CN106884212B - 一种阻燃维纶纤维及其制备方法 - Google Patents
一种阻燃维纶纤维及其制备方法 Download PDFInfo
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/34—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated alcohols, acetals or ketals as the major constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
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Abstract
本发明公开了一种阻燃维纶纤维及其制备方法，阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，所述阻燃整理剂为表面改性无机阻燃剂，该阻燃维纶纤维及其制备步骤如下：1)维纶纺丝原液的准备：2)纺丝：3)后处理。本发明将表面改性无机阻燃剂粉末粘附至维纶纺丝原液的表面，并与维纶纺丝原液表层的聚乙烯醇进行快速混合，随着维纶纺丝原液固化成型以及缩甲醛处理，表面改性无机阻燃剂在维纶纤维的表层得到固定，形成一种具有皮芯结构的阻燃维纶纤维，具有良好的阻燃效果。
Description
技术领域
本发明属于化学纤维技术领域，尤其是涉及一种阻燃维纶纤维及其制备方法。
背景技术
维纶是聚乙烯醇缩醛纤维的商品名称，也叫维尼纶。其性能接近棉花，有“合成棉花”之称，是现有合成纤维中吸湿性最大的品种。在各类阻燃纤维中，阻燃维纶因其兼具高强度、阻燃和吸湿性好等优异性能，受到业内外广泛关注。“维纶纤维是由PVA的水溶液经湿法纺丝，再和甲醛缩合而制成的一种合成纤维。”
阻燃维纶纤维的制备主要有两种方法，即为接枝共聚和机械混合。接枝共聚是将具有阻燃能力的单体接入到聚乙烯醇的大分子中；机械混合则是在纺织原液中加入阻燃剂。在以上的两种方法所制备的阻燃维纶纤维为均相的混合，为了获得较好的阻燃效果往往需要接入或共混较多的阻燃剂，较大的阻燃剂用量会对纺丝工艺以及纤维的机械性能产生较大的影响。在纤维的燃烧过程中，纤维表层首先受到热的作用，若在纤维的表层分布有较多、稳定性良好的且具有较好的阻燃效果的单体或阻燃剂，即在纤维中阻燃剂是一种非均相的分布则可以阻止燃烧的蔓延。可以认为提高阻燃纤维表层的阻燃剂分布与用量则将有助于提高纤维的阻燃性能，也可以减少阻燃剂的用量。当前，对于阻燃剂非均相分布的阻燃维纶纤维开发较缺乏。
发明内容
为克服采用均相混合制备阻燃维纶纤维存在阻燃剂用量大，对纤维的机械性能影响较大的问题，本发明提供一种阻燃维纶纤维及其制备方法。
本发明是通过以下技术实现的：
一种阻燃维纶纤维，所述阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，所述阻燃整理剂为表面改性无机阻燃剂。
优选地，所述表面改性无机阻燃剂的制备步骤如下：将无机阻燃剂改性液于超声波条件下处理60～120min后得粘稠膏状物，将所得粘稠膏状物经干燥、粉碎得中心粒径为0.01～0.1μm的表面改性无机阻燃剂。
优选地，所述无机阻燃剂改性液的原料重量百分配比为：油酸10～15份、硬酯酸10～15份、蓖麻油酸钙15～30份、硬酯酸钙15～30份、三聚氯氰1～5份、无机阻燃剂60～80份。
优选地，所述无机阻燃剂三氧化二锑、氢氧化镁和氢氧化铝中的一种或几种。
优选地，超声波的功率为250～350W，频率为40KHz。
阻燃剂的选择与使用对阻燃维纶的制备至关重要。在常用的阻燃剂中，卤系、磷系阻燃剂以其阻燃效果好、不影响材料物化性能而得到广泛的应用。然而，卤系、磷系阻燃剂最为重要的缺点为聚合物在燃烧时发烟量大、易放出腐蚀性气体和有害性气体，容易造成二次危害，虽可达到阻燃作用，但所释放的气体将对人体产生重大的伤害。因此，以三氧化二锑、氢氧化铝、氢氧化镁为代表的无机阻燃剂在应用时是依靠化学分解吸热以及释放出水而起到阻燃作用的，以其无毒性、不腐蚀、分解后生成产物化学性质稳定，不会产生二次危害。三氧化二锑、氢氧化铝、氢氧化镁等无机阻燃剂直接与纺丝进行混合，虽可以达到阻燃，但其用量较大，分散效果欠佳。
在本发明中，发明人对三氧化二锑、氢氧化铝、氢氧化镁等无机阻燃剂进行表面改性，使表面有机化，大大提高了与聚乙烯醇的相容性，在提高维纶纤维阻燃性能的同时，也对维纶的力学性能有了明显的改善，对于提高维纶的综合性能具有重要的意义。在对三氧化二锑、氢氧化铝、氢氧化镁等无机阻燃剂进行表面改性时，超声波对改性的顺利进行至关重要。
一种阻燃维纶纤维的制备方法，制备步骤如下：
1)维纶纺丝原液的准备：将经过水洗后的聚乙烯醇溶于80～95℃水中，得到维纶纺丝原液(1)；
2)纺丝：由计量泵输出的维纶纺丝原液(1)经喷丝板(2)喷出后，进入纺丝甬道(3)，携带有表面改性无机阻燃剂的工业氮气由入风口(4)进入纺丝甬道(3)，由出风口(5)吹出，由纺丝甬道(3)而出的维纶纺丝原液(1)被引入凝固浴(6)中固化成型，即得聚乙烯醇纤维；
3)后处理：聚乙烯醇纤维经导丝辊(7)、热压辊(8)、缩甲醛处理浴(9)、水洗浴(10)、干燥辊(11)，收集得到阻燃维纶纤维(12)。
优选地，所述维纶纺丝原液(1)中聚乙烯醇的重量百分比浓度为18～22％。
优选地，所述工业氮气中表面改性无机阻燃剂的浓度为500～2000mg/L，通气量为0.1～0.3m3/min；所述热压辊(8)的温度为100～120℃，压力为0.5～1.0MPa。
优选地，所述凝固浴(6)为浓度420～450g/L的硫酸钠；所述缩甲醛处理浴(9)包括50～70g/L甲醛，230～240g/L硫酸、70～80g/L硫酸钠。
优选地，所述纺丝甬道(3)为圆柱形，长度为25～35cm，直径为20～40cm；所述入风口(4)顶端低于喷丝板(2)出丝口水平位置1～3cm，所述出风口(5)底端高于纺丝甬道(3)最低端1～3cm。
传统利用湿法纺丝设备制备得的维纶为腰圆形的皮芯结构，其组分相同。在本发明中，发明人设计将表面改性无机阻燃剂与维纶纺丝原液表层的聚乙烯醇进行混合，越到纤维表面，表面改性无机阻燃剂的浓度越高。本发明所采用的无机阻燃剂表面经过了有机化改性，与聚乙烯醇混合效果良好。本发明所制得的维纶纤维表层虽掺有表面改性无机阻燃剂，但其主体仍为聚乙烯醇，故维纶纤维表层性能与芯层聚乙烯醇相似，受外力的响应也相似，缩甲醛处理后也相似。与传统的无机阻燃剂在共混纺丝的均匀分散不同，本发明着重于将表面改性无机阻燃剂填充于表层的聚乙烯醇中。使其阻燃性能得到充分的发挥，大大提高了无机阻燃剂的直接阻燃效果，即在纤维与火源直接接触时即被遏制。因此，可以在取得良好阻燃效果时，大大减少无机阻燃剂的用量。
在本发明中，阻燃维纶纤维采用普通湿法纺丝设备进行纺丝，只需要增加纺丝甬道可以达到纺制阻燃维纶纤维的目的。纺丝甬道的使用是本发明得以实现的重要区域。本发明所使用的气体为工业氮气，其它惰性气体也同样适用。工业氮气靠近喷丝板，携带有表面改性无机阻燃剂，在通过纺丝甬道时，工业氮气与维纶纺丝原液接触的同时，表面改性无机阻燃剂随之粘附至维纶纺丝原液的表面并与维纶纺丝原液表层的聚乙烯醇进行快速混合。随着维纶纺丝原液在凝固浴中固化成型，表面改性无机阻燃剂在维纶纤维的表层得到固定，形成一种具有皮芯结构的阻燃维纶纤维。
本发明的有益效果在于：
1)在超声波的辅助下，利用油酸、硬酯酸、蓖麻油酸钙、硬酯酸钙、三聚氯氰对无机阻燃剂进行有机化表面改性，使所得表面改性无机阻燃剂与聚乙烯醇及其缩甲醛产物都具有良好的相容性；
2)将表面改性无机阻燃剂粉末粘附至维纶纺丝原液的表面，并与维纶纺丝原液表层的聚乙烯醇进行快速混合，随着维纶纺丝原液固化成型以及缩甲醛处理，表面改性无机阻燃剂在维纶纤维的表层得到固定，形成一种具有皮芯结构的阻燃维纶纤维，表面改性无机阻燃剂分布于维纶纤维的表面，具有良好的阻燃效果；
3)将表面改性无机阻燃剂填充于维纶纤维的表层，使其阻燃性能得到充分的发挥，大大提高了无机阻燃剂的直接阻燃效果，即在纤维与火源直接接触时即被遏制，可以在取得良好阻燃效果时，大大减少无机阻燃剂的用量。
附图说明
图1为本发明的工艺流程图。
图中，1-维纶纺丝原液，2-喷丝板，3-纺丝甬道，4-入风口，5-出风口，6-凝固浴，7-导丝辊，8-热压辊，9-缩甲醛处理浴，10-水洗浴，11-干燥辊，12-阻燃维纶纤维。
具体实施方式
下面结合附图对本发明作进一步的说明。
实施例1
本实施例一种阻燃维纶纤维，该阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，其中，阻燃整理剂为表面改性无机阻燃剂。
表面改性无机阻燃剂的制备步骤如下：称取油酸10Kg、硬酯酸10Kg、蓖麻油酸钙15Kg、硬酯酸钙15Kg、三聚氯氰1Kg、三氧化二锑60Kg并进行混合，得到无机阻燃剂改性液。该所得无机阻燃剂改性液于超声波条件下(功率为250W，频率为40KHz)处理60min后得粘稠膏状物，将所得粘稠膏状物经干燥、粉碎得中心粒径为0.01μm的表面改性无机阻燃剂。
结合附图1，本实施例一种阻燃维纶纤维的制备步骤如下：
1)维纶纺丝原液的准备：将经过水洗后的聚乙烯醇溶于80℃水中，得到维纶纺丝原液1；该维纶纺丝原液1中聚乙烯醇的重量百分比浓度为18％；
2)纺丝：由计量泵输出的维纶纺丝原液1经喷丝板2喷出后，进入纺丝甬道3，携带有表面改性无机阻燃剂的工业氮气由入风口4进入纺丝甬道3，由出风口5吹出，由纺丝甬道3而出的维纶纺丝原液1被引入凝固浴6中固化成型，即得聚乙烯醇纤维；在纺丝过程中，工业氮气中表面改性无机阻燃剂的浓度为500mg/L，通气量为0.1m3/min；纺丝甬道3为圆柱形，长度为25cm，直径为20cm；入风口4顶端低于喷丝板2出丝口水平位置1cm，所述出风口5底端高于纺丝甬道3最低端1cm；
3)后处理：聚乙烯醇纤维经导丝辊7、热压辊8、缩甲醛处理浴9、水洗浴10、干燥辊11，收集得到阻燃维纶纤维12；其中，热压辊8的温度为100℃，压力为0.5MPa；凝固浴6为浓度420g/L的硫酸钠；缩甲醛处理浴9包括50g/L甲醛，230g/L硫酸、70g/L硫酸钠。
根据GB/T 5454-1997《纺织品燃烧性能试验氧指数法》标准对阻燃维纶纤维进行试验氧指数法的测试，测得其氧指数法为30.7％，表明其阻燃性较好。
实施例2
本实施例一种阻燃维纶纤维，该阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，其中，阻燃整理剂为表面改性无机阻燃剂。
表面改性无机阻燃剂的制备步骤如下：称取油酸15Kg、硬酯酸15Kg、蓖麻油酸钙30Kg、硬酯酸钙30Kg、三聚氯氰5Kg、氢氧化镁80Kg并进行混合，得到无机阻燃剂改性液。该所得无机阻燃剂改性液于超声波条件下(功率为350W，频率为40KHz)处理120min后得粘稠膏状物，将所得粘稠膏状物经干燥、粉碎得中心粒径为0.1μm的表面改性无机阻燃剂。
结合附图1，本实施例一种阻燃维纶纤维的制备步骤如下：
1)维纶纺丝原液的准备：将经过水洗后的聚乙烯醇溶于95℃水中，得到维纶纺丝原液1；该维纶纺丝原液1中聚乙烯醇的重量百分比浓度为22％；
2)纺丝：由计量泵输出的维纶纺丝原液1经喷丝板2喷出后，进入纺丝甬道3，携带有表面改性无机阻燃剂的工业氮气由入风口4进入纺丝甬道3，由出风口5吹出，由纺丝甬道3而出的维纶纺丝原液1被引入凝固浴6中固化成型，即得聚乙烯醇纤维；在纺丝过程中，工业氮气中表面改性无机阻燃剂的浓度为2000mg/L，通气量为0.3m3/min；纺丝甬道3为圆柱形，长度为35cm，直径为40cm；入风口4顶端低于喷丝板2出丝口水平位置3cm，所述出风口5底端高于纺丝甬道3最低端3cm；
3)后处理：聚乙烯醇纤维经导丝辊7、热压辊8、缩甲醛处理浴9、水洗浴10、干燥辊11，收集得到阻燃维纶纤维12；其中，热压辊8的温度为120℃，压力为1MPa；凝固浴6为浓度450g/L的硫酸钠；缩甲醛处理浴9包括70g/L甲醛，240g/L硫酸、80g/L硫酸钠。
根据GB/T 5454-1997《纺织品燃烧性能试验氧指数法》标准对阻燃维纶纤维进行试验氧指数法的测试，测得其氧指数法为33.2％，表明其阻燃性较好。
实施例3
本实施例一种阻燃维纶纤维，该阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，其中，阻燃整理剂为表面改性无机阻燃剂。
表面改性无机阻燃剂的制备步骤如下：称取油酸13Kg、硬酯酸12Kg、蓖麻油酸钙20Kg、硬酯酸钙25Kg、三聚氯氰3Kg、氢氧化铝70Kg并进行混合，得到无机阻燃剂改性液。该所得无机阻燃剂改性液于超声波条件下(功率为300W，频率为40KHz)处理90min后得粘稠膏状物，将所得粘稠膏状物经干燥、粉碎得中心粒径为0.05μm的表面改性无机阻燃剂。
结合附图1，本实施例一种阻燃维纶纤维的制备步骤如下：
1)维纶纺丝原液的准备：将经过水洗后的聚乙烯醇溶于90℃水中，得到维纶纺丝原液1；该维纶纺丝原液1中聚乙烯醇的重量百分比浓度为20％；
2)纺丝：由计量泵输出的维纶纺丝原液1经喷丝板2喷出后，进入纺丝甬道3，携带有表面改性无机阻燃剂的工业氮气由入风口4进入纺丝甬道3，由出风口5吹出，由纺丝甬道3而出的维纶纺丝原液1被引入凝固浴6中固化成型，即得聚乙烯醇纤维；在纺丝过程中，工业氮气中表面改性无机阻燃剂的浓度为1000mg/L，通气量为0.2m3/min；纺丝甬道3为圆柱形，长度为30cm，直径为30cm；入风口4顶端低于喷丝板2出丝口水平位置2cm，所述出风口5底端高于纺丝甬道3最低端2cm；
3)后处理：聚乙烯醇纤维经导丝辊7、热压辊8、缩甲醛处理浴9、水洗浴10、干燥辊11，收集得到阻燃维纶纤维12；其中，热压辊8的温度为110℃，压力为0.8MPa；凝固浴6为浓度430g/L的硫酸钠；缩甲醛处理浴9包括60g/L甲醛，235g/L硫酸、75g/L硫酸钠。
根据GB/T 5454-1997《纺织品燃烧性能试验氧指数法》标准对阻燃维纶纤维进行试验氧指数法的测试，测得其氧指数法为31.9％，表明其阻燃性较好。
Claims (6)
1.一种阻燃维纶纤维，其特征在于，所述阻燃维纶纤维的表层为阻燃整理剂与聚乙烯醇缩甲醛的混合物，所述阻燃整理剂为表面改性无机阻燃剂；
所述阻燃维纶纤维的制备方法，步骤如下：
1)维纶纺丝原液的准备：将经过水洗后的聚乙烯醇溶于80～95℃水中，得到维纶纺丝原液(1)；
2)纺丝：由计量泵输出的维纶纺丝原液(1)经喷丝板(2)喷出后，进入纺丝甬道(3)，携带有表面改性无机阻燃剂的工业氮气由入风口(4)进入纺丝甬道(3)，由出风口(5)吹出，由纺丝甬道(3)而出的维纶纺丝原液(1)被引入凝固浴(6)中固化成型，即得聚乙烯醇纤维；
3)后处理：聚乙烯醇纤维经导丝辊(7)、热压辊(8)、缩甲醛处理浴(9)、水洗浴(10)、干燥辊(11)，收集得到阻燃维纶纤维(12)；
所述表面改性无机阻燃剂的制备步骤如下：将无机阻燃剂改性液于超声波条件下处理60～120min后得粘稠膏状物，将所得粘稠膏状物经干燥、粉碎得中心粒径为0.01～0.1μm的表面改性无机阻燃剂；所述无机阻燃剂改性液的原料重量百分配比为：油酸10～15份、硬酯酸10～15份、蓖麻油酸钙15～30份、硬酯酸钙15～30份、三聚氯氰1～5份、无机阻燃剂60～80份；所述无机阻燃剂三氧化二锑、氢氧化镁和氢氧化铝中的一种或几种。
2.根据权利要求1所述的一种阻燃维纶纤维，其特征在于，超声波的功率为250～350W，频率为40KHz。
3.根据权利要求1所述的一种阻燃维纶纤维，其特征在于，所述维纶纺丝原液(1)中聚乙烯醇的重量百分比浓度为18～22％。
4.根据权利要求1所述的一种阻燃维纶纤维，其特征在于，所述工业氮气中表面改性无机阻燃剂的浓度为500～2000mg/L，通气量为0.1～0.3m3/min；所述热压辊(8)的温度为100～120℃，压力为0.5～1.0MPa。
5.根据权利要求1所述的一种阻燃维纶纤维，其特征在于，所述凝固浴(6)为浓度420～450g/L的硫酸钠；所述缩甲醛处理浴(9)包括50～70g/L甲醛，230～240g/L硫酸、70～80g/L硫酸钠。
6.根据权利要求1所述的一种阻燃维纶纤维，其特征在于，所述纺丝甬道(3)为圆柱形，长度为25～35cm，直径为20～40cm；所述入风口(4)顶端低于喷丝板(2)出丝口水平位置1～3cm，所述出风口(5)底端高于纺丝甬道(3)最低端1～3cm。
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| CN101343781A (zh) * | 2008-08-05 | 2009-01-14 | 青岛大学 | 一种阻燃聚乙烯醇/SiO2复合纤维的制备方法 |
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| CN101033581A (zh) * | 2007-03-30 | 2007-09-12 | 苏州大学 | 一种用于织物的阻燃剂及其合成方法 |
| CN101343782A (zh) * | 2008-08-05 | 2009-01-14 | 青岛大学 | 一种无机阻燃聚乙烯醇纤维的制备方法 |
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