JP3160277U - Polylactic acid-based spunbond nonwoven fabric - Google Patents
Polylactic acid-based spunbond nonwoven fabric Download PDFInfo
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- JP3160277U JP3160277U JP2010002403U JP2010002403U JP3160277U JP 3160277 U JP3160277 U JP 3160277U JP 2010002403 U JP2010002403 U JP 2010002403U JP 2010002403 U JP2010002403 U JP 2010002403U JP 3160277 U JP3160277 U JP 3160277U
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- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 41
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 39
- 239000004626 polylactic acid Substances 0.000 title claims abstract description 37
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims abstract description 36
- 239000000835 fiber Substances 0.000 claims abstract description 27
- 229930182843 D-Lactic acid Natural products 0.000 claims abstract description 25
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 claims abstract description 25
- 229940022769 d- lactic acid Drugs 0.000 claims abstract description 25
- 229920001577 copolymer Polymers 0.000 claims abstract description 17
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920001059 synthetic polymer Polymers 0.000 abstract 1
- 239000004416 thermosoftening plastic Substances 0.000 abstract 1
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000002074 melt spinning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000007334 copolymerization reaction Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004049 embossing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 229920003232 aliphatic polyester Polymers 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- WSQZNZLOZXSBHA-UHFFFAOYSA-N 3,8-dioxabicyclo[8.2.2]tetradeca-1(12),10,13-triene-2,9-dione Chemical compound O=C1OCCCCOC(=O)C2=CC=C1C=C2 WSQZNZLOZXSBHA-UHFFFAOYSA-N 0.000 description 1
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- BELBBZDIHDAJOR-UHFFFAOYSA-N Phenolsulfonephthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2S(=O)(=O)O1 BELBBZDIHDAJOR-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 150000001718 carbodiimides Chemical class 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229960003531 phenolsulfonphthalein Drugs 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
【課題】 耐熱性が付与されてなるポリ乳酸系重合体により構成されるスパンボンド不織布を提供する。【解決手段】 Ｄ−乳酸とＬ−乳酸との共重合体であって、該共重合体におけるＤ−乳酸の含有量が０．８モル％以下である重合体を主成分とする連続繊維によって構成されることを特徴とするポリ乳酸系スパンボンド不織布である。Ｄ−乳酸とＬ−乳酸との共重合体のカルボキシル末端基濃度が２０モル／ｔｏｎ以下であることが好ましい。連続繊維は、Ｄ−乳酸とＬ−乳酸との共重合体と、ポリ乳酸以外の他の熱可塑性合成重合体とが複合してなる複合繊維であることも好ましい。【選択図】 図１PROBLEM TO BE SOLVED: To provide a spunbonded nonwoven fabric composed of a polylactic acid polymer imparted with heat resistance. SOLUTION: A continuous fiber composed mainly of a copolymer of D-lactic acid and L-lactic acid, wherein the content of D-lactic acid in the copolymer is 0.8 mol% or less. It is a polylactic acid-based spunbonded nonwoven fabric characterized by being constituted. It is preferable that the carboxyl end group concentration of the copolymer of D-lactic acid and L-lactic acid is 20 mol / ton or less. The continuous fiber is also preferably a composite fiber formed by combining a copolymer of D-lactic acid and L-lactic acid and a thermoplastic synthetic polymer other than polylactic acid. [Selection] Figure 1
Description
本考案は、熱安定性に優れたポリ乳酸系スパンボンド不織布に関するものである。 The present invention relates to a polylactic acid-based spunbonded nonwoven fabric excellent in thermal stability.
近年、石油を原料とする合成繊維は、焼却時の発熱量が多いため、自然環境保護の見地から見直しが必要とされている。これに対し、自然界において生分解する脂肪族ポリエステルからなる繊維が開発されており、環境保護への貢献が期待されている。脂肪族ポリエステルの中でも、ポリ乳酸系重合体は、比較的高い融点を有することから、広い分野に使用されることが期待されている。 In recent years, synthetic fibers using petroleum as a raw material have a large amount of heat generated during incineration, and therefore need to be reviewed from the viewpoint of protecting the natural environment. In contrast, fibers made of aliphatic polyester that biodegrades in nature have been developed and are expected to contribute to environmental protection. Among aliphatic polyesters, polylactic acid polymers are expected to be used in a wide range of fields because they have a relatively high melting point.
しかしながら、ポリ乳酸系重合体からなる繊維や不織布は、高温での力学特性に劣るため、通常の雰囲気下で用いる場合は問題ないが、高温雰囲気下では変形やへたりが生じる。このため、例えば、炎天下に晒されるような自動車用の内装材には不向きである。また、例えば、ポリ乳酸系長繊維不織布を成形用カーペットに使用した際において、１３０℃、１４０℃といった成形温度にて成形した場合には、高温下での不織布の強力・伸度の低さが成形性を悪くし、特に、深絞り成形を行った部分においてはカーペット基布が破れてしまうといった問題が発生している。 However, fibers and non-woven fabrics made of polylactic acid-based polymers are inferior in mechanical properties at high temperatures, so there is no problem when used in a normal atmosphere. For this reason, for example, it is unsuitable for the interior material for motor vehicles exposed to the sun. In addition, for example, when a polylactic acid-based long-fiber nonwoven fabric is used for a carpet for molding, when it is molded at a molding temperature such as 130 ° C. or 140 ° C., the strength and elongation of the nonwoven fabric at high temperatures are low. There is a problem that the carpet base fabric is torn, particularly in the portion where the deep drawing has been performed, resulting in poor moldability.
本件出願人は、このような状況に鑑みて、ポリ乳酸系重合体からなる長繊維不織布が有する欠点を補うべく、スパンボンド法により得られたポリ乳酸系繊維ウェブと芳香族ポリエステルからなる繊維ウェブとを積層し交絡により一体化することによって耐熱性を付与する技術を提案している（特許文献１）。 In view of such circumstances, the applicant of the present application has made a fiber web made of a polylactic acid fiber web and an aromatic polyester obtained by a spunbond method in order to compensate for the shortcomings of the long fiber nonwoven fabric made of a polylactic acid polymer. Has been proposed (Patent Literature 1).
本考案は、耐熱性が付与されてなるポリ乳酸系重合体により構成されるスパンボンド不織布を提供することを課題とする。 An object of the present invention is to provide a spunbonded nonwoven fabric composed of a polylactic acid polymer to which heat resistance is imparted.
本考案は、Ｄ−乳酸とＬ−乳酸との共重合体であって、該共重合体のＤ−乳酸の含有量が０．８モル％以下である重合体を主成分とする連続繊維によって構成されることを特徴とするポリ乳酸系スパンボンド不織布を要旨とするものである。 The present invention is a copolymer of D-lactic acid and L-lactic acid, wherein the copolymer has a D-lactic acid content of 0.8 mol% or less as a main component. The gist of the present invention is a polylactic acid-based spunbonded non-woven fabric characterized by being constituted.
以下、本考案について詳細に説明する。 Hereinafter, the present invention will be described in detail.
本考案のポリ乳酸系スパンボンド不織布は、Ｄ−乳酸とＬ−乳酸との共重合体であるポリ乳酸を主成分とする連続繊維によって構成される。Ｄ−乳酸とＬ−乳酸との共重合体であるポリ乳酸は、Ｄ−乳酸の含有量が０．８モル％以下のＬ−乳酸を主体とするものであり、乳酸以外の他の成分を共重合するものではなく、ホモポリ乳酸である。本考案では、市場で容易に入手できるＤ−乳酸の含有量が１モル％以上のポリ乳酸ではなく、Ｄ−乳酸の含有量をより低減させて１モル％未満のホモポリ乳酸とし、このホモポリ乳酸を用いてスパンボンド不織布とすることにより、不織布に耐熱性や高温下での耐久性を付与することができる。本考案に用いるＤ−乳酸の含有量が０．８モル％以下であるポリ乳酸は、融点が１７０℃以上である。 The polylactic acid-based spunbonded nonwoven fabric of the present invention is composed of continuous fibers whose main component is polylactic acid, which is a copolymer of D-lactic acid and L-lactic acid. Polylactic acid, which is a copolymer of D-lactic acid and L-lactic acid, is mainly composed of L-lactic acid having a D-lactic acid content of 0.8 mol% or less. It does not copolymerize and is homopolylactic acid. In the present invention, it is not a polylactic acid having a D-lactic acid content of 1 mol% or more that is readily available in the market, but a D-lactic acid content is further reduced to a homopolylactic acid having a content of less than 1 mol%. By using as a spunbonded nonwoven fabric, heat resistance and durability at high temperatures can be imparted to the nonwoven fabric. The polylactic acid having a D-lactic acid content of 0.8 mol% or less used in the present invention has a melting point of 170 ° C. or higher.
また、本考案のスパンボンド不織布におけるＤ−乳酸とＬ−乳酸との共重合体であるポリ乳酸のカルボキシル末端基濃度は、２０モル／ｔｏｎ以下であることが好ましく、より好ましくは１０モル／ｔｏｎ以下である。カルボキシル末端基濃度を２０モル／ｔｏｎ以下とすることにより、スパンボンド不織布の耐熱性や高温下での耐久性が良好となる。カルボキシル末端基濃度を２０モル／ｔｏｎ以下とする方法としては、原料となるポリ乳酸において、カルボキシル末端基濃度を低減させたものを用いるとよく、例えば、原料となるポリ乳酸にモノカルボジイミド類やジカルボジイミド類などの末端封鎖剤を添加することにより行うとよい。なお、カルポキシル末端基濃度の測定としては、ＪＩＳ Ｋ ００７０ 酸価 中和滴定法に準じて、以下のように行った。すなわち、５０ｍｌ三角フラスコに０．１５ｇの試料と２０ｍｌの溶剤（塩化メチレン）を入れ、これに指示薬（フェノールレッド）を加えた後、０．１モル／ｌの水酸化カリウム溶液で滴定した。 In addition, the carboxyl end group concentration of polylactic acid which is a copolymer of D-lactic acid and L-lactic acid in the spunbonded nonwoven fabric of the present invention is preferably 20 mol / ton or less, more preferably 10 mol / ton. It is as follows. By setting the carboxyl end group concentration to 20 mol / ton or less, the heat resistance and durability at high temperatures of the spunbonded nonwoven fabric are improved. As a method for setting the carboxyl end group concentration to 20 mol / ton or less, it is preferable to use a polylactic acid as a raw material with a reduced carboxyl end group concentration. It is good to carry out by adding terminal blockers, such as carbodiimides. Carboxyl end group concentration was measured according to JIS K 0070 acid value neutralization titration method as follows. That is, a 0.15 g sample and 20 ml of a solvent (methylene chloride) were placed in a 50 ml Erlenmeyer flask, and an indicator (phenol red) was added thereto, followed by titration with a 0.1 mol / l potassium hydroxide solution.
本考案において、連続繊維は、上記したＤ−乳酸とＬ−乳酸との共重合体のみからなる単相の形態であってもよいが、Ｄ−乳酸とＬ−乳酸との共重合体と、ポリ乳酸以外の他の熱可塑性重合体とが複合してなる複合の形態である複合繊維であってもよい。ポリ乳酸以外の他の熱可塑性重合体と複合することにより、本考案のスパンボンド不織布に種々の性能を付与することができる。複合の形態としては、例えば、図１に示すような芯鞘型が挙げられる。また、貼り合わせ型、分割型等の形態のものが挙げられる。なお、図１には、芯部にポリ乳酸、鞘部に他の熱可塑性重合体が配されるように示したが、用途や性能に応じて、芯部に他の熱可塑性重合体を配し、鞘部にポリ乳酸を配してもよい。ポリ乳酸以外の他の熱可塑性重合体としては、ブチレンテレフタレートやエチレンテレフタレートを主たる繰り返し単位とする芳香族ポリエステル、ポリエチレンやポリプロピレン等のポリオレフィン、ナイロン６等のポリアミドが挙げられる。 In the present invention, the continuous fiber may be in the form of a single phase consisting only of the above-mentioned copolymer of D-lactic acid and L-lactic acid, but a copolymer of D-lactic acid and L-lactic acid, It may be a composite fiber in the form of a composite formed by a composite with a thermoplastic polymer other than polylactic acid. By combining with other thermoplastic polymers than polylactic acid, various performances can be imparted to the spunbonded nonwoven fabric of the present invention. Examples of the composite form include a core-sheath type as shown in FIG. Moreover, the thing of forms, such as a bonding type | mold and a split type, is mentioned. Although FIG. 1 shows polylactic acid in the core and other thermoplastic polymer in the sheath, other thermoplastic polymer is arranged in the core depending on the application and performance. And polylactic acid may be arranged in the sheath. Examples of other thermoplastic polymers other than polylactic acid include aromatic polyesters mainly composed of butylene terephthalate and ethylene terephthalate, polyolefins such as polyethylene and polypropylene, and polyamides such as nylon 6.
本考案のスパンボンド不織布は、公知のスパンボンド装置を用いて高速で溶融紡糸を行うことにより得られる。すなわち、原料となるポリ乳酸、さらに複合繊維を得る場合は他の熱可塑性重合体を準備し、紡糸口金を介して溶融紡糸し、紡糸口金から吐出した糸条を従来公知の横吹き付けや環状吹きつけ等の冷却装置を用いて冷却せしめた後、吸引装置を用いて牽引細化して引き取る。高速で溶融紡糸することにより、ポリ乳酸を良好に分子配向させて結晶化させることができ、耐熱性がより向上する。溶融紡糸の際の牽引速度は４０００ｍ／分以上、より好ましくは５０００ｍ／分以上である。牽引細化により引き取った多数の繊維が堆積してなるスパンボンド不織ウェブは、公知の手段により不織布化すればよく、例えば、繊維同士を熱接着する方法や、繊維同士を機械的に三次元交絡する方法等が挙げられる。 The spunbond nonwoven fabric of the present invention can be obtained by performing melt spinning at a high speed using a known spunbond apparatus. That is, when obtaining polylactic acid as a raw material and further composite fibers, other thermoplastic polymers are prepared, melt-spun through a spinneret, and yarn discharged from the spinneret is sprayed by a conventionally known lateral spray or annular blow. After cooling using a cooling device such as a paddle, it is pulled and thinned using a suction device. By melt spinning at high speed, polylactic acid can be crystallized with good molecular orientation, and the heat resistance is further improved. The pulling speed at the time of melt spinning is 4000 m / min or more, more preferably 5000 m / min or more. The spunbond nonwoven web formed by depositing a large number of fibers taken up by pulverization may be formed into a non-woven fabric by a known means, for example, a method of thermally bonding fibers or mechanically three-dimensionally connecting fibers. The method of entanglement etc. are mentioned.
本考案のスパンボンド不織布は、耐熱性および熱安定性が良好であるため、熱に対して細心の注意を要しないため、得られるスパンボンド不織布に熱を付与する後加工を施す際に安定して加工を行うことができる。また、耐熱性が良好であるため、様々な分野に展開することが可能となる。例えば、高温の媒体を濾過するフィルター、アイロン掛けを行う衣料用芯地、走行時にエンジン周りで温度の上昇する自動車や車輌に用いる部材、自動車内装材であるシートの部材，天井材，吸音材，パネル材等に好適に用いることができる。また、耐熱性および熱安定性に加え、高温下での耐久性が向上するため、在庫品の保管や輸送等においては倉庫内での雰囲気温度等の保管環境への細心の注意を要しなくなるため取り扱いが容易となり、また、品質保持期間を長く設定することが可能となるため経済的である。 Since the spunbonded nonwoven fabric of the present invention has good heat resistance and thermal stability, it does not require meticulous attention to heat. Therefore, the spunbonded nonwoven fabric is stable when post-processing to give heat to the resulting spunbonded nonwoven fabric. Can be processed. Moreover, since heat resistance is favorable, it can expand | deploy to various fields. For example, a filter for filtering a high-temperature medium, an ironing garment, a member used for an automobile or a vehicle whose temperature rises around the engine during traveling, a member of a sheet that is an automobile interior material, a ceiling material, a sound absorbing material, It can be suitably used for panel materials and the like. In addition to heat resistance and thermal stability, durability at high temperatures is improved, so it is not necessary to pay close attention to the storage environment such as the ambient temperature in the warehouse when storing and transporting inventory. Therefore, it is easy to handle, and it is economical because the quality retention period can be set long.
本考案のポリ乳酸系スパンボンドは、Ｄ−乳酸とＬ−乳酸との共重合体であって、該共重合体におけるＤ−乳酸の含有量が０．８モル％以下である重合体を主成分とする連続繊維によって構成されることから、耐熱性および熱安定性が良好となる。 The polylactic acid-based spunbond of the present invention is a copolymer of D-lactic acid and L-lactic acid, and a polymer having a D-lactic acid content of 0.8 mol% or less in the copolymer is mainly used. Since it is comprised by the continuous fiber used as a component, heat resistance and heat stability become favorable.
次に、実施例に基づき本発明を具体的に説明する。しかし、本発明はこれらの実施例のみに限定されるものではない。なお、以下の実施例、比較例における各種物性値は、下記の方法により測定した。
（１）メルトフローレート（ｇ／１０分）：ＡＳＴＭ−Ｄ−１２３８（Ｅ）に記載の方法に準じて、温度２１０℃、荷重２１６０ｇｆで測定した。以下、メルトフローレートを「ＭＦＲ」と記す。
Next, based on an Example, this invention is demonstrated concretely. However, the present invention is not limited only to these examples. In addition, the various physical-property values in a following example and a comparative example were measured with the following method.
(1) Melt flow rate (g / 10 min): Measured at a temperature of 210 ° C. and a load of 2160 gf according to the method described in ASTM-D-1238 (E). Hereinafter, the melt flow rate is referred to as “MFR”.
（２）融点Ｔｍ（℃）：示差走査型熱量計（パーキンエルマ社製、ＤＳＣ−２型）を用い、試料質量を５ｍｇとし、昇温速度を１０℃／分で測定し、得られた融解吸熱曲線の最大値の温度を融点Ｔｍ（℃）とした。 (2) Melting point Tm (° C.): Using a differential scanning calorimeter (manufactured by Perkin Elma, DSC-2), the sample mass was 5 mg, the temperature rising rate was measured at 10 ° C./min, and the obtained melting The maximum temperature of the endothermic curve was defined as the melting point Tm (° C.).
（３）繊度（デシテックス 以下、「ｄｔｅｘ」と記す）：不織布ウエブより５０本の繊維の繊維径を光学顕微鏡で測定し、密度補正して求めた平均値を繊度（ｄｔｅｘ）とした。 (3) Fineness (Decitex, hereinafter referred to as “dtex”): The fiber diameter of 50 fibers from the nonwoven fabric web was measured with an optical microscope, and the average value obtained by density correction was defined as fineness (dtex).
（４）目付（ｇ／ｍ２）：標準状態の試料から長さ１０ｃｍ、幅５ｃｍの試料片１０点を作成し、各試料片の質量（ｇ）を秤量し、得られた値の平均値を単位面積あたりに換算して、目付（ｇ／ｍ２）とした。 (4) Weight per unit area (g / m 2 ): Ten sample pieces having a length of 10 cm and a width of 5 cm were prepared from a sample in a standard state, the mass (g) of each sample piece was weighed, and the average value of the obtained values Was converted to a unit area (g / m 2 ).
（５）引張強力（Ｎ／５ｃｍ幅）及び破断伸度（％）：ＪＩＳ−Ｌ−１９０６に準じて測定した。すなわち、不織布の経方向（ＭＤ）および緯方向（ＣＤ）のそれぞれについて、長さ２０ｃｍ、幅５ｃｍの試料片各１０点を準備し、試料片を定速伸張型引張試験機（オリエンテック社製テンシロンＵＴＭ−４−１−１００）に取り付け、つかみ間隔１０ｃｍ、引張速度２０ｃｍ／分で伸張し、伸長−荷重曲線を描いた。得られた伸長−荷重曲線から求められる最大荷重値(Ｎ／５ｃｍ幅)の平均値を引張強力(Ｎ／５ｃｍ幅)とし、破断時の伸度の平均値を破断伸度（％）とした。 (5) Tensile strength (N / 5 cm width) and elongation at break (%): Measured according to JIS-L-1906. That is, for each of the warp direction (MD) and the weft direction (CD) of the nonwoven fabric, 10 sample pieces each having a length of 20 cm and a width of 5 cm were prepared, and the sample pieces were subjected to a constant speed extension type tensile tester (manufactured by Orientec). Tensilon UTM-4-1-100) and stretched at a gripping interval of 10 cm and a tensile speed of 20 cm / min to draw an elongation-load curve. The average value of the maximum load value (N / 5 cm width) obtained from the obtained elongation-load curve was defined as tensile strength (N / 5 cm width), and the average value of elongation at break was defined as elongation at break (%). .
（６）乾熱収縮率（％）：２０ｃｍ×２０ｃｍの試料片３枚を準備し、これを高温雰囲気下（温度１４０℃、１５０℃）へ投入して５分間放置して加熱した後、取り出して室温にて冷却し、下式より不織布のＭＤおよびＣＤの乾熱収縮率を算出した。
乾熱収縮率（％）＝[（Ａ０−Ａ１）／Ａ０]×１００
なお、式中のＡ０は加熱前のＭＤ方向あるいはＣＤ方向の寸法（ｍｍ）、Ａ１は加熱後のＭＤ方向あるいはＣＤ方向の寸法（ｍｍ）
(6) Dry heat shrinkage rate (%): Three sample pieces of 20 cm × 20 cm were prepared, put into a high temperature atmosphere (temperatures of 140 ° C. and 150 ° C.), left to heat for 5 minutes, and then taken out. The mixture was cooled at room temperature, and the dry heat shrinkage rate of MD and CD of the nonwoven fabric was calculated from the following formula.
Dry heat shrinkage (%) = [(A 0 −A 1 ) / A 0 ] × 100
Incidentally, A 0 is heated prior to the MD or CD direction dimension in the formula (mm), A 1 is the MD or CD direction dimension after heating (mm)
（７）熱安定性：前記乾熱収縮率の測定にて得られたＭＤ方向の乾熱収縮率の値により、不織布の熱安定性を下記により評価した。
○：乾熱収縮率が２％未満で熱安定性が良好
△：乾熱収縮率が２％以上３％未満
×：乾熱収縮率が３％以上
(7) Thermal stability: The thermal stability of the non-woven fabric was evaluated as follows based on the value of the dry heat shrinkage in the MD direction obtained by the measurement of the dry heat shrinkage.
○: Dry heat shrinkage rate is less than 2% and thermal stability is good Δ: Dry heat shrinkage rate is 2% or more and less than 3% ×: Dry heat shrinkage rate is 3% or more
（８）耐久性：試料を温度６０℃、湿度８０％の恒温恒湿槽内に投入し、４００時間放置した後に取り出し、恒温恒湿槽内への投入前後の強力の比率（強力保持率）を算出した。 (8) Durability: The sample was put into a constant temperature and humidity chamber at a temperature of 60 ° C. and a humidity of 80%, taken out after standing for 400 hours, and the strength ratio before and after being put into the constant temperature and humidity chamber (strong retention rate). Was calculated.
実施例１
融点１７８℃、ＭＦＲ３５．６ｇ／１０分のポリ乳酸（Ｄ−乳酸／Ｌ乳酸の共重合比が０．８／９９．２）を用意した。このポリ乳酸をスパンボンド法により溶融紡糸した。詳細には、溶融したポリ乳酸中にタルクが０．５質量％となるように、個別に計量した後、エクストルーダー型溶融押出機を用いて溶融し、紡糸温度２２０℃、単孔吐出量１．７ｇ／分の条件下で溶融紡糸を行った。吐出糸条は、冷却装置にて冷却した後、引き続き紡糸口金の下方に設けたエアーサッカーにて牽引速度５０００ｍ／分で牽引細化し、公知の開繊機を用いて開繊し、移動するスクリーンコンベア上にウェブとして捕集堆積させた。堆積した連続繊維の単糸繊度は３．２ｄｔｅｘであった。
Example 1
A polylactic acid (copolymerization ratio of D-lactic acid / L lactic acid of 0.8 / 99.2) having a melting point of 178 ° C. and an MFR of 35.6 g / 10 minutes was prepared. This polylactic acid was melt-spun by a spunbond method. Specifically, after individually weighing so that talc is 0.5% by mass in the melted polylactic acid, it is melted using an extruder-type melt extruder, and the spinning temperature is 220 ° C., the single-hole discharge rate is 1 Melt spinning was carried out under the condition of 7 g / min. The screen conveyor, which is cooled by a cooling device, is continuously refined at a towing speed of 5000 m / min by an air soccer provided below the spinneret, and is opened using a known opening machine and moved. It was collected and deposited as a web on top. The single yarn fineness of the deposited continuous fibers was 3.2 dtex.
次いで、ウェブをロール表面温度を１４５℃に設定したエンボス装置に通して部分的に熱圧着して、ポリ乳酸系スパンボンド不織布を得た。 Next, the web was partially thermocompression-bonded through an embossing apparatus in which the roll surface temperature was set to 145 ° C. to obtain a polylactic acid-based spunbonded nonwoven fabric.
実施例２
実施例１において、ポリ乳酸として、融点１７６℃、ＭＦＲ２１．７ｇ／１０分、Ｄ−乳酸／Ｌ乳酸の共重合比が０．６／９９．４）を用いたこと、溶融紡糸の際の紡糸温度を２１０℃としたこと、エンボス装置に通す際のロール表面温度を１４０℃としたこと以外は、実施例１と同様にしてポリ乳酸系スパンボンド不織布を得た。不織布を構成する連続繊維の単糸繊度は３．３ｄｔｅｘであった。
Example 2
In Example 1, a polylactic acid having a melting point of 176 ° C., an MFR of 21.7 g / 10 minutes, and a copolymerization ratio of D-lactic acid / L lactic acid of 0.6 / 99.4) was used for spinning during melt spinning. A polylactic acid-based spunbonded nonwoven fabric was obtained in the same manner as in Example 1 except that the temperature was 210 ° C and the roll surface temperature when passing through an embossing device was 140 ° C. The single yarn fineness of the continuous fibers constituting the nonwoven fabric was 3.3 dtex.
実施例３
実施例１において、ポリ乳酸として、融点１７８℃、ＭＦＲ２１．７ｇ／１０分、Ｄ−乳酸／Ｌ乳酸の共重合比が０．１／９９．９）を用いたこと以外は、実施例１と同様にしてポリ乳系スパンボンド不織布を得た。不織布を構成する連続繊維の単糸繊度は３．１ｄｔｅｘであった。また、得られたスパンボンド不織布について、カルボキシル末端基濃度を測定したところ、９モル／ｔｏｎであった。
Example 3
Example 1 is the same as Example 1 except that the melting point is 178 ° C., the MFR is 21.7 g / 10 min, and the copolymerization ratio of D-lactic acid / L lactic acid is 0.1 / 99.9). Similarly, a poly milk-based spunbond nonwoven fabric was obtained. The single yarn fineness of the continuous fibers constituting the nonwoven fabric was 3.1 dtex. Moreover, when the carboxyl end group density | concentration was measured about the obtained spun bond nonwoven fabric, it was 9 mol / ton.
比較例１
実施例１において、ポリ乳酸として、融点１６８℃、ＭＦＲ２０．３ｇ／１０分、Ｄ−乳酸／Ｌ乳酸の共重合比が１．４／９８．６）を用いたこと、溶融紡糸の際の紡糸温度を２１０℃としたこと、エンボス装置に通す際のロール表面温度を１４０℃としたこと以外は、実施例１と同様にしてポリ乳酸系スパンボンド不織布を得た。不織布を構成する連続繊維の単糸繊度は３．２ｄｔｅｘであった。
Comparative Example 1
In Example 1, polylactic acid having a melting point of 168 ° C., MFR of 20.3 g / 10 min, and a copolymerization ratio of D-lactic acid / L lactic acid of 1.4 / 98.6) was used for spinning during melt spinning. A polylactic acid-based spunbonded nonwoven fabric was obtained in the same manner as in Example 1 except that the temperature was 210 ° C and the roll surface temperature when passing through an embossing device was 140 ° C. The single yarn fineness of the continuous fibers constituting the nonwoven fabric was 3.2 dtex.
得られた実施例１〜３、比較例１の評価結果を表１に示した。 The evaluation results of Examples 1 to 3 and Comparative Example 1 obtained are shown in Table 1.
表１からも明らかなように、本考案のスパンボンド不織布は、高温雰囲気下（１４０℃〜１６０℃）での乾熱収縮率が小さく熱安定性に優れたものであった。耐久性については、実施例３のものと比較例１のもののみ評価したが、本考案のスパンボンド不織布である実施例３の強力保持率は９８％、比較例１の強力保持率は６０％であり、本考案のスパンボンド不織布は耐久性に優れていた。 As is clear from Table 1, the spunbonded nonwoven fabric of the present invention had a small dry heat shrinkage under a high temperature atmosphere (140 ° C. to 160 ° C.) and was excellent in thermal stability. For durability, only those of Example 3 and Comparative Example 1 were evaluated, but the strength retention of Example 3 which is the spunbonded nonwoven fabric of the present invention was 98%, and the strength retention of Comparative Example 1 was 60%. The spunbond nonwoven fabric of the present invention was excellent in durability.
１ ポリ乳酸
２ ポリ乳酸以外の他の熱可塑性重合体
1
Claims (3)
The continuous fiber is a composite fiber formed by combining a copolymer of D-lactic acid and L-lactic acid and a thermoplastic polymer other than polylactic acid. Polylactic acid-based spunbond nonwoven fabric.
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