JP2001262469A - Super high-molecular weight polyethylene fiber excellent in adhesivity and method for manufacturing the same - Google Patents
Super high-molecular weight polyethylene fiber excellent in adhesivity and method for manufacturing the sameInfo
- Publication number
- JP2001262469A JP2001262469A JP2000072765A JP2000072765A JP2001262469A JP 2001262469 A JP2001262469 A JP 2001262469A JP 2000072765 A JP2000072765 A JP 2000072765A JP 2000072765 A JP2000072765 A JP 2000072765A JP 2001262469 A JP2001262469 A JP 2001262469A
- Authority
- JP
- Japan
- Prior art keywords
- molecular weight
- weight polyethylene
- fiber
- treatment
- silane coupling
- 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.)
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Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、複合材料の極性高分子
マトリックスとの接着性に優れ、補強材料として優れた
超高分子量ポリエチレン繊維及びその製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ultra-high molecular weight polyethylene fiber having excellent adhesion to a polar polymer matrix of a composite material and excellent as a reinforcing material, and a method for producing the same.
【０００２】[0002]
【従来の技術】従来から極性高分子マトリックス材料中
に、フィラメント形態の強化材料を埋め込む繊維強化複
合材料が使用されてきた。この強化材料としてはガラス
繊維、炭素繊維、アラミド繊維などが挙げられ、炭素繊
維は弾性率及び引張強度において極めて優れて優れ、ま
たガラス繊維は安価である、さらに、アラミド繊維は軽
量である等の優れた利点を有する。しかし、いずれも比
重が約１．４以上と高く、極性高分子マトリックスの補
強材として用いた時得られた繊維強化複合材料の重量が
大きくなる欠点があった。その点ポリエチレンは比重が
１．０であり、それで得られた繊維は軽量化ができ繊維
強化補強材料の重量を軽減できることが容易に予測でき
るが、従来のポリエチレン繊維は引張強度が低く強化材
料としての補強効果が小さという問題があった。そこ
で、引張強度が３ＧＰａ以上、弾性率が１００ＧＰａ以
上の超高分子量のポリエチレン繊維が特開昭５５−１０
７５０６号公報、特開平６−２８０１０９号公報等で提
案され、この超高分子量のポリエチレン繊維の表面を例
えばコロナ放電処理等で活性化し極性高分子マトリック
スとの接着力を強化する方法が特開昭６０−１４６０７
８号公報等で提案されている。ところが、この公報方法
ではコロナ放電処理中に繊維が高温となり結晶の部分融
解を起こし引張強度が低下したり、あるいは官能基が高
密度に形成されず極性高分子マトリックスとの接着性が
劣る等の問題があった。この接着性の改質のためポリエ
チレン繊維の紡出時の条件を特定なものにすることで、
接着性を改善する超高分子量のポリエチレン繊維繊維が
例えば特開昭６２−１８４１１０号公報、特開平６−２
８０１０８号公報等で提案されているが、いずれも極性
高分子マトリックスとの接着強度が充分でなく、強化材
料として満足の行くものではなかった。2. Description of the Related Art A fiber-reinforced composite material in which a reinforcing material in the form of a filament is embedded in a polar polymer matrix material has conventionally been used. Examples of the reinforcing material include glass fiber, carbon fiber, and aramid fiber.Carbon fiber is extremely excellent in elastic modulus and tensile strength, glass fiber is inexpensive, and aramid fiber is lightweight. Has excellent advantages. However, each has a drawback that the specific gravity is as high as about 1.4 or more, and the weight of the fiber-reinforced composite material obtained when used as a reinforcing material for the polar polymer matrix is increased. In that respect, polyethylene has a specific gravity of 1.0, and it can easily be predicted that the fiber obtained therefrom can be reduced in weight and the weight of the fiber-reinforced reinforcing material can be reduced, but the conventional polyethylene fiber has a low tensile strength and is used as a reinforcing material. However, there is a problem that the reinforcing effect is small. Therefore, an ultrahigh molecular weight polyethylene fiber having a tensile strength of 3 GPa or more and an elastic modulus of 100 GPa or more is disclosed in
JP-A-7506 and JP-A-6-280109 propose a method of activating the surface of this ultrahigh molecular weight polyethylene fiber by, for example, corona discharge treatment to enhance the adhesive force with a polar polymer matrix. 60-14607
No. 8 has been proposed. However, in this publication method, the fiber becomes high temperature during corona discharge treatment, causing partial melting of the crystal and lowering the tensile strength, or the functional groups are not formed at a high density and the adhesion to the polar polymer matrix is poor. There was a problem. By making the conditions at the time of spinning polyethylene fibers specific for this adhesion improvement,
Ultrahigh molecular weight polyethylene fibers for improving the adhesiveness are disclosed in, for example, JP-A-62-184110 and JP-A-6-2.
No. 80108 proposes such a method, but none of them has a sufficient adhesive strength with a polar polymer matrix and is not satisfactory as a reinforcing material.
【０００３】[0003]
【発明が解決しようとする課題】こうした現状に鑑み、
本発明者等は、鋭意研究を続けた結果、超高分子量のポ
リエチレン繊維を、物理的処理を２回以上行った後、特
定のシランカップリング剤で処理を施すことで、引張強
度や初期弾性率が高い上に、高い接着力を有し、極性高
分子マトリックスとのせん断強度が高い超高分子量のポ
リエチレン繊維が得られることを見出して本発明を完成
したものである。すなわち、In view of the current situation,
The inventors of the present invention have conducted intensive studies and have found that, after performing physical treatment twice or more on ultra-high molecular weight polyethylene fibers, the fibers are treated with a specific silane coupling agent to obtain tensile strength and initial elasticity. The inventors have found that an ultrahigh molecular weight polyethylene fiber having a high modulus, a high adhesive strength, and a high shear strength with a polar polymer matrix can be obtained, thereby completing the present invention. That is,
【０００４】本発明は、接着性に優れ、かつ引張強度、
初期弾性率の高い超高分子量ポリエチレン繊維を提供す
ることを目的とする。[0004] The present invention provides excellent adhesiveness, tensile strength,
An object is to provide an ultrahigh molecular weight polyethylene fiber having a high initial elastic modulus.
【０００５】また、本発明は、上記超高分子量ポリエチ
レン繊維の製造方法を提供することを目的とする。Another object of the present invention is to provide a method for producing the above ultrahigh molecular weight polyethylene fiber.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成する本発
明は、エチレンを主体とし、重量平均分子量が１００万
以上の超高分子量ポリエチレンからなる繊維であって、
物理的処理が２回以上施され、次いでアミノ系シランカ
ップリング剤処理され、引張強度が２．５ＧＰａ以上、
初期弾性率が１００ＧＰａ以上であることを特徴とする
超高分子量ポリエチレン繊維及びその製造方法に関す
る。SUMMARY OF THE INVENTION The present invention, which achieves the above objects, is a fiber comprising ultra-high molecular weight polyethylene mainly composed of ethylene and having a weight average molecular weight of 1,000,000 or more,
Physical treatment is performed twice or more, then amino-based silane coupling agent treatment, tensile strength is 2.5 GPa or more,
The present invention relates to an ultrahigh molecular weight polyethylene fiber having an initial elastic modulus of 100 GPa or more and a method for producing the same.
【０００７】本発明の超高分子量ポリエチレン繊維は、
エチレンを主体とし、少量の他のモノマー例えばα−オ
レフィン、アクリル酸及びその誘導体、メタクリル酸及
びその誘導体、ビニルシラン及びその誘導体などとの共
重合体であってもよく、重量平均分子量が１００万以上
の超高分子量で、かつ物理的処理が２回以上施され、次
いでアミノ系シランカップリング剤処理され、引張強度
が２．５Ｐａ以上、弾性率が１００ＧＰａ以上の接着性
に優れたポリエチレン繊維である。[0007] The ultrahigh molecular weight polyethylene fiber of the present invention comprises:
Mainly ethylene, it may be a copolymer with a small amount of other monomers such as α-olefin, acrylic acid and its derivatives, methacrylic acid and its derivatives, vinylsilane and its derivatives, and has a weight average molecular weight of 1,000,000 or more. An ultra-high molecular weight, physical treatment is performed twice or more, and then an amino-based silane coupling agent treatment is performed, and the tensile strength is 2.5 Pa or more, and the elastic modulus is 100 GPa or more. .
【０００８】このように本発明の超高分子量ポリエチレ
ン繊維は、２回以上、好ましくは２〜４回の物理的処理
が施され、その後アミノ系シランカップリング剤処理が
施された繊維であるが、前記物理的処理とはコロナ放電
処理、火炎処理、電子線照射、紫外線照射等の処理をい
う。この物理的処理を２回以上、好ましくは２〜４回行
うことで繊維表面に水酸基やカルボキシル基の官能基が
均一に生成し極性高分子マトリックスとの接着強度が向
上する。物理的処理が１回では、官能基の生成が不十分
で好ましくなく、４回以上では超高分子ポリエチレン繊
維の引張強度や初期弾性率が低下して好ましくない。特
に好ましい物理的処理はコロナ放電処理であり、放電量
を２００〜１０００Ｗの範囲で行うのがよい。[0008] As described above, the ultrahigh molecular weight polyethylene fiber of the present invention is a fiber that has been subjected to physical treatment twice or more, preferably 2 to 4 times, and then treated with an amino silane coupling agent. The physical treatment means a treatment such as a corona discharge treatment, a flame treatment, an electron beam irradiation, and an ultraviolet irradiation. By performing this physical treatment two or more times, preferably two to four times, a functional group such as a hydroxyl group or a carboxyl group is uniformly formed on the fiber surface, and the adhesive strength with the polar polymer matrix is improved. One physical treatment is not preferable because the functional groups are insufficiently generated, and four or more physical treatments are not preferable because the tensile strength and the initial elastic modulus of the ultrahigh molecular weight polyethylene fiber decrease. Particularly preferred physical treatment is corona discharge treatment, and the discharge amount is preferably in the range of 200 to 1000 W.
【０００９】前記物理的処理に続いて本発明の超高分子
量ポリエチレン繊維は、アミノ系シランカップリング剤
処理に供されるが、該アミノ系シランカップリング処理
に使用するシランカップリング剤としては、例えばＮ−
（２−アミノエチル）−３−アミノプロピルメチルジメ
トキシシラン、３−アミノプロピルトリエトキシシラ
ン、３−グリシドキシプロピルトリメトキシシラン、Ｎ
−β−（Ｎ−ビニルベンジルアミノエチル）γ−アミノ
プロピルトリメトキシシラン塩酸塩、アリルオキシ−２
−アミノエチルアミノメチルジシラザン、３−アリルア
ミノプロピルトリメトキシシラザン、ビニルトリメトキ
シシラン、ビニルトリエトキシシラン、ビニルトリクロ
ロシラン等のアミノ系シランカップリング剤が挙げら
れ、このアミノ系シランカップリング処理により超高分
子ポリエチレン繊維は極性高分子マトリックスとの強固
な界面せん断力が得られる。Following the physical treatment, the ultrahigh molecular weight polyethylene fiber of the present invention is subjected to an amino-based silane coupling agent treatment. The silane coupling agent used in the amino-based silane coupling treatment includes: For example, N-
(2-aminoethyl) -3-aminopropylmethyldimethoxysilane, 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, N
-Β- (N-vinylbenzylaminoethyl) γ-aminopropyltrimethoxysilane hydrochloride, allyloxy-2
-Aminoethylaminomethyldisilazane, 3-allylaminopropyltrimethoxysilazane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltrichlorosilane, and other amino-based silane coupling agents, and the like. Ultra-high molecular weight polyethylene fibers have a strong interfacial shear force with the polar polymer matrix.
【００１０】上記極性高分子マトリックス材料として
は、エポキシ、ポリアミド、不飽和ポリエステル、フェ
ノール、アクリル、ポリメチルメタクリル等の樹脂が挙
げられ、好ましくはエポキシ、ポリアミド、不飽和ポリ
エステル樹脂がよい。Examples of the polar polymer matrix material include resins such as epoxy, polyamide, unsaturated polyester, phenol, acryl and polymethyl methacryl, and preferably epoxy, polyamide and unsaturated polyester resin.
【００１１】[0011]
【実施例】以下に本発明を実施例に基づいて具体的に説
明するが、本発明はこれに限定されるものではない。な
お、アミノ系シランカップリング剤処理後のポリエチレ
ン繊維の引張強度、初期弾性率、官能基量及び極性高分
子カップリング材料との界面せん断強度は、以下の測定
方法による。 （ｉ）引張強度、初期弾性率は、引張試験機（商品名オ
ートグラフＡＧＳ−１０００、島津製作所製）を用いて
求めた。 （ｉｉ）官能基量はＸ線光電子分析法により求めた。 （ｉｉｉ）界面せん断強度は微小液滴引抜法から求め
た。EXAMPLES The present invention will be specifically described below based on examples, but the present invention is not limited to these examples. The tensile strength, initial elastic modulus, amount of functional group, and interfacial shear strength with the polar polymer coupling material of the polyethylene fiber after the amino-based silane coupling agent treatment are measured by the following methods. (I) The tensile strength and the initial elastic modulus were determined using a tensile tester (trade name Autograph AGS-1000, manufactured by Shimadzu Corporation). (Ii) The functional group content was determined by X-ray photoelectron analysis. (Iii) The interfacial shear strength was determined by a microdroplet drawing method.
【００１２】実施例 重量平均分子量１５０万の超高分子ポリエチレンをから
なる超高分子ポリエチレン繊維を４００、８００Ｗの放
電量でコロナ放電処理を行った。処理後のポリエチレン
繊維表面の官能基量は表１のとおりであった。EXAMPLE Ultra-high-molecular-weight polyethylene fibers made of ultra-high-molecular-weight polyethylene having a weight-average molecular weight of 1.5 million were subjected to a corona discharge treatment at a discharge amount of 400 or 800 W. The functional group content on the polyethylene fiber surface after the treatment was as shown in Table 1.
【００１３】[0013]
【表１】 [Table 1]
【００１４】上記表１にみるように２回のコロナ放電で
官能基が有効に生成している。この繊維にエポキシ樹脂
（エピコート８２８、油化シェルエポキシ社製）と硬化
剤（エポメートＬＸ−１、油化シェルエポキシ社製）と
の混合物を液滴として付与し、８０℃で３時間硬化処理
をした後、界面せん断強度を微小液滴引抜法で求めた。
その結果を表２に示す。As shown in Table 1 above, the functional groups are effectively generated by two corona discharges. A mixture of an epoxy resin (Epicoat 828, manufactured by Yuka Shell Epoxy) and a curing agent (Epomate LX-1, manufactured by Yuka Shell Epoxy) is applied to the fiber as droplets, and cured at 80 ° C. for 3 hours. After that, the interfacial shear strength was determined by a microdroplet drawing method.
Table 2 shows the results.
【００１５】[0015]
【表２】 [Table 2]
【００１６】次いで、コロナ放電処理を２回行った繊維
をＮ−（２−アミノエチル）−３−アミノプロピルメチ
ルジメトキシシランのトルエン１０ｗｔ％溶液に２５℃
で３時間浸漬したのち、先のエポキシ樹脂の液滴をつけ
８０℃で３時間硬化させ、界面せん断強度を測定した。
その結果を表３に示す。Next, the fiber subjected to the corona discharge treatment twice was added to a 10 wt% solution of N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane in toluene at 25 ° C.
After immersion for 3 hours, the epoxy resin droplets were applied and cured at 80 ° C. for 3 hours, and the interfacial shear strength was measured.
Table 3 shows the results.
【００１７】[0017]
【表３】 上記表３から明らかなようにアミノ系シランカップリン
グ剤処理することで本発明の超高分子ポリエチレン繊維
はエポキシ樹脂との界面せん断強度が該アミノ系シラン
カップリング剤処理をしない超高分子ポリエチレン繊維
に比して約１．６倍に向上していた。[Table 3] As is evident from Table 3 above, the ultra-high molecular weight polyethylene fiber of the present invention has an interfacial shear strength with an epoxy resin which is not treated with the amino type silane coupling agent. Was improved about 1.6 times as compared with.
【００１８】[0018]
【発明の効果】本発明のポリエチレン繊維は極性高分子
マトリックス材料との接着力が高く、かつ引張強度、弾
性率の低下が少なく、強化材料として優れ、得られた構
造材料は軽量であるが、高い強度を有し工業材料として
有用である。The polyethylene fiber of the present invention has a high adhesive strength to a polar polymer matrix material, a small decrease in tensile strength and elastic modulus, is excellent as a reinforcing material, and the obtained structural material is lightweight. It has high strength and is useful as an industrial material.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｄ０６Ｍ 101:20 Ｄ０６Ｍ 101:20 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification code FI Theme coat ゛ (Reference) D06M 101: 20 D06M 101: 20
Claims (5)
００万以上の超高分子量ポリエチレンからなる繊維であ
って、物理的処理が２回以上施され、かつアミノ系シラ
ンカップリング剤処理がなされ、引張強度が２．５ＧＰ
ａ以上、弾性率が１００ＧＰａ以上であることを特徴と
する超高分子量ポリエチレン繊維。An ethylene-based resin having a weight average molecular weight of 1
A fiber made of ultra-high molecular weight polyethylene of 100,000 or more, which has been subjected to a physical treatment twice or more, an amino-based silane coupling agent treatment, and a tensile strength of 2.5 GP.
An ultrahigh molecular weight polyethylene fiber having an elastic modulus of at least a and an elastic modulus of at least 100 GPa.
００万以上の超高分子量ポリエチレン繊維を２回以上の
物理的処理をしたのち、アミノ系シランカップリング剤
処理することを特徴とする超高分子量ポリエチレン繊維
の製造方法。2. A composition mainly comprising ethylene and having a weight average molecular weight of 1
A method for producing ultrahigh molecular weight polyethylene fibers, comprising subjecting 100,000 or more ultrahigh molecular weight polyethylene fibers to physical treatment twice or more, and then treating with an amino-based silane coupling agent.
特徴とする請求項２記載の超高分子量ポリエチレン繊維
の製造方法。3. The method for producing ultrahigh molecular weight polyethylene fibers according to claim 2, wherein the physical treatment is a corona discharge treatment.
Ｗで２回以上行われることを特徴とする請求項３記載の
超高分子量ポリエチレン繊維の製造方法。4. The method according to claim 1, wherein the corona discharge treatment has a discharge amount of 200 to 1000.
The method for producing ultra-high molecular weight polyethylene fiber according to claim 3, wherein the step is performed twice or more with W.
中にアミノ基又はイミノ基を有するシランカップリング
剤による処理であることを特徴とする請求項２記載の超
高分子量ポリエチレン繊維の製造方法。5. The method for producing ultrahigh molecular weight polyethylene fibers according to claim 2, wherein the treatment with an amino silane coupling agent is a treatment with a silane coupling agent having an amino group or an imino group in a molecule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000072765A JP4315311B2 (en) | 2000-03-15 | 2000-03-15 | Ultra high molecular weight polyethylene fiber excellent in adhesiveness and production method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000072765A JP4315311B2 (en) | 2000-03-15 | 2000-03-15 | Ultra high molecular weight polyethylene fiber excellent in adhesiveness and production method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2001262469A true JP2001262469A (en) | 2001-09-26 |
| JP4315311B2 JP4315311B2 (en) | 2009-08-19 |
Family
ID=18591123
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000072765A Expired - Fee Related JP4315311B2 (en) | 2000-03-15 | 2000-03-15 | Ultra high molecular weight polyethylene fiber excellent in adhesiveness and production method thereof |
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|---|---|
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