JP6540914B1 - 手袋の製造方法 - Google Patents
手袋の製造方法 Download PDFInfo
- Publication number
- JP6540914B1 JP6540914B1 JP2018557955A JP2018557955A JP6540914B1 JP 6540914 B1 JP6540914 B1 JP 6540914B1 JP 2018557955 A JP2018557955 A JP 2018557955A JP 2018557955 A JP2018557955 A JP 2018557955A JP 6540914 B1 JP6540914 B1 JP 6540914B1
- Authority
- JP
- Japan
- Prior art keywords
- urethane resin
- aqueous
- thickener
- mass
- glove
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/155—Halides of elements of Groups 2 or 12 of the Periodic Table
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Abstract
Description
温度計、窒素ガス、導入管、及び撹拌機を備えた窒素置換された容器中で、ポリテトラメチレンエーテルグリコール(数平均分子量;2000)500質量部、2,2’−ジメチロールプロピオン酸(以下「DMPA」と略記する。)25質量部、ジシクロヘキシルメタンジイソシアネート(以下「H12MDI」と略記する。)128質量部、及びメチルエチルケトン620質量部の存在下、反応物の規定のNCO%に達する時点まで70℃で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。
次いで、前記ウレタンプレポリマーの有機溶剤溶液に、中和剤としてトリエチルアミン23質量部加えて攪拌し、更に水830質量部加え撹拌することにより、前記ウレタンプレポリマーが水に分散した乳化液を得た。
得られた乳化液とヒドラジン2.6質量部を含む鎖伸長剤水溶液3.2質量部とを混合し鎖伸長反応することによってウレタン樹脂(A−1)の水分散体を得た。次いで、この水分散体を脱溶剤することにより、不揮発分;30質量%の水性ウレタン樹脂組成物(X−1)を得た。
温度計、窒素ガス、導入管、及び撹拌機を備えた窒素置換された容器中で、ポリカーボネートジオール(宇部興産株式会社製「エタナコールUH−200」、数平均分子量;2000)250質量部、DMPA18質量部、H12MDI90質量部、及びメチルエチルケトン236質量部の存在下、反応物の規定のNCO%に達する時点まで70℃で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。
次いで、前記ウレタンプレポリマーの有機溶剤溶液に、中和剤としてトリエチルアミン16質量部加えて攪拌し、更に水797質量部加え撹拌することにより、前記ウレタンプレポリマーが水に分散した乳化液を得た。
得られた乳化液とヒドラジン5.0質量部を含む鎖伸長剤水溶液6.3質量部とを混合し鎖伸長反応することによってウレタン樹脂(A−2)の水分散体を得た。次いで、この水分散体を脱溶剤することにより、不揮発分;35質量%の水性ウレタン樹脂組成物(X−2)を得た。
温度計、窒素ガス、導入管、及び撹拌機を備えた窒素置換された容器中で、1,6−ヘキサンジオール(以下「HG」と略記する。)155質量部、ネオペンチルグリコール137質量部、アジピン酸424質量部添加し、120℃でそれらを溶融した。次いで、撹拌しながら3時間〜4時間かけて220℃へ昇温し5時間保持した後、150℃まで冷却した後、DMPAを88質量部添加し、150℃で撹拌しながら5時間〜10時間保持した後、メチルエチルケトン300質量部添加することによって、不揮発分70量%のカルボキシル基を有するポリエステルポリオールのメチルエチルケトン溶液(X−3−a)を調製した。
温度計、窒素ガス、導入管、及び撹拌機を備えた窒素置換された容器中で、上記カルボキシル基を有するポリエステルポリオール(X−3−a)のメチルエチルケトン溶液198質量部、ポリエステルポリオール(DIC株式会社製「クリスボンCMA−654」、数平均分子量;1,500)160質量部、HG19質量部、トリレンジイソシアネート75質量部、及びメチルエチルケトン152質量部の存在下、反応物の規定のNCO%に達する時点まで70℃で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。
次いで、ウレタンプレポリマーの有機溶剤溶液に、中和剤としてトリエチルアミン17.2質量部加えて攪拌し、更に水を653質量部、ピペラジン7.7質量部を加え混合し鎖伸長反応することによってウレタン樹脂(A−3)の水分散体を得た。次いで、この水分散体を脱溶剤することにより、不揮発分;40質量%の水性ウレタン樹脂組成物(X−3)を得た。
温度計、窒素ガス、導入管、及び撹拌機を備えた窒素置換された容器中で、ポリテトラメチレングリコール(三菱化学株式会社製、数平均分子量:2,000)1,000質量部、日油株式会社製「ユニルーブ75DE−60」(ポリオキシエチレンオキシプロピレングリコール、ポリオキシエチレン構造/ポリオキシプロピレン構造(質量割合)=75/25、数平均分子量:約3,000)50質量部、日油株式会社製「ユニルーブ75MB−900」(ポリオキシエチレンオキシプロピレングリコールモノブチルエーテル、ポリオキシエチレン構造/ポリオキシプロピレン構造(質量割合)=75/25、数平均分子量約3,400)50質量部、H12MDI183質量部、及びメチルエチルケトン1,283質量部の存在下、反応物の規定のNCO%に達する時点まで70℃で反応させることによって、末端にイソシアネート基を有するウレタンプレポリマーのメチルエチルケトン溶液を得た。
次いで、ウレタンプレポリマーの有機溶剤溶液に、水を2,566質量部加え撹拌することにより、水性ウレタン樹脂の水分散体を得た。得られた乳化液と、ピペラジン13.5質量部を含む鎖伸長剤水溶液135質量部とを混合し鎖伸長反応することによってウレタン樹脂(A’−1)の水分散体を得た。次いで、この水分散体を脱溶剤することにより、不揮発分;40質量%の水性ウレタン樹脂組成物(X’−1)を得た。
水性ウレタン樹脂組成物(X−1)100質量部に、水で10質量%に希釈したカルボキシメチルセルロース(第一工業製薬株式会社製「セロゲンWS−C」、以下「CMC」と略記する。)6.3質量部をメカニカルミキサーにて800rpmで10分間撹拌し、次いで遠心脱泡器を使用して脱泡させて配合液を作製した。前記配合液(増粘剤を含む水性ウレタン樹脂組成物)の粘度は、2,600mPa・sであった。
手型にナイロン繊維による編み手袋を装着し、5質量%の硝酸カルシウム水溶液中に3分間浸漬させた後、引きあげた。次いで、前記増粘させた配合液中に繊維編み手袋を30秒浸漬させ、ウレタン樹脂の凝固皮膜を形成させた後に引き上げた。その後、該手型を水に60分間浸漬させ引きあげた。次いで、該手型を70℃で20分間乾燥し、連続して120℃で30分間乾燥させた。次いで、手型から編み手袋を取り出し、皮膜を有する手袋を得た。
用いる水性ウレタン樹脂組成物の種類、増粘剤(B)の種類、及び量を表1〜3に示す通りに変更した以外は、実施例1と同様にして手袋を作製した。
調整例で使用したポリオールの数平均分子量は、ゲル・パーミエーション・クロマトグラフィー(GPC)法により、下記の条件で測定した値を示す。
カラム:東ソー株式会社製の下記のカラムを直列に接続して使用した。
「TSKgel G5000」(7.8mmI.D.×30cm)×1本
「TSKgel G4000」(7.8mmI.D.×30cm)×1本
「TSKgel G3000」(7.8mmI.D.×30cm)×1本
「TSKgel G2000」(7.8mmI.D.×30cm)×1本
検出器:RI(示差屈折計)
カラム温度:40℃
溶離液:テトラヒドロフラン(THF)
流速:1.0mL/分
注入量:100μL(試料濃度0.4質量%のテトラヒドロフラン溶液)
標準試料:下記の標準ポリスチレンを用いて検量線を作成した。
東ソー株式会社製「TSKgel 標準ポリスチレン A−500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−1000」
東ソー株式会社製「TSKgel 標準ポリスチレン A−2500」
東ソー株式会社製「TSKgel 標準ポリスチレン A−5000」
東ソー株式会社製「TSKgel 標準ポリスチレン F−1」
東ソー株式会社製「TSKgel 標準ポリスチレン F−2」
東ソー株式会社製「TSKgel 標準ポリスチレン F−4」
東ソー株式会社製「TSKgel 標準ポリスチレン F−10」
東ソー株式会社製「TSKgel 標準ポリスチレン F−20」
東ソー株式会社製「TSKgel 標準ポリスチレン F−40」
東ソー株式会社製「TSKgel 標準ポリスチレン F−80」
東ソー株式会社製「TSKgel 標準ポリスチレン F−128」
東ソー株式会社製「TSKgel 標準ポリスチレン F−288」
東ソー株式会社製「TSKgel 標準ポリスチレン F−550」
調製例にて得た水性ウレタン樹脂組成物をレーザー回折/散乱式粒度分布測定装置(株式会社堀場製作所製「LA−910」)を使用して、分散液として水を使用し、相対屈折率=1.10、粒子径基準が面積の時の平均粒子径を測定した。
調整例にて得た水性ウレタン樹脂組成物を乾燥し、乾燥固化した樹脂粒子の0.05g〜0.5gを、300mL三角フラスコに秤量し、次いで、テトラヒドロフランとイオン交換水との質量割合[テトラヒドロフラン/イオン交換水]が80/20の混合溶媒約80mLを加えそれらの混合液を得た。
次いで、前記混合液にフェノールフタレイン指示薬を混合した後、あらかじめ標定された0.1mol/Lの水酸化カリウム水溶液で滴定し、滴定に用いた水酸化カリウム水溶液の量から下記計算式(2)に従い、水性ウレタン樹脂(A)の酸価(mgKOH/g)を求めた。
計算式 A=(B×f×5.611)/S (2)
式中、Aは樹脂の固形分酸価(mgKOH/g)、Bは滴定に用いた0.1mol/L水酸化カリウム水溶液の量(mL)、fは0.1mol/L水酸化カリウム水溶液のファクター、Sは樹脂粒子の質量(g)、5.611は水酸化カリウムの式量(56.11/10)である。
実施例及び比較例で得られた手袋を、日立ハイテクテクノロジー株式会社製走査型電子顕微鏡「SU3500」(倍率:2,000倍)を使用して観察し、以下のように評価した。
「A」;電子顕微鏡写真の手袋の断面図において、縦長状のセルが多数確認される。
「B」;電子顕微鏡写真の手袋の断面図において、孔が多数確認される。
「C」;上記以外のもの。
実施例及び比較例で得られた手袋を手に装着し、指を曲げ伸ばしたときの感触により以下のように評価した。なお、樹脂が凝固しなかったものは、柔軟性の評価ができなかったため、「−」とした。
「A」;ソフト感、指の動かしやすさ共に優れている。
「B」;ソフト感、指の動かしやすさが感じられる。
「C」;ソフト感、指の動かしやすさがやや劣る。
「D」;ソフト感、指の動かしやすさが全く感じられない。
実施例及び比較例で得られた手袋を手に装着し、机(メラニン化粧板)をこすった時の感触により以下のように評価した。なお、樹脂が凝固しなかったものは、グリップ性の評価ができなかったため、「−」とした。
「A」;グリップ感に優れている。
「B」;グリップ感が感じられる。
「C」;グリップ感がやや劣る。
「D」;グリップ感が全く感じられない。
・「ALA」:Borcher社製「Borch Gel ALA」、ポリアクリル酸のナトリウム塩
・「MC」:メチルセルロース
・「L75N」:Borchers社「Borch Gel L75N」(1,6−ヘキサンジイソシアネート、数平均分子量が3,000のポリエチレングリコール及び数平均分子量が6,000のポリエチレングリコールの反応物と、ポリオキシエチレンジスチレン化フェニルエーテルと、アセチレングリコールと、水(含有率:50質量%)とを含むもの、オキシエチレン基の含有量:1.6×10−2mol/g)
・「T10」:DIC株式会社製「アシスター T10」(1,6−ヘキサンジイソシアネート及び数平均分子量が6,000のポリエチレングリコールの反応物と、ポリオキシエチレンジスチレン化フェニルエーテルと、水(含有率:75質量%)とを含むもの、オキシエチレン基の含有量:2.1×10−2mol/g)
Claims (3)
- 酸価が0.01mgKOH/g以上の水性ウレタン樹脂(A)を含む水性ウレタン樹脂組成物に、
オキシエチレン基の含有量が2×10−2mol/g以下の増粘剤(B)を、
前記水性ウレタン樹脂(A)100質量部に対して0.01〜30質量部の範囲で加えて、400mPa・s以上の粘度に増粘させた液を得た後、
(i)増粘させた液に繊維編み手袋を浸漬させ、次いで、金属塩(c−1)を含む凝固浴(C)で凝固する、又は、
(ii)あらかじめ金属塩(c−1)を含む凝固浴(C)に浸漬させた繊維編み手袋を、増粘させた液に浸漬させ凝固する
ものであり、前記水性ウレタン樹脂(A)の凝固の際に、加熱工程を経ないことを特徴とする手袋の製造方法。 - 前記増粘剤(B)が、セルロース増粘剤、アクリル増粘剤、及び、ウレタン増粘剤からなる群より選ばれる1種以上である請求項1記載の手袋の製造方法。
- 前記金属塩(c−1)が、硝酸カルシウムである請求項1又は2記載の手袋の製造方法。
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