CN105694750A - 一种新型耐高温聚氯乙烯胶带的制作方法 - Google Patents

一种新型耐高温聚氯乙烯胶带的制作方法 Download PDF

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CN105694750A
CN105694750A CN201610073413.1A CN201610073413A CN105694750A CN 105694750 A CN105694750 A CN 105694750A CN 201610073413 A CN201610073413 A CN 201610073413A CN 105694750 A CN105694750 A CN 105694750A
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polyvinyl chloride
coating
plasticizer
ultraviolet light
temperature
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王凤
黄志达
金春明
李爽
杨玉昆
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Hebei Yongle Tape Co Ltd
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HEBEI HUAXIA ENTERPRISE CO Ltd
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Application filed by HEBEI HUAXIA ENTERPRISE CO Ltd filed Critical HEBEI HUAXIA ENTERPRISE CO Ltd
Priority to CN201610073413.1A priority Critical patent/CN105694750A/zh
Priority to CN202011308233.XA priority patent/CN112500805A/zh
Priority to ES16888943T priority patent/ES2879991T3/es
Priority to US16/074,608 priority patent/US20190055433A1/en
Priority to EP21178815.3A priority patent/EP3916064B1/en
Priority to KR1020187025099A priority patent/KR102521225B1/ko
Priority to ES16888944T priority patent/ES2812204T5/es
Priority to EP16888943.4A priority patent/EP3412741B1/en
Priority to PCT/CN2016/081908 priority patent/WO2017133121A1/zh
Priority to JP2018541302A priority patent/JP6775025B2/ja
Priority to PCT/CN2016/081923 priority patent/WO2017133122A1/zh
Priority to CN201680080847.2A priority patent/CN108603081A/zh
Priority to US16/074,965 priority patent/US20190040288A1/en
Priority to EP16888944.2A priority patent/EP3412742B2/en
Priority to KR1020187025105A priority patent/KR102547510B1/ko
Priority to JP2018541363A priority patent/JP6861215B2/ja
Priority to CN201680002203.1A priority patent/CN107960097B/zh
Priority to ES21178815T priority patent/ES2936804T3/es
Publication of CN105694750A publication Critical patent/CN105694750A/zh
Priority to HK18114365.8A priority patent/HK1255534A1/zh
Priority to US17/145,537 priority patent/US20210371709A1/en
Priority to US17/385,086 priority patent/US20220186084A1/en
Pending legal-status Critical Current

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Abstract

本发明涉及一种将可紫外光交联的热熔压敏粘合剂施用于耐高温的聚氯乙烯膜上制作成耐高温胶带的方法和生产工艺。耐高温的聚氯乙烯膜是含液体高分子型增塑剂、固体高分子增塑剂和热稳定剂的耐高温型材料。热熔压敏粘合剂可在130-150℃下直接涂布于耐高温聚氯乙烯膜上，然后用紫外光进行交联固化，制成耐高温聚氯乙烯胶带。相对传统的聚氯乙烯胶带具有无挥发性，耐高温和环保性高等优点。

Description

一种新型耐高温聚氯乙烯胶带的制作方法
技术领域
本发明涉及一种将可紫外光交联的热熔压敏粘合剂施用于耐高温的聚氯乙烯膜上制成胶带的方法和生产工艺。耐高温的聚氯乙烯膜是含液体高分子型增塑剂、固体高分子增塑剂和热稳定剂的耐高温型材料。热熔压敏粘合剂可在130-150℃下直接涂布于耐高温的聚氯乙烯膜上，然后用紫外光进行辐照交联制成聚氯乙烯胶带。
以软聚氯乙烯(SPVC)薄膜为基材的电气压敏胶带因其具有优良的机械性能，阻燃性能，电绝缘性能，耐热变形性能和优越的加工应用性能等而广泛应用于汽车，机械制造，仪器仪表和家电等领域。但聚氯乙烯薄膜基材含有低分子增塑剂如邻苯二甲酸二辛酯(DOP)，邻苯二甲酸二丁酯(DBP)和磷酸三正丁酯(TBP)等，具有较差的耐温性能。另外这些低分子增塑剂会迁移到胶粘剂层中致使胶带的粘合力下降，从而无法达到工业上的应用要求。传统的高分子聚氯乙烯提高了耐高温性能，但无法在大于120℃的高温下涂布。
目前工业上的软聚氯乙烯胶带产品都是用溶剂型橡胶压敏粘合剂直接涂布于软聚氯乙烯薄膜上制成的。溶剂型橡胶压敏粘合剂中含大量有机溶剂，一般为甲苯。在涂布过程中，有机溶剂会部分挥发到大气造成环境污染。所得的聚氯乙烯胶带也含有溶剂残留，残留溶剂会在使用过程中缓慢释放出来而污染到使用环境，如汽车的室内环境。完全不能满足欧盟委员会颁布的《关于在电子电气中限制使用某些有物质指令》(ROHS指令)要求。而且溶剂型橡胶压敏粘合剂的涂布工艺所用能耗较高，涂布设备的占地面积较大，因而生产成本较高。
紫外光交联的热熔压敏粘合剂具有很好的环保性，而且所需设备小巧，能耗较低，因而生产成本较低。更重要的是这种类型压敏粘合剂具有较好的抗增塑剂性能，高分子增塑剂的迁移不会导致胶带的性能下降很大。因此这类热熔压敏粘合剂能广泛满足工业上的需求。但用低分子增塑剂和传统高分子增塑剂增塑的聚氯乙烯膜，其耐温性能都不够高。涂布时候为了防止聚氯乙烯膜受到热破坏，只能降低涂布时的温度，并使用能量较低的紫外灯。降低涂布温度，粘合剂的粘度变高，流动性能变差，会导致涂层的不均匀。这样就会限制涂布速度，降低生产效率。我们的专利CN101372607描述了乳液压敏粘合剂粘剂在聚氯乙烯膜上的应用。但在耐高温和耐湿性能上，紫外光交联型热熔粘合剂的性能具有更大的优势。
发明内容
本发明提供了一种新的耐高温聚氯乙烯胶带的制作方法。这种制作方法是：将可紫外光交联的热熔压敏粘合剂在130-150℃温度下直接热熔涂布于耐高温聚氯乙烯薄膜基材上，再经紫外光辐照交联制成这种新的耐高温聚氯乙烯胶带。
这种新的耐高温聚氯乙烯胶带的制作方法，采用了耐高温型聚氯乙烯薄膜作为基材。这种耐高温聚氯乙烯薄膜除主体聚氯乙烯树脂外，还采用了液体高分子增塑剂、固体高分子增塑剂和热稳定剂。本发明所采用的液体高分子增塑剂是液体己二酸乙二醇聚酯增塑剂和液体己二酸丙二醇聚酯增塑剂等；所用的固体高分子增塑剂是乙烯-醋酸乙烯共聚物(EVA)、乙烯-丙烯酸甲酯共聚物(EMA)、乙烯-丙烯酸乙酯共聚物(EEA)、乙烯-丙烯酸丁酯共聚物(EBA)、丁腈橡胶粉(NBR)和氯化聚乙烯(CPE)等；所用的热稳定剂是非铅类的液体或固体钡锌稳定剂、镉钡锌稳定剂、钙锌稳定剂、有机锡类稳定剂等。此外，根据需要还采用一些色料和填料。
这种耐高温聚氯乙烯薄膜基材的采用可以把胶带的热熔涂布温度提高到150℃，从而加快了涂布速度，提高了生产效率。另外，这种聚氯乙烯膜中高分子增塑剂的应用，减低了膜中的增塑剂向胶层的迁移。也就是说，胶带在储存和使用过程中或经60-80℃的高温烘烤后，虽然可能发生了基材的少量增塑剂向胶层的迁移，但胶带的性能仍能保持满足工业上的应用需求。因此，用本发明这种制作方法制作的聚氯乙烯胶带具有环保、耐高温、低VOC等优良性能。
(紫外光交联的)总所周知，热熔压敏粘合剂不含溶剂，(所以)在涂布加工过程不需要溶剂回收体系，有环保和节能等优点。(常用的热熔压敏粘合剂的涂布方式是夹缝式挤压和淋膜式涂布。)相对于传统的水性和溶剂型压敏粘合剂的涂布设备，热熔压敏粘合剂的涂布设备占地面积小，操作需要的人工少，可以大大提高生产效率。热熔压敏粘合剂的熔融粘度是非常重要的一个参数，熔融粘度的大小直接影响到涂布速度的快慢。目前工业上采用的橡胶型热熔压敏粘合剂的熔融粘度一般都比较大，用以涂布聚氯乙烯(SPVC)薄膜来制造SPVC胶带时，只能采用复杂的转移涂布方法(即先将其涂布在防粘纸上干燥后再将胶层转移到SPVC薄膜上的方法)，无法采用简单的直接涂布方法。因为直接涂布时，必须(为了提高涂布速度，)升高橡胶型热熔压敏粘合剂的温度到150℃以上以降低其粘度，才能进行正常涂布(是最常用的一个办法)。但涂布时粘合剂温度的提高却会带来很多负面的影响，比如能破坏不耐高温的基材(尤其是SPVC基材)使其产生热变形甚至热降解，也能增加粘合剂的不稳定性。本发明采用的可紫外光交联的热熔压敏粘合剂的熔融粘度比橡胶型热熔压敏粘合剂低，可以在较低温度(130-150℃)下在SPVC基材上进行直接涂布，不会破坏软聚氯乙烯薄膜基材。本发明在涂布生产过程中还对SPVC基材进行冷却，以达到进一步的保护作用。
已知的可紫外光交联热熔压敏粘合剂的主要成份是丙烯酸酯类单体及其共聚合物的混合物。在丙烯酸酯类单体中，除了采用常用的丙烯酸正丁酯，丙烯酸异辛酯，丙烯酸，甲基丙烯酸，丙烯酸羟乙酯，丙烯酸羟丙酯外，还采用了甲基丙烯酰胺，N-羟甲基丙烯酰胺，N-丁氧基丙烯酰胺，β-CEA等特殊单体。其它特殊软单体比如丙烯酸正辛酯，顺丁烯二酸二丁酯，顺丁烯二酸二辛酯和丙烯酸降冰片酯或其混合物有时也被采用。为增加粘合力，可以使用松香树脂、萜烯树脂、石油树脂及其相应的氢化、酯化改性树脂等增粘树脂。为了防止粘合剂的老化，通常还加入适量的防老剂。紫外光交联的热熔压敏粘合剂还必须包含一种或多种光敏引发剂，最常用的光敏引发剂是苯乙酮和二苯甲酮的衍生物。光敏引发剂在紫外光的照射下，更具体说是UVc的辐射下，产生自由基团，从而使粘合剂中的丙烯酸酯类单体进一步聚合并使丙烯酸酯聚合物产生交联而固化。
在本发明所采用的可紫外光交联热熔压敏粘合剂的组成中，除上述各种成分外，还含有一种或多种可聚合光敏引发剂与丙烯酸酯单体的共聚物，或者含一种或多种可聚合光敏引发剂的低聚体和丙烯酸酯聚合物的混合物。这种可聚合光敏引发剂是含甲基丙烯酰氧基或丙烯酰氧基的苯乙酮或二苯甲酮衍生物。例如，2-羟基-4-(甲基丙烯酰氧基)二苯甲酮。因此，本发明所采用的可紫外光交联热熔压敏粘合剂的特征是含有一种或多种可聚合光敏引发剂与丙烯酸酯单体的共聚物，或者是含一种或多种可聚合光敏引发剂的低聚体和丙烯酸酯聚合物的混合物。含可聚合光敏引发剂的低聚体能降低热熔粘合剂的粘度，从而降低涂布温度，更好的保护聚氯乙烯基材。在可紫外光交联的热熔压敏粘合剂组成中采用高分子量光敏引发剂，可以进一步降低胶层的挥发性，使胶带更好地满足环保的要求。
本发明一种新的耐高温聚氯乙烯胶带的制造过程是在热熔涂布机上采用夹缝式挤压、滚棒式或淋膜式涂布工艺完成的。将耐高温聚氯乙烯膜基材安装到放卷轴上，并引出至收卷轴。设定熔胶箱温度为130-140℃，涂布头温度为130-150℃，根据上胶的重量调整胶泵的转速和主机速度的比值。设定收卷张力和放卷张力，并打开冷却装置。调整主机速度，将涂布头慢慢靠至聚氯乙烯膜面，打开胶泵开关进行涂布，调整涂布头和基材之间的间隙距离，调整涂布机速度进行涂布，本发明所采用的热熔胶粘剂涂布量是10-35克重/每平方米。胶层经一组紫外灯的紫外光辐照进行交联固化。本发明所用紫外灯是高压汞灯，中低压汞灯或者LED灯，其紫外光的最小辐照能量需达到10mJ/cm2。交联固化后的胶带再经收卷分切后即制得所述的耐高温聚氯乙烯胶带制品。在涂布过程中为了防止聚氯乙烯膜基材在紫外光照射时受到破坏，应对聚氯乙烯膜进行冷却保护。本发明所采用的冷却方式可以是水冷凝、或风冷却方式，也可以同时采用水冷凝和风冷却。
性能测试：将所制得的可紫外光交联热熔压敏粘合剂用上述方法热熔涂布于0.15毫米厚的聚氯乙烯薄膜基材上，制得胶层厚度为20微米的电气压敏粘合剂粘带小卷。经过在60度，8小时老化以后，按照以下标准对胶粘性能进行测试：1)中国国家标准GB/T2792-1998测试180°剥离强度，2)中国国家标准GB/4852-1984测试胶带初粘性能，3)按照VW60360(LV312)评估耐高温等级，4)按照中国国家标准GB/T4581-1988测试胶带的持粘性能。
具体实施例
下面叙述本发明的一些具体的实施例和比较例，但本发明并不限于这些实施例。
本发明的实施例和比较例采用以下聚氯乙烯膜
1.耐高温型聚氯乙烯膜
聚氯乙烯膜配方如下(wt％重量比例)
原材料混合以后经高速搅拌机混合、高温开炼机、挤出机、三辊或者四辊压延机进行高温压延制备成聚氯乙烯膜。
2.目前市场上普遍使用的含DOP增塑剂的聚氯乙烯膜
实施例1
丙烯酸正丁酯，丙烯酸异辛酯，丙烯酸甲酯，丙烯酸和可共聚的光敏引发剂的丙烯酸酯共聚物按照上面描写的方式施用到上述耐高温聚氯乙烯膜上，制成聚氯乙烯胶带。应用的涂布温度为140℃。
实施例2
丙烯酸正丁酯，丙烯酸和可共聚的光敏引发剂的丙烯酸酯共聚物按照上面描写的方式施用到上述耐高温聚氯乙烯膜上，制成聚氯乙烯胶带。应用的涂布温度为140℃。
实施例3
20％丙烯酸正丁酯，丙烯酸和可共聚的光敏引发剂的低聚体和丙烯酸酯(丙烯酸正丁酯，丙烯酸)聚合物的混合物按照上面描写的方式施用到上述耐高温聚氯乙烯膜上，制成聚氯乙烯胶带。应用的涂布温度为130℃。
比较例1
丙烯酸正丁酯，丙烯酸异辛酯，丙烯酸甲酯，丙烯酸和可共聚的光敏引发剂的丙烯酸酯共聚物因为直接涂布于含DOP增塑剂的聚氯乙烯膜会使膜受到破坏，所以本比较例中只能采用转移涂布方式，即先涂布于离型纸上，然后转移到含DOP增塑剂的聚氯乙烯膜。应用的涂布温度为140℃。
比较例2
目前工业上普遍使用的Huaxia863。所用的胶水是溶剂型橡胶体系，所用的聚氯乙烯膜属于耐高温型聚氯乙烯膜。
比较例3
目前工业上普遍使用的HuaxiaUD110。所用的胶水是溶剂型橡胶体系，所用的聚氯乙烯膜属于含DOP增塑剂的聚氯乙烯膜。
表1各种可紫外光交联的热熔压敏胶的性能数据
从表1的实施例1-3的性能数据可以看出可紫外光交联的热熔压敏胶能显著提高聚氯乙烯胶带的耐高温性能，达到125℃耐温等级。用溶剂型橡胶制成的胶带耐高温等级为105℃(比较例2)。从比较例1和比较例3测试结果可以得知，可紫外光交联的热熔压敏胶抗低分子增塑剂性能不如溶剂型橡胶。总的来说，可紫外光交联的热熔压敏胶适合于施用于含高分子增塑剂的耐高温聚氯乙烯膜，而所制得胶带符合工业应用指标。而且胶带有优良的耐高温性能，适用于电缆束的包复和捆扎。尤其适用于汽车车体中的电缆束的包复和捆扎。

Claims (12)

1.一种新型耐高温聚氯乙烯胶带的制作方法，其特征在于：将可紫外光交联的热熔压敏粘合剂在130-150℃温度下直接在热熔涂布机上热熔涂布于耐高温聚氯乙烯薄膜上，再经一组紫外灯的紫外光辐照交联制成，为防止聚乙烯膜在涂布和紫外光照射时受到破坏，对聚氯乙烯膜进行了冷却保护。
2.根据权利要求1所述的耐高温聚氯乙烯薄膜，其特征在于：该薄膜是一种含有液体高分子型增塑剂、固体高分子增塑剂和热稳定剂的耐高温材料，该聚氯乙烯薄膜在热熔涂布过程中不会受到热破坏，且高温涂布时薄膜的收缩率较低。
3.根据权利要求1所述的可紫外光交联的热熔压敏粘合剂，其特征在于：在其组成中，含有一种或多种可聚合光敏引发剂与丙烯酸酯单体的共聚物，或者是含一种或多种可聚合光敏引发剂的低聚体和丙烯酸酯聚合物的混合物。
4.根据权利要求3所述的可紫外光交联的热熔压敏粘合剂，其特征在于：在其组成中，可含有热稳定剂，光稳定剂，增粘树脂和增塑剂。
5.根据权利要求2所述的液体高分子型增塑剂，其特征在于：它们是液体己二酸乙二醇聚酯增塑剂和液体己二酸丙二醇聚酯增塑剂。
6.根据权利要求2所述的固体高分子增塑剂，其特征在于：它们是乙烯-醋酸乙烯共聚物(EVA)、乙烯-丙烯酸甲酯共聚物(EMA)、乙烯-丙烯酸乙酯共聚物(EEA)、乙烯-丙烯酸丁酯共聚物(EBA)、丁腈橡胶粉(NBR)和氯化聚乙烯(CPE)。
7.根据权利要求2所述的热稳定剂，其特征在于：它们是非铅类的液体或固体钡锌稳定剂、镉钡锌稳定剂、钙锌稳定剂、有机锡类稳定剂。
8.根据权利要求3所述的可聚合光敏引发剂，其特征在于：它们是含甲基丙烯酰氧基或丙烯酰氧基的苯乙酮或二苯甲酮衍生物。
9.根据权利要求1所述的热熔涂布，其特征在于：热熔粘合剂的涂布量是10-35克/每平方米。
10.根据权利要求1所述的紫外灯，其特征在于：它们是高压汞灯、中低压汞灯或LED灯，其紫外光辐照能量应达到10mJ/cm2。
11.根据权利要求1所述的涂布方式，其特征是夹缝式挤压、滚棒式或淋膜式涂布方式。
12.根据权利要求1所述的冷却保护，其特征是可以使用水冷凝或风冷却方式，或同时使用水冷凝和风冷却。
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CN202011308233.XA CN112500805A (zh) 2016-02-03 2016-02-03 一种新型耐高温聚氯乙烯胶带的制作方法
ES21178815T ES2936804T3 (es) 2016-02-03 2016-05-12 Adhesivo sensible a la presión de fusión en caliente reticulado por UV utilizado para una cinta adhesiva aislante de poli(cloruro de vinilo)
PCT/CN2016/081923 WO2017133122A1 (zh) 2016-02-03 2016-05-12 一种耐高温聚氯乙烯胶带的制作方法
EP16888944.2A EP3412742B2 (en) 2016-02-03 2016-05-12 Method for manufacturing high-temperature-resistant polyvinyl-chloride adhesive tape
EP21178815.3A EP3916064B1 (en) 2016-02-03 2016-05-12 Uv-crosslinked hot-melt pressure-sensitive adhesive used for polyvinyl-chloride insulated adhesive tape
KR1020187025099A KR102521225B1 (ko) 2016-02-03 2016-05-12 폴리염화비닐 절연 접착 테이프에 사용되는 uv 가교된 핫멜트 감압성 접착제
ES16888944T ES2812204T5 (es) 2016-02-03 2016-05-12 Método para fabricar cinta adhesiva de poli(cloruro de vinilo) resistente a altas temperaturas
EP16888943.4A EP3412741B1 (en) 2016-02-03 2016-05-12 Uv-crosslinked hot-melt pressure-sensitive adhesive used for polyvinyl-chloride insulated adhesive tape
PCT/CN2016/081908 WO2017133121A1 (zh) 2016-02-03 2016-05-12 应用于聚氯乙烯绝缘胶带的紫外光交联热熔压敏胶黏剂
JP2018541302A JP6775025B2 (ja) 2016-02-03 2016-05-12 耐高温性ポリ塩化ビニル粘着テープの製造方法
ES16888943T ES2879991T3 (es) 2016-02-03 2016-05-12 Adhesivo sensible a la presión de fusión en caliente reticulado por UV utilizado para cinta adhesiva aislante de poli(cloruro de vinilo)
CN201680080847.2A CN108603081A (zh) 2016-02-03 2016-05-12 一种耐高温聚氯乙烯胶带的制作方法
US16/074,965 US20190040288A1 (en) 2016-02-03 2016-05-12 Method for manufacturing high-temperature-resistant polyvinyl-chloride adhesive tape
US16/074,608 US20190055433A1 (en) 2016-02-03 2016-05-12 Uv-crosslinked hot-melt pressure-sensitive adhesive used for polyvinyl-chloride insulated adhesive tape
KR1020187025105A KR102547510B1 (ko) 2016-02-03 2016-05-12 내고온성 폴리비닐 클로라이드 접착 테이프의 제조방법
JP2018541363A JP6861215B2 (ja) 2016-02-03 2016-05-12 ポリ塩化ビニル絶縁粘着テープに用いられるｕｖ架橋性ホットメルト感圧性接着剤
CN201680002203.1A CN107960097B (zh) 2016-02-03 2016-05-12 应用于聚氯乙烯绝缘胶带的紫外光交联热熔压敏胶黏剂
HK18114365.8A HK1255534A1 (zh) 2016-02-03 2018-11-09 一種耐高溫聚氯乙烯膠帶的製作方法
US17/145,537 US20210371709A1 (en) 2016-02-03 2021-01-11 Uv-crosslinked hot-melt pressure-sensitive adhesive used for polyvinyl chloride insulation adhesive tape
US17/385,086 US20220186084A1 (en) 2016-02-03 2021-07-26 Method for manufacturing high temperature-resistant polyvinyl chloride adhesive tape

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CN106188930A (zh) * 2016-06-24 2016-12-07 河北华夏实业有限公司 一种适用于热熔压敏胶涂布的聚氯乙烯薄膜及其制备方法
CN106188930B (zh) * 2016-06-24 2020-12-11 河北永乐胶带有限公司 一种适用于热熔压敏胶涂布的聚氯乙烯薄膜及其制备方法
CN107841252A (zh) * 2017-11-20 2018-03-27 河北新天坛压敏胶科技有限公司 压敏胶及其制备方法和胶粘带
CN111403083A (zh) * 2019-12-13 2020-07-10 上海谦恒电气有限公司 耐酸碱耐磨损环保电缆
CN111378391A (zh) * 2020-04-27 2020-07-07 广东硕成科技有限公司 一种耐高温汽车喷漆遮蔽用保护膜及其制备方法
CN111378391B (zh) * 2020-04-27 2021-09-28 广东硕成科技有限公司 一种耐高温汽车喷漆遮蔽用保护膜及其制备方法
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Inventor after: Wang Feng

Inventor after: Jin Chunming

Inventor after: Li Shuang

Inventor after: Qi Shuqin

Inventor after: Yang Yukun

Inventor before: Wang Feng

Inventor before: Huang Zhida

Inventor before: Jin Chunming

Inventor before: Li Shuang

Inventor before: Yang Yukun

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Effective date of registration: 20170323

Address after: No. 9, Yan Dong Road, Baoding Industrial Park, Zhuozhou Development Zone, Hebei, China

Applicant after: Hebei Yongle adhesive tape Co., Ltd.

Address before: Yan Yi Road Industrial Park Development Zone in Zhuozhou province Hebei City, No. 9 (middle Huaxia group)

Applicant before: Hebei Huaxia Enterprise Co., Ltd.

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160622