TW202031694A - 全氟彈性體組成物、交聯全氟彈性體及成形品 - Google Patents
全氟彈性體組成物、交聯全氟彈性體及成形品 Download PDFInfo
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Abstract
一種組成物,其含有全氟彈性體、相對於前述全氟彈性體100重量份而言為55~75重量份之碳黑,與下述式(1)表示之交聯劑(式(1)中,A為單鍵、-O-、伸烷基,或氟化伸烷基。R1
、R2
、R3
係分別獨立地為氫原子、氟原子、烷基,或氟化烷基。惟R1
、R2
、R3
之至少1個為氟原子或氟化烷基)。
Description
本發明係關於含有全氟彈性體之組成物、交聯全氟彈性體,及由交聯全氟彈性體得到的成形體。
於各種產業中,水蒸氣係於發電等各種用途中被使用。橡膠O形環等之密封材,係用於此等水蒸氣流過的配管或裝置,發揮防止水蒸氣流出至外部的角色。
近年來,於發電廠中,以提高發電效率為目標,水蒸氣的溫度有較以往上昇的傾向,伴隨於此,對密封材亦變得要求高溫水蒸氣性。
特別是地熱發電或高溫岩體發電等之發電廠、油田等在地底深處所用的密封材,當密封對象氣體之壓力急速解放時會曝露於急減壓環境。此時,於高壓氣體環境下溶存於密封材之氣體在減壓時會一口氣膨脹,於密封材造成龜裂。
作為適於耐熱性、耐蒸氣性、耐急減壓性之密封材,係使用交聯全氟彈性體製之密封材。作為交聯全氟彈性體之交聯劑,已知有各種交聯劑,例如一般廣為人知有異三聚氰酸三烯丙酯(TAIC)(參照專利文獻1等)。
[先前技術文獻]
[專利文獻]
[專利文獻1]國際公開第2010/099057號
但是,以TAIC為代表之一般的交聯結構中,使用極限為200℃強,不耐於其以上之溫度區域的高溫蒸氣環境下之使用,因此係有前述地熱發電或高溫岩體發電等之發電廠、油田等於地底深處在200℃以上之高溫高壓蒸氣環境下的使用困難之問題。
本發明係有鑑於上述課題而為者,其目的為提供耐熱性、耐蒸氣性及耐急減壓性優良的交聯全氟彈性體及用以得到其之組成物。
依照本發明,係提供以下之組成物、交聯全氟彈性體及成形體。
1. 一種組成物,其含有全氟彈性體、
相對於前述全氟彈性體100重量份而言為55~75重量份之碳黑,與
下述式(1)表示之交聯劑;
(式(1)中,A為單鍵、-O-、伸烷基,或氟化伸烷基。R1
、R2
、R3
係分別獨立地為氫原子、氟原子、烷基,或氟化烷基。惟R1
、R2
、R3
之至少1個為氟原子或氟化烷基)。
2. A為單鍵、伸烷基,或氟化伸烷基1之組成物。
3. 一種交聯全氟彈性體,其係使如1或2之組成物交聯而得到。
4. 一種成形品,其包含如3之交聯全氟彈性體。
5. 如4之成形品,其係O形環。
依照本發明,可提供耐熱性、耐蒸氣性及耐急減壓性優良的交聯全氟彈性體及用以得到其之組成物。
以下說明本發明之一實施形態。再者,本發明不限於本實施形態。
本發明之組成物,含有全氟彈性體、交聯劑與碳黑。
上述式(1)中,A為單鍵、-O-、伸烷基,或氟化伸烷基。較佳為單鍵、伸烷基,或氟化伸烷基;更佳為氟化伸烷基。
伸烷基或氟化伸烷基之伸烷基,可為直鏈亦可為分支,碳數較佳為1~15(更佳為碳數2~8、又更佳為碳數3~6)。
氟化伸烷基,伸烷基可一部分或全部被氟化。較佳為全氟伸烷基。
前述伸烷基可例示亞甲基、伸乙基、伸丙基、伸丁基、伸戊基、伸己基、伸庚基等。
上述式(1)中,R1
、R2
、R3
係分別獨立地為氫原子、氟原子、烷基,或氟化烷基。惟R1
、R2
、R3
之至少1個為氟原子或氟化烷基。
烷基或氟化烷基之烷基,可為直鏈亦可為分支,碳數較佳為1~15(更佳為碳數1~6、又更佳為碳數1~4)。
氟化烷基,烷基可一部分或全部被氟化。較佳為全氟烷基。
前述烷基可例示甲基、乙基、丙基等。
R1
、R2
、R3
較佳分別獨立地為氫原子,或氟原子。
上述式(1)中,A與-CR1
=CR2
R3
,可為鄰位、間位或對位的任意者,較佳為對位;更佳為A與2個
-CR1
=CR2
R3
均為對位。
交聯劑之添加量,相對於全氟彈性體100重量份而言,較佳為2~10重量份、更佳為5~8重量份。添加量越多,越有耐蒸氣性、耐熱性改善的傾向。惟過多時有變硬之虞。
關於全氟彈性體,例如可例示來自以下單體之重複單位。可包含來自1或2個以上之單體的重複單位。
CF2
=CF2
(四氟乙烯)、
CF2
=CFCF3
(六氟丙烯)、
本發明所用之全氟彈性體,較佳為包含碘及/或溴、更佳為包含碘,作為交聯(硬化)時之自由基的攻擊部位。可藉由過氧化物而硬化之全氟彈性體,例如記載於日本特開2006-9010等。
全氟彈性體,一般而言,就全部聚合物重量而言,係含有0.001重量%~5重量%、較佳為0.01重量%~ 2.5重量%的碘。碘原子可沿著鏈及/或於末端部位存在。
全氟彈性體,較佳為由在末端部位具有乙烯型之1個不飽和的全氟化烯烴等之共聚物來製造。
共聚單體可例示如以下。
・ CF2
=CFOR2f
全氟烷基乙烯基醚類(PAVE)
(式中,R2f
為碳數1~6之全氟烷基、例如三氟甲基或五氟丙基)。
・ CF2
=CFOXo
全氟氧烷基乙烯基醚類
(式中,Xo
為包含1個以上之醚基的碳數1~12之全氟氧烷基、例如全氟-2-丙氧基丙基)。
・ CFX2
=CX2
OCF2
OR’’f
(I-B)
(式中,R’’f
為碳數2~6之直鏈或分支全氟烷基、碳數5、6之環狀全氟烷基,或包含1~3個氧原子的碳數2~6之直鏈或分支全氟氧烷基,X2
為F)。
式(I-B)之全氟乙烯基醚類,較佳以下式表示。
CFX2
=CX2
OCF2
OCF2
CF2
Y (II-B)
(式中,Y為F或OCF3
,X2
係如上述定義)。
較佳的單體組成物,可例示如以下。
四氟乙烯(TFE) 50~85莫耳%、PAVE 15~50莫耳%;
TFE 50~85莫耳%、MOVE 15~50莫耳%。
全氟彈性體,亦可包含來自偏二氟乙烯(vinylidene fluoride)之單元、可含碘及/或溴之碳數3~8之氟烯烴類。
本發明中,含有碳黑作為填充劑。碳黑之平均粒子徑較佳為100nm以上,更佳為250nm以上。相對於全氟彈性體100重量份而言,組成物含有碳黑55~75重量份、較佳為58~72重量份、更佳為60~70重量份。藉由使用上述式(1)表示之交聯劑,且含有特定量之碳黑,耐急減壓性變佳。
本發明之組成物可含有交聯起始劑。交聯起始劑可使用通常所使用者。例如可例示過氧化物、偶氮化合物等。
相對於全氟彈性體100g而言,交聯起始劑較佳為添加0.3~35mmol、更佳為添加1~15mmol、又更佳為添加1.5~10mmol。添加量越多,越有耐蒸氣性、耐熱性改善的傾向。惟過多時有焦化或發泡之虞。
本發明之組成物可含有可塑劑。可塑劑可列舉全氟聚醚等之氟系可塑劑。相對於全氟彈性體100重量份而言,可塑劑較佳為添加1~9重量份、更佳為添加1~5重量份。含有可塑劑時,製造性變佳。
上述組成物亦可含有交聯輔助劑。
交聯輔助劑可列舉氧化鋅、活性氧化鋁、氧化鎂、四級銨鹽、四級鏻鹽、胺等。藉由含有交聯輔助劑,可提高交聯效率、耐熱性。相對於全氟彈性體100重量份而言,交聯輔助劑通常添加0.1~10重量份。
上述全氟彈性體組成物中,可摻合碳黑以外之填充劑。只要不損及本發明之效果,則填充劑可使用作為彈性體之填充劑而一般所知者。例如可列舉二氧化矽、硫酸鋇、二氧化鈦、半晶質氟聚合物、全氟聚合物等。
又,亦可依需要,適量摻合增黏劑、顏料、偶合劑、抗氧化劑、安定劑等。
本發明之組成物,可實質上由全氟彈性體、交聯劑及碳黑所構成,或亦可僅由此等所構成。實質上所構成,係指此等成分,佔組成物之85重量%以上,90重量%以上,95重量%以上,或98重量%以上。
使本發明之組成物交聯,而得到交聯全氟彈性體。
一階段加熱的情況時,交聯條件較佳為於100~250℃加熱10分鐘~5小時。
二階段加熱的情況時,通常,作為一次交聯,係於模具中置入原料,一邊加壓加工一邊交聯。1次交聯例如係於150~200℃加熱5~60分鐘。之後,由模具取出,進行2次交聯。2次交聯例如係於150~350℃加熱1~100小時。交聯可使用電爐等來進行。藉由以2次交聯賦予熱歷程,可防止使用中之變形等。
交聯可於惰性氣體環境或大氣中進行。
惰性氣體可使用氮、氦、氬等,較佳為氮。於惰性氣體環境下,氧濃度較佳為10ppm以下、更佳為5ppm以下。
以上述製法所得之交聯全氟彈性體,可使用作為密封材,可作為墊片或密封環等之成形體來使用。
[實施例]
實施例1
混合全氟彈性體(PFE40Z、3M公司(股))100重量份、式(1)之化合物(R1
、R2
、R3
為氟,A為-(CF2
)6
-)(交聯劑)7重量份、碳黑(MT)(Thermax N990、cancarb(股))65重量份、氟系可塑劑(Krytox VPF16256、Chemours(股))3重量份、作為交聯起始劑之有機化氧化物(Perhexa 25B、日本油脂(股))2重量份,調製組成物。再者,交聯劑係參照WO2016/017187合成。
使上述組成物交聯,製造包含交聯氟彈性體之尺寸不同的2種O形環(外徑約25.90mm、內徑約15.24mm,及外徑約32.06mm、內徑約25.00mm)(成形體)。交聯條件,1次交聯係170℃、40分鐘、2次交聯係於氮環境下310℃、4小時。
對於所得之成形體進行以下評估。結果示於表1。
(1)耐急減壓(耐RGD)性
試驗係根據NORSOK規格實施。將O形環,以壓縮率成為15%(常溫)、相對於溝容積而言O形環之填充率成為80%的方式設置於內部具有容納O形環之溝的治具上,將該治具封入於壓力容器。於100℃、300℃將壓力容器內之壓力上昇至15MPa,首次係保持68小時,之後以減壓速度2MPa/min急減壓至大氣壓,於該狀態下保持1小時。重複進行該昇壓與減壓的循環,第2次以後,使將壓力容器內之壓力上昇至15MPa後之保持時間交互變更為6小時、12小時,重複8次。試驗後,將O形環於4個部位切斷,觀察截面。於100℃及300℃之試驗,係分別使用2個O形環。
測定存在於該切斷面之龜裂個數、長度,以表2所示基準,評估耐急減壓性。表2之線徑,係試驗前之O形環的線徑(初期線徑)。分數0~3為可,4、5為不可。
(2)耐熱性
將所得之O形環,用平板2枚,使用間隔件以壓縮25%的方式以螺栓鎖入,準備緊固體,將該緊固體以吉爾老化烘箱(geer oven)在特定條件(大氣環境中200、250、300℃×72小時)進行熱曝露。之後,由吉爾老化烘箱取出,趁緊固體尚熱的時候將O形環釋放,放冷至常溫後,測定線徑,由下式算出壓縮永久變形(單位:%)。以該壓縮永久變形作為耐熱性。
壓縮永久變形=(初期線徑-熱曝露後線徑)/(初期線徑-間隔件厚度)×100
(3)耐蒸氣性
使用具有使O形環成為壓縮率25%之溝與使水進入其內側之空間的壓力容器,將O形環置入溝中,於空間中置入水,以螺栓鎖緊。將容器於吉爾老化烘箱中以特定條件(250℃、300℃×72小時)保持,使水成為飽和蒸氣。之後,由吉爾老化烘箱中取出,放冷至常溫後,將O形環釋放。
接著,將經上述處理之O形環,用平板2枚,以成為與溝深度相同之壓縮率的方式使用間隔件壓縮,以螺栓鎖入,將緊固體以特定條件(250、300℃×1小時)熱曝露後,由吉爾老化烘箱中取出,趁緊固體尚熱的時候將O形環釋放,放冷至常溫後,測定線徑,由下式算出壓縮永久變形(單位:%)。以該試驗結果作為耐蒸氣性。壓縮永久變形越小,耐蒸氣性越高。
壓縮永久變形=(初期線徑-熱曝露後線徑)/(初期線徑-溝深度)×100
比較例1
除了將碳黑(MT)之摻合量變更為50重量份以外,係與實施例1同樣地製作2種O形環。結果示於表1。
比較例2
除了將交聯劑變更為異三聚氰酸三烯丙酯(TAIC)以外,係與實施例1同樣地製作2種O形環。結果示於表1。
比較例3
除了將碳黑(MT)之摻合量變更為80重量份以外,係與實施例1同樣地嘗試製作O形環,但成形性有問題。
耐急減壓性之試驗,係於100℃及300℃之各溫度下,使用2個O形環來實施。就耐急減壓性而言,比較例1及2均較實施例1為差。又,就比較例2而言,300℃72小時之耐蒸氣性的試驗結果亦較實施例1為差。
本發明之交聯氟彈性體,可利用作為地熱發電、高溫岩體發電等之發電廠;油田、壓縮機、高壓閥所使用之O形環等之密封材的材料。
上述係詳細說明了幾個本發明之實施形態及/或實施例,但所屬技術領域中具有通常知識者,容易在實質上不脫離本發明之新穎的教示及效果下,對此等例示之實施形態及/或實施例施加許多變更。因此,此等之許多變更係包含於本發明之範圍中。
本說明書記載之文獻及本案依巴黎條約作為優先權基礎案的內容全部援用於此。
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