CN106977840B - 一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法 - Google Patents
一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法。先将聚氯乙烯材料在真空烘箱中干燥，加入碳酸钙填料并均匀搅拌；再加入热稳定剂、塑化剂，均匀搅拌，待保温结束后，加入以表面改性剂改性后的纳米氧化铝晶须，均匀搅拌，最终物料投入到双螺杆挤出机中进行挤出造粒，再投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。本发明制备出的纳米氧化铝晶须/聚氯乙烯复合薄膜可以广阔的应用在各种大小型的充气玩具、跳床、水池、帐篷等休闲娱乐设备，满足人们对生活品质的不懈追求。
Description
技术领域
本发明属于纳米复合材料的制备工艺领域，涉及一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法。
背景技术
随着社会的不断发展进步，人们出行休闲娱乐方式变得丰富多彩，水上充气玩具变得更加流行。市场上的充气玩具大多采用聚氯乙烯树脂作为基体材料，但是长时间使用后，PVC材料会出现耐热性、耐紫外光老化性能和强度变差等问题。纳米氧化铝晶须具有硬度高、高温强度大、抗氧化性能好、热膨胀系数小等优异性能，因而被广泛地用作聚合物填料以提高其强度和耐热性。纳米氧化铝晶须/聚氯乙烯复合薄膜兼具上述两种材料优势于一体，受到普遍关注，可以广泛应用于各种大小型的充气玩具、跳床、水池、帐篷等休闲娱乐设备，满足人们对高品质生活的不懈追求。
发明内容
本发明的目的是为了改进现有技术的不足而提供一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法，该方法原材料便宜易得，工艺过程简单，这种材料可满足于高耐磨和高强的充气休闲娱乐设备的需要。
本发明的技术方案为：一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法，其具体步骤如下：
(1)纳米氧化铝晶须加入乙醇溶剂中，加入表面改性剂，进行超声波震荡(一般0.4-0.6h)，过滤烘干，在130～150℃下活化7-9h后冷却，得到改性后的纳米氧化铝晶须；
(2)将聚氯乙烯材料在真空烘箱中干燥，再冷却至30～40℃，加入碳酸钙填料并均匀搅拌；
(3)向步骤(2)加入热稳定剂、塑化剂，均匀搅拌，控制温度为50～110℃，并进行保温2～8小时；
(4)待保温结束后，向步骤(3)中加入步骤(1)得到的改性后的纳米氧化铝晶须，均匀搅拌，搅拌温度保持在50～110℃之间；
(5)待步骤(4)结束后，将温度降至40～50℃的最终物料投入到双螺杆挤出机中进行挤出造粒；
(6)将步骤(5)中得出的粒料投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。
优选步骤(1)中纳米氧化铝晶须的粒径为25-60nm。优选步骤(1)中表面改性剂为硅烷偶联剂、钛酸酯偶联剂或铝酸酯偶联剂一种或多种；氧化铝晶须与偶联剂的重量比为5：1-5。
优选步骤(2)中PVC与碳酸钙填料的重量比为100：3-10。优选步骤(2)中真空烘箱的温度为75-85℃，干燥时间为10-12h。
优选步骤(3)中热稳定剂为二盐基硬脂酸铅、硬脂酸钙或二月桂酸二丁基锡的一种或多种；PVC与热稳定剂的重量比为100：2-5。优选步骤(3)中增塑剂为邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)或癸二酸二正丁酯(DBS)的一种或多种；其中PVC与塑化剂的重量比为100：10-15。
优选步骤(4)中PVC与改性后纳米氧化铝晶须的重量比为100：10-25。优选步骤(5)中双螺杆转速为270～330rpm。
本发明所制备的高强耐磨纳米聚氯乙烯复合薄膜的拉力强度大于2800N/5cm，断裂伸长率大于200％。
有益效果：
本发明方法以及高强耐磨纳米聚氯乙烯复合薄膜具有如下特点：
(1)原料价廉，降低成本。本方法以高耐磨、高强的纳米氧化铝晶须和PVC复合为原料制得高强、耐磨的复合薄膜材料，极大地降低生产成本。
(2)耐高温，强度高。本方法中采用的纳米氧化铝晶须作为增强材料，具有硬度高、高温强度大、抗氧化性能好、热膨胀系数小等优异性能。
具体实施方式
以下例子所述的份数均为重量份。
实例1
将10份平均粒径为30nm的纳米氧化铝晶须加入乙醇中混合均匀再加入5份硅烷偶联剂和1份钛酸酯偶联剂，进行超声波震荡0.5h，过滤烘干，在130℃下活化7h后冷却至室温，得到改性后的10份纳米氧化铝晶须。将100份聚氯乙烯材料在75℃的真空烘箱中干燥时间为12h，再冷却至30℃，加入5份CaCO3填料并搅拌均匀。加入1份二盐基硬脂酸铅和1份二月桂酸二丁基锡热稳定剂，5份邻苯二甲酸二辛酯(DOP)和5份癸二酸二正丁酯(DBS)塑化剂，均匀搅拌，搅拌温度65℃，并进行保温3h。把改性后纳米氧化铝晶须和PVC混合，均匀搅拌，搅拌温度保持在60℃之间。将温度降至40℃的最终物料投入到双螺杆挤出机中进行挤出造粒，双螺杆转速为300rpm。将得出的粒料投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。经过试验验证，纳米氧化铝晶须在聚氯乙烯中分散均匀，复合薄膜的拉力强度为2850N/5cm，断裂伸长率为215％。得到的薄膜具有较好的耐磨性、较高的拉伸强度等优异性能。
实例2
20份平均粒径为35nm的纳米氧化铝晶须加入乙醇中混合均匀再加入4份硅烷偶联剂、1份钛酸酯偶联剂和1份铝酸酯偶联剂，进行超声波震荡0.6h，过滤烘干，在140℃下活化9h后冷却至室温，得到改性后的纳米氧化铝晶须。将100份PVC在80℃的真空烘箱中干燥11h后，再冷却至35℃，加入6份CaCO3填料并搅拌均匀。加入1份二盐基硬脂酸铅和2份硬脂酸钙热稳定剂，5份邻苯二甲酸二丁酯(DBP)和6份癸二酸二正丁酯(DBS)塑化剂，均匀搅拌，搅拌温度85℃，并进行保温4h。把改性后20份纳米氧化铝晶须和PVC混合，均匀搅拌，搅拌温度保持在70℃之间。将温度降至45℃的最终物料投入到双螺杆挤出机中进行挤出造粒，双螺杆转速为310rpm。将得出的粒料投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。经过试验验证，纳米氧化铝晶须在聚氯乙烯中分散均匀，复合薄膜的拉力强度为2950N/5cm，断裂伸长率为221％。得到的薄膜具有较好的耐磨性、较高的拉伸强度等优异性能。
实例3
15份平均粒径为40nm的纳米氧化铝晶须加入乙醇中混合均匀再加入3份硅烷偶联剂、1份钛酸酯偶联剂和2份铝酸酯偶联，进行超声波震荡0.5h，过滤烘干，在150℃下活化7h后冷却至室温，得到改性后的纳米氧化铝晶须。将100份PVC在85℃的真空烘箱中干燥11h后，再冷却至40℃，加入8份CaCO3填料并搅拌均匀。加入2份硬脂酸钙和2份二月桂酸二丁基锡热稳定剂，3份邻苯二甲酸二丁酯(DBP)、3份邻苯二甲酸二辛酯和5份癸二酸二正丁酯(DBS)塑化剂，均匀搅拌，搅拌温度90℃，并进行保温2h。把改性后15份纳米氧化铝晶须和PVC混合，均匀搅拌，搅拌温度保持在85℃之间。将温度降至45℃的最终物料投入到双螺杆挤出机中进行挤出造粒，双螺杆转速为305rpm。将得出的粒料投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。经过试验验证，纳米氧化铝晶须在聚氯乙烯中分散均匀，复合薄膜的拉力强度大于2930N/5cm，断裂伸长率大于216％，得到的薄膜具有较好的耐磨性、较高的拉伸强度等优异性能。
实例4
25份平均粒径为50nm的纳米氧化铝晶须加入乙醇中混合均匀再加入4份硅烷偶联剂、2份钛酸酯偶联剂和2份铝酸酯偶联，进行超声波震荡0.6h，过滤烘干，在140℃下活化8h后冷却至室温，得到改性后的纳米氧化铝晶须。将100份PVC在75℃的真空烘箱中干燥12h后，再冷却至30℃，加入7份CaCO3填料并搅拌均匀。加入1份二盐基硬脂酸铅、2份硬脂酸钙和2份二月桂酸二丁基锡热稳定剂，5份邻苯二甲酸二丁酯(DBP)、5份邻苯二甲酸二辛酯和5份癸二酸二正丁酯(DBS)塑化剂均匀搅拌，搅拌温度80℃，并进行保温7h。把改性后25份纳米氧化铝晶须和PVC混合，均匀搅拌，搅拌温度保持在80℃之间。将温度降至50℃的最终物料投入到双螺杆挤出机中进行挤出造粒，双螺杆转速为310rpm。将得出的粒料投入到挤出成型机中，确定薄膜尺寸，进行牵引、切割，最终得到复合薄膜。经过试验验证，纳米氧化铝晶须在聚氯乙烯中分散均匀，复合薄膜的拉力强度大于2955N/5cm，断裂伸长率大于233％，得到的薄膜具有较好的耐磨性、较高的拉伸强度等优异性能。
Claims (8)
1.一种高强耐磨纳米聚氯乙烯复合薄膜的制备方法，其具体步骤如下：
(1)纳米氧化铝晶须加入乙醇溶剂中，加入表面改性剂，进行超声波震荡，过滤烘干，在130～150℃下活化7-9h后冷却，得到改性后的纳米氧化铝晶须；其中氧化铝晶须与偶联剂的重量比为5：1-5；
(2)将聚氯乙烯材料在真空烘箱中干燥，再冷却至30～40℃，加入碳酸钙填料并均匀搅拌；其中PVC与碳酸钙填料的重量比为100：3-10；
(3)向步骤(2)加入热稳定剂、塑化剂，均匀搅拌，控制温度为50～110℃，并进行保温2～8小时；
(4)待保温结束后，向步骤(3)中加入步骤(1)得到的改性后的纳米氧化铝晶须，均匀搅拌，搅拌温度保持在50～110℃之间；其中PVC与改性后纳米氧化铝晶须的重量比为100：10-25；
(5)待步骤(4)结束后，将温度降至40～50℃的最终物料投入到双螺杆挤出机中进行挤出造粒；
(6)将步骤(5)中得出的粒料投入到挤出成型机中，进行牵引、切割，最终得到复合薄膜。
2.根据权利要求1所述的制备方法，其特征在于步骤(1)中纳米氧化铝晶须的粒径为25-60nm。
3.根据权利要求1所述的制备方法，其特征在于步骤(1)中表面改性剂为硅烷偶联剂、钛酸酯偶联剂或铝酸酯偶联剂一种或多种。
4.根据权利要求1所述的制备方法，其特征在于步骤(2)中真空烘箱的温度为75-85℃，干燥时间为10-12h。
5.根据权利要求1所述的制备方法，其特征在于步骤(3)中热稳定剂为二盐基硬脂酸铅、硬脂酸钙或二月桂酸二丁基锡的一种或多种；PVC与热稳定剂的重量比为100：2-5。
6.根据权利要求1所述的制备方法，其特征在于步骤(3)中塑化剂为邻苯二甲酸二丁酯、邻苯二甲酸二辛酯或癸二酸二正丁酯的一种或多种；其中PVC与塑化剂的重量比为100：10-15。
7.根据权利要求1所述的制备方法，其特征在于步骤(5)中双螺杆转速为270～330rpm。
8.根据权利要求1所述的制备方法，其特征在于高强耐磨纳米聚氯乙烯复合薄膜的拉力强度大于2800N/5cm，断裂伸长率大于200％。
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