CN111622019B - 一种纸板用防火涂层材料及其制备方法 - Google Patents
一种纸板用防火涂层材料及其制备方法 Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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- D21H19/00—Coated paper; Coating material
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- D21H19/00—Coated paper; Coating material
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Abstract
本发明涉及防火涂层材料，具体涉及一种纸板用防火涂层材料，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液43‑65份、聚硅氧烷1‑5份、氧化石墨烯1‑3份、颜填料32‑40份、阻燃剂10‑18份、稀释剂5‑12份、无机纤维3‑8份。本发明的有益效果在于：（1）有机硅氟改性后的聚氨酯乳液可显著提升涂层的粘附强度，耐温性能和阻燃效果；（2）采用氧化石墨烯改性后的颜填料体系的分散性好，不易团聚，品质更稳定；（3）本发明所述纸板防火涂层材料的加工工艺简单，使用方便，制成的纸板耐磨性能好，抗撞击性能强。
Description
技术领域
本发明属于防火涂层材料技术领域，具体涉及一种纸板用防火涂层材料及其制备方法。
背景技术
瓦楞纸箱是用瓦楞纸板制成的刚性纸质容器。半个多世纪以来，瓦楞纸箱以其优越的使用性能和良好的加工性能逐渐取代了木箱等运输包装容器，成为运输包装的主力军。它除了保护商品、便于仓储、运输之外，还起到美化商品，宣传商品的作用。瓦楞纸箱属于绿色环保产品，它利于环保，利于装卸运输。
另一方面，纸板也是一种极易燃烧的材料，在温度高的环境下容易燃烧，存在安全隐患，因此，需应用防火涂层。防火涂层的应用在我国起步较晚，尤其是应用于纸板这一块，但是发展较快，目前我国已经研究出了各种性能的防火涂层材料。如中国专利CN2013105382296公开了一种纸板防火涂层材料及其制备方法，所述涂层材料由如下质量百分配比的原料制成：碳纤维、无水亚硫酸盐、氯化钾、粉煤灰、硅酸盐溶液等。虽然现有技术涂层材料提供了较好的防火性能，但是瓦楞酯箱在运输过程中，纸箱于地面，纸箱与纸箱之间，纸箱与接触物之间等会发生摩擦、挤压、碰撞，表面涂层极易脱落，破坏瓦楞纸箱的完整性和美观性。因此急需开发新型瓦楞纸箱用防火涂层材料，提高粘贴强度和力学性能。
发明内容
为解决现有技术的不足，本发明提供一种纸板用防火涂层材料及其制备方法，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液43-65份、聚硅氧烷1-5份、氧化石墨烯1-3份、颜填料32-40份、阻燃剂10-18份、稀释剂5-12份、无机纤维3-8份；所述改性聚氨酯丙烯酸酯乳液是以甲基丙烯酸羟乙酯封端的水性聚氨酯与甲基丙烯酸甲酯、甲基丙烯酸羟丙酯、乙烯基三异丙氧基硅烷、二全氟辛基乙基丙烯酸酯共聚得到的改性聚氨酯丙烯酸酯乳液。改性后的聚氨酯丙烯酸酯乳液引入了有机硅和全氟烷基链，显著提升了涂层膜的耐温、耐摩擦性能；另一方面，引入的羟基侧链更容易与纸板中含有的有机含氧化合物键合，提高涂层与纸板界面的粘附强度。
所述改性聚氨酯丙烯酸酯乳液的制备方法，包括如下步骤：(1)将聚醚二醇、1,4-丁二醇、二羟甲基丙酸和N-甲基吡咯烷酮按质量比加入反应釜中，110℃下真空除水后降至80℃；然后加入异佛尔酮二异氰酸酯，少量二月桂酸二丁基锡，保温反应2h后降至65℃，加入甲基丙烯酸羟乙酯，反应2-3h后降至40℃，加入三乙胺中和至pH7-8；最后加入去离子水，剧烈搅拌乳化，得甲基丙烯酸羟乙酯封端的聚氨酯乳液；(2)先将基丙烯酸羟乙酯封端的聚氨酯乳液与甲基丙烯酸甲酯、甲基丙烯酸羟丙酯、乙烯基三异丙氧基硅烷、二全氟辛基乙基丙烯酸酯按质量比混合均匀获得混合单体；将40％的混合单体加入反应釜中，开启搅拌，缓慢滴加二乙二醇丁醚，滴加完毕后，搅拌20-30min，然后滴加引发剂过氧化苯甲酰，滴加完毕后，升高温度到90-95℃，保温反应2-3h；然后升高温度到105-110℃，滴加剩余的60％混合单体，滴加完毕后继续反应1-2h，反应完毕后降至60℃，加N,N-二甲基乙醇胺中和，加水乳化得改性聚氨酯丙烯酸酯乳液。
所述聚硅氧烷是以低含氢硅油、聚醚F-6为主要原料，利用硅氢加成反应制备的聚醚改性聚硅氧烷；改性后的聚硅氧烷降低了与改性环氧树脂乳液的表面张力能，实现颜填料界面的较好润湿，提高了颜填料的分散性；
所述氧化石墨烯与颜填料复合使用，通过将氧化石墨烯包覆到颜填料的表面形成一层超润滑膜，提高颜填料的分散性，抑制其团聚。另一方面，石墨烯还可以与阻燃剂协同提高改性聚氨酯丙烯酸酯的耐热性能，进一步提高阻燃效果；
所述颜填料为纳米二氧化硅25-30份、纳米氧化锌12-18份、纳米氧化铝5-12份的混合物；
所述阻燃剂为钛酸酯改性聚磷酸铵；具体方法是将钛酸酯、石油醚与聚磷酸铵按质量比混合后剧烈搅拌，离心分离干燥制得；
所述稀释剂为正丁醇、丙二醇、聚乙二醇400中的至少一种；
所述无机纤维为陶瓷纤维、高硅氧纤维、氧化铝纤维中的至少一种。
本发明还提供所述纸板防火涂层材料的制备方法，具体包括如下步骤：
(1)将各种颜填料、氧化石墨烯、改性阻燃剂、无机纤维按质量比依次加入研磨机中，研磨3-5h，得混合体系；
(2)向反应釜中按质量比依次加入改性聚氨酯丙烯酸酯乳液、聚硅氧烷、稀释剂，剧烈搅拌制得混合乳液；然后向混合乳液中加入步骤1所得的混合体系，升高温度到60-65℃，保温反应2-3h，降至室温，出料得纸板用防火涂料。
本发明的有益效果在于：(1)有机硅氟改性后的聚氨酯乳液可显著提升涂层的粘附强度，耐温性能和阻燃效果；(2)采用氧化石墨烯改性后的颜填料体系的分散性好，不易团聚，品质更稳定；(3)本发明所述纸板防火涂层材料的加工工艺简单，使用方便，制成的纸板耐磨性能好，抗撞击性能强。
具体实施方式
下面以实施例对本发明进行详细说明，所举实施例仅用于对本发明的原理和特征进行描述，只用于解释本发明，并非用于限定本发明的范围。
实施例1.
本实施例提供一种纸板用防火涂层材料及其制备方法，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液45份、聚硅氧烷2份、氧化石墨烯1.5份、颜填料32份、阻燃剂10份、正丁醇5份、陶瓷纤维3份；
所述改性聚氨酯丙烯酸酯乳液是以甲基丙烯酸羟乙酯封端的水性聚氨酯100份与甲基丙烯酸甲酯18份、甲基丙烯酸羟丙酯8份、乙烯基三异丙氧基硅烷13份、二全氟辛基乙基丙烯酸酯15份共聚得到的改性聚氨酯丙烯酸酯乳液。
所述改性聚氨酯丙烯酸酯乳液的制备方法，包括如下步骤：(1)将聚醚二醇500g、1,4-丁二醇90g、二羟甲基丙酸67g和N-甲基吡咯烷酮5L按质量比加入反应釜中，110℃下真空除水后降至80℃；然后加入异佛尔酮二异氰酸酯556g，少量二月桂酸二丁基锡1g，保温反应2h后降至65℃，加入甲基丙烯酸羟乙酯65g，反应2-3h后降至40℃，加入三乙胺中和至pH7-8；最后加入去离子水2900mL，剧烈搅拌乳化，得甲基丙烯酸羟乙酯封端的聚氨酯乳液；(2)将步骤(1)制得的甲基丙烯酸羟乙酯封端的聚氨酯乳液1000g与甲基丙烯酸甲酯180g、甲基丙烯酸羟丙酯80g、乙烯基三异丙氧基硅烷130g、二全氟辛基乙基丙烯酸酯150g按质量比混合均匀获得混合单体；将40％的混合单体加入反应釜中，开启搅拌，缓慢滴加二乙二醇丁醚130g，滴加完毕后，搅拌20-30min，然后滴加引发剂过氧化苯甲酰10g，滴加完毕后，升高温度到90-95℃，保温反应2-3h；然后升高温度到105-110℃，滴加剩余的60％混合单体，滴加完毕后继续反应1-2h，反应完毕后降至60℃，加N,N-二甲基乙醇胺中和，加水乳化得改性聚氨酯丙烯酸酯乳液。
所述聚硅氧烷是以低含氢硅油、聚醚F-6为主要原料，利用硅氢加成反应制备的聚醚改性聚硅氧烷；
所述氧化石墨烯与颜填料复合使用，通过将氧化石墨烯包覆到颜填料的表面形成一层超润滑膜，提高颜填料的分散性，抑制其团聚。
所述颜填料为纳米二氧化硅26份、纳米氧化锌15份、纳米氧化铝8份的混合物；
所述阻燃剂为钛酸酯改性聚磷酸铵；具体方法是将钛酸酯2份、石油醚100份与聚磷酸铵50份按质量比混合后剧烈搅拌，离心分离干燥制得；
本发明还提供所述纸板防火涂层材料的制备方法，具体包括如下步骤：
(1)将颜填料320g、氧化石墨烯15g、钛酸酯改性聚磷酸铵100g、陶瓷纤维按质量比依次加入研磨机中，研磨3-5h，得混合体系；
(2)向反应釜中按质量比依次加入改性聚氨酯丙烯酸酯乳液450g、聚硅氧烷20g、正丁醇50g，剧烈搅拌制得混合乳液；然后向混合乳液中加入步骤1所得的混合体系，升高温度到60-65℃，保温反应2-3h，降至室温，出料得纸板用防火涂料。
实施例2.
本实施例提供一种纸板用防火涂层材料及其制备方法，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液50份、聚硅氧烷3份、氧化石墨烯2份、颜填料35份、阻燃剂13份、聚乙二醇4008份、氧化铝纤维5份；
所述改性聚氨酯丙烯酸酯乳液是以甲基丙烯酸羟乙酯封端的水性聚氨酯乳液100份与甲基丙烯酸甲酯16份、甲基丙烯酸羟丙酯9份、乙烯基三异丙氧基硅烷12份、二全氟辛基乙基丙烯酸酯18份共聚得到的改性聚氨酯丙烯酸酯乳液。其制备方法同实施例1；
所述聚硅氧烷同实施例1；
所述氧化石墨烯同实施例1；
所述颜填料为纳米二氧化硅20份、纳米氧化锌20份、纳米氧化铝5份的混合物；
所述阻燃剂及其制备方法同实施例1；
本发明所用防火涂层材料的制备方法同实施例1，仅需将各组分等量替换即可。
实施例3.
本实施例提供一种纸板用防火涂层材料及其制备方法，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液60份、聚硅氧烷5份、氧化石墨烯3份、颜填料38份、阻燃剂18份、丙二醇12份、氧化铝纤维8份；
所述改性聚氨酯丙烯酸酯乳液是以甲基丙烯酸羟乙酯封端的水性聚氨酯乳液100份与甲基丙烯酸甲酯19份、甲基丙烯酸羟丙酯9份、乙烯基三异丙氧基硅烷10份、二全氟辛基乙基丙烯酸酯20份共聚得到的改性聚氨酯丙烯酸酯乳液。其制备方法同实施例1；
所述聚硅氧烷同实施例1；
所述氧化石墨烯同实施例1；
所述颜填料为纳米二氧化硅18份、纳米氧化锌20份、纳米氧化铝7份的混合物；
所述阻燃剂及其制备方法同实施例1；
本发明所用防火涂层材料的制备方法同实施例1，仅需将各组分等量替换即可。
对比例
本对比例选用现有专利技术CN2015102626438，制备的纸板用防火涂料的组成按重量份数如下：改性三元乙丙橡胶、环氧值为0.45mol/100g的纳米橡胶改性环氧树脂60份、聚氨酯35份、聚四氟乙烯12份、聚硅氧烷26份、尿素8份、二氯二苯甲酮8份、碳酸钙3份、方解石6份、硬脂酸锌2份、氧化铝含量为42％的氧化铝纤维8份、羟乙基纤维素3份、甲苯二异氰酸酯8份、丙烯酸乳液2份、硬脂酸钙分散剂8份、硼酸锌阻燃剂1份、丙酮稀释剂5份、去离子水12份；
将本发明实施例和对比例制备的阻燃涂料，分别测试其阻燃效果，具体方法是：对每组样品取3块1000mm*30mm*5mm的瓦楞纸板，在表面涂上本发明和对比例制备的涂料，在干燥无风的环境中，通过明火源点燃后再移去，待其完全熄灭后，记录其平均燃烧时间以及平均燃烧距离，结果见表1：
表1.防火涂层材料的阻燃效果
由表1数据可见，本发明制备的涂层材料的阻燃效果好，粘贴强度高，对现有技术改进大。以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (5)
1.一种纸板用防火涂层材料，所述涂层材料按重量份数包括如下配方组成：改性聚氨酯丙烯酸酯乳液 43-65份、聚硅氧烷 1-5份、氧化石墨烯 1-3份、颜填料 32-40份、阻燃剂10-18份、稀释剂 5-12份、无机纤维 3-8份；
所述改性聚氨酯丙烯酸酯乳液是以甲基丙烯酸羟乙酯封端的水性聚氨酯与甲基丙烯酸甲酯、甲基丙烯酸羟丙酯、乙烯基三异丙氧基硅烷、二全氟辛基乙基丙烯酸酯共聚得到的改性聚氨酯丙烯酸酯乳液；
所述聚硅氧烷是以低含氢硅油、聚醚F-6为主要原料，利用硅氢加成反应制备的聚醚改性聚硅氧烷；
所述氧化石墨烯与颜填料复合使用，通过将氧化石墨烯包覆到颜填料的表面形成一层超润滑膜，提高颜填料的分散性，抑制其团聚；
所述颜填料为纳米二氧化硅 25-30份、纳米氧化锌 12-18份、纳米氧化铝 5-12份的混合物。
2.根据权利要求1所述的一种纸板用防火涂层材料，其特征在于，所述阻燃剂为钛酸酯改性聚磷酸铵；具体方法是将钛酸酯、石油醚与聚磷酸铵按质量比混合后剧烈搅拌，离心分离干燥制得。
3.根据权利要求1所述的一种纸板用防火涂层材料，其特征在于，所述稀释剂为正丁醇、丙二醇、聚乙二醇400中的至少一种。
4.根据权利要求1所述的一种纸板用防火涂层材料，其特征在于，所述无机纤维为陶瓷纤维、高硅氧纤维、氧化铝纤维中的至少一种。
5.权利要求1-4中任一项所述的一种纸板防火涂层材料的制备方法，具体包括如下步骤：
（1）将各种颜填料、氧化石墨烯、改性阻燃剂、无机纤维按质量比依次加入研磨机中，研磨3-5h，得混合体系；
（2）向反应釜中按质量比依次加入改性聚氨酯丙烯酸酯乳液、聚硅氧烷、稀释剂，剧烈搅拌制得混合乳液；然后向混合乳液中加入步骤1所得的混合体系，升高温度到60-65℃，保温反应2-3h，降至室温，出料得纸板用防火涂料。
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| CN104893435A (zh) * | 2015-05-21 | 2015-09-09 | 芜湖蒲草电子商务有限公司 | 一种瓦楞纸箱用耐磨防火涂料及其制备方法 |
| CN106010415A (zh) * | 2016-05-24 | 2016-10-12 | 吉林省大鱼资产管理有限公司 | 一种全水发泡冷熟化泡沫防火填缝胶及其制备方法 |
| CN109354957A (zh) * | 2018-10-27 | 2019-02-19 | 国网河南省电力公司方城县供电公司 | 一种电力设备用水性涂料及其制备方法 |
| CN110105800A (zh) * | 2019-05-09 | 2019-08-09 | 海洋化工研究院有限公司 | 一种防火隔热涂料及其制备方法 |
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| CN104893435A (zh) * | 2015-05-21 | 2015-09-09 | 芜湖蒲草电子商务有限公司 | 一种瓦楞纸箱用耐磨防火涂料及其制备方法 |
| CN106010415A (zh) * | 2016-05-24 | 2016-10-12 | 吉林省大鱼资产管理有限公司 | 一种全水发泡冷熟化泡沫防火填缝胶及其制备方法 |
| CN109354957A (zh) * | 2018-10-27 | 2019-02-19 | 国网河南省电力公司方城县供电公司 | 一种电力设备用水性涂料及其制备方法 |
| CN110105800A (zh) * | 2019-05-09 | 2019-08-09 | 海洋化工研究院有限公司 | 一种防火隔热涂料及其制备方法 |
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