JP3593539B2 - Processing method for cellulose fiber products - Google Patents
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Description
【０００１】
【発明の属する技術分野】
本発明は綿、麻などのセルロース繊維品の処理方法に関する。更に詳しくはセルロース繊維品に防しわ性、寸法安定性、ウォッシュ・アンド・ウェア性、ドレープ性、可縫性を付与する処理方法に関するものである。
【０００２】
【従来の技術】
従来、セルロース繊維品に防縮性及びウォッシュ・アンド・ウェア性を付与する方法として、▲１▼グリオキザールやエポキシ樹脂を用いて架橋する方法、▲２▼高圧水蒸気を用いてセルロース繊維品を処理する方法、及び▲３▼シルケット加工や液体アンモニア加工によるセルロース繊維品の改質法が提案されている。
【０００３】
【発明が解決しようとする課題】
しかし、上記▲１▼の方法はセルロース繊維品の引張強度や引裂強度が低下したり、繊維品が変色するおそれがあるばかりでなく、これらの樹脂で加工した繊維品には人体に有害なホルマリンが残留することがあった。また上記▲２▼の方法は処理装置が高価であるにもかかわらず十分な性能が得られにくい問題点があった。更に上記▲３▼の方法はシルケット加工や液体アンモニア加工だけではセルロース繊維品の改質効果が不十分であり、樹脂加工を併用しなければならない煩わしさがあった。
本発明の目的は、セルロース繊維品に対して、強度低下や変色を起こすことなく、ホルマリンの残留もなく、簡便に防しわ性、寸法安定性、ウォッシュ・アンド・ウェア性、ドレープ性、可縫性を付与するセルロース繊維品の処理方法を提供することにある。
【０００４】
【課題を解決するための手段】
請求項１に係る発明は、０．５〜３重量％のアンモニウム塩を含むｐＨ５．０〜８．５の第１水溶液にセルロース繊維品を３０〜６０℃で２０〜６０分間含浸する工程と、前記第１水溶液に含浸したセルロース繊維品を１〜１０重量％の柔軟剤を含むｐＨ６〜９の第２水溶液に含浸する工程と、前記第２水溶液に含浸したセルロース繊維品を１０〜３０重量％の形態安定化剤と１〜１５重量％のアルカリ剤を含むｐＨ９〜１１の第３水溶液に含浸する工程と、前記第３水溶液に含浸したセルロース繊維品を１４０〜１８０℃で４５〜１８０秒間乾熱処理する工程と、前記乾熱処理したセルロース繊維品を０．０１〜１重量％の酸を含むｐＨ０．５〜４の第４水溶液に含浸する工程とを含むセルロース繊維品の処理方法である。
【０００５】
請求項１に係る方法によれば、第１水溶液で処理すると、セルロース繊維表面の濡れ性を改善し、側鎖の末端基の活性化を促進させる。また、第２水溶液で処理すると、セルロース繊維を柔軟化するとともに強力低下を抑制する。また、第３水溶液で処理すると、セルロースのアモルファス領域を改質し、擬似結晶領域を増大させる。乾熱処理を行うと、第３水溶液による処理工程での反応が完了する。最後に第４水溶液で処理すると、第３水溶液による処理でアルカリ性となったセルロース繊維品が酸により中性化される。この結果、これらの処理の相乗効果により、セルロース繊維品の防しわ性、寸法安定性、ウォッシュ・アンド・ウェア性、ドレープ性、可縫性が改善される。
【０００６】
【発明の実施の形態】
本発明のセルロース繊維品を構成するセルロース繊維としては綿、麻等の天然セルロース繊維、レーヨン、キュプラ、ポリノジック等の再生セルロース繊維、リヨセル等の溶剤紡糸セルロース繊維がある。セルロース繊維品としては、これらの繊維から作られるスライバー、糸、織物、編物、不織布等がある。本発明のセルロース繊維品はセルロース繊維１００％である必要はなく、他の繊維、例えば羊毛繊維、絹繊維等の蛋白繊維、、ポリエステル、アセテート、ナイロン等の化学繊維との混紡、混織、混編を行った繊維品を含む。この場合セルロース繊維を少なくとも５０重量％含む。
本発明の第１水溶液は、０．５〜３重量％、好ましくは０．８〜１．５重量％のアンモニウム塩を含むｐＨ５．０〜８．５、好ましくはｐＨ７．５〜８．５の水溶液である。上記アンモニウム塩が０．５重量％未満では薬剤の浸透効果が十分に達されずセルロース繊維表面の濡れ性が改善されない。また３重量％を越えた場合には薬品が過剰となる。アンモニウム塩としては、炭酸水素アンモニウム、炭酸アンモニウム、硫酸水素アンモニウム、硫酸アンモニウム、リン酸一アンモニウム、リン酸二アンモニウム及びリン酸三アンモニウム等が例示される。これらを単独又は組み合わせて用いる。この第１水溶液にセルロース繊維品を含浸して３０〜６０℃、好ましくは３５〜５０℃で２０〜６０分間、好ましくは２０〜４５分間処理する。処理温度及び処理時間が上限値を越えると処理が不均一になり、下限値未満になると処理不足になる。
【０００７】
本発明の第２水溶液は、１〜１０重量％、好ましくは１〜５重量％の柔軟剤を含むｐＨ６〜９、好ましくはｐＨ７〜８の水溶液である。上記柔軟剤が１重量％未満では引裂強度を保持することができず、好ましい風合いが得られない。１０重量％を越えるとべとついて風合不良になるとともに、滑脱抵抗力が低下する。柔軟剤としては、シリコーン樹脂、エポキシシリコーン樹脂、変成シリコーン等が例示される。これらを単独又は組み合わせて用いる。
本発明の第３水溶液は、１０〜３０重量％、好ましくは１０〜２０重量％の形態安定化剤と、１〜１５重量％、好ましくは１〜６重量％のアルカリ剤を含むｐＨ９〜１１、好ましくはｐＨ１０〜１１の水溶液である。上記形態安定化剤が１０重量％未満ではセルロース繊維品の形態が安定化せず、３０重量％を越えると薬品が過剰となる。形態安定化剤としては、ヒドロキシエチル化合物やメトキシエチル化合物が例示される。上記アルカリ剤が１重量％未満では薬剤の固着が不十分であり、１５重量％を越えると強力低下が著しくなる。アルカリ剤としては、炭酸ナトリウム、水酸化ナトリウム、アンモニア水、炭酸水素アンモニウムが例示される。これらを単独又は組み合わせて用いる。
本発明の第４水溶液は、０．０１〜１重量％、好ましくは０．０５〜０．２重量％の酸を含むｐＨ０．５〜４、好ましくはｐＨ２〜３の水溶液である。上記酸が０．５重量％未満では中和が不十分であり、４重量％を越えるとセルロース繊維品が損傷する。酸としては、酢酸、硫酸、蟻酸、塩酸が例示される。これらを単独又は組み合わせて用いる。
【０００８】
【実施例】
次に本発明の実施例を比較例とともに説明する。
＜実施例１＞
麻１００％シャツ地を用意した。浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％とアンモニウム塩である炭酸水素アンモニウム１０ｇ／ｌ（１．０ｇ重量％）を含むｐＨ８．０の第１水溶液に上記シャツ地を含浸し、４０℃で３０分間処理した。
次いで反応性シリコーン樹脂エマルジョン（ツヤック（株）４０−Ｑ−ＳＩ）３．０重量％とエポキシシリコーン樹脂（ツヤック（株）４０−Ｑ−ＳＥ）１．０重量％と浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）２．０重量％を含む２０℃でｐＨ７．５の第２水溶液を用意し、上記第２水溶液に０．２分間含浸した後、マングルで脱液し、１１０℃で５分間乾燥した。
次に浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％と形態安定化剤であるビスヒドロキシエチルスルホン（ツヤック（株）４０−ＢＳ−５０）１５．０重量％と炭酸ナトリウム４．０重量％を含むｐＨ１０．５の第３水溶液に上記シャツ地を含浸し、２５℃で３０分間処理した。
次に１６０℃で９０秒間前記第３水溶液で処理した上記シャツ地を乾熱処理した。更に酢酸０．１重量％を含む第４水溶液に、前記乾熱処理したセルロース繊維品を含浸し、４０℃で１５分間処理した。
【０００９】
＜実施例２＞
実施例１と同じ麻１００％シャツ地を用意し、実施例１と同じ第１水溶液に実施例１と同様に上記シャツ地を含浸して処理した。
次いで、反応性シリコーン樹脂エマルジョン（ツヤック（株）４０−Ｑ−ＳＩ）３．０重量％とエポキシシリコーン樹脂（ツヤック（株）４０−Ｑ−ＳＥ）２．０重量％と浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）２．０重量％を含む２０℃でｐＨ７．５の第２水溶液を用意し、上記第２水溶液に０．２分間含浸した後、マングルで脱液し、１１０℃で５分間乾燥した。
次に実施例１と同じ第３水溶液に実施例１と同様に上記シャツ地を含浸して処理した。更に実施例１と同様に上記シャツ地を乾熱処理した。更に実施例１と同じ第４水溶液に実施例１と同様に上記シャツ地を含浸して処理した。
【００１０】
＜実施例３＞
実施例１と同じ麻１００％シャツ地を用意した。浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％とアンモニウム塩である硫酸アンモニウム１０ｇ／ｌ（１．０ｇ重量％）を含むｐＨ５．４の第１水溶液に上記シャツ地を含浸し、４０℃で３０分間処理した。
次いで実施例１と同じ第２水溶液を用意し、上記硫酸アンモニウムを含む第１水溶液で処理したシャツ地を実施例１と同様に上記第２水溶液に含浸した後、脱液し乾燥した。
次に実施例１と同じ第３水溶液に実施例１と同様に上記シャツ地を含浸して処理した。更に実施例１と同様に上記シャツ地を感熱処理した。更に実施例１と同じ第４水溶液に実施例１と同様に上記シャツ地を含浸して処理した。
＜実施例４＞
実施例１と同じ麻１００％シャツ地を用意した。第１水溶液の処理を３０℃で２０分間にした以外は、実施例１と同様に処理した。
【００１１】
＜比較例１＞
実施例１と同じ麻１００％シャツ地を用意した。実施例１において、第１水溶液による処理を行わない以外、実施例１とそれぞれ同じ第２水溶液、第３水溶液、乾熱処理及び第４水溶液を用いて実施例１と同様に上記シャツ地を処理した。
＜比較例２＞
実施例１と同じ麻１００％シャツ地を用意した。実施例１において、第２水溶液による処理を行わない以外、実施例１とそれぞれ同じ第１水溶液、第３水溶液、乾熱処理及び第４水溶液を用いて実施例１と同様に上記シャツ地を処理した。
【００１２】
＜実施例５＞
綿１００％シャツ地を用意した。浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％とアンモニウム塩である炭酸水素アンモニウム１０ｇ／ｌ（１．０ｇ重量％）を含むｐＨ８．０の第１水溶液に上記シャツを含浸し、４０℃で３０分間処理した。
次いで反応性シリコーン樹脂エマルジョン（ツヤック（株）４０−Ｑ−ＳＩ）３．０重量％とエポキシシリコーン樹脂（ツヤック（株）４０−Ｑ−ＳＥ）１．０重量％と浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）２．０重量％を含む２０℃でｐＨ７．５の第２水溶液を用意し、上記第２水溶液に０．２分間含浸した後、マングルで脱液し、１１０℃で５分間乾燥した。
次に浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％と形態安定化剤であるビスヒドロキシエチルスルホン（ツヤック（株）４０−ＢＳ−５０）１５．０重量％と炭酸ナトリウム４．０重量％を含むｐＨ１０．５の第３水溶液に上記シャツ地を含浸し、２５℃で３０分間処理した。
次に１６０℃で９０秒間前記第３水溶液で処理した上記シャツ地を乾熱処理した。更に酢酸０．１重量％を含む第４水溶液に前記乾燥処理したセルロース繊維品を含浸し、４０℃で１５分間処理した。
【００１３】
＜実施例６＞
実施例５と同じ綿１００％シャツ地を用意し、実施例５と同じ第１水溶液に実施例５と同様に上記シャツ地を含浸して処理した。
次いで、反応性シリコーン樹脂エマルジョン（ツヤック（株）４０−Ｑ−ＳＩ）３．０重量％とエポキシシリコーン樹脂（ツヤック（株）４０−Ｑ−ＳＥ）２．０重量％と浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）２．０重量％を含む２０℃でｐＨ７．５の第２水溶液を用意し、上記第２水溶液に０．２分間含浸した後、マングルで脱液し、１１０℃で５分間乾燥した。
次に実施例５と同じ第３水溶液に実施例５と同様に上記シャツ地を含浸して処理した。更に実施例５と同様に上記シャツ地を乾熱処理した。更に実施例５と同じ第４水溶液に実施例５と同様に上記シャツ地を含浸して処理した。
【００１４】
＜実施例７＞
実施例５と同じ綿１００％シャツ地を用意した。浸透洗浄精練剤（ツヤック（株）２１−ＤＦ−１０）０．５重量％とアンモニウム塩である硫酸アンモニウム１０ｇ／ｌ（１．０ｇ重量％）を含むｐＨ５．４の第１水溶液に上記シャツ地を含浸し、４０℃で３０分間処理した。
次いで実施例５と同じ第２水溶液を用意し、上記硫酸アンモニウムを含む第１水溶液で処理したシャツ地を実施例５と同様に上記第２水溶液に含浸した後、脱液し乾燥した。
次に実施例５と同様に第３水溶液に実施例５と同様に上記シャツ地を含浸して処理した。更に実施例５と同様に上記シャツ地を感熱処理した。更に実施例５と同じ第４水溶液に実施例５と同様に上記シャツ地を含浸して処理した。
＜実施例８＞
実施例５と同じ綿１００％シャツ地を用意した。第１水溶液の処理を３０℃で２０分間にした以外は、実施例５と同様に処理した。
【００１５】
＜比較例３＞
実施例５と同じ綿１００％シャツ地を用意した。実施例５において、第１水溶液による処理を行わない以外、実施例５とそれぞれ同じ第２水溶液、第３水溶液、乾熱処理及び第４水溶液を用いて実施例５と同様に上記シャツ地を処理した。
＜比較例４＞
実施例５と同じ綿１００％シャツ地を用意した。実施例５において、第２水溶液による処理を行わない以外、実施例５とそれぞれ同じ第１水溶液、第３水溶液、乾熱処理及び第４水溶液を用いて実施例５と同様に上記シャツ地を処理した。
【００１６】
＜評価１＞
実施例１〜８で処理したシャツ地と、比較例１〜４で処理したシャツ地について、それぞれの防しわ性を調べるための試験方法（ＪＩＳ Ｌ１０５９−１９９８（モンサント法）） により評価した。この試験方法では、大きさ１５ｍｍ×４０ｍｍのシャツ地試料片を２枚の金属片からできた金属試料挟に挟み込んで、５００ｇの荷重を５分間かけた後、除重する。一端を試料挟に挟み込んだまま試料片の他端を試料挟から取り出し、試料片の自由端を下に向け、５分後の開角度を１８０で除して百分率（防しわ率）を求める。この結果を表１に示す。
表１から明らかなように、第１〜第４水溶液のうち、第１水溶液又は第２水溶液で処理しなかった比較例１〜４のシャツ地の防しわ率が３１．７〜４５．６％と小さかったのに対して、第１〜第４水溶液で処理した実施例１〜８のシャツ地の防しわ率は６３．５〜７７．８％と大きく、防しわ率が良好であった。
【００１７】
【表１】
＜評価２＞
実施例１〜８で処理したシャツ地と、比較例１〜４で処理したシャツ地について、それぞれの寸法変化率を調べるための試験方法（ＪＩＳ Ｌ１０９６−１９９９ ８．６４ Ｄ法）により評価した。この試験方法では、大きさ約２５ｃｍ×２５ｃｍのシャツ地試料片を採取し、２０ｃｍ×２０ｃｍのところにマークを付した後、約５０℃の石けん水溶液中に試料片を２０分間浸漬する。試料片を取り出し、約５０℃の温水で２０分間水洗した後、脱水し、水平状態で自然乾燥する。浸漬前と乾燥後の試料片のマークの間隔を測定し、百分率（寸法変化率）を求める。この結果を表２に示す。
表２から明らかなように、第１〜第４水溶液のうち、第１水溶液又は第２水溶液で処理しなかった比較例１〜４のシャツ地の寸法変化率が−８．８〜−３．６％と大きく収縮したのに対して、第１〜第４水溶液で処理した実施例１〜８のシャツ地の寸法変化率は−２．２〜−０．３％と小さく良好であった。
【００１９】
【表２】
＜評価３＞
実施例１〜８で処理したシャツ地と、比較例１〜４で処理したシャツ地について、それぞれのウォッシュ・アンド・ウェア性を調べるための試験方法（ＪＩＳＬ１０９６−１９９９ ８．２３．１ Ａ法）により評価した。この試験方法では、大きさ約４０ｃｍ×４０ｃｍのシャツ地試料片を採取し、試料片の端にほつれ防止を施し、所定の箇所にマークを付した後、約４０℃の温水で洗濯機を用いて洗濯する。試料片を脱水することなく、たて方向が垂直になるように、数箇所をつかみ、室温で風通しのないところでつるして乾燥する。洗濯前と乾燥後の試料片のマークの間隔を測定し、百分率（寸法変化率）を求める。この結果を表３に示す。表３から明らかなように、第１〜第４水溶液のうち、第１水溶液又は第２水溶液で処理しなかった比較例１〜４のシャツ地の洗濯後のしわの評価が２．０〜２．５級と低い等級であったのに対して、第１〜第４水溶液で処理した実施例１〜８のシャツ地の洗濯後のしわの評価は３．０〜３．８級と高い等級となり、実施例１〜８のシャツ地はウォッシュ・アンド・ウェア性が高いことが判った。
【００２１】
【表３】
＜評価４＞
実施例１〜８で処理したシャツ地と、比較例１〜４で処理したシャツ地について、それぞれのウォッシュ・アンド・ウェア性を調べるためのウールマーク試験方法 Ｎｏ．２８１ （ＩＷＳ ＴＭ２８１） により評価した。この試験方法では、大きさ５００×５００ ｍｍの織物試料を採取し、試料の端にほつれ防止を施し、所定の箇所にマークを付した後、４０℃±３℃の温水で洗濯機で洗濯する。洗濯を３サイクル行った後、乾燥した。乾燥したシャツ地にアイロンをかけた後、適当な布帛のなめらかさ用の写真と比較してシャツ地のなめらかさを調べた。この結果を表４に示す。
表４から明らかなように、第１〜第４水溶液のうち、第１水溶液又は第２水溶液で処理しなかった比較例１〜４のシャツ地の洗濯後のシャツ地のなめらかさの評価が２級と低い等級であったのに対して、第１〜第４水溶液で処理した実施例１〜８のシャツ地の洗濯後のシャツ地のなめらかさの評価は３〜３−４級と高い等級となった。
【００２３】
【表４】
【発明の効果】
以上述べたように、本発明の処理方法によれば、アンモニウム塩を含む第１水溶液でセルロース繊維表面の濡れ性を改善するとともに、側鎖の末端基の活性化を促進させ、柔軟剤を含む第２水溶液でセルロース繊維を柔軟化するとともに強力低下を抑制し、形態安定化剤とアルカリ剤を含む第３水溶液でセルロースのアモルファス領域を改質し、擬似結晶領域を増大させることにより、セルロース繊維品に対して、強度低下や変色を起こすことなく、ホルマリンの残留もなく、簡便に防しわ性、寸法安定性、ウォッシュ・アンド・ウェア性、ドレープ性、可縫性を付与することができる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for treating cellulosic fiber products such as cotton and hemp. More particularly, the present invention relates to a treatment method for imparting wrinkle resistance, dimensional stability, wash-and-wear, drape, and sewability to a cellulose fiber product.
[0002]
[Prior art]
Conventionally, as methods for imparting shrinkage resistance and wash-and-wear properties to cellulose fiber products, (1) a method of crosslinking using glyoxal or epoxy resin, and (2) a method of treating cellulose fiber products using high-pressure steam. And (3) A method for modifying cellulose fiber products by mercerizing or liquid ammonia processing has been proposed.
[0003]
[Problems to be solved by the invention]
However, the above method (1) not only reduces the tensile strength and tear strength of the cellulosic fiber product and may cause discoloration of the fiber product, but also produces formalin harmful to the human body for the fiber product processed with these resins. May remain. In addition, the above method (2) has a problem that it is difficult to obtain sufficient performance even though the processing apparatus is expensive. Further, in the method (3), the effect of modifying the cellulose fiber product is not sufficient only by the mercerizing process or the liquid ammonia process, and there is a trouble that the resin process must be used in combination.
An object of the present invention is to provide a cellulose fiber product that does not cause a decrease in strength or discoloration, has no formalin residue, and easily prevents wrinkles, dimensional stability, wash-and-wear, drape, and sewing. An object of the present invention is to provide a method for treating a cellulose fiber product that imparts properties.
[0004]
[Means for Solving the Problems]
The invention according to claim 1 is a step of impregnating the cellulose fiber product with a first aqueous solution containing 0.5 to 3% by weight of ammonium salt and having a pH of 5.0 to 8.5 at 30 to 60 ° C for 20 to 60 minutes; A step of impregnating the cellulose fiber product impregnated in the first aqueous solution with a second aqueous solution having a pH of 6 to 9 containing 1 to 10% by weight of a softener; Impregnating with a third aqueous solution having a pH of 9 to 11 and containing a form stabilizer and an alkali agent of 1 to 15% by weight, and drying the cellulose fiber impregnated with the third aqueous solution at 140 to 180 ° C. for 45 to 180 seconds. A method for treating a cellulose fiber product, comprising a heat treatment step and a step of impregnating the dry heat-treated cellulose fiber product with a fourth aqueous solution containing 0.01 to 1% by weight of acid and having a pH of 0.5 to 4.
[0005]
According to the method of the first aspect, when treated with the first aqueous solution, the wettability of the cellulose fiber surface is improved, and the activation of the terminal group of the side chain is promoted. When treated with the second aqueous solution, the cellulose fibers are softened and the strength is suppressed from decreasing. In addition, treatment with the third aqueous solution modifies the amorphous region of cellulose and increases the pseudocrystalline region. When the dry heat treatment is performed, the reaction in the treatment step using the third aqueous solution is completed. Finally, when the treatment is performed with the fourth aqueous solution, the cellulose fiber product that has become alkaline by the treatment with the third aqueous solution is neutralized with an acid. As a result, the synergistic effect of these treatments improves the wrinkle resistance, dimensional stability, wash and wear, drape, and sewability of the cellulosic fibrous article.
[0006]
BEST MODE FOR CARRYING OUT THE INVENTION
Examples of the cellulose fiber constituting the cellulose fiber product of the present invention include natural cellulose fibers such as cotton and hemp, regenerated cellulose fibers such as rayon, cupra, and polynosic, and solvent-spun cellulose fibers such as lyocell. Cellulose fiber products include slivers, yarns, woven fabrics, knits, and nonwoven fabrics made from these fibers. The cellulose fiber product of the present invention does not need to be 100% cellulose fiber, but can be blended, blended, or mixed with other fibers, for example, protein fibers such as wool fibers and silk fibers, and chemical fibers such as polyester, acetate, and nylon. Includes knitted textiles. In this case, it contains at least 50% by weight of cellulose fibers.
The first aqueous solution of the present invention has a pH of 5.0 to 8.5, preferably 7.5 to 8.5, containing 0.5 to 3% by weight, preferably 0.8 to 1.5% by weight of ammonium salt. It is an aqueous solution. If the amount of the ammonium salt is less than 0.5% by weight, the effect of penetrating the drug is not sufficiently achieved, and the wettability of the cellulose fiber surface is not improved. On the other hand, if it exceeds 3% by weight, the chemical becomes excessive. Examples of the ammonium salt include ammonium hydrogen carbonate, ammonium carbonate, ammonium hydrogen sulfate, ammonium sulfate, monoammonium phosphate, diammonium phosphate, and triammonium phosphate. These may be used alone or in combination. This first aqueous solution is impregnated with a cellulose fiber product and treated at 30 to 60 ° C, preferably 35 to 50 ° C for 20 to 60 minutes, preferably 20 to 45 minutes. If the processing temperature and the processing time exceed the upper limit values, the processing becomes uneven, and if the processing temperature and the processing time are less than the lower limit values, the processing becomes insufficient.
[0007]
The second aqueous solution of the present invention is an aqueous solution containing 1 to 10% by weight, preferably 1 to 5% by weight of a softening agent and having a pH of 6 to 9, preferably a pH of 7 to 8. If the softener is less than 1% by weight, the tear strength cannot be maintained, and a favorable texture cannot be obtained. If it exceeds 10% by weight, the feeling becomes poor and the sliding resistance decreases. Examples of the softener include a silicone resin, an epoxy silicone resin, and a modified silicone. These may be used alone or in combination.
The third aqueous solution of the present invention has a pH of 9 to 11, containing 10 to 30% by weight, preferably 10 to 20% by weight of a form stabilizer and 1 to 15% by weight, preferably 1 to 6% by weight of an alkaline agent. Preferably, it is an aqueous solution having a pH of 10 to 11. When the amount of the above-mentioned form stabilizer is less than 10% by weight, the form of the cellulose fiber product is not stabilized, and when it exceeds 30% by weight, the chemical becomes excessive. Examples of the form stabilizer include a hydroxyethyl compound and a methoxyethyl compound. When the amount of the alkaline agent is less than 1% by weight, fixation of the agent is insufficient, and when the amount exceeds 15% by weight, the strength is significantly reduced. Examples of the alkaline agent include sodium carbonate, sodium hydroxide, aqueous ammonia, and ammonium hydrogen carbonate. These may be used alone or in combination.
The fourth aqueous solution of the present invention is an aqueous solution containing 0.01 to 1% by weight, preferably 0.05 to 0.2% by weight of acid and having a pH of 0.5 to 4, preferably pH 2 to 3. If the acid is less than 0.5% by weight, the neutralization is insufficient, and if it exceeds 4% by weight, the cellulose fiber product is damaged. Examples of the acid include acetic acid, sulfuric acid, formic acid, and hydrochloric acid. These may be used alone or in combination.
[0008]
【Example】
Next, examples of the present invention will be described together with comparative examples.
<Example 1>
A hemp 100% shirt fabric was prepared. The above shirt was added to a first aqueous solution of pH 8.0 containing 0.5% by weight of an osmotic cleaning scouring agent (Zuyak Co., Ltd. 21-DF-10) and 10 g / l (1.0 g% by weight) of ammonium bicarbonate as an ammonium salt. The ground was impregnated and treated at 40 ° C. for 30 minutes.
Next, 3.0% by weight of a reactive silicone resin emulsion (Tsack Co., Ltd. 40-Q-SI), 1.0% by weight of an epoxy silicone resin (Tsack Co., Ltd. 40-Q-SE), and a penetrating cleaning scouring agent (Tsuk (TM)) 21-DF-10) A second aqueous solution containing 2.0% by weight and having a pH of 7.5 at 20 ° C. was prepared, impregnated with the second aqueous solution for 0.2 minutes, then drained with a mangle, and then returned to 110 ° C. For 5 minutes.
Next, 0.5% by weight of an osmotic cleaning scouring agent (Zyak Corporation 21-DF-10) and 15.0% by weight of a bishydroxyethyl sulfone (Zyak Corporation 40-BS-50) as a form stabilizer were added. The shirt fabric was impregnated with a third aqueous solution containing 4.0% by weight of sodium carbonate and having a pH of 10.5, and treated at 25 ° C. for 30 minutes.
Next, the shirt fabric treated with the third aqueous solution at 160 ° C. for 90 seconds was subjected to dry heat treatment. Further, the dried and heat-treated cellulose fiber product was impregnated with a fourth aqueous solution containing 0.1% by weight of acetic acid, and treated at 40 ° C. for 15 minutes.
[0009]
<Example 2>
The same hemp 100% shirting material as in Example 1 was prepared, and the same first aqueous solution as in Example 1 was impregnated with the shirting material as in Example 1 and treated.
Next, 3.0% by weight of a reactive silicone resin emulsion (Tsack Co., Ltd. 40-Q-SI), 2.0% by weight of an epoxy silicone resin (Tsack Co., Ltd. 40-Q-SE), and a penetrating cleaning scouring agent (Tsack) 21-DF-10) A second aqueous solution containing 2.0% by weight and having a pH of 7.5 at 20 ° C. was prepared, impregnated with the second aqueous solution for 0.2 minutes, and then drained with a mangle. Dry at 5 ° C. for 5 minutes.
Next, the same third aqueous solution as in Example 1 was impregnated with the above-mentioned shirting material in the same manner as in Example 1 and treated. Further, the shirt fabric was subjected to dry heat treatment in the same manner as in Example 1. Further, the shirting material was impregnated and treated in the same manner as in Example 1 in the same fourth aqueous solution as in Example 1.
[0010]
<Example 3>
The same hemp 100% shirting material as in Example 1 was prepared. The above shirt fabric was placed in a first aqueous solution having a pH of 5.4 containing 0.5% by weight of an osmotic cleaning scouring agent (Zuack 21-DF-10) and 10 g / l (1.0 g% by weight) of ammonium sulfate, which is an ammonium salt. Impregnated and treated at 40 ° C. for 30 minutes.
Next, the same second aqueous solution as in Example 1 was prepared, and the shirting material treated with the first aqueous solution containing ammonium sulfate was impregnated with the second aqueous solution in the same manner as in Example 1, and then drained and dried.
Next, the same third aqueous solution as in Example 1 was impregnated with the above-mentioned shirting material in the same manner as in Example 1 and treated. Further, the shirt fabric was heat-treated in the same manner as in Example 1. Further, the shirting material was impregnated and treated in the same manner as in Example 1 in the same fourth aqueous solution as in Example 1.
<Example 4>
The same hemp 100% shirting material as in Example 1 was prepared. The treatment was performed in the same manner as in Example 1 except that the treatment of the first aqueous solution was performed at 30 ° C. for 20 minutes.
[0011]
<Comparative Example 1>
The same hemp 100% shirting material as in Example 1 was prepared. In Example 1, the shirting was treated in the same manner as in Example 1 except that the treatment with the first aqueous solution was not performed, but using the same second aqueous solution, third aqueous solution, dry heat treatment, and fourth aqueous solution as in Example 1, respectively. .
<Comparative Example 2>
The same hemp 100% shirting material as in Example 1 was prepared. In the first embodiment, the shirting was treated in the same manner as in the first embodiment using the same first aqueous solution, third aqueous solution, dry heat treatment, and fourth aqueous solution, respectively, except that the treatment with the second aqueous solution was not performed. .
[0012]
<Example 5>
A 100% cotton shirting fabric was prepared. The above shirt was added to a first aqueous solution of pH 8.0 containing 0.5% by weight of an osmotic cleaning scouring agent (Zuyak Co., Ltd. 21-DF-10) and 10 g / l (1.0 g% by weight) of ammonium bicarbonate as an ammonium salt. And treated at 40 ° C. for 30 minutes.
Next, 3.0% by weight of a reactive silicone resin emulsion (Tsack Co., Ltd. 40-Q-SI), 1.0% by weight of an epoxy silicone resin (Tsack Co., Ltd. 40-Q-SE), and a penetrating cleaning scouring agent (Tsuk (TM)) 21-DF-10) A second aqueous solution containing 2.0% by weight and having a pH of 7.5 at 20 ° C. was prepared, impregnated with the second aqueous solution for 0.2 minutes, then drained with a mangle, and then returned to 110 ° C. For 5 minutes.
Next, 0.5% by weight of an osmotic cleaning scouring agent (Zyak Corporation 21-DF-10) and 15.0% by weight of a bishydroxyethyl sulfone (Zyak Corporation 40-BS-50) as a form stabilizer were added. The shirt fabric was impregnated with a third aqueous solution containing 4.0% by weight of sodium carbonate and having a pH of 10.5, and treated at 25 ° C. for 30 minutes.
Next, the shirt fabric treated with the third aqueous solution at 160 ° C. for 90 seconds was subjected to dry heat treatment. Further, the dried cellulose fiber product was impregnated with a fourth aqueous solution containing 0.1% by weight of acetic acid and treated at 40 ° C. for 15 minutes.
[0013]
<Example 6>
The same 100% cotton shirting material as in Example 5 was prepared, and the same first solution as in Example 5 was impregnated with the above-described shirting material and treated.
Next, 3.0% by weight of a reactive silicone resin emulsion (Tsack Co., Ltd. 40-Q-SI), 2.0% by weight of an epoxy silicone resin (Tsack Co., Ltd. 40-Q-SE), and a penetrating cleaning scouring agent (Tsack) 21-DF-10) A second aqueous solution containing 2.0% by weight and having a pH of 7.5 at 20 ° C. was prepared, impregnated with the second aqueous solution for 0.2 minutes, and then drained with a mangle. Dry at 5 ° C. for 5 minutes.
Next, the same third aqueous solution as in Example 5 was impregnated with the above-mentioned shirting material in the same manner as in Example 5 and treated. Further, the shirt fabric was subjected to dry heat treatment in the same manner as in Example 5. Further, the same fourth aqueous solution as in Example 5 was impregnated with the above-mentioned shirting material and treated in the same manner as in Example 5.
[0014]
<Example 7>
The same 100% cotton shirting fabric as in Example 5 was prepared. The above shirting material was placed in a first aqueous solution having a pH of 5.4 containing 0.5% by weight of an osmotic cleaning scouring agent (Zuack 21-DF-10) and 10 g / l (1.0 g% by weight) of ammonium sulfate as an ammonium salt. Impregnated and treated at 40 ° C. for 30 minutes.
Next, the same second aqueous solution as in Example 5 was prepared, and the shirting material treated with the first aqueous solution containing ammonium sulfate was impregnated with the second aqueous solution in the same manner as in Example 5, then drained and dried.
Next, the third aqueous solution was impregnated with the above-mentioned shirting material and treated in the same manner as in Example 5. Further, the shirt fabric was heat-treated in the same manner as in Example 5. Further, the same fourth aqueous solution as in Example 5 was impregnated with the above-mentioned shirting material and treated in the same manner as in Example 5.
Example 8
The same 100% cotton shirting fabric as in Example 5 was prepared. The same treatment as in Example 5 was performed except that the treatment of the first aqueous solution was performed at 30 ° C. for 20 minutes.
[0015]
<Comparative Example 3>
The same 100% cotton shirting fabric as in Example 5 was prepared. In Example 5, the shirting was treated in the same manner as in Example 5 except that the treatment with the first aqueous solution was not performed, and the same second aqueous solution, third aqueous solution, dry heat treatment, and fourth aqueous solution were used. .
<Comparative Example 4>
The same 100% cotton shirting fabric as in Example 5 was prepared. In Example 5, the shirting was treated in the same manner as in Example 5, except that the treatment with the second aqueous solution was not performed, but using the same first aqueous solution, third aqueous solution, dry heat treatment, and fourth aqueous solution, respectively. .
[0016]
<Evaluation 1>
The shirting materials treated in Examples 1 to 8 and the shirting materials treated in Comparative Examples 1 to 4 were evaluated by a test method (JIS L1059-1998 (Monsanto method)) for examining the respective wrinkle resistance. In this test method, a 15 mm × 40 mm shirt base sample piece is sandwiched between metal sample sandwiches made of two metal pieces, a load of 500 g is applied for 5 minutes, and then the weight is removed. The other end of the sample piece is taken out of the sample piece with one end sandwiched between the sample pieces, and the free end of the sample piece is directed downward, and the opening angle after 5 minutes is divided by 180 to obtain a percentage (wrinkle prevention rate). Table 1 shows the results.
As is clear from Table 1, the wrinkle prevention ratio of the shirting materials of Comparative Examples 1 to 4 which were not treated with the first aqueous solution or the second aqueous solution among the first to fourth aqueous solutions was 31.7 to 45.6%. On the other hand, the shirt fabrics of Examples 1 to 8 which were treated with the first to fourth aqueous solutions had a large wrinkle prevention ratio of 63.5 to 77.8%, and the wrinkle prevention ratio was good.
[0017]
[Table 1]
<Evaluation 2>
The shirting materials treated in Examples 1 to 8 and the shirting materials treated in Comparative Examples 1 to 4 were evaluated by a test method (JIS L1096-1999 8.64 D method) for examining the respective dimensional change rates. In this test method, a piece of shirt base material having a size of about 25 cm × 25 cm is collected, a mark is made at a position of 20 cm × 20 cm, and the sample piece is immersed in a soap aqueous solution at about 50 ° C. for 20 minutes. The sample piece is taken out, washed with warm water of about 50 ° C. for 20 minutes, dehydrated, and naturally dried in a horizontal state. The interval between the marks on the sample piece before immersion and after drying is measured, and the percentage (dimensional change rate) is determined. Table 2 shows the results.
As is clear from Table 2, among the first to fourth aqueous solutions, the dimensional change rates of the shirt fabrics of Comparative Examples 1 to 4 which were not treated with the first aqueous solution or the second aqueous solution were -8.8 to -3. While the shrinkage was as large as 6%, the dimensional change rates of the shirt fabrics of Examples 1 to 8 which were treated with the first to fourth aqueous solutions were as small as -2.2 to -0.3%, which was favorable.
[0019]
[Table 2]
<Evaluation 3>
A test method (JISL1096-1999 8.23.1 A method) for examining the wash-and-wear property of the shirting material treated in Examples 1 to 8 and the shirting material treated in Comparative Examples 1 to 4. Was evaluated. In this test method, a piece of shirt fabric having a size of about 40 cm × 40 cm is collected, the end of the sample piece is subjected to fraying prevention, a mark is provided at a predetermined position, and then a washing machine is used with warm water of about 40 ° C. And wash. Without dehydrating the sample piece, grasp several places so that the vertical direction is vertical, and hang and dry at room temperature in a place without ventilation. The interval between marks on the sample piece before and after washing is measured, and the percentage (dimensional change rate) is determined. Table 3 shows the results. As is clear from Table 3, among the first to fourth aqueous solutions, the evaluation of wrinkles after washing of the shirt fabrics of Comparative Examples 1 to 4 which were not treated with the first aqueous solution or the second aqueous solution was 2.0 to 2. The wrinkle evaluation after washing of the shirting fabrics of Examples 1 to 8 treated with the first to fourth aqueous solutions was as high as 3.0 to 3.8, whereas the grade was as low as 0.5. It was found that the shirting materials of Examples 1 to 8 had high wash and wear properties.
[0021]
[Table 3]
<Evaluation 4>
The wool mark test method for examining the wash-and-wear property of the shirt fabrics treated in Examples 1 to 8 and the shirt fabrics treated in Comparative Examples 1 to 4 was performed. 281 (IWS TM281). In this test method, a fabric sample having a size of 500 × 500 mm is collected, the end of the sample is subjected to fraying prevention, a mark is provided at a predetermined position, and the sample is washed in a washing machine with warm water of 40 ° C. ± 3 ° C. . After 3 cycles of washing, it was dried. After ironing the dried shirting, the smoothness of the shirting was examined by comparing it to a picture for smoothness of the appropriate fabric. Table 4 shows the results.
As is clear from Table 4, among the first to fourth aqueous solutions, the smoothness of the shirting after washing of the shirting of Comparative Examples 1 to 4 which was not treated with the first aqueous solution or the second aqueous solution was 2 In contrast to the low grade, the evaluation of the smoothness of the shirting after the washing of the shirting of Examples 1 to 8 treated with the first to fourth aqueous solutions was as high as 3 to 3-4 grade. It became.
[0023]
[Table 4]
【The invention's effect】
As described above, according to the treatment method of the present invention, the first aqueous solution containing an ammonium salt improves the wettability of the surface of the cellulose fiber, promotes the activation of the end group of the side chain, and contains a softener. The second aqueous solution softens the cellulose fiber and suppresses the strength reduction, and the third aqueous solution containing the form stabilizer and the alkali agent modifies the amorphous region of the cellulose and increases the pseudocrystalline region, thereby increasing the cellulose fiber. The product can be easily provided with wrinkle resistance, dimensional stability, wash and wear, drape, and sewability without causing a decrease in strength or discoloration and without remaining formalin.
Claims (6)
前記第１水溶液に含浸したセルロース繊維品を１〜１０重量％の柔軟剤を含むｐＨ６〜９の第２水溶液に含浸する工程と、
前記第２水溶液に含浸したセルロース繊維品を１０〜３０重量％の形態安定化剤と１〜１５重量％のアルカリ剤を含むｐＨ９〜１１の第３水溶液に含浸する工程と、
前記第３水溶液に含浸したセルロース繊維品を１４０〜１８０℃で４５〜１８０秒間乾熱処理する工程と、
前記乾熱処理したセルロース繊維品を０．０１〜１重量％の酸を含むｐＨ０．５〜４の第４水溶液に含浸する工程と
を含むセルロース繊維品の処理方法。Impregnating the cellulose fiber product with a first aqueous solution having a pH of 5.0 to 8.5 containing 0.5 to 3% by weight of an ammonium salt at 30 to 60 ° C. for 20 to 60 minutes;
Impregnating the cellulose fiber product impregnated with the first aqueous solution with a second aqueous solution having a pH of 6 to 9 and containing 1 to 10% by weight of a softener;
Impregnating the cellulose fiber product impregnated with the second aqueous solution with a third aqueous solution having a pH of 9 to 11 and containing 10 to 30% by weight of a form stabilizer and 1 to 15% by weight of an alkaline agent;
Performing a dry heat treatment on the cellulose fiber product impregnated with the third aqueous solution at 140 to 180 ° C. for 45 to 180 seconds;
Impregnating the dried and heat-treated cellulose fiber article with a fourth aqueous solution having a pH of 0.5 to 4 and containing 0.01 to 1% by weight of an acid.
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