TWI386444B - 摻入填料之氟樹脂薄片之製造方法及摻入填料之氟樹脂薄片 - Google Patents
摻入填料之氟樹脂薄片之製造方法及摻入填料之氟樹脂薄片 Download PDFInfo
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- TWI386444B TWI386444B TW096110057A TW96110057A TWI386444B TW I386444 B TWI386444 B TW I386444B TW 096110057 A TW096110057 A TW 096110057A TW 96110057 A TW96110057 A TW 96110057A TW I386444 B TWI386444 B TW I386444B
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- Prior art keywords
- fluororesin
- filler
- sheet
- processing aid
- fluororesin sheet
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Description
本發明係有關摻入填料之氟樹脂薄片之製造方法及摻入填料之氟樹脂薄片,更詳而言之,係有關作為密封材等使用的摻入填料之氟樹脂薄片的製造方法及摻入填料之氟樹脂薄片。
摻入填料之氟樹脂薄片,係將填料填充於氟樹脂中而加工成薄片狀者,除了氟樹脂所具有之耐藥品性、耐熱性、非黏著性、低摩擦性以外,藉由附加填料所具有之固有功能、特性,或是改善氟樹脂之缺點的耐摩擦性或抗潛變性,而很多使用於密封材等。
以密封材而言,係將金屬、石墨、無機填料等填充於氟樹脂中而使導熱率、耐摩擦性、潛變特性等提升者,為使用於薄片狀襯墊(gasket)或格蘭迫緊(gland packing)之編織等。
在美國專利第3315020號說明書(專利文獻1)中,揭示將PTEE與填料與加工助劑的混合物予以擠壓成型後,使其經過1對之壓延輥輪一次或複數次以進行壓延(滾軋延展,本文中依日文稱為壓延),而得到長尺寸之薄片的技術。然而,利用此技術而製作由摻入填料之氟樹脂薄片所構成的薄片狀襯墊時,若提高填料之填充率時,雖然應力鬆弛特性會有優良之傾向,但氣密性低,無法得到可滿足之密封材者。
另一方面,在日本特開2004-323717號公報(專利文獻2)中,揭示一種摻入填料之氟樹脂薄片,其係將含有氟樹脂、膨潤性礦物、填料及加工助劑的組成物予以擠壓成形後,使其通過壓延輥輪而延伸成薄片狀。此摻入填料之氟樹脂薄片,即使是在氟樹脂之填充率低、且填料之填充率高之情形,其應力鬆弛率、抗張強度等也都優異。
專利文獻1:美國專利第3315020號說明書專利文獻2:日本特開2004-323717號公報
然而,在專利文獻2所記載的摻入填料之氟樹脂薄片中,由於作為填補形成硬且粒子狀之無機系填料相互間的空隙之黏合劑(binder)的氟樹脂會有不足的傾向,故可知從密封性能之點而言,尚有更進一步改進的餘地。
本發明係有鑒於上述問題而研創者,其目的係提供一種摻入填料之氟樹脂薄片及其製造方法,其中,即使是在氟樹脂之填充率低、且填料之填充率高時,亦可兼顧高之應力鬆弛性與高之氣密性(密封性能)兩方面。
本發明人等經精心研究之結果,發現在製造摻入填料之氟樹脂薄片時之壓延步驟中,藉由緩緩地使加工助劑揮發,而可製造出使高之應力鬆弛性與高之氣密性兩者同時成立的摻入填料之氟樹脂薄片,因而完成本發明。
本發明摻入填料之氟樹脂薄片之製造方法的特徵為包括:將含有氟樹脂、填料及加工助劑的薄片形成用樹脂組成物,以輥輪溫度40至80℃進行壓延的步驟;該加工助劑係含有分餾溫度為120℃以下之石油系烴溶劑在30質量%以上(惟,將加工助劑重量當作為100質量%)。
上述組成物中的上述氟樹脂與上述填料的質量比,係以氟樹脂:填料=1:0.1至2為較佳。
在上述組成物中,相對於氟樹脂與填料之合計100重量份,上述加工助劑以含有5至50重量份為較佳。
本發明之製造方法,係以包含藉由上述壓延步驟而調製之壓延薄片予以更進一步壓延的步驟為較佳。
本發明之摻入填料之氟樹脂薄片,其特徵係藉由上述之本發明之摻入填料之氟樹脂薄片之製造方法而製造。
若依據本發明之製造方法,即使氟樹脂之填充率低、且填料之填充率高,亦可製造出兼具高之應力鬆弛特性與高之氣密特性兩方面的摻入填料之氟樹脂薄片。
本發明之摻入填料之氟樹脂薄片之製造方法,係包括將含有氟樹脂、填料及加工助劑的薄片形成用樹脂組成物以輥輪溫度40至80℃進行壓延的步驟;而該加工助劑係含有分餾溫度為120℃以下之石油系烴溶劑在30質量%以上(惟,將加工助劑重量作為100質量%)。
<氟樹脂>以氟樹脂而言,除了四氟乙烯樹脂(Polytetrafluoro ethylene,即PTFE)以外,可使用如改質PTFE、偏二氟乙烯樹脂(Polyvinylidene fluoride,即PVDF)、四氟乙烯-乙烯共聚樹脂(Ehtylene tetrafluoro ethylene copolymer,即ETFE)、三氟氯乙烯樹脂(Polychlorotrifluoro ethylene,即PCTFE)、四氟乙烯-六氟丙烯乙烯共聚樹脂(Fluorinated ethylene propylene copolymer,即FEP)及四氟乙烯-全氟烷基共聚樹脂(Tetrafluoro ethylene-perfluoroalkyl copolymer,即PFA)等以往公知之氟樹脂中之任一者。其中,尤以使用藉由乳化聚合所得之PTFE,在進行擠壓成形、壓延等之時的加工性方面較佳。
以氟樹脂而言,可直接使用粉末狀物,亦可使用將氟樹脂微粒子分散於水中而成之分散液。當使用分散液時,於氟樹脂分散液中僅添加適量之水、填料、加工助劑等並加以攪拌,即可獲得摻入填料之氟樹脂薄片形成用之組成物,藉由使用該組成物,而可更有效地得到摻入填料之氟樹脂薄片。
<填料>以填料而言,因應目的需求而使用:石墨、碳黑、膨脹石墨、活性碳、碳奈米管等碳系填料;滑石、雲母、黏土、碳酸鈣、氧化鎂等無機填料;或PPS(Polyphenylene sulfide,聚苯硫)等樹脂之粉體。此外,亦可將由碳纖維、芳香族聚醯胺纖維(aramid fiber)、岩綿(rock wool)等所構成之纖維材長10mm以下之纖維材作為填料使用。
若依據本發明,即使是在氟樹脂之填充率低、且填料之填充率高之情形,亦可製造出兼顧高之應力鬆弛性與高之氣密性兩者同時成立的摻入填料之氟樹脂薄片,上述氟樹脂與上述填料的質量比為1:0.1至2,較佳為1:1至1.8。
<加工助劑>在上述氟樹脂薄片形成用組成物中,含有加工助劑。本發明所用之加工助劑,係含有分餾溫度為120℃以下(較佳為110℃以下)之石油系烴溶劑為30質量%以上,較佳為50質量%以上(惟,將加工助劑重量作為100質量%),尤以該加工助劑在本質上,僅由分餾溫度為120℃以下之石油系烴溶劑所構成者為特佳。分餾溫度之下限值雖無特別限制,但若分餾溫度過低時,由於在壓延步驟中,加工助劑之揮發變得過度快速,故會有變得難以使加工助劑緩緩地揮發、去除的情形,所以,分餾溫度亦可為80℃左右。
分餾溫度為120℃以下之石油系烴溶劑,以代表例而言可列舉如石蠟(paraffin)系溶劑,以市售品而言,可列舉例如Isopar C(烴系有機溶劑、分餾溫度:97至104℃、Exxon Mobil有限公司製)等。
在以往之摻入填料之氟樹脂薄片之製造方法中,以加工助劑而言,一般係使用分餾溫度高(例如180至250℃)之石油系烴溶劑。此等加工助劑,雖然在壓延作業中溶劑不會揮發,可以安定地進行壓延作業,而廣泛被使用,但在下述之壓延步驟中,即使提升輥輪溫度,亦難以揮發。
除了分餾溫度為120℃以下之石油系烴溶劑之外,可包含於加工助劑中的成分,可列舉如分餾溫度超過120℃之石油系烴溶劑等。分餾溫度超過120℃之石油系烴溶劑,以市售品而言可列舉例如Isopar G(烴系有機溶劑、分餾溫度:158至175℃、Exxon Mobil有限公司製)等。
在薄片形成用樹脂組成物中,相對於氟樹脂與填料之合計100重量份,此加工助劑係含有5至50重量份,較佳為10至30重量份為較理想。加工助劑若以此等份量含有時,則在下述之壓延步驟之初期階段,即可使氟樹脂充分膨潤。
薄片形成用樹脂組成物,其本質上,係僅由以上述氟樹脂、填料、加工助劑所構成。
若要調製含有此等成分的氟樹脂薄片形成用樹脂組成物,係將上述各成分依任意順序以一次或以少量分為複數次添加至容器內,進行攪拌.混合即可。
一般之摻入填料之氟樹脂薄片之製造方法,係包含下列順序步驟:攪拌步驟、預成形步驟、壓延步驟、乾燥步驟、煅燒步驟。
<攪拌步驟>在攪拌步驟中,如上述地,將氟樹脂、填料、加工助劑以任意順序攪拌、混合。當攪拌效率差時,可多添加加工助劑,而在攪拌完畢後,可將多餘之加工助劑藉由過濾而去除。
<預成形步驟>在預成形步驟中,係將上述氟樹脂薄片形成用樹脂組成物予以擠壓成形,而製造預成形物(Preform)(擠壓成形物)。
擠壓成形物(預成形物)之形狀並無特別限定,但考慮到其後之薄片形成效率、薄片性狀之均質性等之時,以桿狀或螺帶狀較為理想。
在本發明之製造方法中,在下述壓延步驟中由於使加工助劑緩緩地揮發,故混合步驟及預成形步驟,係以加工助劑不會揮發之方式,溫度以比在壓延步驟中之輥輪溫度更低的溫度下進行為較佳。
<壓延步驟>在接續於預成形步驟的壓延步驟中,係使預成形物通過以二軸輥輪為代表的壓延輥輪之間,予以壓延、成形為薄片狀。在以往之技術中,壓延步驟係在非加熱下進行,具體而言,係於室溫附近之10至30℃左右之溫度下進行,且由於一般係使用分餾溫度為高(例如180至250℃)之石油系烴溶劑作為加工助劑,故在此壓延步驟中,加工助劑幾乎不會揮發。
此加工助劑,係為了使氟樹脂膨潤、容易纖維化而使用。藉由在攪拌步驟、預成形步驟、壓延步驟中,將壓縮力、剪斷力附加於薄片形成用樹脂組成物,而使一部分之氟樹脂進行纖維化而在氟樹脂薄片,藉由基材之複雜化而賦予薄片強度、應力鬆弛特性。然而,若氟樹脂在經壓延之氟樹脂薄片之內部中膨潤時,則由於此薄片為柔軟且易變形,故推測受到二軸輥輪等之壓縮,會優先引起往平面方向之變形,而難以造成薄片內部之緻密化。同時,所謂薄片內部之緻密化,係指因溶劑揮發所產生的組成物內部空孔會藉由壓延而被填補。
在本發明之製造方法中,此壓延步驟係以輥輪溫度40至80℃而進行,而且,由於使用含有多量之分餾溫度低(120℃以下)之石油系烴溶劑的加工助劑,故在實施藉二軸輥輪之壓延的期間,薄片形成用樹脂組成物中之(預成形物中之)加工助劑會緩緩地揮發、而被去除。所以,在壓延步驟之初期階段中,由於加工助劑存在量多,故可使氟樹脂膨潤並纖維化;且在壓延步驟之後期階段中,由於加工助劑之殘存量少,基於加工助劑之揮發在薄片內部形成之新空孔就少,故推測可使薄片優先往平面方向變形並可進行薄片內部之緻密化。
此外,由於是在較高之溫度下進行壓延,故可稍微降低氟樹脂之硬度,使氟樹脂薄片會變得更容易緻密化。
另一方面,若使壓延步驟在低於40℃之溫度下進行,則會有使加工助劑變得難以揮發之傾向。又,若在超過80℃之溫度下進行壓延,則由於加工助劑會過度地揮發,在壓延步驟初期之時間點的殘存加工助劑會變少,故無法使氟樹脂充分膨潤、纖維化,所得之摻入填料之氟樹脂薄片的強度有變差之傾向。又,組成物中之加工助劑因急速地氣化而產生膨脹現象,摻入填料之氟樹脂薄片的氣密性亦有降低的傾向。
另外,在本發明之製造方法中,較佳為含有將藉由上述壓延步驟所調製之壓延薄片予以更進一步壓延的步驟,亦即重覆複數次壓延步驟。藉由重覆進行壓延,可使氟樹脂薄片內部更為緻密化。又,當重覆進行壓延步驟時,每重覆壓延一次,輥輪間隔就會變狹窄些。
當藉由二軸輥輪將上述預形成物予以壓延而形成薄片時,例如只要設定輥輪間距離為0.5至20mm,將輥輪表面移動速度(薄片擠出速度)設定為5至50mm/秒,而壓延預成型物即可。
<乾燥步驟>在乾燥步驟中,藉由將上述經壓延之薄片放置於常溫中,或是在氟樹脂之沸點以下之溫度加熱,以去除加工助劑。
<煅燒步驟>在煅燒步驟中,係將乾燥後之薄片在氟樹脂熔點以上之溫度加熱,使其燒結。以加熱溫度而言,若考慮到有必要將薄片整體均勻地煅燒、在過度高溫下會產生氟系有害氣體時,則雖然隨著氟樹脂之種類不同而多少有所差異,但一般是以340至370℃為適當。
藉由如此之本發明的製造方法,而製造摻入填料之氟樹脂薄片。此摻入填料之氟樹脂薄片,其應力鬆弛性與氣密性皆高,依據JIS R3453之抗張強度為8Mpa以上,且對於由該薄片所作成之ψ 48mm×ψ 67mm×厚度1.5mm襯墊(gasket)試驗片以面壓19.6Mpa(200kgf/cm2
G)、氮氣內壓0.98Mpa(1.0kgf/cm2
G)進行氣密試驗時的洩漏量為9×0-5
Pa.m3
/s以下;而以上述抗張強度為10Mpa以上,且洩漏量為7×10-5
Pa.m3
/s以下較佳。
以下,藉由實施例更詳細說明本發明,但本發明不受此等實施例所限定。
<試驗方法>由厚度1.5mm之薄片製作試驗片,如下述方式測定氣密性及抗張強度。
洩漏量(氣密性)
將已打孔(punch)為ψ 48mm×ψ 67mm尺寸之襯墊試驗片,裝設於ψ 100mm×高度50mm、表面粗糙度Rmax=12 μm的鋼凸緣(steel flange)之間,藉由壓縮試驗機以面壓成為19.6Mpa(200kgf/cm2
G)之方式負荷荷重。從設有凸緣的壓力導入用之貫通孔,將氮氣內壓0.98Mpa(1.0kgf/cm2
G)往襯墊內徑側予以負荷後,封住壓力導入配管,使其保持1小時。將保持前後之壓力變化以壓力感測器讀取,從壓力之下降求出洩漏量。
抗張強度
依據JIS R3453,製作試驗片並測定抗張強度。
將PTFE細粉末(CD-1,旭硝子股份公司製)400g、NK-300(微粉末黏土,昭和KDE股份公司製)600g、以及Isopar C(烴系有機溶劑、分餾溫度:97至104℃、Exxon Mobil有限公司製)250g以揉合機(kneader)混合5分鐘後,藉由放置於室溫(25℃)中16小時而使其熟成,調製薄片形成用組成物。
將此組成物於室溫(25℃)中以模口300mm×20mm之擠出機進行擠壓,製作預形成物。
將此預形成物,以輥輪徑700mm、輥輪間隔20mm、輥輪速度6m/分鐘、輥輪溫度40℃之條件下,藉由二軸輥輪來進行壓延。在剛進行完畢此壓延步驟後,將所得之薄片以輥輪間隔10mm再度進行壓延。更進一步,在剛進行完畢此壓延步驟後,將所得之薄片以輥輪間隔5mm再度進行壓延。最後,在剛進行完畢此壓延步驟後,將所得之薄片以輥輪間隔1.5mm再度進行壓延,而得到厚度1.5mm之薄片。
將此薄片於室溫(25℃)中放置24小時後並去除溶劑後,於電爐內以350℃煅燒3小時,得到薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為4.0×10-5
Pa.m3
/s,抗張強度為11MPa。
除了使用Isopar C 125g及Isopar G(烴系有機溶劑、分餾溫度:158至175℃、Exxon Mobil有限公司製)125g替代Isopar C 250g以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為6.0×10-5
Pa.m3
/s,抗張強度為10MPa。
除了將輥輪溫度從40℃變更為80℃以外,其餘皆依照與實施例2相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為4.0×10-5
Pa.m3
/s,抗張強度為11MPa。
除了使用Isopar G 250g替代Isopar C 250g,並將輥輪溫度從40℃變更為80℃以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為1.0×10-4
Pa.m3
/s,抗張強度為11MPa。
除了使用Isopar G 250g替代Isopar C 250g以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為2.0×10-4
Pa.m3
/s,抗張強度為10MPa。
除了使用Isopar M(烴系有機溶劑、分餾溫度:218至253℃、Exxon Mobil有限公司製)250g替代Isopar C 250g,並將輥輪溫度從40℃變更為80℃以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為8.0×10-4
Pa.m3
/s,抗張強度為10MPa。
除了將輥輪溫度從40℃變更為25℃以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為4.0×10-4
Pa.m3
/s,抗張強度為10MPa。
除了將輥輪溫度從40℃變更為100℃以外,其餘皆依照與實施例1相同之方法,而製造薄片襯墊。
此薄片襯墊之洩漏量(氣密性)為1.0×10-3
Pa.m3
/s,抗張強度為6MPa。
Claims (6)
- 一種摻入填料之氟樹脂薄片之製造方法,其特徵為:包括將含有氟樹脂、填料及加工助劑的薄片形成用樹脂組成物以輥輪溫度40至80℃進行壓延的步驟;該加工助劑為含有分餾溫度為120℃以下之石油系烴溶劑在30質量%以上(惟,將加工助劑重量當作100質量%)。
- 如申請專利範圍第1項之摻入填料之氟樹脂薄片之製造方法,其中,該組成物中的該氟樹脂與該填料的質量比,係氟樹脂:填料=1:0.1至2。
- 如申請專利範圍第1項之摻入填料之氟樹脂薄片之製造方法,其中,相對於氟樹脂與填料之合計100重量份,該加工助劑含有5至50重量份。
- 如申請專利範圍第2項之摻入填料之氟樹脂薄片之製造方法,其中,相對於氟樹脂與填料之合計100重量份,該加工助劑含有5至50重量份。
- 如申請專利範圍第1至4項中任一項之摻入填料之氟樹脂薄片之製造方法,其係包含將藉由上述壓延步驟所調製之壓延薄片予以更進一步壓延的步驟。
- 一種摻入填料之氟樹脂薄片,其係藉由申請專利範圍第1至5項中任一項之摻入填料之氟樹脂薄片之製造方法所製得。
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JP2010023412A (ja) | 2008-07-23 | 2010-02-04 | Nippon Valqua Ind Ltd | 軟質シートの製造方法 |
JP5449739B2 (ja) | 2008-10-17 | 2014-03-19 | 日本ゴア株式会社 | 通気性複合シートの製造方法 |
JP5491758B2 (ja) | 2009-03-31 | 2014-05-14 | 日本バルカー工業株式会社 | 充填材入りフッ素樹脂シート、その製造方法およびガスケット |
JP5578841B2 (ja) * | 2009-12-08 | 2014-08-27 | 日本バルカー工業株式会社 | 充填材入りフッ素樹脂シートの製造方法および充填材入りフッ素樹脂シート |
WO2011116498A1 (zh) * | 2010-03-25 | 2011-09-29 | 华尔卡密封件制品(上海)有限公司 | 氟树脂片材 |
JP5989371B2 (ja) * | 2012-03-24 | 2016-09-07 | 日本バルカー工業株式会社 | 配管シール用フッ素樹脂製ガスケット |
JP6120639B2 (ja) * | 2013-03-29 | 2017-04-26 | 日本バルカー工業株式会社 | 配管シール用フッ素樹脂製ガスケットの面圧保持性の評価方法 |
JP2016104883A (ja) * | 2016-02-12 | 2016-06-09 | 日本バルカー工業株式会社 | 配管シール用フッ素樹脂製ガスケット |
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