TWI555833B - 水性乳液組成物 - Google Patents
水性乳液組成物 Download PDFInfo
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- TWI555833B TWI555833B TW102110204A TW102110204A TWI555833B TW I555833 B TWI555833 B TW I555833B TW 102110204 A TW102110204 A TW 102110204A TW 102110204 A TW102110204 A TW 102110204A TW I555833 B TWI555833 B TW I555833B
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- acid
- fluorine
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- 239000000203 mixture Substances 0.000 title claims description 23
- 239000000839 emulsion Substances 0.000 title claims description 21
- 229910052731 fluorine Inorganic materials 0.000 claims description 45
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 40
- 239000011737 fluorine Substances 0.000 claims description 39
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 38
- 125000000217 alkyl group Chemical group 0.000 claims description 33
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- 229910052799 carbon Inorganic materials 0.000 claims description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
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- 239000002981 blocking agent Substances 0.000 description 4
- 125000005843 halogen group Chemical group 0.000 description 4
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
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- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical group NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 description 3
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- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- YFYABWXIJBTAAM-UHFFFAOYSA-M trimethyl(2-phenyltetradecan-2-yl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCC(C)([N+](C)(C)C)C1=CC=CC=C1 YFYABWXIJBTAAM-UHFFFAOYSA-M 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
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Description
本發明為關於一種水性乳液組成物,在以水性乳液加工處理時,在處理浴中存在有雜質時之安定性、及加工處理浴對機械衝擊之安定性優異,且可維持高的撥水撥油性及在該方面之耐久性。
已知具有全氟烷基或全氟烯基及丙烯酸基或甲基丙烯酸基之聚合性化合物的聚合物可作為纖維織物之撥水撥油劑,特別是該聚合物再以乳化劑分散在水性介質中之水性分散液已廣泛使用在工業上。
然而,在先前之一般水性分散液經過稀釋調合之撥水撥油劑加工浴中,經常發生:在加工處理中由前處理步驟混入附著在加工布等中之雜質,或水性分散液之分散性降低而發生乳液粒子凝集、沉降,或者因受所處理之布材在放入處理浴中時及取出時之機械衝擊而使分散液崩解,引起乳液粒子凝集、沉降,因此降低撥水撥油性能、及在滾輪上附著聚合物而污染布材之問題。因此,先前之水性分散液對雜質之安定性、及在處理步驟中之機械安定性並不充足。
對雜質之安定性優異的方法方面,已有下述提案:日本特開平9-118877號公報、日本特開平9-125051號公報、日本特開平9-302335號公報、日本特開平9-118877號公報、日本特開平9-125051號公報、日本特開2000-169735號公報,惟近年來,隨著撥水撥油加工之多樣性,並未達到可提供完全令人滿意之安定性。
[專利文獻1]日本特開平9-118877號公報
[專利文獻2]日本特開平9-125051號公報
[專利文獻3]日本特開平9-302335號公報
[專利文獻4]日本特開平9-118877號公報
[專利文獻5]日本特開平9-125051號公報
[專利文獻6]日本特開2000-169735號公報
本發明之目的所提供之水性乳液組成物,係具有優異之化學安定性(對雜質之安定性)及機械安定性者。
亦即,本發明提供一種水性乳液組成物,係包含:(A)含氟烷基之聚合物
(B)包含具有醯胺基及胺基之醯胺-胺界面活性劑的界面活性劑。
特別是,本發明提供一種水性乳液組成物,係包含:(A)含氟烷基之聚合物(B)界面活性劑,包含(B1)具有醯胺基及胺基之醯胺-胺界面活性劑(B2)非離子性界面活性劑。
本發明之水性乳液組成物,在處理浴中存在有雜質(如:染料固定劑)時之安定性、及加工處理浴中對機械衝擊之安定性優異,且可維持高的撥水撥油性及在該方面之耐久性。該水性乳液組成物不會引起粒子之沉降,亦不使滾輪上附著聚合物而污染布材的情形發生。
本發明之水性乳液組成物,可使用作為表面處理劑,如:撥水撥油劑、防污加工劑使用。
本發明之表面處理劑,可賦予優異之撥水撥油性、防污性及在該方面之耐久性。
本發明之水性乳液組成物係含氟聚合物之水性乳液。
本發明之水性乳液組成物係包含:
(A)含氟烷基之聚合物、(B)包含具有醯胺基及胺基之醯胺-胺界面活性劑的界面活性劑、及(C)水介質。
含氟聚合物係:具有由含氟單體所衍生之重複單元的均聚合物、具有由2種以上之含氟單體所衍生的重複單元之共聚物、或具有由可與由含氟單體所衍生之重複單元共聚之其它聚合性化合物所衍生之重複單元的共聚物。
本發明中,含氟聚合物(A)宜具有下述重複單元:(A1)由含氟單體所衍生之重複單元、及(A2)依其必要而存在之由非氟非交聯性單體所衍生之重複單元、(A2)依其必要而存在之由非氟交聯性單體所衍生之重複單元。
[(A1)含氟單體]
含氟單體一般為具有全氟烷基或全氟烯基及丙烯酸基或甲基丙烯酸基或α-取代丙烯酸基之聚合性化合物。
含氟單體以下述式所示之化合物為佳:CH2=C(-X)-C(=O)-Y-Z-Rf[式中,X為氫原子、一價有機基或鹵素原子;Y為-O-或-NH-;Z為直接鍵結或二價有機基;Rf為碳數1至20之氟烷基。]。Z可為例如:碳數1至20之直鏈或支鏈之脂族
基(尤其是伸烷基),可例舉如:式-(CH2)x-(式中,x為1至10。)所示之基、或式-R2(R1)N-SO2-或式-R2(R1)N-CO-所示之基(式中,R1為碳數1至10之烷基;R2為碳數1至10之直鏈伸烷基或支鏈伸烷基。)、或式-CH2CH(OR3)CH2-(Ar-O)p-(式中,R3為氫原子、或碳數1至10之醯基(如:甲醯基或乙醯基等);Ar為視其必要含取代基之伸芳基;p表示0或1。)所示之基、或式-CH2-Ar-(O)q-(式中,Ar為視其必要含取代基之伸芳基;q為0或1。)所示之基、-(CH2)m-SO2-(CH2)n-基或-(CH2)m-S-(CH2)n-基(但,m為1至10,n為0至10)。
含氟單體(A1)係以下述通式(I)所示之丙烯酸酯為佳:CH2=C(-X)-C(=O)-Y-Z-Rf (I)[式中,X為氫原子、碳數1至21之直鏈或支鏈之烷基、氟原子、氯原子、溴原子、碘原子、CFX1X2基(但,X1及X2為氫原子、氟原子、氯原子、溴原子或碘原子。)、氰基、碳數1至21之直鏈或支鏈之氟烷基、取代或非取代之苯甲基、取代或非取代之苯基;Y為-O-或-NH-;Z為碳數1至10之脂基、碳數6至18之芳基或環脂基、-CH2CH2N(R1)SO2-基(但,R1為碳數1至4之烷基。)、-CH2CH(OZ1)CH2-(Ph-O)p-基(但,Z1為氫原子或乙醯基;Ph為伸苯基;p為0或1。)、-(CH2)n-Ph-O-基(但,Ph為伸苯基;n為0至10。)、-(CH2)m-SO2-(CH2)n-基或-(CH2)m-S-(CH2)n-基(但,m為1至10;n為0至10。);Rf為碳數1至20之直鏈或支鏈之氟烷基。]。
含氟單體中,Rf基以全氟烷基較佳。Rf基之碳數,以1至12,如1至6為佳,特別以4至6更佳。Rf基之例,可舉如:-CF3-、-CF2CF3、-CF2CF2CF3、-CF(CF3)2、-CF2CF2CF2CF3、-CF2CF(CF3)2、-C(CF3)3、-(CF2)4CF3、-(CF2)2CF(CF3)2、-CF2C(CF3)3、-CF(CF3)CF2CF2CF3、-(CF2)5CF3、-(CF2)3CF(CF3)2、-(CF2)4CF(CF3)2、-C8F17等。
Z係以碳數1至10之脂基、碳數6至18之芳基或環脂基、-CH2CH2N(R1)SO2-基(但,R1為碳數1至4之烷基。)、-CH2CH(OZ1)CH2-(Ph-O)p-基(但,Z1為氫原子或乙醯基;Ph為伸苯基;p為0或1。)、-(CH2)n-Ph-O-基(但,Ph為伸苯基;n為0至10。)、-(CH2)m-SO2-(CH2)n-基或-(CH2)m-S-(CH2)n-基(但,m為1至10;n為0至10。)較佳。脂基係以伸烷基(特別為碳數1至4,如1或2。)較佳。芳基或環脂基可取代亦可未被取代。S基或SO2基亦可直接鍵結於Rf基。
含氟單體(A1)之具體例,可舉以下所示之例,但並不限於此。
CH2=C(-H)-C(=O)-O-(CH2)2-Rf
CH2=C(-H)-C(=O)-O-C6H4-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)2-Rf
CH2=C(-H)-C(=O)-O-(CH2)2N(-CH3)SO2-Rf
CH2=C(-H)-C(=O)-O-(CH2)2N(-C2H5)SO2-Rf
CH2=C(-H)-C(=O)-O-CH2CH(-OH)CH2-Rf
CH2=C(-H)-C(=O)-O-CH2CH(-OCOCH3)CH2-Rf
CH2=C(-H)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-H)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-H)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-H)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-H)-C(=O)-NH-(CH2)2-Rf
CH2=C(-CH3)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-CH3)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-CH3)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-CH3)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-CH3)-C(=O)-NH-(CH2)2-Rf
CH2=C(-F)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-F)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-F)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-F)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-F)-C(=O)-NH-(CH2)2-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-Cl)-C(=O)-NH-(CH2)2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-CF3)-C(=O)-NH-(CH2)2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-CF2H)-C(=O)-NH-(CH2)2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-CN)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-CN)-C(=O)-NH-(CH2)2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)2-S-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)2-S-(CH2)2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)2-SO2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)2-SO2-(CH2)2-Rf
CH2=C(-CF2CF3)-C(=O)-NH-(CH2)2-Rf
CH2=C(-F)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-F)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-F)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-F)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf
CH2=C(-F)-C(=O)-NH-(CH2)3-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-Cl)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-CF3)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-CF2H)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-CN)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-CN)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)3-S-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)3-S-(CH2)2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)3-SO2-Rf
CH2=C(-CF2CF3)-C(=O)-O-(CH2)3-SO2-(CH2)2-Rf[上述式中,Rf,為碳數1至20之氟烷基。]
[(A2)非氟非交聯性單體]
非氟非交聯性單體(A2),係不含氟原子之單體。非氟非交聯性單體(A2)並不具有交聯性官能基。非氟非交聯性單體(A2)與交聯性單體(A3)不同,為非交聯性。非氟非交聯性單體(A2),以具有碳-碳雙鍵之非氟單體較佳。非氟非交聯性單體(A2),以不含氟之乙烯基單體更佳。非氟非交聯性單體(A2),一般為具有1個碳-碳雙鍵之化合物。
較佳之非氟非交聯性單體(A2)為下述式所示之化合物:CH2=CA-T[式中,A為氫原子、甲基、或者氟原子以外之鹵素原子(如氯原子、溴原子及碘原子);T為氫原子、碳數1至20之鏈狀或環狀之烴基、或具有酯鍵之鏈狀或環狀之碳數1至20之有機基。]。
碳數1至20之鏈狀或環狀之烴基之例,可舉如:碳數1至20之直鏈或支鏈的脂族烴基、碳數4至20之環脂族基、碳數6至20之芳族烴基、碳數7至20之芳脂族烴基。
具有酯鍵之鏈狀或環狀之碳數1至20之有機基之例,可舉如:-C(=O)-O-Q及-O-C(=O)-Q(其中,Q,為碳數1至20之直鏈或支鏈之脂族烴基、碳數4至20之環脂族基、碳數6至20之芳族烴基、碳數7至20之芳脂族烴基)。
非氟非交聯性單體(A2)之較佳例,包含如:乙烯、乙酸乙烯酯、丙烯腈、苯乙烯、聚乙二醇(甲基)丙烯酸酯、聚丙二醇(甲基)丙烯酸酯、甲氧基聚乙二醇(甲基)丙烯酸酯、甲氧基聚丙二醇(甲基)丙烯酸酯、及乙烯基烷基醚。但非氟非交聯性單體(A2)並不限於該等例。
非氟非交聯性單體(A2)可為含烷基之(甲基)丙烯酸酯。烷基之碳原子數可為1至30,例如可為:6至30(如10至30)。例如,非氟非交聯性單體(A2)可為下述通式所示之丙烯酸酯:CH2=CA1COOA2[式中,A1為氫原子、甲基、或者氟原子以外之鹵素原子(如氯原子、溴原子及碘原子);A2為CnH2n+1(n=1至30)所示之烷基。]。
非氟非交聯性單體(A2)可為具有環烴基之(甲基)丙烯酸酯單體。具有環烴基之(甲基)丙烯酸酯單體為具有(最好為一價之)環烴基及一價之(甲基)丙烯酸酯基之化合物。一價之環烴基及一價之(甲基)丙烯酸酯基為直接鍵結者。環烴基可舉如:飽和或不飽和之單環基、多環基、交聯環基等。環烴基以飽和者較佳。環烴基之碳數以4至20者較佳。環烴基之例,可舉如:碳數4至20,特別是碳數5至12之環脂基、碳數6至20之芳族基、碳數7至20之芳脂族基。環烴基之碳數,以15以下為佳,特別以如10以下更佳。環烴基之環中的碳原子,以與(甲基)丙烯酸酯基中之酯基直接鍵結者較佳。環烴基以飽和之環脂基較
佳。環烴基之具體例可舉如:環己基、三級丁基環己基、異莰基、二環戊基、二環戊烯基。(甲基)丙烯酸酯基係丙烯酸酯基或甲基丙烯酸酯基,而以甲基丙烯酸酯基較佳。具有環烴基之單體的具體例,可舉如:甲基丙烯酸環己酯、甲基丙烯酸三級丁基環己酯、甲基丙烯酸苯甲酯、甲基丙烯酸異莰酯、丙烯酸異莰酯、甲基丙烯酸二環戊酯、丙烯酸二環戊酯、丙烯酸二環戊烯酯等。
非氟非交聯性單體(A2)亦可為鹵化烯烴。鹵化烯烴,亦可為由1至10個之氯原子、溴原子或碘原子取代之碳數2至20之鹵化烯烴。鹵化烯烴(b),以碳數2至20之氯化烯烴為佳,特別以具有1至5個氯原子之碳數2至5的烯烴更佳。鹵化烯烴(b)之較佳具體例,可舉如:鹵化乙烯,係如:氯化乙烯、溴化乙烯、碘化乙烯;鹵化亞乙烯,係如:氯化亞乙烯、溴化亞乙烯、碘化亞乙烯。
[(A3)非氟交聯性單體]
本發明之含氟聚合物,亦可含由非氟交聯性單體(A3)所衍生之重複單元。非氟交聯性單體(A3)係不含氟原子之單體。非氟交聯性單體(A3),亦可為具有至少2個反應性基及/或碳-碳雙鍵,且不含氟之化合物。非氟交聯性單體(A3),亦可為具有至少2個碳-碳雙鍵之化合物,或至少1個碳-碳雙鍵及至少1個反應性基之化合物。反應性基之例,可舉如:羥基、環氧基、氯化甲基、封端異氰酸酯基(blocked isocyanate group)、胺基、羧基等。
非氟交聯性單體(A3)之例,可舉如:二丙酮
丙烯醯胺、(甲基)丙烯醯胺、N-羥甲基丙烯醯胺、(甲基)丙烯酸羥基甲酯、(甲基)丙烯酸羥基乙酯、(甲基)丙烯酸-3-氯-2-羥基丙酯、(甲基)丙烯酸-2-乙醯基乙醯氧基乙酯、(甲基)丙烯酸-N,N-二甲基胺基乙酯、(甲基)丙烯酸-N,N-二乙基胺基乙酯、丁二烯、異戊二烯、氯丁二烯、(甲基)丙烯酸環氧丙酯等,但並不限於此。
藉由使非氟非交聯性單體(A2)及/或非氟交聯性單體(A3)共聚,可使撥水撥油性及防污性以及此等性能之耐洗淨性、耐洗滌性、對溶劑之溶解性、硬度、觸感等之各種性質依必要而改善。
單體可在選自封端異氰酸酯化合物及有機聚矽氧烷化合物所成之群組的至少1種化合物之存在下進行聚合。封端異氰酸酯化合物(或有機聚矽氧烷化合物)之量,相對於單體100重量份,以0至100重量份為佳,亦可為如1至50重量份。
單體在封端異氰酸酯化合物存在下聚合時,即可得到具有封端異氰酸酯基之含氟聚合物。封端異氰酸酯化合物,係以至少1種封端劑所封端之異氰酸酯。當中封端劑之例可列舉如:肟類、酚類、醇類、硫醇類、醯胺類、亞胺類、咪唑類、尿素類、胺類、亞胺類、吡唑類及活性亞甲基化合物類。封端劑之其它例可舉如:羥基吡啶(pyridinol)類、硫酚類、二酮類及酯類。封端異氰酸酯化合物,亦可再以具親水性基之化合物加以改質。
單體在有機聚矽氧烷化合物(如:硫醇基官
能性有機聚矽氧烷、乙烯基官能性有機聚矽氧烷)存在下聚合時,即可得到含矽氧烷基之含氟聚合物。其一實施形態中,硫醇基官能性有機聚矽氧烷具有包含下述平均式之矽氧單位:(R2SiO)a(RRNSiO)b(RRSSiO)c[式中,a為0至4000、0至1000、或0至400;b為1至1000、1至100、或1至50;c為1至1000、1至100、或1至50;R為獨立之一價有機基,或R為碳數1至30之烴,或R為碳數1至12之一價烷基,或者R為甲基;RN為如上述定義之一價胺基官能性有機基;RS為如上述定義之一價氫硫基官能性有機基。]。
含氟聚合物中,相對於含氟單體(A1)100重量份,非氟非交聯性單體(A2)之量可為1000重量份以下,如為0.1至300重量份,特別為1至200重量份;非氟交聯性單體(A3)之量為50重量份以下,如為30重量份以下,特別為0.1至20重量份。
含氟聚合物之數量平均分子量(Mn),一般可為1000至1000000,如可為2000至500000,特別為3000至200000。含氟聚合物之數量平均分子量(Mn)一般係以GPC(凝膠滲透層析法)測定。
界面活性劑(B)係包含(B1)醯胺-胺界面活性劑。
界面活性劑(B)係除了醯胺-胺界面活性劑(B1)之外,亦可包含其它之界面活性劑,例如:選自非離子性界面活性
劑(B2)及陽離子性界面活性劑(B3)所成之群的至少1種之界面活性劑。以及,其它之界面活性劑,可列舉如:具有氧伸烷基之胺界面活性劑、氧化胺(amine oxide)界面活性劑、兩性界面活性劑。
本發明中,界面活性劑方面,以不使用(在日本特開2000-169735號公報中記載之)具有不飽和三鍵的一元醇或多元醇之(至少含有1個OH基)環氧烷加成物(至少1種之化合物)為佳。
[(B1)醯胺-胺界面活性劑]
醯胺-胺界面活性劑係具有醯胺基及胺基之化合物。
醯胺-胺界面活性劑係以下述式所示之化合物為佳:R1-CONH-(CH2)n-N(R2)(R3)[式中,R1為碳數8至30之烷基或烯基;R2及R3為碳數1至6之烷基;n為1至10。]。
R1以碳數12至24之烷基或烯基較佳。R2及R3以碳數1至4之烷基較佳。n以2至5較佳。
醯胺-胺界面活性劑之具體例,可舉如:二乙基胺基乙基異硬脂醯胺、二甲基胺基乙基油醯胺、二甲基胺基丙基油醯胺、二乙基胺基乙基油醯胺、二乙基胺基丙基油醯胺、二乙基胺基乙基硬脂醯胺、二乙基胺基丙基硬脂醯胺、二丁基胺基乙基硬脂醯胺、二丁基胺基丙基硬脂醯胺、二丙基胺基丙基硬脂醯胺、二丙基胺基乙基硬脂醯胺、二甲基胺基乙基硬脂醯胺、二甲基胺基丙基硬脂醯胺、二乙基胺基乙基棕櫚醯胺、二乙基胺基丙基棕櫚醯胺、
二甲基胺基乙基棕櫚醯胺、二甲基胺基丙基棕櫚醯胺、二乙基胺基乙基二十二烷醯胺、二乙基胺基丙基二十二烷醯胺、二甲基胺基丙基二十二烷醯胺等。
醯胺-胺界面活性劑,亦可為鹽,如:酸鹽或4級銨鹽。該鹽之中,陽離子基為胺基之氮原子,陰離子基為各種基。陰離子基之例,可舉如:鹵素離子、硫酸根離子、可為羥基取代之碳數1至4之羧酸根離子、或碳數1至4之烷基硫酸根離子。
酸鹽係可將醯胺-胺以酸,如:無機酸及/或有機酸中和而得到。無機酸之例,可舉如:鹽酸、硫酸及磷酸等。有機酸之例,可舉如:乙酸、丙酸等之短鏈單羧酸;月桂酸、肉豆蔻酸、棕櫚酸、硬脂酸、油酸、二十二烷酸、芥酸等之長鏈單羧酸;丙二酸、丁二酸、戊二酸、己二酸、順丁烯二酸、反丁烯二酸、苯二甲酸等之二羧酸;乙醇酸、乳酸、羥基丙烯酸、甘油酸、蘋果酸、酒石酸、檸檬酸等之羥基羧酸;聚麩胺酸等之多元羧酸;麩胺酸、天冬胺酸等之酸性胺基酸;烷基硫酸酯、烷基磺酸酯、烷基磷酸酯等。其中,一般使用:無機酸、短鏈單羧酸、二羧酸、羥基羧酸、酸性胺基酸,特別以使用:鹽酸、硫酸、乙酸、琥珀酸、乙醇酸、乳酸、蘋果酸、檸檬酸、麩胺酸為佳。
4級銨鹽,可以醯胺-胺經過4級化而得到。
醯胺-胺界面活性劑,可為非離子性或離子性(陽離子性),而以非離子性者為佳。亦即,本發明中,
為使醯胺-胺界面活性劑不具離子性,以不添加酸等離子性化物質為佳。
[(B2)非離子性界面活性劑]
非離子性界面活性劑,係具有氧伸烷基之非離子性界面活性劑。該氧伸烷基中的伸烷基之碳數,以2至10為佳。非離子性界面活性劑之分子中的氧伸烷基之數,一般以2至100為佳。
非離子性界面活性劑可為直鏈狀及/或支鏈狀之脂族(飽和及/或不飽和)基之環氧烷加成物、直鏈狀及/或支鏈狀之脂酸(飽和及/或不飽和)之聚烷二醇酯、聚氧伸乙基(POE)/聚氧伸丙基(POP)共聚物(無規共聚物或嵌段共聚物)、乙炔二醇(acetylene glycol)之環氧烷加成物等。此等之中,以環氧烷加成部分及聚烷二醇部分之構造為聚氧伸乙基(POE)或聚氧伸丙基(POP)或POE/POP共聚物(可為無規共聚物亦可為嵌段共聚物)為佳。
同時,非離子性界面活性劑,在環境上之問題(生物分解性、環境荷爾蒙等)之觀點上以不含芳族基之構造為佳。
非離子性界面活性劑可為下述式所世之界面活性劑:R1O-(CH2CH2O)p-(R2O)q-R3[式中,R1為碳數1至22之烷基或碳數2至22之烯基或醯基;R2為碳數3以上(如:3至10)之伸烷基;R3為氫原子、碳數1至22之烷基或碳數2至22之烯基;p為2以上之數;q為0或1以上之數。]。
R1以碳數8至20為佳,特別以10至18更佳。R1之較佳具體例可舉如:月桂基、十三烷基、油基。
R2之例可舉如:伸丙基、伸丁基。
非離子性界面活性劑中,p可為3以上之數(如:5至200)。q可為2以上之數(如:5至200)。亦即,-(R2O)q-可形成聚氧伸烷基鏈。
非離子性界面活性劑可為中央含有親水性之聚氧伸乙基鏈及疏水性之氧伸烷基鏈(特別是,聚氧伸烷基鏈)之聚氧伸乙基伸烷基烷基醚。疏水性之氧伸烷基鏈之例可舉如:氧伸丙基鏈、氧伸丁基鏈、苯乙烯鏈等,當中以氧伸丙基鏈較佳。
較佳之非離子性界面活性劑為下述式所示之界面活性劑:R1O-(CH2CH2O)p-H[式中,R1及p與上述同義。]。
非離子性界面活性劑之具體例可舉如:
C10H21O-(CH2CH2O)p-(C3H6O)q-H
C12H25O-(CH2CH2O)p-(C3H6O)q-H
C16H31O-(CH2CH2O)p-(C3H6O)q-H
C16H33O-(CH2CH2O)p-(C3H6O)q-H
C18H35O-(CH2CH2O)p-(C3H6O)q-H
C18H37O-(CH2CH2O)p-(C3H6O)q-H
C12H25O-(CH2CH2O)p-(C3H6O)q-C12H25
C16H31O-(CH2CH2O)p-(C3H6O)q-C16H31
C16H33O-(CH2CH2O)p-(C3H6O)q-C12H25
iso-C13H27O-(CH2CH2O)p-(C3H6O)q-H
C10H21COO-(CH2CH2O)p-(C3H6O)q-H
C16H33COO-(CH2CH2O)p-(C3H6O)q-C12H25[式中,p及q與上述同義。]等。
非離子性界面活性劑之具體例,係包含:環氧乙烷與己基酚、異辛基酚、十六烷醇、油酸、烷(C12至C16)硫醇、山梨糖醇酐單脂酸(C7至C19)或烷基(C12至C18)胺等之縮合生成物。
聚氧伸乙基嵌段之比例,相對於非離子性界面活性劑(共聚物)之分子量可為5至80重量%,例如為30至75重量%,特別是40至70重量%。
非離子性界面活性劑之平均分子量,一般為300至5,000,例如為500至3,000。
非離子性界面活性劑可單獨使用1種,亦可將2種以上併用。
非離子性界面活性劑以2種以上之組合較佳。在2種以上之組合中,至少1種之非離子性界面活性劑可為R1基(及/或R3基)為支鏈之烷基(例如:異十三烷基)的R1O-(CH2CH2O)p-(R2O)q-R3[特別是,R1O-(CH2CH2O)p-H]所示之化合物。R1基為支鏈烷基的非離子性界面活性劑之量,相對於非離子性界面活性劑(B2)的合計100重量份,可為5至100重量份,例如為8至50重量份,特別為10至40重
量份。在以2種以上組合時,其餘之非離子性界面活性劑可為R1基(及/或R3基)為(飽和及/或不飽和之)直鏈烷基(如:月桂基(正月桂基))之R1O-(CH2CH2O)p-(R2O)q-R3[特別是R1O-(CH2CH2O)p-H]所示之化合物。
[(B3)陽離子性界面活性劑]
陽離子性界面活性劑以不具醯胺基之化合物為佳。
陽離子性界面活性劑以銨鹽為佳。陽離子性界面活性劑,可為下述式所示之銨鹽:R1 p-N+R2 qX-[式中,R1為C12以上(如:C12至C50)之直鏈狀及/或支鏈狀之脂族(飽和及/或不飽和)基;R2為H或C1至4之烷基、苯甲基、聚氧伸乙基(氧伸乙基之數例如為1(特別是2,尤其是3)至50)(特別以CH3、C2H5更佳);X為鹵素原子(如:氯原子、溴原子及碘原子)、C1至C4之脂酸鹽基;p為1或2;q為2或3;p+q=4。]。R1之碳數,為12至50,如以12至30為佳。
陽離子性界面活性劑之具體例係包含:乙酸十二烷基三甲基銨、氯化三甲基十四碳烷基銨、溴化十六烷基三甲基銨、氯化三甲基十八烷基銨、氯化(十二烷基甲基苯甲基)三甲基銨、氯化苯甲基十二烷基二甲基銨、氯化甲基十二烷基二(氫化聚氧伸乙基)銨、氯化苯甲基十二烷基二(氫化聚氧伸乙基)銨、N-[2-(二乙基胺基)乙基]油醯胺鹽酸鹽。
本發明之組成物視必要亦可含有消泡劑。
特別在因含有界面活性劑而有起泡變多之虞慮時,即有含消泡劑之必要。消泡劑方面,可使用各種水性用者,例如:甲醇、乙醇、丁醇等之類之低級醇;戊醇、聚丙二醇及其衍生物等之類之高級醇;油酸、松油(tall oil)、礦物油、皂等之類之油脂;山梨糖醇酐脂酸酯、聚乙二醇脂酸酯、普盧蘭尼克(Pluronic)型非離子性界面活性劑等之類之界面活性劑;矽氧烷、聚矽氧樹脂等之類之矽氧烷系界面活性劑;可單獨或合併使用。代表性之消泡劑的市售商品,可舉如:ADEKA NATE B、ADEKA NATE B1068等之B系列商品(旭電化工業公司製造);Foamaster DL、NOPCO NXZ、SN Defoamer 113、325、308、368等之SN Defoamer系列商品;Dehydran 1293、Dehydran 1513〔SAN NOPCO公司製造〕;FLOWNON SB-110N、SB-210、510、551、AQUALEN 800、805、AQUALEN 1488〔共榮社化學公司製造〕;Surfynol 104E(Air Products & Chemicals公司製造乙炔系消泡劑);KS-607A〔信越化學社公司製造〕;FS Antifoam(Dow & Corning公司製造);BYK-020、031、073、W(BYK-Chmei公司製造);Dehydran 981(Henkel白水社公司製造);EPAN-410、710、720〔第一工業製藥公司製造〕;Tego Foamex系列商品(TEGO Goldschmidt公司製造);FOAMLEX-747、TY-10、EP系列商品(日華化學社公司製造)等。消泡劑之含量相對於水性乳液,係以0.01至10重量%為佳,特別以0.05至5重量%更佳。
水介質(C),係水單獨、或水與有機溶劑之
混合物(水與有機溶劑之重量比為99.99:0.01至70:30)。有機溶劑(水溶性有機溶劑)可使聚合物之分散性更佳。該有機溶劑之例可舉如:丙酮、甲基乙基酮之類之酮類;乙二醇、聚乙二醇之類之乙二醇衍生物;及聚乙二醇單甲醚、聚乙二醇二甲醚、聚乙二醇單丁醚之類之乙二醇衍生物之烷基醚類;丙二醇、二丙二醇、三丙二醇、聚丙二醇之類之丙二醇衍生物;環狀糊精、糊精之類之聚醚類;乙酸甲酯、乙酸乙酯之類之酯類;N-烷基吡咯啶酮等。有機溶劑之量以聚合物每100重量份可為5至200重量份,如以10至100重量份為佳,特別以20至80重量份更佳。
或者亦可視必要,在水性分散液中含:交聯劑、其它之聚合物、其它之撥水劑、撥油劑、防蟲劑、阻燃劑、抗靜電劑、染料安定劑、防縐劑等之添加劑等。
交聯劑之例,可舉如以:封端異氰酸酯化合物、三聚氰胺樹脂化合物、乙二醛系樹脂化合物、脲系樹脂化合物、交聯性單體(N-羥甲基丙烯醯胺、2-異氰酸根合甲基丙烯酸乙酯之封端化物等)為必須之聚合單位的聚合物等,而以封端異氰酸酯化合物或三聚氰胺樹脂化合物較佳。當中,封端異氰酸酯化合物方面,係不具有聚合性不飽和基之化合物,而以多元異氰酸酯中之異氰酸基為封端劑所封端之構造的化合物較佳。三聚氰胺樹脂化合物方面,可例舉如:三羥甲基三聚氰胺、六羥甲基三聚氰胺等。
本發明之水性分散液在製造上,係在聚合起始劑及界面活性劑之存在下以聚合性化合物,在視必要
加入有機溶劑之水中乳化聚合,得到聚合物之乳濁液。界面活性劑方面,醯胺-胺界面活性劑(B1)為必須者。界面活性劑,亦可視必要再含有其它界面活性劑,如:非離子性界面活性劑(B2)及陽離子性界面活性劑(B3)。醯胺-胺界面活性劑(B1)係可在乳化聚合時包含、亦可在聚合後添加。
界面活性劑之使用量,相對於聚合物100重量份,醯胺-胺界面活性劑(B1):可為0.1至20重量份,以0.2至10重量份為佳,例如為0.3至5重量份;非離子性界面活性劑(B2):可為0至20重量份,以0.1至10重量份為佳,例如為1至8重量份;陽離子性界面活性劑(B3):可為0至20重量份,以0.1至10重量份為佳,例如為0.1至5重量份。
一般而言,相對於界面活性劑之合計,醯胺-胺界面活性劑(B1)之比例以5至100重量%為佳,例如為5至50重量%,特別以10至50重量%更佳。
乳化聚合方面,可採用在聚合起始劑及乳化劑之存在下,以單體在水中乳化,經氮氣取代後,在50至80℃之範圍下以1至10小時,進行攪拌進行共聚之方法操作。聚合起始劑,可使用:過氧化苯甲醯、過氧化月桂醯、過苯甲酸三級丁酯、1-羥基環己基氫過氧化物、3-羧基丙醯過氧化物、過氧化乙醯、偶氮二異丁脒-二鹽酸鹽、偶氮二異丁腈、過氧化鈉、過硫酸鉀、過硫酸銨等之水溶性物種及偶氮二異丁腈、過氧化苯甲醯、過氧化二(三
級丁基)、過氧化月桂醯、氫過氧化異丙苯、過氧化三甲基乙酸三級丁酯、過氧化二碳酸二異丙酯等之油溶性物種。聚合起始劑相對於單體100重量份,可在0.01至10重量份之範圍下使用。
為可得到放置安定性優良之共聚物水分散液,可使用高壓均質機及超音波均質機之類可賦予強力粉碎能量之乳化裝置,使單體在水中微粒化,再使用聚合起始劑進行聚合者為佳。在單體並無法完全互溶時,以再添加可使此類單體充分互溶之互溶化劑,如:水溶性有機溶劑及低分子量之單體為佳。在添加互溶化劑時,可使乳化性及共聚性更佳。
水溶性有機溶劑方面,可例舉如:丙酮、甲基乙基酮、乙酸乙酯、丙二醇、二丙二醇單甲醚、二丙二醇、三丙二醇、乙醇等,而相對於水100重量份,以1至50重量份為佳,例如可在10至40重量份之範圍使用。同時,低分子量之單體,可例舉如:甲基丙烯酸甲酯、甲基丙烯酸環氧丙酯、甲基丙烯酸-2,2,2-三氟乙酯等,相對於單體之總量100重量份,可在1至50重量份,例如在10至40重量份之範圍使用。
水性乳液組成物中,含氟共聚物之濃度,例如可為0.01至50重量%。
水性分散液所適用之基體為纖維製品或固體薄片。基體以例如布之薄片狀物為佳。纖維製品之例,可舉如:纖維本身、纖維構成之線、纖維構成之布。固體
薄片係與纖維所構成之布不同,為不存在空隙之薄片。
基體可為薄膜、纖維、線、織布、毯及以天然聚合物物質及經過改質之天然聚合物物質及合成聚合物物質所得到之長纖(filament)、纖維或線所製成之薄片。
本發明之分散液,適合以塗布、浸漬、噴霧、浸軋、滾輪被覆或此類方法組合使用在基體上。例如,先以浴液之固形分量為0.1至10重量%製成浸軋浴使用,其次將基體在該浴液中浸軋,再以壓輥將過剩之液體去除,並乾燥收縮(基體上之乾燥聚合物之重量)成為基體之約0.01至1重量%即可使用。此外處理基體視必要宜再加熱至100至200℃。
本發明中,基體係以處理劑(分散液)處理。所謂「處理」係將處理劑,以浸漬、噴霧、塗布等應用在基體上之意。藉由處理,即可使處理劑之有效成分的含氟聚合物浸透至基體內部及/或附著在基體之表面。
實施例
以下再以所示之實施例及比較例,更詳細說明本發明。其特性係如下測定。
[撥水撥油性]
先將聚合物分散液以水稀釋使固形分濃度成為1重量%之方式而調整處理液。再將聚酯布浸漬於該處理液中,並以壓布機以4kg/cm2、4m/分鐘壓軋,在以170℃加熱處理1分鐘後,再評估處理布之撥水撥油性(HL0)。洗滌耐久性係依照JIS-L-0217-103法,以40℃之洗滌液洗滌10次
後,再以滾筒乾燥機進行乾燥,之後評估其撥水撥油性(HL10)。
該撥水性係依照下述表1所示之JIS-L-1092的噴霧法以撥水性No.表示。
撥油性係依照AATCC-TM118而以下述表2所示之試驗溶液在試驗布上滴3滴,再觀察30秒後之浸透狀態,而以未呈浸漬之試驗溶液所賦予之撥油性的最高點為其撥油性。
[上膠(gum up)性]
先將聚合物分散液以自來水稀釋使固形分濃度為1.8重量%,再將該處理液加入可調整溫度為40℃之浸軋浴中,以壓輥可連續處理成寬度20cm及長度80cm之棉布捲,以壓輥壓力0.55Mpa進行連續處理。經過1小時後,再以目視觀察壓輥之聚合物之附著狀態,並依照下述表3之基準判定上膠性。
[機械安定性]
先將聚合物分散液以自來水稀釋使固形分濃度成為0.9重量%,再調整溫度為40℃並同時以均質機以2,500rpm×5分鐘攪拌,再將發生之渣滓以黑棉布過濾。同樣地,另對以染料固定劑以60ppm添加之情形進行試驗,並依照下述表4之基準判定渣滓產生性。而以無渣滓為佳。
實施例1
在1L之高壓釜中加入140g之C8F17CH2CH2OCOCH=CH2、18g之丙烯酸硬脂酯、4.5g之N-羥甲基丙烯醯胺、1.1g之甲基丙烯酸-3-氯-2-羥基丙酯、62.5g之三丙二醇、380g
之純水、1.8g之油酸二甲基胺基丙基醯胺、14.2g之聚氧伸乙基月桂基醚、3.5g之聚氧伸乙基油基醚、6.1g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充1.1g之月桂硫醇、45g之氯乙烯。再加入1.4g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
實施例2
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之油酸二甲基胺基丙基醯胺、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
實施例3
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、6.5g之油酸二甲基胺基丙基醯胺、3.4g之聚氧伸乙基月桂基
醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
實施例4
在1L之高壓釜中加入133g之C6F13CH2CH2OCOCCl=CH2、30g之丙烯酸硬脂酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之油酸二甲基胺基丙基醯胺、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
實施例5
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、30g之丙烯酸硬脂酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之硬脂酸二甲基胺基丙基醯胺、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫
醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例1
在1L之高壓釜中加入140g之C8F17CH2CH2OCOCH=CH2、18g之丙烯酸硬脂酯、4.5g之N-羥甲基丙烯醯胺、1.1g之甲基丙烯酸-3-氯-2-羥基丙酯、62.5g之三丙二醇、380g之純水、14.2g之聚氧伸乙基月桂基醚、3.5g之聚氧伸乙基油基醚、6.1g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充1.1g之月桂硫醇、45g之氯乙烯。再加入1.4g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例2
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之
後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例3
在1L之高壓釜中加入133g之C6F13CH2CH2OCOCCl=CH2、30g之丙烯酸硬脂酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例4
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之單硬脂酸聚氧伸乙基山梨醣醇酐、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例5
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之單月桂酸聚乙二醇、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例6
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之氧化二甲基月桂基胺、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
比較例7
在1L之高壓釜中加入133g之C6F13CH2CH2OCOC(CH3)=
CH2、10g之丙烯酸硬脂酯、20g之甲基丙烯酸異莰酯、4.1g之二丙酮丙烯醯胺、55g之三丙二醇、370g之純水、1.6g之二甲基胺基丙基油醯胺、1.0g之2,4,7,9-四甲基-5-癸基-4,7-二醇之聚環氧乙烷加成物(為具有不飽和三鍵的二醇之環氧烷加成物)、3.4g之聚氧伸乙基月桂基醚、7g之聚氧伸乙基油基醚、4.2g之聚氧伸乙基異十三烷基醚,於60℃下加溫後,再以超音波乳化分散。在乳化後再加壓填充0.4g之月桂硫醇、35g之氯乙烯。再加入2.9g之2,2-偶氮二(2-脒基丙烷)2鹽酸鹽,並於60℃下反應3小時,即可得聚合物之水性分散液。之後以純水調整濃度使固形分濃度成為30重量%並測定該水性分散液之特性。
各例之特性如表5所示。
本發明之水性乳液組成物,可作為表面處理劑,如:撥水撥油劑、防污加工劑使用。
Claims (9)
- 一種水性乳液組成物,其包含:(A)含氟烷基之聚合物(B)界面活性劑,包含(B1)具有醯胺基及胺基之醯胺-胺界面活性劑(B2)非離子性界面活性劑,其中,非離子性界面活性劑(B2)為下述式所示之界面活性劑,R1O-(CH2CH2O)p-H[式中,R1為碳數1至22之烷基或碳數2至22之烯基或醯基;p為2以上之數]。
- 如申請專利範圍第1項所述之組成物,其中,含氟烷基之聚合物(A)具有碳數6之全氟烷基。
- 如申請專利範圍第1項或第2項所述之組成物,其中,界面活性劑係不含有具有不飽和三鍵之單元醇或多元醇之環氧烷加成物。
- 如申請專利範圍第1項或第2項所述之組成物,其中,醯胺-胺界面活性劑(B1),為下述式所示之化合物,R1-CONH-(CH2)n-N(R2)(R3)[式中,R1為碳數8至30之烷基或烯基;R2及R3為碳數1至6之烷基;n為1至10]。
- 如申請專利範圍第1項或第2項所述之組成物,其中,醯胺-胺界面活性劑之量,相對於聚合物(A)100重量份為0.1至20重量份。
- 如申請專利範圍第或1項第2項所述之組成物,其中,在至少1種之非離子性界面活性劑(B2)中,R1基為支鏈之烷基。
- 如申請專利範圍第1項或第2項所述之組成物,其中,組成物為撥水撥油劑及/或防污加工劑。
- 一種基材之處理方法,係將基材以如申請專利範圍第1項至第7項中任一項所述之水性乳液組成物進行處理者。
- 一種處理基材,係藉由如申請專利範圍第8項所述之處理方法而得者。
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TW474985B (en) * | 1996-06-21 | 2002-02-01 | Daikin Ind Ltd | Fluorine-containing, water-dispersion type water and oil repelling agent |
CN1620492A (zh) * | 2002-01-21 | 2005-05-25 | 大金工业株式会社 | 防水防油水性分散液 |
Also Published As
Publication number | Publication date |
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EP2829572A4 (en) | 2016-01-20 |
US9932504B2 (en) | 2018-04-03 |
EP2829572B1 (en) | 2019-04-24 |
US20150080510A1 (en) | 2015-03-19 |
CN104204079A (zh) | 2014-12-10 |
TW201343888A (zh) | 2013-11-01 |
JP2013224418A (ja) | 2013-10-31 |
JP5569614B2 (ja) | 2014-08-13 |
EP2829572A1 (en) | 2015-01-28 |
WO2013141249A1 (ja) | 2013-09-26 |
KR20140120949A (ko) | 2014-10-14 |
KR101531142B1 (ko) | 2015-06-23 |
CN104204079B (zh) | 2016-03-23 |
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