JP3541966B2 - Method for producing nonwoven fabric of polybenzazole fiber - Google Patents

Method for producing nonwoven fabric of polybenzazole fiber Download PDF

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Publication number
JP3541966B2
JP3541966B2 JP18242094A JP18242094A JP3541966B2 JP 3541966 B2 JP3541966 B2 JP 3541966B2 JP 18242094 A JP18242094 A JP 18242094A JP 18242094 A JP18242094 A JP 18242094A JP 3541966 B2 JP3541966 B2 JP 3541966B2
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Japan
Prior art keywords
nonwoven fabric
polybenzazole
aspirator
polybenzazole fiber
yarn
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JP18242094A
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JPH0849156A (en
Inventor
和之 矢吹
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Toyobo Co Ltd
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Toyobo Co Ltd
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Priority to JP18242094A priority Critical patent/JP3541966B2/en
Application filed by Toyobo Co Ltd filed Critical Toyobo Co Ltd
Priority to EP95928723A priority patent/EP0775221B1/en
Priority to PCT/US1995/009818 priority patent/WO1996004413A1/en
Priority to ES95928723T priority patent/ES2186726T3/en
Priority to DE69529221T priority patent/DE69529221T2/en
Priority to US08/793,039 priority patent/US5756040A/en
Priority to CA 2194989 priority patent/CA2194989A1/en
Publication of JPH0849156A publication Critical patent/JPH0849156A/en
Priority to MXPA/A/1997/000815A priority patent/MXPA97000815A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/74Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/10Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between yarns or filaments made mechanically

Description

【0001】
【産業上の利用分野】
本発明は高強度・高弾性率ポリベンゾオキサゾール系の不織布の製造方法に関する。さらに詳しくは、不織布の製造方法を著しく容易にする製糸方法に関するものである。
【0002】
【従来の技術】
ポリベンザゾール繊維は現在市販されているスーパー繊維の代表であるポリパラフェニレンテレフタルアミド繊維の2倍以上の強度と弾性率を持つ。したがって次世代のスーパー繊維として期待されている。ポリベンザゾール重合体のポリリン酸溶液から繊維を製造することは公知である。例えば、紡糸方法については米国特許5296185号、米国特許5294390号があり、熱処理方法については米国特許5288445号が提案がなされている。しかしながらポリベンザゾール繊維の不織布の製法についての先行技術は発明者らの知るかぎりにおいて存在しない。
【0003】
【発明が解決しようとする課題】
ポリベンザゾール繊維不織布を、従来法で製造されたポリベンザゾール繊維の長繊維または短繊維を用いて従来の方法でオフラインで製造することができる。また一般的な湿式紡糸によるオンラインでの不織布と同様に、凝固後の繊維あるいは乾燥後の繊維を不織布製造工程に導き不織布を製造することも可能である。しかしながらポリベンザゾール繊維は効率的な製造方法で作成しても水洗および乾燥工程が長く、水洗および乾燥工程を不織布として通過させることができれば、紡糸速度を落とすことなく効率的に水洗乾燥することができるので、極めて経済的である。即ち、湿式紡糸を用いる不織布の製造方法としては前代未聞であるが、ポリエステルやプロピレンの不織布の製造工程のように紡出糸をネットコンベアに直接捕集し不織布にする工程が応用できれば、紡糸速度に対し不織布の工程移送速度は極めて遅くできる。抽出、水洗、乾燥、熱処理と言った長時間を要する工程が不織布では逆に容易になる。このためポリベンザゾール繊維の不織布が、安く製造できる可能性がある。問題はポリベンザゾール繊維はポリベンザゾールポリマーとポリリン酸からなるドープは極めて粘度が高く紡糸張力が高いため気体による牽引では吐出ドープの伸長が全くできないことである。本発明は、このような技術的困難を克服し、工業的にポリベンザゾール不織布を得る新規な製造方法を提供するものである。
【0004】
【課題を解決するための手段】本発明者らは、ポリベンザゾール不織布の生産を容易にすることを目的とし、鋭意研究し、解決手段を見いだした。即ち、ポリベンザゾールとポリリン酸から成る紡糸ドープを、紡糸口金から紡出する。吐出された糸条は極めて伸長粘度が高く容易にドラフトを与えることができない。そこでゴデットロールで一定速度を糸条に与えた後、流体(液体でも気体でもよい)アスピレータにより引き取アスピレータから吐出される糸条および流体をコンベアネット上で捕集する。捕集後の糸条束からなる不織布を凝固及び/又は抽出しさらに乾燥し容易にポリベンザゾール不織布を得ることができることを見い出した。本発明はその製造方法を主旨とするものである。
【0005】
以下本発明を詳細に説明する。
本発明におけるポリベンザゾール繊維とは、ポリベンザゾールポリマーよりなる繊維をいい、ポリベンザゾール(PBZ)とは、ポリベンゾオキサゾール(PBO)ホモポリマー、ポリベンゾチアゾール(PBT)ホモポリマー及びそれらPBO、PBTのランダム、シーケンシャルあるいはブロック共重合ポリマーをいう。ここでポリベンゾオキサゾール、ポリベンゾチアゾール及びそれらのランダム、シーケンシャルあるいはブロック共重合ポリマーは、例えば Wolfe等の「Liquid Crystalline Polymer Compositions , Process and Products」米国特許第4703103号(1987年10月27日)、「Liquid Crystall-ine Polymer Compositions, Process and Products」米国特許4533692号(1985年8月6日)、「Liquid Crystalline Poly(2,6-Benzothiazole) Composition, Process and Products」米国特許第4533724号(1985年8月6日)、「Liquid Crystalline Polymer Compositions, Process and Products 」米国特許第4533693号(1985年8月6日)、Evers の「Thermooxidative-ly Stable Articulated p-Benzobisoxazole and p-Benzobisthiazole Polymres 」米国特許第4539567号(1982年11月16日)、Tasi等の「Methodfor making Heterocyclic Block Copolymer」米国特許第4578432号(1986年3月25日)、等に記載されている。
PBZポリマーに含まれる構造単位としては、好ましくはライオトロピック液晶ポリマーから選択される。モノマー単位は構造式(a)〜(h)に記載されているモノマー単位からなり、さらに好ましくは、本質的に構造式(a)〜(c)から選択されたモノマー単位からなる。
【0006】
【化1】

Figure 0003541966
【0007】
【化2】
Figure 0003541966
【0008】
PBZポリマーのドープを形成するための好適な溶媒としては、クレゾールやそのポリマーを溶解し得る非酸化性の酸が含まれる。好適な酸溶媒の例としては、ポリリン酸、メタンスルホン酸および高濃度の硫酸あるいはそれらの混合物が挙げられる。さらに適する溶媒はポリリン酸及びメタンスルホン酸である。また最も適する溶媒は、ポリリン酸である。
【0009】
溶媒中のポリマー濃度は好ましくは少なくとも約7重量%であり、さらに好ましくは少なくとも10重量%、最も好ましくは少なくとも14重量%である。最大濃度は、例えばポリノーの溶解性やドープ粘度といった実際上の取扱い性により限定される。それらの限界要因のために、ポリマー濃度は通常では20重量%を超えることはない。
【0010】
好適なポリマーやコポリマーあるいはドープは公知の手法により合成される。例えば Wolfe等の米国特許第4533693号(1985年8月6日)、Sybert等の米国特許4772678号(1988年9月20日)、Harrisの米国特許第4847350号(1989年7月11日)に記載される方法で合成される。PBZポリマーは、Gregory 等の米国特許第5089591号(1992年2月18日)によると、脱水性の酸溶媒中での比較的高温、高剪断条件下において高い反応速度での高分子量化が可能である。
【0011】
このようにして重合されるドープは紡糸部に供給され、紡糸口金から通常100 ℃以上の温度で吐出される。口金細孔の配列は通常円周状、格子状に複数個配列されるが、その他の配列であってもよい。口金細孔数は特に限定されないが、紡糸口金面における紡糸細孔の配列は、吐出糸条間の融着などが発生しないような孔密度を保つ必要がある。
【0012】
次に本発明の要点となるが、該紡糸口金から吐出されたドープ(ポリリン酸を抽出する前の状態にある糸条)を応力隔離装置もしくは液体流を用いた揺動可能なアスピレータにより高い張力で延伸する。該応力隔離装置もしくは液体流アスピレータと紡糸口金の間に冷却風を用いて糸条を冷却するいわゆるクエンチチェンバーを設けることは早い紡速を得るために有効である。
【0013】
応力隔離装置はいわゆるゴデットロールなどを用いたものが一般的である。ロールは耐腐食性の材質で出来たものが望ましく、表面がテフロンなどの離型性に優れるものが望ましい。応力隔離装置を用いた場合はその下流に不織布製造用のアスピレータを設け、該アスピレータを用いてネットコンベアなどの不織布捕集装置に糸条を捕集する。アスピレータが気体である場合は、該気体の温度を調整することにより捕集された不織布の単繊維間に融着が発生し適度な交絡が得られ用途によっては望ましい。アスピレータに供給する気体は、空気または窒素ガスなどの不活性ガスまたは炭酸ガスあるいはこれらの混合ガスが好適である。アスピレーター出口からはおよそ20〜300m/秒の噴流が噴出する。
【0015】
不織布としての捕集雰囲気は液体中でも気体中でも良いが、ネットコンベアなどで捕捉した不織布は引き続き凝固および又は抽出され、最終的に抽出浴中において糸条が含有するリン酸を99.0%以上、好ましくは99.5%以上となる。本発明における抽出媒体として用いられる液体に特に限定はないが好ましくはポリベンゾオキサゾールに対して実質的に相溶性を有しない水、メタノール、等である。また抽出浴を多段に分離しリン酸水溶液の濃度を順次薄くし最終的に水で水洗してもよい。さらに該不織布は水酸化ナトリウム水溶液などで中和され、さらに水洗される。
【0016】
水洗後の不織布はベルトコンベアーなどの捕集装置とともに高温空気などを用いた乾燥機により乾燥される。かくして得られる不織布を構成する単繊維は25g/d以上の十分な強度と、約700g/dの十分に高弾性率を有しているが、該不織布を直ちにもしくは別途、350℃以上で熱処理を施すことにより単繊維の弾性率は1500g/d以上に向上する。
【0017】
該不織布は必要に応じて、接着剤処理、ニードルパンチやウオータパンチなどの交絡処理、あるいはカレンダー加工される。
【0018】
得られた不織布は、優れた耐熱性と優れた引き裂き強力を有し、耐熱防護材、断熱防護材、耐摩耗防護材あるいは耐炎防護材として、他の繊維から得れた不織布にない優れた特徴を有する。
【0019】
【実施例】
以下に実施例を示すが本発明はこれらの実施例に限定されるものではない。
<実施例1>
米国特許4533693号示す方法により得られた、30℃のメタンスルホン酸溶液で測定した固有粘度が24.4dL/gのポリベンゾオキサゾール14.0(重量)%と五酸化リン含量率83.17%のポリリン酸からなる紡糸ドープを紡糸に用いた。ドープは金属網状の濾材を通過させ、次いで2軸からなる混練装置で混練と脱泡を行った後、昇圧させ、重合体溶液温度を170℃に保ち、図1に示す装置を用いて、孔数334を有する紡糸口金から170℃で紡出し、温度60℃の冷却風を用いて吐出糸条を冷却した後、表面をテフロン加工したゴデットロールに巻き付け200m/分の糸条速度を与えた。次いで圧搾空気を供給流体とするアスピレターを用いて牽引しネットコンベアーで捕集した。ネットコンベアの移送速度は20cm/分である。次いで補集された不織布をネットコンベアごと温度22±2℃に保った10%のリン酸水溶液からなる抽出浴中に導入した。引き続いてネットコンベア上に捕集したままの不織布をさらに第二の抽出浴中でイオン交換水で糸条を洗浄した後、0.1規定の水酸化ナトリウム溶液侵漬し中和処理した。さらに水洗浴で洗浄した後、190℃に保たれた空気乾燥室で5分間該不織布を乾燥し、目付55g/m2 、水分率0.8%の不織布を得た。該不織布から任意に単繊維を20本取り出して強伸度測定した平均値は、繊度1.5デニール、強度は35g/d、弾性率800g/d、伸度4.5%であった。この不織布をさらにウオーターパンチを用いて交絡処理を施した。得られた不織布は良好な外観を有し、400℃のオーブン中で5時間加熱した後も形態の変化は認められなかった。
【0021】
<比較例1>冷却風温度を80℃とした他は実施例1と同じ紡出条件を用いてポリベンズビスオキサゾール繊維を紡糸口金より押し出した。図2に示すように、実施例1と異なりゴデットロールを用いることなく、圧搾空気を用いたアスピレータで吐出糸条を延伸し、該糸条を直接ネットコンベアに振り落とした。捕集された不織布は実施例1と同じく抽出、中和、水洗、乾燥工程を経てウエッブとして巻き取った。しかし気体を用いたアスピレータでは十分な牽引力が得られず、連続した繊維による不織布が得られず、糸切れと同時にアスピレータにドープがつまり、事実上不織布の作製が出来なかった。
【0022】
【発明の効果】
本発明により、耐熱、耐炎、耐磨耗に優れるポリベンザゾール不織布が従来の方法を用いるのに比べ、容易にかつ安価に製造可能になる。
【図面の簡単な説明】
【図1】本発明の実施例1の装置の模式図
【図2】比較例1の装置の模式図
【符号の説明】
1:紡糸ヘッド、2:クエンチチャンバー、3:テフロンコートしたゴデットロール、4:圧搾空気アスピレータ、5:不織布捕集ネットコンベアー、6:凝固浴ネットコンベアー、7:抽出浴ネットコンベアー、8:中和浴ネットコンベアー、9:水洗浴ネットコンベアー、10:乾燥機、11:ワインダー、14 :圧搾空気アスピレーター [0001]
[Industrial applications]
The present invention relates to a method for producing a high-strength, high-modulus polybenzoxazole-based nonwoven fabric. More particularly, the present invention relates to a spinning method that significantly facilitates a method for producing a nonwoven fabric.
[0002]
[Prior art]
Polybenzazole fibers have twice or more the strength and modulus of elasticity of polyparaphenylene terephthalamide fibers, which are representatives of currently marketed super fibers. Therefore, it is expected as a next-generation super fiber. It is known to make fibers from polyphosphoric acid solutions of polybenzazole polymers. For example, U.S. Pat. No. 5,296,185 and U.S. Pat. No. 5,294,390 have been proposed for the spinning method, and U.S. Pat. No. 5,288,445 has been proposed for the heat treatment method. However, there is no prior art about the method of producing a nonwoven fabric of polybenzazole fibers as far as the inventors know.
[0003]
[Problems to be solved by the invention]
Polybenzazole fiber nonwoven fabrics can be produced off-line in a conventional manner using long fibers or short fibers of polybenzazole fibers produced in a conventional manner. In addition, similarly to a general wet-spinning on-line non-woven fabric, it is also possible to guide a coagulated fiber or a dried fiber to a non-woven fabric manufacturing step to produce a non-woven fabric. However, even if the polybenzazole fiber is prepared by an efficient manufacturing method, the washing and drying steps are long, and if the washing and drying steps can be passed as a nonwoven fabric, the washing and drying can be efficiently performed without reducing the spinning speed. It is very economical. That is, although it is unheard of as a method of manufacturing a nonwoven fabric using wet spinning, if the process of directly collecting spun yarn on a net conveyor and forming the nonwoven fabric as in the process of manufacturing a nonwoven fabric of polyester or propylene can be applied, the spinning speed is increased. On the other hand, the process transfer speed of the nonwoven fabric can be extremely slow. On the other hand, processes that require a long time, such as extraction, washing, drying, and heat treatment, are facilitated with a nonwoven fabric. Therefore, there is a possibility that a nonwoven fabric of polybenzazole fiber can be manufactured at a low cost. The problem is that the dope composed of polybenzazole polymer and polyphosphoric acid is extremely high in viscosity and high in spinning tension, so that the ejection dope cannot be stretched at all by pulling with a gas. The present invention overcomes such technical difficulties and provides a novel production method for obtaining a polybenzazole nonwoven fabric industrially.
[0004]
Means for Solving the Problems The present inventors have made intensive studies and aimed at finding a solution for the purpose of facilitating the production of a polybenzazole nonwoven fabric. That is, a spinning dope composed of polybenzazole and polyphosphoric acid is spun from a spinneret. The discharged yarn has a very high elongational viscosity and cannot be easily drafted. So after giving a constant speed yarn at godet roll, the fluid (may be a liquid or a gas) Hikito Ru by aspirator. The yarn and fluid discharged from the aspirator are collected on a conveyor net. It has been found that a nonwoven fabric composed of a bundle of collected yarns is coagulated and / or extracted, and further dried to easily obtain a polybenzazole nonwoven fabric. The present invention aims at the manufacturing method.
[0005]
Hereinafter, the present invention will be described in detail.
The polybenzazole fiber in the present invention refers to a fiber made of a polybenzazole polymer, and the polybenzazole (PBZ) refers to a polybenzoxazole (PBO) homopolymer, a polybenzothiazole (PBT) homopolymer and their PBO, PBT refers to random, sequential or block copolymers. Here, polybenzoxazole, polybenzothiazole and their random, sequential or block copolymers are described, for example, in Wolfe et al., "Liquid Crystalline Polymer Compositions, Process and Products", U.S. Pat. No. 4,703,103 (October 27, 1987); "Liquid Crystall-ine Polymer Compositions, Process and Products" U.S. Patent No. 4,533,692 (August 6, 1985), "Liquid Crystalline Poly (2,6-Benzothiazole) Composition, Process and Products" U.S. Patent No. 4,533,724 (1985) Aug. 6), "Liquid Crystalline Polymer Compositions, Process and Products", U.S. Pat. No. 4,533,693 (August 6, 1985); No. 4,539,567 (November 16, 1982), Tasi et al., “Method for mak ing Heterocyclic Block Copolymer ", U.S. Patent No. 4,578,432 (March 25, 1986).
The structural unit contained in the PBZ polymer is preferably selected from a lyotropic liquid crystal polymer. The monomer unit consists of the monomer units described in structural formulas (a) to (h), and more preferably essentially consists of the monomer units selected from structural formulas (a) to (c).
[0006]
Embedded image
Figure 0003541966
[0007]
Embedded image
Figure 0003541966
[0008]
Suitable solvents for forming the dope of the PBZ polymer include cresol and non-oxidizing acids that can dissolve the polymer. Examples of suitable acid solvents include polyphosphoric acid, methanesulfonic acid and concentrated sulfuric acid or mixtures thereof. Further suitable solvents are polyphosphoric acid and methanesulfonic acid. The most suitable solvent is polyphosphoric acid.
[0009]
The concentration of the polymer in the solvent is preferably at least about 7% by weight, more preferably at least 10% by weight, and most preferably at least 14% by weight. The maximum concentration is limited by practical handling properties such as, for example, the solubility and dope viscosity of polyno. Because of these limiting factors, the polymer concentration does not usually exceed 20% by weight.
[0010]
Suitable polymers, copolymers or dopes are synthesized by known techniques. For example, US Pat. No. 4,533,693 to Wolfe et al. (August 6, 1985), US Pat. No. 4,772,678 to Sybert et al. (September 20, 1988), and US Pat. No. 4,847,350 to Harris (July 11, 1989). Synthesized in the manner described. According to Gregory et al., US Pat. No. 5,089,959 (February 18, 1992), PBZ polymers can be polymerized at a high reaction rate under a relatively high temperature and high shear condition in a dehydrating acid solvent. It is.
[0011]
The dope polymerized in this way is supplied to the spinning section and discharged from the spinneret at a temperature of usually 100 ° C. or higher. The arrangement of the base pores is usually plural in a circumferential or lattice shape, but other arrangements are also possible. The number of spinneret pores is not particularly limited, but the arrangement of the spinneret pores on the spinneret face must maintain a pore density that does not cause fusion between the discharge yarns.
[0012]
Next, the gist of the present invention is that the dope discharged from the spinneret (the yarn before extracting polyphosphoric acid) is subjected to a high tension by a stress isolator or a swingable aspirator using a liquid flow. Stretch. Providing a so-called quench chamber for cooling the yarn by using cooling air between the stress isolator or the liquid flow aspirator and the spinneret is effective for obtaining a high spinning speed.
[0013]
The stress isolation device generally uses a godet roll or the like. The roll is desirably made of a corrosion-resistant material, and the roll is desirably one having excellent releasability such as Teflon. When a stress isolator is used, an aspirator for producing a nonwoven fabric is provided downstream of the stress isolator, and the aspirator is used to collect the yarn in a nonwoven fabric collector such as a net conveyor. When the aspirator is a gas, by adjusting the temperature of the gas, fusion occurs between the collected single fibers of the nonwoven fabric, and an appropriate entanglement is obtained, which is desirable in some applications. The gas supplied to the aspirator is preferably an inert gas such as air or nitrogen gas, a carbon dioxide gas, or a mixed gas thereof. A jet of about 20 to 300 m / sec is ejected from the aspirator outlet.
[0015]
The collection atmosphere as a nonwoven fabric may be a liquid or a gas, but the nonwoven fabric captured by a net conveyor or the like is continuously coagulated and / or extracted, and finally the phosphoric acid contained in the yarn in the extraction bath is 99.0% or more. Preferably, it is 99.5% or more. The liquid used as the extraction medium in the present invention is not particularly limited, but is preferably water, methanol, or the like, which has substantially no compatibility with polybenzoxazole. Alternatively, the extraction bath may be separated into multiple stages, the concentration of the phosphoric acid aqueous solution may be gradually reduced, and finally, the aqueous solution may be washed with water. Further, the nonwoven fabric is neutralized with a sodium hydroxide aqueous solution or the like, and further washed with water.
[0016]
The washed nonwoven fabric is dried by a dryer using hot air or the like together with a collecting device such as a belt conveyor. The monofilament constituting the non-woven fabric thus obtained has a sufficient strength of 25 g / d or more and a sufficiently high elastic modulus of about 700 g / d, but the non-woven fabric is heat-treated immediately or separately at 350 ° C. or more. The application improves the elastic modulus of the single fiber to 1500 g / d or more.
[0017]
The nonwoven fabric is subjected to an adhesive treatment, a confounding treatment such as a needle punch or a water punch, or a calendering process, if necessary.
[0018]
The obtained non-woven fabric has excellent heat resistance and excellent tear strength, and has excellent features not found in non-woven fabrics obtained from other fibers as a heat-resistant protective material, heat-insulating protective material, wear-resistant protective material or flame-resistant protective material. Having.
[0019]
【Example】
Examples are shown below, but the present invention is not limited to these examples.
<Example 1>
14.0% by weight of a polybenzoxazole having an intrinsic viscosity of 24.4 dL / g measured by a methanesulfonic acid solution at 30 ° C. and a phosphorus pentoxide content of 83.17%, obtained by a method described in US Pat. No. 4,533,693. Was used for spinning. The dope was passed through a metal mesh filter medium, and then kneaded and defoamed with a kneading device consisting of two shafts. The pressure was increased, the temperature of the polymer solution was kept at 170 ° C., and pores were formed using the device shown in FIG. The yarn was spun at 170 ° C. from a spinneret having the number 334, and the discharged yarn was cooled using cooling air at a temperature of 60 ° C., and then wound around a godet roll whose surface was processed with Teflon to give a yarn speed of 200 m / min. Next, it was pulled using an aspirator using compressed air as a supply fluid, and collected by a net conveyor. The transfer speed of the net conveyor is 20 cm / min. Next, the collected nonwoven fabric together with the net conveyor was introduced into an extraction bath composed of a 10% phosphoric acid aqueous solution maintained at a temperature of 22 ± 2 ° C. Subsequently, the non-woven fabric collected on the net conveyor was further washed with ion-exchanged water in a second extraction bath, and then neutralized by immersion in a 0.1 N sodium hydroxide solution. After further washing with a water washing bath, the nonwoven fabric was dried in an air drying room kept at 190 ° C. for 5 minutes to obtain a nonwoven fabric having a basis weight of 55 g / m 2 and a water content of 0.8%. The average value of the strength and elongation measured by taking out 20 single fibers arbitrarily from the nonwoven fabric was 1.5 denier, the strength was 35 g / d, the elastic modulus was 800 g / d, and the elongation was 4.5%. This nonwoven fabric was further subjected to a confounding treatment using a water punch. The obtained nonwoven fabric had a good appearance, and no change in morphology was observed even after heating in an oven at 400 ° C. for 5 hours.
[0021]
<Comparative Example 1> A polybenzbisoxazole fiber was extruded from a spinneret under the same spinning conditions as in Example 1 except that the cooling air temperature was 80 ° C. As shown in FIG. 2, unlike Example 1, the discharged yarn was drawn by an aspirator using compressed air without using a godet roll, and the yarn was directly dropped onto a net conveyor. The collected nonwoven fabric was wound as a web through the extraction, neutralization, water washing, and drying steps as in Example 1. However, a gas-based aspirator could not provide sufficient traction force, could not obtain a nonwoven fabric made of continuous fibers, and the aspirator was doped at the same time as the yarn was broken.
[0022]
【The invention's effect】
According to the present invention, a polybenzazole nonwoven fabric excellent in heat resistance, flame resistance, and abrasion resistance can be easily and inexpensively manufactured as compared with a conventional method.
[Brief description of the drawings]
FIG. 1 is a schematic view of an apparatus according to Example 1 of the present invention. FIG. 2 is a schematic view of an apparatus according to Comparative Example 1 .
1: Spinning head, 2: Quench chamber, 3: Teflon-coated godet roll, 4: Compressed air aspirator, 5: Non-woven fabric collecting net conveyor, 6: Coagulation bath net conveyor, 7: Extraction bath net conveyor, 8: Neutralization bath Net conveyor, 9: Rinse bath net conveyor, 10: Dryer, 11: Winder, 14 : Compressed air aspirator

Claims (2)

ポリリン酸とポリベンザゾールからなる紡糸ドープを紡糸口金から押しだし、次いで得られたドープフィラメントをゴデットロールで一定の糸条速度を与えた後、液体流または気体流を用いたアスピレータで牽引して捕集面上に分散堆積し、次いでネットコンベア上でポリリン酸を洗浄除去し乾燥することを特徴とするポリベンザゾール繊維不織布の製造法。A spin dope composed of polyphosphoric acid and polybenzazole is pushed out from a spinneret, and the obtained dope filament is given a constant yarn speed by a godet roll, and then collected by being pulled by an aspirator using a liquid stream or a gas stream. A method for producing a polybenzazole fiber nonwoven fabric, comprising dispersing and depositing on a surface, and then washing and removing polyphosphoric acid on a net conveyor and drying. ポリベンザゾール繊維不織布を交絡処理することを特徴とする請求項1記載のポリベンザゾール繊維不織布の製造法。The method for producing a polybenzazole fiber nonwoven fabric according to claim 1, wherein the nonwoven fabric of the polybenzazole fiber is entangled.
JP18242094A 1994-08-03 1994-08-03 Method for producing nonwoven fabric of polybenzazole fiber Expired - Fee Related JP3541966B2 (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
JP18242094A JP3541966B2 (en) 1994-08-03 1994-08-03 Method for producing nonwoven fabric of polybenzazole fiber
PCT/US1995/009818 WO1996004413A1 (en) 1994-08-03 1995-08-02 Process of making polybenzazole nonwoven fabric
ES95928723T ES2186726T3 (en) 1994-08-03 1995-08-02 PROCEDURE FOR PREPARATION OF A FABRIC NON-WOVEN POLIBENZOXAZOL.
DE69529221T DE69529221T2 (en) 1994-08-03 1995-08-02 METHOD FOR PRODUCING POLYBENZAZOLE FLEECE
EP95928723A EP0775221B1 (en) 1994-08-03 1995-08-02 Process of making polybenzazole nonwoven fabric
US08/793,039 US5756040A (en) 1994-08-03 1995-08-02 Process of making polybenzazole nonwoven fabric
CA 2194989 CA2194989A1 (en) 1994-08-03 1995-08-02 Process of making polybenzazole nonwoven fabric
MXPA/A/1997/000815A MXPA97000815A (en) 1994-08-03 1997-01-31 Procedure for preparing non-woven fabrics depolibenza

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US5534205A (en) * 1994-08-05 1996-07-09 The Dow Chemical Company Method for preparing polybenzoxazole or polybenzothiazole fibers
US5633161A (en) * 1995-03-29 1997-05-27 Millennium Pharmaceuticals, Inc. Murine gene fomy030 coding for tumor progression inhibitor
DE602007010308D1 (en) * 2006-07-31 2010-12-16 Du Pont FLEECE TRAIL WITH POLYARENAZOLE MICROFIBERS AND METHOD FOR THE PRODUCTION THEREOF
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US5164131A (en) * 1990-09-19 1992-11-17 The Dow Chemical Company Methods for synthesizing pulps and short fibers containing polybenzazole polymers
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CA2194989A1 (en) 1996-02-15
EP0775221A4 (en) 1997-11-12
ES2186726T3 (en) 2003-05-16
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