TW202246425A - 熔融性氟樹脂底漆 - Google Patents
熔融性氟樹脂底漆 Download PDFInfo
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- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
本發明提供一種在以水為分散介質之水系底漆中之分散穩定性得到提高之熔融性氟樹脂底漆。
本發明之熔融性氟樹脂底漆之特徵在於包含四氟乙烯/六氟丙烯共聚物（FEP）粒子、耐熱性樹脂、非離子性界面活性劑及水，且上述FEP之平均粒徑為10～60 μm，上述耐熱性樹脂為選自由聚醯胺醯亞胺樹脂、聚醚碸及聚醯亞胺樹脂所組成之群中至少一種，上述FEP粒子與上述耐熱性樹脂之固形物成分質量比為50：50～95：5，非離子性界面活性劑為聚氧乙烯烷基醚系界面活性劑，上述熔融性氟樹脂底漆包含以質量基準計為10～60%之水。
Description
本發明係關於一種熔融性氟樹脂底漆。
一般而言，利用氟樹脂所具有之優異之耐熱性、耐化學品性、阻燃性等，廣泛使用氟樹脂、其中廣泛使用全氟聚合物作為化學工場或半導體工場中之耐蝕襯裡用塗佈材料。然而，全氟聚合物與金屬之密合性較差，因此於大多數情形，會將對金屬基材之密合性優異之底漆層作為由全氟聚合物所構成之面塗層（topcoat）之下塗層，設置於金屬基材之表面。
先前，已知有各種底漆，其等使各種金屬基材、與以四氟乙烯/全氟烷基乙烯基醚共聚物（PFA）粒子或四氟乙烯/六氟丙烯共聚物（FEP）粒子等熔融性全氟聚合物為主成分之膜厚50 μm以上之面塗層接著。例如，有以有機溶劑為分散介質之底漆、或含有醯胺系樹脂作為黏合劑樹脂之主成分之粉體狀底漆等。
專利文獻1中揭示有一種氟樹脂被覆用底漆組成物，其係使聚醚碸、聚醯胺醯亞胺及/或聚醯亞胺、氟樹脂、以及金屬粉末溶解或分散於有機溶劑中而成者。
專利文獻2中揭示有一種底漆組成物，其特徵在於含有聚芳基酮系樹脂、鈦有機化合物、氟樹脂，且鈦有機化合物中所含之鈦之含量為特定量。
專利文獻3中揭示有一種ETFE塗料用底漆，其係由乙烯/四氟乙烯共聚物（ETFE）粒子、選自由聚醯胺醯亞胺樹脂、聚醚碸樹脂及聚醯亞胺樹脂所組成之群中至少一種耐熱性樹脂、以及聚氧乙烯烷基醚系界面活性劑所構成。
先前技術文獻
專利文獻
專利文獻1：日本特開平6-264000號公報
專利文獻2：日本特開2010-83924號公報
專利文獻3：日本專利第6753546號公報
[發明所欲解決之課題]
本發明之目的在於提供一種熔融性氟樹脂底漆，其可於金屬基材等被塗裝物與由熔融性全氟聚合物所構成之面塗層之間獲得較高之接著強度。
[解決課題之技術手段]
本發明係一種熔融性氟樹脂底漆，其特徵在於：包含四氟乙烯/六氟丙烯共聚物（FEP）粒子、耐熱性樹脂、非離子性界面活性劑及水，且上述FEP之平均粒徑為10～60 μm，上述耐熱性樹脂為選自由聚醯胺醯亞胺樹脂、聚醚碸及聚醯亞胺樹脂所組成之群中至少一種，上述FEP粒子與上述耐熱性樹脂之固形物成分質量比為50：50～95：5，非離子性界面活性劑為聚氧乙烯烷基醚系界面活性劑，上述熔融性氟樹脂底漆包含以質量基準計為10～60%之水。
較佳為進而含有選自由乙炔二醇系界面活性劑、醇、酮、酯及芳香族烴所組成之群中至少一種之分散介質。
較佳為FEP粒子之熔體流動速率為0.1～50 g/10分鐘。
較佳為進而含有相對於FEP粒子之固形物成分以質量基準計為0.001～5%之熱穩定劑。
本發明亦係一種底漆皮膜，其由上述熔融性氟樹脂底漆所形成。
本發明亦係一種積層體，其係於上述底漆皮膜之上設有包含熔融性全氟聚合物之皮膜者。
本發明亦係一種塗裝物品，其係於金屬基材上設有上述積層體者。
本發明亦係一種塗裝物品，其係於金屬基材之內表面設有上述積層體者，上述金屬基材為配管、管道管（pipe）或導管（duct）。
[發明之效果]
根據本發明，可於金屬基材等被塗裝物與由熔融性全氟聚合物所構成之面塗層之間獲得較高之接著強度。又，根據本發明，可提供一種在以水為分散劑之水系底漆中之分散穩定性得到提高之熔融性氟樹脂底漆。
以下，對本發明進行詳細說明。
本發明之熔融性氟樹脂底漆之特徵在於，其係包含四氟乙烯（TFE）/六氟丙烯（HFP）共聚物（FEP）粒子、耐熱性樹脂、非離子性界面活性劑及水者，且上述FEP之平均粒徑為10～60 μm，上述耐熱性樹脂為選自由聚醯胺醯亞胺樹脂、聚醚碸及聚醯亞胺樹脂所組成之群中至少一種，上述FEP粒子與上述耐熱性樹脂之固形物成分質量比為50：50～95：5，非離子性界面活性劑為聚氧乙烯烷基醚系界面活性劑，上述熔融性氟樹脂底漆包含以質量基準計為10～60%之水。
根據持有設備之情況等，存在欲使用液狀底漆而非粉體狀底漆之市場需求。於使用液體底漆之情形時，希望為水系底漆，但於以水為分散介質之底漆中，熔融性氟樹脂粒子之分散穩定性存在問題。
本發明提供一種在以水為分散介質之水系底漆中之分散穩定性得到提高之熔融性氟樹脂底漆。
FEP粒子於熔融性氟樹脂中亦具有相對較高之耐熱性、耐蝕性、阻燃性，於全氟聚合物中具有相對較低之熔點，就該方面而言，適宜用於底漆。
又，為了於被塗裝物與由熔融性全氟聚合物所構成之面塗層之間獲得較高之接著強度，須使用粒徑較大之FEP粒子。
然而，於熔融性氟樹脂粒子中，FEP粒子尤其是疏水性較強，於其粒徑較大為10～60 μm之情形時，使其分散於水中極為困難。本發明之熔融性氟樹脂底漆藉由使用聚氧乙烯烷基醚系界面活性劑作為非離子性界面活性劑，而實現FEP粒子在底漆中之優異之分散穩定性。
如上所述，上述FEP粒子之平均粒徑為10～60 μm。若平均粒徑過小，則無法介隔底漆皮膜獲得被塗裝物與由熔融性全氟聚合物所構成之面塗層之間的較高之接著強度。另一方面，若平均粒徑變得過大，則難以形成均勻之底漆皮膜，而有與面塗層之間之接著強度局部地發生降低之虞。又，粒子之沈澱變得顯著，無法保持靜置穩定性。上述平均粒徑之較佳之下限為11 μm，更佳之下限為15 μm，並且較佳之上限為50 μm。
上述平均粒徑係藉由雷射繞射法所測得[商品名：Microtrac公司之MT-3300II]之體積基準中值粒徑。
上述FEP較佳為熔體流動速率（MFR）為0.1～50 g/10分鐘。若處於上述熔體流動速率之範圍內，則所獲得之底漆皮膜與熔融性全氟聚合物皮膜之密合性因上述FEP粒子之流動特性而進一步提高。又，上述底漆皮膜不易產生應力龜裂或壓力龜裂，耐蝕性提高。上述熔體流動速率之更佳之下限為0.5 g/10分鐘，更佳之上限為30 g/10分鐘。
於本說明書中，上述FEP之MFR係以依據ASTM D2116，於溫度372℃、2.16 Kg之負載從直徑2 mm之噴嘴歷時10分鐘所擠出之重量表示。
上述FEP可藉由調整下述共聚組成或分子量，而具有上述範圍內之熔體流動速率。
作為上述FEP，並無特別限定，較佳為TFE單位與HFP單位之莫耳比（TFE單位/HFP單位）為70/30以上且未達99/1之共聚物。更佳之莫耳比為70/30以上且98.9/1.1以下，進而較佳之莫耳比為80/20以上且98.9/1.1以下。若TFE單位過少，則機械物性存在降低傾向，若過多，則熔點變得過高，成形性存在降低傾向。
上述FEP樹脂只要為具有上述組成者，便亦可為進而使其他單體聚合而成者。作為上述其他單體，例如可例舉全氟烷基乙烯基醚（PAVE）等。
上述其他單體通常較佳為FEP樹脂之15 mol%以下。更佳之上限為10 mol%，進而較佳之上限為5 mol%。
上述FEP粒子之製造方法並無特別限定，例如可藉由乳化聚合等先前公知之聚合方法等進行共聚而獲得。藉由共聚所獲得之FEP係視需要以成為具有上述範圍內之平均粒徑之FEP粒子之方式進行粉碎。作為上述粉碎之方法，並無特別限定，例如可使用先前公知之方法。例如可例舉利用輥將藉由上述乳化聚合法所獲得之FEP乾燥粉末壓縮成片狀，利用粉碎機進行粉碎並進行分級之方法等。於使用乳化聚合或懸浮聚合而獲得上述FEP之情形時，上述FEP只要為滿足上述各條件者，便亦可不只單離出所獲得之樹脂成分而以分散狀態使用。
作為上述聚氧乙烯烷基醚系界面活性劑，例如較佳為下式所表示者：
R-O-A-H
（式中，R為直鏈狀或支鏈狀之碳數5～18之烷基，A為具有5～20個氧乙烯基之聚氧乙烯鏈）。
作為R之烷基之碳數更佳為10～16。作為上述烷基，可例示癸基、月桂基、十三烷基、鯨蠟基、硬脂基等，可為直鏈狀亦可為支鏈狀。
上述聚氧乙烯鏈更佳為具有7～15個氧乙烯基。
就界面活性能力優異之方面、為水溶性之方面、容易獲取之方面等而言，較佳為R為碳數10～16之烷基，且聚氧伸烷基鏈具有7～15個氧乙烯基之聚氧乙烯烷基醚系界面活性劑。該界面活性劑之製造原料可使用天然或合成之高級醇，但較佳為完全不含烷基酚類。
上述聚氧乙烯烷基醚系界面活性劑之含量較佳為相對於上述FEP粒子為1.0～20.0質量%。上述含量更佳為3.0質量%以上，進而較佳為5.0質量%以上。又，更佳為15.0質量%以下，進而較佳為10.0質量%以下。
若處於該範圍內，則獲得上述FEP粒子之分散穩定性優異之底漆。
上述聚氧乙烯烷基醚系界面活性劑較佳為HLB為10～15。更佳之HLB範圍為12～14。若處於該範圍內，則可使氟樹脂粒子於水中穩定地分散。
再者，於本發明中，HLB係利用格里芬法（Griffin method）藉由下述計算式定義之值。
HLB值＝20×[親水部之化學式量之總和]/分子量
上述聚氧乙烯烷基醚系界面活性劑容易熱分解，難以殘存於焙燒後之塗膜中，因此於所獲得之底漆皮膜中，不易妨礙上述FEP粒子及上述耐熱性樹脂所帶來之密合性效果。因此，底漆皮膜與被塗裝物及熔融性全氟聚合物皮膜之密合性提高。
本發明之熔融性氟樹脂底漆包含耐熱性樹脂。上述耐熱性樹脂為選自由聚醯胺醯亞胺樹脂（PAI）、聚醚碸樹脂（PES）及聚醯亞胺樹脂（PI）所組成之群中至少一種。作為上述耐熱性樹脂，其中就耐熱性方面而言，較佳為PAI。
PAI係由分子結構中具有醯胺鍵及醯亞胺鍵之聚合物所構成之樹脂。作為上述PAI，並無特別限定，例如可例舉由藉由下述各反應所獲得之高分子量聚合物所構成之樹脂等，上述反應例如為：分子內具有醯胺鍵之芳香族二胺與焦蜜石酸等芳香族四元羧酸之反應；1,2,4-苯三甲酸酐等芳香族三元羧酸與4,4-二胺基苯醚等二胺或二苯基甲烷二異氰酸酯等二異氰酸酯之反應；分子內具有芳香族醯亞胺環之二元酸與二胺之反應。就耐熱性優異之方面而言，上述PAI較佳為由主鏈中具有芳香環之聚合物所構成者。
PES係由具有下述通式：
所表示之重複單位之聚合物所構成之樹脂。作為PES，並無特別限定，例如可例舉由藉由二氯二苯基碸與雙酚之縮聚所獲得之聚合物所構成之樹脂等。
PI係由分子結構中具有醯亞胺鍵之聚合物所構成之樹脂。作為上述PI，並無特別限定，例如可例舉由下述高分子量聚合物所構成之樹脂等，該高分子量聚合物係藉由焦蜜石酸酐等芳香族四元羧酸酐與4,4-二胺基苯醚等二胺之反應等所獲得者。就耐熱性優異之方面而言，上述PI較佳為由主鏈中具有芳香環之聚合物所構成者。
上述耐熱性樹脂適宜的是粒子狀。其平均粒徑較佳為0.5～20 μm，更佳為1～10 μm。若耐熱性樹脂粒子之平均粒徑處於該範圍內，則可獲得均勻之水分散體。
上述平均粒徑係藉由雷射繞射法所測得[商品名：Microtrac公司之MT-3300II]之體積基準中值粒徑。
上述FEP粒子與上述耐熱性樹脂之固形物成分質量比為50：50～95：5。若上述FEP粒子過少，則所獲得之底漆皮膜與熔融性全氟聚合物皮膜之密合性變差而引起層間剝離，若過多，則上述底漆皮膜與被塗裝物之密合力降低。上述固形物成分質量比之較佳之下限為70：30，更佳之下限為76：24，並且較佳之上限為85：15。
本發明之熔融性氟樹脂底漆係包含水者。水之含量以質量基準計為10～60%。
水之含量之下限更佳為20質量%，進而較佳為25質量%。水之上限更佳為50質量%，進而較佳為40質量%。若水之含量處於該範圍內，則可獲得均勻之水分散體。
本發明之熔融性氟樹脂底漆較佳為進而含有選自由乙炔二醇系界面活性劑、醇、酮、酯及芳香族烴所組成之群中至少一種之分散介質。作為上述分散介質，就熔融性氟樹脂在水中之分散穩定性之方面而言，特佳為乙炔二醇系界面活性劑。
上述乙炔二醇系界面活性劑係分子中具有碳-碳三鍵之界面活性劑。作為上述乙炔二醇系界面活性劑，例如可例舉乙炔二醇（於同一分子內同時具有乙炔鍵及2個羥基）界面活性劑、對乙炔二醇加成環氧烷單元所得之界面活性劑。
作為此種乙炔二醇系界面活性劑，具體而言，例如可例舉下述通式（1）所表示之化合物、及/或下述通式（2）所表示之化合物。
上述乙炔二醇系界面活性劑較佳為在熱重量分析中300℃時之殘量為3.0質量%以上。藉由使用在熱重量分析中300℃時之殘量為3.0質量%以上之乙炔二醇系界面活性劑，即便為於熱熔融時以高溫進行加熱之情形，乙炔二醇系界面活性劑亦殘存於塗膜中，藉此可發揮各種功能，就該方面而言較佳。
於本發明中，300℃時之殘存質量比例係使用示差熱-熱重量測定裝置[TG-DTA]（商品名：TG/DTA7200；Hitachi High-Tech Science公司製造），將試樣10 mg以10℃/分鐘之升溫速度從室溫進行升溫，於300℃所殘存之試樣之質量比例。
於本發明中，乙炔二醇系界面活性劑較佳為上述通式（2）所表示之乙炔二醇之環氧乙烷加成物。乙炔二醇之環氧乙烷加成物容易成為在上述熱重量分析中300℃時之殘量滿足3.0質量%以上者，藉此於高溫之加熱硬化時亦可獲得良好之效果，就該方面而言較佳。
上述乙炔二醇系界面活性劑亦可使用市售品。例如可例舉：Surfynol（註冊商標）440、465、485、SE、2502、Olfine（註冊商標）PD-002W、EXP.4200、E1004、E1010（均為日信化學工業公司製造）、Acetylenol（註冊商標）E00、Acetylenol E13T、Acetylenol E40、Acetylenol E60、Acetylenol E100、Acetylenol E200（以上為川研精細化學股份有限公司製造）等。
上述乙炔二醇系界面活性劑較佳為HLB超過4，更佳為5以上。進而較佳為6以上，最佳為8以上。
HLB較高之乙炔二醇系界面活性劑之耐熱性優異。
再者，於本發明中，HLB係利用格里芬法，藉由下述計算式定義之值。
HLB值＝20×[親水部之化學式量之總和]/分子量
本發明之熔融性氟樹脂底漆較佳為，乙炔二醇系界面活性劑之含量相對於上述FEP粒子為0.05～5.0質量%。上述乙炔二醇系界面活性劑之含量之下限更佳為0.1質量%，進而較佳為0.5質量%。上述乙炔二醇系界面活性劑之上限更佳為3.5質量%，進而較佳為2.8質量%。若乙炔二醇系界面活性劑之含量處於該範圍內，則熔融性氟樹脂底漆之分散穩定性較為良好。
本發明之熔融性氟樹脂底漆亦可進而含有用以使上述耐熱性樹脂溶解之耐熱性樹脂溶解溶劑。在使上述耐熱性樹脂溶解於上述耐熱性樹脂溶解溶劑中，並均勻地分散於熔融性氟樹脂底漆內之情形時，可藉由塗佈而使上述耐熱性樹脂遍及至被塗裝物上之各角落，可提高與上述被塗裝物之密合性。
作為上述耐熱性樹脂溶解溶劑，可使用能夠溶解上述耐熱性樹脂之溶劑，較佳為1氣壓（atm）下之沸點為100℃以上者。
上述耐熱性樹脂溶解溶劑可例舉：N-甲基-2-吡咯啶酮、N-乙基-2-吡咯啶酮、N-丁基-2-吡咯啶酮、3-烷氧基-N,N-二甲基丙醯胺、二甲基亞碸、1,3-二甲基-2-咪唑啶酮、3-甲基-2-
唑啶酮、N-甲醯基嗎福啉、N-乙醯基嗎福啉、二甲基伸丙基脲、甲基苯基醚、二乙醚、乙二醇、苯乙酮、甲基乙基酮、甲基異丁基酮、環己酮、環戊酮、二甲苯、甲苯、乙醇及2-丙醇等。
其中，更佳為選自由N-乙基-2-吡咯啶酮、N-丁基-2-吡咯啶酮、3-烷氧基-N,N-二甲基丙醯胺、1,3-二甲基-2-咪唑啶酮、3-甲基-2-唑啶酮、N-甲醯基嗎福啉、N-乙醯基嗎福啉及二甲基伸丙基脲所組成之群中至少一種。
上述3-烷氧基-N,N-二甲基丙醯胺由N(CH
3)
2COCH
2CH
2OR
11（R
11為烷基）所表示。烷氧基（R
11O基）並無特別限定，較佳為包含碳數1～6左右之低級烷基之烷氧基，更佳為甲氧基、乙氧基、丙氧基或丁氧基。作為上述3-烷氧基-N,N-二甲基丙醯胺，特佳為3-甲氧基-N,N-二甲基丙醯胺（N(CH
3)
2COCH
2CH
2OCH
3）。
上述耐熱性樹脂溶解溶劑較佳為相對於上述耐熱性樹脂為10質量%以上。若處於上述範圍內，則更容易使上述耐熱性樹脂遍及至被塗裝物上，更容易提高與被塗裝物之密合性。更佳之下限為50質量%。若上述耐熱性樹脂溶解溶劑增加，則與被塗裝物之密合性存在提高傾向，但鑒於工業性生產，較佳之上限為500質量%，更佳之上限為350質量%。
於本發明之熔融性氟樹脂底漆中，N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺及γ-丁內酯之合計量較佳為相對於上述熔融性氟樹脂塗料用底漆未達0.1質量%。上述合計量更佳為未達0.01質量%，進而較佳為未達0.001質量%。
上述合計量係藉由液相層析法所測定之值。
本發明之熔融性氟樹脂底漆亦較佳為均不含N-甲基-2-吡咯啶酮、N,N-二甲基乙醯胺、N,N-二甲基甲醯胺及γ-丁內酯。
本發明之熔融性氟樹脂底漆亦可為進而含有熱穩定劑者。本發明之熔融性氟樹脂底漆藉由含有上述熱穩定劑，可防止由熔融性氟樹脂皮膜形成中之加熱等所導致之上述FEP及上述耐熱性樹脂之氧化而減輕熱劣化，其結果為，可進一步提高密合穩定性。
作為上述熱穩定劑，就防止上述FEP及上述耐熱性樹脂之氧化之方面而言，較佳為胺系抗氧化劑及/或有機含硫化合物。
作為上述胺系抗氧化劑，例如可例舉於分子中具有苯基、萘基等芳香族性烴基之芳香族胺，例如可例舉：N,N'-二苯基-對苯二胺、N,N'-二-2-萘基-對苯二胺、二苯胺與二異丁烯之反應產物等苯二胺系化合物；二萘胺、苯基-α-萘胺、苯基-β-萘胺、4,4'-雙(α,α'-二甲基苄基)二苯胺、苯基環己基-對苯二胺、苯乙烯化二苯胺等其他芳香族二級胺化合物等。
作為上述胺系抗氧化劑，可例舉具有以苯并三唑為基本骨架之化學結構之苯并三唑系化合物，係可形成金屬鹽等鹽者。作為上述苯并三唑系化合物，並無特別限定，例如可例舉：苯并三唑、2-(2-羥基-5-甲基苯基)苯并三唑、2-(2-羥基-5-四辛基苯基)苯并三唑等。
作為上述有機含硫化合物，例如可例舉2-巰基苯并咪唑、2-巰基甲基苯并咪唑等巰基苯并咪唑系化合物；2-巰基苯并噻唑、2-巰基苯并噻唑之環己基胺鹽、二硫化二苯并噻唑（dibenzothiazyl disulfide）、2-(N,N'-二乙基硫胺基甲醯基硫)苯并噻唑、2-(4'-
啉二硫)苯并噻唑、N-環己基-2-苯并噻唑次磺醯胺、N-氧聯二伸乙基-2-苯并噻唑次磺醯胺、N-第三丁基-2-苯并噻唑次磺醯胺、N,N'-二環己基-2-苯并噻唑次磺醯胺、N,N'-二異丙基苯并噻唑-2-次磺醯胺等巰基苯并噻唑系化合物；2-巰基咪唑啉等巰基咪唑啉系化合物；伸戊基二硫代胺基甲酸、哌可二硫代胺基甲酸（pipecolyl dithiocarbamic acid）、二甲基二硫代胺基甲酸、二乙基二硫代胺基甲酸、二丁基二硫代胺基甲酸、N-乙基-N-苯基二硫代胺基甲酸等二硫代胺基甲酸類等；其等亦可為例如Zn、Sn、Cd、Cu、Fe等之金屬鹽、哌啶鹽、哌可鹽等有機鹽等。
作為上述有機含硫化合物，例如可例舉秋蘭姆（thiuram）系化合物，例如可例舉：一硫化四甲基秋蘭姆等一硫化秋蘭姆；二硫化四甲基秋蘭姆、二硫化四乙基秋蘭姆、二硫化四丁基秋蘭姆等二硫化秋蘭姆；四硫化二伸戊基秋蘭姆等其他秋蘭姆系化合物等。
作為上述有機含硫化合物，又，例如較佳為與氮原子鍵結之氫原子之至少1個可被取代為碳數1～6之飽和或不飽和烴基之硫脲，亦可為硫脲、N,N'-二乙基硫脲、N,N'-二丁基硫脲、二月桂基硫脲、N,N'-二苯基硫脲等硫脲衍生物等。
作為上述熱穩定劑，其中，就要求在本發明之熔融性氟樹脂底漆或面塗層之熔融性全氟聚合物塗料中所含之熔融性氟樹脂之熔點附近之溫度以上、例如於約250℃以上之高溫的穩定性之方面而言，較佳為含芳香環之化合物，更佳為芳香族胺、巰基苯并噻唑系化合物及巰基苯并咪唑系化合物。
上述熱穩定劑可藉由先前公知之方法進行製造，但通常可使用市售品。
作為上述熱穩定劑，可使用一種或組合兩種以上而使用。於組合使用之情形時，上述熱穩定劑之質量係所組合之所有熱穩定劑之合計質量。
於本發明之熔融性氟樹脂底漆中包含上述熱穩定劑之情形時，就熱穩定效果、及防止上述熱穩定劑之分解所致之起泡之觀點而言，相對於上述FEP粒子之固形物成分，上述熱穩定劑較佳為0.001～5質量%。更佳之下限為0.003質量%，更佳之上限為2質量%。
本發明之熔融性氟樹脂底漆亦可視需要進而含有添加劑。作為上述添加劑，並無特別限定，例如可例舉一般塗料之底漆中所使用者等。作為上述添加劑，例如可例舉：顏料、填充材、調平劑、固體潤滑劑、沈澱防止劑、水分吸收劑、表面調整劑、觸變性賦予劑、黏度調節劑、抗膠凝劑、紫外線吸收劑、光穩定劑、塑化劑、抗分色劑、防結皮劑、抗擦傷劑、防黴劑、抗菌劑、抗氧化劑、抗靜電劑、矽烷偶合劑等。
作為上述添加劑，具體而言，例如可例舉：碳、氧化鈦、紅丹、雲母等著色顏料、防銹顏料、焙燒顏料、體質顏料、光致發光扁平顏料、鱗片狀顏料、木粉、石英砂、碳黑、黏土、滑石、金剛石、氟化金剛石、鋼玉、矽石、氮化硼、碳化硼、碳化矽、熔鋁氧、電氣石、翡翠、鍺、氧化鋯、碳化鋯、金綠寶石、黃玉、綠寶石、石榴石、玻璃、玻璃粉、雲母粉、金屬粉（金、銀、銅、鉑、不鏽鋼、鋁等）、各種強化材、各種增量材、導電性填料等。
相對於上述熔融性氟樹脂底漆，上述添加劑之含量較佳為0～10.0質量%，更佳為0～5.0質量%。
本發明之熔融性氟樹脂底漆例如係藉由先前公知之方法等進行製備。例如可例舉將上述FEP粒子、耐熱性樹脂、非離子性界面活性劑、水、以及視需要之分散介質、熱穩定劑等進行混合，進而視需要添加上述耐熱性樹脂溶解溶劑並進行攪拌而使其分散之方法等。
本發明之熔融性氟樹脂底漆係用以形成設置於熔融性全氟聚合物皮膜之下的底漆皮膜者，較佳為用以形成下述之底漆皮膜者，即，以與熔融性全氟聚合物皮膜之下直接相接之方式設置之底漆皮膜。再者，熔融性全氟聚合物皮膜之下意指該熔融性全氟聚合物皮膜與被塗裝物（基材）之間。關於上述熔融性全氟聚合物皮膜，將於下文敍述。
將本發明之熔融性氟樹脂底漆塗佈於被塗裝物上，適當地進行乾燥或加熱，藉此可形成底漆皮膜。
作為上述被塗裝物，只要為可供熔融性全氟聚合物皮膜形成者，便無特別限定。
本發明之熔融性氟樹脂底漆較佳為直接塗佈於由金屬或非金屬無機材料所構成之基材上，或塗佈於由耐熱性樹脂所構成之層（以下亦稱為耐熱層）之上，更佳為直接塗佈於由金屬或非金屬無機材料所構成之基材上。
作為上述金屬，可例舉鐵、鋁、銅等金屬單質及其等之合金類等。作為上述合金類，可例舉不鏽鋼（SUS）等。作為上述非金屬無機材料，可例舉琺瑯、玻璃、陶瓷等。上述基材亦可於包含金屬或非金屬無機材料之同時包含其他材料。
作為上述基材，較佳為由金屬所構成者，更佳為由鋁或不鏽鋼所構成者。
本發明之熔融性氟樹脂底漆特別適用於金屬基材。作為上述金屬基材，具體而言，可例舉配管、管道管、導管等工業零件相關用途等。於其等之內表面塗佈熔融性氟樹脂底漆。於需要耐熱性、耐化學品性、阻燃性之用途中，廣泛應用熔融性全氟聚合物塗料作為面塗層，但要想確保上述金屬基材與熔融性全氟聚合物皮膜之接著性，就在保持耐熱性、耐化學品性、阻燃性之基礎上賦予接著性之方面而言，有利的是將本發明之熔融性氟樹脂底漆用於上述金屬基材。
針對上述被塗裝物，亦可視需要預先實施清洗、噴砂等表面處理。上述噴砂係吹送矽砂、氧化鋁粉等砂，由於使被塗裝物之表面粗糙化，故而會提高密合性，就該方面而言，較佳為進行上述噴砂。
作為對上述被塗裝物進行塗佈之方法，並無特別限定，可根據被塗裝物之形態等進行適當選擇，例如可例舉噴霧塗裝、浸漬塗裝、刷塗、靜電塗裝等先前公知之方法等。上述塗佈可按照乾燥膜厚成為5～100 μm之方式進行。亦可於上述塗佈時進行加熱，例如較佳為於60～120℃下進行塗佈。可於上述加熱之前在室溫進行乾燥，藉由乾燥可緩和上述加熱條件。
本發明亦係關於一種底漆皮膜，其由本發明之熔融性氟樹脂底漆所形成。
本發明之底漆皮膜與被塗裝物及熔融性全氟聚合物皮膜之密合性優異。
上述底漆被膜之膜厚適宜的是5～100 μm。更佳為20～80 μm。
於本發明之底漆皮膜中，烷基酚類之含量較佳為相對於上述底漆皮膜為0.10質量ppm以下，更佳為0.05質量ppm以下，進而較佳為未達0.05質量ppm。較佳為完全不含烷基酚類。
上述烷基酚類之含量係藉由液相層析法所測定之值。
於上述底漆皮膜之上塗佈熔融性全氟聚合物塗料，進行加熱焙燒，藉此可形成熔融性全氟聚合物皮膜。
本發明亦係一種積層體，其係於底漆皮膜之上設有包含熔融性全氟聚合物之皮膜者。
上述熔融性全氟聚合物塗料係以熔融性全氟聚合物為主成分者，可為視需要適當地含有添加劑等其他成分者，並無特別限定。
作為上述熔融性全氟聚合物，例如可例舉：四氟乙烯/六氟丙烯共聚物[FEP]、四氟乙烯/全氟(烷基乙烯基醚)共聚物[PFA]等。上述熔融性全氟聚合物係以上述全氟單體為單體成分者。熔融性全氟聚合物塗料係包含其等中之一種以上者。
作為上述熔融性全氟聚合物，必須為熔融性。若為熔融性，則可藉由下述焙燒進行熔融而成膜。
上述熔融性全氟聚合物之熔融性一般以MFR表示作為流動性之指標。MFR係以若為FEP則依據ASTM D2116、若為PFA則依據ASTM D3307，於既定之負載從直徑2 mm之噴嘴歷時10分鐘所擠出之重量表示者。MFR係於372℃進行測定。就藉由塗裝本發明之熔融性全氟聚合物塗料而獲得之塗膜之調平性、塗膜強度等方面而言，上述熔融性全氟聚合物之MFR較佳為0.1～100 g/10分鐘。更佳之下限為0.5 g/10分鐘，更佳之上限為50 g/10分鐘。
上述熔融性全氟聚合物塗料較佳為粉體塗料。作為上述粉體塗料之製法，並無特別限定，例如可例舉先前公知之方法等，可使用下述等方法：視需要將熔融性全氟聚合物及其他成分進行熔融混練後進行粉碎之方法；藉由上述FEP粒子之粉碎方法中所說明之方法進行粉碎並進行分級之方法。
但是，於經由對氟樹脂粒子之液體分散液進行噴霧乾燥之步驟而製造粉體塗料的方法中，用以使液體分散液穩定化之界面活性劑有時會殘存於粉體塗料中，甚至殘存於所塗佈之皮膜中。於此種情形時，會損害全氟聚合物皮膜之耐熱性或耐化學品性，因此欠佳。
上述粉體塗料可用作以下塗料，例如：藉由靜電塗裝法來形成一般膜厚為20～100 μm之薄塗皮膜之塗料、藉由靜電塗裝法來形成一般膜厚為100～1500 μm之厚塗皮膜之塗料、藉由旋轉襯裡法來形成一般膜厚為1000～5000 μm之厚塗皮膜之塗料。於藉由靜電塗裝法來獲得厚塗皮膜時，在多數情況會將下述步驟反覆進行2次以上：將粉體塗料塗佈於被塗裝物後，進行加熱焙燒而使其成膜。
藉由靜電塗裝法來形成薄塗皮膜之粉體塗料中所含之熔融性全氟聚合物較佳為平均粒徑為5～50 μm。若平均粒徑未達5 μm，則於塗佈時容易發生靜電排斥，存在難以獲得平滑皮膜之傾向，即便平均粒徑超過50 μm，亦存在難以獲得平滑皮膜之傾向。更佳之平均粒徑之範圍為10～40 μm。
藉由靜電塗裝法來形成厚塗皮膜之粉體塗料中所含之熔融性全氟聚合物較佳為平均粒徑為20～100 μm。若平均粒徑未達20 μm，則存在難以獲得厚塗皮膜之傾向，若平均粒徑超過100 μm，則存在塗佈效率降低之傾向。更佳之平均粒徑之範圍為30～90 μm。
藉由旋轉襯裡法來形成厚塗皮膜之粉體塗料中所含之熔融性全氟聚合物較佳為平均粒徑為150～500 μm。若平均粒徑未達150 μm，或平均粒徑超過500 μm，則存在氣泡容易殘留於皮膜中之傾向，存在難以獲得平滑皮膜之傾向。更佳之平均粒徑之範圍為200～450 μm。
上述粉體塗料之平均粒徑係藉由雷射繞射法所測得[商品名：Microtrac公司之MT-3300II]之體積基準中值粒徑。
本發明中所使用之粉體塗料可在藉由塗佈於被塗裝物後進行加熱焙燒而使其成膜等方式進行施工後，作為耐蝕襯裡等而用於各種用途。對於本發明中所使用之粉體塗料，藉由在本發明之範圍內如上所述般調整平均粒徑、熔體流動速率等，可將其製成適宜上述塗佈方法或適宜獲得焙燒後之膜厚之粉體塗料。
本發明亦係關於一種塗裝物品，其係於被塗裝物上設有積層體者，該積層體具有形成於上述被塗裝物上之本發明之底漆皮膜、及形成於上述底漆皮膜上之熔融性全氟聚合物皮膜。
於本發明之塗裝物品中，上述底漆皮膜與上述被塗裝物及上述全氟聚合物皮膜之密合性優異。
尤其是，本發明亦係一種塗裝物品，其係於金屬基材上設有上述積層體者。較佳為製成下述塗裝物品，其於作為金屬基材之配管、管道管、導管等之內表面設置有上述積層體。
關於上述被塗裝物、上述底漆皮膜、上述熔融性全氟聚合物皮膜，如上所述。
於本發明之塗裝物品中，較佳為上述被塗裝物與上述底漆皮膜直接相接。又，較佳為上述底漆皮膜與上述全氟聚合物皮膜直接相接。又，亦可於上述全氟聚合物皮膜上進而設置有層，但較佳為上述熔融性全氟聚合物皮膜為最外層。
[實施例]
以下，基於實施例對本發明進行具體說明。
於以下實施例中，在未特別提及之情形時，「份」「%」分別表示「質量份」「質量%」。
（實施例1）
將FEP粉末（MFR：20 g/10 min，平均粒徑：30 μm）33.0 g、作為耐熱性樹脂之聚醯胺醯亞胺（PAI，昭和電工材料公司製造）之粉碎物即平均粒徑1.5 μm之PAI粒子10.0 g、聚氧乙烯烷基醚系界面活性劑（日油公司製造）1.90 g、乙炔二醇系界面活性劑（日信化學公司製造）1.0 g及純水25.0 g放入至不鏽鋼容器中，使用螺旋漿攪拌機，以300 rpm充分攪拌20分鐘，繼而，一面攪拌一面添加N-甲基-2-吡咯啶酮（NMP）20.0 g而使其充分地分散，從而獲得FEP塗料用底漆。
（實施例2）
使FEP粉末成為36.1 g，使PAI粒子成為6.9 g，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例3）
使用聚醚碸（PES，住友化學公司製造）之粉碎物即平均粒徑5.0 μm之PES粒子來代替聚醯胺醯亞胺作為耐熱性樹脂，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例4）
使用聚醯亞胺（PI，三菱瓦斯化學公司製造）之粉碎物即平均粒徑8.0 μm之PI粒子來代替聚醯胺醯亞胺作為耐熱性樹脂，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例5）
使聚氧乙烯烷基醚系界面活性劑之添加量成為6.0 g，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例6）
僅使用上述聚氧乙烯烷基醚系界面活性劑作為界面活性劑，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例7）
使用3-甲氧基-2-丙醯胺來代替N-甲基-2-吡咯啶酮（NMP），除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（實施例8）
追加0.5 g胺系抗氧化劑（大內新興化學公司製造），除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（比較例1）
使用聚氧乙烯烷基苯醚系界面活性劑（Sigma-Aldrich Japan公司製造）來代替上述聚氧乙烯烷基醚系界面活性劑，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（比較例2）
使FEP粉末成為41.0 g，使PAI粒子成為2.0 g，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（比較例3）
使FEP粉末成為21.0 g，使PAI粒子成為22.0 g，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
（比較例4）
FEP粉末之平均粒徑為5 μm，除此以外，以與實施例1相同之方式獲得FEP塗料用底漆。
＜評估方法＞
（熔融性氟樹脂底漆之密合試驗）
將成為80目氧化鋁之TOSA EMERY（宇治電化學工業公司製造）以0.5 MPa之壓力進行噴砂至經除脂之鐵基材（100 mm×200 mm×5 mm），利用空氣去除噴砂粉後，將藉由上述方式所獲得之熔融性氟樹脂底漆以乾燥膜厚成為15～20 μm之方式藉由噴霧進行塗裝，於80℃乾燥30分鐘，繼而，靜電塗裝FEP粉體塗料（MFR：20 g/10 min，平均粒徑：40 μm），並於320℃進行30分鐘焙燒，從而獲得具有厚度約800 μm之塗裝膜之塗裝物。用刀對該塗膜切出10 mm寬度之條紋，使用島津公司製造之Autograph DSC-500，以50 mm/分鐘之速度進行90度之剝離試驗。又，準備將上述塗裝物浸漬於98℃之沸水中24小時後者，以相同之條件進行剝離試驗。將結果示於表1。
（熔融性氟樹脂底漆之沈澱性評估）
將80 ml之藉由上述方式所獲得之熔融性氟樹脂底漆放入至100 ml燒杯中，藉由目視並使用樹脂棒來評估剛攪拌後、24小時後及1週後之粒子之沈澱狀態。將結果示於表1。
無沈澱：目視時無沈積，於利用樹脂棒進行攪拌時底面無粒子成分之沈積。
少量沈澱：目視時無沈積，但於利用樹脂棒進行攪拌時底面有粒子成分之沈積。
有沈澱：目視時可見沈積，於利用樹脂棒進行攪拌時底面亦有粒子成分之沈積。
（熔融性氟樹脂底漆之再分散性評估）
將80 ml之藉由上述方式所獲得之熔融性氟樹脂底漆放入至100 ml燒杯中並靜置24小時及1週，使用樹脂棒對靜置後之熔融性氟樹脂底漆進行攪拌，進行再分散評估。將結果示於表1。再者，於未進行評估之情形時，記載為「-」。
良好：沈積之粒子容易均勻地分散。
不良：沈積之粒子不容易均勻地分散。
[表1]
[產業上之可利用性]
| 接著力（kg/cm）90°剝離 | 沈澱性 | 再分散性 | |||||
| 初期 | 98℃熱水×24小時後 | 剛攪拌後 | 24小時後 | 1週後 | 24小時後 | 1週後 | |
| 實施例1 | 14 | 12 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 實施例2 | 14 | 11 | 無沈澱 | 少量沈澱 | 有沈澱 | 良好 | 良好 |
| 實施例3 | 13 | 10 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 實施例4 | 14 | 11 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 實施例5 | 14 | 10 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 實施例6 | 14 | 10 | 無沈澱 | 少量沈澱 | 有沈澱 | 良好 | 良好 |
| 實施例7 | 14 | 11 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 實施例8 | 15 | 13 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 比較例1 | 14 | 9 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 比較例2 | 13 | 11 | 少量沈澱 | 有沈澱 | - | 不良 | 不良 |
| 比較例3 | 9 | 3 | 無沈澱 | 無沈澱 | 少量沈澱 | - | 良好 |
| 比較例4 | 6 | 2 | 無沈澱 | 無沈澱 | 無沈澱 | - | - |
本發明之熔融性氟樹脂底漆因具有上述構成，而於水系中分散穩定性優異，可於金屬基材等被塗裝物與由熔融性全氟聚合物塗料所構成之面塗層之間獲得較高之接著強度，尤其適宜作為面向金屬基材之熔融性氟樹脂底漆。
無
無
Claims (8)
- 一種熔融性氟樹脂底漆，其特徵在於：包含四氟乙烯/六氟丙烯共聚物(FEP)粒子、耐熱性樹脂、非離子性界面活性劑及水，且 上述FEP之平均粒徑為10～60 μm，上述耐熱性樹脂為選自由聚醯胺醯亞胺樹脂、聚醚碸及聚醯亞胺樹脂所組成之群中至少一種， 上述FEP粒子與上述耐熱性樹脂之固形物成分質量比為50：50～95：5， 非離子性界面活性劑為聚氧乙烯烷基醚系界面活性劑， 上述熔融性氟樹脂底漆包含以質量基準計為10～60%之水。
- 如請求項1之熔融性氟樹脂底漆，其進而含有選自由乙炔二醇系界面活性劑、醇、酮、酯及芳香族烴所組成之群中至少一種之分散介質。
- 如請求項1或2之熔融性氟樹脂底漆，其中，FEP粒子之熔體流動速率為0.1～50 g/10分鐘。
- 如請求項1至3中任一項之熔融性氟樹脂底漆，其進而含有相對於FEP粒子之固形物成分以質量基準計為0.001～5%之熱穩定劑。
- 一種底漆皮膜，其由請求項1至4中任一項之熔融性氟樹脂底漆所形成。
- 一種積層體，其係於請求項5之底漆皮膜之上設有包含熔融性全氟聚合物之皮膜者。
- 一種塗裝物品，其係於金屬基材上設有請求項6之積層體者。
- 一種塗裝物品，其係於金屬基材之內表面設有請求項6之積層體者，上述金屬基材為配管、管道管（pipe）或導管（duct）。
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