CN112852016B - Pvc用含氮热稳定剂组合物及其应用 - Google Patents

Pvc用含氮热稳定剂组合物及其应用 Download PDF

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CN112852016B
CN112852016B CN202110040667.4A CN202110040667A CN112852016B CN 112852016 B CN112852016 B CN 112852016B CN 202110040667 A CN202110040667 A CN 202110040667A CN 112852016 B CN112852016 B CN 112852016B
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臧亚南
徐云慧
巩志行
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Ningbo Huishuo New Material Co ltd
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Abstract

本发明公开了PVC用含氮热稳定剂组合物极其应用，热稳定剂组合物，包括作为主热稳定剂A的二苯胺类防老剂，作为主热稳定剂B的咪唑类防老剂，作为辅助热稳定剂Ａ的棕榈酸锌盐，作为辅助热稳定剂Ｂ的酚类抗氧剂以及作为辅助热稳定剂C的亚磷酸酯类抗氧剂。选择橡胶二胺类防老剂和咪唑类防老剂作为PVC的主热稳定剂，拓展了橡胶防老剂的用途；所使用的防老剂均无毒环保，且能提高PVC的热稳定性。

Description

PVC用含氮热稳定剂组合物及其应用
技术领域
本发明属于塑料助剂领域，具体涉及PVC用含氮热稳定剂组合物及其应用。
背景技术
近年来，PVC用含氮热稳定剂日益引起人们的重视。早期主要使用硫脲、脂肪胺、尿素及吲哚等一些小分子化合物。后来，逐步发展为使用巴比妥酸及其衍生物、苯基脲及苯基硫脲及其衍生物、某些酰胺和酰亚胺、蒽醌衍生物、吡唑啉酮衍生物、脲衍生物以及嘧啶类化合物等。CN 107129594 B介绍了一种PVC用含氮类热稳定剂-三唑基化合物，将其与和硬脂酸锌、多元醇、β-二酮、环氧化合物和长链脂肪酸等制成复合热稳定剂。将所制得的PVC试片置于180℃的烘箱中，随着时间的延长，PVC试片的颜色逐渐很深，说明PVC脱HCl的反应持续进行，最长160min PVC试片的颜色变黑，说明PVC发生了较大幅度地降解，已完全失去使用性。CN 108329275 A介绍了制备氨基脲嘧啶马来酰胺酸的方法，并将其与硬脂酸钙、硬脂酸锌、乙酰丙酮钙、乙酰丙酮锌和β-二酮中的一种或多种并用作为PVC热稳定剂。结果表明，在190-195℃的料温下，平衡时间最长可达22min。CN 111072574 A介绍了制备5,6-二氨基-1,3-二烃取代尿嘧啶的方法，并将其与硬脂酸锌、硬脂酸钙和季戊四醇中的一种或多种并用作为PVC的热稳定剂，研究结果表明，在180℃的烘箱中，经过65min，PVC的颜色已经变深；在180-185℃的料温下，PVC最长平衡时间为4104s。
发明内容
为了克服上述现有技术的不足，本发明专利所要解决的技术问题在于提供一种能提高PVC静态热稳定性和动态热稳定剂、无毒环保的含氮PVC热稳定剂组合物。
本发明是通过如下技术方案实现的，PVC用含氮热稳定剂组合物，热稳定剂组合物，包括作为主热稳定剂A的二苯胺类防老剂，作为主热稳定剂B的咪唑类防老剂，作为辅助热稳定剂A的棕榈酸锌盐，作为辅助热稳定剂B的酚类抗氧剂以及作为辅助热稳定剂C的亚磷酸酯类抗氧剂。
作为本发明所述的PVC用含氮热稳定剂组合物的优选方案：所述主热稳定剂A为：4,4'-二(苯基异丙基)二苯胺(KY-405)或4,4'-二(苯基异丙基)二苯胺(KY-405)与4,4'-二辛基二苯胺(防老剂ODA)并用。
作为本发明所述的PVC用含氮热稳定剂组合物的优选方案：所述主热稳定剂B为：2-硫醇基苯并咪唑锌盐(防老剂MBZ)或2-巯基苯并咪唑(防老剂MB)；
2-巯基苯并咪唑(防老剂MB)使用时需与作为辅助热稳定剂A的棕榈酸锌二者并用；
2-硫醇基苯并咪唑锌盐(防老剂MBZ)使用时无需额外添加作为辅助热稳定剂A的棕榈酸锌。
作为本发明所述的PVC用含氮热稳定剂组合物的优选方案：所述辅助热稳定剂B为：四[β-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯(抗氧剂1010)或6-(4-羟基-3,5-二叔丁基苯氨基)-2,4-二正辛硫基-1,3,5-三嗪(抗氧剂565)。
作为本发明所述的PVC用含氮热稳定剂组合物的优选方案：所述辅助热稳定剂C为：二亚磷酸季戊四醇二异葵酯(抗氧剂3010)、双(2,4-二叔丁基苯酚)季戊四醇二亚磷酸酯(抗氧剂626)或季戊四醇二亚磷酸双十八酯(抗氧剂618)。
所述的PVC用含氮热稳定剂组合物应用，当PVC为100份时，在其中加入的热稳定剂组合物的各组分质量份数为：
主热稳定剂A为4,4'-二(苯基异丙基)二苯胺(KY-405)，其用量为1-1.5份；
当使用4,4'-二(苯基异丙基)二苯胺(KY-405)与4,4'-二辛基二苯胺(防老剂ODA)并用时，两者的质量份数比为(0.8-1.2)：(0.3-0.7)；
所述主热稳定剂B为2-硫醇基苯并咪唑锌盐(防老剂MBZ)，其用量为0.5-1.5份,不添加辅助热稳定剂A棕榈酸锌；
当主热稳定剂B为2-巯基苯并咪唑(防老剂MB)，需与辅助热稳定剂A棕榈酸锌并用，两者用量均为0.5-1.0份；
辅助热稳定剂B的用量为0.4-0.6份，辅助热稳定剂C的用量为0.2-0.5份；
除此之外，还需加入增塑剂10-50份以及润滑剂0.2-1份；
所述增塑剂包括主增塑剂和副增塑剂；所述主增塑剂为环氧大豆油，其环氧值大于等于6；所述副增塑剂为磷酸三辛酯(TOP)、甘油三醋酸酯或甘油三丁酸酯；所述主增塑剂的用量为8-30份，所述副增塑剂的用量优选为2-20份；
所述润滑剂为聚乙烯蜡与石蜡并用，其用量均为0.1-0.5份；
具体制备方法是，在高混机中，将上述原料进行混合，再将混合后的材料在高温开炼机中混炼均匀，高温开炼机的辊温控制在120-130℃；混炼均匀后，在平板硫化机中压制得到PVC试片。
本发明的有益效果为：选择橡胶二胺类防老剂和咪唑类防老剂作为PVC的主热稳定剂，拓展了橡胶防老剂的用途；所使用的防老剂均无毒环保，且能提高PVC的热稳定性。
附图说明
图1是实施例1-3和对比例所制得PVC试片动态热稳定性分析，(转矩流变仪法，185℃，60r/min)。
具体实施方式
下面结合实施例对本发明做进一步说明。
实施例1：
称取PVC、100份(质量份，以下同)，在其中加入的PVC热稳定剂组合物的用量为防老剂KY-405、1.0份，防老剂MBZ、1.0份，抗氧剂1010、0.5份，抗氧剂3010、0.2份。除此之外，再加入环氧大豆油(环氧值为6.5)25份，TOP、15份，聚乙烯蜡、0.3份，石蜡、0.3份。
具体制备方法是，在高混机中加入PVC，防老剂KY405、防老剂MBZ、抗氧剂1010、抗氧剂3010，以及环氧大豆油、TOP、聚乙烯蜡和石蜡进行混合。将混合后的材料在高温开炼机中混炼均匀，高温开炼机的辊温设置为120℃。混炼均匀后，在平板硫化机中压制得到PVC试片。
实施例2：
称取PVC、100份(质量份，以下同)，在其中加入的PVC热稳定剂组合物的用量为防老剂KY-405、1.0份，防老剂ODA、0.5份，防老剂MB、1.0份，棕榈酸锌、0.5份，抗氧剂565、0.5份，抗氧剂626、0.2份。除此之外，再加入环氧大豆油(环氧值为6.5)、20份，甘油三丁酸酯、20份，聚乙烯蜡、0.1份、石蜡、0.1份。
具体制备方法是，在高混机中加入PVC，防老剂KY405、防老剂ODA、防老剂MB、棕榈酸锌、抗氧剂565、抗氧剂626，以及环氧大豆油、甘油三丁酸酯、聚乙烯蜡和石蜡进行混合。将混合后的材料在高温开炼机中混炼均匀，高温开炼机的辊温设置为120℃。混炼均匀后，在平板硫化机中压制得到PVC试片。
实施例3：
称取PVC、100份(质量份，以下同)，在其中加入的PVC热稳定剂组合物的用量为防老剂KY405、1.0份，防老剂MBZ、0.5份，抗氧剂565、0.5份，抗氧剂618、0.2份。除此之外，再加入环氧大豆油(环氧值为6.5)、20份，甘油三醋酸酯、10份，聚乙烯蜡、0.2份，石蜡、0.3份。
具体制备方法是，在高混机中加入PVC，防老剂KY405、防老剂MBZ、抗氧剂565、抗氧剂618，以及环氧大豆油、甘油三醋酸酯、聚乙烯蜡和石蜡进行混合。将混合后的材料，在高温开炼机中混炼均匀，高温开炼机的辊温设置为120℃。混炼均匀后，在平板硫化机中压制得到PVC试片。
对比例：
具体制备方法是，在高混机中加入PVC、100份，硬脂酸铅、1.5份，硬脂酸钡、1.5份，以及环氧大豆油(环氧值为6.5)、20份，TOP、10份，聚乙烯蜡、0.4份和石蜡、0.2份进行混合。混合均匀在高温开炼机中混炼均匀，高温开炼机的辊温设置为120℃；混炼均匀后，在平板硫化机中压制得到PVC试片。
将实施例1-3和对比例所制得的PVC试片进行静态热稳定性分析-烘箱法，温度为200℃，第一次置于烘箱4小时后取样，而后每隔30分钟取样，观察试片颜色变化，结果见表1所示。
表1 PVC试片的静态热稳定性-烘箱法
Figure BDA0002895204730000041
Figure BDA0002895204730000051
Figure BDA0002895204730000061
从表1可以看出，将实施例和对比例放入200℃的烘箱中，实施例经过1320min，试片由白色逐渐变为土黄色。而对比例仅仅经过300min就变为黑褐色。说明实施例的静态热稳定性优于对比例。
将实施例1-3和对比例所制得的PVC试片进行动态热稳定性分析-转矩流变仪法，温度为185℃，结果见图1所示。
从实施例1-3和对比例所制备的PVC试样加入转矩流变仪(185℃，60r/min)时，刚开始未来得及塑化，所以扭矩大幅度提高。随着塑化的进行，扭矩下降。对比例在1200s以后扭矩提高，说明此时PVC发生交联，在2700s以后，扭矩快速下降，说明此时PVC开始大幅度降解。实施例1在4200s以后扭矩小幅上升，实施例2在4500s以后扭矩小幅上升，说明PVC有可能发生轻度交联，但未对PVC性能造成很大影响。实施例3在4300s左右扭矩快速下降，说明PVC开始快速降解。实施例1-3的动态热稳定性优于对比例。

Claims (1)

1.一种PVC用含氮热稳定剂组合物应用，其特征在于：
当PVC为100份时，在其中加入的热稳定剂组合物的各组分质量份数为：
主热稳定剂A为4,4'-二(苯基异丙基)二苯胺，其用量为1-1.5份；
当使用4,4'-二(苯基异丙基)二苯胺与4,4'-二辛基二苯胺并用时，两者的质量份数比为（0.8-1.2）：（0.3-0.7）；
所述主热稳定剂B为2-硫醇基苯并咪唑锌盐，其用量为0.5-1.5份,不添加辅助热稳定剂A棕榈酸锌；
当主热稳定剂B为2-巯基苯并咪唑，需与辅助热稳定剂A棕榈酸锌并用，两者用量均为0.5-1.0份；
辅助热稳定剂B的用量为0.4-0.6份，辅助热稳定剂C的用量为0.2-0.5份；
除此之外，还需加入增塑剂10-50份以及润滑剂0.2-1份；
所述增塑剂包括主增塑剂和副增塑剂；所述主增塑剂为环氧大豆油，其环氧值大于等于6；所述副增塑剂为磷酸三辛酯、甘油三醋酸酯或甘油三丁酸酯；所述主增塑剂的用量为8-30份，所述副增塑剂的用量为2-20份；
所述润滑剂为聚乙烯蜡与石蜡并用，其用量均为0.1-0.5份；
具体制备方法是，在高混机中，将上述原料进行混合，再将混合后的材料在高温开炼机中混炼均匀，高温开炼机的辊温控制在120-130℃；混炼均匀后，在平板硫化机中压制得到PVC试片；
所述辅助热稳定剂B为：四[β-(3，5-二叔丁基-4-羟基苯基)丙酸]季戊四醇酯或6-(4-羟基-3,5-二叔丁基苯氨基)-2,4-二正辛硫基-1,3,5-三嗪；
所述辅助热稳定剂C为：二亚磷酸季戊四醇二异癸酯、双（2,4-二叔丁基苯酚）季戊四醇二亚磷酸酯或季戊四醇二亚磷酸双十八酯。
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US6362264B1 (en) * 1996-12-20 2002-03-26 Ck Witco Corporation Stabilizer for food contact and medical grade PVC
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