TW202200866A - 凝固物的製造方法 - Google Patents
凝固物的製造方法 Download PDFInfo
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- TW202200866A TW202200866A TW110115651A TW110115651A TW202200866A TW 202200866 A TW202200866 A TW 202200866A TW 110115651 A TW110115651 A TW 110115651A TW 110115651 A TW110115651 A TW 110115651A TW 202200866 A TW202200866 A TW 202200866A
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- urethane resin
- compound
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- aqueous
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Classifications
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Abstract
本發明提供一種凝固物的製造方法,其特徵在於,使以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂(X)的水分散體含浸於纖維基材,繼而,浸漬於凝固劑(Y)中。於構成胺基甲酸酯樹脂(X)的原料的合計質量中,所述具有非離子性基的化合物(a1)的使用率較佳為5質量%以下。所述凝固劑(Y)較佳為選自由金屬化合物(Y1)、酸化合物(Y2)、及除所述酸化合物(Y2)以外的非金屬合物(Y3)所組成的群組中的一種以上。根據本發明的製造方法,可獲得手感、耐鹼性及耐染色性優異的凝固物。
Description
本發明是有關於一種凝固物的製造方法。
胺基甲酸酯樹脂由於其機械強度及手感良好,廣泛用於合成皮革(包括人工皮革)、塗佈劑、接著劑、手套、衣料等的製造。所述胺基甲酸酯樹脂中,迄今為止,含有N,N-二甲基甲醯胺(dimethyl formamide,DMF)的溶劑系胺基甲酸酯樹脂為主流。然而,以歐洲的DMF限制、中國或台灣的揮發性有機化合物(volatile organic compounds,VOC)排出限制的強化、大型服裝製造企業的DMF限制等為背景,謀求基於弱溶劑化、水系化、無溶劑化等的環境和諧對策。
於此種環境下,胺基甲酸酯樹脂分散於水中而成的胺基甲酸酯樹脂水分散體(聚胺基甲酸酯分散體(dispersion))開始用於所述用途中。然而,與先前的溶劑系胺基甲酸酯樹脂不同,於所述胺基甲酸酯樹脂水分散體的情況下,於使其含浸於纖維基材中的情況下,由於向纖維基材內部的填充狀態並非多孔,或者於乾燥步驟中胺基甲酸酯樹脂偏析(遷移(migration))到纖維基材的表面,存在不均勻且手感變差的缺點。
另外,作為於所述用途中進行脫溶劑化的方法,為了使胺基甲酸酯樹脂含浸於微小的纖維間隔,開發了低黏度的胺基甲酸酯樹脂水分散體,或為了使胺基甲酸酯樹脂均勻地凝固,開發了賦予了感熱凝固性的胺基甲酸酯樹脂水分散體(例如,參照專利文獻1)。然而,已經指出於所述胺基甲酸酯樹脂水分散體中,胺基甲酸酯樹脂液的黏度於感熱凝固的中途暫時降低,胺基甲酸酯樹脂附著限制於纖維的交織點,因此加工品的手感會變得不良。因此,需要利用特殊的海島結構纖維不織布進行加工,含浸加工後需要纖維海部分的鹼溶解提取步驟,但已經指出由於鹼提取步驟的提取條件因加工量、使用纖維而各不相同,因此容易變得提取不充分,於實際生產線上產生手感不良或殘留海部所致的染色不良的問題。
[現有技術文獻]
[專利文獻]
[專利文獻1]日本專利特開2016-84463號公報
[發明所欲解決之課題]
本發明所欲解決的課題在於提供一種製造手感、耐鹼性及耐染色性優異的凝固物的方法。
[解決課題之手段]
本發明提供一種凝固物的製造方法,其特徵在於,使以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂(X)的水分散體含浸於纖維基材,繼而,浸漬於凝固劑(Y)中。
[發明的效果]
根據本發明的製造方法,可獲得手感、耐鹼性及耐染色性優異的凝固物。
本發明的凝固物的製造方法是使以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂(X)的水分散體含浸於纖維基材,繼而,浸漬於凝固劑(Y)中。
作為所述纖維基材,例如例如可使用聚酯纖維、聚乙烯纖維、尼龍纖維、丙烯酸纖維、聚胺基甲酸酯纖維、乙酸酯纖維、嫘縈纖維、聚乳酸纖維、棉、麻、絹、羊毛、玻璃纖維(glass fiber)、碳纖維、由該些的混紡纖維等所形成的不織布、織布、編織物等的纖維基材;使聚胺基甲酸酯樹脂等樹脂含浸於所述不織布中而成者;於所述不織布進而設置多孔質層者;熱塑性胺基甲酸酯(thermoplastic urethane,TPU)等樹脂基材等。
本發明中,作為所述胺基甲酸酯樹脂(X),必須使用以具有非離子性基的化合物(a1)為原料的所謂的非離子性胺基甲酸酯樹脂。作為所述胺基甲酸酯樹脂(X),較佳為不含陽離子性基及陰離子性基,藉此可獲得具有更優異的耐鹼性及耐染色性的凝固物。
作為所述具有非離子性基的化合物(a1),例如可列舉具有氧乙烯結構的化合物,例如可使用聚乙二醇、聚氧乙烯聚氧丙烯二醇、聚氧乙烯聚氧四亞甲基二醇、聚乙二醇二甲醚等具有氧乙烯結構的聚醚多元醇。該些化合物既可單獨使用亦可併用兩種以上。該些中,就可更簡便地控制親水性並且可獲得更優異的耐鹼性及耐染色性的方面而言,較佳為使用選自由聚乙二醇、聚氧乙烯聚氧丙烯二醇、及聚乙二醇二甲醚所組成的群組中的一種以上的化合物,特佳為聚乙二醇。
作為所述具有非離子性基的化合物(a1)的數量平均分子量,就可獲得更優異的耐鹼性、耐染色性、乳化性及水分散穩定性的方面而言,較佳為200~10,000的範圍,更佳為300~3,000的範圍,更佳為300~2,000的範圍。再者,所述具有非離子性基的化合物(a1)的數量平均分子量表示藉由凝膠滲透管柱層析(gel permeation chromatography,GPC)法測定的值。
作為所述具有非離子性基的化合物(a1)的使用比例,就可獲得更優異的耐鹼性、耐染色性、乳化性及水分散穩定性的方面而言,於構成胺基甲酸酯樹脂(X)的原料的合計質量中,較佳為5質量%以下,更佳為4質量%以下,進而佳為0.25質量%~3.5質量%的範圍,特佳為0.5質量%~3質量%的範圍。
作為所述胺基甲酸酯樹脂(X),具體而言,例如可使用具有非離子性基的化合物(a1)、鏈伸長劑(a2)、多元醇(a3)、與聚異氰酸酯(a4)的反應產物。
作為所述鏈伸長劑(a2),可使用分子量小於500(較佳為50~450的範圍)者,具體而言,可使用:乙二醇、二乙二醇、三乙二醇、丙二醇、二丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、六亞甲基二醇、蔗糖、亞甲基二醇、甘油、山梨糖醇、雙酚A、4,4'-二羥基聯苯、4,4'-二羥基二苯基醚、三羥甲基丙烷等具有羥基的鏈伸長劑;乙二胺、1,2-丙二胺、1,6-六亞甲基二胺、哌嗪、2,5-二甲基哌嗪、異佛爾酮二胺、1,2-環己烷二胺、1,3-環己烷二胺、1,4-環己烷二胺、4,4'-二環己基甲烷二胺、3,3'-二甲基-4,4'-二環己基甲烷二胺、1,4-環己烷二胺、肼等具有胺基的鏈伸長劑等。該些鏈伸長劑既可單獨使用亦可併用兩種以上。再者,所述鏈伸長劑(a2)的分子量表示根據化學式算出的值。
作為所述鏈伸長劑(a2),就即使於30℃以下的比較低的溫度下亦可容易進行鏈伸長且可抑制反應時的能量消耗的方面、及藉由導入脲基而可獲得更優異的機械強度、造膜性、手感及剝離強度的方面而言,較佳為使用具有胺基的鏈伸長劑(以下,簡稱為「胺系鏈伸長劑」),就即使將胺基甲酸酯樹脂(X)高固體成分化亦可獲得更優異的乳化性、及水分散穩定性的方面而言,更佳為使用分子量為30~250的範圍的胺系鏈伸長劑。再者,於併用兩種以上來作為所述鏈伸長劑的情況下,所述分子量表示其平均值,只要平均值包含於所述較佳的分子量的範圍內即可。
作為所述鏈伸長劑(a2)的使用比例,就可獲得更優異的機械強度、造膜性、手感、剝離強度、乳化性、水分散穩定性的方面;胺基甲酸酯樹脂(X)的高固體成分化變得更容易的方面而言,於構成胺基甲酸酯樹脂(X)的原料的合成質量中,進而佳為0.1質量%~30質量%的範圍,特佳為0.5質量%~10質量%的範圍。
作為所述多元醇(a3),例如可使用所述具有非離子性基的化合物(a1)以外的聚醚多元醇、聚酯多元醇、聚丙烯酸多元醇、聚碳酸酯多元醇、聚丁二烯多元醇等。該些多元醇既可單獨使用亦可併用兩種以上。
作為所述多元醇(a3)的數量平均分子量,就所獲得的皮膜的機械強度的方面而言,較佳為500~100,000的範圍,更佳為800~10,000的範圍。再者,所述多元醇(a3)的數量平均分子量表示藉由凝膠滲透管柱層析(GPC)法測定的值。
作為所述多元醇(a3)的使用比例,就可獲得更優異的機械強度的方面而言,於構成胺基甲酸酯樹脂(X)的原料的合計質量中,進而佳為40質量%~90質量%的範圍,特佳為50質量%~80質量%的範圍。
作為所述聚異氰酸酯(a4),例如可使用:苯二異氰酸酯、甲苯二異氰酸酯、二苯基甲烷二異氰酸酯、苯二甲基二異氰酸酯、萘二異氰酸酯、聚亞甲基聚苯基聚異氰酸酯、碳二醯亞胺化二苯基甲烷聚異氰酸酯等芳香族聚異氰酸酯;六亞甲基二異氰酸酯、離胺酸二異氰酸酯、環己烷二異氰酸酯、異佛爾酮二異氰酸酯、二環己基甲烷二異氰酸酯、苯二甲基二異氰酸酯、四甲基苯二甲基二異氰酸酯、二聚酸二異氰酸酯、降冰片烯二異氰酸酯等脂肪族聚異氰酸酯或脂環式聚異氰酸酯等。該些聚異氰酸酯既可單獨使用亦可併用兩種以上。
作為所述聚異氰酸酯(a4)的使用比例,就可獲得更優異的機械強度的方面而言,於構成胺基甲酸酯樹脂(X)的原料的合計質量中,進而佳為5質量%~40質量%的範圍,特佳為10質量%~35質量%的範圍。
作為所述胺基甲酸酯樹脂(X)的平均粒徑,就可獲得更優異的手感、水分散穩定性及造膜性的方面而言,較佳為0.01 μm~1 μm的範圍,更佳為0.05 μm~0.9 μm的範圍。再者,所述胺基甲酸酯樹脂(X)的平均粒徑的測定方法於後述的實施例中進行記載。
接下來,對本發明中使用的胺基甲酸酯樹脂水分散體的製造方法進行說明。
作為本發明中使用的胺基甲酸酯樹脂水分散體的製造方法,較佳為具有如下步驟:使所述具有非離子性基的化合物(a1)、所述多元醇(a3)及所述聚異氰酸酯(a4)於無溶媒下反應而獲得具有異氰酸酯基的胺基甲酸酯預聚物(i)(以下,簡稱為「預聚物步驟」),接著,使胺基甲酸酯預聚物(i)分散於所述水中(以下簡稱為「乳化步驟」),其後使所述鏈伸長劑(a2)反應而獲得胺基甲酸酯樹脂(X)的步驟(以下,簡稱為「鏈伸長步驟」)。
關於所述預聚物步驟,重要的是於無溶媒下進行。於現有技術中,於進行預聚物步驟時,一般於甲基乙基酮、丙酮等有機溶媒中進行,但於乳化步驟後需要餾去所述有機溶劑的脫溶劑步驟,於實際生產現場需要數天的生產天數。另外,於所述脫溶劑步驟中亦難以完全餾去有機溶劑,大多數情況下殘留有稍許的有機溶劑,對於環境應對而言難以完全應對。另一方面,於本發明的製造方法中,藉由於無溶媒下進行所述預聚物步驟,可獲得完全不含有機溶劑的胺基甲酸酯樹脂水分散體,且其生產步驟亦能夠實現省力化。
作為所述預聚物步驟中的、所述具有非離子性基的化合物(a1)及所述多元醇(a3)所具有的羥基的合計與所述聚異氰酸酯(a4)所具有的異氰酸酯基的莫耳比[異氰酸酯基/(羥基)],就可獲得更優異的表面平滑性、造膜性、手感、剝離強度、耐鹼性、耐染色性及機械強度的方面而言,較佳為1.1~3的範圍,更佳為1.2~2的範圍。
所述預聚物步驟的反應例如可列舉於50℃~120℃下進行1小時~10小時。
所述預聚物步驟可藉由使用:包括攪拌翼的反應釜;捏合機、連續式捏合機、錐形輥、單軸擠出機、雙軸擠出機、三軸擠出機、萬能混合機、塑磨機(Plastomill)、旋渦型混煉機等混煉機;TK均質混合機、菲爾米克斯(Filmix)、伊巴拉米爾德(Ebaramilder)、庫萊爾米克斯(Clearmix)、高速攪拌器(Ultra-turrax)、卡維特龍(Cavitron)、生物混合機(Biomixer)等旋轉式分散混合機;超音波式分散裝置;在線混合機(inline mixer)等的無可動部而可藉由流體自身的流動進行混合的裝置等來進行。
所述乳化步驟較佳為於水未蒸發的溫度下進行,例如可列舉10℃~90℃的範圍,所述乳化步驟可使用與所述預聚物步驟同樣的設備進行。其中,就可簡便地獲得胺基甲酸酯樹脂的含有率高的胺基甲酸酯樹脂水分散體的方面而言,較佳為使用混煉機,更佳為雙軸擠出機。
另外,作為所述乳化步驟前的所述預聚物於100℃下的黏度,就可獲得更優異的手感、耐久性的方面而言,較佳為100 mPa·s~100,00,000 mPa·s的範圍,較佳為1,000 mPa·s~1,000,000 mPa·s的範圍。再者,所述預聚物的黏度表示使用安東帕(ANTON-PAAR)公司製造的「MCR302」,於軸:平行板夾具(d=0.94 mm)、頻率:1 Hz的條件下測定的值。
所述鏈伸長步驟是藉由所述胺基甲酸酯預聚物(i)所具有的異氰酸酯基與所述鏈伸長劑(a1)的反應而使胺基甲酸酯預聚物(i)高分子量化從而獲得胺基甲酸酯樹脂(X)的步驟。作為所述鏈伸長步驟時的溫度,就生產性的方面而言,較佳為於50℃以下進行。
作為所述鏈伸長步驟中的、所述胺基甲酸酯預聚物(i)所具有的異氰酸酯基與所述鏈伸長劑(a1)所具有的羥基及胺基的合計的莫耳比[(羥基及胺基)/異氰酸酯基],就可獲得更優異的耐鹼性、耐染色性、造膜性及機械強度的方面而言,較佳為0.8~1.1的範圍,更佳為0.9~1的範圍。
所述鏈伸長步驟可使用與所述預聚物步驟同樣的設備進行。
作為本發明中使用的胺基甲酸酯樹脂水分散體中的所述胺基甲酸酯樹脂(X)的含有率,其製造時較佳為50質量%~80質量%的範圍。如此,藉由水分散體中的所謂的胺基甲酸酯樹脂(X)固體成分高,胺基甲酸酯樹脂水分散體的乾燥性提高,因此可獲得更優異的手感、耐樹脂脫落、耐鹼性及耐染色性。但是,製造後,亦可進而於水中稀釋。
作為本發明中使用的水,可使用離子交換水、蒸餾水等。該些水既可單獨使用亦可併用兩種以上。
本發明中使用的胺基甲酸酯樹脂水分散體含有所述胺基甲酸酯樹脂(X)及所述水作為必需成分,但視需要亦可含有其他添加劑。
作為所述其他添加劑,例如可使用:乳化劑、交聯劑、中和劑、增黏劑、胺基甲酸酯化觸媒、填充劑、顏料、染料、阻燃劑、調平劑、抗結塊劑、成膜助劑、發泡劑等。該些添加劑既可單獨使用亦可併用兩種以上。該些添加劑根據使用發泡片材的目的來適當決定。再者,本發明中使用的胺基甲酸酯樹脂水分散體於其製造步驟中不含有機溶劑,但作為所述添加劑,允許包含有機溶劑。該些中,於獲得更優異的乳化性及水分散穩定性的基礎上,較佳為使用乳化劑。
作為所述乳化劑,例如可使用:聚氧乙烯壬基苯基醚、聚氧乙烯月桂基醚、聚氧乙烯苯乙烯基苯基醚、聚氧乙烯山梨糖醇四油酸酯、聚乙烯-聚丙烯共聚物等非離子性乳化劑;油酸鈉等脂肪酸鹽、烷基硫酸酯鹽、烷基苯磺酸鹽、烷基磺基琥珀酸鹽、萘磺酸鹽、聚氧乙烯烷基硫酸鹽、烷烴磺酸鈉鹽、烷基二苯醚磺酸鈉鹽等陰離子性乳化劑;烷基胺鹽、烷基三甲基銨鹽、烷基二甲基苄基銨鹽等陽離子性乳化劑等。該些乳化劑既可單獨使用亦可併用兩種以上。該些中,就可進一步停電胺基甲酸酯樹脂向纖維基材的樹脂脫落的方面而言,較佳為使用陰離子性乳化劑。
作為所述乳化劑的使用量,就可獲得更優異的樹脂脫落的減少、耐鹼性及耐染色性的方面而言,相對於胺基甲酸酯樹脂(X)(=固體成分)100質量份,較佳為7質量份以下,更佳為0質量%~5質量%的範圍。
所述凝固劑(Y)是將胺基甲酸酯樹脂(X)凝固而成,例如可使用金屬化合物(Y1)、酸化合物(Y2)、所述酸化合物(Y2)以外的非金屬化合物(Y3)等。
作為所述金屬化合物(Y1),例如可使用:氯化鈣、乙酸鎂、氯化鈉等一價金屬化合物;硝酸鈣、硝酸鋅、氯化鋅、硫酸鋁等多價金屬化合物等。該些化合物既可單獨使用亦可併用兩種以上。
作為所述酸化合物(Y2),例如可使用:琥珀酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、富馬酸、馬來酸、庚二酸、辛二酸、壬二酸、癸二酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、酒石酸、檸檬酸、鳥頭酸、麩胺酸、天冬胺酸等。該些酸既可單獨使用亦可併用兩種以上。
作為所述非金屬化合物(Y3),例如可使用:氯化銨、四甲基氯化銨、四乙基氯化銨、四丙基氯化銨、四丁基氯化銨、四己基氯化銨、四辛基氯化銨、四苯基氯化銨、三乙基甲基氯化銨、三乙基己基氯化銨、三辛基甲基氯化銨、三辛基丁基氯化銨、三辛基苄基氯化銨、三甲基苄基氯化銨、三丁基苄基氯化銨、三苯基異丁基氯化銨、三苯基苄基氯化銨、溴化銨、四甲基溴化銨、四乙基溴化銨、四丙基溴化銨、四丁基溴化銨、四己基溴化銨、四辛基溴化銨、四苯基溴化銨、三乙基甲基溴化銨、三乙基己基溴化銨、三辛基甲基溴化銨、三辛基丁基溴化銨、三辛基苄基溴化銨、三甲基苄基溴化銨、三丁基苄基溴化銨、三苯基異丁基溴化銨、三苯基苄基溴化銨、碘化銨、四甲基碘化銨、四乙基碘化銨、四丙基碘化銨、四丁基碘化銨、四己基碘化銨、四辛基碘化銨、四苯基碘化銨、三乙基甲基碘化銨、三乙基己基碘化銨、三辛基甲基碘化銨、三辛基丁基碘化銨、三辛基苄基碘化銨、三甲基苄基碘化銨、三丁基苄基碘化銨、三苯基異丁基碘化銨、三苯基苄基碘化銨等鹵化銨;鹽酸銨、磷酸銨、硼酸銨、氫氟酸銨、硫酸銨、硝酸銨、矽酸銨、磷酸銨等無機酸銨:甲酸銨、乙酸銨、丙酸銨、蘋果酸銨、胺磺酸銨等有機酸銨;四苯基氯化鏻、四苯基碘化鏻、四甲基溴化鏻、四丁基氯化鏻、四丁基溴化鏻、四丁基碘化鏻等無機酸鏻;乙酸四丁基鏻等有機酸鏻;乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-2-丙醇、1-戊醇、2-戊醇、2-甲基-2-丁醇、1-己醇、2-己醇、環己醇、2-甲基-2-戊醇、3-甲基-3-戊醇等醇溶媒等。該些非金屬凝固劑既可單獨使用亦可併用兩種以上。
作為所述凝固劑(Y),於以上所述化合物中,就可獲得更優異的凝固性及耐染色性的方面而言,較佳為一價的金屬化合物及/或無機酸銨,更佳為氯化鈉及/或硫酸銨。
所述凝固劑(Y)可用作凝固浴,作為所述凝固浴中的所述凝固劑(Y)的含量,較佳為1質量%~30質量%的範圍,更佳為5質量%~20質量%的範圍。
接下來,對本發明的凝固物的製造方法進行說明。
本發明的凝固物的製造方法是使以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂(X)的水分散體含浸於所述纖維基材,繼而,浸漬於所述凝固劑(Y)中。
作為於所述纖維基材中含浸所述水性胺基甲酸酯樹脂水分散體中的方法,例如可列舉將所述纖維基材直接放入儲存有所述水性胺基甲酸酯樹脂水分散體的槽中,其後利用軋液機(mangle)等擠壓多餘物質的方法。作為所述含浸時間,例如為1分鐘~30分鐘的範圍。
繼而,取出所述含浸基材,進而浸漬於包括所述凝固劑(Y)的凝固浴中,藉此胺基甲酸酯樹脂(X)凝固,從而可獲得纖維基材的表面或內部附著有凝固物的狀態下的纖維基材。作為此時的含浸/凝固時間,例如為1分鐘~30分鐘的範圍。
具有胺基甲酸酯樹脂的凝固物的纖維基材視需要可於所述凝固後,於流水中浸泡例如10分鐘~2小時,清洗除去不需要的凝固劑。
以上,根據本發明的製造方法,可獲得手感、耐鹼性及耐染色性優異的凝固物。
[實施例]
以下,使用實施例對本發明進行更詳細的說明。
[合成例1]
於辛酸亞錫0.1質量份的存在下,使聚醚多元醇(三菱化學股份有限公司製造的「PTMG2000」,數量平均分子量:2,000,以下簡稱為「PTMG2000」)1,000質量份、聚乙二醇(日油股份有限公司製造的「PEG600」,數量平均分子量:600,以下簡稱為「PEG」)38質量份、與二環己基甲烷二異氰酸酯(以下簡稱為「HMDI」)262質量份於100℃下反應,直至NCO%達到2.8質量%為止,獲得胺基甲酸酯預聚物A1。所獲得的胺基甲酸酯預聚物A1的黏度為7,280 mPa·s。
將加熱至70℃的A1以及作為乳化劑的十二烷基苯磺酸鈉20質量%水溶液(第一工業製藥股份有限公司製造的「尼歐根(Neogen)S-20F」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A1:10 kg/時、乳化劑水溶液:2.0 kg/時、水:6.5 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的哌嗪(以下簡稱為「PP」)的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為50質量%的胺基甲酸酯樹脂水分散體(1)。
[合成例2]
於辛酸亞錫0.1質量份的存在下,將PTMG2000 1,000質量份、PEG600 19質量份、HMDI 262質量份混合,並使其於100℃下反應,直至NCO%達到3.1質量%為止,獲得胺基甲酸酯預聚物A2。所獲得的胺基甲酸酯預聚物A2的黏度為7,280 mPa·s。
將加熱至70℃的A2以及作為乳化劑的十二烷基苯磺酸鈉20質量%水溶液(第一工業製藥股份有限公司製造的「尼歐根(Neogen)S-20F」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A2:10 kg/時、乳化劑水溶液:2.0 kg/時、水:0.1 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的異佛爾酮二胺(以下簡稱為「IPDA」)的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為60質量%的胺基甲酸酯樹脂水分散體(2)。
[合成例3]
於辛酸亞錫0.1質量份的存在下,將PTMG2000 1,000質量份、PEG 18質量份、HMDI 262質量份混合,並使其於100℃下反應,直至NCO%達到3.1質量%為止,獲得胺基甲酸酯預聚物A3。所獲得的胺基甲酸酯預聚物A3的黏度為7,280 mPa·s。
將加熱至70℃的A3以及作為乳化劑的聚丙烯聚乙烯共聚物(艾迪科(ADEKA)股份有限公司製造的「普朗尼克(Pluronic)L-64」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A3:10 kg/時、乳化劑:0.5 kg/時、水:5.8 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的IPDA的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為50質量%的胺基甲酸酯樹脂水分散體(3)。
[合成例4]
於辛酸亞錫0.1質量份的存在下,將PTMG2000 1,000質量份、PEG 18質量份、HMDI 262質量份混合,並使其於100℃下反應,直至NCO%達到3.1質量%為止,獲得胺基甲酸酯預聚物A4。所獲得的胺基甲酸酯預聚物A4的黏度為7,280 mPa·s。
將加熱至70℃的A4以及作為乳化劑的十二烷基苯磺酸鈉20質量%水溶液(第一工業製藥股份有限公司製造的「尼歐根(Neogen)S-20F」)、聚丙烯聚乙烯共聚物(艾迪科(ADEKA)股份有限公司製造的「普朗尼克(Pluronic)L-64」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A5:10 kg/時、乳化劑水溶液S-20F:1.3 kg/時、乳化劑L-64:0.3 kg/時、水:2.4 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的乙二胺(以下簡稱為「EA」)的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為60質量%的胺基甲酸酯樹脂水分散體(4)。
[合成例5]
於辛酸亞錫0.1質量份的存在下,使聚碳酸酯二醇多元醇(宇部興產股份有限公司製造的「艾塔納科(ETERNACOLL)UH-200」,數量平均分子量:2,000)1,000質量份、PEG 38質量份、與HMDI 262質量份於100℃下反應,直至NCO%達到2.8質量%為止,獲得胺基甲酸酯預聚物A5。所獲得的胺基甲酸酯預聚物A5的黏度為29,000 mPa·s。
將加熱至70℃的A5以及作為乳化劑的十二烷基苯磺酸鈉20質量%水溶液(第一工業製藥股份有限公司製造的「尼歐根(Neogen)S-20F」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A1:10 kg/時、乳化劑水溶液:2.0 kg/時、水:6.5 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的PP的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為50質量%的胺基甲酸酯樹脂水分散體(5)。
[比較合成例1]
於辛酸亞錫0.1質量份的存在下,將PTMG2000 1,000質量份、二羥甲基丙酸(以下簡稱為「DMPA」)18質量份、HMDI 262質量份混合,並使其於100℃下反應,直至NCO%達到2.4質量%為止,獲得胺基甲酸酯預聚物B1。所獲得的胺基甲酸酯預聚物B1的黏度為949,000 mPa·s。
將加熱至70℃的B1、以及作為中和劑的三乙胺、作為乳化劑的聚丙烯聚乙烯共聚物(艾迪科(ADEKA)股份有限公司製造的「普朗尼克(Pluronic)L-64」)、水同時供給至雙軸擠出機(TEM-18SS:東芝機械製造)並加以混合,藉此獲得乳化液。供給液各自的流量為A5:10 kg/時、中和劑:0.1 kg/時、乳化劑L-64:0.3 kg/時、水:8.5 kg/時,雙軸擠出機運轉條件為50℃、260 rpm。
其後,立即添加胺基含量相當於NCO基的95%的哌嗪(以下簡稱為「PP」)的水稀釋液進行鏈伸長,最終獲得不揮發成分的含有率為50質量%的胺基甲酸酯樹脂水分散體(R1)。
[實施例1~實施例3]
於所獲得的胺基甲酸酯樹脂水分散體(1)~胺基甲酸酯樹脂水分散體(3)各1,000質量份中加入離子交換水,以固體成分成為30質量%的方式進行調整,進而加入增黏劑(博爾徹(Borchers)公司製造的「博爾赤凝膠(Borchi Gel)L75N」)10質量份,於機械混合機中以2,000 rpm進行攪拌,製作調配液。
繼而,使聚酯纖維不織布(單位面積重量250 g/m2
)含浸於所述調配液中後,使用橡膠輥軋液機以含浸量成為200%的方式擠取不需要的調配液。繼而,使含有調配液的不織布於25℃的5質量%氯化鈉水溶液的凝固浴(以下簡稱為「NaCl」)中浸漬3分鐘,使胺基甲酸酯樹脂凝固。進而,一面向凝固後的加工布灑水,一面利用橡膠輥軋液機擠壓10次來進行水洗。最後,利用120℃的熱風乾燥機乾燥30分鐘,獲得具有凝固物的纖維基材。
[實施例4~實施例5]
於所獲得的胺基甲酸酯樹脂水分散體(4)~胺基甲酸酯樹脂水分散體(5)各1,000質量份中加入離子交換水,以固體成分成為30質量%的方式進行調整,進而加入增黏劑(博爾徹(Borchers)公司製造的「博爾赤凝膠(Borchi Gel)L75N」)10質量份,於機械混合機中以2,000 rpm進行攪拌,製作調配液。
繼而,使聚酯纖維不織布(單位面積重量250 g/m2
)含浸於所述調配液中後,使用橡膠輥軋液機以含浸量成為200%的方式擠取不需要的調配液。繼而,使含有調配液的不織布於25℃的5質量%的硫酸銨水溶液的凝固浴(以下簡稱為「硫酸銨」)中浸漬3分鐘,使胺基甲酸酯樹脂凝固。進而,一面向凝固後的加工布灑水,一面利用橡膠輥軋液機擠壓10次來進行水洗。最後,利用120℃的熱風乾燥機乾燥30分鐘,獲得具有凝固物的纖維基材。
[比較例1]
於所獲得的胺基甲酸酯樹脂水分散體(1)1,000質量份中加入離子交換水,以固體成分成為30質量%的方式進行調整,進而加入增黏劑(博爾徹(Borchers)公司製造的「博爾赤凝膠(Borchi Gel)L75N」)10質量份,於機械混合機中以2,000 rpm進行攪拌,製作調配液。
繼而,使聚酯纖維不織布(單位面積重量250 g/m2
)含浸於所述調配液中後,利用120℃的熱風乾燥機加熱乾燥30分鐘,藉此進行感熱凝固,從而獲得纖維基材。
[比較例2]
於所獲得的胺基甲酸酯樹脂水分散體(R1)1,000質量份中與實施例1~實施例4同樣地加入離子交換水,以固體成分成為30質量%的方式進行調整,進而加入交聯劑(日清紡化學公司製造的「卡保迪萊(Carbodilite)V-02-L2」)50質量份、增黏劑(博爾徹(Borchers)公司製造的「博爾赤凝膠(Borchi Gel)L75N」)10質量份,於機械混合機中以2,000 rpm進行攪拌,製作調配液。
繼而,實施與實施例1~實施例4同樣的加工,獲得具有凝固物的纖維基材。
[數量平均分子量等的測定方法]
合成例及比較合成例中使用的多元醇等的數量平均分子量表示藉由凝膠滲透管柱層析(gel permeation chromatography,GPC)法並於下述的條件下測定而獲得的值。
測定裝置:高速GPC裝置(東曹(Tosoh)股份有限公司製造的「HLC-8220GPC」)
管柱:將東曹股份有限公司製造的下述管柱串聯連接來使用。
「TSKgel G5000」(7.8 mmI.D.×30 cm)×1根
「TSKgel G4000」(7.8 mmI.D.×30 cm)×1根
「TSKgel G3000」(7.8 mmI.D.×30 cm)×1根
「TSKgel G2000」(7.8 mmI.D.×30 cm)×1根
檢測器:RI(示差折射計)
管柱溫度:40℃
溶離液:四氫呋喃(tetrahydrofuran,THF)
流速:1.0 mL/分鐘
注入量:100 μL(試樣濃度為0.4質量%的四氫呋喃溶液)
標準試樣:使用下述標準聚苯乙烯來製作標準曲線。
(標準聚苯乙烯)
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 A-500」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 A-1000」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 A-2500」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 A-5000」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-1」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-2」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-4」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-10」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-20」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-40」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-80」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-128」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-288」
東曹股份有限公司製造的「TSKgel 標準聚苯乙烯 F-550」
[胺基甲酸酯樹脂(X)的平均粒徑的測定方法]
針對實施例及比較例中所獲得的胺基甲酸酯樹脂水分散體,使用雷射繞射/散射式粒度分佈測定裝置(堀場製作所股份有限公司製造的「LA-910」),並將水用作分散液,測定相對折射率=1.10、粒徑基準為面積時的平均粒徑。
[手感的評價方法]
藉由觸感對所獲得的加工布以如下方式進行評價。
「A」:硬挺感、充實感皆特別優異。
「B」:有硬挺感,亦可感覺到充實感。
「C」:硬挺感、充實感稍差。
「D」:完全未感覺到硬挺感、充實感。
[耐鹼性的評價方法]
於具有攪拌翼的SUS製可分離式燒瓶中放入1質量%氫氧化鈉水溶液,加熱至95℃。將加工布放入燒瓶內,以50 rpm攪拌30分鐘。其後,取出含浸加工布,一面向加工布灑水,一面利用橡膠輥軋液機擠壓10次來進行水洗。最後,利用120℃的熱風乾燥機乾燥30分鐘而獲得纖維基材,藉由觸感對所獲得的纖維基材進行評價。
「A」:硬挺感、充實感皆特別優異。
「B」:有硬挺感,亦可感覺到充實感。
「C」:硬挺感、充實感稍差。
「D」:完全未感覺到硬挺感、充實感。
[耐染色性的評價方法]
於PTFE製耐壓容器中放入5質量%且pH4.5的0.5 M乙酸鈉緩衝液以及所述[耐鹼性的評價方法]的試驗後的加工布,於120℃下加熱24小時。其後,一面向取出後的加工布灑水,一面利用橡膠輥軋液機擠壓10次來進行水洗。最後,利用120℃的熱風乾燥機乾燥30分鐘而獲得纖維基材,藉由觸感對所獲得的纖維基材進行評價。
「A」:硬挺感、充實感皆特別優異。
「B」:有硬挺感,亦可感覺到充實感。
「C」:硬挺感、充實感稍差。
「D」:完全未感覺到硬挺感、充實感。
[表1]
表1 | 實施例1 | 實施例2 | 實施例3 | 實施例4 | 實施例5 | 比較例1 | 比較例2 | |
胺基甲酸酯樹脂水分散體 | (1) | (2) | (3) | (4) | (5) | (1) | (R1) | |
具有非離子性基的化合物(a1) | 種類 | PEG | PEG | PEG | PEG | PEG | PEG | DMPA |
使用率 (質量%、胺基甲酸酯原料中) | 2.9 | 1.5 | 1.5 | 1.5 | 1.5 | 2.9 | 1.4 | |
胺基甲酸酯樹脂(X)的含有率(質量%) | 50 | 60 | 60 | 60 | 50 | 50 | 50 | |
胺基甲酸酯樹脂(X)的平均粒徑(μm) | 0.17 | 0.19 | 0.18 | 0.18 | 0.18 | 0.17 | 0.17 | |
凝固劑(Y) | 種類 | NaCl | NaCl | NaCl | 硫酸銨 | 硫酸銨 | - | NaCl |
手感的評價 | A | A | A | A | A | D | A | |
耐鹼性的評價 | A | A | A | A | A | C | A | |
耐染色性的評價 | A | A | A | A | A | C | C |
可知具有藉由本發明的製造方法獲得的凝固物的加工布如實施例1~實施例4般,具有優異的手感、耐鹼性及耐染色性。
另一方面,比較例1為不使用凝固劑(Y)而進行感熱凝固的形態,手感、耐鹼性及耐染色性不良。比較例2為代替胺基甲酸酯樹脂(X)而使用不以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂,並利用凝固劑(Y)進行凝固的形態,耐染色性不良。
Claims (3)
- 一種凝固物的製造方法,其特徵在於,使以具有非離子性基的化合物(a1)為原料的胺基甲酸酯樹脂(X)的水分散體含浸於纖維基材中,繼而,浸漬於凝固劑(Y)中。
- 如請求項1所述的凝固物的製造方法,其中,於構成胺基甲酸酯樹脂(X)的原料的合計質量中,所述具有非離子性基的化合物(a1)的使用率為5質量%以下。
- 如請求項1或請求項2所述的凝固物的製造方法,其中,所述凝固劑(Y)為選自由金屬化合物(Y1)、酸化合物(Y2)、及除所述酸化合物(Y2)以外的非金屬化合物(Y3)所組成的群組中的一種以上。
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