TWI625434B - 阻燃纖維、紗線及由其製得之織物 - Google Patents

阻燃纖維、紗線及由其製得之織物 Download PDF

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TWI625434B
TWI625434B TW100134435A TW100134435A TWI625434B TW I625434 B TWI625434 B TW I625434B TW 100134435 A TW100134435 A TW 100134435A TW 100134435 A TW100134435 A TW 100134435A TW I625434 B TWI625434 B TW I625434B
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Taiwan
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melamine
zinc
flame retardant
flame
fiber
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TW100134435A
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TW201229338A (en
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黛柏拉Ｍ 薩則提
Deborah M. Sarzotti
湯瑪斯Ｅ 史密特
Thomas E. Schmitt
安德魯Ｗ 布里基斯
Andrew W. Briggs
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英威達紡織(英國)有限公司
Invista Textiles (U.K.) Ltd.
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Publication of TW201229338A publication Critical patent/TW201229338A/zh
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    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/44—Yarns or threads characterised by the purpose for which they are designed
    • D02G3/443—Heat-resistant, fireproof or flame-retardant yarns or threads
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
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    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
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    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
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    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
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    • D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • D03D15/513—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads heat-resistant or fireproof
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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    • D04H1/4334—Polyamides
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    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
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    • D04H1/43835—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
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    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
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    • D04H3/009—Condensation or reaction polymers
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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    • D06M15/667—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain
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    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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    • D04H1/43832—Composite fibres side-by-side
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
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    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
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Abstract

本發明揭示用部分芳族聚醯胺及非鹵化阻燃添加劑製得之工業纖維及紗線。由此等纖維及紗線製得之織物顯示優於傳統阻燃耐綸6,6織物之阻燃性。另外，所揭示的纖維及紗線當與其他阻燃纖維摻合時不顯示阻燃耐綸6,6摻合織物所常見之危險的「支架效應(scaffolding effect)」。

Description

阻燃纖維、紗線及由其製得之織物
本發明大體上係關於工業纖維、紗線及織物，且特定言之係關於包含部分芳族聚醯胺及非鹵化阻燃添加劑之阻燃纖維、紗線及由其製得之織物。
阻燃(FR)織物在軍事環境與非軍事環境兩者中均至關重要。消防人員、賽車手及石油化學工作人員僅為受益於阻燃織物之附加保護作用的少數幾個非軍事群組。然而，阻燃織物之真正益處在於軍事。除吾人之軍隊必須應付之不期望的環境之外，非常規現代化戰爭之到來亦會產生甚至更不利之環境。詳言之，欲使大規模士兵護送隊喪失活動能力之簡易***裝置(improvised explosive device，「IED」)之使用使得個別軍隊保護極其重要。
除防彈織物及人體鎧甲之外，阻燃織物在保護士兵免遭IED方面發揮至關重要作用。IED由眾多材料(例如高***性裝藥、可燃液體、榴散彈等)構建，一些IED充當射彈(projectile)及其他IED充當引爆後之燃燒彈。因此，軍事織物必須具有不同構造以處理來自IED之大量威脅。
保護服中基本上使用兩種類型之阻燃織物：(1)由阻燃有機纖維(例如芳族聚醯胺、阻燃人造絲、聚苯并咪唑、改良丙烯酸纖維等)製得之織物；及(2)由已加以後處理來賦予阻燃性之習知材料(例如棉花)製得之阻燃織物。Nomex及Kevlar芳族聚醯胺尤其為最常見類型之阻燃合成纖維。此等纖維係藉由將間芳族聚醯胺或對芳族聚醯胺聚合物溶液紡絲(solution spinning)成纖維而製得。芳族聚醯胺在極熱下不熔融，為天然阻燃劑，但必須經溶液紡絲。令人遺憾的是，Nomex不十分舒適且其生產困難且昂貴。Kevlar之生產亦困難且昂貴。
後處理阻燃劑施用於織物且可分類成兩種基本類型：(1)耐久阻燃劑；及(2)不耐久阻燃劑。對於保護服，處理必須經得起洗熨，因此僅選擇耐久處理。當今，最通常之耐久阻燃劑化學依賴於磷基FR試劑及化學品或樹脂以將FR試劑固定在織物上。
一種已由於其可加工性及強度而經廣泛研究之聚合物纖維為耐綸6,6纖維。少量(約12%)脂族耐綸纖維可與棉花摻合且經化學處理以產生阻燃織物。因為棉花為主要纖維組分，所以此織物稱為「FR棉花」織物。耐綸纖維賦予FR棉花織物及衣服優越耐磨性。然而，因為耐綸可經熔融加工(亦即熱塑性)且不提供固有耐火性，所以FR織物中之耐綸纖維之量有限。嘗試化學改質脂族耐綸纖維及增加耐綸纖維含量同時仍達成足夠阻燃性尚未成功。實際上，Deopura及Alagirusamy在其最新書聚酯及聚醯胺(Polyesters and Polyamides)(The Textile Institute 2008，第320頁)中陳述「在用於...耐綸纖維之新穎及/或改良反應性阻燃共聚單體或習知...阻燃添加劑方面似乎不可能將會有任何較大突破」。
使用熱塑性纖維與非熔融耐火纖維(例如脂族聚醯胺與經FR處理之棉花)之摻合物之問題為所謂「支架效應」。(參見Horrocks等人，Fire Retardant Materials,第148頁,§ 4.5.2(2001))。一般而言，熱塑性纖維(包括經FR試劑處理或改質之熱塑性纖維)會在遠離火源時藉由收縮而自行熄滅或在當熔融聚合物在遠離火源時滴落且熄滅時而自行熄滅。FR聚酯纖維為具有此特性之纖維。當FR聚酯纖維與非熔融阻燃纖維，諸如經FR處理之棉花摻合時，非熔融纖維會形成含碳支架(「支架效應」)且熱塑性FR聚酯纖維束縛於火焰中並將繼續燃燒。實質上，在垂直可燃性測試期間，熱塑性纖維聚合物熔融且沿著非熱塑性稀紗布(scrim)行進並通往火焰且織物完全燃燒。另外，在衣服中，熔融聚合物可滴落且黏著於人類皮膚並對穿戴者產生額外損傷。
需要的是消除「支架效應」、提供良好阻燃性、防止滴落及黏著且耐磨之經改良阻燃耐綸摻合物。因此，需要找到可與阻燃添加劑一起摻合成某一纖維之熔融加工聚合物的組合，該纖維應可針織或編織或製備成非編織、自行熄滅、不滴落、耐磨/耐久之阻燃織物、棉絮(batting)或衣服。
本文揭示之本發明提供一種由經熔融加工之聚醯胺及非鹵素阻燃添加劑製得之阻燃織物。令人驚奇地，發現部分芳族聚醯胺在與阻燃添加劑摻合時可熔融加工成阻燃性優於與相同阻燃劑摻合時之脂族聚醯胺(例如耐綸6,6)之纖維。此結果出乎意料，因為與「支架效應」及不良阻燃性相關之部分芳族聚醯胺具有熱塑性(亦即在加熱後熔融)。
在一態樣中，揭示一種包含部分芳族聚醯胺及非鹵素阻燃劑之阻燃纖維。部分芳族聚醯胺可包含芳族二胺單體及脂族二酸單體。此外，部分芳族聚醯胺可包含芳族及脂族二胺及二酸之聚合物或共聚物，包括MXD6。舉例而言，MXD6係指由間二甲苯二胺(MXDA)及己二酸產生之聚醯胺。
在另一態樣中，揭示用揭示之阻燃纖維製得之阻燃紗線及織物。紗線亦可包含其他天然或合成纖維，包括連續長絲纖維及短纖維。其他纖維可為固有阻燃纖維或經阻燃劑處理。織物亦可包含其他天然紗線、合成紗線或兩者之摻合物。其他紗線可經阻燃劑處理或含有經阻燃劑處理之纖維。織物可經染色且具有所施用之其他阻燃及非阻燃整理劑。
術語「耐火」、「阻燃」及「FR」在此項技術中具有細微差異。該等術語在用法方面之差異涉及描述在諸如垂直火焰測試之條件下抵抗燃燒、以較慢速率燃燒及能夠自行熄滅之織物。出於本發明之目的，術語「耐火」及「阻燃」可互換使用且意欲包括具有一或多種所要性質，諸如抗燃燒性、緩慢燃燒性、自行熄滅性等之任何織物。
揭示一種包含部分芳族聚醯胺及非鹵素阻燃添加劑之阻燃纖維。部分芳族聚醯胺可包括的聚合物或共聚物包括選自由以下組成之群之單體：芳族二胺單體、脂族二胺單體、芳族二酸單體、脂族二酸單體及其組合。部分芳族聚醯胺亦可包括或僅為包括芳族二胺及非芳族二酸之MXD6。其他部分芳族聚醯胺可基於芳族二酸，諸如對苯二甲酸(聚醯胺6T)或間苯二甲酸(聚醯胺6I)或其摻合物(聚醯胺6T/6I)。部分芳族聚醯胺之熔融或加工溫度在約240℃(對於MXD6)至約355℃(對於聚醯胺醯亞胺)之範圍內，包括約260℃、280℃、300℃、320℃及340℃。耐綸6及耐綸6,6之熔融溫度分別為約220℃及260℃。熔融溫度愈低，聚醯胺聚合物愈容易加工成纖維。以下為常見部分芳族聚合物及某些比較性非芳族物及其相關熔融溫度之清單。
部分芳族聚醯胺亦可包括多種部分芳族醯胺之共聚物或混合物。舉例而言，MXD6可在形成纖維之前與耐綸6/6T摻合。此外，部分芳族聚合物可與脂族聚醯胺或多種脂族聚醯胺之共聚物或混合物摻合。舉例而言，MXD6可在形成纖維之前與耐綸6,6摻合。
非鹵素阻燃添加劑可包括：三聚氰胺之縮合產物(包括蜜白胺(melam)、蜜勒胺(melem)及聚蜜勒亞胺(melon))；三聚氰胺與磷酸之反應產物(包括磷酸三聚氰胺、焦磷酸三聚氰胺及聚磷酸三聚氰胺(MPP))；三聚氰胺之縮合產物與磷酸之反應產物(包括聚磷酸蜜白胺、聚磷酸蜜勒胺、聚磷酸聚蜜勒亞胺)；氰尿酸三聚氰胺(MC)；二乙基次膦酸鋅(DEPZn)；二乙基次膦酸鋁(DEPAl)；二乙基次膦酸鈣；二乙基次膦酸鎂；雙酚A雙(次膦酸二苯酯)(BPADP)；間苯二酚雙(磷酸2,6-二(二甲苯)酯)(RDX)；間苯二酚雙(磷酸二苯酯)(RDP)；氮氧化磷；硼酸鋅；氧化鋅；錫酸鋅；羥基錫酸鋅；硫化鋅；磷酸鋅；矽酸鋅；氫氧化鋅；碳酸鋅；硬脂酸鋅；硬脂酸鎂；八鉬酸銨；鉬酸三聚氰胺；八鉬酸三聚氰胺；偏硼酸鋇；二茂鐵；磷酸硼；硼酸硼；氫氧化鎂；硼酸鎂；氫氧化鋁；三水合氧化鋁；甘脲及3-胺基-1,2,4-***-5-硫醇之三聚氰胺鹽；鉀、鋅及鐵之脲唑鹽；1,2-乙烷二基-4-4'-雙-***啶-3,5,二酮；聚矽氧；Mg、Al、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Mo、Sn、Sb、Ba、W及Bi之氧化物；多面寡聚倍半氧矽烷；矽鎢酸(SiTA)；磷鎢酸；鎢酸之三聚氰胺鹽；直鏈、分支鏈或環狀磷酸酯或膦酸酯；螺雙膦酸酯；螺雙磷酸酯及奈米粒子，諸如碳奈米管及奈米黏土(包括(但不限於)基於蒙脫石(montmorillonite)、敘永石(halloysite)及合成鋰皂石(laponite)之奈米黏土)。
阻燃添加劑以約1%至約25% w/w，包括約5%至約20% w/w、約5%至約10%、及約10%之量存在。阻燃添加劑之平均粒徑小於約3微米，包括小於約2微米及小於約1微米。
阻燃添加劑之粒徑可藉由研磨製程製備，該製程包含噴氣研磨各組分或共研磨組分之摻合物以降低粒徑。此項技術中已知之其他濕磨或乾磨技術(例如介質研磨)亦可用於降低添加劑粒徑以進行纖維紡絲。適當時，研磨可涉及在研磨製程中之任何適合點，可能在壓力下將液體研磨助劑注射入研磨機中。添加此等液體助劑以使阻燃系統穩定及/或防止黏聚。有助於粒子潤濕及/或防止再黏聚之其他組分亦可在研磨阻燃添加劑、摻合阻燃添加劑與聚合物、及/或纖維紡絲製程期間之任何適合點經添加。
阻燃劑可在擠壓機中與聚合材料混配。一種替代性方法涉及在濃度高於最終聚醯胺纖維產物中所要之濃度下將阻燃組合物分散於聚合物中，且形成母體混合物。母體混合物可經研磨或粒化且所得顆粒與其他聚醯胺樹脂乾式摻合且此摻合物用於纖維紡絲製程中。另一替代性方法涉及在聚合製程之適合點向聚合物中添加阻燃添加劑中之一些或所有組分。
阻燃纖維可為短纖維或連續長絲。阻燃纖維亦可含於非編織織物，諸如紡黏(spun bond)織物、熔噴(melt blown)織物或其組合中。長絲橫截面可為任何形狀，包括圓形、三角形、星形、方形、橢圓形、雙葉形、三葉形或扁平形。另外，可使用已知締鬈加工法使長絲締鬈。如上所論述，紡成纖維之部分芳族聚醯胺亦可包括其他部分芳族或脂族聚合物。當紡絲此等纖維時，一種以上聚醯胺聚合物之混合物可在紡成紗線之前加以摻合或可以諸如並排組態或芯鞘組態之雙組分形式產生含有至少一種部分芳族聚醯胺聚合物及另一部分芳族聚醯胺聚合物或脂族聚合物之複絲紗。
阻燃短纖維可紡成阻燃紗線。該紗線可包含100%阻燃纖維，或可為與其他短纖維(阻燃短纖維與非阻燃短纖維兩者)之摻合物以製得短纖維加撚紗線。其他纖維可包括棉花、羊毛、亞麻、***、絲、耐綸、溶解性纖維素(lyocell)、聚酯及人造絲。以上短纖維加撚紗線亦可包含其他熱塑性或非熱塑性纖維，諸如纖維素纖維、芳族聚醯胺纖維、酚醛(novoloid)纖維、酚樹脂(phenolic)纖維、聚酯纖維、氧化丙烯酸纖維、改良丙烯酸纖維、三聚氰胺纖維、聚(對伸苯基苯并雙噁唑)(PBO)纖維、聚苯并咪唑(PBI)纖維或聚磺醯胺(PSA)纖維、氧化聚丙烯腈(PAN)纖維(諸如部分氧化PAN)及其摻合物。如本文所用，纖維素包括棉花、人造絲及溶解性纖維素。熱塑性/非熱塑性纖維可為阻燃纖維。諸如芳族聚醯胺、PBI或PBO之某些纖維在火焰暴露之後維持強度，且當用於摻合紗線及織物中時有效降低可燃性測試之後的織物燒焦長度。
包含用揭示之阻燃纖維製得之阻燃紗線的織物在織物垂直可燃性測試(ASTM D6413)中將自行熄滅。在用100%之揭示之阻燃纖維製得的織物中或在如上揭示之阻燃纖維與切斷紡絲纖維的摻合物中達成自行熄滅特性。用揭示之阻燃紗線製得之織物亦可包括其他紗線，諸如纖維素纖維、芳族聚醯胺纖維、酚樹脂纖維、聚酯纖維、氧化丙烯酸纖維、改良丙烯酸纖維、三聚氰胺纖維、棉花纖維、絲纖維、亞麻纖維、***纖維、羊毛纖維、人造絲纖維、溶解性纖維素纖維、聚(對伸苯基苯并雙噁唑)(PBO)纖維、聚苯并咪唑(PBI)纖維及聚磺醯胺(PSA)纖維、部分氧化丙烯酸(包括部分氧化聚丙烯腈)纖維、酚醛纖維、羊毛纖維、亞麻纖維、***纖維、絲纖維、耐綸(無論FR或非FR)纖維、聚酯(無論FR或非FR)纖維、抗靜電纖維及其組合。織物可用其他阻燃添加劑及必要時整理劑處理。一種處理棉花之例示性方法可見於由Cotton Incorporated,Cary,North Carolina發表之技術通報『Fabric Flame Retardant Treatment』(2003)中，該通報以全文引用的方式併入本文中。織物可為編織、針織及非編織織物。非編織織物包括由梳棉網(carded web)、濕式佈層(wet-lay)或紡黏/熔噴製程製得之織物。
纖維、紗線及織物亦可含有其他組分，諸如：紫外穩定劑、抗微生物劑、漂白劑、光學增亮劑、抗氧化劑、顏料、染料、拒汙劑(soil repellant)、防污劑(stain repellant)、奈米粒子及防水劑。紫外穩定劑、抗微生物劑、光學增亮劑、抗氧化劑、奈米粒子及顏料可在熔融紡絲之前添加至阻燃纖維中或在纖維形成之後作為後處理劑添加。染料、拒汙劑、防污劑、奈米粒子及防水劑可在纖維及/或織物形成之後作為後處理劑添加。對於紗線及織物，可添加其他組分作為後處理劑。用揭示之阻燃纖維製得之織物亦可具有用於達成耐磨性或控制液體/蒸氣滲透之塗層或層壓薄膜。
如圖1a-1h中所示，相較於用習知耐綸6,6阻燃纖維製得之模製層壓片，用所揭示之阻燃聚合物製得之模製層壓片展示優越阻燃性(如使用ASTM D-6413所量測)。
圖2為與阻燃熱塑性及非熱塑性纖維相關之支架效應之圖解說明。圖3a-3d比較用所揭示之阻燃纖維及阻燃人造絲製得之織物與用耐綸6,6阻燃纖維及阻燃人造絲製得之織物。此處，用所揭示之阻燃纖維製得之織物(圖3b及3d)不遭受支架問題，而耐綸6,6織物(圖3a及3c)遭受。圖4展示在各種濃度之各種阻燃添加劑之情況下，耐綸6,6及MXD6聚合物之垂直可燃性資料。該圖展示使用MXD6超過耐綸6,6之出乎意料之優點。
定義：
餘焰(after flame)意謂：「在已移除燃燒源之後材料持續燃燒。」[來源：ATSM D6413織物耐火性標準測試方法(垂直方法)(Standard test Method for Flame Resistance of Textiles(Vertical Method))]。
燒焦長度(char length)意謂：「在已施加規定撕力之後，直接暴露於火焰之織物邊緣至可見織物損傷之最遠處的距離。」[來源：ATSM D6413織物耐火性標準測試方法(垂直方法)]。
滴落(drip)意謂：「缺乏足夠數量或壓力以形成連續流之液體流動。」[來源：全國防火協會(National Fire Protection Association，NFPA)標準2112，關於用於保護工業人員對抗急驟燃燒之耐火衣服的標準(Standard on Flame-Resistant Garments for Protection of Industrial Personnel Against Flash Fire)]。
熔融(melt)意謂：『材料對熱所起之產生流動或滴落跡象之反應。』[來源：全國防火協會(NFPA)標準2112，關於用於保護工業人員對抗急驟燃燒之耐火衣服的標準]。
自行熄滅(self extinguishing)意謂：材料在燃燒源移除之後將不持續燃燒或燃燒將在試樣完全燒毀之前停止。由ATSM D6413織物耐火性標準測試方法(垂直方法)測試。
測試方法：
根據ASTM D-6413織物耐火性標準測試方法(垂直測試)測定阻燃性。
製備擠壓模製層壓片：聚合物與或不與FR添加劑一起擠壓模製成尺寸約10 cm×10 cm且稱重約10公克之薄膜。在模製之前，將編織玻璃纖維稀紗布置放在聚合物混合物之上及之下。玻璃纖維稀紗布防止聚合物在垂直可燃性測試期間遠離火焰而收縮或熔融且可預測「支架效應」之可能存在性。稀紗布之重量為最終層壓片之約7%。模製溫度為聚合物熔融溫度以上約攝氏25度。
實例
實例1-7：用所揭示之阻燃纖維之各種態樣製得之模製層壓片之阻燃性。
使用以上技術製備測試層壓片。實例1係用MXD6且在無阻燃添加劑之情況下製得。實例2係用MXD6及10% w/w MPP(聚磷酸三聚氰胺)添加劑製得。實例3係用MXD6及10% w/w MC(氰尿酸三聚氰胺)添加劑製得。實例4係用MXD6及10% w/w DEPZn(二乙基次膦酸鋅)添加劑製得。實例5係用MXD6及10% w/w DEPAl(二乙基次膦酸鋁)製得。實例6係用MXD6及2% w/w SiTA(矽鎢酸)製得。實例7係用MXD6及20% w/w MC添加劑製得。結果報導於下表1中。
比較實例1-4：用耐綸6,6及阻燃添加劑製得之模製層壓片之阻燃性。
使用以上技術製備測試層壓片。比較實例1係用耐綸6,6且在無阻燃添加劑之情況下製得。比較實例2係用耐綸6,6及10% w/w MPP添加劑製得。比較實例3係用耐綸6,6及10% w/w MC添加劑製得。比較實例4係用耐綸6,6及10% w/w DEPZn添加劑製得。比較實例5係用耐綸6,6且在無阻燃添加劑之情況下製得。結果報導於下表1中。
如以上表1中所示，所揭示之阻燃層壓片自行熄滅且相較於耐綸6,6對應物具有較短餘焰時間(after flame time)。另外，所揭示之阻燃層壓片亦不產生燃燒滴落，此為任何阻燃織物之所要特性。因為基於MXD6與耐綸6,6之聚合物兩者均可熔融加工，所以用以上MXD6聚合物獲得之結果為驚人且出乎意料的。
實例8-18：用所揭示之阻燃纖維及阻燃人造絲製得之織物之阻燃性。在以下實例中，阻燃熱塑性紗線與切斷FR人造絲紡紗(Lenzing FR)組合且針織成管狀織物。摻合織物含有約50%之各紗線。在可燃性測試之前自織物移除纖維整理劑及針織油。
實例8為含有2% w/w MPP添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例9為含有5% w/w MPP添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例10為含有10% w/w MPP添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例11為含有2% w/w DEPAl添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例12為含有5% w/w DEPAl添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例13為含有10% w/w DEPAl添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例14為含有5% w/w DEPZn添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。實例15為含有10% w/w DEPZn添加劑之阻燃MXD6纖維與阻燃人造絲纖維之織物摻合物。結果報導於下表2中。
比較實例6-8：用耐綸6,6阻燃纖維及阻燃人造絲製得之織物之阻燃性。
比較實例6為含有5% w/w MPP添加劑之阻燃耐綸6,6纖維與阻燃人造絲纖維之織物摻合物。比較實例7為含有10% w/w MPP添加劑之阻燃耐綸6,6纖維與阻燃人造絲纖維之織物摻合物。比較實例8為含有10% w/w DEPAl添加劑之阻燃耐綸6,6與阻燃人造絲纖維之織物摻合物。結果報導於下表2中。
此處，MXD6與阻燃人造絲纖維之摻合物展示優於耐綸6,6與阻燃人造絲纖維之比較摻合物的結果。如上所論述，此等結果為驚人且出乎意料的。
儘管本發明已結合其特定態樣加以描述，但顯然許多替代、修改及變化將為熟習此項技術者根據先前描述而顯而易知。因此，本發明意欲包括屬於申請專利範圍之精神及範疇之所有此等替代、修改及變化。
圖1a-1h展示所揭示之阻燃聚合物及習知耐綸6,6阻燃聚合物之各種態樣的阻燃性。
圖2展示支架效應問題。
圖3a-3d展示當與阻燃人造絲摻合時之所揭示織物，及與阻燃人造絲摻合之耐綸6,6阻燃劑之2個態樣的阻燃性。
圖4比較在多種添加劑之情況下，MXD6相對於耐綸6,6之餘焰時間。

Claims (23)

  1. 一種包含至少一種纖維之阻燃織物，其中該纖維包含部分芳族聚醯胺及非鹵素阻燃添加劑，且另外其中該織物能夠在垂直可燃性測試中自行熄滅。
  2. 如請求項1之阻燃織物，其中該部分芳族聚醯胺包含芳族及脂族二胺及二酸之聚合物或共聚物。
  3. 如請求項2之阻燃織物，其中該部分芳族聚醯胺另外包含芳族二胺單體及脂族二酸單體。
  4. 如請求項1之阻燃織物，其中該部分芳族聚醯胺為MXD6。
  5. 如請求項1之阻燃織物，其中該等非鹵素阻燃添加劑係選自由以下組成之群：三聚氰胺之縮合產物(包括蜜白胺(melam)、蜜勒胺(melem)及聚蜜勒亞胺(melon))；三聚氰胺與磷酸之反應產物(包括磷酸三聚氰胺、焦磷酸三聚氰胺及聚磷酸三聚氰胺(MPP))；三聚氰胺之縮合產物與磷酸之反應產物(包括聚磷酸蜜白胺、聚磷酸蜜勒胺、聚磷酸聚蜜勒亞胺)；氰尿酸三聚氰胺(MC)；二乙基次膦酸鋅(DEPZn)；二乙基次膦酸鋁(DEPAl)；二乙基次膦酸鈣；二乙基次膦酸鎂；雙酚A雙(次膦酸二苯酯)(BPADP)；間苯二酚雙(磷酸2,6-二(二甲苯)酯)(RDX)；間苯二酚雙(磷酸二苯酯)(RDP)；氮氧化磷；硼酸鋅；氧化鋅；錫酸鋅；羥基錫酸鋅；硫化鋅；磷酸鋅；矽酸鋅；氫氧化鋅；碳酸鋅；硬脂酸鋅；硬脂酸鎂；八鉬酸銨；鉬酸三聚氰胺；八鉬酸三聚氰胺；偏硼酸鋇；二茂鐵；磷酸硼；硼酸硼；氫氧化鎂；硼酸鎂；氫氧化鋁；三水合氧化鋁；甘脲及3-胺基-1,2,4-***-5-硫醇之三聚氰胺鹽；鉀、鋅及鐵之脲唑鹽；1,2-乙烷二基-4-4'-雙-***啶-3,5，二酮；聚矽氧；Mg、Al、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Mo、Sn、Sb、Ba、W及Bi之氧化物；多面寡聚倍半氧矽烷；碳奈米管；奈米黏土；矽鎢酸(SiTA)；磷鎢酸；鎢酸之三聚氰胺鹽；直鏈、分支鏈或環狀磷酸酯或膦酸酯；螺雙膦酸酯；螺雙磷酸酯及其組合。
  6. 如請求項1之阻燃織物，其中該非鹵素阻燃添加劑係選自由以下組成之群：MPP、MC、DEPZn、DEPAl及其組合。
  7. 如請求項1至6中任一項之阻燃織物，其中該非鹵素阻燃添加劑係以約5重量%至約10重量%之濃度存在。
  8. 一種包含至少一種纖維之阻燃織物，其中該纖維包含部分芳族聚醯胺及非鹵素阻燃添加劑，且另外其中該織物能夠在垂直可燃性測試中具有小於約60秒之餘焰時間。
  9. 如請求項8之阻燃織物，其中該部分芳族聚醯胺包含芳族及脂族二胺及二酸之聚合物或共聚物。
  10. 如請求項9之阻燃織物，其中該部分芳族聚醯胺另外包含芳族二胺單體及脂族二酸單體。
  11. 如請求項8之阻燃織物，其中該部分芳族聚醯胺為MXD6。
  12. 如請求項8之阻燃織物，其中該等非鹵素阻燃添加劑係選自由以下組成之群：三聚氰胺之縮合產物(包括蜜白胺(melam)、蜜勒胺(melem)及聚蜜勒亞胺(melon))；三聚氰胺與磷酸之反應產物(包括磷酸三聚氰胺、焦磷酸三聚氰胺及聚磷酸三聚氰胺(MPP))；三聚氰胺之縮合產物與磷酸之反應產物(包括聚磷酸蜜白胺、聚磷酸蜜勒胺、聚磷酸聚蜜勒亞胺)；氰尿酸三聚氰胺(MC)；二乙基次膦酸鋅(DEPZn)；二乙基次膦酸鋁(DEPAl)；二乙基次膦酸鈣；二乙基次膦酸鎂；雙酚A雙(次膦酸二苯酯)(BPADP)；間苯二酚雙(磷酸2,6-二(二甲苯)酯)(RDX)；間苯二酚雙(磷酸二苯酯)(RDP)；氮氧化磷；硼酸鋅；氧化鋅；錫酸鋅；羥基錫酸鋅；硫化鋅；磷酸鋅；矽酸鋅；氫氧化鋅；碳酸鋅；硬脂酸鋅；硬脂酸鎂；八鉬酸銨；鉬酸三聚氰胺；八鉬酸三聚氰胺；偏硼酸鋇；二茂鐵；磷酸硼；硼酸硼；氫氧化鎂；硼酸鎂；氫氧化鋁；三水合氧化鋁；甘脲及3-胺基-1,2,4-***-5-硫醇之三聚氰胺鹽；鉀、鋅及鐵之脲唑鹽；1,2-乙烷二基-4-4'-雙-***啶-3,5，二酮；聚矽氧；Mg、Al、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Mo、Sn、Sb、Ba、W及Bi之氧化物；多面寡聚倍半氧矽烷；碳奈米管；奈米黏土；矽鎢酸(SiTA)；磷鎢酸；鎢酸之三聚氰胺鹽；直鏈、分支鏈或環狀磷酸酯或膦酸酯；螺雙膦酸酯；螺雙磷酸酯及其組合。
  13. 如請求項8之阻燃織物，其中該非鹵素阻燃添加劑係選自由以下組成之群：MPP、MC、DEPZn、DEPAl及其組合。
  14. 如請求項8至13中任一項之阻燃織物，其中該非鹵素阻燃添加劑係以約5重量%至約10重量%之濃度存在。
  15. 一種阻燃纖維，其包含至少一種部分芳族聚醯胺、至少一種脂族聚醯胺及至少一種非鹵素阻燃添加劑。
  16. 如請求項15之阻燃纖維，其另外包含第二部分芳族聚醯胺。
  17. 如請求項16之阻燃纖維，其中該至少一種部分芳族聚醯胺為MXD6且該第二部分芳族聚醯胺為耐綸6/6T。
  18. 如請求項15之阻燃纖維，其中該至少一種部分芳族聚醯胺包含芳族及脂族二胺及二酸之聚合物或共聚物。
  19. 如請求項18之阻燃纖維，其中該至少一種部分芳族聚醯胺另外包含芳族二胺單體及脂族二酸單體。
  20. 如請求項15之阻燃纖維，其中該至少一種部分芳族聚醯胺為MXD6。
  21. 如請求項15之阻燃纖維，其中該等非鹵素阻燃添加劑係選自由以下組成之群：三聚氰胺之縮合產物(包括蜜白胺(melam)、蜜勒胺(melem)及聚蜜勒亞胺(melon))；三聚氰胺與磷酸之反應產物(包括磷酸三聚氰胺、焦磷酸三聚氰胺及聚磷酸三聚氰胺(MPP))；三聚氰胺之縮合產物與磷酸之反應產物(包括聚磷酸蜜白胺、聚磷酸蜜勒胺、聚磷酸聚蜜勒亞胺)；氰尿酸三聚氰胺(MC)；二乙基次膦酸鋅(DEPZn)；二乙基次膦酸鋁(DEPAl)；二乙基次膦酸鈣；二乙基次膦酸鎂；雙酚A雙(次膦酸二苯酯)(BPADP)；間苯二酚雙(磷酸2,6-二(二甲苯)酯)(RDX)；間苯二酚雙(磷酸二苯酯)(RDP)；氮氧化磷；硼酸鋅；氧化鋅；錫酸鋅；羥基錫酸鋅；硫化鋅；磷酸鋅；矽酸鋅；氫氧化鋅；碳酸鋅；硬脂酸鋅；硬脂酸鎂；八鉬酸銨；鉬酸三聚氰胺；八鉬酸三聚氰胺；偏硼酸鋇；二茂鐵；磷酸硼；硼酸硼；氫氧化鎂；硼酸鎂；氫氧化鋁；三水合氧化鋁；甘脲及3-胺基-1,2,4-***-5-硫醇之三聚氰胺鹽；鉀、鋅及鐵之脲唑鹽；1,2-乙烷二基-4-4'-雙-***啶-3,5，二酮；聚矽氧；Mg、Al、Ti、Cr、Mn、Fe、Co、Ni、Cu、Zn、Zr、Mo、Sn、Sb、Ba、W及Bi之氧化物；多面寡聚倍半氧矽烷；碳奈米管；奈米黏土；矽鎢酸(SiTA)；磷鎢酸；鎢酸之三聚氰胺鹽；直鏈、分支鏈或環狀磷酸酯或膦酸酯；螺雙膦酸酯；螺雙磷酸酯及其組合。
  22. 如請求項15之阻燃纖維，其中該非鹵素阻燃添加劑係選自由以下組成之群：MPP、MC、DEPZn、DEPAl及其組合。
  23. 如請求項15至22中任一項之阻燃纖維，其中該非鹵素阻燃添加劑係以約5重量%至約10重量%之濃度存在。
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