TWI830808B - 多孔層結構體及其製造方法 - Google Patents

多孔層結構體及其製造方法 Download PDF

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Publication number
TWI830808B
TWI830808B TW108140605A TW108140605A TWI830808B TW I830808 B TWI830808 B TW I830808B TW 108140605 A TW108140605 A TW 108140605A TW 108140605 A TW108140605 A TW 108140605A TW I830808 B TWI830808 B TW I830808B
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Taiwan
Prior art keywords
porous layer
water
layer structure
base material
polyurethane resin
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TW108140605A
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English (en)
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TW202030078A (zh
Inventor
鈴木悠介
村川達三
佐佐木一弥
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日商大日精化工業股份有限公司
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Abstract

本發明之多孔層結構體係包含基材、與形成於該基材上而成之聚胺酯多孔層者，藉由JIS L1099 A-1(氯化鈣法)對上述多孔層結構體進行測定所獲得之透濕度A為2000~10000g/(m2‧24h)，根據藉由JIS L1099 A-1(氯化鈣法)對上述基材單獨進行測定所獲得之透濕度B與上述透濕度A，利用特定式所獲得之透濕度損失比率為75%以下，且基材與聚胺酯多孔層之接合面之剝離強度為0.7kgf/in以上。

Description

多孔層結構體及其製造方法
本發明係關於一種多孔層結構體及其製造方法。
聚胺酯系樹脂於耐磨耗性、彎曲性、可撓性、柔軟性、加工性、接著性、耐化學品性等諸多物性方面優異，並且對各種加工法之適應性亦優異。因此，被廣泛用作合成仿革(人工皮革與合成皮革之統稱)用材料、各種塗佈劑、油墨、塗料等之黏合劑，或者膜、片材及各種成型物用材料，提出有適用於各種用途之聚胺酯系樹脂。
其中，藉由對樹脂賦予親水性而能夠在水中乳化分散之聚胺酯樹脂水分散體於塗佈後加以乾燥，藉此容易獲得機械物性、耐久性、耐化學品性及耐磨耗性等性能優異之覆膜，從而廣泛用於塗料、接著劑、纖維加工處理劑、紙處理劑及油墨等。迄今為止，該等用途中使用的是溶解於有機溶劑之溶劑系胺酯。然而，由於存在有機溶劑之毒性、火災之危險性、環境污染性等問題，近年來逐漸轉而使用聚胺酯樹脂水分散體代替溶劑系胺酯。
於使用聚胺酯樹脂水分散體進行加工時，為了提高加工品之質感等目的，廣泛利用實施各種處理獲得多孔結構之方法。
例如，於專利文獻1中提出有如下方法：於基材塗佈包含(A)含親水性官能基之樹脂、特定量之(B)銨鹽及(C)非離子性增黏劑之水系分散液而形成塗膜，對該塗膜進行感熱凝膠化處理製成凝膠化膜，使凝膠化膜乾燥 固化而形成皮膜。
[先前技術文獻] [專利文獻]
專利文獻1：日本專利第5706897號公報
根據專利文獻1，即便升高乾燥溫度或增大風量等而加快乾燥效率，亦可抑制皮膜表面上產生龜裂等，顯著提高整體之生產效率，並且不論使用何種基材，均可形成較厚之皮膜。然而，根據專利文獻1中揭載之剖面照片，可知皮膜(胺酯多孔層)中形成之氣泡大部分為獨立氣泡，因此就良好之柔軟性或透濕性之方面而言可謂仍需改善。
又，不僅具有如上所述之特性、並且就耐久性之方面而言耐龜裂性或剝離強度良好可謂亦為今後所必須。
綜上，本發明之目的在於提供一種柔軟性、耐龜裂性及剝離強度良好之多孔層結構體及其製造方法。
本發明者等人經過銳意研究，結果發現藉由下述本發明可解決上述課題，從而完成本發明。即，本發明如下所述。
[1]一種多孔層結構體，其係包含基材、與形成於該基材上而成之聚胺酯多孔層者，藉由JIS L1099 A-1(氯化鈣法)對上述多孔層結構體進行測定所獲得之透濕度A為2000~10000g/(m2‧24h)， 根據藉由JIS L1099 A-1(氯化鈣法)對上述基材單獨進行測定所獲得之透濕度B與上述透濕度A，利用下述式所獲得之透濕度損失比率為75%以下，且基材與聚胺酯多孔層之接合面之剝離強度為0.7kgf/in以上。
式) 透濕度損失比率(%)=(1-(透濕度A/透濕度B))×100
[2]如[1]記載之多孔層結構體，其中上述聚胺酯多孔層之厚度為0.1~1.0mm，且上述聚胺酯多孔層之密度為0.10~0.90g/cm3。
[3]一種多孔層結構體之製造方法，其係如[1]或[2]記載之多孔層結構體之製造方法，且包括如下步驟：(1)含水基材製作步驟，其係於基材塗佈基材處理用水溶液而製成含水基材，該基材處理用水溶液包含含有至少一種以上之鹽之多孔層形成輔助劑A；(2)塗膜結構體製作步驟，其係於上述含水基材上塗佈發泡組合物而製成塗膜結構體，該發泡組合物係對包含含有至少一種以上之鹽之多孔層形成輔助劑B、發泡穩定劑、水溶性樹脂及聚胺酯樹脂水分散體之調配液進行發泡處理而成；(3)第1乾燥步驟，其係對上述塗膜結構體實施乾燥處理；(4)洗淨步驟，其係於第1乾燥步驟後進行洗淨；及(5)第2乾燥步驟，其係於洗淨步驟後實施乾燥處理；並且上述聚胺酯樹脂水分散體中之聚胺酯樹脂粒子包含多元醇成分、異氰酸酯成分、及具有1個以上之活性氫基且具有氧化伸烷基(alkylene oxide)之親水性氧化伸烷基成分，且上述親水性氧化伸烷基成分相對於聚胺酯樹脂粒子之含量為1~25質量%。
[4]如[3]記載之多孔層結構體之製造方法，其中於上述含水基材製作 步驟、上述塗膜結構體製作步驟及上述洗淨步驟中，實質上不使用有機溶劑。
[5]如[3]或[4]記載之多孔層結構體之製造方法，其中上述發泡處理為機械發泡。
根據本發明，可提供一種柔軟性、耐龜裂性及剝離強度良好之多孔層結構體及其製造方法。
1:聚胺酯多孔層
2:氣泡
3:孔
4:基材
10:基材
10A:含水基材
10B:塗膜結構體
10C:多孔質結構體
12A:輥
12B:輥
12C:輥
12D:輥
12E:輥
12F:輥
12G:輥
12H:輥
12J:對輥
14:含水處理槽
14A:基材處理用水溶液
16:發泡組合物
17:刮漿板
18:發泡槽
19:乾燥裝置
20:洗淨槽
20A:洗淨水
22:洗淨槽
圖1係說明本發明之一實施形態之多孔層結構體之製造製程之概略說明圖。
圖2係表示本發明之一實施形態之多孔層結構體之推測之剖面結構之模式性概略剖視圖。
以下，對本發明進行詳細說明。再者，於本發明中，所謂聚胺酯樹脂係聚胺酯樹脂及聚胺酯-脲樹脂之統稱。
[1.多孔層結構體]
本發明之多孔層結構體包含基材、與形成於該基材上之聚胺酯多孔層，藉由JIS L1099 A-1(氯化鈣法)對該多孔層結構體進行測定所獲得之透濕度A為2000~10000g/(m2‧24h)。
此處，所謂透濕度係藉由JIS L1099 A-1(氯化鈣法)進行測定，將透過纖維製品(多孔層結構體或基材)之水蒸氣之質量換算成平均1m2之該纖維製品於24小時內所透過之水蒸氣之質量，於本發明之情形時，將其用於多孔層中之水蒸氣之易通過性之指標。
即，於透濕度A超過10000g/(m2‧24h)越來越大之情形時，推測多孔層中形成之氣泡為連續氣泡、且形成了厚度方向上平行之連續氣泡。其結果，若產生局部之剝離力，則容易對樹脂層造成破壞，實用上不耐用。另一方面，若如本發明之透濕度A為2000~10000g/(m2‧24h)，則推測具有例如直徑較大之氣泡彼此共有該等上形成之小孔而構成連續氣泡之類的複雜形態。其結果，與形成了厚度方向上平行之連續氣泡之情形相比，即便產生局部之剝離力，亦可發揮較高之耐久性(剝離強度)。又，當然具有透濕性，且亦可良好地維持柔軟性。再者，若透濕度A未達2000g/(m2‧24h)，則透濕性能不充分。
該透濕度A較佳為2200~10000g/(m2‧24h)，更佳為2500~10000g/(m2‧24h)。
又，根據藉由JIS L1099 A-1(氯化鈣法)對多孔質結構體之基材單獨進行測定所獲得之透濕度B與透濕度A，利用下述式所獲得之透濕度損失比率為75%以下。
式) 透濕度損失比率(%)=(1-(透濕度A/透濕度B))×100
所謂透濕度損失比率，表示相對於基材單獨之透濕度，因基材上形成之樹脂層(多孔質層)等而損失之透濕度之程度，若其超過75%，則作為結構體之透濕度明顯受損。透濕度損失比率較佳為60%以下，更佳為50%以下。
基材與聚胺酯多孔層之接合面之剝離強度為0.7kgf/in以上，較佳為0.75kgf/in以上，進而較佳為0.80kgf/in以上。若剝離強度未達0.7kgf/in，則無法獲得充分之耐久性。推測本發明中之0.7kgf/in以上之剝離強度係起因於直徑較大之氣泡彼此共有該等上形成之小孔而構成連 續氣泡之類的複雜形態。
就兼備良好之剝離強度與柔軟性之觀點而言，聚胺酯多孔層之厚度較佳為0.1~1.0mm，更佳為0.2~0.8mm。
多孔質結構體中之聚胺酯多孔層之密度較佳為0.10~0.90g/cm3，更佳為0.3~0.9g/cm3，進而較佳為0.4~0.8g/cm3。藉由聚胺酯多孔層之密度為0.10g/cm3以上，可獲得良好之剝離強度，藉由為0.90g/cm3以下，可使所獲得之結構體之柔軟性變得良好。
作為基材，可列舉使用如下所述之樹脂之膜、織布、不織布、合成皮革等。又，基材可為發泡基材。
作為樹脂，可列舉：聚氯乙烯樹脂、聚乙烯系樹脂、聚丙烯系樹脂、熱塑性聚烯烴等烯烴系樹脂、乙烯丙烯二烯系樹脂、苯乙烯丙烯腈系樹脂、聚碸系樹脂、聚苯醚系樹脂、丙烯酸系樹脂、矽酮系樹脂、氟系樹脂、聚酯系樹脂、聚醯胺系樹脂、聚醯亞胺系樹脂、聚苯乙烯系樹脂、聚胺酯系樹脂、聚碳酸酯系樹脂、降
Figure 108140605-A0305-02-0008-5
烯系樹脂、纖維素系樹脂、聚乙烯醇系樹脂、聚乙烯醇縮甲醛系樹脂、聚乙烯醇縮丁醛系樹脂、聚乙烯吡咯啶酮系樹脂、聚乙烯醇縮醛系樹脂、聚乙酸乙烯酯系樹脂、工程塑膠、生物降解性塑膠等。
尤其作為汽車用之內裝材用，可列舉：聚氯乙烯樹脂、熱塑性聚烯烴、聚胺酯、聚丙烯等。
又，於基材為發泡基材之情形時，可使用氯乙烯樹脂之類的基材。
基材之厚度較佳為0.2~1.5mm，於基材為發泡基材而使其發泡之情形時，發泡後之厚度較佳為0.3~4.5mm。
[2.多孔層結構體之製造方法]
本發明之多孔層結構體之製造方法係製造本發明之多孔層結構體之方法，且包括如下步驟：(1)含水基材製作步驟，其係於基材塗佈基材處理用水溶液而製成含水基材，該基材處理用水溶液包含含有至少一種以上之鹽之多孔層形成輔助劑A；(2)塗膜結構體製作步驟，其係於上述含水基材上塗佈發泡組合物而製成塗膜結構體，該發泡組合物係對包含含有至少一種以上之鹽之多孔層形成輔助劑B、發泡穩定劑、水溶性樹脂及聚胺酯樹脂水分散體之調配液進行發泡處理而成；(3)第1乾燥步驟，其係對上述塗膜結構體實施乾燥處理；(4)洗淨步驟，其係於第1乾燥步驟後進行洗淨；及(5)第2乾燥步驟，其係於洗淨步驟後實施乾燥處理。
以下，參照圖1對各步驟進行說明。
(含水基材製作步驟)
於含水基材製作步驟中，如圖1所示，將捲成捲筒狀之基材10自輥12A捲出，一面將其利用輥12B、12C、12D張架，一面使之於輥12C之位置在含水處理槽14之基材處理用水溶液14A中通過。藉此，使基材處理用水溶液14A含浸塗佈於基材10。再者，基材10之詳細說明如上文所述。
基材處理用水溶液14A包含含有至少一種以上之鹽之多孔層形成輔助劑A。
作為多孔層形成輔助劑A中之鹽，可列舉：與銨、鎂、鈣等之硫酸鹽或氯化物等。該等較佳為於水溶液中含有5~40質量%。藉由含有5~40質量%，可促進調配液之固化。
含水量可藉由在基材處理用水溶液14A中之浸漬時間及/或含水量調整輥(輥12E)等進行調整。含水量亦取決於基材10之種類，例如相對於基材10，較佳為設為200~400質量%左右。
基材處理用水溶液14A之溫度並無特別限定，較佳為設為10~40℃左右。再者，作為向基材之塗佈方法，並不限於含浸塗佈，可適當採用噴塗、輥塗、刷塗等塗佈方法，但考慮到實用性，較佳為含浸塗佈。
於含浸塗佈後，將所捲出之基材10例如利用一對含水量調整輥(輥12E)壓縮、脫水成規定之含水量，而製成含水基材10A。
(塗膜結構體製作步驟)
含水基材10A係利用刮漿板17以特定厚度塗佈特定之發泡組合物16而製成塗膜結構體10B。
發泡組合物16係將包含含有至少一種以上之鹽之多孔層形成輔助劑B、發泡穩定劑、水溶性樹脂及聚胺酯樹脂水分散體之調配液於發泡槽18內進行發泡處理而成。
此處，作為多孔層形成輔助劑B之至少一種以上之鹽，可例示與多孔層形成輔助劑A中之至少一種以上之鹽相同者，多孔層形成輔助劑B與多孔層形成輔助劑A可設為同一組成，亦可設為不同組成。至少一種以上之鹽較佳為於調配液中占5~40質量%。
又，作為調配液所含有之發泡穩定劑，可列舉：矽酮系發泡穩定劑、非離子系發泡穩定劑、金屬鹽系發泡穩定劑等。就泡保持之觀點而言，調配液中之發泡穩定劑較佳為相對於聚胺酯樹脂為0.1~3質量%。
作為水溶性樹脂，可列舉：聚乙烯醇、甲基纖維素、三仙膠等多糖 類、水溶性聚胺酯樹脂、水溶性丙烯酸系樹脂等。就泡保持及製膜輔助之觀點而言，調配液中之水溶性樹脂較佳為5~40質量%。
調配液中之聚胺酯樹脂水分散體係以成為所需之胺酯多孔層之厚度之方式調整其量。
發泡處理之方法並無特別限定，較佳為對原料進行機械攪拌使其中混入空氣而發泡之機械發泡。
作為於含水基材10A上塗佈發泡組合物16之方法，可應用刀式塗佈機、刮刀塗佈機、MB反向塗佈機等塗佈方法，但並無特別限定，可視目標之塗敷厚度來選擇最佳之塗敷方法。
就確保發泡性之觀點而言，塗佈後之塗膜厚度較佳為200~2000μm，更佳為600~1000μm。
藉由含水基材製作步驟進行基材之含水處理，並藉由塗膜結構體製作步驟進行發泡組合物之塗佈處理，經過該兩種處理，可更為提高基材與胺酯多孔層之密接性。
(第1乾燥步驟)
將塗膜結構體10B捲出至乾燥裝置19來實施乾燥處理。乾燥溫度較佳為設為例如100~150℃。藉由乾燥處理，塗膜結構體之塗膜固化，與此同時，因發泡產生之氣泡彼此一部分合為一體，共有直徑小於氣泡徑之孔，獲得形成有連續氣泡之多孔質結構體10C。
再者，該狀態下之多孔質結構體10C由於附著有未反應物或無用物，故而實施洗淨處理。
(洗淨步驟)
將上述多孔質結構體10C捲出至洗淨槽20，於洗淨槽20內之洗淨水 20A中通過來實施洗淨處理。於圖1所示之例中，一面利用輥12E、輥12F、一對輥12G、輥12H及一對輥12J張架一面捲出，於輥12F、輥12H之位置在洗淨槽20內之洗淨水20A中通過。洗淨例如可將洗淨水20之溫度設為40~50℃左右而進行，或增加輥之數量、增加浸漬次數、或延長浸漬時間而進行調整。藉此充分地進行洗淨，送至第2乾燥步驟。
作為洗淨水，通常使用蒸餾水。
(第2乾燥步驟)
將洗淨步驟後之多孔質結構體10C捲出至乾燥裝置22來實施乾燥處理。乾燥溫度只要為可使洗淨時所含之水充分地乾燥之溫度即可，較佳為設為例如120~150℃。
於第2乾燥步驟後，藉由輥12J捲取成捲筒狀，而製造本發明之經潔淨化之多孔質結構體10C。
於上述含水基材製作步驟、上述塗膜結構體製作步驟及上述洗淨步驟中，較佳為實質上不使用有機溶劑，更佳為完全不使用有機溶劑。
此處，作為塗膜結構體製作步驟之調配液中所調配之聚胺酯樹脂水分散體之聚胺酯樹脂粒子，使用如下聚胺酯樹脂粒子，其包含多元醇成分、異氰酸酯成分、及具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分，且親水性氧化伸烷基成分相對於聚胺酯樹脂粒子之含量為1~25質量%。
以下，對聚胺酯樹脂水分散體進行說明。
[聚胺酯樹脂水分散體]
本發明之聚胺酯樹脂水分散體係聚胺酯樹脂粒子於水中分散而成 者，如上所述，聚胺酯樹脂粒子包含多元醇成分、異氰酸酯成分、及具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分，且親水性氧化伸烷基成分相對於聚胺酯樹脂粒子之含量為1~25質量%。藉由使用該聚胺酯樹脂粒子，容易將透濕度A、透濕度損失比率及剝離強度調整至所需之範圍。又，聚胺酯樹脂水分散體較佳為含有40質量%以上之不揮發成分。進而，聚胺酯樹脂粒子之體積平均粒徑較佳為0.3~5μm。
於本發明中，藉由包含具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分(以下有時簡稱為「親水性氧化伸烷基成分」)作為聚胺酯樹脂粒子之構成成分，即便聚胺酯樹脂粒子之體積平均粒徑為0.3~5μm之相對較大之粒徑，亦可滿足分散穩定性與製膜性。又，由於體積平均粒徑為0.3~5μm，故而容易使不揮發成分達到40質量%以上，由於不揮發成分為40質量%以上，故而可謂具有較迄今為止之聚胺酯樹脂水分散體高之生產性。
此處推測，親水性氧化伸烷基成分於樹脂粒子之表面發揮利用其氧化伸烷基之立體阻礙效應，從而即便大粒徑之樹脂粒子發生沈澱，但由於氧化伸烷基使粒子彼此排斥，故亦防止凝集。其結果，即便為了使不揮發成分達到40質量%以上而將體積平均粒徑設為0.3~5μm，亦可獲得良好之分散穩定性。
再者，本發明中之所謂「不揮發成分」係指下文記述之聚胺酯樹脂粒子或不揮發性之添加劑等，具體而言，指將2g之聚胺酯樹脂水分散體於120℃下乾燥2小時之情形時獲得之固體成分。
以下，對構成聚胺酯樹脂水分散體所含之聚胺酯樹脂粒子之各成分進行更詳細之說明。
<聚胺酯樹脂粒子>
構成本發明之聚胺酯樹脂粒子之聚胺酯樹脂主要包含多元醇成分、異氰酸酯成分、及具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分。
〔多元醇成分〕
作為成為本發明中之多元醇成分的多元醇，可例示以下之(1)~(6)。
(1)聚碳酸酯多元醇
作為聚碳酸酯多元醇，可列舉：聚四亞甲基碳酸酯二醇、聚五亞甲基碳酸酯二醇、聚新戊基碳酸酯二醇、聚六亞甲基碳酸酯二醇、聚(1,4-環己烷二亞甲基碳酸酯)二醇等聚碳酸酯二醇、及該等之無規/嵌段共聚物等。
(2)聚醚多元醇
作為聚醚多元醇，可列舉：使環氧烷(環氧乙烷、環氧丙烷、環氧丁烷等)及雜環式醚(四氫呋喃等)之任一者進行聚合或共聚合而獲得者。具體而言，可列舉：聚丙二醇、聚乙二醇-聚四亞甲基二醇(嵌段或無規)、聚四亞甲基醚二醇及聚六亞甲基二醇等。
再者，聚醚多元醇中之環氧乙烷(EO)含有比率設為未達50質量%。
(3)聚酯多元醇
作為聚酯多元醇，可列舉：使脂肪族系二羧酸(例如：琥珀酸、己二酸、癸二酸、戊二酸及壬二酸等)及芳香族系二羧酸(例如：間苯二甲酸及對苯二甲酸等)之至少任一者、與低分子量二醇類(例如：乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,5-戊二醇、1,6-六亞甲基二醇、新戊二醇及1,4-雙羥基甲基環己烷等)進行縮聚合而獲得者。
具體而言，可列舉：聚己二酸乙二酯二醇、聚己二酸丁二酯二醇、聚六亞甲基己二酸酯二醇、聚己二酸新戊酯二醇、聚己二酸乙二酯/丁二酯二醇、聚己二酸新戊酯/己酯二醇、聚-3-甲基戊烷己二酸酯二醇及聚間苯二甲酸丁二酯二醇等。
(4)聚內酯多元醇
作為聚內酯多元醇，可列舉：聚己內酯二醇及聚-3-甲基戊內酯二醇等。
(5)聚烯烴多元醇
作為聚烯烴多元醇，可列舉：聚丁二烯二醇及聚異戊二烯二醇、或其氫化物等。
(6)聚甲基丙烯酸酯二醇
作為聚甲基丙烯酸酯二醇，可列舉：α,ω-聚甲基丙烯酸甲酯二醇及α,ω-聚甲基丙烯酸丁酯二醇等。
多元醇之數量平均分子量只要為500以上，則並無特別限制，較佳為500~4,000左右，更佳為1000~3000左右。該等多元醇可單獨使用或將2種以上組合使用，但就長期耐久性之觀點而言，較佳為包含聚碳酸酯二醇。
再者，數量平均分子量係聚苯乙烯換算之數量平均分子量，通常可藉由凝膠滲透層析法(GPC)之測定求出。
〔異氰酸酯成分〕
作為成為本發明中之異氰酸酯成分的異氰酸酯，並無特別限定，較佳為脂肪族二異氰酸酯、脂環族二異氰酸酯、芳香族二異氰酸酯等二官能之聚異氰酸酯。
聚異氰酸酯之具體例為：甲苯二異氰酸酯、4-甲氧基-1,3-苯二異氰酸酯、4-異丙基-1,3-苯二異氰酸酯、4-氯-1,3-苯二異氰酸酯、4-丁氧基-1,3-苯二異氰酸酯、2,4-二異氰酸酯-二苯醚、均三甲苯二異氰酸酯、4,4'-二苯基甲烷二異氰酸酯、伸荰基二異氰酸酯、1,5-萘二異氰酸酯、聯苯胺二異氰酸酯、鄰硝基聯苯胺二異氰酸酯、4,4-二異氰酸二苄酯、1,4-四亞甲基二異氰酸酯、1,5-五亞甲基二異氰酸酯、1,6-六亞甲基二異氰酸酯、1,10-十亞甲基二異氰酸酯、1,4-環己二異氰酸酯、二甲苯二異氰酸酯、4,4'-亞甲基雙(異氰酸環己酯)、1,5-四氫萘二異氰酸酯、異佛爾酮二異氰酸酯、二環己基甲烷4,4'-二異氰酸酯等。其中，較佳為至少包含二環己基甲烷4,4'-二異氰酸酯。
再者，於如車輛用途或淺色系用途等需要柔軟性、機械物性及耐變色性之情形時，較佳為將4,4'-二苯基甲烷二異氰酸酯與脂肪族二異氰酸酯或脂環族二異氰酸酯併用。
聚異氰酸酯成分之異氰酸基當量相對於全部成分之羥基當量的比較佳為1.1~2.2，更佳為1.2~1.9。若NCO/OH為1.2~1.9，則柔軟性及耐久性均更良好。
〔具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分〕
具有1個以上之活性氫基且具有氧化伸烷基之親水性氧化伸烷基成分對聚胺酯樹脂粒子賦予水分散性。水分散性變得良好之原因尚不明確，但推測如下：氧化伸烷基以自聚胺酯樹脂粒子之表面伸出之方式突出至水中，藉此，其發揮阻礙其他聚胺酯樹脂粒子接近之立體阻礙效應。
於親水性氧化伸烷基成分中，所謂活性氫係指會與異氰酸 酯之異氰酸基反應之氫原子，可列舉：羥基、巰基、胺基等中之氫原子，該等之中，較佳為羥基之氫原子。
又，氧化伸烷基成為表現出親水性之親水性基，助益於聚胺酯樹脂粒子之水分散性。該氧化伸烷基之碳數較佳為例如2~12，具體而言，可列舉：氧化乙烯、1,2-或1,3-氧化丙烯、1,2-、2,3-或1,3-氧化丁烯、四氫呋喃、3-甲基四氫呋喃、α-氧化烯烴、氧化苯乙烯及表鹵醇(表氯醇等)等。其中，較佳為包含氧化乙烯作為氧化伸烷基。
於具有氧化伸烷基之親水成分中，較佳為含有至少50質量%以上之氧化乙烯之重複單元，更佳為含有70質量%以上，進而較佳為氧化伸烷基即為氧化乙烯。
作為成為親水性氧化伸烷基成分之化合物，可列舉：聚乙二醇、聚氧乙烯-聚氧丙烯共聚物二醇、聚氧乙烯-聚氧丁烯共聚物二醇、聚氧乙烯-聚氧伸烷基共聚物二醇，及該等之甲醚、乙醚、丁醚等單烷基醚類，對該等之單烷基醚類加成1,3-二醇之類的二醇而成之聚伸烷基二醇單烷基醚之二醇加成體。
其中，較佳為聚乙二醇；聚乙二醇單甲醚及聚乙二醇單乙醚等之類的聚乙二醇單烷基醚；對聚乙二醇單烷基醚加成1,3-二醇之類的二醇而成之聚乙二醇單烷基醚之二醇加成體等。
尤其就不僅進一步提高分散穩定性，亦使再分散性變得良好，發揮優異之耐熱性之觀點而言，更佳為聚乙二醇單烷基醚及聚乙二醇單烷基醚之二醇加成體，進而較佳為聚乙二醇單烷基醚之二醇加成體。
推測於聚胺酯樹脂粒子中，該等取得適於發揮分散性及熱穩定性之形態。
成為親水性氧化伸烷基成分之化合物之數量平均分子量較佳為500~3000，更佳為700~2000。
作為聚乙二醇之市售品，例如可列舉：日油股份有限公司製造之「PEG#200」、「PEG#300」、「PEG#400」、「PEG#600」、「PEG#1000」、「PEG#1500」、「PEG#1540」、「PEG#2000」等。
作為聚乙二醇單甲醚之市售品，例如可列舉：日油股份有限公司製造之「Uniox M-400」、「Uniox M-550」、「Uniox M-1000」、「Uniox M-2000」等。
作為聚乙二醇單烷基醚之二醇加成體之市售品，例如可列舉：Evonic公司製造之「TEGOMER D3403」等。
以上為較佳之成分之例示，本發明並不限定於該等。因此，不僅是上述之例示，其他之目前在售之容易自市場購入之化合物均可使用。
親水性氧化伸烷基成分相對於聚胺酯樹脂粒子之含量為1~25質量%，較佳為3~20質量%，更佳為5~10質量%。若含量未達1質量%，則分散穩定性降低，或製膜性降低、產生龜裂。若超過25質量%，則有機械物性降低、水分散體增黏之可能性，導致作業性降低或不揮發成分減少。
又，藉由含有1~20質量%之親水性氧化伸烷基成分，可減慢成膜時之乾燥(水分之蒸發)速度，抑制龜裂產生。
〔聚胺酯樹脂粒子之體積平均粒徑〕
本發明之聚胺酯樹脂粒子之體積平均粒徑為0.3~5μm。若聚胺酯樹脂粒子之體積平均粒徑未達0.3μm，則水分散體之黏度上升，致使必須減少不揮發成分。另一方面，若體積平均粒徑超過5μm，則粒子容易沈澱。
就此觀點而言，聚胺酯樹脂粒子之體積平均粒徑較佳為0.3~5.0μm，更佳為0.3~3.0μm，進而較佳為0.3~1.5μm。
〔聚胺酯樹脂水分散體之黏度〕
聚胺酯樹脂水分散體於25℃下之黏度較佳為3000mPa‧s以下，更佳為2000mPa‧s以下。藉由使黏度為2000mPa‧s以下，於製造時容易實施異物去除(過濾等)，可提高生產效率。
〔聚胺酯樹脂水分散體之製造方法〕
作為本發明中之聚胺酯樹脂水分散體之製造方法，例如可列舉：方法(1)，其係經過反應步驟與乳化及高分子量化步驟之方法，該反應步驟係使多元醇、成為親水性氧化伸烷基成分之化合物及異氰酸酯進行反應，該乳化及高分子量化步驟係於反應後添加界面活性劑等，添加離子交換水與二胺等之混合液而一面乳化一面高分子化，其中，將乳化及高分子量化步驟中之添加有界面活性劑等時之攪拌設為100~300rpm左右之慢攪拌，將添加有離子交換水與二胺等之混合液時之攪拌設為4000~6000rpm左右之強攪拌；以及方法(2)，其於具有槽內循環用攪拌翼與剪力賦予用攪拌翼之攪拌槽中，至少使多元醇、異氰酸酯及成為親水性氧化伸烷基成分之化合物進行反應並進行乳化。
藉由該製造方法，可以上述較高之不揮發性成分濃度高效率地製造具有上述體積平均粒徑之聚胺酯樹脂粒子。又，可成為所需之黏度。
關於方法(2)，具體而言，可藉由如下方式進行製造：於具備可達成均一化且亦可應對超高黏度液之攪拌翼之反應容器(上述攪拌槽)中使多元醇、視需要添加之短鏈二醇、異氰酸酯、及成為親水性氧化伸烷基成分之化合物進行反應，其後，添加短鏈二胺等鏈伸長劑或鏈伸長終止 劑、界面活性劑、作為分散介質之離子交換水，進行乳化並進行反應。
再者，於方法(1)中亦可適當添加短鏈二醇或短鏈二胺等鏈伸長劑或鏈伸長終止劑等。
又，作為上述攪拌槽，例如可列舉：於攪拌槽內具有2個以上之攪拌翼，例如具有2個以槽內循環為目的之攪拌翼、1個以對槽內賦予高剪力為目的之剪力賦予用攪拌翼之攪拌裝置，其中，較佳為於反應容器內之上部、底部、及上部與底部之中間部這3個位置具有攪拌翼之攪拌裝置。具體而言，可列舉：高黏度高剪切複合攪拌裝置(製品名：NANOVisK，Sumitomo Heavy Industries Process Equipment股份有限公司製造)、或真空乳化攪拌裝置(MIZUHO INDUSTRIAL股份有限公司製造)。
於上述(1)及(2)之製造方法中，若需要，則亦可使用有機溶劑進行反應，繼而進行減壓，藉此去除有機溶劑，而製造聚胺酯樹脂水分散體。
作為有機溶劑，例如可列舉：酮系溶劑(丙酮、甲基乙基酮、甲基異丁基酮、環己酮等)、芳香族系烴溶劑(甲苯、二甲苯、Swasol(Cosmo Oil股份有限公司製造之芳香族系烴溶劑)、Solvesso(Exon Chemical股份有限公司製造之芳香族系烴溶劑)等)、脂肪族系烴溶劑(正己烷等)。該等之中，就操作性之觀點而言，較佳為甲基乙基酮、丙酮及四氫呋喃等。
作為界面活性劑，可列舉：非反應性之非離子性界面活性劑。
作為上述非離子性界面活性劑，例如可列舉：聚氧乙烯烷基醚等二醇醚、及乙炔二醇等。
作為短鏈二胺，可列舉：乙二胺、三亞甲基二胺、六亞甲基二胺及八亞甲基二胺等脂肪族二胺化合物；苯二胺、3,3'-二氯-4,4'-二胺基二苯基甲烷、4,4'-亞甲基雙(苯基胺)、4,4'-二胺基二苯醚及4,4'-二胺基二苯碸等芳香族二胺化合物；環戊烷二胺、環己二胺、4,4-二胺基二環己基甲烷、1,4-二胺基環己烷及異佛爾酮二胺等脂環式二胺化合物；肼、甲二醯肼、己二酸二醯肼、癸二酸二醯肼、鄰苯二甲酸二醯肼等肼類等。該等之中，更佳為肼(水合肼)。
短鏈二醇為數量平均分子量未達500之化合物，可列舉：乙二醇、1,2-丙二醇、1,3-丙二醇、1,3-丁二醇、1,4-丁二醇、1,6-己二醇及新戊二醇等脂肪族二醇類及其氧化伸烷基低莫耳加成物(數量平均分子量未達500)、二乙二醇、三乙二醇、二丙二醇等伸烷基醚二醇；1,4-雙羥基甲基環己烷及2-甲基-1,1-環己烷二甲醇等脂環式系二醇類及其氧化伸烷基低莫耳加成物(數量平均分子量未達500)、苯二甲醇等芳香族二醇類及其氧化伸烷基低莫耳加成物(數量平均分子量未達500)、雙酚A、硫代雙酚及磺化雙酚等雙酚類及其氧化伸烷基低莫耳加成物(數量平均分子量未達500)、及C1~C18之烷基二乙醇胺等烷基二烷醇胺類等化合物。該等之中，較佳為脂肪族二醇類。
<聚胺酯樹脂水分散體中之不揮發成分之量>
於本發明中，由於聚胺酯樹脂水分散體中之不揮發成分為40質量%以上，故而於乾燥步驟中藉由揮發向系外排出之揮發成分之量較少，可削減乾燥所需之能量。
於本發明中，就削減乾燥步驟中使用之能量之觀點而言，聚胺酯樹脂水分散體中之不揮發成分之量較佳為41質量%以上，更佳為45質量%以 上。上限值並無特別限定，例如為70質量%左右。
本發明之聚胺酯樹脂水分散體如上所述揮發成分之量較少，因此與先前相比可容易地去除揮發成分，藉由經過乾燥步驟，能夠使聚胺酯樹脂粒子融合而膜化。此處，所謂膜化係指例如於離型紙上以膜厚度成為40μm之方式塗佈本發明之聚胺酯樹脂水分散體，於120℃下乾燥5分鐘後，可保持膜形態地自剝離紙上剝離。
<添加劑>
本發明之聚胺酯樹脂水分散體視需要可含有添加劑。作為添加劑，例如可列舉：消光劑、抗氧化劑(受阻酚系、亞磷酸酯系、硫醚系等)、光穩定劑(受阻胺系等)、紫外線吸收劑(二苯甲酮系、苯并三唑系等)、氣體變色穩定劑(肼系等)、金屬減活劑等。
作為消光劑，可列舉：樹脂粒子、二氧化矽粒子、滑石、氫氧化鋁、硫酸鈣、矽酸鈣、碳酸鈣、碳酸鎂、碳酸鋇、氧化鋁矽酸鹽、分子篩、高嶺土、雲母及雲母(mica)等。於本發明之聚胺酯樹脂水分散體含有消光劑之情形時，可使作為表皮材之覆膜呈現消光色調。
如上所述之本發明之多孔層結構體若於電子顯微鏡下觀察其剖面，則如圖2所示，基材4上之聚胺酯多孔層1中因發泡產生之氣泡2彼此其一部分合為一體，而共有直徑小於氣泡徑之孔3，從而形成連續氣泡。藉由此種構成，成為柔軟性、耐龜裂性及剝離強度良好之多孔層結構體。
本發明之多孔層結構體可較佳地應用於天然皮革、合成仿革、人工皮革等仿革、塑膠片狀物、各種膜、塑膠成型物、橡膠成型物等。
[實施例]
以下，列舉實施例及比較例對本發明進行更具體之說明，但本發明並不限定於此。又，以下出現之「份」表示質量份、「%」表示質量%。
<作為聚胺酯樹脂水分散體之PUD1~12及比較PUD1~8之製作>
[含末端NCO基之胺酯預聚物合成步驟]
對具備攪拌機、回流冷卻管、溫度計、氮氣吹送管及人孔之反應容器進行氮氣置換後，按照表1及表2中記載之調配，添加多元醇、鏈伸長劑、成為作為親水成分之親水性氧化伸烷基成分的化合物、異氰酸酯，一面攪拌一面升溫，於95℃下反應，藉此獲得末端具有NCO基之胺酯預聚物。
再者，聚異氰酸酯成分之異氰酸基當量相對於全部成分之羥基當量的比(NCO/OH)設為1.5。
[乳化及高分子量化反應]
將所獲得之含末端NCO基之胺酯預聚物移至不鏽鋼容器內，使用裝配有直徑50mm之分散翼之T.K.勻相分散機(特殊機化工工業公司製造)以100~300rpm緩慢攪拌5分鐘。繼而，以表1及2中記載之調配添加界面活性劑，於比較PUD7、8之情形時亦添加中和劑，並進行攪拌直至變得均勻。確認到系內均勻後，以4000~6000rpm強力攪拌10分鐘，並以表1及2中記載之調配添加離子交換水(分散劑)與二胺之混合液，進行乳化並進行高分子量化，藉此獲得作為聚胺酯樹脂水分散體之PUD1~12及比較PUD1~8。
<聚胺酯原料>
‧多元醇A：宇部興產股份有限公司製造之UH-100(聚碳酸酯二醇；數量平均分子量1000)
‧成為親水性氧化伸烷基成分之化合物B：宇部興產股份有限公司製造之PEG1000(聚乙二醇；數量平均分子量1000)
‧成為親水性氧化伸烷基成分之化合物C：Evonic公司製造之TEGOMER D 3403(聚乙二醇單甲醚-1,3-二醇；數量平均分子量1000)
‧成為親水性氧化伸烷基成分之化合物D：日油股份有限公司製造之Uniox M-1000(聚氧乙烯單甲醚；數量平均分子量1000)
‧親水成分E：Bis-MPA(二羥甲基丙酸)
‧鏈伸長劑F：1,4-丁二醇
‧異氰酸酯G：Sumika Covestro Urethane股份有限公司製造之Desmodur W(二環己基甲烷4,4'-二異氰酸酯)
‧二胺H：60%水合肼
‧界面活性劑I：日本乳化劑股份有限公司製造之Newcol 2306-Y(聚氧伸烷基烷基醚；EOPO非離子系界面活性劑)
‧中和劑J：三乙基胺
‧分散介質K：離子交換水
(不揮發成分測定)
使用電子天平計測不鏽鋼容器之重量(g0)，稱取所獲得之各聚胺酯水分散體2g至不鏽鋼容器中(g1)。繼而，將裝有所稱取之聚胺酯水分散體之不鏽鋼容器於120℃下乾燥2小時，計測乾燥後之重量(g2)。根據所獲得之各重量及以下式(1)，測定不揮發成分。
不揮發成分(質量%)=(g2-g0)/(g1-g0)×100 式(1)
(酸值)
比較PUD7、8之酸值係根據親水成分等之調配量，以計算值之方式算出。
Figure 108140605-A0305-02-0025-1
再者，表1、2中之調配之數值為質量份。
Figure 108140605-A0305-02-0026-2
<多孔層結構體之製作>
使用20質量%之硫酸銨水溶液或20質量%之氯化鎂水溶液作為基布含浸用多孔層形成輔助劑(多孔層形成輔助劑A)，將基材(聚酯之圓形針織基布，厚度1mm)浸漬於該水溶液中並塗佈而製成含水基材(含水基材製作步驟)。再者，含水率設為200~400質量%。
製備以表3及表4所示之比率包含多孔層形成輔助劑B(20質量%之硫酸銨水溶液或20質量%之氯化鎂水溶液)、矽酮系添加劑(Shin-Etsu Silicones公司製造之矽酮發泡穩定劑)、水溶性樹脂(15質量%聚乙烯醇水溶液)、聚胺酯系增黏劑(大日精化工業公司製造，RESAMINE D-870T)、及聚胺酯樹脂水分散體之調配液。利用分散翼以3000rpm攪拌調配液2分鐘，藉此以機械發泡之方式進行發泡處理而製成發泡組合物。將其以塗敷厚度成為1000μm之方式塗佈於含水基材上而製成塗膜結構體(塗膜結構體 製作步驟)。
其後，於150℃、5~10分鐘之條件下對塗膜結構體進行乾燥處理(第1乾燥步驟)。
乾燥結束後，藉由45℃之熱水浴將所殘留之多孔層形成輔助劑等洗淨(洗淨步驟)。
確認到已充分洗淨後，去除多餘之水分，於120℃、5~10分鐘之條件下進行乾燥處理(第2乾燥步驟)，而獲得實施例1~24、比較例1~20之多孔層結構體(合成仿革)。
<胺酯多孔層之密度>
將所製作之多孔層結構體切成10cm×10cm見方，基於下述式算出胺酯多孔層之密度。
(1)多孔層結構體之重量測定及計算
根據多孔層結構體整體之重量：A、塗敷基材之重量：B，自下述式求出胺酯多孔層之重量：C。
C=A-B(g)
(2)多孔層結構體之厚度測定及計算
根據多孔層結構體整體之厚度：D、塗敷基材之厚度：E，自下述式求出胺酯多孔層之厚度：F。
F=D-E(cm)
(3)胺酯多孔層之密度計算
藉由下述式求出胺酯多孔層之密度。
胺酯多孔層密度=C÷(F×10×10)(g/cm3)
<評估方法>
(表面龜裂評估方法)
藉由目視確認於所製作之多孔層結構體之中央部分10cm×10cm之範圍內有無長度1mm以上之龜裂存在，並進行評估。
○：無龜裂、×：有龜裂
(剝離評估)
於所製作之多孔層結構體之樹脂塗敷面熱壓接Polycotape 6000號(奧田產業公司製造)，藉由自動立體測圖儀(島津製作所公司製造)測定T型剝離強度。
(透濕度)
自所製作之多孔層結構體切出試驗片，依據JIS L1099 A-1(氯化鈣法)評估多孔層結構體之透濕度A。
(透濕度損失比率)
測定所製作之多孔層結構體之透濕度A及結構體所使用之基材之透濕度B，藉由下述式算出透濕度損失比率。
透濕度損失比率(%)=(1-(多孔層結構體透濕度A/基材透濕度B))×100
再者，基材之透濕度B係對用於製作多孔層結構體之基材進行切割，並依據JIS L1099 A-1(氯化鈣法)評估透濕度。
Figure 108140605-A0305-02-0029-3
Figure 108140605-A0305-02-0030-4
實施例均耐龜裂性、剝離強度良好。再者，比較例無法測定之原因在於：因表面產生龜裂而無法進行正常值測定(比較例1、3、5、7、8、9、11、13、15、16、20)，或因水滲入至基材多孔層間而無法進行正常值測定(比較例17、18)。
10:基材
10A:含水基材
10B:塗膜結構體
10C:多孔質結構體
12A:輥
12B:輥
12C:輥
12D:輥
12E:輥
12F:輥
12G:輥
12H:輥
12J:對輥
14:含水處理槽
14A:基材處理用水溶液
16:發泡組合物
17:刮漿板
18:發泡槽
19:乾燥裝置
20:洗淨槽
20A:洗淨水
22:洗淨槽

Claims (5)

  1. 一種多孔層結構體，其係包含基材、與形成於該基材上而成之聚胺酯多孔層者，藉由JIS L1099 A-1(氯化鈣法)對上述多孔層結構體進行測定所獲得之透濕度A為2000~10000g/(m2‧24h)，根據藉由JIS L1099 A-1(氯化鈣法)對上述基材單獨進行測定所獲得之透濕度B與上述透濕度A，並利用下述式所獲得之透濕度損失比率為75%以下，且基材與聚胺酯多孔層之接合面之剝離強度為0.7kgf/in以上，式) 透濕度損失比率(%)=(1-(透濕度A/透濕度B))×100。
  2. 如請求項1之多孔層結構體，其中上述聚胺酯多孔層之厚度為0.1~1.0mm，且上述聚胺酯多孔層之密度為0.10~0.90g/cm3。
  3. 一種多孔層結構體之製造方法，其係如請求項1或2之多孔層結構體之製造方法，且包括如下步驟：(1)含水基材製作步驟，其係於基材塗佈基材處理用水溶液而製成含水基材，該基材處理用水溶液包含含有至少一種以上之鹽之多孔層形成輔助劑A；(2)塗膜結構體製作步驟，其係於上述含水基材上塗佈發泡組合物而製成塗膜結構體，該發泡組合物係對包含含有至少一種以上之鹽之多孔層形成輔助劑B、發泡穩定劑、水溶性樹脂及聚胺酯樹脂水分散體之調配液 進行發泡處理而成；(3)第1乾燥步驟，其係對上述塗膜結構體實施乾燥處理；(4)洗淨步驟，其係於第1乾燥步驟後進行洗淨；及(5)第2乾燥步驟，其係於洗淨步驟後實施乾燥處理；並且上述聚胺酯樹脂水分散體中之聚胺酯樹脂粒子包含多元醇成分、異氰酸酯成分、及具有1個以上之活性氫基且具有氧化伸烷基(alkylene oxide)之親水性氧化伸烷基成分，且上述親水性氧化伸烷基成分相對於聚胺酯樹脂粒子之含量為1~25質量%。
  4. 如請求項3之多孔層結構體之製造方法，其中於上述含水基材製作步驟、上述塗膜結構體製作步驟及上述洗淨步驟中，實質上不使用有機溶劑。
  5. 如請求項3或4之多孔層結構體之製造方法，其中上述發泡處理為機械發泡。
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