CN112795359A - 一种水性箱包、手袋喷胶及其制备方法 - Google Patents
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Abstract
本发明公开了一种水性箱包、手袋喷胶及其制备方法，涉及聚氨酯技术领域，其按重量份包括以下原料：聚丙二醇40‑50份、聚碳酸酯二元醇10‑16份、端羟基聚丁二烯10‑16份、2,4'‑二苯基甲烷二异氰酸酯15‑25份、甲基丙烯酸甲酯7‑15份、1,4‑丁二醇10‑20份、三羟甲基丙烷1‑2份、改性氧化石墨烯1‑4份、二月桂酸二丁基锡0.05‑0.5份、硅烷偶联剂3‑5份、高岭土3‑7份、抗氧剂0.1‑0.5份、增塑剂0.05‑1份。本发明制备的聚氨酯喷胶具有力学性能佳、耐水解、不易黄变、稳定性好等优点，能够与几乎所有的帆布、织物、纸板、铝塑板、尼龙带进行贴合，且即喷即粘，可用于箱包、手袋、革制品等胶粘用；其制备零VOC排放，水性环保、安全可靠，有很好的社会和经济效益。
Description
技术领域
本发明涉及聚氨酯技术领域，尤其涉及一种水性箱包、手袋喷胶及其制备方法。
背景技术
胶黏剂是现代工业发展中必不可少的重要材料之一，粘接技术在现代国民经济的各个领域中发挥着重大作用。聚氨酯胶黏剂是指在分子链中含有氨基甲酸酯基团(-NHCOO-)或异氰酸酯基(-NCO)的胶黏剂，其具有高度的活性与极性，与多种材料如泡沫塑料、木材、皮革、织物、纸张、陶瓷等多孔材料，以及金属、玻璃、橡胶、塑料等表面光洁的材料都有优良的化学粘结力，此外，聚氨酯胶黏剂还具有良好的韧性、可调节性、粘合工艺简便、极佳的耐低温性能以及优良的稳定性等特性。正是由于聚氨酯胶黏剂这种优良的粘接性能和对多种基材的粘接适应性，使其应用领域不断扩大，被普遍应用于汽车、家具、建筑、纺织等领域。
但由于聚氨酯胶黏剂的耐高温和耐水性能一般，在某些特殊粘合环境中，大分子中的活泼基团因高温或者与活性介质分子发生水解、氧化等化学反应，大分子主价键发生破坏、裂解，导致粘接强度下降，出现不耐酸碱或者不耐水等问题。将聚氨酯胶黏剂用于箱包、手袋加工，存在粘接强度不高、耐水解性能不佳、易发生黄变等问题。
发明内容
基于背景技术存在的技术问题，本发明提出了一种水性箱包、手袋喷胶及其制备方法。
本发明提出的一种水性箱包、手袋喷胶，其按重量份包括以下原料：聚丙二醇40-50份、聚碳酸酯二元醇10-16份、端羟基聚丁二烯10-16份、2,4'-二苯基甲烷二异氰酸酯15-25份、甲基丙烯酸甲酯7-15份、1,4-丁二醇10-20份、三羟甲基丙烷1-2份、改性氧化石墨烯1-4份、二月桂酸二丁基锡0.05-0.5份、硅烷偶联剂3-5份、高岭土3-7份、抗氧剂0.1-0.5份、增塑剂0.05-1份。
优选地，所述改性氧化石墨烯的制备如下：将氧化石墨烯分散到水中，然后加入EDC和NHS，搅拌，再加入氨基二氧化硅，升温，搅拌反应，最后加入乙二胺，搅拌反应，离心，洗涤，干燥，即得改性氧化石墨烯。
优选地，所述改性氧化石墨烯的制备如下：将氧化石墨烯分散到水中，然后加入EDC和NHS，搅拌20-30min，再加入氨基二氧化硅，升温至40-50℃，搅拌反应7-10h，最后加入乙二胺，搅拌反应1.5-2.5h，离心，洗涤，干燥，即得改性氧化石墨烯。
优选地，所述改性氧化石墨烯的制备中，氧化石墨烯、EDC、NHS、氨基二氧化硅、乙二胺的重量比为1：1.2-1.5：0.3-0.6：3-5：0.3-0.5。
优选地，所述聚碳酸酯多元醇为聚碳酸亚己酯二醇。
本发明还提出了上述水性箱包、手袋喷胶的制备方法，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸酯二元醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至80-85℃反应2-3h，降温至70-75℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应1.5-2.5h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应3-5h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，乳化分散60-90min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
优选地，S2中，乳化分散的转速为4000-6000r/min。
有益效果：本发明采用聚醚多元醇、聚碳酸酯多元醇、端羟基聚丁二烯为多元醇单体，以二苯基甲烷二异氰酸酯为异氰酸酯单体，制得的聚氨酯预聚体具有良好的耐热性、耐水解性和力学性能。
改性氧化石墨烯制备中，利用氧化石墨烯表面羧基、环氧基等活性基团与氨基二氧化硅表面的氨基发生酰胺缩合反应，使得氧化石墨烯包覆在二氧化硅表面形成核壳结构，再采用乙二胺试剂对氧化石墨烯表面进行改性，使其表面带有氨基；将该改性氧化石墨烯添加到聚氨酯预聚体中，其在扩链过程中参与反应从而嵌入到聚氨酯链段中，提高材料的耐温性、拉伸强度和剥离强度。
本发明制备的聚氨酯交联剂乳液具有力学性能佳、耐水解、不易黄变、稳定性好，能够与几乎所有的帆布、织物、纸板、铝塑板、尼龙带进行贴合，且即喷即粘，可用于箱包、手袋、革制品等胶粘用；且其制备零VOC排放，水性环保、安全可靠，有很好的社会和经济效益。
具体实施方式
下面，通过具体实施例对本发明的技术方案进行详细说明。
实施例1
本发明提出的一种水性箱包、手袋喷胶，其按重量份包括以下原料：聚丙二醇40份、聚碳酸亚己酯二醇16份、端羟基聚丁二烯16份、2,4'-二苯基甲烷二异氰酸酯15份、甲基丙烯酸甲酯7份、1,4-丁二醇10份、三羟甲基丙烷2份、改性氧化石墨烯1份、二月桂酸二丁基锡0.05份、硅烷偶联剂3份、高岭土3份、抗氧剂0.1份、增塑剂0.05份；
其中，改性氧化石墨烯的制备如下：将1份氧化石墨烯分散到水中，然后加入1.2份EDC和0.3份NHS，搅拌20min，再加入3份氨基二氧化硅，升温至40℃，搅拌反应10h，最后加入0.3份乙二胺，搅拌反应1.5h，离心，洗涤，干燥，即得改性氧化石墨烯。
本发明还提出了上述水性箱包、手袋喷胶的制备方法，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸亚己酯二醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至80℃反应3h，降温至70℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应1.5h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应3h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，于4000r/min转速下高速乳化分散90min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
实施例2
本发明提出的一种水性箱包、手袋喷胶，其按重量份包括以下原料：聚丙二醇50份、聚碳酸亚己酯二醇10份、端羟基聚丁二烯10份、2,4'-二苯基甲烷二异氰酸酯25份、甲基丙烯酸甲酯15份、1,4-丁二醇20份、三羟甲基丙烷1份、改性氧化石墨烯4份、二月桂酸二丁基锡0.5份、硅烷偶联剂5份、高岭土7份、抗氧剂00.5份、增塑剂1份；
其中，改性氧化石墨烯的制备如下：将1份氧化石墨烯分散到水中，然后加入1.5份EDC和0.6份NHS，搅拌30min，再加入5份氨基二氧化硅，升温至50℃，搅拌反应7h，最后加入0.5份乙二胺，搅拌反应2.5h，离心，洗涤，干燥，即得改性氧化石墨烯。
本发明还提出了上述水性箱包、手袋喷胶的制备方法，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸亚己酯二醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至85℃反应2h，降温至75℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应2.5h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应5h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，于6000r/min转速下高速乳化分散60min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
实施例3
本发明提出的一种水性箱包、手袋喷胶，其按重量份包括以下原料：聚丙二醇44份、聚碳酸亚己酯二醇15份、端羟基聚丁二烯13份、2,4'-二苯基甲烷二异氰酸酯22份、甲基丙烯酸甲酯9份、1,4-丁二醇17份、三羟甲基丙烷1.5份、改性氧化石墨烯1.5份、二月桂酸二丁基锡0.1份、硅烷偶联剂3.5份、高岭土5份、抗氧剂0.2份、增塑剂0.2份。
其中，将1份氧化石墨烯分散到水中，然后加入1.3份EDC和0.4份NHS，搅拌25min，再加入3.5份氨基二氧化硅，升温至45℃，搅拌反应8h，最后加入0.4份乙二胺，搅拌反应1.5h，离心，洗涤，干燥，即得改性氧化石墨烯。。
本发明还提出了上述水性箱包、手袋喷胶的制备方法，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸亚己酯二醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至80℃反应2h，降温至75℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应2h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应4h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，于5000r/min转速下高速乳化分散60min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
实施例4
本发明提出的一种水性箱包、手袋喷胶，其按重量份包括以下原料：聚丙二醇47份、聚碳酸亚己酯二醇12份、端羟基聚丁二烯12份、2,4'-二苯基甲烷二异氰酸酯24份、甲基丙烯酸甲酯12份、1,4-丁二醇16份、三羟甲基丙烷1份、改性氧化石墨烯2.5份、二月桂酸二丁基锡0.5份、硅烷偶联剂4份、3高岭土6份、抗氧剂0.2份、增塑剂0.5份。
其中，将1份氧化石墨烯分散到水中，然后加入1.4份EDC和0.5份NHS，搅拌30min，再加入4份氨基二氧化硅，升温至50℃，搅拌反应9h，最后加入0.5份乙二胺，搅拌反应2h，离心，洗涤，干燥，即得改性氧化石墨烯。。
本发明还提出了上述水性箱包、手袋喷胶的制备方法，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸亚己酯二醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至85℃反应2.5h，降温至75℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应2h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应5h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，于5000r/min转速下高速乳化分散70min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
对比例
与实施例2相比，区别仅在于：氧化石墨烯未经改性处理。
对本发明实施例1-4和对比例中制备的水性聚氨酯喷胶的性能进行检测，检测标准为GB 19340-2014，结果如表1所示。
表1实施例1-4和对比例中制备的喷胶的性能数据
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 对比例 | |
| 初粘性N/mm | 1.5 | 1.7 | 1.5 | 1.8 | 1.1 |
| 剥离强度N/mm | 3.1 | 3.4 | 3.5 | 3.0 | 2.4 |
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (7)
1.一种水性箱包、手袋喷胶，其特征在于，其按重量份包括以下原料：聚丙二醇40-50份、聚碳酸酯二元醇10-16份、端羟基聚丁二烯10-16份、2,4'-二苯基甲烷二异氰酸酯15-25份、甲基丙烯酸甲酯7-15份、1,4-丁二醇10-20份、三羟甲基丙烷1-2份、改性氧化石墨烯1-4份、二月桂酸二丁基锡0.05-0.5份、硅烷偶联剂3-5份、高岭土3-7份、抗氧剂0.1-0.5份、增塑剂0.05-1份。
2.根据权利要求1所述的水性箱包、手袋喷胶，其特征在于，所述改性氧化石墨烯的制备如下：将氧化石墨烯分散到水中，然后加入EDC和NHS，搅拌，再加入氨基二氧化硅，升温，搅拌反应，最后加入乙二胺，搅拌反应，离心，洗涤，干燥，即得改性氧化石墨烯。
3.根据权利要求2所述的水性箱包、手袋喷胶，其特征在于，所述改性氧化石墨烯的制备如下：将氧化石墨烯分散到水中，然后加入EDC和NHS，搅拌20-30min，再加入氨基二氧化硅，升温至40-50℃，搅拌反应7-10h，最后加入乙二胺，搅拌反应1.5-2.5h，离心，洗涤，干燥，即得改性氧化石墨烯。
4.根据权利要求2或3所述的水性箱包、手袋喷胶，其特征在于，所述改性氧化石墨烯的制备中，氧化石墨烯、EDC、NHS、氨基二氧化硅、乙二胺的重量比为1：1.2-1.5：0.3-0.6：3-5：0.3-0.5。
5.根据权利要求1所述的水性箱包、手袋喷胶，其特征在于，所述聚碳酸酯多元醇为聚碳酸亚己酯二醇。
6.一种基于权利要求1-5任一项所述的水性箱包、手袋喷胶的制备方法，其特征在于，包括以下步骤：
S1、将经脱水处理后的聚丙二醇、聚碳酸酯二元醇、端羟基聚丁二烯加入到反应容器中，加入2,4'-二苯基甲烷二异氰酸酯和甲基丙烯酸甲酯，滴入二月桂酸二丁基锡，升温至80-85℃反应2-3h，降温至70-75℃，然后加入1,4-丁二醇、三羟甲基丙烷、改性氧化石墨烯和适量丙酮，搅拌反应1.5-2.5h，降至室温，加入三乙胺进行中和；
S2、将高岭土加入到硅烷偶联剂的乙醇溶液中，搅拌反应3-5h，然后与抗氧剂、增塑剂一起加入到S1的反应体系中，乳化分散60-90min，减压蒸馏除去丙酮，即得水性聚氨酯胶黏剂。
7.根据权利要求6所述的水性箱包、手袋喷胶的制备方法，其特征在于，S2中，乳化分散的转速为4000-6000r/min。
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