TW201619289A - 難燃性胺酯樹脂組成物 - Google Patents
難燃性胺酯樹脂組成物 Download PDFInfo
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- TW201619289A TW201619289A TW104131978A TW104131978A TW201619289A TW 201619289 A TW201619289 A TW 201619289A TW 104131978 A TW104131978 A TW 104131978A TW 104131978 A TW104131978 A TW 104131978A TW 201619289 A TW201619289 A TW 201619289A
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- resin composition
- ester resin
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- amine ester
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Abstract
本發明之難燃性胺酯樹脂組成物含有聚異氰酸酯化合物、多元醇化合物、三聚化觸媒、發泡劑、及添加劑,且上述添加劑含有紅磷及填料,填料之縱橫比為5~50、平均粒徑為0.1μm以上且未達15μm、並且熔點為750℃以上。
Description
本發明係關於一種難燃性胺酯樹脂組成物。
於公寓等集體住宅、獨幢住宅、學校之各種設施、商業大樓等之外壁等使用經鋼筋等補強之混凝土作為提高建築物之強度之構造材料。
另一方面,混凝土由於有蓄熱性及蓄冷性,故會有如下缺點:在夏季建築物內部因蓄積之熱而被加熱,或在冬季之寒冷時期混凝土被冷卻,結果導致建築物內部被冷卻。為了減輕此種外部溫度通過混凝土而長時間對建築物內部產生之影響,通常對混凝土實施隔熱加工。
因此,作為隔熱層,業界一直使用具備對於火災為難燃性之硬質聚胺酯發泡體。
專利文獻1記載了一種難燃性胺酯樹脂組成物,其含有聚異氰酸酯化合物、多元醇化合物、三聚化觸媒、發泡劑、泡沫穩定劑及添加劑,三聚化觸媒為選自由含氮芳香族化合物、羧酸鹼金屬鹽、三級銨鹽、及四級銨鹽所組成之群中之至少一者,添加物以紅磷作為必需成分並且除紅磷以外亦組合選自由磷酸酯、含磷酸鹽之難燃劑、含溴之難燃劑、含硼
之難燃劑、含銻之難燃劑及金屬氫氧化物所組成之群中之至少一者而成。
專利文獻1:國際公開2014/112394號公報
上述專利文獻1之難燃性胺酯樹脂組成物藉由切為長10cm×寬10cm×厚5cm之由難燃性胺酯樹脂組成物所構成之成形體的放熱性試驗,顯示難燃性及形狀保持性優異。
然而,若使成形體之厚度更薄,則有如下問題:由於容易通熱,故而放熱性試驗中成形體之收縮及變形、尤其厚度方向之變形較大,於噴附或隔熱面板等用途中使用成形體時,無法確保防火方面充分之形狀保持性。
本發明之目的在於提供一種難燃性胺酯樹脂組成物,其可表現較高之難燃性,即便於厚度薄之情形時加熱時形狀保持性亦優異。
根據本發明,提供以下之難燃性胺酯樹脂組成物。
項1.一種難燃性胺酯樹脂組成物,其含有聚異氰酸酯化合物、多元醇化合物、三聚化觸媒、發泡劑、泡沫穩定劑、添加劑、及填料,其特徵在於:上述添加劑含有紅磷,該填料之縱橫比為5~50、平均粒徑為0.1μm以上且未達15μm、熔點為750℃以上。
項2.如項1之難燃性胺酯樹脂組成物,其中,上述填料於空氣條件下之TG/DTA測定中之重量減少率為5%以下。
項3.如項1或2之難燃性胺酯樹脂組成物,其中,上述填料為針狀之無機填料。
項4.如項1至3中任一項之難燃性胺酯樹脂組成物,其中,以由上述聚異氰酸酯化合物及上述多元醇化合物所構成之胺酯樹脂100重量份為基準,上述紅磷為3.5~30重量份,上述填料為3~30重量份。
項5.一種成形體,係由項1至4中任一項之難燃性胺酯樹脂組成物構成。
項6.如項5之成形體,其中,將100mm×100mm×20mm之上述成形體依照ISO-5660試驗方法以輻射熱強度50kW/m2加熱20分鐘時,加熱後相對於加熱前之成形體之長度方向及寬度方向之尺寸大於95mm,且厚度方向之變形未達10mm。
根據本發明,提供一種由即便厚度薄而加熱時形狀保持性亦優異之難燃性胺酯樹脂組成物所構成之成形體。
圖1係試驗用樣品之收縮測定部位之說明圖。(a)X、Y方向之測定,(b)Z方向之測定。
就本發明之難燃性胺酯樹脂組成物加以說明。
首先,就用於難燃性胺酯樹脂組成物之胺酯樹脂進行說明。
胺酯樹脂由作為主劑之聚異氰酸酯化合物及作為硬化劑之多元醇化合物所構成。
作為聚異氰酸酯化合物,例如可列舉:芳香族聚異氰酸酯、脂環族聚異氰酸酯、脂肪族聚異氰酸酯等。
作為芳香族聚異氰酸酯,例如可列舉:苯二異氰酸酯、甲伸苯基二異氰酸酯、苯二甲基二異氰酸酯、二苯甲烷二異氰酸酯、二甲基二苯甲烷二異氰酸酯、三苯甲烷三異氰酸酯、萘二異氰酸酯、多亞甲基多苯基聚異氰酸酯等。
作為脂環族聚異氰酸酯,例如可列舉:環己二異氰酸酯、甲基環己二異氰酸酯、異佛酮二異氰酸酯、二環己基甲烷二異氰酸酯、二甲基二環己基甲烷二異氰酸酯等。
作為脂肪族聚異氰酸酯,例如可列舉:亞甲基二異氰酸酯、伸乙基二異氰酸酯、伸丙基二異氰酸酯、四亞甲基二異氰酸酯、六亞甲基二異氰酸酯等。
聚異氰酸酯化合物可使用一種或兩種以上。就容易使用、容易獲得等理由而言,胺酯樹脂之主劑較佳為二苯甲烷二異氰酸酯。
關於作為胺酯樹脂之硬化劑之多元醇化合物,例如可列舉:聚內酯多元醇、聚碳酸酯多元醇、芳香族多元醇、脂環族多元醇、脂肪族多元醇、聚酯多元醇、聚合物多元醇、聚醚多元醇等。
作為聚內酯多元醇,例如可列舉:聚丙內酯二醇、聚己內酯二醇、聚戊內酯二醇等。
作為聚碳酸酯多元醇,例如可列舉:藉由乙二醇、丙二醇、丁二醇、戊二醇、己二醇、辛二醇、壬二醇等含羥基之化合物與碳酸二乙酯(diethylene carbonate)、碳酸二丙酯等之脫醇反應而獲得之多元醇等。
作為芳香族多元醇,例如可列舉:雙酚A、雙酚F、苯酚酚醛清漆、甲酚酚醛清漆等。
作為脂環族多元醇,例如可列舉:環己二醇、甲基環己二醇、異佛酮二醇、二環己基甲二醇、二甲基二環己基甲二醇等。
作為脂肪族多元醇,例如可列舉:乙二醇、丙二醇、丁二醇、戊二醇、己二醇等。
作為聚酯多元醇,例如可列舉:使多元酸與多元醇進行脫水縮合而獲得之聚合物、使ε-己內酯、α-甲基-ε-己內酯等內酯進行開環聚合而獲得之聚合物、及羥基羧酸與上述多元醇等之縮合物。
此處,作為多元酸,具體而言,例如可列舉:己二酸、壬二酸、癸二酸、對苯二甲酸、間苯二甲酸、丁二酸等。又,作為多元醇,具體而言,例如可列舉:雙酚A、乙二醇、1,2-丙二醇、1,4-丁二醇、二乙二醇、1,6-己二醇、新戊二醇等。
又,作為羥基羧酸,具體而言,例如可列舉:蓖麻油、蓖麻油與乙二醇之反應產物等。
作為聚合物多元醇,例如可列舉:使丙烯腈、苯乙烯、丙烯酸甲酯、甲基丙烯酸酯等乙烯性不飽和化合物接枝聚合於芳香族多元醇、脂環族多元醇、脂肪族多元醇、聚酯多元醇等而成之聚合物、聚丁二烯多元醇、多元醇之改質多元醇或該等之氫化物等。
作為多元醇之改質多元醇,例如可列舉使環氧烷與原料之多元醇進行反應而改質而成者等。
作為多元醇,例如可列舉:甘油及三羥甲基丙烷等三元醇;
新戊四醇、山梨醇、甘露醇、山梨醇酐、雙甘油、二新戊四醇等、蔗糖、葡萄糖、甘露糖、果糖、甲基葡糖苷及其衍生物等四~八元醇;苯酚、間苯三酚(phloroglucin)、甲酚、五倍子酚、兒茶酚、對苯二酚、雙酚A、雙酚F、雙酚S、1-羥基萘、1,3,6,8-四羥基萘、蒽酚(anthrol)、1,4,5,8-四羥基蒽、1-羥基芘等酚聚丁二烯多元醇;蓖麻油多元醇;(甲基)丙烯酸羥基烷基酯之(共)聚合物及聚乙烯醇等多官能(例如官能基數2~100)多元醇、苯酚與甲醛之縮合物(酚醛清漆)。
多元醇之改質方法並無特別限定,可較佳地使用使環氧烷(以下簡稱為AO)加成之方法。
作為AO,可列舉碳數2~6之AO,例如可列舉:環氧乙烷(以下簡稱為EO)、1,2-環氧丙烷(以下簡稱為PO)、1,3-環氧丙烷、1,2-環氧丁烷、1,4-環氧丁烷等。
該等之中,就性狀或反應性之觀點而言,較佳為PO、EO及1,2-環氧丁烷,更佳為PO及EO。作為使用2種以上AO之情形(例如PO及EO)之加成方法,可為嵌段加成,可為無規加成,亦可併用該等。
作為聚醚多元醇,例如可列舉於具有2個以上活性氫之低分子量活性氫化合物等之至少一種之存在下,使環氧乙烷、環氧丙烷、四氫呋喃等環氧烷之至少1種進行開環聚合而獲得之聚合物。
作為具有2個以上活性氫之低分子量活性氫化合物,例如可列舉:雙酚A、乙二醇、丙二醇、丁二醇、1,6-己二醇等二醇類;甘油、三羥甲基丙烷等三醇類;乙二胺、丁二胺等胺類等。
就燃燒時之總放熱量之減少效果較大而言,用於本發明之多
元醇較佳為使用聚酯多元醇或聚醚多元醇。
其中,更佳為使用分子量200~800之聚酯多元醇,進而較佳為使用分子量300~500之聚酯多元醇。
又,異氰酸酯指數係以百分率表示聚異氰酸酯化合物之異氰酸酯基相對於多元醇化合物之羥基之當量比者,該值超過100意味著與羥基相比異氰酸酯基過量。
本發明所使用之胺酯樹脂之異氰酸酯指數的範圍較佳為250~1000之範圍,更佳為250~800之範圍,進而較佳為300~700之範圍。異氰酸酯指數(INDEX)係利用以下方法算出。
INDEX=異氰酸酯之當量數÷(多元醇之當量數+水之當量數)×100
此處,異氰酸酯之當量數=聚異氰酸酯之使用份數×NCO含有率(%)÷100/NCO之分子量
多元醇之當量數=OHV×多元醇之使用份數÷KOH之分子量
OHV為多元醇之羥值(mgKOH/g),水之當量數=水之使用份數×水之OH基之數/水之分子量
再者,上述式中,使用份數之單位為重量(g),NCO基之分子量為42,NCO含有率係以質量%表示聚異氰酸酯化合物中之NCO基之比率者,為了方便上述式之單位換算,將KOH之分子量設為56100,水之分子量設為18,水之OH基個數設為2。
又,難燃性胺酯樹脂組成物含有觸媒、發泡劑、泡沫穩定劑、添加劑及填料。
作為觸媒,例如可列舉:三乙基胺、N-甲基啉雙(2-二甲基胺基乙基)醚、N,N,N',N",N"-五甲基二伸乙基三胺、N,N,N'-三甲基胺基乙基-乙醇胺、雙(2-二甲基胺基乙基)醚、N-甲基,N'-二甲基胺基乙基哌、咪唑環中之二級胺官能基經氰乙基取代的咪唑化合物等含氮原子之觸媒等。
關於用於難燃性胺酯樹脂組成物之觸媒之添加量,相對於胺酯樹脂100重量份,較佳為0.6重量份~10重量份之範圍,更佳為0.6重量份~8份之範圍,進而較佳為0.6重量份~6重量份之範圍,最佳為0.6重量份~3.0重量份之範圍。
為0.6重量份以上之情形時,不產生阻礙胺酯鍵之形成之異常情況,為10重量份以下之情形時,可維持適當之發泡速度,容易處理。
作為較佳之觸媒,包含三聚化觸媒,該三聚化觸媒係:使作為聚胺酯樹脂之主劑之聚異氰酸酯化合物所含之異氰酸酯基反應,使之三聚化,從而促進異氰尿酸酯環(isocyanurate ring)之生成。
三聚化觸媒係使作為聚胺酯樹脂之主劑之聚異氰酸酯化合物所含之異氰酸酯基反應,使之三聚化,從而促進異氰尿酸酯環之生成。
作為三聚化觸媒,可列舉:三(二甲基胺基甲基)苯酚、2,4-雙(二甲基胺基甲基)苯酚、2,4,6-三(二烷基胺基烷基)六氫-對稱三等含氮芳香族化合物;乙酸鉀、2-乙基己酸鉀、羧酸鹼金屬鹽;三甲基銨鹽、三乙基銨鹽、三苯基銨鹽等三級銨鹽;四甲基銨鹽、四乙基銨、四苯基銨鹽等四級銨鹽等。
關於用於難燃性胺酯樹脂組成物之三聚化觸媒的添加量,相
對於胺酯樹脂100重量份,較佳為0.6重量份~10重量份之範圍,更佳為0.6重量份~8重量份之範圍,進而較佳為0.6重量份~6重量份之範圍,最佳為0.6重量份~3.0重量份之範圍。為0.6重量份以上之情形時,不產生阻礙異氰酸酯之三聚化之異常情況,為10重量份以下之情形時,可維持適當之發泡速度,容易處理。
又,用於難燃性胺酯樹脂組成物之發泡劑促進胺酯樹脂之發泡。
作為發泡劑之具體例,例如可列舉:水;丙烷、丁烷、戊烷、己烷、庚烷、環丙烷、環丁烷、環戊烷、環己烷、環庚烷等低沸點之烴;二氯乙烷、氯丙烷、異氯丙烷、氯丁烷、異氯丁烷、氯戊烷、異氯戊烷等氯化脂肪族烴化合物;CHF3、CH2F2、CH3F等氟化合物;三氯單氟甲烷、三氯三氟乙烷、二氯單氟乙烷(例如HCFC141b(1,1-二氯-1-氟乙烷)、HCFC22(氯二氟甲烷)、HCFC142b(1-氯-1,1-二氟乙烷))等氫氯氟碳化合物;HFC-245fa(1,1,1,3,3-五氟丙烷)、HFC-365mfc(1,1,1,3,3-五氟丁烷)等氫氟碳;二異丙醚等醚化合物、或者該等化合物之混合物等有機系物理發泡劑、氮氣、氧氣、氬氣、二氧化碳氣體等無機系物理發泡劑等。
關於發泡劑之範圍,相對於胺酯樹脂100重量份,較佳為0.1重量份~30重量份之範圍。發泡劑相對於胺酯樹脂100重量份,更佳為0.1重量份~18重量份之範圍,進而較佳為0.5重量份~18重量份之範圍,最佳為0.5重量份~10重量份之範圍。
當發泡劑之範圍為0.1重量份以上時,促進氣泡之形成,可獲得良好之發泡體,當30重量份以下時,可防止氣化力變高,氣泡變得粗
大。
作為用於難燃性胺酯樹脂組成物之泡沫穩定劑,例如可列舉如下等之界面活性劑等:聚氧伸烷基烷基醚等聚氧伸烷基泡沫穩定劑、有機聚矽氧烷等聚矽氧泡沫穩定劑。
泡沫穩定劑相對於藉由化學反應而硬化之胺酯樹脂之使用量,係根據所使用之藉由化學反應而硬化之胺酯樹脂進行適當設定,若表示一例,則例如相對於胺酯樹脂100重量份,較佳為0.1重量份~10重量份之範圍。
觸媒、發泡劑及泡沫穩定劑分別可使用一種或兩種以上。
繼而,就用於本發明之難燃性胺酯樹脂組成物之添加劑加以說明。
根據本發明,添加劑含有紅磷作為必需成分。於一實施形態中,添加劑含有紅磷、及磷酸酯。
關於用於本發明之添加劑的添加量,相對於胺酯樹脂100重量份,胺酯樹脂以外之添加劑其總量之範圍較佳在6重量份~70重量份之範圍,更佳在6重量份~40重量份之範圍,進而較佳在6重量份~30重量份之範圍,最佳在6重量份~20重量份之範圍。
於添加劑之範圍在6重量份以上時,可防止由難燃性胺酯樹脂組成物所構成之成形體因火災之熱所形成之緻密殘渣破裂,於70重量份以下時,不阻礙難燃性胺酯樹脂組成物之發泡。
用於本發明之紅磷並無限定,可適當選擇市售品而使用。
關於本發明之耐火胺酯樹脂組成物所使用之紅磷之添加
量,相對於胺酯樹脂100重量份,通常較佳在3.5重量份~30重量份之範圍,更佳在3.5~20重量份之範圍,更佳在6.0重量份~18重量份之範圍。
於紅磷之範圍在3.5重量份以上時,難燃性胺酯樹脂組成物之自熄性得以保持,又,於20重量份以下時,不阻礙難燃性胺酯樹脂組成物之發泡。
於較佳之一實施形態中,相對於難燃性胺酯樹脂組成物之重量,紅磷為2~18重量%。
又,用於本發明之磷酸酯並無特別限定,較佳為使用單磷酸酯、縮合磷酸酯等。
作為單磷酸酯,並無特別限定,例如可列舉:磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、磷酸三(2-乙基己基)酯、磷酸三(丁氧基乙基)酯、磷酸三苯酯、磷酸三甲苯酯(tricresyl phosphate)、磷酸三(二甲苯基)酯(trixylenyl phosphate)、磷酸三(異丙基苯基)酯、磷酸三(苯基苯基)酯、磷酸三萘酯、磷酸甲酚二苯酯(cresyl diphenyl phosphate)、磷酸二甲苯基二苯酯(xylenyl diphenyl phosphate)、磷酸二苯基(2-乙基己基)酯、磷酸二(異丙基苯基)苯酯、磷酸單異癸酯、酸式磷酸2-丙烯醯氧基乙酯(2-acryloyloxyethyl acid phosphate)、酸式磷酸2-甲基丙烯醯氧基乙酯、磷酸二苯基-2-丙烯醯氧基乙酯、磷酸二苯基-2-甲基丙烯醯氧基乙酯、三聚氰胺磷酸酯、二-三聚氰胺磷酸酯、三聚氰胺焦磷酸酯(melamine pyrophosphate)、三苯基氧化膦、三甲酚基氧化膦、甲膦酸二苯酯(methanephosphonate diphenyl)、苯基膦酸二乙酯、間苯二酚雙(二苯基磷酸酯)(resorcinol bis(diphenyl phosphate))、雙酚A雙(二苯基磷酸酯)、磷雜菲(phosphaphenanthrene)、磷
酸三(β-氯丙基)酯等。
作為縮合磷酸酯,並無特別限定,例如可列舉:聚磷酸三烷基酯、間苯二酚聚磷酸苯酯、間苯二酚聚磷酸(二-2,6-二甲苯基)酯(大八化學工業公司製造、商品名PX-200)、對苯二酚聚磷酸(2,6-二甲苯基)酯以及該等之縮合物等縮合磷酸酯。
作為市售之縮合磷酸酯,例如可列舉:間苯二酚聚磷酸苯酯(商品名CR-733S)、雙酚A聚磷酸甲酚酯(商品名CR-741)、芳香族縮合磷酸酯(商品名CR747)、間苯二酚聚磷酸苯酯(ADEKA公司製造、商品名Adekastab PFR)、雙酚A聚磷酸甲酚酯(商品名FP-600、FP-700)等。
上述之中,為了使硬化前之組成物中黏度降低效果及減少初期之放熱量之效果較高,較佳為使用單磷酸酯,更佳為使用磷酸三(β-氯丙基)酯。
磷酸酯可使用一種或兩種以上。
關於磷酸酯之添加量,相對於胺酯樹脂100重量份,較佳為2.5重量份~50重量份之範圍,更佳為2.5重量份~40重量份之範圍,進而較佳為2.5重量份~30重量份之範圍。
於磷酸酯之範圍在2.5重量份以上時,自熄性得以保持,於50重量份以下時,不阻礙難燃性胺酯樹脂組成物之發泡。
再者,作為添加劑,亦可進而添加除紅磷、磷酸酯以外之添加劑。例如,亦可代替磷酸酯或除磷酸酯以外,添加選自由含磷酸鹽之難燃劑、含溴之難燃劑、含硼之難燃劑、含銻之難燃劑及金屬氫氧化物所組
成之群中之至少一種添加劑。
繼而,就用於本發明之難燃性胺酯樹脂組成物之填料加以說明。
填料防止收縮及/或變形。本說明書中,所謂「收縮」,意指包括長度方向之長度、寬度方向之長度、及厚度方向之長度的長度變化,所謂「變形」,意指翹曲等形狀之變化、尤其厚度方向之形狀變化。
填料可為有機系填料,亦可為無機系填料,較佳為無機系填料。填料之縱橫比為5~50,較佳為8~40,更佳為10~40,進而較佳為10~35,最佳為8~25。此處,所謂本說明書中所述之填料之縱橫比,為於利用掃描型電子顯微鏡觀察填料而獲得之圖像中確認之填料的最大長度相對於最小厚度(相對於最大長度垂直之方向)之比(亦稱為直徑/厚度比),為足夠數量之填料即250個以上之平均。
填料之平均粒徑為0.1μm以上且未達15μm,較佳為0.1μm以上且14μm以下,更佳為0.3~10μm。平均粒徑係藉由X射線穿透式沈澱法粒度分佈測定裝置而求出。填料之熔點為750℃以上,較佳為800℃以上,更佳為1,000℃以上。
關於填料之形狀,只要滿足上述縱橫比、平均粒徑、及熔點,則可為針狀填料或板狀填料之任一者,較佳之填料為針狀填料。
針狀意指長徑為短徑之3倍以上者,不僅為所謂針形狀,亦包括紡錘狀、圓柱狀者等。板狀不僅為所謂板形狀,亦包括鱗片狀、薄片狀者等。
作為針狀之無機填料,可例示:鹼性硫酸鎂、硼酸鋁、矽灰
石(wollastonite)、硬矽鈣石、碳鈉鋁石、矽磷灰石、水鋁石(boehmite)、棒狀羥基磷灰石、鈦酸鉀晶鬚、硼酸鋁晶鬚、鎂系晶鬚、矽系晶鬚、針狀氧化鋁、針狀陶瓷、石棉、針狀碳酸鈣、石膏纖維、玻璃纖維、石棉纖維、二氧化矽纖維、氧化鋁纖維、二氧化矽-氧化鋁纖維、氧化鋯纖維、碳纖維(包括奈米碳管等纖維狀、針狀或富勒烯等球狀之新型碳)、石墨纖維、氮化硼纖維、硼纖維、金屬纖維等。
作為板狀之無機填料,可例示鱗片狀石墨、滑石、白雲母(muscovite)及金雲母(phlogopite)等雲母類、絹雲母(sericite)、高嶺土、綠泥石、蒙脫石、多水高嶺土等層狀黏土礦物、板狀碳酸鈣、板狀氫氧化鋁、玻璃薄片、板狀氧化鐵、金屬板狀物等。
於一實施形態中,填料為縱橫比為5~50、平均粒徑為0.1μm以上且未達15μm之針狀無機填料。較佳之填料為矽灰石或鈦酸鉀晶鬚。
填料之添加量相對於胺酯樹脂100重量份,較佳為3~30重量份之範圍,更佳為3重量份~25重量份之範圍,進而較佳為3重量份~18重量份之範圍。於一實施形態中,相對於添加劑6~80重量份,填料為3~30重量份,較佳為相對於添加劑6重量份~60重量份,填料為3重量份~25重量份,更佳為相對於添加劑8.5重量份~48重量份,填料為3重量份~18重量份。
本發明之難燃性胺酯樹脂組成物可併用與上述填料不同之一種或兩種以上無機填充材。
進而,難燃性胺酯樹脂組成物分別可於無損本發明之目的之
範圍,視需要含有酚系、胺系、硫系等抗氧化劑、熱穩定劑、金屬傷害抑制劑、抗靜電劑、穩定劑、交聯劑、潤滑劑、軟化劑、顏料、黏著賦予樹脂等輔助成分、聚丁烯、石油樹脂等黏著賦予劑。
由於難燃性胺酯樹脂組成物會反應而硬化,故其黏度隨著時間經過而變化。因此,於使用難燃性胺酯樹脂組成物之前,將難燃性胺酯樹脂組成物分成兩份以上,防止難燃性胺酯樹脂組成物反應而硬化。並且,於使用難燃性胺酯樹脂組成物時,藉由將分成兩份以上之難燃性胺酯樹脂組成物整合為一份,可獲得難燃性胺酯樹脂組成物。
再者,於將難燃性胺酯樹脂組成物分成兩份以上時,只要以分成兩份以上之難燃性胺酯樹脂組成物之各成分在單獨之情況下不會開始硬化,於將難燃性胺酯樹脂組成物之各成分混合後開始硬化反應之方式分割各成分即可。
於一實施形態中,難燃性胺酯樹脂組成物以由上述聚異氰酸酯化合物及上述多元醇化合物所構成之胺酯樹脂100重量份作為基準,含有0.6~10重量份之範圍之三聚化觸媒、0.1~30重量份之發泡劑、0.1重量份~10重量份之範圍之泡沫穩定劑、及6重量份~80重量份之範圍之添加劑,紅磷為3.5~30重量份,填料為3~30重量份。
難燃性胺酯樹脂組成物之製造方法並無特別限定,例如可藉由如下方法而獲得:將難燃性胺酯樹脂組成物之各成分進行混合之方法;使難燃性胺酯樹脂組成物懸浮於有機溶劑或者加熱使之熔融而製作塗料狀之方法;分散於溶劑而製備漿料等方法;又,於難燃性胺酯樹脂組成物所含之反應硬化性樹脂成分中含有於常溫(約25℃)之溫度下為固體之成分
時,藉由使難燃性胺酯樹脂組成物於加熱下熔融等方法。
難燃性胺酯樹脂組成物可藉由使用單軸擠出機、雙軸擠出機、班布里混合機(Banbury mixer)、混練攪拌機、混練輥、擂潰機、行星式攪拌機等公知之裝置將難燃性胺酯樹脂組成物之各成分進行混練而獲得。
又,亦可事先將胺酯樹脂之主劑及硬化劑分別與填充材等一併混練,於即將注入前利用靜態混合器、動態混合器等進行混練而獲得。
進而,亦可將觸媒除外之難燃性胺酯樹脂組成物之成分、及觸媒於即將注入前同樣地混練而獲得。藉由以上說明之方法,可獲得難燃性胺酯樹脂組成物。
繼而,就本發明之難燃性胺酯樹脂組成物之硬化方法進行說明。
若將上述難燃性胺酯樹脂組成物之各成分加以混合,則反應開始,黏度隨著時間之經過而上升,失去流動性。
例如,藉由將上述難燃性胺酯樹脂組成物注入至模具、框材等容器中並使之硬化,從而可以發泡體之形式獲得由上述難燃性胺酯樹脂組成物所構成之成形體。或者,藉由將上述難燃性胺酯樹脂組成物噴附至被塗構造物並使之硬化,而可以發泡體之形式獲得由上述難燃性胺酯樹脂組成物所構成之成形體。
於獲得由上述難燃性胺酯樹脂組成物所構成之成形體時,可加熱或者施加壓力。
本發明之成形體之厚度並無特別限定,例如為1~50mm。
尤其於20mm以上之情形時,會發揮抑制放熱性試驗時之變形的效果,較為有利。於一實施形態中,本發明之成形體為如下尺寸:將100mm×100mm×20mm(長度方向×寬度方向×厚度方向)之上述成形體依照ISO-5660試驗方法以輻射熱強度50kW/m2加熱20分鐘時,加熱後相對於加熱前之成形體之長度方向及寬度方向之尺寸大於95mm,且厚度方向之變形未達10mm。
關於本發明之由難燃性胺酯樹脂組成物所構成之成形體,就容易操作而言,較佳為比重在0.020-0.130之範圍,更佳在0.020-0.100之範圍,進而較佳在0.030-0.080之範圍,最佳在0.030-0.060之範圍。
關於本發明之由難燃性胺酯樹脂組成物所構成之成形體,較佳為在如下空氣條件下之TG/DTA測定中之重量減少率(1-加熱後之樣品重量/加熱前之樣品重量)×100(%))為5%以下,該空氣條件為:將溫度條件設為以10℃/min之比率自30℃升溫至900℃,將測定環境設為流量100mL/min之空氣流之情形。因此,成形體於加熱後亦可保持較高形狀保持性。
繼而,就本發明之難燃性胺酯樹脂組成物之應用例加以說明。
可使上述難燃性胺酯樹脂組成物成形為厚度薄之面板,配置於建築物、傢俱、汽車、電車、船等構造物。或者,藉由將上述難燃性胺酯樹脂組成物噴附至上述構造物,可於上述構造物之表面形成由難燃性胺酯樹脂組成物所構成之發泡體層。
繼而,就對本發明之纖維強化樹脂成形體實施之耐火試驗加
以說明。
將由難燃性胺酯樹脂組成物所構成之成形體切斷為長100mm、寬100mm及厚20mm,準備錐形卡路里計試驗用樣品。
可使用錐形卡路里計試驗用樣品,測定依照ISO-5660之試驗方法以輻射熱強度50kW/m2加熱20分鐘時之藉由錐形卡路里計試驗測得之總放熱量。
以下,列舉實施例更具體地說明本發明,但本發明並不限定於該等。
實施例1 由難燃性胺酯樹脂組成物所構成之發泡成形體之製造及其性能評價
1.由難燃性胺酯樹脂組成物所構成之發泡成形體之製造
藉由表1及表2所示之組成,分別準備實施例1~20及比較例1~14之難燃性胺酯樹脂組成物。表中之各成分之詳細情況如下所述。
1.多元醇化合物
(A-1)對苯二甲酸聚酯多元醇(川崎化成工業公司製造,製品名:MAXIMOL RFK-505,羥值=250mgKOH/g)
(A-2)對苯二甲酸聚酯多元醇(川崎化成工業公司製造,製品名:MAXIMOL RLK-087,羥值=200mgKOH/g)
2.觸媒
(B-1)三聚化觸媒(辛酸鉀、Momentive Performance Materials公司製造,製品名:K-Zero G)
(B-2)三聚化觸媒(Tosoh公司製造,製品名:TOYOCAT-TR20)
(B-3)胺酯化觸媒(五甲基二伸乙基三胺,Tosoh公司製造,製品名:TOYOCAT-DT)
(B-4)三聚化觸媒(Tosoh公司製造,製品名:TOYOCAT-RX5)
(B-5)胺酯化觸媒(三伸乙基二胺,Tosoh公司製造,製品名:TEDA-L33)
(B-6)胺酯化觸媒(1,2-二甲基咪唑,Tosoh公司製造,製品名:TOYOCAT-DM70)
3.泡沫穩定劑
聚伸烷基二醇系泡沫穩定劑(Dow Corning Toray公司製造,製品名:SH-193)
4.發泡劑
(C-1)純水
(C-2)HFC HFC-365mfc(1,1,1,3,3-五氟丁烷,Nippon Solvay公司製造)及HFC-245fa(1,1,1,3,3-五氟丙烷,Central Glass公司製造)、混合比率HFC-365mfc:HFC-245fa=7:3,以下稱為「HFC」)
5.異氰酸酯化合物(以下稱為「聚異氰酸酯」)
MDI(日本聚胺酯工業公司製造,製品名:MILLIONATE MR-200)黏度:167mPa‧s,NCO含量=32.1%
6.添加劑
(D-1)紅磷(磷化學工業公司製造,製品名:Novaexcel 140)
(D-2)磷酸三(β-氯丙基)酯(大八化學公司製造,製品名:TMCPP,
以下稱為「TMCPP」)
(D-3)含溴之難燃劑(MANAC公司製造,製品名:HBB-b,以下稱為「HBB」)
(D-4)磷酸二氫銨(太平化學產業公司製造)
7.填料
(E-1)矽灰石(SiO2‧CaO)(Kinsei Matec公司製造,製品名:SH-1250)縱橫比10~16、平均粒徑4.5~6.5μm
(E-2)矽灰石(SiO2‧CaO)(Kinsei Matec公司製造,製品名:SH-800)縱橫比15~20、平均粒徑6~9μm
(E-3)矽灰石(SiO2‧CaO)(Kinsei Matec公司製造,製品名:SH-600)縱橫比12~18、平均粒徑9.5~13μm
(E-4)矽灰石(SiO2‧CaO)(Kinsei Matec公司製造,製品名:SH-400)縱橫比12~18、平均粒徑15~25μm
(E-5)矽灰石(SiO2‧CaO)(Kinsei Matec公司製造,製品名:FRW-800)縱橫比2~4、平均粒徑3.5~4.5μm
(E-6)鈦酸鉀晶鬚(K2OnTiO2)(大塚化學公司製造,製品名:Tismo D)縱橫比17~33、平均粒徑0.3~0.6μm
(E-7)鈦酸鉀晶鬚(K2OnTiO2)(大塚化學公司製造,製品名:Terracess TF-S)平均粒徑3~11μm
(E-8)鈦酸鉀晶鬚(K2OnTiO2)(大塚化學公司製造,製品名:Terracess JP)平均粒徑6~13μm
(E-9)氧化鋁(Al2O3‧H2O)(河合石灰工業公司製造,製品名:Cerasur
BMI)縱橫比30~50、平均粒徑4~6μm
(E-10)氧化鋁(Al2O3‧H2O)(河合石灰工業公司製造,製品名:Cerasur BMF)縱橫比40~50、平均粒徑3~5μm
(E-11)氧化鋁(Al2O3‧H2O)(河合石灰工業公司製造,製品名:Cerasur BMM)縱橫比10、平均粒徑0.8~1μm
依照下述表1及表2之組成,將除聚異氰酸酯化合物、HFC成分以外之多元醇化合物、泡沫穩定劑、各種觸媒、發泡劑、添加劑、及填料稱取至1000mL聚丙烯燒杯中,利用手動攪拌器於25℃攪拌10秒。對於攪拌後之混練物添加聚異氰酸酯化合物、HFC成分,利用手動攪拌器攪拌約10秒,製成發泡體。所獲得之難燃性胺酯樹脂組成物隨著時間之經過而失去流動性,獲得實施例1~20及比較例1~14之難燃性胺酯樹脂組成物之發泡成形體。
2.成形體之評價
(總放熱量之測定)
自硬化物以成為100mm×100mm×20mm(長度方向×寬度方向×厚度方向)之方式切出錐形卡路里計試驗用樣品,依據ISO-5660,以輻射熱強度50kW/m2加熱20分鐘。將結果示於表1及2。
(密度之測定)
自硬化物以成為100mm×100mm×20mm(長度方向×寬度方向×厚度方向)之方式切出錐形卡路里計試驗用樣品,使用游標卡尺量測尺寸,利用電子天平量測質量,測出密度。將結果示於表1及2。
20分鐘加熱下之錐形卡路里計之總放熱量於實施例1-19
中均為8MJ/m2以下,本發明之成形體之難燃性優異。關於比較例,亦有如比較例3-5般,於20分鐘加熱下之錐形卡路里計之總放熱量超過8MJ/m2者。
(收縮測定)
測定於上述錐形卡路里計試驗中加熱時之收縮量及變形量(mm)。如圖1(a)所示,X表示長度方向、Y表示寬度方向,如圖1(b)所示,Z表示厚度方向。對於試驗用樣品,於X方向、Y方向上各測定3處,Z方向上於收縮最大處測定,任一方向上均採用收縮最大之數值。將長度方向及寬度方向之成形體之長度大於95mm之情形評為合格,將95mm以下評為不合格,將厚度方向之變形未達10mm評為合格,將10mm以上評為不合格,將於X、Y、Z方向之所有方向合格之情形判定為○,將於X、Y、Z方向之至少一方向上不合格之情形判定為×。將結果示於表1及2。
關於實施例1-20之成形體,變形量均較小,發揮成形體之厚度較薄時之變形抑制效果。
實施例2 各種填料對於發泡成形體之收縮之影響之評價
相對於胺酯樹脂100重量份,將實施例1所使用之各填料設為3重量份、6重量份、或9重量份,除此以外,以與實施例1相同之材料及組成製造發泡成形體。各填料之粒徑利用X射線穿透式沈澱法粒度分佈測定裝置求出,測定縱橫比。
將以與實施例1相同之方式製作之100mm×100mm×20mm之各試驗用樣品供於錐形卡路里計試驗。測定燃燒試驗後之收縮量,將於X、Y、Z方向之所有方向上合格之情形判定為○,將於X、Y、Z方向之至少一方向上不合格之情形判定為×。
又,將填料樣品取樣品量10mg,將溫度條件設為以10℃/min之比率自30℃升溫至900℃,將測定環境設為流量100mL/min之空氣流,使用TG/DTA測定裝置(TG/DTA7300、Hitachi High-Tech Science公司製造)測定重量,測定加熱後之樣品重量/加熱前之樣品重量×100(%)即樣品殘存量。
根據表3所示之結果,判明於填料縱橫比為5~50、平均粒徑為0.1μm以上且未達15μm、並且熔點高於加熱溫度時,以任一添加量,發泡成形體之收縮均較小。又,關於此種填料,樣品於空氣條件下之TG/DTA測定中之填料之重量減少率止於5%以下。
Claims (6)
- 一種難燃性胺酯樹脂組成物,其含有聚異氰酸酯化合物、多元醇化合物、三聚化觸媒、發泡劑、泡沫穩定劑、添加劑、及填料,其特徵在於:上述添加劑含有紅磷,該填料之縱橫比為5~50、平均粒徑為0.1μm以上且未達15μm、並且熔點為750℃以上。
- 如申請專利範圍第1項之難燃性胺酯樹脂組成物,其中,空氣條件下之TG/DTA測定中之上述填料之重量減少率為5%以下。
- 如申請專利範圍第1或2項之難燃性胺酯樹脂組成物,其中,上述填料為針狀之無機填料。
- 如申請專利範圍第1至3項中任一項之難燃性胺酯樹脂組成物,其中,以由上述聚異氰酸酯化合物及上述多元醇化合物所構成之胺酯樹脂100重量份為基準,上述紅磷為3.5~30重量份,上述填料為3~30重量份。
- 一種成形體,係由申請專利範圍第1至4項中任一項之難燃性胺酯樹脂組成物構成。
- 如申請專利範圍第5項之成形體,其中,將100mm×100mm×20mm之上述成形體依照ISO-5660試驗方法以輻射熱強度50kW/m2加熱20分鐘時,加熱後相對於加熱前之成形體之長度方向及寬度方向之尺寸大於95mm,且厚度方向之變形未達10mm。
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