JP2012001836A - Method for manufacturing of polyester nonwoven fabric with good light resistance - Google Patents
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本発明は、耐光性に優れたポリエステル不織布の製造方法に関し、特に細い繊維で構成される耐光性に優れたポリエステル不織布の製造方法に関する。 The present invention relates to a method for producing a polyester nonwoven fabric excellent in light resistance, and particularly relates to a method for producing a polyester nonwoven fabric excellent in light resistance composed of fine fibers.
近年、ポリエステル不織布の用途は発展の一途をたどり、衣料用資材、防護用衣料、家具・インテリア用資材、人工皮革、フィルター、車両用資材、工業用資材、土木・建築用資材、農業・園芸用資材、生活用資材、医療用資材、衛生材料で使用されているが、更なる高機能化への要求は高く、特に、インテリア用資材、土木・建築用資材、農業・園芸用資材、関連では、優れた耐光剤を有する製品が期待されている。 In recent years, the use of polyester nonwoven fabrics has continued to develop, such as clothing materials, protective clothing, furniture and interior materials, artificial leather, filters, vehicle materials, industrial materials, civil engineering and building materials, agriculture and horticulture It is used in materials, household materials, medical materials, and hygiene materials, but there is a high demand for higher functionality, especially in interior materials, civil engineering / architectural materials, agricultural / horticultural materials, etc. Products with excellent light-proofing agents are expected.
しかしながら、ポリエステル不織布の製造においては、複数のノズルを有する成形機で多量の細径繊維を継続的に製造することが必要で、耐光安定剤のブリードアウト等によるノズルへの糸切れによるトラブルを避けるため、耐光安定剤の添加量は制限を受ける。
また、耐光安定剤の分子量が５００以下であると、一般に、ポリエステル不織布の紡糸工程中の周囲への飛散、チルロール、エンボスロール表面への付着等が避けられず、添加量の全てが最終製品中で耐光剤改良剤として機能することはできない。この傾向は、不織布を構成する繊維径が細くなるほど、例えば１５μｍ以下、特に１０μｍ以下になると強まる。また、ポリエステル不織布の耐光性改良には、ポリエステルの重縮合工程中に生成し、そのままポリエステル原料中に残留するオリゴマーを除去することも重要である。
However, in the production of polyester nonwoven fabrics, it is necessary to continuously produce a large amount of small-diameter fibers with a molding machine having a plurality of nozzles, avoiding troubles due to yarn breakage to the nozzles due to light-resistant stabilizer bleed-out, etc. Therefore, the amount of light-resistant stabilizer added is limited.
In addition, when the light stabilizer has a molecular weight of 500 or less, generally, scattering of the polyester nonwoven fabric to the surroundings during the spinning process, adhesion to the surface of the chill roll, embossing roll, etc. cannot be avoided, and all of the added amount is in the final product. It cannot function as a light resistance improver. This tendency becomes stronger as the fiber diameter constituting the nonwoven fabric becomes thinner, for example, 15 μm or less, particularly 10 μm or less. Further, for improving the light resistance of the polyester nonwoven fabric, it is also important to remove oligomers that are generated during the polyester polycondensation process and remain in the polyester raw material as they are.
ポリエステル系高分子材料の優れた耐光安定剤としては、ベンゾトリアゾール系耐光安定剤（紫外線吸収剤）、トリアジン系耐光安定剤（紫外線吸収剤）、ヒンダードアミン系耐光安定剤（紫外線吸収剤）などが知られているが、これらは、ポリエステル不織布に添加する場合に上記した問題を有している。 Known light stabilizers for polyester polymer materials include benzotriazole light stabilizers (ultraviolet absorbers), triazine light stabilizers (ultraviolet absorbers), and hindered amine light stabilizers (ultraviolet absorbers). However, these have the above-mentioned problems when added to a polyester nonwoven fabric.
特許文献１には、超臨界二酸化炭素を利用して各種機能剤をプラスチック成形体に添加して機能化する方法が開示されているが、耐光安定剤の注入、ポリエステル不織布が抱える上記課題に対する解決法は提案されていない。
特許文献２において、ポリプロピレン繊維に対する耐光安定剤注入に関する記載はあるが、ポリエステル不織布に対する具体的開示はない。
Patent Document 1 discloses a method of adding various functional agents to a plastic molded body using supercritical carbon dioxide to functionalize the solution. No law has been proposed.
In Patent Document 2, there is a description regarding injection of a light-resistant stabilizer for polypropylene fibers, but there is no specific disclosure for polyester nonwoven fabrics.
本発明の目的は、ポリエステル不織布、特に、細径のポリエステル繊維を構成材料とするポリエステル不織布にとって困難であった耐光安定剤の多量注入を可能とし、耐光性に優れたポリエステル不織布を製造することにある。 An object of the present invention is to produce a polyester nonwoven fabric excellent in light resistance, which enables a large amount of light-resistant stabilizer, which has been difficult for polyester nonwoven fabrics, particularly polyester nonwoven fabrics composed of small-diameter polyester fibers. is there.
本発明者らは鋭意検討を行なったところ、超臨界二酸化炭素を利用することにより、ポリエステル不織布、特に、細径のポリエステル繊維を構成材料とするポリエステル不織布にとって困難であった耐光安定剤の注入が可能となり、また、耐光性に好ましくないオリゴマー成分の抽出が行なわれることを見出し、本発明を完成させるに至った。 As a result of intensive studies, the present inventors have made it possible to inject a light-resistant stabilizer, which has been difficult for polyester nonwoven fabrics, particularly polyester nonwoven fabrics composed of small-diameter polyester fibers, by using supercritical carbon dioxide. It has become possible, and the inventors have found that the extraction of oligomer components that are not preferred for light resistance is performed, and have completed the present invention.
すなわち、本発明は、［１］超臨界二酸化炭素中において、ポリエステル不織布に耐光安定剤を含浸させる工程を含むことを特徴とする耐光性ポリエステル不織布の製造方法である。 That is, the present invention is [1] a method for producing a light-resistant polyester nonwoven fabric, comprising a step of impregnating a polyester nonwoven fabric with a light-resistant stabilizer in supercritical carbon dioxide.
また、本発明は、［２］耐光安定剤が、ベンゾトリアゾール系耐光安定剤、トリアジン系耐光安定剤およびヒンダードアミン系耐光安定剤から選択されるいずれかであることを特徴とする前記［１］に記載の耐光性ポリエステル不織布の製造方法である。 In addition, the present invention provides [2] wherein the light resistance stabilizer is any one selected from benzotriazole light resistance stabilizers, triazine light resistance stabilizers and hindered amine light resistance stabilizers. It is a manufacturing method of the light-resistant polyester nonwoven fabric of description.
また、本発明は、［３］２重量％以上の耐光安定剤を含浸させることを特徴とする前記［１］または［２］に記載の耐光性ポリエステル不織布の製造方法である。 [3] The method for producing a light-resistant polyester nonwoven fabric according to [1] or [2], wherein [3] a light-resistant stabilizer of 2% by weight or more is impregnated.
また、本発明は、［４］耐光安定剤を含浸させる工程が、密閉容器内において行なわれることを特徴とする前記［１］ないし［３］のいずれかに記載の耐光性ポリエステル不織布の製造方法である。 Further, according to the present invention, [4] the method for producing a light-resistant polyester nonwoven fabric according to any one of [1] to [3], wherein the step of impregnating the light-resistant stabilizer is performed in a sealed container. It is.
本発明の方法により、ポリエステル不織布、特に、細径のポリエステル繊維を構成材料とするポリエステル不織布にとって困難であった耐光安定剤の多量注入を可能とし、耐光性に優れたポリエステル不織布を製造することができる。 According to the method of the present invention, it is possible to produce a polyester nonwoven fabric excellent in light resistance by enabling large-scale injection of a light-resistant stabilizer, which was difficult for polyester nonwoven fabrics, particularly polyester nonwoven fabrics composed of small-diameter polyester fibers. it can.
本発明は、超臨界二酸化炭素中において、ポリエステル不織布に耐光安定剤を含浸させる工程を含むことを特徴とする耐光性に優れたポエステル不織布の製造方法である。 The present invention is a method for producing a polyester nonwoven fabric excellent in light resistance, comprising a step of impregnating a polyester nonwoven fabric with a light-resistant stabilizer in supercritical carbon dioxide.
超臨界二酸化炭素とは、７．３８ＭＰａ以上、かつ３１℃以上の状態にある二酸化炭素を指す。
二酸化炭素は、超臨界状態になると、耐光安定剤の溶解力および不織布中のポリエステル繊維の膨潤力が向上する。超臨界二酸化炭素中に、ポリエステル不織布と耐光安定剤と接触させることで、超臨界流体に溶解した耐光安定剤を、膨潤したポリエステル繊維に、繊維表面から均一に含浸することができる。すなわち、最も露光条件が厳しい繊維表層に効率的に耐光安定剤が効率的に配置できる。
また、膨潤したポリエステル繊維中のオリゴマーが超臨界二酸化炭素に溶解し、ポリエステル繊維中からオリゴマーを抽出除去できる。
その際、密閉容器内にポリエステル不織布と耐光安定剤を含浸させて温度および圧力を調整すると、溶解度の膨潤度を容易かつ安定化するので好ましい。
耐光安定剤をポリエステル不織布に含浸させるには、不織布表面に耐光安定剤を付着させるか、超臨界二酸化炭素で充填された密閉容器内に不織布表面に耐光安定剤の両者を共存させることが好ましい。
Supercritical carbon dioxide refers to carbon dioxide in a state of 7.38 MPa or more and 31 ° C. or more.
When carbon dioxide enters a supercritical state, the dissolving power of the light stabilizer and the swelling power of the polyester fibers in the nonwoven fabric are improved. By contacting the polyester nonwoven fabric and the light-resistant stabilizer in supercritical carbon dioxide, the light-resistant stabilizer dissolved in the supercritical fluid can be uniformly impregnated into the swollen polyester fiber from the fiber surface. That is, the light-resistant stabilizer can be efficiently arranged on the fiber surface layer having the strictest exposure conditions.
Further, the oligomer in the swollen polyester fiber is dissolved in supercritical carbon dioxide, and the oligomer can be extracted and removed from the polyester fiber.
At that time, it is preferable to impregnate the polyester nonwoven fabric and the light-resistant stabilizer in the closed container to adjust the temperature and pressure because the swelling degree of solubility is easily and stabilized.
In order to impregnate the polyester nonwoven fabric with the light-resistant stabilizer, it is preferable to attach the light-resistant stabilizer to the surface of the nonwoven fabric, or to allow both of the light-resistant stabilizer to coexist on the surface of the nonwoven fabric in a closed container filled with supercritical carbon dioxide.
超臨界二酸化炭素中でポリエステル不織布に耐光安定剤を含浸させる工程における温度および圧力は、二酸化炭素が超臨界状態にある条件、かつ不織布を構成するポリエステルの融点以下であれば特に制限はないが、圧力は１０〜３０ＭＰａ、温度は５０℃〜ポリエステルの融点の５０℃以下が好ましい。圧力が１０ＭＰａ未満では、超臨界二酸化炭素の密度が小さくポリエステルへの浸透が十分でなく、３０ＭＰａ超では、設備が大型化して経済的ではない。温度がポリエステルの融点まで５０℃ない場合は、不織布の変形が生じる可能性がある。具体的には、ポリエステルがポリエチレンテレフタレートの場合は５０℃〜１８０℃、ポリブチレンテレフタレートの場合は５０℃〜１６０℃が好ましい。経済的観点から、温度と圧力を調整して、含浸時間を５時間以下とすることが好ましい。 The temperature and pressure in the step of impregnating the polyester nonwoven fabric with the light-resistant stabilizer in supercritical carbon dioxide are not particularly limited as long as the carbon dioxide is in a supercritical state and below the melting point of the polyester constituting the nonwoven fabric. The pressure is preferably 10 to 30 MPa, and the temperature is preferably 50 ° C. to 50 ° C. of the melting point of the polyester. If the pressure is less than 10 MPa, the density of supercritical carbon dioxide is small and the penetration into the polyester is not sufficient, and if it exceeds 30 MPa, the equipment becomes large and not economical. If the temperature is not 50 ° C. up to the melting point of the polyester, the nonwoven fabric may be deformed. Specifically, when the polyester is polyethylene terephthalate, the temperature is preferably 50 ° C to 180 ° C, and when the polyester is polybutylene terephthalate, the temperature is preferably 50 ° C to 160 ° C. From an economic point of view, it is preferable to adjust the temperature and pressure so that the impregnation time is 5 hours or less.
本発明に用いることができる耐光安定剤（耐光剤、光安定剤とも称する。）については特に制限はないが、ポリエステルとの親和性の高さから、ベンゾトリアゾール系耐光安定剤、トリアジン系耐光安定剤およびヒンダードアミン系耐光安定剤が好ましい。これら耐光安定剤は、市場から、ベンゾトリアゾール系耐光安定剤としては、「ＴＩＮＵＶＩＮ Ｐ」、「ＴＩＮＵＶＩＮ ２３４」、「ＴＩＮＵＶＩＮ ３２６」、「ＴＩＮＵＶＩＮ ３２８」、「ＴＩＮＵＶＩＮ ３２９」、トリアジン系耐光安定剤としては、「ＴＩＮＵＶＩＮ １５７７ＦＦ」、ヒンダードアミン系耐光安定剤としては、「ＴＩＮＵＶＩＮ １４４」、「ＴＩＮＵＶＩＮ ７６５」、「ＴＩＮＵＶＩＮ ７７０ＤＦ」（以上ＢＡＳＦ（株）製）が入手できる。 Although there is no restriction | limiting in particular about the light-resistant stabilizer (it is also called a light-resistant agent and a light stabilizer) which can be used for this invention, From the high affinity with polyester, a benzotriazole type light-resistant stabilizer and a triazine type light-resistant stability Agents and hindered amine light resistance stabilizers are preferred. These light stabilizers are commercially available from the market as “TINUVIN P”, “TINUVIN 234”, “TINUVIN 326”, “TINUVIN 328”, “TINUVIN 329”, and as triazine light stabilizers. “TINUVIN 1577FF” and “TINUVIN 144”, “TINUVIN 765”, and “TINUVIN 770DF” (manufactured by BASF Corp.) are available as hindered amine light resistance stabilizers.
耐光安定剤を不織布に含浸させるには、不織布表面に耐光安定剤を付着させるか、超臨界二酸化炭素で充填された密閉容器内に不織布表面に耐光安定剤の両者を共存させることが好ましい。耐光安定剤は、通常０．５重量％以上添加することで改良効果が得られるが、本発明の方法によれば、ポリエステル不織布に耐光安定剤を多量に含浸させることが可能となる。通常、ポリエステル不織布製造装置において、耐光安定剤を１重量％以上添加することはトラブルを生ずる要因となるが、本発明の製造方法によれば、２重量％以上を含浸することが可能であり、極めて耐光性に優れたポリエステル不織布を得ることができる。また、耐光安定剤の不織布への含浸量は、必要とする耐光特性に応じて適宜増減可能である。 In order to impregnate the nonwoven fabric with the light-resistant stabilizer, it is preferable to attach the light-resistant stabilizer to the surface of the nonwoven fabric, or to allow both of the light-resistant stabilizer to coexist on the surface of the nonwoven fabric in a closed container filled with supercritical carbon dioxide. An improvement effect is usually obtained by adding 0.5% by weight or more of the light-resistant stabilizer. However, according to the method of the present invention, the polyester nonwoven fabric can be impregnated with a large amount of the light-resistant stabilizer. Usually, in a polyester nonwoven fabric manufacturing apparatus, adding 1% by weight or more of a light-resistant stabilizer causes trouble, but according to the manufacturing method of the present invention, it is possible to impregnate 2% by weight or more, A polyester nonwoven fabric with extremely excellent light resistance can be obtained. Moreover, the amount of impregnation of the light-resistant stabilizer into the nonwoven fabric can be appropriately increased or decreased according to the required light-resistant characteristics.
本発明にかかるポリエステル不織布の構成材料であるポリエステルは、ジカルボン酸化合物とジヒドロキシ化合物の重縮合、オキシカルボン酸化合物の重縮合、又はこれらの誘導体の混合物の重縮合などによって得られる熱可塑性ポリエステルである。
なかでも好ましいのは、細径繊維の成形性の観点から、酸性分の９５モル％以上がテレフタル酸であり、アルコール成分の９５モル％以上が脂肪族ジオールであるポリアルキレンテレフタレートである。その代表的なものはポリブチレンテレフタレート及びポリエチレンテレフタレートである。
なお、ポリブチレンテレフタレート及びポリエチレンテレフタレートは、重縮合工程中で生成するオリゴマーが残留物となることが避けられないので、良好な耐光性を得るためには、これらのオリゴマーを抽出除去することが好ましい。
The polyester which is a constituent material of the polyester nonwoven fabric according to the present invention is a thermoplastic polyester obtained by polycondensation of a dicarboxylic acid compound and a dihydroxy compound, polycondensation of an oxycarboxylic acid compound, or polycondensation of a mixture of these derivatives. .
Of these, polyalkylene terephthalate, in which 95 mol% or more of the acidic component is terephthalic acid and 95 mol% or more of the alcohol component is an aliphatic diol, is preferable from the viewpoint of moldability of the fine fiber. Typical examples are polybutylene terephthalate and polyethylene terephthalate.
In addition, since polybutylene terephthalate and polyethylene terephthalate are unavoidable that the oligomer produced in the polycondensation step becomes a residue, it is preferable to extract and remove these oligomers in order to obtain good light resistance. .
本発明において用いられるポリエステル不織布について、その不織布の形成法については特に制限はない。例えば、フリース形成法（「乾式法」、「湿式法」、「スパンボンド法」、「メルトブロー法」）、フリース結合法（「サーマルボンド法」、「ケミカルボンド法」、「ニードルパンチ法」、「スパンレース法（水流絡合法）」、「ステッチボンド法」、「スチームジェット法」）などのいずれの方法であってもよい。 There is no restriction | limiting in particular about the formation method of the nonwoven fabric about the polyester nonwoven fabric used in this invention. For example, fleece formation method (“dry method”, “wet method”, “spun bond method”, “melt blow method”), fleece bonding method (“thermal bond method”, “chemical bond method”, “needle punch method”, Any method such as “spun lace method (water entanglement method)”, “stitch bond method”, and “steam jet method” may be used.
本発明にかかる不織布の目付け、構成する繊維径には特に制限はない。ただし、耐光安定剤の注入およびオリゴマー抽出とも、超臨界二酸化炭素の繊維表面への吸着を起点として注入、抽出へ進行するので、比表面積が大きい細径繊維で構成される不織布、また、同じ径の繊維で構成される不織布であれば、繊維分布が疎である低目付け不織布が好ましい。繊維径は１０μ以下、目付けは１０μ繊維径であれば、４０ｇ／ｍ２以下、好ましくは、３０ｇ／ｍ２以下とすることで、大きな効果を得ることができる。 There is no restriction | limiting in particular in the fabric weight of the nonwoven fabric concerning this invention, and the fiber diameter to comprise. However, since both light-resistant stabilizer injection and oligomer extraction proceed to injection and extraction starting from the adsorption of supercritical carbon dioxide on the fiber surface, nonwoven fabric composed of fine fibers with a large specific surface area, and the same diameter If it is a nonwoven fabric comprised by the fiber of this, the low-weight nonwoven fabric with a sparse fiber distribution is preferable. When the fiber diameter is 10 μm or less and the basis weight is 10 μfiber diameter, a great effect can be obtained by setting the fiber diameter to 40 g / m 2 or less, preferably 30 g / m 2 or less.
以下に実施例を挙げて本発明を具体的に説明するが、本発明はこれら実施例によって何ら制限されるものではない。 EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
（縦延伸不織布の製造）
メルトブロー紡糸装置により、極限粘度ＩＶ値が０．６２のポリエステル樹脂（ポリエチレンテレフタレート（ＰＥＴ）。以下同じ。）からなる縦方向に配列したフィラメントウェブを集積し、これを縦方向に延伸して、平均繊維径が約１０μｍ、目付が１５ｇ／ｍ２のもの（縦延伸不織布ａ）を得た。
(Manufacture of longitudinally stretched nonwoven fabric)
Using a melt blow spinning device, filament webs made of polyester resin (polyethylene terephthalate (PET), the same shall apply hereinafter) having an intrinsic viscosity IV value of 0.62 were accumulated and stretched in the longitudinal direction to obtain an average. A fiber having a fiber diameter of about 10 μm and a basis weight of 15 g / m 2 (longitudinal stretch nonwoven fabric a) was obtained.
メルトブロー紡糸装置により、極限粘度ＩＶ値が０．６２のポリエステル樹脂からなる縦方向に配列したフィラメントウェブを集積し、これを縦方向に延伸して、平均繊維径が約１０μｍ、目付が２０ｇ／ｍ２のもの（縦延伸不織布ｂ）を得た。 By means of a melt blow spinning device, filament webs made of polyester resin having an intrinsic viscosity IV value of 0.62 are stacked in the longitudinal direction and stretched in the longitudinal direction to have an average fiber diameter of about 10 μm and a basis weight of 20 g / m. 2 (longitudinal stretch nonwoven fabric b) was obtained.
メルトブロー紡糸装置により、トリアジン系耐光安定剤（紫外線吸収剤）「ＴＩＮＵＶＩＮ１５７７ＦＦ（分子量４２６）」（ＢＡＳＦ社製）を１ｗｔ％混合した極限粘度ＩＶ値が０．６２のポリエステル樹脂からなる縦方向に配列したフィラメントウェブを集積し、これを縦方向に延伸して、平均繊維径が約１０μｍ、目付が１５ｇ／ｍ２のもの（縦延伸不織布ｃ）を得た。なお、１ｗｔ％を超える耐光安定剤の添加では、フィラメント切れが発生した。 Using a melt blow spinning apparatus, the triazine-based light-resistant stabilizer (ultraviolet absorber) “TINUVIN 1577FF (molecular weight 426)” (manufactured by BASF) was mixed in the longitudinal direction composed of a polyester resin having an intrinsic viscosity IV value of 0.62 mixed with 1 wt%. Filament webs were accumulated and stretched in the machine direction to obtain an average fiber diameter of about 10 μm and a basis weight of 15 g / m 2 (longitudinal stretch nonwoven fabric c). When the light stabilizer exceeding 1 wt% was added, filament breakage occurred.
（横延伸不織布の製造）
スプレイ紡糸装置により、極限粘度ＩＶ値が０．５５のポリエステル樹脂を使用して横方向に配列したフィラメントウェブを集積し、これを横方向に延伸して、平均繊維径が約１０μｍ、目付が１５ｇ／ｍ２のもの（横延伸不織布ａ）を得た。
(Manufacture of transversely stretched nonwoven fabric)
Using a spray spinning device, filament webs arranged in the transverse direction using polyester resin having an intrinsic viscosity IV value of 0.55 are collected and stretched in the transverse direction to obtain an average fiber diameter of about 10 μm and a basis weight of 15 g. / M 2 (transversely stretched nonwoven fabric a) was obtained.
スプレイ紡糸装置により、極限粘度ＩＶ値が０．５５のポリエステル樹脂を使用して横方向に配列したフィラメントウェブを集積し、これを横方向に延伸して、平均繊維径が約１０μｍ、目付が２０ｇ／ｍ２のもの（横延伸不織布ｂ）を得た。 Using a spray spinning device, filament webs arranged in the transverse direction using polyester resin having an intrinsic viscosity IV value of 0.55 are collected and stretched in the transverse direction to have an average fiber diameter of about 10 μm and a basis weight of 20 g. / M 2 (transversely stretched nonwoven fabric b) was obtained.
スプレイ紡糸装置により、トリアジン系耐光安定剤（紫外線吸収剤）「ＴＩＮＵＶＩＮ１５７７ＦＦ（分子量４２６）」（ＢＡＳＦ社製）を１ｗｔ％混合した極限粘度ＩＶ値が０．５５のポリエステル樹脂を使用して横方向に配列したフィラメントウェブを集積し、これを横方向に延伸して、平均繊維径が約１０μｍ、目付が１５ｇ／ｍ２のもの（横延伸不織布ｃ）を得た。なお、１ｗｔ％を超えた耐光安定剤の添加では、フィラメント切れが発生した。 Using a spray spinning device, a polyester resin having an intrinsic viscosity IV value of 0.55 mixed with 1 wt% of a triazine light resistance stabilizer (ultraviolet absorber) “TINUVIN 1577FF (molecular weight 426)” (manufactured by BASF) was used in the transverse direction. The arranged filament webs were accumulated and stretched in the transverse direction to obtain an average fiber diameter of about 10 μm and a basis weight of 15 g / m 2 (laterally stretched nonwoven fabric c). When the light stabilizer exceeding 1 wt% was added, filament breakage occurred.
（ポリエステル不織布の製造）
縦延伸不織布と横延伸不織布とを２００℃の加熱エンボスロールにより積層し、経緯直交不織布を得た。組み合わせは、以下のとおりである。なお、不織布Ｃの製造時には、エンボスロールに耐光安定剤の付着が観察された。
不織布Ａ：縦延伸不織布ａと横延伸不織布ａを積層
不織布Ｂ：縦延伸不織布ｂと横延伸不織布ｂを積層
不織布Ｃ：縦延伸不織布ｃと横延伸不織布ｃを積層
(Manufacture of polyester nonwoven fabric)
The longitudinally stretched nonwoven fabric and the laterally stretched nonwoven fabric were laminated by a heated embossing roll at 200 ° C. to obtain a process orthogonal fabric. The combinations are as follows. In addition, at the time of manufacture of the nonwoven fabric C, the adhesion of the light-resistant stabilizer to the embossing roll was observed.
Nonwoven fabric A: Laminated longitudinally stretched nonwoven fabric a and laterally stretched nonwoven fabric a Nonwoven fabric B: Laminated longitudinally stretched nonwoven fabric b and laterally stretched nonwoven fabric b Nonwoven fabric C: Laminated longitudinally stretched nonwoven fabric c and laterally stretched nonwoven fabric c
製造装置（図１）は、二酸化炭素ボンベ１０と、ポンプ１１と、容器１２と、恒温槽１３と、バルブ１４、１５とを含んで構成される。容器１２中には、ポリエステル不織布および耐光安定剤を収容する。恒温槽１３は、容器１２内の温度が所定の温度となるように加温する。その後、流体が充填されたボンベ１０からポンプ１１により所定の圧力に加圧した流体を容器１２に供給する。この流体は、バルブ１４を介して供給され、バルブ１５を介して排出される。また、容器１２は、圧力調整弁およびバルブ１４，１５などによって、内部の圧力が所定の圧力となるように調整される。容器１２内の温度および圧力は、温度計および圧力計などによって測定される。
The manufacturing apparatus (FIG. 1) includes a
（不織布Ａへの耐光安定剤注入−１）
１．不織布Ａから、１８ｃｍ×１５０ｃｍを切り出し、穴あきチューブに巻きつけ、容器１２内に設置した。
２．ガラス濾紙に１０ｗｔ％耐光安定剤「ＴＩＮＵＶＩＮ１５７７ＦＦ（分子量４２６）」（ＢＡＳＦ社製）クロロホルム溶液を滴下、溶液を蒸発させて製造した耐光安定剤坦持体を容器１２内に設置した。
３．恒温槽１３を運転して容器１２を１２０℃とし、バブル１４を開、バブル１５を閉としてポンプ１１を運転してボンベ１０から二酸化炭素を送り込み、容器圧力を上昇させ、容器１２内を、１２０℃、２５ＭＰａとし、バルブ１４を閉とした。
４．１時間処理後、バブル１５を開として、容器１２を大気圧とし、不織布Ａを取り出した。
５．容器１２の内壁に、ポリエステル中から抽出されたオリゴマーが付着していることを確認した。
(Light-resistant stabilizer injection to nonwoven fabric A-1)
1. 18 cm × 150 cm was cut out from the nonwoven fabric A, wound around a perforated tube, and placed in the
2. A 10 wt% light-resistant stabilizer “TINUVIN 1577FF (molecular weight 426)” (manufactured by BASF) was dropped onto a glass filter paper, and the light-resistant stabilizer carrier produced by evaporating the solution was placed in the
3. The
After the treatment for 4.1 hours, the
5). It was confirmed that the oligomer extracted from the polyester adhered to the inner wall of the
（不織布Ａへの耐光安定剤注入−２）
６．別個の不織布Ａにつき、上記４．の処理時間を３時間に変えて、耐光安定剤の注入を行なった。なお、この処理においても、オリゴマーの抽出を確認した。
(Light-resistant stabilizer injection to nonwoven fabric A-2)
6). For the separate nonwoven fabric A, the above 4. The light-resistant stabilizer was injected by changing the treatment time of 3 to 3 hours. In this process, oligomer extraction was also confirmed.
（不織布Ｂへの耐光安定剤注入）
１．不織布Ｂについても、処理時間を２時間処理した以外は、不織布Ａと同様の処理を行なった。また、オリゴマーの抽出を確認した。
(Light-resistant stabilizer injection into nonwoven fabric B)
1. The nonwoven fabric B was also treated in the same manner as the nonwoven fabric A except that the treatment time was treated for 2 hours. Moreover, the extraction of the oligomer was confirmed.
（耐光安定剤注入量の測定）
１．ＴＩＮＵＶＩＮ１５７７ＦＦ（分子量４２６）」（ＢＡＳＦ社製）／クロロホルム溶液の濃度検量線を島津製作所（株）製ＵＶ−ｖｉｓ分光光度計ＵＶ−１７００を使用して作成した。
２．注入処理後の不織布Ａ、不織布Ｂから縦横５ｃｍ×５ｃｍの試験片を切り出し、秤量後、ソックスレー抽出器に入れ、クロロホルムを溶媒で２時間抽出した。抽出液をクロロホルム希釈し、１．で作成した検量線から不織布Ａ、不織布Ｂ中の耐光安定剤濃度を求め、注入量とした。
(Measurement of light stabilizer injection amount)
1. A concentration calibration curve of TINUVIN 1577FF (molecular weight 426) (manufactured by BASF) / chloroform solution was prepared using a UV-vis spectrophotometer UV-1700 manufactured by Shimadzu Corporation.
2. Test pieces of 5 cm × 5 cm in length and width were cut out from the non-woven fabric A and non-woven fabric B after the injection treatment, weighed, put into a Soxhlet extractor, and chloroform was extracted with a solvent for 2 hours. The extract is diluted with chloroform, The light-resistant stabilizer concentration in the non-woven fabric A and non-woven fabric B was obtained from the calibration curve prepared in step 1 and used as the injection amount.
（耐光試験）
１．所定条件で製造した不織布から縦横３５ｃｍ×１８ｃｍの試験片を切り出し、スガ試験機（株）製紫外線フェードメーターＵ４８−ＨＢでカーボンアーク灯照射時間、６３℃、９６ｈｒの耐光試験を行った。
２．試験前後の不織布から縦横５ｃｍ×５ｃｍの試験片を１０枚切り出し、島津製作所（株）製引張試験機ＡＪＳ−Ｊを用いてつかみ具間３ｃｍで引張試験を行った。
(Light resistance test)
1. A test piece of 35 cm × 18 cm in length and width was cut out from the nonwoven fabric produced under the predetermined conditions, and a light resistance test was conducted at a carbon arc lamp irradiation time of 63 ° C. and 96 hours using an ultraviolet fade meter U48-HB manufactured by Suga Test Instruments Co., Ltd.
2. Ten test pieces of 5 cm × 5 cm in length and width were cut out from the nonwoven fabric before and after the test, and a tensile test was performed at 3 cm between the grips using a tensile tester AJS-J manufactured by Shimadzu Corporation.
上記結果から、超臨界二酸化炭素中で耐光安定剤を注入することにより（実施例１、２）、未注入品（比較例１、２）に較べて引張破壊強さの保持率が大幅に向上することが確認できた。また、予め耐光安定剤を練り込んで形成した不織布Ｃ（参考例１）においては、耐光安定剤の注入量の限界、オリゴマーの抽出が行なわれないことから、引張破壊強さの保持率は、実施例１に比べて小さなものとなっている。 From the above results, by injecting a light-resistant stabilizer in supercritical carbon dioxide (Examples 1 and 2), the retention of tensile fracture strength is significantly improved compared to uninjected products (Comparative Examples 1 and 2). I was able to confirm. In addition, in the nonwoven fabric C (Reference Example 1) formed by kneading the light-resistant stabilizer in advance, the limit of the light-resistant stabilizer injection amount and the extraction of the oligomer are not performed. Compared to the first embodiment, it is smaller.
本発明の方法で得られるポリエステル不織布は優れた耐光性を有し、衣料用資材、防護用衣料、家具・インテリア用資材、人工皮革、フィルター、車両用資材、工業用資材、土木・建築用資材、農業・園芸用資材、生活用資材、医療用資材、衛生材料、特に、インテリア用資材、土木・建築用資材、農業・園芸用資材、関連での用途が期待できる。 The polyester nonwoven fabric obtained by the method of the present invention has excellent light resistance, and is used for clothing materials, protective clothing, furniture / interior materials, artificial leather, filters, vehicle materials, industrial materials, civil engineering / building materials. It can be expected to be used in agriculture, horticultural materials, daily life materials, medical materials, sanitary materials, especially interior materials, civil engineering / architectural materials, agricultural / horticultural materials.
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| JP2001295178A (en) * | 2000-04-11 | 2001-10-26 | Toray Ind Inc | Treating agent for fiber, fiber construction treated with the same and method for producing the same |
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