TWI523993B - 阻燃聚對酞酸丙二酯組成物與由其製成之物品 - Google Patents
阻燃聚對酞酸丙二酯組成物與由其製成之物品 Download PDFInfo
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Description
本發明係關於具有改良阻燃性之聚對酞酸丙二酯(poly(trimethylene terephthalate))組成物與由該組成物製成之物品。
聚對酞酸丙二酯(PTT)在各式需求阻燃性之應用中皆具有潛在利用性。然而,對於改善PTT之阻燃性仍存在需求。具體而言,理想為在地毯中使PTT具有改良之輻射板(radiant panel)性能,以得到如該項技術領域中所知的第一級地毯塊(>0.45 Watts/cm2)。
本發明之一種態樣為一聚對酞酸丙二酯基之組成物,其包含:(a)約75至約99.9重量百分比的一樹脂組分,此係基於總組成物重量,其中該樹脂組分包含至少約70重量百分比的一聚對酞酸丙二酯,此係基於該樹脂組分之重量;以及(b)約0.1至約25重量百分比的一添加劑套組,此係基於總組成物重量,其中該添加劑套組包含約0.1至約15重量百分比的一三聚氰胺三聚氰酸鹽(melamine cyanurate)、三聚氰胺焦磷酸鹽(melamine pyrophosphate)、一二乙膦酸之鋅鹽(zinc salt of diethyl phosphinic acid)或其摻合物,此係基於總組成物重量。
本發明之另一種態樣為一地毯,其包含面纖維與一預塗料,其中該面纖維係由一聚對酞酸丙二酯基之組成物製成,該組成物包含:(a)約75至約99.9重量百分比的一樹脂組分,此係基於總組成物重量,其中該樹脂組分包含至少約70重量百分比的一聚對酞酸丙二酯,此係基於該樹脂組分之重量;以及(b)約0.1至約25重量百分比的一添加劑套組,此係基於總組成物重量,其中該添加劑套組包含約0.1至約15重量百分比的一三聚氰胺三聚氰酸鹽、三聚氰胺焦磷酸鹽、一二乙膦酸之鋅鹽或其摻合物,此係基於總組成物重量,並且該預塗料含有一選自三水合鋁(ATH)與氫氧化鎂之阻燃添加劑。
本文中所揭露之組成物含有一樹脂組分,其包含PTT與選擇性之一種或多種其他聚合物,以及一種或多種選自由下列之阻燃化合物:三聚氰胺磷酸鹽、三聚氰胺三聚氰酸鹽與二乙膦酸鋅鹽。可在該樹脂組分中之其他聚合物包括聚對酞酸乙二酯、聚對酞酸丁二酯、耐綸、聚丙烯與其摻合物。因此,術語「PTT基組成物」如本文中所用者,意欲涵括該樹脂組分除了PTT外尚含有一種或多種其他聚合物之組成物。其他聚合物在樹脂組分中之量(基於該樹脂組分總重量)可有所變化,例如可為5、10、15、20或25重量百分比或更高。在某些較佳實施例中(其中一種或多種其他聚合物係與PTT一起存在於該樹脂組分中),該樹脂組分含有75至99重量百分比的PTT與1至25重量百分比的其他聚合物,此係基於該樹脂組分總重量。
在某些實施例中,該樹脂組分包含一由生物衍生1,3-丙二醇製成之聚對酞酸丙二酯。
已意外發現,包含由聚對酞酸丙二酯基組成物製成之面纖維與一預塗料的地毯,其中該預塗料含有一選自三水合鋁與氫氧化鎂之阻燃添加劑,在阻燃性測試中具有預料之外的高效與穩定性能。
在某些實施例中,該樹脂組分中所含的添加劑套組除了特定阻燃劑外,尚含有一種或多種添加劑如退光劑(例如TiO2、硫酸鋅或氧化鋅)、一染料或顏料。該添加劑套組可進一步含有一種或多種添加劑如抗氧化劑、殘留催化劑、著色劑(例如染料)、安定劑、填充劑(例如碳酸鈣)、抗微生物劑、去靜電劑、光學亮光劑、增效劑、加工助劑與/或其他功能性添加劑,通常稱為「成效添加物(chip additives)」。
TiO2與其他可作為顏料與/或退光劑之化合物如硫化鋅或氧化鋅,其使用量可為該項技術領域中用於製造PTT組成物所常用者。例如,若是用於製造纖維,顏料/退光劑總量可為約5重量百分比或更多,此係基於該之PTT基組成物總量,而用於其他應用則可為相對較高之量。可用於作為顏料與/或退光劑之材料實例包括TiO2、ZnO與硫酸鋅。在某些實施例中,TiO2為較佳。當在用於纖維與膜之聚合物中使用時,TiO2之添加量較佳為至少約0.01重量百分比,並且較佳為至多3重量百分比,更佳為至多約2重量百分比(此係基於總組成物重量)。
本文中所用之術語「顏料」係指稱一般在該項技術領域中稱為顏料的那些物質。顏料通常為一乾粉形式之物質,其會賦予一聚合物或由該聚合物製成之物品(例中薄片或纖維)顏色。顏料可為無機或有機並且可為天然或合成。一般而言,顏料為惰性(亦即電中性並且不會與該聚合物反應)並且實質上不溶於其所添加的介質中,例如一聚對酞酸丙二酯組成物。然而,顏料可溶於或部分溶於某些材料中。
較佳為熔融混練該樹脂組分、該阻燃劑與任何其他添加劑。較佳的是,該樹脂組分與添加劑(包括阻燃劑)係混合並在一足以形成一熔融混練組成物的溫度下加熱。該組成物可紡成纖維或形成為其他形狀的物品,較佳為以一連續之方式。
該樹脂組分與添加劑可用熟悉該項技術領域者所知的各式不同方式形成為一混練之組成物。例如,它們可(a)同時加熱與混合、(b)在加熱前於一分開之裝置中預混合或(c)加熱然後混合。該混合、加熱與成形可用現有為此目的設計之設備(例如擠製機或Banbury混合器)進行。該溫度較佳為高於各組分之熔點但低於最低之分解溫度,並且可針對任何PTT與阻燃添加劑的特定組成而調整。該溫度典型為在約180℃至約270℃的範圍中。
阻燃化合物在該PTT基組成物中之用量較佳為0.1百分比至15重量百分比,此係基於總組成物重量。更佳的是,此量為約0.5至約10重量百分比,再更佳為約1至約6重量百分比,又更佳為約2至約6重量百分比,基於總PTT基組成物重量。
在某些實施例中亦提供包含該PTT組成物之物品如纖維、膜與模製零件,此類物品具有改良之阻燃性質。
該組成物可紡成纖維如蓬鬆連續絲(BCF)。此BCF可製成紗並形成為地毯。由該BCF紗製成的地毯可使用任何熟悉該項技術領域者已知的方式製得。典型為使一些紗纜撚在一起以形成一地毯紗並且在一裝置(如熱壓器)中熱定形。或者,可使用連續程序以賦予紗結構穩定性,該連續程序如使用一Suessen熱定形機之乾熱定形,或者如以一Superba熱壓器進行之蒸氣熱壓器熱定形。而後將紗簇絨成一基礎底布,亦稱為簇絨基材。
BCF可使用任何熟悉該項技術領域者已知的方法製成,例如揭露於美國專利第7013628號中者,其揭露由帶有一三角形截面(delta cross section)與具有一總丹尼數約1450丹尼及每絲丹尼數約20.8之纖維製成的BCF。其纖維強度在1.5至2.5克/丹尼的範圍中並且纖維伸長率在55至75百分比的範圍中。此纖維可具有各式截面形狀,取決於紗與由其製成之終端產品(例如地毯)的所欲性質。例如,該截面可為三角形、三葉形、圓形或其他一般用於商品中的形狀。由該纖維製成之紗的總丹尼數可在1000至3000的範圍中,並且每絲丹尼數(dpf)在12至30的範圍中。
在某些實施例(其中該PTT基組成物係用於製造纖維與該纖維係用於製造地毯)中,一黏著性材料(通常稱為該預塗料)係用於將該纖維結合至該簇絨基材。常見的預塗料為乳膠衍生或衍生自一熱熔黏著劑。該乳膠衍生之預塗料或熱熔黏著性預塗料含有一結合聚合性樹脂,並且亦可含有一填充劑如碳酸鈣。在某些情況下,該預塗料亦可含有添加劑如分散劑與/或增稠劑。
用於乳膠衍生預塗料之典型聚合性樹脂包括一聚合性組分如乙酸乙烯酯-乙烯(VAE)、苯乙烯-丁二烯橡膠(SBR)、聚氯乙烯(PVC)、聚酯、聚胺甲酸酯與聚烯烴,特別是聚丙烯。可使用現有熱熔黏著劑或其他非水性黏著劑如乙烯乙酸乙烯酯(EVA)、聚烯烴與聚乙烯作為預塗料,其有時用於取代乳膠以提供較乳膠黏著劑更強之結合。
在較佳實施例中,該預塗料含有一阻燃添加劑如三水合鋁(ATH)或氫氧化鎂(Mg(OH)2)。ATH為較佳。
在一乳膠衍生之預塗料中,在該預塗料中之阻燃添加劑用量部分取決於該結合聚合物或存在之聚合性組分的性質與數量以及預塗料用量,並且可在至多每百份預塗料中聚合性樹脂600份-(phr)的量中變化。(該預塗料中之聚合性組分係與本文中所揭露之組成物(包含PTT)的樹脂組分分別且分開)。使用之典型加料量可高達400 phr如1至400 phr。較佳的是,使用之加料量為每百份阻燃劑100至400份,並且更佳為100至300份。
針對一基於一熱熔黏著劑之預塗料,在該預塗料中之阻燃添加劑如ATH用量係基於黏著劑與填充劑如碳酸鈣之量,並且可在至多約35重量%,例如1至35重量%的量中變化。較佳的是,使用之加料量為1至25重量%的阻燃劑。更佳的是,使用10-25%的阻燃劑。
某些地毯除了該預塗料外尚包括一第二底布。該第二底布黏著至該預塗料並且為該地毯結構之部分,其接觸待鋪毯之表面。在某些應用中,該地毯具有一自黏且自鬆之黏性第二底布;在其他應用中,一黏合劑或膠水係用於該第二底布上。相較於衍生自乙烯基聚合物如PVC之第二底布,衍生自聚烯烴的第二底布典型為需要在該面纖維與預塗料中有較高的阻燃劑加料量。
已發現在該預塗料中之阻燃劑量可基於以下條件進行有利的調整,包括地毯中的面纖維重量,以及第二底布(若存在時)之基重與種類。「基重」為熟悉該項技術領域者已知之術語,並且用於指涉每單位面積(以平方碼計)的地毯、第二底布或預塗料重量(以盎司計)。因此,地毯或預塗料基重典型為以每平方碼盎司數來記述。面纖維係指可為觀察者所見之地毯纖維部分。該面纖維係主要以紗製成,並且這些紗可以修剪、纏繞、修剪與纏繞的方式來修整,或者以熟悉該項技術領域者已知的任何數目修整方式來修整。纖維面重亦典型為以如每平方碼盎司數之單位來記述。當在地毯通常涉及為闊幅地毯的情況下時,該第二底布可為一厚乳膠。或者,當在塊基地毯之情況下時,該第二底布可為烯烴或乙烯基衍生。該第二底布可含有如以玻璃纖維條子稀洋紗(scrim)分離之多個層,並且該多個層中之一個或多個可含有填充劑。
對於許多應用而言,理想為地毯符合ASTM 648E(輻射毯)測試的「第一級」標稱。然而,僅增加地毯纖維中的阻燃劑含量已發現會產生不一致的結果。再者,僅在預塗料中使用較高含量的阻燃劑只具有有限的效果,因為含量過高可對於預塗料之黏著性質產生不利影響,並且會導致簇絨基材從該第二底布上脫離。
已意外發現,當使用一含有ATH之預塗料製成地毯並且一額外阻燃劑存在於該地毯之面纖維時,特別是當該地毯之面纖維係由本文中所揭露之PTT基組成物製成時,可觀察到所得之阻燃性有所提昇(相較於單獨在纖維或預塗料中含有阻燃添加劑的地毯)。更具體而言,此類地毯在輻射板測試中的性能係較基於單獨在面纖維使用阻燃添加劑者為高,或較基於僅在預塗料中使用阻燃添加劑如ATH者為高。在某些實施例中,此提昇之程度係為其輻射板性能值係高以下情況所能達成之輻射板性能值的總合,即單獨在預塗料中含有阻燃劑與單獨在面纖維中含有阻燃劑。此結果使標稱為第一級之地毯塊得以生產。
在較佳實施例中,該地毯在纖維中含有2重量%或更低的阻燃劑,並且其地毯基重為28 oz/yd2或更低,並且在某些實施例中為24 oz/yd2或更低。
用於實例中之PTT為SORONA「半光」聚合物,其可得自E.I. du Pont de Nemours and Company(Wilmington,DE)。用於實例中之阻燃化合物如下表1所列示者。
測定輻射板測試之改善程度的方法,係生產含有阻燃添加劑之蓬鬆連續絲(BCF)以及生產含有該測試用BCF的地毯樣品。
生產各阻燃添加劑在PTT中之一25%濃縮物。將該25%濃縮物、PTT與一顏色顏料放置在三個分開的加料斗中。添加劑送料器(設計為輸送該三個分開加料斗中之內容物)係在纖維熔融紡絲期間,用來以適當之重量百分比混合該PTT、阻燃添加劑與顏色顏料,此係使用一典型之程序,如描述於美國專利第7013628號中者。
使BCF以每英吋4.75撚的撚度加撚,並且經Superba熱成形。而後將纖維簇絨成一每平方碼3.5盎司的非織基礎基材,此已知為Colback形式Colbond。簇絨設定為第13號錠距、0.18英吋絨毛高度,並且纖維面重係如表2所指示者變化。
用於作為一預塗料之乳膠黏著劑係得自BizMax Solutions Inc。該預塗料為VAE基並且含有ATH,其ATH含量在0至300 phr間變化以配合纖維重量。預塗料係以約25 oz/yard2之基重施用於地毯樣品上。
第二底布為一擠製級熱塑性聚烯烴TKP 882D TPO融合物(merge),其含有65重量%(基於TPO之重量)的碳酸鈣作為填充劑,此係得自LyondellBasell公司。將兩個擠製層(各約40 oz/sq yd並且其間有一2.1 oz/yard2的玻璃纖維)施用於該經預塗之基礎基材上。
生產地毯塊樣品並且依據ASTM 648E進行輻射板測試。測定其臨界輻射通量(CRF),並且纖維中不含阻燃添加劑之樣品的測定結果係列示於下表2。
輻射板測試結果係繪示於圖1。在0.45與0.55 watts/cm2的參考直線係結合於圖式中。前者為在輻射板測試中標稱為第一級者所預期的平均值。後者則為用於實務中的平均值,此係在考慮到測試的變異性下,此亦對於一地毯塊生產者提供一舒適餘裕。回歸線之斜率指示,具有較低纖維面重之地毯會在輻射板測試中表現較佳。增加預塗料中之ATH加料量亦提昇地毯塊在輻射板測試中之表現。
在不同加料量下纖維中含有阻燃添加劑OP950以及含有不同ATH加料量之預塗料下,地毯塊的CRF測試結果係示於表3。
圖2顯示在地毯面纖維中之OP950以及在地毯預塗料中之ATH對於地毯在輻射板測試中之性能所產生的影響。以上表1與2中之數據說明,在預塗料中包括ATH以及在地毯樣品之面纖維中包括OP-950所產生的有益效果。考慮對照實例1(在纖維中不含FR添加劑或在預塗料中不含ATH),其CRF為0.38 watts/cm2。在加入200 phr的ATH至預塗料中時(如見於對照實例6中者),會使CRF由0.38提高至0.48 watts/cm2,增加了0.1 CRF單位。請參照實例7,加入剛好2%的OP950至該面纖維中會讓CRF提高至0.44 watts/cm2,較對照實例1中所觀察到者增加了0.06 CRF單位。
若OP950在面纖維中與ATH在預塗料中之效果僅為簡單之加成性,則含有兩者之地毯塊的預期CRF會是0.38 watts/cm2+0.1watts/cm2+0.06 watts/cm2或0.54 watts/cm2。然而,出乎意料的是,實例13中所觀察到的輻射通量為0.63 watts/cm2。
如表4中可見者,若阻燃劑如MPP及MC與ATH一起使用在預塗料中,則亦可在輻射板測試中見到性能提昇。此外,當在預塗料中使用ATH時,MPP與MC之摻合物(實例23)、MPP與OP950之摻合物(實例24)以及MC與OP950之摻合物(實例25)亦大幅改善了地毯樣品之輻射板性能。各摻合物組分之相對重量百分比亦附帶列示於表中。圖3顯示各式阻燃添加劑與其CRF結果。
圖1顯示一臨界輻射通量(critical radiant flux)對地毯塊纖維面重之散佈圖,該地毯塊係使用本文中所揭露之聚對酞酸丙二酯基組成物製成。適配線圖顯示在纖維中不含有任何阻燃劑的情況下,在預塗料中之不同加料量ATH所產生的影響。
圖2顯示一臨界輻射通量對地毯塊纖維面重之散佈圖,該地毯塊係使用本文中所揭露之聚對酞酸丙二酯基組成物製成。適配線圖顯示纖維中含有阻燃添加劑以及預塗料中含有ATH時所產生的影響。
圖3顯示一臨界輻射通量對地毯塊纖維面重之散佈圖,該地毯塊係使用本文中所揭露之聚對酞酸丙二酯基組成物製成。適配線圖顯示纖維中含有阻燃添加劑以及預塗料中含有ATH時所產生的影響。
(無元件符號說明)
Claims (16)
- 一種聚對酞酸丙二酯基之組成物,其包含:(a)約75至約99.9重量百分比的一樹脂組分,此係基於總組成物重量,其中該樹脂組分包含至少約70重量百分比的一聚對酞酸丙二酯,此係基於該樹脂組分之重量;以及(b)約1至約6重量百分比的一三聚氰胺三聚氰酸鹽、三聚氰胺焦磷酸鹽、一二乙膦酸之鋅鹽或其摻合物,此係基於總組成物重量。
- 如請求項1所述之聚對酞酸丙二酯基組成物,其中該三聚氰胺三聚氰酸鹽為一非鹵化之三聚氰胺三聚氰酸鹽。
- 如請求項1所述之聚對酞酸丙二酯基組成物,其中該三聚氰胺三聚氰酸鹽與三聚氰胺焦磷酸鹽為粒狀,並且其平均粒徑係小於約10微米。
- 如請求項1所述之聚對酞酸丙二酯基組成物,其中該聚對酞酸丙二酯為一聚對酞酸丙二酯共聚物。
- 如請求項1所述之聚對酞酸丙二酯基組成物,其中該樹脂組分包含一第二聚合物。
- 如請求項5所述之聚對酞酸丙二酯基組成物,其中該第二聚合物係選自由下列所組成之群組:聚對酞酸乙二酯、聚對酞酸丁二酯與耐綸。
- 如請求項1所述之聚對酞酸丙二酯基組成物,其中該添加劑套組包含TiO2。
- 一種由如請求項1所述之聚對酞酸丙二酯基組成物製成的物品。
- 如請求項8所述之物品,其為纖維之形式。
- 一種由如請求項9所述之纖維製成的地毯。
- 一種包含面纖維與一預塗料之地毯,其中:該面纖維係由如請求項1所述之組成物製成,並且該預塗料含有一選自三水合鋁與氫氧化鎂之阻燃添加劑。
- 如請求項11所述之地毯,其中該預塗料為乳膠衍生並且含有400phr或更低之阻燃劑量,此係基於該預塗料中之樹脂組分總重量。
- 如請求項12所述之地毯,其中該阻燃劑為ATH。
- 如請求項11所述之地毯,其中該預塗料包含一熱熔黏著劑並且含有25重量%或更低之阻燃劑量,此係基於該預塗料中之樹脂組分總重量。
- 如請求項11所述之地毯,其中該預塗料為乳膠衍生並且含有為300phr或更低之阻燃劑三水合鋁量,此係基於該預塗料中之樹脂組分總重量,並且其中該地毯在纖維中含有2重量%或更低的二乙膦酸鋅鹽,其地毯基重為28oz/yd2或更低。
- 如請求項15所述之地毯,其中該地毯展現其輻射板性能值係高以下情況所能達成之輻射板性能值的總合,即單獨在預塗料中含有阻燃劑與單獨在面纖維中含有阻燃劑。
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JP5855647B2 (ja) | 2016-02-09 |
EP3290468A1 (en) | 2018-03-07 |
AU2011265686B2 (en) | 2015-01-15 |
EP2582756B1 (en) | 2018-03-28 |
MX2012014805A (es) | 2013-02-07 |
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