TW201241026A - Use of aqueous dispersions as primers - Google Patents
Use of aqueous dispersions as primers Download PDFInfo
- Publication number
- TW201241026A TW201241026A TW100143229A TW100143229A TW201241026A TW 201241026 A TW201241026 A TW 201241026A TW 100143229 A TW100143229 A TW 100143229A TW 100143229 A TW100143229 A TW 100143229A TW 201241026 A TW201241026 A TW 201241026A
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- TW
- Taiwan
- Prior art keywords
- acid
- group
- polymer
- primer
- dispersion
- Prior art date
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- 239000006185 dispersion Substances 0.000 title claims description 41
- 238000000034 method Methods 0.000 claims abstract description 40
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- IFNXAMCERSVZCV-UHFFFAOYSA-L zinc;2-ethylhexanoate Chemical compound [Zn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O IFNXAMCERSVZCV-UHFFFAOYSA-L 0.000 description 1
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Description
201241026 六、發明說明: 【發明所屬之技術領域】 、、本發明有關一種水性uv反應性底漆之用途,其係 塗布以乙婦-乙酸乙烯酿共聚物(EVA共聚物)或橡膠 為主之基底。本發明進一步提供-種使用水性UV反應 性底漆連結物件之新穎方法。 【先前技術】 財性聚合物分散液為主之熱可活化黏著劑變得 漸增地普遍,因為其料祕簡單及快速製造薄黏著層 而未釋放相tA量揮發性有機化合物(例如 胺?酸§旨分散液在有關欲被製造黏著結合之 ^荷容量特別符合最高要求。熱活化導致結晶或半結晶 聚合物炼化’其變得膠黏且在連結後再度結 曰曰,因而貝獻結合強度。 僅八==性聚胺?_分驗具有㈣無法黏著或 僅7人不滿地黏著於頻繁❹之各種材料之缺 作為鞋底或中底者。為了改良黏著性,預處 理欲被塗布的材料,例如以氯或臭氧處理、電裝 :含有有機溶劑之侵略底漆與υν轄射組合處二〔) :Sei.Teehn()1.,V()1.19,NU,PP. 19-40, 2005〕。 戈有主方法需要使用複雜方法步驟或設備及/ 化學品。已知以聚胺甲酸酿分散液為主且 由,、、柄及UV光固化之水性漆,例如從DE_A和8 201241026 958 °然而,彼等產品較佳被用於多孔吸收基底上’例 如木頭。針對藉助uv光固化之水性漆,未敘述非常佳 黏著性於塑膠材料—特別是具有低乙酸乙烯酯含量之 EVA共聚物或橡膠。 【發明内容】 因此,本發明目的為提供一種連結物件之方法,其 允用含有至少一種選自由聚胺曱酸酯、聚脲及聚胺甲酸 酿-聚脲組成組群的聚合物之水性分散液作為底漆,而 不需要使用有毒或有害物質。 驚人地已發現藉由將使用UV光可聚合的乙烯屬不 飽和單體與可同樣帶有uv可聚合基的聚胺曱酸酯分散 液組合,可製備在乾燥及UV輻射後良好黏著於基底(例 如EVA共聚物及橡膠)之底漆而未使用有機溶劑。 本發明因此提供一種水性分散液作為底漆之用 途,該分散液包括 a) 至少一種選自由聚胺曱酸酯、聚脲及聚胺曱酸酯_ 聚脲組成組群之聚合物, b) 至少一種乙烯屬不飽和化合物,及 c) 至少一種光引發劑, 其係塗布在選自由乙烯_乙酸乙烯酯共聚物,橡膠例如 SBR (笨乙烯丁二烯橡膠)、NBR(腈丁二烯橡膠)、 4 ⑧ 201241026 TR (熱塑性橡膠)、天然橡膠、EpDM (乙烯-丙烯-二 烯橡膠),聚烯烴及其他熱塑性材料,及其混合物組成 組群之基底。 原則上,根據本發明之底漆適合於欲被結合之任何 基底。特別用於以傳統水性、熱可活化黏著劑僅令人不 滿地黏著之基底,且其表面性質被底漆改質以致所提及 的黏著劑良好黏著。實例為乙烯-乙酸乙烯酯共聚物 (EVA )(例如Phylon® )、壓縮模製EVA、模切(die cut)EVA’而且可為橡膠例如SBR (苯乙烯丁二烯橡 膠)、NBR(腈丁二烯橡膠)、TR (熱塑性橡膠)、 天然橡膠、EPDM (乙烯-丙烯-二烯橡膠),聚烯烴及 其他熱塑性材料,及其混合物。 較佳者’基底係選自由乙烯_乙酸乙烯酯共聚物及 橡膠組成組群。特別佳者,基底係乙烯_乙酸乙烯酯共 聚物。最特別佳者認定為含有EVA之基底,該EVA具 有乙酸乙烯酯含量範圍較佳於8至28重量%、特別佳 於14至22重量%之乙酸乙烯酯。 水性底漆含有至少一種選自聚胺甲酸酯、聚脲及聚 胺曱酸酯-聚脲組群之聚合物。對應聚合物已知為水性 分散液且以工業規模可得。其等通常稱為聚胺曱酸酯分 散液(PUD)。 聚胺甲酸酯、聚脲及聚胺甲酸酯_聚脲聚合物含有 鏈延伸成分: (A)至少一種二醇及/或多元醇成分, 201241026
BCD E /fv '\ r\ /(V 至少一種二-及/或聚-異氰酸酯成分, 至少一種含有至少一個親水基之成分, 視情況單-、二-及/或三-胺基官能及/或羥胺 基官能的化合物,及 視情況其他異氰酸酯反應性化合物。 適合的二醇及/或多元醇成分A)係具有至少兩個 對異氰酸酯基有反應性的氫原子及平均分子量較佳為 62至18,000g/mol、特別佳為62至4000g/mol之化合物。 適合的鏈延伸成分實例為聚醚、聚酯、聚碳酸酯、聚内 酯及聚醯胺。較佳多元醇A)含有較佳2至4個、特別 佳2至3個羥基、最特別佳2個羥基。彼類型各種化合 物之混合物亦適合。 開始考慮為聚酯多元醇,特別是線型聚酯二醇或亦 弱分支聚酯多元醇,如可以已知方式從脂族、環脂族或 芳香族二-或聚·羧酸(例如丁二酸、曱基丁二酸、戊二 酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、十一 烧二酸、十二烧二酸、對駄酸、異醜酸、醜酸、四氫醜 酸、六氫酞酸、環己烷二羧酸、順丁烯二酸、反丁烯二 酸、丙二酸或1,2,4-苯三曱酸)及酸酐(例如酞酸酐、 1,2,4-苯三甲酸酐、丁二酸酐)或其混合物與多元醇(例 如乙二醇、二-、三-、四-甘醇、1,2-丙二醇、二-、三-、 四-伸丙二醇、1,3-丙二醇、1,4-丁 二醇、1,3-丁二醇、2,3-丁二醇、1,5-戊二醇、1,6-己二醇、2,2-二曱基-1,3-丙二 6 ⑧ 201241026 醇、1,4-二羥基環己烷、二羥曱基環己 醇、U0-癸二醇、U2_十二烷二醇或 丨,8·辛一 情況伴隨使用更高官能多元醇(例如三羥;2烷 油或新戊四醇)製備。作為製備聚酯多元醇^醇, :有==之環脂族及/或芳香族二及聚:化合 勿代替自由聚賊’低級醇之對應聚竣酸軒或對應聚 羧酸酯或其混合物亦可用於製備聚酯。 〆
聚酉旨多元醇當然亦可為内g旨之同元聚合物或混合 聚合物,其較佳藉由將内酯或内酯混合物(例如丁; 酯、ε-己内酯及/或甲基_ε_己内酯)添加於適合二-及 /或更高官能起始分子(例如以上提及作為聚醋多元醇 的鏈延伸成分之低分子量多元醇)獲得。ε_己内酯之對 應聚合物為較佳。 S 亦開始考慮含有羥基之聚碳酸酯作為聚經基成分 A) ’例如藉由二醇(例如1,4-丁二醇及/或丨6_己_ 醇)與碳酸二芳基酯(例如碳酸二苯酯)、碳酸,二燒^ 酯(例如碳酸二曱酯)或光氣之反應可製備者。至少部 分使用含有羥基之聚碳酸酯可賦予欲改良的聚胺甲酸 酯或聚胺甲酸酯-脲分散液黏著劑之水解穩定性。 適合為聚醚多元醇例如有氧化笨乙稀、環氧乙燒、 環氧丙烷、四氫呋喃、環氧丁烷、表氯醇之聚加成產物、 及其等混合加成及接枝產物,以及藉由多元醇或其現人 物之縮合獲得之聚醚多元醇及藉由多元醇、胺及胺基醇 之烷氧基化獲得者。適合作為鏈延伸成分A)之聚麵多 201241026 元醇為環氧乙烷及環氧丙浐 及接枝聚合物,其藉由將^同元聚合物、混合聚合物 展氧化物添加至低分子量 一知或场(如以上提及作騎衫元醇的鏈延伸成分 者或添加至更高官能低分子量多元醇(例如新戍四 醇或糖)、或添加至水可獲得。 適合成分A)同樣為低分子量二醇、三醇及/或四 醇’例如乙二醇、二-、三-、四-甘醇、1,2-丙二醇、二-、 三-、四-伸丙二醇、1,3-丙二醇、1,4-丁二醇、ι,3-丁二 醇、2,3-丁二醇、1>5_戊二醇 ' ;1,6_己二醇、2,2_二甲基 -1,3-丙二醇、1,4_二羥環己烷、i,4-二曱基環己烷、1,8-辛二醇、1,10-癸二醇、1,12-十二烷二醇、新戊二醇、 1,4-環己二醇、1,4_環己烷二曱醇、1,4-、1,3-、1,2-二羥 苯或2,2-雙-(4-經苯基)-丙烷(雙酚A)、TCD-二醇、 三羥曱基丙院、甘油、新戊四醇、二新戊四醇、或其混 合物,視情況伴隨使用尚未提及的進一步二醇或三醇。 亦可呈提及多元醇(特別是低分子量多元醇)與環 氧乙烷及/或環氧丙烷之多元醇反應產物使用。 低分子量成分A)具有分子量較佳於62至4〇〇 g/mol,且較佳與上述聚酯多元醇、聚内酯、聚醚及/ 或聚碳酸酯組合使用。 存在於根據本發明聚胺甲酸酯之多元醇成分A)呈 用量較佳20至95重量%、特別佳30至90重量%、最 特別佳65至90重量%。 適合為成分B)有每分子含有至少兩個自由異氰酸 ⑤ 201241026 酯基之任何所欲有機化合物。較佳者給定為使用二異氰 酸酯Y(NCO)2,其中Y代表具有4至12個碳原子之二 價脂族烴自由基、具有6至15個碳原子之二價環脂族 烴自由基、具有6至15個碳原子之二價芳香族烴自由 基或具有7至15個碳原子之二價芳脂族烴自由基。較 佳使用之此類二異氰酸酯實例為四亞甲基二異氰酸 酯、曱基五亞曱基二異氰酸酯、六亞曱基二異氰酸酯、 十一亞甲基二異氰酸酯、1,4_二異氰酸基_環己烧、卜異 氰酸基-3,3,5-三曱基-5-異氰酸基曱基_環己燒(= IPDI,異佛酮二異氰酸酯)、4,4、二異氰酸基-二環己 基-甲院、4,4’-二異氰酸基-二環己基丙烧_(2,2)、1,4_二 異氰Isl基本、2,4-二異氰酸基曱笨、2,6-二異氰酸基曱 本、4,4 -一異氰酸基-二苯基曱烧、2,2’-與2,4,-二異氰 酸基-二苯基曱烷、四曱基伸茬基二異氰酸酯、對-伸茬 基二異氰酸酯、對-亞異丙基二異氰酸酯、以及由彼等 化合物組成之混合物。 除了彼等簡單二異氰酸酯外,鍵聯異氰酸酯基的自 由基中含有雜原子及/或每分子具有官能度大於2個 異氰酸酯基之聚異氰酸酯亦為適合者。前者係例如由至 少兩個異鼠酸醋構成且具有二聚異氰酸(uretdi〇ne)、 三聚異氰酸、胺曱酸乙酯、脲甲酸酯、縮二脲、碳二醯 亞胺、亞胺基D号二π井二酮(iminooxadiazinedione)及/ 或〇号二_三綱(0仰(^2丨11故丨0116)結構之聚異氰酸§旨,其 係藉由簡單脂族、環脂族、芳脂族及/或芳香族二異氰 201241026 酸酯之改質而製備。4·異氰酸基甲基“,心辛烷二異氰酸 酯(壬烷三異氰酸酯)可被提及作為每分子具有大於2 個異氰酸酯基之未改質聚異氰酸酯的實例。 較佳二異氰酸酯B)為六亞甲基二異氰酸酯(= HDI)、十二亞甲基二異氰酸酯、1,4-二異氰酸基-環己 烧、1-異氛酸基-3,3,5-三甲基-5-異氰酸基甲基-環己烷 (—IPDI)、4,4’-二異氰酸基_二環己基_曱烷、2,4_二 異氰酸基曱苯、2,6·二異氰酸基甲苯、4,4,_二異氰酸基_ 二苯基曱烷、2,2’-與2,4,-二異氰酸基二苯基甲烷、以及 由彼等化合物組成之混合物。 特別佳成分B)為六亞甲基二異氰酸酯及丨_異氰酸 基-3,3,5-三曱基-5-異氰酸基曱基_環己烷。 成分B)存在於根據本發明聚胺甲酸酯呈用量5至 60重量%、較佳6至45重量%、特別佳呈用量7至25 重量%。 適合成分C)為例如含有磺酸鹽或羧酸鹽基之成 分,例如額外帶有磺酸鹽及/或羧酸鹽基之二胺基化合 物及二經基化合物,例如以下之鈉、鐘、卸、三級胺鹽: N-(2-胺乙基)-2-胺基乙烧續酸、N-(3-胺丙基)-2-胺基乙 烧續酸、N-(3-胺丙基)-3-胺基丙烧續酸、N-(2-胺乙基)-3_ 胺基丙烷磺酸、類似羧酸、二羥曱基丙酸、二羥曱基丁 酸、上下文内lmol二胺(例如1,2·乙二胺或異佛酮二 胺)與2mol丙烯酸或順丁烯二酸的麥可加成反應之產 201241026 酸係以其等鹽形式頻繁直接使用作為磺酸越或羧 酸鹽。然而,亦可能在製備聚胺甲酸酯期間 若干或所有形成鹽所需之中和劑。 一 特別適合及較佳於形成鹽之三級胺為例如三乙 胺、二曱基環己胺、乙基二異丙胺。亦可使用其他胺以 形成鹽,例如氨、二乙醇胺、三乙醇胺、二甲基乙醇胺、 曱基二乙醇胺、胺基曱基丙醇及亦提及者與其他胺之混 合物。直到形成預聚合物後才權宜地添加此等胺。 亦可使用其他中和劑,例如中和目的用之氫氧化 鈉、鉀、鐘、鈣。 進一步適合成分c)為具有非離子性親水作用之單 -或二-官能聚趟’其係以醇或胺起始的環氧乙烧聚合物 或環氧乙烧/環氧丙烧共聚物為主,例如聚鍵LB25 (Bayer MaterialScience AG ;德國)或 MPEG 750 :甲 氧基聚乙二醇’分子量750g/mol(如Pluri〇i® 750,BASF AG,德國)。 幸乂佳成刀C)為N-(2-胺乙基)-2·胺基乙烧續酸自旨及 二曱基丙酸之鹽與二羥曱基丁酸之鹽。 成分C)存在於根據本發明聚胺甲酸酯呈用量較佳 0.1至15重量%、特別佳〇5至1〇重量%、.最特別佳 0.8至5重量%、又更佳〇9至3 〇重量%。 適合成分D)為單_、二_、三·官能胺及/或單·、 二-、三-官能羥胺,例如脂族及/或脂環一級及/或二 級單胺’例如乙胺、二乙胺、丙胺與丁胺之同分異構物、 201241026 較高級線型脂族單胺及環脂族單胺(例如環己胺)。進 一步實例為胺醇,亦即分子中含有胺基及羥基之化合 物,例如乙醇胺、N-曱基乙醇胺、二乙醇胺、二異丙醇 胺、1,3-二胺基-2-丙醇、N-(2-羥乙基)-乙二胺、N,N-雙 (2-羥乙基)-乙二胺及2-丙醇胺。進一步實例為二胺及三 胺,例如1,2-乙二胺、1,6-六亞甲基二胺、1-胺基-3,3,5-三甲基-5-胺甲基-環己烷(異佛酮二胺)、哌畊、1,4_ 二胺基環己烷、雙-(4-胺基環己基)-曱烷及二伸乙三 胺。己二酸二醯肼、肼及肼水合物亦為適合者。當然亦 可使用數個已提及之化合物D)(視情況與尚未提及的 化合物D) —起)之混合物。 較佳成分D)為1,2-乙二胺、1-胺基-3,3,5-三曱基 -5_胺曱基-環己烷、二伸乙三胺、二乙醇胺、乙醇胺、 N-(2-經乙基)-乙二胺及N,N-雙(2-經乙基)-乙二胺。 成分D)較佳作為鏈延伸劑用來建立更高分子量, 或作為單官能化合物用來限制分子量,及/或視情況額 外合併進一步反應性基(例如自由經基)作為進一步交 聯部位。 成分D)存在於根據本發明聚胺甲酸酯呈用量較佳 0至10重量%、特別佳〇至5重量%、最特別佳呈用 量0.2至3重量%。 視情況伴隨使用之成分E)可為例如具有2至22 個碳原子之脂族、環脂族或芳香族單醇(例如乙醇、丁 醇、己醇、環己醇、異丁醇、苄醇、硬脂醇、2-乙基乙 ⑧ 201241026 醇)’及傳統用於異氰酸酯基且在升溫下可被再次移除 之封阻劑(例如丁酮肟、二甲基吡唑、己内醯胺、丙二 酸酯、***、二甲基***、第三丁基-苄胺、環戊酮羧 乙酯(cyclopentanonecarboxyethyl ester))。 成分E)可存在於根據本發明聚胺曱酸酯呈用量較 佳0至20重量%、最佳〇至1〇重量%。 伴隨使用成分E)可導致例如根據本發明除了反應 性羧基外含有進一步反應性基之聚胺甲酸酯分散液,其 允許例如使用不同交聯機制(雙重固化),以便達到特 殊性質例如兩階段的、視情況交錯固化或特別高的交聯 密度。 在本發明較佳具體實例中,底漆含有至少一種結晶 或半結晶聚胺曱酸酯或聚胺曱酸酯_聚脲聚合物。 關於結晶或半結晶意指根據DIN 65467以加熱速 率20 K/min的DSC測量中,聚合物具有對應熔融焓之 熔融峰>3 J/g、較佳>15 j/g、特別佳>30 J/g、最特別 佳>50 J_/g。熔融峰係由聚合物中規律部分結構熔融造 成。 結晶或半結晶聚胺甲酸酯或聚胺甲酸酯·聚脲聚合 物較佳含有以線型二羧酸及/或其等衍生物(例如酐、 酯或酸氯化物)及脂族或環脂族線型或分支多元醇為主 之二-或更高官能聚酯多元醇A)。特別佳者給定為 自由己二酸、丁二酸、癸二酸及十二烷二酸組成組群之 二羧酸;最特別佳作為成分A)者為己二酸。使用此等 13 201241026 呈用里、所有緩酸總量為基礎至少80 mol%、較佳85 至 100 m〇1%、特別佳 90 至 1〇〇 m〇i%。 可視情況伴隨使用其他脂族、環脂族或芳香族二叛 ,此類一羧酸實例為戊二酸、壬二酸、1,4-、1,3-、 ,i,2-i衣己烷-二羧酸、對酞酸或異酞酸。使用此等呈用 量以所有敌酸總量為基礎不超過2G mGl%、較佳〇至 15mol%、特別佳 〇至 1〇m〇1%。 聚醋A)之較佳多元醇成分係選自由單乙二醇、1,3-丙一醇、丨,4-丁二醇、1,5-戊二醇、1,6-己二醇及新戊二 醇組成之組群;特別佳作為多元醇成分為1,4-丁烷二醇 及1,6-己烷二醇,最特別佳為丨,4•丁烷二醇。使用此等 呈用量以所有多元醇總量為基礎較佳至少80 mol%、特 別佳 90 至 100 mol%。 可視情況伴隨使用其他脂族或環脂族線型或分支 多元醇。如此多元醇實例為二甘醇、羥三曱基乙酸新戊 一酉日(hydroxypivalic acid neopentyl glycol)、環己烧-二 曱醇、1,5-戊二醇、ι,2·戊二醇、19-壬二醇、三羥曱基 丙院、甘油或新戊四醇。使用此等呈用量以所有多元醇 總量為基礎不超過2〇mol %、特別佳〇至l〇mol %。 二或多種此類聚酯A)之混合物亦為適合者。 較佳使用以己二酸與1,4-丁二醇或己二酸與ι,6-己 二醇或己二酸與1,6-己二醇及新戊二醇的混合物為主 之聚酯A)。 根據本發明聚胺甲酸酯具有固體含量較佳15至70 201241026 特別佳25至⑼重量%、最特別佳3q至別重 里%。阳值較佳範圍為、特別佳6至1〇。 =於〜或兩,段反應,織分散於錢用水分散, ==r後可藉由蒸德移除若干或所有伴隨使 、根據本發明水性聚胺甲酸s旨或⑽ψ㈣旨·聚腺分 散液之製備可以-或多個階段均質相或在多·階段反應 情況中部分以分散相進行。當已完全或部分進行聚加成 時,進行分散、乳化或溶解步驟。然後於分散相視 進行進一步聚加成或改質。先前技藝已知之所有方法可 用於製備’例如乳化劑/剪切力、丙酮、預聚合物混合、 熔融乳化、酮亞胺及固體自發分散方法或其衍生。此等 方法總結可見於]Vlethoden der organischen Chemie (Houben-Weyl, Erweiterungs- und Folgebande zur 4 Auflage, Volume E20, H. Bartl and J. Falbe, Stuttgart, New York,Thieme 1987, p. 1671-1682)。熔融乳化、預 聚合物混合及丙酮方法為較佳。丙酮方法為特別佳。 原則上,可將所有經基官能的成分稱重,然後添加 所有異氰酸酯官能的成分,進行混合物反應以生成異氰 酸酯官能的聚胺曱酸酯,然後與胺基官能的成分反應。 15 201241026 亦可,反向製備,將異氰_成分導入反應容 器,添加 經基S %的成分’反應以生成聚胺甲義,然後與胺基 B月t*的成分反應以生成最終產物。 般將所有或若干製備聚胺甲酸酯預聚合物之羥 基^能的成分A)、視情況C)及視情況E)放置於反 應器’視情況用與水互溶但對異氰_旨基惰性之溶劑稀 釋,然後均質化。然後在室溫至12〇。。計量加入成分 B) ’製備異氰酸g旨官能的聚胺曱酸自旨。此反應可以一 皆段或數個階段舉行。進行—個階段反應可例如將成 刀=)及/或E)放置於反應器,在與異氰酸酯官能的 成分B)反應後添加成分A),然後能夠與若干仍存在 的異氰酸酯基反應至結束。 適合溶劑為例如丙酮、甲基異丁基酮、丁酮、四氫 呋喃、二咩烷、乙腈、二伸丙二醇、二曱醚及i•曱基_2_ 吡咯_,其可不但於製備開始時添加,而且稍晚時部分 添加。丙酮及丁酮為較佳。可在常壓或升壓下進行反應。 針對製備預聚合物,羥基官能及視情況胺基官能的 成分用量係產生異氰酸酯指數較佳1〇5至2 5、特別佳 1.15至1.95、最特別佳1.2至1.7。 異氰酸S旨g能的預聚合物與進一步經基官能及/ 或胺基官能(較佳僅胺基官能)的成分D)及視情況C) 之進一步反應(所謂鏈延伸)係選擇反應度(以1〇〇% 異氰酸酯基為基礎)較佳25至150%、特別佳40至85 %經基及/或胺基之方式進行。 201241026 在反應度超過100%情況中(其為可能、但較少偏 好),首先適當使在異氰酸酯加成反應意義内為單官能 之所有成分與預聚合物反應,然後使用二-或更高-官能 鏈延伸成分,以獲得盡可能完整合併所有鏈延伸分子。 反應度一般藉由跟隨反應混合物之NCO含量監 控。至終可進行光譜測量(例如紅外光譜或近-紅外光 譜、決定折射指數)、及化學分析(例如滴定移除的樣 品)兩者。 為了加速異氰酸酯加成反應,可使用所處技術領域 中熟習技藝人士已知用於加速NCO-OH反應之傳統觸 媒。實例為三乙胺、1,4_二氮雙環-[2,2,2]辛烷、氧化二 丁錫、二辛酸錫或二月桂酸二丁錫、雙_(2-乙基己酸) 錫、二辛酸鋅、雙-(2-乙基己酸)鋅或其他有機金屬化合 物。 在分散之前、分散期間或分散之後可進行異氰酸酯 官能的預聚合物與成分D)及視情況C) 之鏈延伸。較 佳者’在分散之前舉行鏈延伸。若使用成分C)作為鏈 延伸成分’在分散步驟之前與彼成分鏈延伸則為必要。 鍵延伸一般於溫度10至100°C、較佳25至60°C進 行。 、、在本發明範疇内術語鏈延伸亦包含視情況單官能 成刀D) <反應,由於其等單官能度而作為鏈終止劑’ 因此未造成增加、但導致分子量之限制。 鍵延伸成分當添加於反應混合物時可用有機溶劑 201241026 及/或用水稀釋。其等可呈任何所欲順序連續添加,或 藉由添加混合物而同時添加。 為了製備聚胺曱酸酯分散液’視情況以顯著剪切 μ(例如強力攪拌)將預聚合物導入分散水,或反之將分 散水授拌人郷合物。然後可進行鏈延伸若其尚未於均 勻相發生。 在分散期間及/或之後,可蒸餾掉已視情況使用之 有機溶劑,例如丙酮。 較佳製備方法係敘述如下: 將成分A)、視情況成分c)及視情況成分E)及 ,情況溶劑放置於反應器並加熱達20至1〇〇。(:。盡可 月b地快^速以攪拌計量加入成分B)。使用反應熱,在4〇 f 15〇C^f#反應混合物,直到異氰酸§旨含量達到或些 A低於理論值。可視情況添加觸媒^混合物然後藉由添 加/谷7稀釋至固體含量25至95重量%、較佳35至8〇 重量/^,然後藉由添加用水及/或溶劑稀釋之成分 D),視情況與成分c) 一起,在⑽至丨劝艽進行鏈延 伸。反應時間2至60分鐘後,藉由添加蒸顧水或藉由 轉移入谷||之_水中進行分散,在分散步驟期間或之 後蒸餾掉所用若干或所有溶劑。 .根據本發明分散液可以其等單獨或與下列一起使 用.塗布絲著技術巾6知之!έ、_、辅助物質及添加 =特別疋乳化劑及光穩定劑(例如UV吸收劑及立體 卜礙胺(HALS))’及抗氧化劑、填料及輔助物質, 201241026 例如抗沉降劑、消泡劑及/或潤濕劑、流動改良劑、反 應稀釋劑、塑化劑、中和劑、觸媒、輔助溶劑及/或增 稠劑’及添加劑例如顏料、著色劑或抗油劑(mattifying agent)。亦可添加膠黏劑。 添加劑可在加工之前立即添加於根據本發明產 物。然而’亦可能在分㈣結麵間或之前添加至少若 干添加劑。 選擇及計量添加此等可被加至個別成分及/或呈 全體混合物之物質原則上已知於熟習技藝人士,且可藉 助簡單初步試驗料及錢㈣^應用而無過度花費。 光引發劑係藉由光化輕射及起始自由基聚合乙稀 屬不飽和化合物可活化之引發劑。活化輻㈣光化,例 如uv及/或可見光具有波長2〇〇至75〇nm、較佳2〇〇 至600nm、特別佳200至50〇nm。 光引發劑為本身已知之商業銷售化合物,區別為單 分子(類型I)及雙分子(類型U)引發劑。(類型υ 系統為例如芳香族酮化合物,例如二笨基酮與三級胺、 垸基二苯基_、4,4’_雙(二甲胺基)二笨基_ (米其勒 函同)、蒽酮及經自化的二苯基_或提及類型之混合物做 組合。亦適合者為(麵Π)弓!發劑,例如安息香及其 衍生物、二苯乙二酮縮酮、氧化醯基膦,例如氧化2,4,6_ 三曱基·^醢基_二苯顏、氡化雙縣膦、笨基乙紐 酯、樟腦醌、α-胺基苯烷酮、α,α_二烷氧基苯乙酮及α_ 羥基苯烷酮。亦可有利使用此等化合物之混合物。適合 201241026 引發劑係例如以名稱Irgacure®與Darocur®( Ciba, Basel, CH)及 Esacure® ( Fratelli Lamberti,Adelate,IT )商業 可獲得。 光引發劑之使用濃度係熟習技藝人士已知及/或 視情況以簡単初步試驗決定。給予特別考慮UV輕射之 波長、強度與劑量,及照射中遍及底漆之氧含量。較佳 者給予濃度〇· 1重量%至10重量%、特別佳1 .〇重量% 至4.5重量% ’各個案中以底漆固體含量為基礎。 在另一的具體實例中’聚胺曱酸酯、聚脲或聚胺甲 酸酯-聚脲含有乙烯屬不飽和雙鍵。較佳.經治在製備聚 合物中按比例使用含有丙稀酸酯及/或曱基丙烯酸酉旨 基〔下文稱為(甲基)丙稀酸酯〕之經基官能的成分A)、 C)或E),實現將彼等基併入聚合物。較佳羥基官能 的(甲基)丙烯酸酯係選自由(甲基)丙烯酸2-經乙基 酯、聚單(甲基)丙埽酸環氧乙院酯 '聚單(甲基)丙 烯酸環氧丙烧酯、聚單(曱基)丙稀酸環氧烧酯、聚單 (曱基)丙稀酸(ε-己内醋)醋(例如Pemcure® 12A (Cognis,Dttsseldorf,DE))、(甲基)丙烯酸 2-羥丙 基酯、(曱基)丙烯酸4-羥丁基酯、(曱基)丙稀酸 3-經基-2,2-二甲基丙基自旨、及多元Sf·(例如三經曱基丙 烧、甘油、新戊四醇、二新戊四醇、山梨醇、乙氧化三 經曱基丙烧、丙氧化三經曱基丙烧或烧氧化的三經曱基 丙烷、甘油、新戊四醇、二新戊四醇或其商業混合物) 之丙烯酸及/或甲基丙烯酸部分酯組成組群。單醇之丙 201241026 烯酸醋為特別佳。亦適合者係可從含有雙鍵的酸與視情 況含有雙鍵的單體環氧化合物反應獲得之醇,例如(甲 基)丙稀酸與(曱基)丙烯酸環氧丙基酯或叔碳酸 (versatic acid)之環氧丙基酯之反應產物。 進步可冑b以其等單獨或與上述單體化合物組合 使用含有(曱基)丙烯酸酯基之異氰酸酯反應性寡聚或 聚合不飽和化合物。較佳者給予使用含羥基的聚酯丙烯 酸醋具有 OH 含量 230 mgKOH/g 至 $300 mgKOH/g、 特別佳g 60 mg KOH/g至$ 200 mg KOH/g、最特別佳 27〇mgKOH/g至$120mgKOH/g。總共7組單體組份 可用於製備羥基官能的聚酯丙烯酸酯: L (環)烷二醇,例如具有(環)脂族鍵結羥基且具 分子量範圍^62 g/mol至$286 g/mol之二元醇, 例如乙二醇、1,2-與 1,3-丙二醇、1,2-、1,3·與 1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、環 己烷-1,4-二曱醇、1,2-與1,4-環己二醇、2-乙基-2-丁基丙二醇,含有醚氧之二醇,例如二甘醇、三甘 醇、四甘醇、二伸丙二醇、三伸丙二醇、具有分子 量範圍 2200 g/mol 至 $4000 g/mol、較佳 ^300 g/mol 至 $2000 g/mol、特別佳 2450 g/mol 至 S 1200 g/mol之聚乙、聚丙或聚丁二醇。可同樣使 用上述二醇與ε-己内酯或其他内酯之反應產物作 為二醇。 2· 具有分子量範圍2 92 g/mol至$254 g/mol之三-及 21 201241026 更高元醇,例如甘油、三經曱基丙烧、新戍四酉予 二新戊四醇及山梨醇,或以彼等醇起始的聚謎’例 如1 mol三羥甲基丙烷與4 mo1環氧乙烧之反應產 物。 3. 單醇,例如乙醇、1-與2-丙醇、1-與2-丁醇、1-己 醇、2-乙基己醇、環己醇及苄醇。 4. 具有分子量範圍2 104 g/mol至$ 600 g/mol之二梭 酸及/或其等酐’例如酞酸、酞酸酐、異酜酸、四 氫献酸、四氫献酸針、六氫欧酸、六氫酖酸酐、環 己烷二羧酸、順丁烯二酸酐、反丁烯二酸、丙二酸、 丁二酸、丁二酸酐、戊二酸、己二酸、庚二酸、辛 二酸、癸二酸、十二烷二酸、氫化的二聚體脂肪酸。 5. 更高官能羧酸或其等酐,例如1,2,4-苯三甲酸及 1,2,4-苯三曱酸酐。 6. 單羧酸,例如安息香酸、環己烷羧酸、2_乙基己酸、 己酸、辛酸、癸酸、月桂酸、天然及合成脂肪酸。 7. 丙烯酸、甲基丙稀酸或丙稀酸二聚體。 適合含羥基的聚酯丙烯酸酯包含至少一種組群j 或2組份與至少一種組群4或5組份及至少一種組群7 組伤之反應產物。具有分散個之組群亦可視情況被併 入此類。目而,可按比例使麟乙二醇及 /或曱氧絲乙二醇作為祕分。可提及之化合物包含 例如醇起始的聚乙二醇、聚丙二醇及其等嵌段共聚物, 22 ⑧ 201241026 以及彼等聚乙二醇之單曱醚。聚乙二醇1500及/或聚 乙一和早曱喊為特別適合。 進一步可在酯化後使若干羧基(特別是(曱基)丙 烯酸者)與單·、二-或聚環氧化物反應。較佳者給予例 如單體、寡聚或聚合雙酚A、雙酚F、己二醇、丁二醇 及/或三羥甲基丙烷之環氧化物(環氧丙基醚)或其等 乙氧化及/或丙氧化衍生物。此反應可被特別用於增加 聚酯(曱基)丙烯酸酯之OH數,因為於各個案中環氧 化物/酸反應形成OH基。所得產物之酸數較佳為go mg KOH/g 至 S 20 mg KOH/g、特別佳 g 1 mg KOH/g 至 S 10 mg KOH/g、最特別佳 ^ 2 mg KOH/g 至 S 5 mg KOH/g。反應較佳藉由觸媒催化,例如三苯膦、二乙醇 硫醚、齒化錄及/或鱗、及/或錯化合物或錫化合物(例 如乙基己酸錫(II))。 同樣較佳者為具有OH含量^20 mg KOH/g至 S 300 mg KOH/g、特別佳 g 1〇〇 mg KOH/g 至 S 280 mg KOH/g、最特別佳 $ 150 mg KOH/g 至 $ 250 mg KOH/g 之含羥基的(曱基)丙浠酸環氧酯,或具有〇H含量較 佳 ^ 20 mg KOH/g 至 $ 300 mg KOH/g、特別佳 2 40 mg KOH/g 至 S 150 mg KOH/g、最特別佳 $ 5〇 mg K〇H/g 至S 100 mg KOH/g之含羥基的聚胺甲酸酯(曱基)丙 烯酸酯’以及其相互混合物及與含經基的不飽和聚醋之 混合物’以及與聚酯(曱基)丙烯酸酯之混合物或含經 基的聚酯與聚酯(曱基)丙烯酸酯之混合物。含經基的 23 201241026 二氧酯係特別基於丙烯酸及/或曱基丙 酚A、雙酚F、己二醇及/ 二二•之%氧化物(環氧丙基化合物)或其等乙氧化 及/或丙氧化抓物之反應絲。 、跡^烯屬不飽和化合物較佳選自由丙烯_、曱基丙 人巴讀sl、乙軸、乙_及乙稀基芳香族化 之組群。較佳者’⑽屬不飽和化合物含有芳 脂族基。其等一般具有分子量低於500 g/mol。 給予㈣_旨及甲基__,特別是具有丙 -夂,甲基丙烯酸基〔下文稱為「(甲基)丙烯酸 4之官能度為2或更小者。對應化合物亦可以其等 早獨或呈混合物使用。 Μ具有1至2G個碳原子之舰乙稀sl為例如月桂酸 ’知、硬脂酸乙締酿、丙酸乙稀醋、叔碳酸乙稀醋及 乙稀S旨。可提及之乙_實例包含乙絲曱基鍵或 ^基異丁細。含有1至4個碳原子的醇之乙稀酯為 開始考慮乙婦基甲苯、鄰.與對基苯乙稀、鄰_ 乙烯、4_正丁基苯乙歸、4_正癸基苯乙稀及較佳 乙烯作為乙烯基芳香族化合物。 最特卿料具有動旨族或料祕之乙稀屬不 =lb合物。此類乙烯屬不飽和化合物係選自例如由 稀酸苯氧基乙基醋、(甲基)丙烯酸苯氧基 = 乙酉旨、具有平均乙氧化程度n=(U至4.0 (基)丙稀酸雙盼A乙氧化乙酉旨、(甲基)丙婦酸 ⑧ 24 201241026 環己酯、(甲基)丙烯酸第三丁基環己基酯之同分異構 物、(曱基)丙烯酸降莰基酯、(曱基)丙烯酸異莰基 酯、(曱基)丙烯酸二環戊二烯基酯或(f基)丙烯酸 四氫糠基酯、(曱基)丙烯酸環狀三羥曱丙烷縮曱醛酯 (cyclic trimethylolpropanformal (meth)acrylate)、二(曱 基)丙稀酸三環癸烧二曱酯組成之組群。又進一步較佳 者為(甲基)丙烯酸四氫呋喃酯、二(曱基)丙烯酸三 環癸院二甲酯及(甲基)丙烯酸二環戊二烯基酯。 乙烯屬不飽和化合物或乙烯屬不飽和化合物之混 合物的使用量為以聚合物為基礎25 〇重量%至$5〇重 量%、特別佳glO.O重量%至^30.0重量%。 可以各種方式進行合併乙烯屬不飽和化合物及光 =發劑。兩者可在製備聚合物期間或之後各種時刻單獨 合併或一起合併。若使用固體光引發劑,可較佳首先使 用乙烯屬不飽和化合物作為光引發劑之溶劑。可使用乙 不飽和化合物及/或光引發劑作為製備聚合物之 ’容=使其與聚合物乳化於水。預聚合物混合方法及溶 =散方法特別適合於使用乙稀屬不飽和化合物及/ ^光引發劑作為溶劑,因而降低聚合物/預聚合物炫體 之黏其有利於形成乳液。若乙_不飽和化 二勿或。光弓丨發劑具有在製備聚合物中亦反應之官能 土則可在合成聚合物後添加對應化合物。 化人、丨而h後同樣可將光引發劑及/或乙稀屬不飽和 5物併入聚合物於水之乳液。剪切力為必要的,其可 25 201241026 藉助猜II、分散ϋ及混合ϋ(特別是靜態混合器)施 予。就方法而論’此等係將疏水或部分親水液體併入聚 合物乳液之已知方法。可能(但不偏好> #助輔助 協助合併,例如乳化劑或能夠形成保護膠體之物質。 在進一步之具體實例中,可將次要用量—高至% 重量%進-步聚合物(特別是已乳化或可乳化於水之聚 合物)併人根據本發明之底漆。實例為經改f之聚_ (亦較少偏好、_化的聚馳)、聚乙酸乙㈣或醇、 以及其共聚物、聚(曱基)丙歸酸g旨及/或聚苯乙婦_ 聚(甲基)丙稀酸醋共聚物。 根據本發明底漆可含有於黏著劑、表面塗料、油漆 及印刷油墨技術中傳統之添加劑及/或輔助物質及/ 或溶劑。此類物質特別為穩定劑、抗老化劑、光穩定劑 (例如UV吸收劑及立體障礙胺(HALS))、及抗氧 化劑以及輔助物質,例如抗沉降劑、消泡劑及/或潤濕 劑、流動改良劑、塑化劑、抗靜電劑、觸媒及/或流變 控制添加劑(例如增稠劑)、以及顏料及/或著色劑。 較不偏好使用溶劑,即使有也呈次要用量使用。 作為填料可使用礦物填料、視情況亦可使用玻璃纖 維、碳黑、奈米級材料,例如氧化矽溶膠或氧化鋁或其 他金屬氧化物、碳奈米管(例如Baytubes®,Bayer MaterialScience AG, Leverkusen)。 根據本發明所用底漆較佳具有固體含量1至75重 量%。底漆之固體含量及黏度係特別適應於應用方法及 ⑧ 201241026 乾燥後獲得之所欲膜層。藉由製備濃縮分散液及隨後用 水稀釋’可調整固體含量於寬廣範圍内’特別是範圍3 至55重量%(取決於所用物質)。如水性塗布技術已知及 傳統’藉助改變流變學之傳統增稠劑及/或添加劑,可 控制黏度及其他流變性質於寬廣範圍内。較佳者,針對 藉助刷塗之應用,調整底漆至固體含量較佳為3至 重量%、特別佳5至25重量%,且調整為牛頓^ 微剪切稀化之流變性質。底漆因此具有至 一 之複合黏度。 似7黏度 本發明因此進-步提供一種連結物 括至少下列步驟 方法’其包 I) 用水性分散液作為底漆塗布物件, 〇至少一種選自由聚胺甲酸§旨、^刀散^包括 醋-聚脲組成組群之聚合物,聰及1胺甲酸 b) 至〉、種乙歸屬不飽和化合物 c) 至少一種光引發劑; II) 移除水; III) 用光化輻射照射; IV )用黏著劑塗布物件; V) 移除水; VI) 使物件與其自身接觸或與視 ” WC物;= 較佳者給卜種連結物件之方法,其包括至少下列 27 201241026 步驟 i)用水性分散液作為底漆塗布物件,該分散液包括 a) 至少一種選自由聚胺甲酸酯、聚脲及聚胺曱酸 酯-聚脲組群組成之聚合物, b) 至少一種乙烯屬不飽和化合物,及 c) 至少一種光引發劑; Π)移除水; III) 用光化輻射照射; IV) 用包括至少一種水性分散液之熱可活化黏著劑塗 布物件,該分散液包括至少一種選自由聚胺曱二 酯、聚脲及聚胺甲酸酯-聚脲組成組群之聚合物; V) 移除水; ’ VI)供應熱;及 VII)使物件與其自身接觸或與視情況已根據方法步 驟υ至νυ或!vhVI)處理之進一步物件接 觸。 底漆可於步驟I) 物件表面。 被塗敷於全部物件表面或僅部分 在步驟I)巾錄據本發縣漆 或多:預處理。欲結合的表面獅製造 =清除灰塵、污物、滑脂及任何黏著脫_。此清理 =藉由洗滌及/或機械作用進行 如擦拭、刷 :條係顯著地更有效。 射或超音波處理組合時,洗 t清理溶液可用Γ先條。與機械作用例如 ⑧ 28 特殊情況中可有 進—是義輕射例如 面。 稭助臭氧或機械粗化以活化表 步驟I)中奸诚士 喷霧進行塗敷。㈣佳藉助刷塗、、浸泡或 法及轉移法。舉 塗、汜流、澆灌、印刷 雙鍵之早熟聚合。’、、排除韓射,因其可導致底漆中 步驟II)中,移 、 溫下於供ii+細^7。進行移除水係較佳藉由在升 烘箱、喷霧乾燥与)二:動及視情況亦除濕空氣(對流 用微波。組合數個U㈡=(ir、nir)i可使 於基底不件㈣達到的最大溫度維持低 半或遭受其他損害之極限。 ^ 、中,使物件暴露於光化輻射。有利地使 用乾燥期間導入底漆層之熱能。 進行$田射固化較佳藉由高能量轄射作用,亦即 幸:射或日光(較佳光波長g2()()nm至g75()nm),或 藉由尚旎量電子照射(電子輻射,例如2 90 keV至g 3〇〇 keV)。用於光或11¥光之輻射源為例如中等或高壓汞 蒸η*燈。汞蒸汽可藉由摻雜其他元素(例如鎵或鐵)而 改質。可同樣使用雷射、脈衝燈(以名稱υν閃光燈韓 射器熟知)、_素燈或準分子輻射器。輻射器可以固定 方式安裝,以致欲被照射的物件藉助機械設備而移動通 過輻射源,或輻射器可移動,則欲被照射的物件於固化 201241026 期間不改變其位置。傳統於uv固化情況中足以交聯之 轄射劑量範圍為2 80 mJ/cm2至$ 5000 mJ/cm2、於輻射 強度 2 80 mW/cm2 至 S 3000 mW/cm2。 照射亦可視情況排除氧進行,例如於鈍氣(inert gas) 大氣或減少氧的大氣下。適合鈍氣較佳為氮、二氧化 碳、惰性氣體(noble gas)或燃燒氣體。再者,藉由用對 輻射呈透明之媒質覆蓋乾燥底漆層可進行照射。其實例 為塑膠膜、玻璃或液體(例如水)。 取決於輻射劑量、輻射強度、間隔及進一步固化條 件,底漆所用引發劑之類型及濃度係以熟習技藝人士已 知方式或藉由初步試驗改變或最佳化。針對將乾燥底漆 固化於複雜形狀之三維表面上’特別有利以複數個輻射 器進行,選擇其排列以致(若可能)塗料各點接收固化 輻射之最佳劑量及強度。特別是,欲避免非照射區域(陰 影地區)。 為了盡可能完全聚合乾燥底漆之雙鍵,已證明盡可 能尚的照射溫度及盡可能高的強度與劑量為有利的。另 -方面’取決於所用物件,可有利地 =件上之熱負載不會變得太大。特別是,若由於= 溫度’則薄物件或由具有低玻璃轉移溫度 =科1得之物件可具有衫控形之傾向。 L,、j利地藉助適合遽器或適合輻射器建構,使盡^ 此少Η的紅外線輻射作用於物件上。 =蓋了 形可藉由減少對練射劑量而抵銷。然而,必 30 201241026 須的特定輻射劑量及強度,以便盡可能完全聚合。如此 情況中特別有利地在惰性或減少氧的條件下進行固 化,因為當乾燥底漆上大氣之氧含量減少時,固化所需 劑量降低。 α κ文衣您來輻射器特別佳用於固化。針對固化 荨,料較佳使用劑量g 200 mJ/cm2至g 2000 mJ/Cm、於輻射強度 ^ 20〇 mW/cm2 至 s 2000 mw/cm2。 =驟IV) + ’將黏著劑塗敷。在本發 活化黏著劑。不口物之水性熱可 均未較先===== 本發明方法範,内之総 f確刀而§,使用根據 :使用在無底漆下該.,二:= 使用可乳化於水之聚異氰^兄中較佳者給予 em 0 206 059、de_a:=合物。此等為例如 史所敘述之化合物。聚以納或DE_A _ 24 624 分散液為基礎為(U至2、〇 ^醋^合物之使用量以水性 光、待別佳1.5至6重妙以、較佳〇.5至】0重量 201241026 =V)中’移除‘進行移除水係 溫下於供箱中乾燥並以移動及視情況亦料^ 烘箱、噴霧乾燥器)以及熱輻射(ir、Nir?。、, H皮。組合數個此等乾燥方法為可能及有利的。' = 也’、擇乾燥條件以致達_最大溫度維持低於笑^ 爻控制地變形或遭受其他損害之極限。 土 _不 物VI)卜施予壓力及視情況於升溫下將兩個 物=連結。就方法而論對應先前技藝,連結動作本身並 未提供特殊特徵。使崎連結之條件適應所用 基底。其等可由熟習技藝人士以適合試驗決定。 ^連、、·β可視情況繼之以熱處理,其中於升溫下維持黏 ,結合,以便造成任何存在的交聯劑反應。再者,可進 行冷卻,藉此使連結物件再次冷卻至周圍溫度。 適合交聯劑較佳為聚異氰酸酯(亦呈潛在反應性或 嵌段聚異氰酸酯形式)、聚吖環丙烷與聚碳二醯亞胺、 及亦視情況三聚氰胺。親水性聚異氰酸酯為特別佳於水 ,塗布組成物。交聯劑之用量及官能度特別相配於特別 疋熱負載下黏著結合之所欲強度,且視情況藉助簡單試 驗决疋再者,固化期間黏著劑中交聯劑反應之所需溫 度相配於選擇交聯劑時之乾燥及固化方法。許多可能的 父聯劑減少塗布組成物之貯存壽命,因為其等於水性分 散液中已緩慢反應。因此應在接近塗敷前對應地添加交 聯劑。取決於親水性程度,本身已知之適當方法(例如 以適當剪切力攪拌、藉助混合器分散或合併)用於將交 ⑧ 32 201241026 聯劑併入水性分散液。親水性聚異氰酸酯係例如以名稱
Desmodur®與 Bayhydur® (Bayer MaterialScience AG, Leverkusen, DE)及 Rhodocoat®( Perstorp,SE)可獲得。 本發明進一步提供由根據本發明方法製造之物 件。由根據本發明方法製造之物件為例如鞋子(特別是 運動鞋)’運動物件(例如球、球拍及裝備),及傢俱、 織物、膜及其複合物,來自電腦、電信及消費電子領域 之物件,機動車輛及航空器且特別是内部零件。 【實施方式】 藉助下列實施例更詳細解釋本發明。實施例中,所 用單位具有下列意義: 異氰酸酯含量:呈%表示,在與丁胺反應後以0.1 mol/1氫氯酸反滴定,根據DIN EN ISO 11909決定。 黏度:旋轉黏度計(Haake,type VT 550),於23eC 測量及剪切梯度(除非另予指示)為D 1/40 s-1。 除非另予指示,否則實施例中百分率為重量%。 實施例中,由其等商業名稱指示之化合物意指: Dispercoll® U 54 —陰離子高分子量聚胺甲酸酯分散液 (約 50 % 固體含量),Bayer MaterialScience AG, Leverkusen,D(U 54),用於製備熱可活化水性黏著劑。 Dispercoll UXP 2682—陰離子聚胺曱酸酯分散液(約50 % 固體含量),Bayer MaterialScience AG,Leverkusen,D (XP 2682),用於製備低溫熱可活化之水性黏著劑。 33 201241026
Desmodur® DN—可乳化於水性聚合物分散液之親水性 脂族聚異氰酸酯,以六亞曱基二異氰酸酯(HDI)為主。 NCO 含量 21.8% ;黏度 1250 mPa s。Bayer MaterialScience AG, Leverkusen, D °
Borchi® Gel L 75 N-聚胺甲酸酯為主之非離子液體增 稠劑,OMG Borchers GmbH, Langenfeld,D。
Irgacure® 500、Irgacure 819 DW、Lucirin® TPO-L—光 引發劑,BASF SE,Ludwigshafen,D。
Esacure® TZT—光引發劑,Fratelli Lamberti SpA,Adelate, IT。 下列單體係從 CRAY VALLEY,F-92062 PARIS LA D0FENSE CEDEX - France 的 SARTOMER 部門獲得: SR256 丙烯酸2-(2-乙氧基乙氧基)乙基酯(EOEOEA) SR285 丙烯酸四氫糠基酯(THFA) SR339C丙烯酸2-苯氧基乙基酯(pea) SR506D丙烯酸異莰基醋(IBOA) SR423 甲基丙烯酸異莰基酯(IBOMA) SR833S三環癸烷二曱醇二丙烯酸酯(TCDDA) 下列單體係從BASF SE,Ludwigshafen,D獲得: Laromer®DCPA丙烯酸二氫環戊二烯基酯(DCPA)
Laromer® HDDA 1,6-己二醇二丙稀酸酯(HDDA ) 基底: EVA1 -具有乙酸乙烯酯含量約16 %之射出模製 ⑧ 34 201241026 EVA-Midsole-Phylon EVA2 —具有乙酸乙烯酯含量約20 %之壓縮模製 EVA-Midsole-Phylon EVA3 —具有乙酸乙烯酯含量約18%之射出模製 EVA-Midsole-Phylon 皮革一試驗基底:SATRA Standard-Upper-Leather (SATRA UK ) 橡膠一黑色鞋底橡膠NBR (來自Ube Industries Ltd.以 73%聚丁二烯橡膠BR150L為主) 藉助微差掃描熱量測定法(DSC) — DIN 65467-A 決定陰離子聚胺甲酸酯分散液的熔融峰之熔融給。 將分散液洗灌入特夫綸盤,然後於室溫乾燥七日, 製造Dispercoll® U 54及U XP 2682之乾燥聚合物膜。 從臈上剪下具有質量l〇mg之塊件並導入DSC坩堝,然 後與蓋子用坩堝壓機(crucible press)關閉。將掛禍放置 RT下於熱量計的測量槽中並冷卻至_丨⑽。ς。進行=欠 加熱範圍-100X:至+100°C。加熱速率為20 K/min,以 320 K/min冷卻進行加熱循環。以氮潤洗實行冷卻塊與 測量槽之熱偶合,壓縮機冷卻測量槽。 〃 針對U 54,發現熔融峰於+48.5°C具熔融焓51 3 J/g,同時XP 2682展現波峰於+51.0它具熔融焓料5 j/g (各情況係來自第1次加熱的數值)。 35 201241026 製備UV固化聚胺曱酸酯分散液(UVPUD) 將210.3g經基官能的聚酯丙稀酸酯Laromer® PE44F (BASF AG,Ludwigshafen,DE)、701.3g C4-聚 醚 Tetrathane® 2000 (Invista,Wichita,USA)、43.6 g 二羥甲基丙酸、0.7 g二月桂酸二丁錫、390.0 g丙酮放 置於具有攪拌器、内部溫度計及氣體入口(氣流1 1/h) 之反應容器中;添加157.0g Desmodur® W (環脂族二 異氮酸S旨,Bayer MaterialScience AG,Leverkusen, DE) 及 80.3g Desmodur® Η (脂族二異氰酸酯;Bayer MaterialScience AG,Leverkusen,DE)之混合物,加熱 混合物以致達成固定丙酮回流。在彼溫度進行攪拌直到 反應混合物具有NCO含量1.6%。 然後冷卻混合物至40°C,添加33.6 g乙基二異丙 胺。於40°C 5分鐘攪拌後,將反應混合物澆灌入2250 g 20 C的水並迅速授拌。然後添加於125.〇g水;^ 42.6g異 佛酮二胺。 在未加熱或冷卻下攪拌30分鐘後,於真空中 (50mbar ’最大50°C)蒸餾產物直到達到固體含量35 重量%。分散液具有PH值8.3及平均粒徑1〇〇nm (雷 射相關光譜測量:Zetasizer 1000, Malvern Instruments, Malvern,UK)。4mm燒杯中流動時間:18s。 製備聚胺曱酸酯分散液、UV可固化(甲基)丙烯酸酯 單體及光引發劑之混合物 ⑧ 36 201241026 =相試驗表巾指示之提及聚胺甲_分散 直放置於容器,添加討論試驗表中指示之提及單體用量 及加_拌。5分鐘雜後’添加討論試驗表中指示之 提及光引發·量並同樣地加_拌、然後用去礦質水 建立表中指示之固體含量。5分_拌後, 靜置隔存》 製備水性、熱可活化、後交聯黏著劑 將100.0 g DiSperc〇U u 54放置於反應容器,添加 4.0 g Desmodur DN及加強攪拌。5分鐘㈣後,添加 1.0 g Borchi Gel L 75 N於水之2〇%溶液並同樣地加強
擾拌。5分鐘授拌後’留下調物靜置3G分鐘。黏度 然後為1250 mPas。由於交聯劑異氰酸醋De_durDN 誘發之適用期’在2.5小時之生產内消耗黏著調配物。 製備水性清理溶液 將50,0g氫氧化納、l〇.〇g家庭洗潔液Falter〇1 (清 理劑丨辰度具30%活性物質,Faiter chemie GmbH & CO KG,Krefeld)、50,0g異丙醇及89〇 (^水混合及溶解。 預處理EVA或橡膠基底 形態A:使用溶劑 37 201241026 此乙酸乙醋之纖維布清理欲結合的表面,施予 :被壓力擦拭五次。然後在通風良好位置留下表面未覆 盍至少一小時。 形態B :使用水性清理溶液 將欲結合的表面浸沒於超音波浴之水性清理溶液 中’並以超音波清理10分鐘。然後令溶液滴離表面, 並使表面短暫浸沒於5%檸檬酸水溶液。令溶液再次滴 離後,將表面以去礦質水潤洗一次,在通風良好位置留 下未覆盖至少一小時。 塗敷底漆於EVA或橡膠,乾燥及UV照射 將討論試驗表中提及之底漆藉助精細刷子(China brush)盡可能薄及平坦地塗敷於基底。然後在3(TC於 循環空氣烘箱中進行短時間乾燥,直到從膜移除水《在 試驗不同形式中,獲得層厚大約5 μιη至10 μιη。用中 壓汞輻射器(可調整燈電源60、80或120 W/cm燈長) 進行UV照射。除非另予指示,否則於120 W/cm及波 峰強度1700 mW/cm2與劑量1200 mJ/cm2 (以來自 International Light Inc.之 IL 390C 劑量計測量)將底漆 乾燥後立即進行照射。 EVA或橡膠基底與皮革之結合 在根據試驗表清理且視情況塗布底漆後’將根據試 ⑧ 201241026 驗表具有寬3 cm及長10 cm之EVA或橡膠基底條帶塗 布有水性、熱可活化、後交聯黏著劑。將具有等面積之 皮革塊件連續兩次塗布黏著劑。藉助精細刷子(China brush)以大約bog/m2 (濕)塗敷。各塗敷後,將黏著 劑在65°C於循環空氣烘箱中乾燥5分鐘並藉助熱活 化,在塗布黏者劑之兩個表面已放置一起後’立即以壓
平機按壓(PROTOS Schuhmaschinen Frankfurt a. M D 4 bar線路壓力,30 s)。 ’ ’ 3曰後藉助剝離試驗(根據DIN ΕΝ 1392以1〇〇 mm/rnin拉伸速度180。剝離)測試黏著結合之強度。 試驗中評估基底上材料是否撕裂(正面結果)或結二^ 否分離(負面結果)。 ° & 39 201241026 試驗表1:單體及照射之影響 底漆 撕裂試驗 實施例 聚合物 用量〔g〕 單體 用量〔g〕 基底 3曰後撕 裂之材料 1 (C) U 54 200 (無) — EVA3 否 2(C) U 54 200 (無) — EVA1 否 3 U 54 200 EOEOEA 20 EVA3 部分 4 U 54 200 EOEOEA 20 EVA1 否 5 U 54 200 THFA 20 EVA3 是 6 U 54 200 THFA 20 EVA1 是 7 U 54 200 PEA 20 EVA3 部分 8 U 54 200 PEA 20 EVA1 否 9 U 54 200 DCPA 20 EVA3 是 10 U 54 200 DCPA 20 EVA1 是 11 U 54 200 IBOA 20 EVA3 部分 12 U 54 200 IBOA 20 EVA1 否 13 U 54 200 IBOMA 20 EVA3 部分 14 U 54 200 TCDDA 20 EVA3 是 15 U 54 200 TCDDA 20 EVA1 是 16 U 54 200 HDDA 20 EVA3 部分 17 UVPUD 200 TCDDA 20 EVA3 是 18 UVPUD 200 TCDDA 20 EVA1 部分 ⑧ 40 201241026 所有試驗中,使用2.0%Irgacure 500作為光引發 劑。以溶劑清理EVA。如上述塗敷、乾燥及照射底漆。 然後如上述與皮革結合。 比較例1 (C)及2 (C)顯示在無單體下未達到良 好黏著結合。根據本發明實施例顯示取決於基底性質, 某些單體導致更好黏著結合。相較於試驗14及15,試 驗17及18顯示底漆之聚胺曱酸酯分散液在有及無UV 反應性基兩者下導致良好結合。 201241026 試驗表2 :預處理EVA之影響 底漆 撕裂試 驗 實施例 聚合物 用量〔 單體 用量〔 基底 預處理 3曰後 g〕 g〕 撕裂之 材料 19 (C) U 54 200 (無) 一 EVA3 B -水 否 性 20 (C) U 54 200 (無) — EVA1 B -水 否 性 21 U 54 200 TCDDA 20 EVA3 (無) 部分 22 U 54 200 TCDDA 20 EVA1 (無) 否 14 U 54 200 TCDDA 20 EVA3 A —溶 是 劑 15 U 54 200 TCDDA 20 EVA1 A —溶 是 劑 23 U 54 200 TCDDA 20 EVA3 B -水 是 性 24 U 54 200 TCDDA 20 EVA1 B -水 是 性 所有試驗中,使用2.0%Irgacure 500作為光引發 劑。如上述塗敷、乾燥及照射底漆。然後如上述與皮革 結合。 ⑧ 42 201241026 試驗14、15、19 (C)至24顯示清理EVA材料為 有利,用水性清理達到的結果等於以溶劑擦拭獲得的結 果。 試驗表3 : PUD及單體用量之影響 底漆 撕裂試驗 實施例 聚合物 用量〔g〕 單體 用量〔g〕 基底 3日後撕 裂之材料 1(c) U 54 200 (無) — EVA3 否 2(C) U 54 200 (無) — EVA1 否 25 (C) UVPUD 200 (無) — EVA3 否 26 ( C) UVPUD 200 (無) — EVA1 否 27 (C) (無) 氺 TCDDA 氺 EVA3 部分 28 (C) (無) 氺 TCDDA 氺 EVA1 否 14 U 54 200 TCDDA 20 EVA3 是 15 U 54 200 TCDDA 20 EVA1 是 29 U 54 200 TCDDA 30 EVA3 是 30 U 54 200 TCDDA 30 EVA1 是 31 U 54 200 TCDDA 15 EVA3 是 32 U 54 200 TCDDA 15 EVA1 是 33 U 54 200 TCDDA 10 EVA3 是 34 U 54 200 TCDDA 10 EVA1 部分 35 U 54 200 TCDDA 5 EVA3 部分 36 U 54 200 TCDDA 5 EVA1 否 43 201241026 * )-藉助 0.2%Disponil FES 32 (乳化劑,Cognis SE,Dtisseldorf,D)與 Ultra-Turrax,將 TCDDA 加工成具 有限制貯存穩定性之20%乳液。 所有試驗中,使用2.0%Irgacure 500作為光引發 劑。以浴劑清理EVA。如上述塗敷、乾燥及照射底漆。 然後如上述與皮革結合。 試驗 1(C)、2(C)、14、15、25(C)至 36 顯 不遍及廣泛濃度範圍組合PUD與單體作為底漆導致良 好結果,同時PUD、UVpUD或單體其等自身單獨無法 引起足夠良好結合。 试驗表4 .各種基底 底漆 撕裂試驗 實施例 聚合物 用量〔g〕 單體 用量〔g〕 基底 3曰後撕 裂之材料 1 (C) U 54 200 (無) EVA3 否 2(C) U 54 200 (無) EVA1 否 37 (C) U 54 200 (無) 橡膠 否 39 (C) (無) EVA3 否 40 (〇 (無) EVA1 否 41 (C) (無) 橡膠 否 14 U 54 200 TCDDA 20 EVA3 是 15 U 54 200 TCDDA 20 EVA1 且 疋 43 U 54 200 TCDDA 20 EVA2 是 44 U 54 200 TCDDA 20 橡膠 是 201241026 所有試驗中,使用2.0%Irgacure 500作為光引發 劑。以溶劑清理EVA。如上述塗敷、乾燥及照射底漆。 然後如上述與皮革結合。 試驗 1(C) '2(0、37(C)至 42(C)、14、 15、43至44顯示良好結合,且該良好結合無法出現於 無底漆或有底漆但無UV可固化單體之任何基底,同時 根據本發明之底漆對各種基底引起改良黏著性。 試驗表5 :光引發劑及UV輻射之影響 底漆 撕裂試 驗 實施 聚合物 用 單體 用 光引發 照射 3曰後撕 例 量 量 劑 裂之材 C C 料 g〕 g〕 46 XP 200 TCDDA 19 Irgacure Hg ; 是 2682 500 1700mW/cm2 » 1200mJ/cm2 47 XP 200 TCDDA 19 Irgacure Ga ; 是 2682 500 148mW/cm2 t 554mJ/cm2 48 XP 200 TCDDA 19 Esacure Ga ; 是 45 201241026 2682 TZT 148mW/cm2 t 554mJ/cm2 49 XP 200 TCDDA 19 Lucirin Ga ; 是 2682 TPO-L 148mW/cm2 554mJ/cm2 50 XP 200 TCDDA 19 Irgacure Ga ; 部分 2682 819 DW 148mW/cm2 » 554mJ/cm2 所有光引發劑在試驗中各以2.0%的量使用。使用 以水性預處理(型態B)之EVA1作為基底。如上述塗 敷、乾燥底漆。根據表照射(Hg—中壓汞燈120W/cm, Ga-鎵摻雜的中壓燈60W/cm)。然後如上述與皮革結 合。 試驗46至50顯示根據本發明底漆之照射條件(亦 即光引發劑、強度、燈類型)可在寬廣範圍内變化。 【圖式簡單說明】 無 【主要元件符號說明】 無 46 ⑧
Claims (1)
- 201241026 七 申請專利範圍: 1. 一種水性分散液作為底漆之用途,該分散液包括 a) 至少一種選自由聚胺曱酸酯、聚脲及聚胺曱 酸酯-聚脲組成之組群之聚合物, b) 至少一種乙烯屬不飽和化合物,及 c) 至少一種光引發劑, 其係塗布至選自由乙烯-乙酸乙烯酯共聚物、 橡膠、聚烯烴及其混合物組成之組群之基底。 2. —種連結物件之方法,其包括至少下列步驟 I) 用水性分散液作為底漆以塗布物件,該分散 液包括 a) 至少一種選自由聚胺曱酸酯、聚脲及聚胺 曱酸酯-聚脲組成之組群之聚合物, b) 至少一種乙烯屬不飽和化合物,及 c) 至少一種光引發劑; II) 移除水; III) 用光化輻射照射; IV) 用黏著劑塗布物件; V) 移除水; VI) 使該物件與其自身接觸或與視情況已根據方 法步驟I)至V)或IV)至V)處理之進一步 物件接觸。 47 201241026 3. 根據申請專利範圍第2項之方法,其中步驟I)之 該聚合物為結晶或半結晶。 4. 根據申請專利範圍第2項之方法,其中根據DIN 65467以加熱速率20 K/min的DSC測量中,步驟 I)之該聚合物具有對應熔融焓之熔融峰>3 J/g。 5. 根據申請專利範圍第2項之方法,其中步驟之 該聚合物含有乙烯屬不飽和雙鍵。 6. 根據申請專利範圍第2或5項之方法,其中該乙 烯屬不飽和化合物係選自由丙烯酸酯、甲基丙烯 酸酯、巴豆酸酯、乙烯醚、乙烯酯及乙烯基芳香 族化合物組成之組群。 7. 根據申請專利範圍第2、5或6項之方法其中該 乙烯屬不飽和化合物含有芳香族或環脂族基。/ 8·=申請專利範圍第2項之方法,其中該黏著劑 糸3有至少一種水性分散液之熱可活化黏著劑, 該分散液含有至少-種選自由聚胺甲酸龍 及聚胺甲酸酯-聚脲組成之組群之聚合物。人 根據申請專利範圍第2項之方法,其中該方法額 48 201241026 外包括供應熱於基底之步驟Va)。 10. 根據申請專利範圍第2項之方法,其中該物件係 選自由乙烯-乙酸乙烯酯共聚物,橡膠例如SBR(苯 乙烯丁二烯橡膠)、NBR(腈丁二烯橡膠)、TR (熱塑性橡膠)、天然橡膠、EPDM (乙烯-丙烯- 二烯橡膠),聚烯烴及其他熱塑性材料,及其混 合物組成之組群之材料。 11. 一種物件,其係由根據申請專利範圍第2至9項 中任一項之方法製造。 49 201241026 四、指定代表圖: (一) 本案指定代表圖為: 無 (二) 本代表圖之元件符號簡單說明: 無 五、本案若有化學式時,請揭示最能顯示發明特徵的化 學式= 無 ⑧
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EP3536726A1 (en) * | 2018-03-06 | 2019-09-11 | Covestro Deutschland AG | Coated product or article and method for manufacturing the same |
WO2020081279A1 (en) * | 2018-10-17 | 2020-04-23 | Dow Global Technologies Llc | A coating composition, a coated fabric, a method of making a coated fabric, and an article made from the coated fabric |
KR102279044B1 (ko) * | 2019-11-18 | 2021-07-19 | 송준혁 | 복합탄성중합체 조성물과 구조보강용 층 그리고 복합탄성중합체의 시공방법 |
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- 2011-11-21 SG SG2013030853A patent/SG189974A1/en unknown
- 2011-11-21 EP EP20110785423 patent/EP2643375B1/en active Active
- 2011-11-21 US US13/989,514 patent/US20130273359A1/en not_active Abandoned
- 2011-11-21 BR BR112013012452A patent/BR112013012452A2/pt not_active IP Right Cessation
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- 2011-11-21 JP JP2013540312A patent/JP2014502301A/ja not_active Withdrawn
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TWI537296B (zh) | 2016-06-11 |
ZA201304751B (en) | 2014-12-23 |
WO2012069412A1 (en) | 2012-05-31 |
MX2013004610A (es) | 2013-12-02 |
EP2643375B1 (en) | 2014-08-27 |
JP2014502301A (ja) | 2014-01-30 |
EP2643375A1 (en) | 2013-10-02 |
US20130273359A1 (en) | 2013-10-17 |
SG189974A1 (en) | 2013-06-28 |
AU2011333950A1 (en) | 2013-07-04 |
CA2819076A1 (en) | 2012-05-31 |
RU2013128890A (ru) | 2015-01-10 |
BR112013012452A2 (pt) | 2016-08-30 |
IL225877A0 (en) | 2013-06-27 |
KR20130135263A (ko) | 2013-12-10 |
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