JP5496194B2 - アミロース含有繊維、その製造法およびその利用 - Google Patents
アミロース含有繊維、その製造法およびその利用 Download PDFInfo
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- JP5496194B2 JP5496194B2 JP2011519577A JP2011519577A JP5496194B2 JP 5496194 B2 JP5496194 B2 JP 5496194B2 JP 2011519577 A JP2011519577 A JP 2011519577A JP 2011519577 A JP2011519577 A JP 2011519577A JP 5496194 B2 JP5496194 B2 JP 5496194B2
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- Prior art keywords
- amylose
- rayon fiber
- containing rayon
- rayon
- substance
- Prior art date
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
(項目1) アミロース含有レーヨン繊維の製造方法であって、
アミロースのアルカリ水溶液とビスコースとを混合して混合液を得る工程;および
該混合液を紡糸してアミロース含有レーヨン繊維を得る工程
を包含し、
該アミロースは、重量平均分子量が約3×104以上約2×105以下の酵素合成アミロースである、方法。
該化学物質を含有する溶液または気体と、項目9または10に記載のアミロース含有レーヨン繊維とを接触させることにより、該化学物質を前記アミロースに包接させる工程
を包含し、該化学物質はアミロースにより包接可能な物質であり、該化学物質はヨウ素およびポリヨウ化物イオン以外の物質である、方法。
(1.1)アミロース
「アミロース」とは、本明細書中で用いられる場合、D−グルコースを構成単位とする糖であって、主にα−1,4−グルコシド結合によって連結された糖単位を少なくとも2糖単位以上有する実質的に直鎖状の多糖をいう。本発明で使用されるアミロース分子においては、好ましくは、α−1,4−グルコシド結合によってのみ糖単位の間が連結されている。「直鎖状」とは、分岐がないことをいう。分岐は、例えば1つのグルコース残基の1位、4位および6位の3箇所にグルコース残基が連結した構造により形成される。「実質的に直鎖状」とは、完全に直鎖状のものと少数の分岐を含む直鎖状のものとを包含する。分岐の数は、グルコース残基10000個あたり約100個以下が好ましく、約50個以下がより好ましく、約10個以下がより好ましく、約1個以下が特に好ましく、0個であることが最も好ましい。アミロースは、直鎖状α−グルカンおよびα−1,4−グルカンと同義語である。直鎖状アミロースのうち、分岐が全くないアミロースを完全直鎖状アミロースという。
(1)α−グルカンホスホリラーゼ(Glucan phosphorylase:GP)(例えば、馬鈴薯由来)により、α−グルコース−1−リン酸(alpha−glucose−1−phosphate)のグルコシル基をプライマーであるマルトヘプタオースなどに転移することによりα−1,4−グルカン鎖を合成する方法;
(2)プライマー、スクロースおよび無機リン酸またはグルコース−1−リン酸を基質として、スクロースホスホリラーゼおよびグルカンホスホリラーゼを同時に作用させてα−1,4−グルカン鎖を合成する方法(以下、SP−GP法という)(Waldmann,H.ら,Carbohydrate Research,157(1986)c4−c7;WO2002/097107)。この方法は、他の方法よりも安価に直鎖状グルカンを合成し得るという利点を有する;
(3)プライマーおよびスクロースを基質として使用して、アミロスクラーゼを作用させることによりα−1,4−グルカン鎖を合成する方法。
レーヨン繊維原料としては、当該分野で公知の任意のビスコースが使用され得る。ビスコースは、当該分野で公知の方法によって製造され得る。例えば、亜硫酸パルプを17〜18%の苛性ソーダ液に浸漬する。パルプはアルカリ繊維素となって容積が4〜5倍に膨張する。これを圧搾して過剰のアルカリを搾り取り、粉砕機に入れて粉砕してかき混ぜる。これを老成させ、二硫化炭素と反応させてザンテートを形成する。ザンテートに希薄苛性ソーダ溶液を加え、液体状にしたものをビスコースという。
本願発明ではアミロースに包接される物質(ゲスト物質ともいう)は、アミロースに包接され得る物質であれば、任意の物質であり得る。ゲスト物質は、分子、化合物、原子、イオンなどであり得る。特定の実施形態では、ゲスト物質は、ヨウ素およびポリヨウ化物イオン以外の物質である。
(2.1)アミロースのアルカリ水溶液
本発明の製造法においては、アミロースのアルカリ水溶液が作製される。アルカリ溶液中のアミロースの量は、好ましくは約1重量%以上であり、より好ましくは約5重量%以上であり、さらに好ましくは約10重量%以上であり、最も好ましくは約15重量%以上である。アルカリ溶液中のアミロースの量は、好ましくは約60重量%以下であり、より好ましくは約50重量%以下であり、さらに好ましくは約40重量%以下であり、さらに好ましくは約30重量%以下であり、さらに好ましくは約25重量%以下であり、最も好ましくは約20重量%以下である。アミロース濃度が低すぎると、ビスコースに添加される水量が多くなり、紡糸性が悪くなる場合がある。アミロース濃度が高すぎると、ビスコース中に均一にアミロースを混合しにくくなる場合がある。
本発明においては、当該分野で公知の従来のビスコースが用いられ得る。アミロースのアルカリ水溶液と混合することにより希釈されることを考えて濃度が適切に調節されることが好ましい。
上記アミロースのアルカリ水溶液とビスコースとは、当該分野で公知の任意の方法によって混合され得る。混合方法は特に限定されない。ビスコース中にアミロースのアルカリ水溶液を添加および混合するための装置としては、インジェクション型またはホモミキサー型の装置を用いて行えばよい。添加および混合の時期についても任意でよく、たとえば、ビスコースを脱泡した後でも、脱泡する前に行い添加及び混合後に脱泡してもよい。
アミロースを含有するビスコース液は、従来公知の方法で紡糸されてアミロース含有レーヨントウが得られ得る。紡糸後はトウの形態となっているが、トウの形態のまま、あるいはトウを任意の繊維長となるように切断し、その後、従来公知の方法で精練すれば機能性レーヨン繊維が得られる。アミロース含有レーヨントウを後加工時に切断する場合もある。
得られたアミロース含有レーヨン繊維は、例えば、その繊維を製造した後に、溶媒中で加熱工程および冷却工程を行うことにより、アミロースの包接力が向上され得る。
得られたアミロース含有レーヨン繊維は、例えば、アルカリで処理した後中和することにより、アミロースの包接力が向上され得る。
本発明のアミロース含有レーヨン繊維は、レーヨン繊維中にアミロースが分散および保持されている。ここで、レーヨン繊維中でアミロースはほぼ均一に分散および保持されていると考えられる。
本発明のアミロース含有レーヨン繊維は、洗浄によりアミロースが実質的に溶出しない。本明細書中で使用される場合、用語「洗浄によりアミロースが実質的に溶出しない」とは、洗浄により溶出するアミロースの量がアミロース含有レーヨン繊維中に含まれるアミロースのうちの10重量%以下であることを意味する。アミロース含有レーヨン繊維からのアミロースの溶出しやすさは、以下の条件で決定されることが好ましい:アミロース含有レーヨン繊維を40倍量の洗濯液(0.75mg/mLの洗剤水溶液。洗剤として例えば、ライオン株式会社製トップ(24%界面活性剤(アルファスルホ脂肪酸エステルナトリウム、脂肪酸ナトリウム、ポリオキシエチレンアルキルエーテル)、その他成分としてアルカリ剤(炭酸塩)、溶解促進剤、酵素、蛍光増白剤、漂白剤含有)に3時間浸漬した後濾過フィルターで12,000×gにて4分間遠心濾過して得られた濾液中のアミロース量を測定し、溶出したアミロースの割合を計算する。
本明細書中では、用語「ゲスト物質を包接する能力を有する」とは、アミロースがゲスト物質を包接できる状態にあることをいう。包接とは、分子内包接のほか分子間包接も含む。分子内包接とはアミロース1分子にゲスト物質が包接される現象をいう。分子間包接とは複数のアミロース分子間またはアミロース分子とセルロース分子の間にゲスト物質が包接される現象をいう。
本発明のアミロース含有レーヨンの包接力は、ゲスト物質としてノニルフェノールを用いることで測定する。
カラムとしてTSKgel ODS−100Z(TOSOH製)を用い、検出器としてUV検出器SPD−6A(島津製作所製)を用い、送液ポンプとしてLC−6A(島津製作所製)を用いる。カラムを40℃に保ち、溶離液として80%メタノールを流速1.0mL/分で用いて分析する。
本発明のアミロース含有レーヨン繊維は、種々の形態で利用され得る。本発明のアミロース含有レーヨン繊維は、そのままの綿状で、または単独でもしくは他の繊維と混紡して糸として、または編織物、不織布(紙状の湿式不織布を含む)などの布帛として、衣料、カーテン、寝具、障子紙、壁紙、帽子、カーペット、ソファの表皮材、その他の消臭グッズなどとして好適に用いることができる。本発明のアミロース含有レーヨン繊維は、通常のレーヨン繊維と同じように様々な2次加工品に利用できる。このような2次加工品には、綿(わた)、糸、不織布、布、紙などがある。アミロース含有レーヨン繊維からこれらの二次加工品を製造する方法は当該分野で公知である。例えば、アミロース含有レーヨン繊維から紙を製造する場合には、短い繊維に切断したアミロース含有レーヨン繊維を通常の紙の原料と混合して、または短いアミロース含有レーヨン繊維を単独で抄紙することにより、アミロース含有レーヨン繊維から紙が製造され得る。さらにこれら2次加工品をさらに高度に加工した、衣類、ファブリック、フィルター、化粧品用加工品、医療用品、日用品、包装用品、生理用品などの衛生材料などの製品にも利用できる。ファブリックとは、生地、織物などを使用した製品のことであり、インテリア産業では、生地および織物の総称から少し広い意味で用いられることが多く、カーテン、テーブルクロス、椅子およびソファの張り布地、クッション、ベッドカバーなど、布を使ったものを全般にさし、布の壁装材をも包含する。
本発明のアミロース含有レーヨン繊維の利用目的は、大きく以下の二つに分類することが出来る。(1)ゲスト物質を包接させずにそのまま利用する方法と、(2)ゲスト物質を包接させた状態で利用する方法である。
ゲスト物質を包接させずにそのまま利用する方法においては、アミロースが様々な物質を包接する機能を、(A)消臭、(B)濃縮(回収)、(C)除去、(D)精製、などの目的に利用することができる。以下、それぞれの利用目的について説明する。
「消臭」とは、におい成分を捕集する(とじこめる)ことを意味する。捕集できるにおい成分の例は、(1.3)の(c)に記載されるとおりである。消臭目的での具体的な製品例は、消臭機能付ペットシーツ、消臭機能付衣類、消臭機能付衛生用品、消臭機能付寝具、空気清浄機用フィルター、壁紙などが挙げられる。
「濃縮」とは、希薄な状態に存在しているターゲット物質を捕集して濃度を上昇させることを意味している。濃縮されるターゲット物質は、アミロースに包接可能な物質であれば、どのような物質であってもよい。ターゲット物質の例は、(1.3)に記載されるとおりである。濃縮目的での具体的な製品例としては、これらのターゲット物質の回収用フィルターおよびカラム(例えば、界面活性剤回収用フィルターおよびカラム、脂肪酸回収用フィルターおよびカラム、生理機能物質(例えば、医薬品の有効成分;ポリフェノール;フラボノイド;アルカロイド;酸;ビタミン類)回収用フィルターおよびカラム、アルキル化合物回収用フィルターおよびカラムなど)が挙げられる。また、アミロース含有レーヨン繊維をそのまま、混合物を含む容器などに入れ、目的物質を吸着(包接)させた後アミロース含有レーヨン繊維を回収し、それから目的物質を溶出させて回収するというバッチ式の使用方法もある。
「除去」とは、ターゲット物質または製品に混入している夾雑物質を捕集して除去することを意味している。除去されるターゲット物質および夾雑物質は、アミロースに包接可能な物質であれば、どのような物質であってもよい。除去されるターゲット物質および夾雑物質の例は、(1.3)に記載されるとおりである。除去目的での具体的な製品例としては、タールまたはニコチン除去フィルター、排気ガス成分(例えばピレン化合物)除去用フィルター、水浄化用フィルターおよびカラム、空気清浄用フィルター、マスク、クリーニング製品、パーソナル洗浄製品などが挙げられる。また、アミロース含有レーヨン繊維をそのまま、製品を含む容器などに入れ、夾雑物質を除去するという使用方法もある。
「精製」とは、混合物から特定の物質を精製して純粋な物質にすることを意味している。精製される物質は、アミロースに包接可能な物質であれば、どのような物質であってもよい。精製される物質の例は、(1.3)に記載されるとおりである。精製目的での具体的な製品例としては、これらのターゲット物質の精製用フィルターおよびカラム(例えば、界面活性剤精製用フィルターおよびカラム、脂肪酸精製用フィルターおよびカラム、生理機能物質(例えば、医薬品の有効成分;ポリフェノール;フラボノイド;アルカロイド;酸;ビタミン類)精製用フィルターおよびカラム、アルキル化合物精製用フィルターおよびカラムなどが挙げられる。また、アミロース含有レーヨン繊維をそのまま、混合物を含む容器などに入れ、目的物質を吸着(包接)させた後アミロース含有レーヨン繊維を回収し、それから目的物質を溶出させて回収するというバッチ式の使用方法もある。
ゲスト物質を包接させた状態で利用する方法においては、様々なゲスト物質を工夫することにより(E)殺菌または抗菌、(F)防虫または防カビ、(G)付香または消臭、(H)安定化、(I)徐放、(J)紫外線防止、(K)化粧機能の付与、(L)医療用機能の付与、などの目的に利用することができる。以下、それぞれの利用目的について説明する。
「殺菌」とは、微生物を殺すことをいう。「抗菌」とは、微生物の増殖を抑制または阻止することをいう。微生物とは、顕微鏡的大きさの生物をいう。微生物の例としては、細菌、真菌(例えば、酵母)、原生動物、ウイルスなどが挙げられる。殺菌または抗菌目的の製品は、その製品表面または製品内部において、微生物を殺したり、増殖できなくしたりすることを目的とする製品である。
「防虫」とは、虫を寄せ付けないことおよび虫がつくのを防ぐことである。「防カビ」とは、カビの繁殖を防ぐことである。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例としては、防虫剤および防カビ剤が挙げられる。防虫剤の例は、上記(1.3)の(b)に記載されるとおりである。防カビ剤の例は、上記(1.3)の(j)に記載されるとおりである。
「付香」とは、香味成分(香料)を添加して着香することである。「消臭」とは、においを消すことである。
「安定化」とは、単独では不安定で分解または変性する物質の分解または変性を防止することをいう。単独のままでは不安定な物質を包接することにより、その物質が安定化されて、単独の場合よりも長期に保存され得る。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例としては、光、紫外線、熱、酸素などにより分解されやすく、アミロースに包接され得る物質が挙げられる。
「徐放」とは、物質を徐々に放出することである。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例は、上記(1.3)の(e)に記載されるとおりである。
「紫外線防止」とは、紫外線量を減少させるかなくすことである。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例としては、紫外線吸収物質(紫外線吸収剤ともいう)が挙げられる。紫外線吸収物質の例は、上記(1.3)の(f)に記載されるとおりである。
「化粧機能の付与」とは、保湿作用、美白作用、抗炎症作用、血行促進作用、抗酸化作用、制汗作用、清涼作用、細胞腑活化作用など、化粧品において通常付与されることが期待される機能をいう。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例としては、保湿成分、美白成分、抗炎症剤、細胞賦活化剤および酸化防止剤が挙げられる。保湿成分、美白成分、抗炎症剤、細胞賦活化剤および酸化防止剤の例は、上記(1.3)の(g)に記載されるとおりである。
「医療用機能の付与」とは、医療目的の機能を付与することをいう。この目的のためにアミロース含有レーヨン繊維に包接させるゲスト物質の例としては、医薬品の有効成分、および育毛剤が挙げられる。医薬品の有効成分の例は、上記(1.3)の(d)に記載されるとおりである。
本明細書中では、用語「化学物質含有溶液」は、化学物質を含む溶液をいう。化学物質は、アミロースによって包接される任意の化学物質であり得る。例えば、この化学物質は、上記(1.3)で説明した任意のゲスト物質であり得る。ただし、化学物質は、ヨウ素でもポリヨウ化物イオンでもない。なお、本明細書中で「ヨウ素」とは、ヨウ素分子およびヨウ化物イオンの両方を含む。ただし、「ヨウ素またはポリヨウ化物イオン」という場合の「ヨウ素」はヨウ素分子を意味する。化学物質含有溶液は、化学物質を含有する溶液であれば任意の溶液であり得る。
アミロース含有レーヨン繊維とゲスト物質を接触させることにより、ゲスト物質をアミロース含有レーヨン繊維に包接させることができる。接触させる方法には、例えば、ゲスト物質を含む溶液にアミロース含有レーヨン繊維を浸すような液相で接触させる方法;アミロース含有レーヨン繊維にゲスト物質を含む溶液を噴霧する、ゲスト化合物の蒸気を接触させるなどの気相で接触させる方法がある。ゲスト物質が約130℃〜約150℃の水溶液中に溶存し得る物質である場合、アミロース含有レーヨン繊維とゲスト物質とを接触させる工程で、「(2.5)加熱冷却処理」または「(2.6)アルカリ処理」を同時に行うことで、ゲスト物質の包接量を上げることができる。このようなゲスト物質の場合、接触工程と「(2.5)加熱冷却処理」または「(2.6)アルカリ処理」を同時に行うことが好ましい。
20mMリン酸緩衝液(pH7.0)、20g/Lスクロース、および種々の濃度のマルトオリゴ糖混合物(3880、232、77、44または8.8mg/リットル)を含有する反応液(1リットル)に、国際公開第2004/113525号パンフレットの実施例2−1Aに記載の方法に従って調製し、精製した馬鈴薯塊茎由来の耐熱化グルカンホスホリラーゼ(国際公開第2004/113525号パンフレットの配列番号34のアミノ酸配列を有するもの;1単位/ml)と、国際公開第2005/24008号パンフレットの実施例2Aに記載の方法に従って調製した耐熱化Streptococcus mutans由来スクロースホスホリラーゼ(国際公開第2005/24008号パンフレットの配列番号22のアミノ酸配列を有するもの;1単位/ml)を加えて37℃で16時間保温し、反応終了後、生成したα−1,4−グルカンの収率(%)、重量平均分子量(Mw)、重合度および分散度(Mw/Mn)を決定した。各結果を下記の表1に示す。
合成例1で合成し、本発明で使用したグルカンの分子量を以下の方法により測定した。
原料パルプ(LDPT:日本製紙ケミカル製)から常法に従ってビスコースを調製した。このビスコースは、セルロース含有率9重量%、アルカリ含有率5重量%で、落球粘度60秒であった。
実施例1−1から1−4および比較例1−2から1−3で製造したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてノニルフェノールを用いて測定した。
実施例1−2、1−4および比較例1−3で製造したアミロース含有レーヨン繊維または比較例1−1で製造したコントロールのレーヨン繊維を洗濯試験に供し、アミロース含有レーヨン繊維中のアミロースの安定性を確認した。
実施例1−4で製造した平均分子量1.174×105のアミロース含有レーヨン繊維(20%仕込み)をニードルパンチ法で厚さ約3mmの不織布に加工しアミロース含有レーヨン不織布を得た。この不織布を直径7cmの円板状に切り取って、アミロース含有レーヨン不織布フィルター(実施例4)を得た。
耐圧ガラス試験管(10mL)に実施例1−4で作製したアミロース含有レーヨン繊維50mgと水系溶媒(50容量%メタノール水溶液、50容量%エタノール水溶液または50容量%1−プロパノール水溶液)3mLを入れて密栓し、130℃にて30分間ヒートブロックで加熱した。レーヨン繊維を取り出して吸引ろ過し、オーブン中で50℃にて2時間加熱して乾燥させ、その後室温で放冷することにより、加熱処理されたアミロース含有レーヨン繊維(50%メタノール水溶液:実施例5−1;50%エタノール水溶液:実施例5−2;50%1−プロパノール水溶液:実施例5−3)を得た。以下の実施例8で確認されたように、この加熱処理によってアミロース含有レーヨン繊維の包接力が向上した。
実施例1−4で作製したアミロース含有レーヨン繊維50mgにメタノール、エタノール、または1−プロパノールを約1mL噴霧してガラス容器に密封し、オーブン中で130℃にて30分間加熱後、室温に放冷することにより冷却した。これをオーブン中で50℃にて2時間加熱して乾燥し、その後室温で放冷することにより、アルコール処理されたアミロース含有レーヨン繊維(メタノール噴霧:実施例6−1、エタノール噴霧:実施例6−2、1−プロパノール噴霧:実施例6−3)を得た。以下の実施例8と同様の方法で、このアルコール処理によってアミロース含有レーヨン繊維の包接力が向上したことが確認される。
実施例1−4で作製したアミロース含有レーヨン繊維50mgを、3mLの1N NaOH水溶液に室温で1時間浸漬後、取り出し、1N塩酸水溶液を加えて中和した。これを取り出して水で洗浄後、オーブン中で50℃にて2時間加熱して乾燥し、その後室温で放冷することにより、アルカリ処理されたアミロース含有レーヨン繊維を得た。以下の実施例8と同様の方法で、このアルカリ処理によってアミロース含有レーヨン繊維の包接力が向上したことが確認される。
包接力の評価にあたり、ゲスト分子としてノニルフェノールを用いた。
カラムとしてTSKgel ODS−100Z(TОSОH製)を用い、検出器としてUV検出器SPD−6A(島津製作所製)を用い、送液ポンプとしてLC−6A(島津製作所製)を用いた。カラムを40℃に保ち、溶離液としては80%メタノールを流速1.0mL/分で用いた。結果を表5に示す。
環境汚染物質のゲスト分子の例として、ノニルフェノールを用いた。
カラムとしてTSKgel ODS−100Z(TОSОH製)を用い、検出器としてUV検出器SPD−6A(島津製作所製)を用い、送液ポンプとしてLC−6A(島津製作所製)を用いた。カラムを40℃に保ち、溶離液としては80%メタノールを流速1.0mL/分で用いた。結果を表6に示す。
耐圧ガラス試験管(10mL)に実施例1−4で作製したアミロース含有レーヨン繊維50mgと濃度100ppmのノニルフェノールを含む50%メタノール水溶液3mLを入れて密栓し、130℃にて30分間ヒートブロックで加熱し、室温に15時間放冷することにより冷却した。レーヨン繊維を浸漬・加熱する前後のこの水溶液中のノニルフェノール濃度を液体クロマトグラフィーで測定した。浸漬前後のノニルフェノール量の差から、レーヨン繊維へのノニルフェノールの吸着を求めた。
カラムとしてTSKgel ODS−100Z(TОSОH製)を用い、検出器としてUV検出器SPD−6A(島津製作所製)を用い、送液ポンプとしてLC−6A(島津製作所製)を用いた。カラムを40℃に保ち、溶離液としては80%メタノールを流速1.0mL/分で用いた。結果を表7に示す。
紫外線吸収剤のゲスト分子の例として、ノニルフェノールを用いた。
実施例11で製造されたノニルフェノール包接アミロース含有レーヨン不織布に200nm−450nmの紫外光および可視光を照射して反射スペクトルを測定することにより、このレーヨン不織布の紫外線防御効果を試験した。
殺菌剤のゲスト分子の例として、抗生物質を用いる。
消臭剤のゲスト分子の例として、ラウリルメタクリレートを用いる。
実施例4で作製したアミロースレーヨン不織布フィルターまたは実施例10で作製したコントロールレーヨン不織布フィルター(アミロース不含)を、悪臭物質(ノネナール、酪酸、吉草酸、イソ吉草酸)を含む密閉容器中に入れて2時間および24時間放置する。その後、不織布フィルターを入れる前後の容器中の空気に含まれる悪臭物質の量をガスクロマトグラフィーで測定し、比較する。
防虫剤のゲスト分子の例として、ピレスロイドを用いる。
実施例1−4で作製したアミロースレーヨンまたは比較例1−1で作製したレーヨン(コントロール)を、ノニルフェノールを含む浴中に入れて一晩放置する。その後、レーヨンを取り出し、水で洗浄後、少量のメタノールで溶出することにより、この目的の化学物質を濃縮し回収する。
安定化されることを目的とする物質(ゲスト分子)の例として、色素を用いる。
20mMリン酸緩衝液(pH7.0)、20g/Lスクロース、およびマルトオリゴ糖混合物(245mg/リットル)を含有する反応液(1リットル)に、国際公開第2004/113525号パンフレットの実施例2−1Aに記載の方法に従って調製し、精製した馬鈴薯塊茎由来の耐熱化グルカンホスホリラーゼ(国際公開第2004/113525号パンフレットの配列番号34のアミノ酸配列を有するもの;1単位/ml)と、国際公開第2005/24008号パンフレットの実施例2Aに記載の方法に従って調製した耐熱化Streptococcus mutans由来スクロースホスホリラーゼ(国際公開第2005/24008号パンフレットの配列番号22のアミノ酸配列を有するもの;1単位/ml)を加えて37℃で16時間保温し、反応終了後、生成したα−1,4−グルカンの重量平均分子量(Mw)、重合度および分散度(Mw/Mn)を決定した。結果を下記の表8に示す。
原料パルプ(LDPT:日本製紙ケミカル製)から常法に従ってビスコースを調製した。このビスコースは、セルロース含有率9重量%、アルカリ含有率5重量%で、落球粘度60秒であった。
実施例19−1および19−2で製造した平均分子量3.00×104のアミロースを含有するレーヨン繊維の包接力を、ゲスト物質としてノニルフェノールを用いて調べた。コントロールとして、比較例1−1で製造したレーヨン繊維の包接力も測定した。ノニルフェノールの包接操作方法および包接力の評価方法は実施例2と同様であった。結果を表10に示す。
実施例1−4のアミロース含有レーヨン繊維およびコントロールの比較例1−1のレーヨン繊維の消臭力をゲスト物質としてペラルゴン酸およびノネナールを用いて測定した。これらのレーヨン繊維は、綿の状態で使用した。ペラルゴン酸およびノネナールは代表的な悪臭物質である。ペラルゴン酸は腐敗臭のような不快な臭いを持つ物質であり、可塑剤、ラッカー、接着剤、アルキド樹脂および柔軟剤の製造に使用される。さらに、ペラルゴン酸は30代男性の発する悪臭の原因物質として知られている。ノネナールは中高年特有の体臭である加齢臭の原因物質として知られている。
カラムとしてDB−WAX(J&W)を用い、測定機として質量分析計GC−MS5050A(島津製作所)を用いた。カラムを200℃に保ち、キャリアガスとしてヘリウムを用いた。
結果を表11および表12に示す。
実施例1−1および1−2のアミロース含有レーヨン繊維30重量%と、比較例1−1のレーヨン繊維70重量%とを混紡し、60番手の混紡糸を作製した。これを用いて、筒編み生地を作製した(実施例22のアミロース含有レーヨン生地)。比較として、アミロース含有レーヨン繊維を配合しないこと以外は同じ方法で筒編み生地(比較例22)を作製した。
実施例22で作製したアミロース含有レーヨン生地およびコントロールのレーヨン生地の消臭力をゲスト物質としてペラルゴン酸およびノネナールを用いて測定した。
カラムとしてDB−WAX(J&W)を用い、測定機として質量分析計GC−MS5050A(島津製作所製)を用いた。カラムを200℃に保ち、キャリアガスとしてヘリウムを用いた。
結果を表13および表14に示す。
実施例1−2、実施例1−4、実施例19−1および実施例19−2で作製したアミロース含有レーヨン繊維および比較例1−1で作製したコントロールのレーヨン繊維の包接力をゲスト物質としてメントールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した
ガスクロマトグラフ装置にはGC−2014(島津製作所製)、カラムにULBONHR−Thermon−600T(0.25mmφ×25m、信和化工製)、キャリアガスにヘリウムガス、検出器に水素炎イオン化検出器(島津製作所製)を用いた。気化室温度は280℃、カラム温度は150℃、検出器温度は250℃で行ない、キャリアガスの圧力は150kPaに保った。結果を表15に示す。
実施例1−4で作製した平均分子量1.174×105のアミロース含有レーヨン繊維を40重量%、ポリプロピレン・ポリエチレン芯鞘繊維(チッソ製 ES繊維)を60重量%を、空気流で開繊、混合し、カード機によりウェブを作製後、ヒートロールで加熱することによりサーマルボンド不織布(約20g/m2)(実施例25)を作製した。比較として、アミロース含有レーヨン繊維を配合しないポリプロピレン・ポリエチレン芯鞘繊維のサーマルボンド不織布(約20g/m2)(比較例25)を作製した。
実施例25で作製したアミロース含有レーヨン繊維40%配合のサーマルボンド不織布および比較例25で作製したコントロールのサーマルボンド不織布それぞれ1.3gに2%メントールのメタノール溶液6.5mL添加し、100℃のオーブン中で乾燥させて、溶媒および余分なメントールを揮発させた。15時間後、オーブンから取り出し、メントール包接したアミロース含有レーヨン繊維40%配合のサーマルボンド不織布およびコントロールのサーマルボンド不織布を得た。
実施例26で作製したメントール包接アミロース含有レーヨン繊維40%配合サーマルボンド不織布の安定性を調べるために、100℃(湿度測定不能、乾燥状態)および25℃(湿度30%)環境下に10日間静置した。5日目、10日目にサンプリングして、不織布100mg中のメントール量を測定した。メントールの抽出法および分析法は実施例24と同様であった。メントール残存率(%)は以下の式で求めた。
実施例26で作製したメントール包接アミロース含有レーヨン繊維40%配合サーマルボンド不織布の加湿条件下における徐放性を調べた。
実施例1−4で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてリナロールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてケトン系香料メントンを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてアルデヒド系香料シトロネラールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてアルデヒド系香料ノナナールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてアルコール系香料ゲラニオールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてアルコール系香料シトロネロールを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
実施例1−2で作製したアミロース含有レーヨン繊維および比較例1−1で製造したコントロールのレーヨン繊維の包接力をゲスト物質としてエステル系香料の酢酸リナリルを用いて評価した。これらのレーヨン繊維は、綿の状態で使用した。
メントールを包接させたアミロース含有レーヨンからのメントールの徐放性における、アミロースの重合度の影響を調べた。
実施例29(リナロール)、実施例30(メントン)、実施例31(シトロネラール)、実施例32(ノナナール)、実施例33(ゲラニオール)、実施例34(シトロネロール)および実施例35(酢酸リナリル)で作製した各芳香成分包接アミロース含有レーヨン繊維の加湿条件下における徐放性を調べた。実施例36で確認されたように、平均分子量3.00×104〜1.174×105の範囲ではアミロースの分子量による徐放性の差は、ほとんどなかったので、実施例1―2のアミロース含有レーヨン繊維で代表させて徐放性を調べた。
アミロース含有レーヨン繊維のメントールの包接量を、アミロース粉末の包接量と比較した。実施例38で確認されたように、平均分子量3.00×104〜1.174×105の範囲では、アミロースはどの分子量でも、レーヨンに練り込むことにより、アミロースの重量当たりの包接量が大きく上昇したので、ここでは実施例1―2のアミロース含有レーヨン繊維および試料2の平均分子量4.62×104の酵素合成アミロース粉末で代表させて調べた。すなわち、いずれの試料においてもアミロースの平均分子量は4.62×104であった。
Claims (25)
- アミロース含有レーヨン繊維の製造方法であって、
アミロースのアルカリ水溶液とビスコースとを混合して混合液を得る工程;および
該混合液を紡糸してアミロース含有レーヨン繊維を得る工程
を包含し、
該アミロースは、重量平均分子量が3×104以上2×105以下の酵素合成アミロースである、方法。 - 前記アミロース含有レーヨン繊維が、加熱冷却処理される、請求項1に記載の方法。
- 前記アミロース含有レーヨン繊維が、アルカリ処理される、請求項1に記載の方法。
- 前記アミロース含有レーヨン繊維をヨウ素およびポリヨウ化物イオン以外のゲスト物質と接触させて該ゲスト物質を該アミロース含有レーヨン繊維のアミロース中に包接させる工程を包含し、該ゲスト物質が、殺菌剤、抗菌剤、防虫成分、におい成分、生理機能物質、紫外線吸収物質、化粧品成分、着色料、染料、消臭成分および防カビ成分からなる群より選択される、請求項1に記載の方法。
- 前記アミロース含有レーヨン繊維をアミロースのゲスト物質と接触させない、請求項1に記載の方法。
- 前記酵素合成アミロースが、α−1,6−グルコシド結合を含まないアミロースである、請求項1に記載の方法。
- 前記酵素合成アミロースの分散度が3.0以下である、請求項1に記載の方法。
- 前記アミロース含有レーヨン繊維中の前記酵素合成アミロースの含有量が0.01重量%以上50重量%以下である、請求項1に記載の方法。
- ゲスト物質を包接する能力を有するアミロース含有レーヨン繊維であって、該レーヨン繊維中のアミロースは、洗浄により実質的に溶出せず、かつ該レーヨン繊維中に分散しており、該アミロースは、重量平均分子量が3×104以上2×105以下の酵素合成アミロースであり、該アミロースはゲスト物質を包接していない、アミロース含有レーヨン繊維。
- アミロースの含有量が0.01重量%以上50重量%以下である、請求項9に記載のアミロース含有レーヨン繊維。
- アミロース含有レーヨン繊維であって、該レーヨン繊維中のアミロースは、洗浄により実質的に溶出せず、かつ該レーヨン繊維中に分散しており、該アミロースは、重量平均分子量が3×104以上2×105以下の酵素合成アミロースであり、該アミロースはヨウ素およびポリヨウ化物イオン以外のゲスト物質を包接している、アミロース含有レーヨン繊維。
- アミロースの含有量が0.01重量%以上50重量%以下である、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として殺菌剤を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として香料を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として紫外線吸収物質を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として生理機能物質を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として防虫成分を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- ゲスト物質として消臭成分を包接している、請求項11に記載のアミロース含有レーヨン繊維。
- 前記酵素合成アミロースが、α−1,6−グルコシド結合を含まないアミロースである、請求項9または11に記載のアミロース含有レーヨン繊維。
- 前記酵素合成アミロースの分散度が3.0以下である、請求項9または11に記載のアミロース含有レーヨン繊維。
- 化学物質を濃縮、回収、除去または単離するために、該化学物質を繊維中に捕捉する方法であって、
該化学物質を含有する溶液または気体と、請求項9に記載のアミロース含有レーヨン繊維とを接触させることにより、該化学物質を前記アミロースに包接させる工程を包含し、該化学物質はアミロースにより包接可能な物質であり、該化学物質はヨウ素およびポリヨウ化物イオン以外の物質である、方法。 - 請求項9に記載のアミロース含有レーヨン繊維を含む、前記ゲスト物質の濃縮、回収、除去または単離用の製品。
- 請求項9または11に記載のアミロース含有レーヨン繊維を含む、織物、編物、不織布または紙より得られた製品。
- 請求項9に記載のアミロース含有レーヨン繊維を含む、消臭用製品。
- 請求項15に記載のアミロース含有レーヨン繊維を含む、紫外線防止用製品。
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