CN115491928B - 一种双壳层复合氮磷微胶囊阻燃型牛皮纸及其制备方法 - Google Patents
一种双壳层复合氮磷微胶囊阻燃型牛皮纸及其制备方法 Download PDFInfo
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Abstract
一种双壳层复合氮磷微胶囊阻燃型牛皮纸及其制备方法,该发明以牛皮纸为基材,通过复合乳化剂的制备、聚磷酸铵/二氧化硅微胶囊的制备、聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备、双壳层复合氮磷微胶囊阻燃牛皮纸的制备等步骤,利用聚磷酸铵作为芯材与无机阻燃剂、二氧化硅为内壁材与抑烟剂、乙基纤维素为外壁材与炭源,利用表面涂布法将分散好的阻燃液涂布到牛皮纸上,制备出具有高阻燃性能、低吸湿性能及一定抑烟性能的阻燃牛皮纸。该制备流程以及制备用阻燃剂,可广泛用于多种纸材料的阻燃,尤其适用于牛皮纸、白卡纸、瓦楞纸、浸渍纸等包装用纸、工业用纸或类似材料或其他木材植物纤维衍生物如刨花板、胶合板等,可大大增强其阻燃性能。
Description
技术领域
本发明属于阻燃剂制备与改性领域,具体为乙基纤维素/二氧化硅/聚磷酸铵双壳层复合微胶囊阻燃剂制备及其改性处理牛皮纸的制备方法。
技术背景
微胶囊技术又称微胶囊化,是指利用一定技术手段将固体、液体或气体包裹在微小的半透性或封闭胶囊的过程,通过将芯材包裹在微胶囊壁材中,达到保持芯材的物理化学性质的目的。一般被包裹在内部的物质称为芯材,包裹芯材的物质称为壁材。由于其可以通过将芯材与外界环境隔离以达到某些功能性改进效果,如缓释、保护、隔离、发泡等,微胶囊技术被广泛应用于食品、化工、农业、建筑、阻燃等多个领域。
随着微胶囊技术的发展,目前已有许多对阻燃剂进行微胶囊化处理以改善其缺陷的相关报道。通过微胶囊技术,可以改善某些阻燃剂的缺陷,使其更好地应用于家具、建筑等领域。无卤膨胀型阻燃剂近年来因其低毒、高效等优点得到了广泛的研究和应用。其中氮磷系阻燃剂通过释放NH3和形成磷酸阻燃层的气相和固相方式对基材发挥阻燃作用,相较于卤系阻燃剂具有无毒无味、不产生有害气体,对环境友好的优势和特点。聚磷酸铵(APP)作为一种氮磷系阻燃剂,目前在许多领域被广泛应用。然而,聚磷酸铵存在吸湿性高、破坏基材强度、烟气释放量大的弊端,严重影响其在基材中的应用。为了改进聚磷酸铵的以上缺点,目前已有多种有机材料作为壳层被用于聚磷酸铵的微囊化处理,如三聚氰胺-甲醛树脂、聚脲、环氧树脂等,所制备的聚磷酸铵微胶囊表现出良好的基材相容性与阻燃性能。但这些壳材料的单体绝大多数来自化石原料,其中一部分甚至有毒性,因此在制备与使用的过程中会对周围环境造成潜在的危害,因此寻找一种绿色环保的壳材料具有重要的意义。
作为一种生物基高分子材料,乙基纤维素(EC)因其具有优异的疏水性、热稳定性、无毒环保等优点,被广泛应用于涂料、微胶囊、胶粘剂等领域。因此,EC可以作为壳材料,制备MAPP,提高APP与基材的相容性,同时解决APP吸湿性大的问题;EC作为壳层,是一种可生物降解的材料,可以减少合成过程中造成的环境危害;此外,EC可以作为炭源,与APP组成IFR体系以提供更好的阻燃性能。
牛皮纸是由针叶木的木材纤维,经过化学方法制浆,再放入打浆机中进行打浆,加入胶料、染料后,在造纸机中抄造而成的一类纸张,具有原料来源广泛、易批量生产、加工性能好、印刷适应性好、防霉防潮、可回收再利用等优点,在食品包装、办公文具、服装吊牌、档案保存等领域具有广泛应用。牛皮纸与其他纸质材料一样,具有易燃性,在高温环境下极易被引燃。当牛皮纸用于物流包装、档案保存等领域时,如果发生火灾,牛皮纸会加速和扩大火灾,灭火处理不及时时会对人民的生命财产安全造成不可估量的损失。因此牛皮纸的阻燃处理在牛皮纸当前以及未来的发展中极其重要和关键。同时阻燃处理过的牛皮纸大多在阻燃过程中会产生大量烟气,在火灾中易对人体造成灼烧皮肤与呼吸道的危害,使人体受到二次伤害,因此减少阻燃牛皮纸燃烧时烟尘的释放,对于牛皮纸的安全使用同样具有关键的意义。
为了解决上述问题,可以将聚磷酸铵作为芯材,纳米二氧化硅与乙基纤维素作为壁材,采用微胶囊技术将聚磷酸铵包覆。纳米二氧化硅作为一种一维颗粒材料,具有极高的热稳定性与隔热性能。由于硅和磷之间的协同作用,纳米二氧化硅在改善膨胀体系阻燃和抑烟性能上有较好的效果。
利用纳米二氧化硅与乙基纤维素作为双壁材包覆聚磷酸铵,制备双壳层复合氮磷微胶囊作为膨胀型阻燃体系。通过将微胶囊分散成阻燃液,涂覆到牛皮纸上,制备出具有高阻燃性能、低吸湿性能以及一定抑烟性能的阻燃牛皮纸。
发明内容
本发明所解决的技术问题在于提供一种双壳层复合氮磷微胶囊阻燃牛皮纸的制备方法,该发明以牛皮纸为基材主体,通过将制备出的聚磷酸铵/二氧化硅/乙基纤维素微胶囊涂覆在基材表面,最终制备出阻燃牛皮纸。该方法也可制备其他种类纸材料,如瓦楞纸板、卡纸等,可以有效提高纸材料的阻燃性能。
本发明所解决的技术问题采用以下技术方案来实现:
一种双壳层复合氮磷微胶囊阻燃牛皮纸的制备方法,包括以下步骤:
(1)复合乳化剂的制备:将辛烷基苯酚聚氧乙烯醚-10(OP-10)、脂肪酸甲酯乙氧基化物(FMEE)以及异构十三醇聚氧乙烯醚(TO-10)按照一定比例在一定温度条件下进行共混并搅拌均匀,得到复合乳化剂。
(2)聚磷酸铵/二氧化硅微胶囊的制备:将蒸馏水与无水乙醇按照一定比例混合,并在一定温度条件下搅拌均匀;加入聚磷酸铵与乳化剂并搅拌,用滴管逐滴加入氨水调节pH至一定范围;随后用滴管逐滴加入一定量的硅酸四乙酯并在一定温度条件下反应一段时间;之后经过真空抽滤、洗涤并在一定温度条件下进行干燥,得到聚磷酸铵/二氧化硅微胶囊。
(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备:将乙基纤维素按照一定比例加入相应量乙酸乙酯中并在一定温度条件下充分搅拌至乙基纤维素完全溶于,制备乙基纤维素有机溶液;随后将步骤(2)制备好的聚磷酸铵/二氧化硅微胶囊按照一定比例添加至乙基纤维素有机溶液中,在一定温度条件下进行充分搅拌;随后在一定温度条件下干燥至恒重,并用粉碎机将干燥后的固体样品粉碎,过筛,得到聚磷酸铵/二氧化硅/乙基纤维素微胶囊。
(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备:将制备好的聚磷酸铵/二氧化硅/乙基纤维素微胶囊按照一定比例加入蒸馏水中并在一定温度条件下搅拌均匀,制备阻燃液;随后利用表面涂布法在一定温度条件下用涂布棒对牛皮纸进行双面涂布,然后在一定温度条件下干燥至恒重,得到双壳层复合氮磷微胶囊阻燃牛皮纸。
为保证制备样品的优异性能,作为优选,上述步骤(1)复合乳化剂的制备中辛烷基苯酚聚氧乙烯醚-10(OP-10)、脂肪酸甲酯乙氧基化物(FMEE)以及异构十三醇聚氧乙烯醚(TO-10)的质量比为10:A:B,其中A取值范围为0~10、B取值范围为0~10。
作为优选,上述步骤(1)复合乳化剂的制备中混合搅拌的温度为25~45℃,搅拌时间大于10min。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵的聚合度大于50。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵、乳化剂、硅酸四乙酯质量比为50~350:1:40~100。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中蒸馏水与无水乙醇的质量比为7:C,C取值范围为3~9;二者混合温度为40~60℃。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵与无水乙醇的质量比为8:D,D取值范围为5~15。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中调节pH范围为8~12。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中硅酸四乙酯的滴加速度为1~5mL/min,反应温度为30~60℃,反应时间为1~3h。
作为优选,上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中洗涤所用溶液为蒸馏水与无水乙醇按照5:E制备的乙醇溶液,E取值范围为1.0~4.0;干燥温度为60~100℃,干燥温度为12~36h。
作为优选,上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中乙基纤维素的粘度为180-220mPa·s。
作为优选,上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中乙基纤维素与乙酸乙酯的质量比为1:F,F取值范围为10~30。
作为优选,上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中聚磷酸铵/二氧化硅微胶囊添加到乙基纤维素有机溶液后搅拌时间大于30min,温度范围为25~75℃。
作为优选,上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中干燥温度为30~100℃。
作为优选,上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中所过筛目数为80~300目。
作为优选,上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中聚磷酸铵/二氧化硅/乙基纤维素微胶囊与蒸馏水的质量比为1:G,G取值范围为1~5。
作为优选,上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中阻燃液的搅拌温度为25~65℃。
作为优选,上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中涂布温度为25~65℃。
作为优选,上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中干燥温度为30~80℃。
具体实施案例
为了更好地表述本发明的技术手段、制备流程,下面结合具体实施案例进行阐述本发明。
实施例1
首先将辛烷基苯酚聚氧乙烯醚-10(OP-10)、脂肪酸甲酯乙氧基化物(FMEE)以及异构十三醇聚氧乙烯醚(TO-10)按照质量比10:7:3在40℃下进行共混并搅拌均匀,得到复合乳化剂;将蒸馏水与无水乙醇按照质量比为7:5混合,并在45℃条件下搅拌均匀;随后将聚磷酸铵与制备好的乳化剂按照质量比为10:1分别添加进乙醇溶液中,其中聚磷酸铵与无水乙醇的质量比为4:5;逐滴加入氨水,调节反应体系pH至9~10;搅拌均匀后以1mL/min的速度向体系中逐滴加入硅酸四乙酯,并在45℃下反应2h;随后对溶液进行真空抽滤,并将过滤物用蒸馏水与无水乙醇按照质量比为7:3进行洗涤,随后在80℃下干燥24h,得到聚磷酸铵/二氧化硅微胶囊;将乙基纤维素与乙酸乙酯按照质量比为1:19进行混合,在25℃下搅拌至乙基纤维素完全溶解于乙酸乙酯,制备乙基纤维素有机溶液,随后将制备好的聚磷酸铵/二氧化硅微胶囊按照与乙基纤维素有机溶液质量比为1:20添加至乙基纤维素有机溶液中,并在25℃下进行充分搅拌至聚磷酸铵/二氧化硅微胶囊分散均匀;随后在60℃条件下干燥至恒重,并用粉碎机将干燥后的固体样品粉碎,过150目筛,得到聚磷酸铵/二氧化硅/乙基纤维素微胶囊;将制备好的聚磷酸铵/二氧化硅/乙基纤维素微胶囊按照质量比1:3加入相应量蒸馏水中并在25℃下搅拌均匀,制备阻燃液;随后利用表面涂布法在25℃下用涂布棒对牛皮纸进行双面涂布,然后在60℃下干燥至恒重,得到双壳层复合氮磷微胶囊阻燃牛皮纸。。
按照上述得到了聚磷酸铵基阻燃牛皮纸的极限氧指数可达29%,纵向抗张强度达到9.25kPa,断裂伸长率达到2.72%,10天后的吸水率为1.46%。利用热重分析测试,结果显示与未添加任何阻燃剂的牛皮纸比较,上述步骤制备的聚磷酸铵基阻燃牛皮纸的初始热分解温度升高,最大失重速率所处温度降低,同时残炭量也从22.75%上升到27.43%。上述性能满足了阻燃牛皮纸在包装、办公、档案保存等领域的应用需求。
以上描述了本发明的基本原理、主要特征及本发明的优点。本行业的技术人员应该了解,本发明不受实施例限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明的精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (1)
1.一种双壳层复合氮磷微胶囊阻燃牛皮纸的制备方法,包括以下步骤:
(1)复合乳化剂的制备:将辛烷基苯酚聚氧乙烯醚-10(OP-10)、脂肪酸甲酯乙氧基化物(FMEE)以及异构十三醇聚氧乙烯醚(TO-10)按照一定比例在一定温度条件下进行共混并搅拌均匀,得到复合乳化剂;
(2)聚磷酸铵/二氧化硅微胶囊的制备:将蒸馏水与无水乙醇按照一定比例混合,并在一定温度条件下搅拌均匀;加入聚磷酸铵与乳化剂并搅拌,用滴管逐滴加入氨水调节pH至一定范围;随后用滴管逐滴加入一定量的硅酸四乙酯并在一定温度条件下反应一段时间;之后经过真空抽滤、洗涤并在一定温度条件下进行干燥,得到聚磷酸铵/二氧化硅微胶囊;
(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备:将乙基纤维素按照一定比例加入相应量乙酸乙酯中并在一定温度条件下充分搅拌至乙基纤维素完全溶于,制备乙基纤维素有机溶液;随后将步骤(2)制备好的聚磷酸铵/二氧化硅微胶囊按照一定比例添加至乙基纤维素有机溶液中,在一定温度条件下进行充分搅拌;随后在一定温度条件下干燥至恒重,并用粉碎机将干燥后的固体样品粉碎,过筛,得到聚磷酸铵/二氧化硅/乙基纤维素微胶囊;
(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备:将制备好的聚磷酸铵/二氧化硅/乙基纤维素微胶囊按照一定比例加入蒸馏水中并在一定温度条件下搅拌均匀,制备阻燃液;随后利用表面涂布法在一定温度条件下用涂布棒对牛皮纸进行双面涂布,然后在一定温度条件下干燥至恒重,得到双壳层复合氮磷微胶囊阻燃牛皮纸;
为保证制备样品的优异性能,上述步骤(1)复合乳化剂的制备中辛烷基苯酚聚氧乙烯醚-10(OP-10)、脂肪酸甲酯乙氧基化物(FMEE)以及异构十三醇聚氧乙烯醚(TO-10)的质量比为10:A:B,其中A取值范围为0~10、B取值范围为0~10;
上述步骤(1)复合乳化剂的制备中混合搅拌的温度为25~45 ℃,搅拌时间大于10 min;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵的聚合度大于50;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵、乳化剂、硅酸四乙酯质量比为50~350:1:40~100;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中蒸馏水与无水乙醇的质量比为7:C,C取值范围为3~9;二者混合温度为40~60 ℃;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中聚磷酸铵与无水乙醇的质量比为8:D,D取值范围为5~15;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中调节pH范围为8~12;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中硅酸四乙酯的滴加速度为1~5mL /min,反应温度为30~60 ℃,反应时间为1~3 h;
上述步骤(2)聚磷酸铵/二氧化硅微胶囊的制备中洗涤所用溶液为蒸馏水与无水乙醇按照5:E制备的乙醇溶液,E取值范围为1.0~4.0;干燥温度为60~100 ℃,干燥温度为12~36h;
上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中乙基纤维素的粘度为180-220 mPa·s;
上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中乙基纤维素与乙酸乙酯的质量比为1:F,F取值范围为10~30;
上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中聚磷酸铵/二氧化硅微胶囊添加到乙基纤维素有机溶液后搅拌时间大于30 min,温度范围为25~75 ℃;
上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中干燥温度为30~100 ℃;
上述步骤(3)聚磷酸铵/二氧化硅/乙基纤维素微胶囊的制备中所过筛目数为80~300目;
上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中聚磷酸铵/二氧化硅/乙基纤维素微胶囊与蒸馏水的质量比为1:G,G取值范围为1~5;
上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中阻燃液的搅拌温度为25~65℃;
上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中涂布温度为25~65 ℃;
上述步骤(4)双壳层复合氮磷微胶囊阻燃牛皮纸的制备中干燥温度为30~80 ℃。
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