CN110734530B - 一种改性聚氨酯面料树脂及其制备方法 - Google Patents
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Abstract
本发明公开了一种改性聚氨酯面料树脂及其制备方法，包括卷筒、固定槽、固定辊和改性聚氨酯面料树脂本体，本发明通过设置了改性聚氨酯面料树脂本体，微胶囊填充型自修复涂层能够具有优良的抵抗裂纹扩展的能力和耐蚀性，从而增加改性聚氨酯面料树脂本体的耐火性，并且通过设置了第一加固凸块和第二加固凸块起到增加改性聚氨酯面料树脂层和双组分聚氨酯胶粘剂固定稳定性的作用，并且加固层具有优异的耐高温性，同时增设了改性碳纳米管，改性碳纳米管具有极高的强度、韧性和弹性模量，达到了增加聚氨酯面料树脂的强度和耐热性的优点。
Description
技术领域
本发明涉及改性聚氨酯面料树脂相关领域，具体是一种改性聚氨酯面料树脂及其制备方法。
背景技术
聚氨酯由于其原料品种及组成的多样性，因而可合成各种各样性能的高分子材料，例如从其本体材料(即不含溶剂)的外观性严主讲，可得到由柔软至坚硬的弹性体，泡沫材料，聚氨酯从其本体性质(或者说其固化物)而言，基本上届弹性体性质，它的一些物理化学性质如粘接强度，机械性能，耐久性，耐低温性，耐药品性，主要取决于所生成的聚氨酯固化物的化学结构。
由有机硅低聚物与聚氨酯树脂共同制成的一类改性树脂，一般以含活性羟基的聚酯树脂组分先与含活性羟基(或烷氧基)的有机硅低聚物反应，生成仍富含活性羟基的有机硅改性聚酯，然后以异氰酸酯组分作为交联剂制成，多用于制备双组分聚氨酯漆，能在常温固化，提高其耐热性和耐候性，现在的聚氨酯面料树脂强度不高，耐热性能差，在高温下易软化分解，使其机械性能急剧下降，一般情况下，在温度超过80℃时不能长期使用，而短期温度不能超过120℃。
本发明内容
因此，为了解决上述不足，本发明在此提供一种改性聚氨酯面料树脂及其制备方法。
本发明是这样实现的，构造一种改性聚氨酯面料树脂及其制备方法，该装置包括包括卷筒、固定槽、固定辊和改性聚氨酯面料树脂本体，所述卷筒中部开设有固定槽，所述固定辊采用间隙配合的方式贯穿于固定槽内侧，并且固定辊与固定槽内侧转动配合，所述卷筒上端缠绕有改性聚氨酯面料树脂本体，所述改性聚氨酯面料树脂本体包括微胶囊填充型自修复涂层、第一加固凸块、改性聚氨酯面料树脂层、改性碳纳米管、V形加固块、加固层、双组分聚氨酯胶粘剂和第二加固凸块，所述微胶囊填充型自修复涂层上端等距分布有第一加固凸块，所述改性聚氨酯面料树脂层与微胶囊填充型自修复涂层上端无缝粘合，所述改性聚氨酯面料树脂层内部等距分布有改性碳纳米管，所述加固层将微胶囊填充型自修复涂层和双组分聚氨酯胶粘剂左右两侧覆盖，所述加固层右端固定有V形加固块，所述微胶囊填充型自修复涂层与双组分聚氨酯胶粘剂下端无缝粘合，所述微胶囊填充型自修复涂层采用原位聚合法制备了内含二聚环戊二烯的脲醛树脂微胶囊，所述加固层为合成半PU革用聚氨酯树脂。
优选的，所述第一加固凸块和第二加固凸块均由两个大小不一的梯形凸起构成。
优选的，所述改性碳纳米管的质量百分含量为0.02wt.％～5wt.％。
优选的，所述双组分聚氨酯胶粘剂由含端羟基的主剂和含端NCO基团的固化剂组成。
本发明具有如下优点：本发明通过改进在此提供一种改性聚氨酯面料树脂及其制备方法，与同类型设备相比，具有如下改进：
本发明所述一种改性聚氨酯面料树脂及其制备方法，通过设置了改性聚氨酯面料树脂本体，微胶囊填充型自修复涂层能够具有优良的抵抗裂纹扩展的能力和耐蚀性，从而增加改性聚氨酯面料树脂本体的耐火性，并且通过设置了第一加固凸块和第二加固凸块起到增加改性聚氨酯面料树脂层和双组分聚氨酯胶粘剂固定稳定性的作用，并且加固层具有优异的耐高温性，同时增设了改性碳纳米管，改性碳纳米管具有极高的强度、韧性和弹性模量，达到了增加聚氨酯面料树脂的强度和耐热性的优点。
附图说明
图1是本发明结构示意图；
图2是本发明改性聚氨酯面料树脂本体剖面结构示意图；
图3是本发明制备流程结构示意图；
图4是本发明加固层质量结构示意图。
其中：卷筒-1、固定槽-2、固定辊-3、改性聚氨酯面料树脂本体-4、微胶囊填充型自修复涂层-41、第一加固凸块-42、改性聚氨酯面料树脂层-43、改性碳纳米管-44、V形加固块-45、加固层-46、双组分聚氨酯胶粘剂-47、第二加固凸块-48。
具体实施方式
下面将结合附图1-4对本发明进行详细说明，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明通过改进在此提供一种改性聚氨酯面料树脂及其制备方法，包括包括卷筒1、固定槽2、固定辊3和改性聚氨酯面料树脂本体4，所述卷筒1中部开设有固定槽2，所述固定辊3采用间隙配合的方式贯穿于固定槽2内侧，并且固定辊3与固定槽2内侧转动配合，所述卷筒1上端缠绕有改性聚氨酯面料树脂本体4，所述改性聚氨酯面料树脂本体4包括微胶囊填充型自修复涂层41、第一加固凸块42、改性聚氨酯面料树脂层43、改性碳纳米管44、V形加固块45、加固层46、双组分聚氨酯胶粘剂47和第二加固凸块48，所述微胶囊填充型自修复涂层41上端等距分布有第一加固凸块42，所述改性聚氨酯面料树脂层43与微胶囊填充型自修复涂层41上端无缝粘合，所述改性聚氨酯面料树脂层43内部等距分布有改性碳纳米管44，所述加固层46将微胶囊填充型自修复涂层41和双组分聚氨酯胶粘剂47左右两侧覆盖，所述加固层46右端固定有V形加固块45，所述微胶囊填充型自修复涂层41与双组分聚氨酯胶粘剂47下端无缝粘合，所述微胶囊填充型自修复涂层41采用原位聚合法制备了内含二聚环戊二烯的脲醛树脂微胶囊，所述加固层46为合成半PU革用聚氨酯树脂。
进一步的，所述第一加固凸块42和第二加固凸块48均由两个大小不一的梯形凸起构成。
进一步的，所述改性碳纳米管44的质量百分含量为0.02wt.％～5wt.％。
进一步的，所述双组分聚氨酯胶粘剂47由含端羟基的主剂和含端NCO基团的固化剂组成。
进一步的，包括以下步骤：
步骤一：原材料的准备和混合：
将微胶囊填充型自修复涂层41、改性碳纳米管44和加固层46进行分别制备；
步骤二：改性碳纳米管的制备：
25℃下，将0.7g碳纳米管加入到砂芯酸化器中，将砂芯酸化器悬空置于含有2.5mL硝酸的80mL密闭反应釜中，然后升温至150℃，酸化4.5h，反应结束冷却至室温，除去硝酸溶液，70℃真空烘箱干燥后得到酸化碳纳米管，然后取0.1g酸化碳纳米管加入到反应器中，超声分散1.5h，用质量分数为20wt.％～30wt.％的氨水调节pH至8.0～11.0，用恒压滴液漏斗向反应体系中在1.5h内滴加含有1mL正硅酸四乙酯和1mL钛酸正丁酯的60mL乙醇混合溶液，反应8h，过滤，用60mL乙醇洗涤五次，然后用60mL去离子水洗涤五次，在80℃真空烘箱中干燥36h，得改性碳纳米管44；
步骤三：微胶囊填充型自修复涂层的制备：
把内含二聚环戊二烯的脲醛树脂微胶囊与催化剂同时加入反应釜中，由于内含二聚环戊二烯的脲醛树脂微胶囊在介质中是可溶的，而其聚合物在整个体系中不可溶，所以聚合反应在分散相与连续相的界面上发生，反应原料逐渐聚合，当反应产物反应到一定体积后，将逐渐沉积在芯材物质的表面，从而形成微胶囊填充型自修复涂层，并且原位聚合反应的芯材为乙烯、石蜡、环氧树脂、甲基丙烯酸甲酯；
步骤四：加固层的制备：
依次将8-25％的聚酯多元醇、1-6％的聚碳酸酯多元醇、1-3％的聚乙二醇投入反应釜中，并搅拌均匀，随后加入含量为35-65％的二甲基乙酰胺，升温至35-65℃，并充分搅拌20-35分钟，接下来加入含量为8-25％的二苯基甲烷二异氰酸酯和0-0.01％的环保锡催化剂，保持搅拌，升温至65-85℃，反应3小时，最后加入余下的二甲基乙酰胺，形成加固层46；
步骤五：最终产品的制备：
将制备后的微胶囊填充型自修复涂层41、改性碳纳米管44、加固层46和双组分聚氨酯胶粘剂47在改性聚氨酯面料树脂层43上端进行热压平成型。
本发明通过改进提供一种改性聚氨酯面料树脂及其制备方法，按照如下方式运行；
第一，在使用时，首先进行原材料的准备和混合，将胶囊填充型自修复涂层41、改性碳纳米管44和加固层46进行分别制备；
第二，随后，25℃下，将0.7g碳纳米管加入到砂芯酸化器中，将砂芯酸化器悬空置于含有2.5mL(质量分数70wt.％)硝酸的80mL密闭反应釜中，然后升温至150℃，酸化4.5h。反应结束冷却至室温，除去硝酸溶液，70℃真空烘箱干燥后得到酸化碳纳米管。然后取0.1g酸化碳纳米管加入到反应器中，超声分散1.5h。用质量分数为20wt.％～30wt.％的氨水调节pH至8.0～11.0，用恒压滴液漏斗向反应体系中在1.5h内滴加含有1mL正硅酸四乙酯和1mL钛酸正丁酯的60mL乙醇混合溶液，反应8h。过滤，用60mL乙醇洗涤五次，然后用60mL去离子水洗涤五次，在80℃真空烘箱中干燥36h，得改性碳纳米管44，对改性碳纳米管44进行制备；
第三，然后，把内含二聚环戊二烯(DCPD)的脲醛树脂(UF)微胶囊(DCPD-UF)与催化剂同时加入反应釜中，由于内含二聚环戊二烯(DCPD)的脲醛树脂(UF)微胶囊(DCPD-UF)在介质中是可溶的，而其聚合物在整个体系中不可溶，所以聚合反应在分散相与连续相的界面上发生，反应原料逐渐聚合，当反应产物反应到一定体积后，将逐渐沉积在芯材物质的表面，从而形成胶囊填充型自修复涂层41，并且常用于原位聚合反应的芯材有乙烯、石蜡、环氧树脂、甲基丙烯酸甲脂等，对胶囊填充型自修复涂层41进行制备；
第四，接下来，依次将8-25％的聚酯多元醇、1-6％的聚碳酸酯多元醇、1-3％的聚乙二醇，并搅拌均匀，随后加入含量为35-65％的二甲基乙酰胺，升温至35-65℃，并充分搅拌20-35分钟，接下来加入含量为8-25％的二苯基甲烷二异氰酸酯和0-0.01％的环保锡催化剂，保持搅拌，升温至65-85℃，反应3小时，最后加入余下的二甲基乙酰胺，对加固层46进行制备；
第五，随后将制备后的微胶囊填充型自修复涂层41、改性碳纳米管44、加固层46和双组分聚氨酯胶粘剂47在改性聚氨酯面料树脂层43上端通过粘合胶进行热压平成型；
第六，通过设置了改性聚氨酯面料树脂本体4，微胶囊填充型自修复涂层41能够具有优良的抵抗裂纹扩展的能力和耐蚀性，从而增加改性聚氨酯面料树脂本体4的耐火性，并且通过设置了第一加固凸块42和第二加固凸块48起到增加改性聚氨酯面料树脂层43和双组分聚氨酯胶粘剂47固定稳定性的作用，并且加固层46具有优异的耐高温性，同时增设了改性碳纳米管44，改性碳纳米管44具有极高的强度、韧性和弹性模量，达到了增加聚氨酯面料树脂的强度和耐热性。
本发明通过改进提供一种改性聚氨酯面料树脂及其制备方法，通过设置了改性聚氨酯面料树脂本体4，微胶囊填充型自修复涂层41能够具有优良的抵抗裂纹扩展的能力和耐蚀性，从而增加改性聚氨酯面料树脂本体4的耐火性，并且通过设置了第一加固凸块42和第二加固凸块48起到增加改性聚氨酯面料树脂层43和双组分聚氨酯胶粘剂47固定稳定性的作用，并且加固层46具有优异的耐高温性，同时增设了改性碳纳米管44，改性碳纳米管44具有极高的强度、韧性和弹性模量，达到了增加聚氨酯面料树脂的强度和耐热性的优点。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点,并且本发明使用到的标准零件均可以从市场上购买,异形件根据说明书的和附图的记载均可以进行订制,各个零件的具体连接方式均采用现有技术中成熟的螺栓铆钉、焊接等常规手段，机械、零件和设备均采用现有技术中,常规的型号,加上电路连接采用现有技术中常规的连接方式,在此不再详述。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (5)
1.一种改性聚氨酯面料树脂，包括卷筒(1)、固定槽(2)和固定辊(3)，所述卷筒(1)中部开设有固定槽(2)，所述固定辊(3)采用间隙配合的方式贯穿于固定槽(2)内侧，并且固定辊(3)与固定槽(2)内侧转动配合；
其特征在于：还包括改性聚氨酯面料树脂本体(4)，所述卷筒(1)上端缠绕有改性聚氨酯面料树脂本体(4)，所述改性聚氨酯面料树脂本体(4)包括微胶囊填充型自修复涂层(41)、第一加固凸块(42)、改性聚氨酯面料树脂层(43)、改性碳纳米管(44)、V形加固块(45)、加固层(46)、双组分聚氨酯胶粘剂(47)和第二加固凸块(48)，所述微胶囊填充型自修复涂层(41)上端等距分布有第一加固凸块(42)，所述改性聚氨酯面料树脂层(43)与微胶囊填充型自修复涂层(41)上端无缝粘合，所述改性聚氨酯面料树脂层(43)内部等距分布有改性碳纳米管(44)，所述加固层(46)将微胶囊填充型自修复涂层(41)和双组分聚氨酯胶粘剂(47)左右两侧覆盖，所述加固层(46)右端固定有V形加固块(45)，所述微胶囊填充型自修复涂层(41)与双组分聚氨酯胶粘剂(47)下端无缝粘合，所述微胶囊填充型自修复涂层(41)采用原位聚合法制备了内含二聚环戊二烯的脲醛树脂微胶囊，所述加固层(46)为合成半PU革用聚氨酯树脂。
2.根据权利要求1所述一种改性聚氨酯面料树脂，其特征在于：所述第一加固凸块(42)和第二加固凸块(48)均由两个大小不一的梯形凸起构成。
3.根据权利要求1所述一种改性聚氨酯面料树脂，其特征在于：所述改性碳纳米管(44)的质量百分含量为0.02wt.％～5wt.％。
4.根据权利要求1所述一种改性聚氨酯面料树脂，其特征在于：所述双组分聚氨酯胶粘剂(47)由含端羟基的主剂和含端NCO基团的固化剂组成。
5.根据权利要求1-4任一项所述一种改性聚氨酯面料树脂的制备方法，其特征在于：包括以下步骤：
步骤一：原材料的准备和混合：
将微胶囊填充型自修复涂层(41)、改性碳纳米管(44)和加固层(46)进行分别制备；
步骤二：改性碳纳米管的制备：
25℃下，将0.7g碳纳米管加入到砂芯酸化器中，将砂芯酸化器悬空置于含有2.5mL硝酸的80mL密闭反应釜中，然后升温至150℃，酸化4.5h，反应结束冷却至室温，除去硝酸溶液，70℃真空烘箱干燥后得到酸化碳纳米管，然后取0.1g酸化碳纳米管加入到反应器中，超声分散1.5h，用质量分数为20wt.％～30wt.％的氨水调节pH至8.0～11.0，用恒压滴液漏斗向反应体系中在1.5h内滴加含有1mL正硅酸四乙酯和1mL钛酸正丁酯的60mL乙醇混合溶液，反应8h，过滤，用60mL乙醇洗涤五次，然后用60mL去离子水洗涤五次，在80℃真空烘箱中干燥36h，得改性碳纳米管(44)；
步骤三：微胶囊填充型自修复涂层的制备：
把内含二聚环戊二烯的脲醛树脂微胶囊与催化剂同时加入反应釜中，由于内含二聚环戊二烯的脲醛树脂微胶囊在介质中是可溶的，而其聚合物在整个体系中不可溶，所以聚合反应在分散相与连续相的界面上发生，反应原料逐渐聚合，当反应产物反应到一定体积后，将逐渐沉积在芯材物质的表面，从而形成微胶囊填充型自修复涂层，并且原位聚合反应的芯材为乙烯、石蜡、环氧树脂、甲基丙烯酸甲酯；
步骤四：加固层的制备：
依次将8-25％的聚酯多元醇、1-6％的聚碳酸酯多元醇、1-3％的聚乙二醇投入反应釜中，并搅拌均匀，随后加入含量为35-65％的二甲基乙酰胺，升温至35-65℃，并充分搅拌20-35分钟，接下来加入含量为8-25％的二苯基甲烷二异氰酸酯和0-0.01％的环保锡催化剂，保持搅拌，升温至65-85℃，反应3小时，最后加入余下的二甲基乙酰胺，形成加固层(46)；
步骤五：最终产品的制备：
将制备后的微胶囊填充型自修复涂层(41)、改性碳纳米管(44)、加固层(46)和双组分聚氨酯胶粘剂(47)在改性聚氨酯面料树脂层(43)上端进行热压平成型。
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