃ AS−Ｄ（アミノ変性率2.7、ポリエーテル変性率9.3） AS−Ｅ（アミノ変性率2.8） CS（カルボキシ変性率6.0） ［但し、AS−Ａ〜CSにおいて、a,b,dは整数。e,fは平均
10。］ 〈発明の効果〉 第１表の結果からも明らかなように、以上説明した本発
明には、アクリル系の前駆体繊維の工程通過性を保持し
つつ、該前駆体繊維に優れた分繊性を付与し、とりわけ
耐炎化工程での該前駆体繊維相互間の融着を防止できる
という効果がある。

Claims (1)

    【特許請求の範囲】
  1. 【請求項１】アクリル系の前駆体繊維を200〜300℃で耐
    炎化処理し、引き続き炭素化処理して炭素繊維を製造す
    るに際し、該前駆体繊維に次の一般式（Ｉ）で示される
    オルガノポリシロキサンと一般式（II）で示されるアミ
    ノ変性ポリシロキサンとが該オルガノポリシロキサン／
    該アミノ変性ポリシロキサン＝10/90〜90/10（重量比）
    の割合から成る油剤を0.01〜５重量％塗布した後、耐炎
    化処理することを特徴とする炭素繊維の製造における前
    駆体繊維の融着防止方法。 一般式（Ｉ）： ［但し、Ｒはメチル基又はフェニル基。m,nはオルガノ
    ポリシロキサンの25℃における粘度が５〜1000センチス
    トークスとなる１以上の整数。］ 一般式（II）： ［但し、Ｘは炭素数３〜５のアルキレン基。Ｙは炭素数
    ２〜６のアルキレン基。p,qはアミノ変性ポリシロキサ
    ンの25℃における粘度が10〜10000センチストークスと
    なる１以上の整数。］
JP59193671A 1984-09-14 1984-09-14 炭素繊維の製造における前駆体繊維の融着防止方法 Expired - Lifetime JPH0686707B2 (ja)

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JP59193671A JPH0686707B2 (ja) 1984-09-14 1984-09-14 炭素繊維の製造における前駆体繊維の融着防止方法
KR1019850005525A KR880000496B1 (ko) 1984-09-14 1985-07-31 탄소섬유 제조용 유제
EP85306306A EP0174806B1 (en) 1984-09-14 1985-09-05 Lubricating agents for the production of carbon yarns

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JP59193671A JPH0686707B2 (ja) 1984-09-14 1984-09-14 炭素繊維の製造における前駆体繊維の融着防止方法

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JPS6175881A JPS6175881A (ja) 1986-04-18
JPH0686707B2 true JPH0686707B2 (ja) 1994-11-02

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US5185006A (en) * 1990-12-17 1993-02-09 Becton, Dickinson And Company Lubricated metal articles and assembly containing same
JP4456253B2 (ja) * 2000-10-16 2010-04-28 竹本油脂株式会社 炭素繊維製造用合成繊維処理剤及び炭素繊維製造用合成繊維の処理方法
KR101138291B1 (ko) * 2009-05-08 2012-04-24 국방과학연구소 라이오셀계 탄소섬유 및 탄소직물의 제조방법
JP6167735B2 (ja) * 2013-08-01 2017-07-26 三菱ケミカル株式会社 炭素繊維前駆体アクリル繊維用油剤組成物と炭素繊維前駆体アクリル繊維用油剤組成物分散液、および炭素繊維前駆体アクリル繊維束の製造方法
US11629266B2 (en) * 2018-10-10 2023-04-18 Dow Global Technologies Llc Waterborne composition
JP6671698B1 (ja) 2019-05-30 2020-03-25 竹本油脂株式会社 炭素繊維前駆体用処理剤及び炭素繊維前駆体

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3717575A (en) * 1971-05-25 1973-02-20 Union Carbide Corp Spandex lubricant
US4078104A (en) * 1975-02-28 1978-03-07 Sws Silicones Corporation Release composition for bituminous materials
JPS51116225A (en) * 1975-04-04 1976-10-13 Japan Exlan Co Ltd An improved process for producing carbon fibers
JPS5234025A (en) * 1975-09-08 1977-03-15 Japan Exlan Co Ltd Process for producing carbon fibers having excellent performances
JPS52148227A (en) * 1976-05-10 1977-12-09 Mitsubishi Rayon Co Ltd Preparation of carbon fiber from acrylic fiber
JPS597832B2 (ja) * 1979-05-17 1984-02-21 ト−レ・シリコ−ン株式会社 繊維処理剤
US4311626A (en) * 1980-09-25 1982-01-19 Toray Silicone Company, Ltd. Silicone compositions for the treatment of fibers
JPS5926707B2 (ja) * 1981-03-31 1984-06-29 信越化学工業株式会社 繊維質物用処理剤

Also Published As

Publication number Publication date
EP0174806A3 (en) 1988-01-27
KR860002614A (ko) 1986-04-28
EP0174806B1 (en) 1992-01-29
KR880000496B1 (ko) 1988-04-08
EP0174806A2 (en) 1986-03-19
JPS6175881A (ja) 1986-04-18

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