CN114573856B - 一种改性pvc发泡垫子及其制备方法 - Google Patents

一种改性pvc发泡垫子及其制备方法 Download PDF

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CN114573856B
CN114573856B CN202210214841.7A CN202210214841A CN114573856B CN 114573856 B CN114573856 B CN 114573856B CN 202210214841 A CN202210214841 A CN 202210214841A CN 114573856 B CN114573856 B CN 114573856B
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翁跃丰
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Cixi Saijie Commodity Co ltd
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Abstract

本发明公开了一种改性PVC发泡垫子的制备方法，其包括以下步骤：S1：将由PVC粉、改性废橡胶粉、增塑剂、无机填料、添加剂、色料、发泡剂和助剂复配的原料混合成混合浆料，静置6～12h进行预发泡；S2：将步骤S1处理后的混合浆料涂布形成浆料层，逐步升温至185～220℃进行发泡反应，发泡操作10～60min后，冷却成预定厚度的发泡垫体；S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子。本发明制备得到的改性PVC发泡垫子，其安全环保，具有优异的热稳定性、耐磨性、自清洁性、防潮性及回弹性，可保证不同户外复杂环境下使用的可靠性和舒适性。

Description

一种改性PVC发泡垫子及其制备方法
技术领域
本发明涉及塑料的技术领域，尤其涉及一种改性PVC发泡垫子及其制备方法。
背景技术
随着社会的进步，人们生活水平的提高，户外生活成为人们的追求。户外用品的需求越来越多，这对户外用品行业提出了更高的要求，户外用品也需要不断的改良以适应新的生活需求。
PVC垫子化学稳定性好，抗拉、抗弯、抗压和抗冲击能力强。但是户外环境复杂，现有的户外PVC垫子回弹性、防潮性及热稳定性差，并且整体舒适性不佳，在清晨的野外草地铺设和垫子被雨水淋湿时，垫子容易吸潮，难以快速得到恢复利用；当垫子铺设在沙石、粘土等坚硬物质上时，人体坐在垫子上时，容易被坚硬物质所顶起，其舒适性差，另外垫子回弹性差，降低了垫子的使用寿命；而炎热的夏天，垫子在高温的作用下，容易产生一定的粘性，其舒适性降低。
发明内容
鉴于以上现有技术的不足之处，本发明提供了一种改性PVC发泡垫子，以解决现有PVC垫子热稳定性、耐磨性、自清洁性、防潮性及回弹性等各项性能无法兼顾，难以保证不同户外复杂环境下使用的可靠性和舒适性的问题。
为达到以上目的，本发明采用的技术方案为：
一种改性PVC发泡垫子的制备方法，所述制备方法包括以下步骤：
步骤S1：将由PVC粉、改性废橡胶粉、增塑剂、无机填料、添加剂、色料、发泡剂和助剂复配的原料混合成混合浆料，静置6～12h进行预发泡；
步骤S2：将步骤S1处理后的混合浆料涂布形成浆料层，先逐步升温至60～90℃，继续发泡操作5～30min，再逐步升温至195～220℃进行发泡反应，发泡操作0.5～3min后，冷却成预定厚度的发泡垫体；
步骤S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子。
本发明发泡垫子原料通过预发泡、逐步升温后发泡进行分步发泡，提高发泡垫体的发泡倍率，并有效控制发泡垫体的发泡过程，防止PVC熔体发泡过程中气泡破裂导致的塌孔和并孔，并可在发泡垫体内部形成连续性的相连通气泡，提高发泡垫体的回弹性。
优选地，所述助剂由无水乙醇和四氢呋喃复配得到。所述助剂不仅有助于稀释原料，使发泡垫体原料复配成液体，而且利用无水乙醇的易挥发性，可在静置过程中进行发泡垫体的预发泡。
优选地，按重量份计，所述原料分别为80～120份PVC粉、20～30份改性废橡胶粉、5～15份增塑剂、1.5～2份无机填料、2～7份添加剂、1～10份色料、0.5～5.5份发泡剂和50～150份助剂。
优选地，所述改性废橡胶粉的改性方法为：按重量份称取100份废橡胶粉和10～30份PVC粉加入密炼机中，再加入相当于废橡胶粉质量5～10％的甲基丙烯酸酯和相当于废橡胶粉质量0.1～0.5％的引发剂，经溶胀和混炼均匀后，在硫化温度100～200℃下经过硫化和界面反应得到所述改性废橡胶粉。所述废橡胶粉选用氟橡胶、硅橡胶或氟硅橡胶中的一种。废橡胶粉和PVC粉先在甲基丙烯酸酯单体中进行溶胀，然后通过密炼机混炼均匀，使得甲基丙烯酸酯单体和引发剂分散均匀，再通过高温硫化加工成型；甲基丙烯酸酯单体在溶胀的橡胶/PVC共混聚合物中进行原位聚合，并与橡胶/PVC共混聚合物形成互穿或半互穿聚合物网络结构；通过改性后的废橡胶粉，不仅有利于与PVC粉相容，提高发泡垫子的力学性能，而且有助于提高发泡垫子的防潮性能和耐候性，进一步延长发泡垫子的使用寿命。另外，本发明发泡垫子通过改性橡胶粉的添加，大大增强了PVC熔体的强度，从而有效地避免了高发泡过程中气泡破裂导致的塌孔和并孔。
优选地，所述增塑剂为邻苯二甲酸二辛酯、邻苯二甲酸二丁酯、邻苯二甲酸二壬酯、邻苯二甲酸丁苄酯中的至少一种。增塑剂的添加，提高了发泡垫体的加工性能。
优选地，所述无机填料为轻质碳酸钙、高岭土、氧化锌、炭黑、云母粉、硅微粉中的至少一种。无机填料的添加，则起到补强作用，并进一步提高发泡垫子的耐磨性。
优选地，所述添加剂为结构式I所示的吡啶盐衍生物离子液体，
，
其中，式中R1选自甲基或乙基；X-为BF4 -或PF6 -,m与n的比值为1～4∶1。
所述吡啶盐衍生物离子液体的具体制备方法为：将吡啶类化合物和2-溴乙基丙烯酸酯以摩尔比1∶1溶于乙腈或四氢呋喃溶液中，在搅拌下加热回流11～12小时后过滤，得到丙烯酸酯取代的吡啶衍生物；将丙烯酸酯取代的吡啶衍生物与丙烯酸三氟乙酯以1～4∶1的摩尔比进行共聚而得到结构式I所示的吡啶盐衍生物离子液体。
本发明添加的吡啶盐衍生物离子液体，先通过吡啶类化合物与2-溴乙基丙烯酸酯进行取代反应，然后与丙烯酸三氟乙酯进行聚合反应得到。本发明的吡啶盐衍生物离子液体不仅促进了原料中无机组分和有机组分的相容性，使两者均匀分散，提高了发泡垫子的整体性能，有效减少局部出现开裂的问题；而且添加剂中含有的多个吡啶盐结构提高了发泡垫子的热稳定性和阻燃性能；另外，该添加剂所带的多个含氟官能团降低了聚氯乙烯发泡垫子的水汽透过率，提高了发泡垫子的防潮性能和自清洁性能，而丙烯酸酯结构的共聚物则促进了发泡垫子的易加工性能。
优选地，所述色料为钛白粉、玫瑰红、中铬黄、偶氮红、酞青绿、酞青蓝中的至少一种。
优选地，所述发泡剂由偶氮二甲酰胺或N，N-二亚硝基五亚甲基四胺与碳酸氢钠复配得到。本发明复配的发泡剂，受热时分解平缓、放出的热量较少，获得的发泡垫子泡孔均匀细密，使得发泡垫子的撕裂强度和断裂伸长率等力学性能进一步得到改善。
本发明的另外一方面是提供一种改性PVC发泡垫子，所述改性PVC发泡垫子采用如上述改性PVC发泡垫子的制备方法制备得到。
本发明的有益效果：
相对于现有PVC垫子，本发明改性PVC发泡垫子，不仅安全环保，具有优异的热稳定性、耐磨性及回弹性，而且具有良好的自清洁性和防潮性，可保证不同户外复杂环境下发泡垫子使用的可靠性和舒适性。
具体实施方式
以下描述用于揭露本发明以使本领域技术人员能够实现本发明。以下描述中的优选实施例只作为举例，本领域技术人员可以想到其他显而易见的变型。
实施例1
本实施例的改性PVC发泡垫子的制备方法，其包括以下步骤：
步骤S1：将由80份PVC粉、20份改性废橡胶粉、5份邻苯二甲酸二辛酯、1.5份轻质碳酸钙、2份添加剂、1份钛白粉、0.5份发泡剂和50份助剂复配的原料混合成混合浆料，静置6h进行预发泡；所述助剂由质量比为1：5的无水乙醇和四氢呋喃复配得到；所述发泡剂由质量比为1：2的偶氮二甲酰胺与碳酸氢钠复配得到；
步骤S2：将步骤S1处理后的混合浆料涂布形成浆料层，先逐步升温至70℃，继续发泡操作10min，再逐步升温至195℃进行发泡反应，发泡操作3min后，冷却成预定厚度的发泡垫体；
步骤S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子。
所述改性废橡胶粉的改性方法为：按重量份称取100份废橡胶粉和10份PVC粉加入密炼机中，再加入相当于废橡胶粉质量5％的甲基丙烯酸酯和相当于废橡胶粉质量0.1％的引发剂过硫酸钠，先溶胀60min，再混炼均匀，最后在硫化温度150℃下经过硫化和界面反应得到所述改性废橡胶粉。所述废橡胶粉选用氟橡胶。
所述添加剂为吡啶盐衍生物离子液体（化学式如结构式I所示），所述吡啶盐衍生物离子液体的具体制备方法为：将0.1mol的4-甲基吡啶和0.1mol的2-溴乙基丙烯酸酯溶于1L乙腈溶液中，在搅拌下加热回流12小时后过滤，并将滤饼溶于去离子水中，加入氟硼酸钠，出现大量的白色沉淀丙烯酸酯取代的吡啶衍生物；将0.1mol的丙烯酸酯取代的吡啶衍生物与0.025mol的丙烯酸三氟乙酯溶于1L乙醇溶液中，加入0.01g偶氮二异丁腈作为自由基引发剂进行共聚而得到结构式I所示的吡啶盐衍生物离子液体。
其化学结构的表征如下：H1NMR(DMSO-d6):δ1.14(3H),1.71-1.86(8H),2.23-2.39(14H),2.43-2.58(4H),4.38-4.61(10H),4.70-4.82(8H),7.53-7.66(8H),8.66-8.79(8H)。由此可以说明丙烯酸三氟乙酯与丙烯酸酯取代的吡啶衍生物基本上以1∶4的比例共聚。
实施例2
本实施例的改性PVC发泡垫子的制备方法，其包括以下步骤：
步骤S1：将由100份PVC粉、25份改性废橡胶粉、10份邻苯二甲酸二丁酯、2份氧化锌、5份添加剂、4份玫瑰红、3.5份发泡剂和90份助剂复配的原料混合成混合浆料，静置12h进行预发泡；所述助剂由质量比为1：5的无水乙醇和四氢呋喃复配得到；所述发泡剂由质量比为1：2的N，N-二亚硝基五亚甲基四胺与碳酸氢钠复配得到；所述添加剂同实施例1；
步骤S2：将步骤S1处理后的混合浆料涂布形成浆料层，先逐步升温至90℃，继续发泡操作30min，再逐步升温至200℃进行发泡反应，发泡操作1min后，冷却成预定厚度的发泡垫体；
步骤S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子。
所述改性废橡胶粉的改性方法为：按重量份称取100份废橡胶粉和20份PVC粉加入密炼机中，再加入相当于废橡胶粉质量7％的甲基丙烯酸酯和相当于废橡胶粉质量0.3％的引发剂过硫酸钠，先溶胀60min，再混炼均匀，最后在硫化温度200℃下经过硫化和界面反应得到所述改性废橡胶粉。所述废橡胶粉选用硅橡胶。
实施例3
本实施例的改性PVC发泡垫子的制备方法，其包括以下步骤：
步骤S1：将由120份PVC粉、30份改性废橡胶粉、15份邻苯二甲酸二壬酯、2份炭黑、7份添加剂、10份酞青蓝、5.5份发泡剂和150份助剂复配的原料混合成混合浆料，静置12h进行预发泡；所述助剂由质量比为1：5的无水乙醇和四氢呋喃复配得到；所述发泡剂由质量比为1：2的偶氮二甲酰胺与碳酸氢钠复配得到；所述添加剂同实施例1；
步骤S2：将步骤S1处理后的混合浆料涂布形成浆料层，先逐步升温至90℃，继续发泡操作30min，再逐步升温至220℃进行发泡反应，发泡操作3min后，冷却成预定厚度的发泡垫体；
步骤S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子。
所述改性废橡胶粉的改性方法为：按重量份称取100份废橡胶粉和30份PVC粉加入密炼机中，再加入相当于废橡胶粉质量10％的甲基丙烯酸酯和相当于废橡胶粉质量0.5％的引发剂过硫酸钠，先溶胀60min，再混炼均匀，最后在硫化温度200℃下经过硫化和界面反应得到所述改性废橡胶粉。所述废橡胶粉选用氟橡胶。
对比例1
本对比例的改性PVC发泡垫子的制备方法，其步骤基本与实施例1相同，不同之处在于，本对比例的制备方法，步骤S1的原料中未含改性废橡胶粉。
对比例2
本对比例的改性PVC发泡垫子的制备方法，其步骤基本与实施例1相同，不同之处在于，本对比例的制备方法，步骤S1的原料中废橡胶粉未经改性处理。
对比例3
本对比例的改性PVC发泡垫子的制备方法，其步骤基本与实施例1相同，不同之处在于，本对比例的制备方法，步骤S1的原料中未含结构式I所示的吡啶盐衍生物离子液体添加剂。
对比例4
本对比例的改性PVC发泡垫子的制备方法，其步骤基本与实施例1相同，不同之处在于，本对比例的制备方法，步骤S1的原料中发泡剂仅为偶氮二甲酰胺。
将实施例1～3及对比例1～4制备得到的改性PVC发泡垫子进行性能测试，其性能结果如表1所示：
表1
拉伸强度，MPa 伸长率，% 氧指数，% 热稳定性，h 耐磨性，% 回弹性,% 防潮性
实施例1 8.1 258 30.5 15 4.84 24.8 优
实施例2 7.8 264 29.2 16 5.18 26.2 优
实施例3 7.9 281 28.7 15 5.03 25.5 优
对比例1 7.6 152 28.6 12 3.38 9.7 差
对比例2 6.8 232 29.3 11 3.67 21.2 良
对比例3 7.5 251 25.7 10 4.12 23.7 良
对比例4 7.8 224 29.2 13 4.72 16.8 优
其中，拉伸强度和伸长率采用CTM6000万能试验机(上海协强仪器)测试；氧指数按GB/T2406.2-2009进行测试。
热稳定性测试方法，根据GB2917-82《聚氯乙烯热稳定性测试方法-刚果红法和pH法》中的刚果红法进行，通过稳定时间评价热稳定性。
耐磨性测试方法，裁切长*宽*厚为10*10*2cm的发泡垫子样品置于摩擦试验机上，打磨样品1000转后，计算得到样品磨损前后的平均质量损失量，即磨损率，用于评价样品的耐磨性。
回弹性测试方法，裁切长*宽*厚为10*10*2cm的发泡垫子样品置于具有平整表面的板上，将重量为50g的钢球从距离样品1米高的高度下落，以使该球与样品发生碰撞，通过测量样品撞击后的回弹高度，得到样品的回弹性能。
防潮性测试方法，将发泡垫子置于容器温度为20度，湿度为90%RH的恒温恒湿箱中7天。测试结束后，以3级评分标准通过目测方式评价测试样品的表面水份情况。评价标准：优：没有观察到水珠凝结在样品表面；良：观察到少量水珠凝结在样品表面；差：观察到大量水珠凝结在样品表面。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是本发明的原理，在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明的范围内。

Claims (6)

1.一种改性PVC发泡垫子的制备方法，其特征在于，所述制备方法包括以下步骤：
步骤S1：将由PVC粉、改性废橡胶粉、增塑剂、无机填料、添加剂、色料、发泡剂和助剂复配的原料混合成混合浆料，静置6～12h进行预发泡；
步骤S2：将步骤S1处理后的混合浆料涂布形成浆料层，逐步升温至195～220℃进行发泡反应，发泡操作0.5～3min后，冷却成预定厚度的发泡垫体；
步骤S3：采用模具热压步骤S2得到的发泡垫体，使其成型出所需轮廓造型，经裁切后得到所述改性PVC发泡垫子；
所述改性废橡胶粉的改性方法为：按重量份称取100份废橡胶粉和10～30份PVC粉加入密炼机中，再加入相当于废橡胶粉质量5～10％的甲基丙烯酸酯和相当于废橡胶粉质量0.1～0.5％的引发剂，经溶胀和混炼均匀后，在硫化温度100～200℃下经过硫化和界面反应得到所述改性废橡胶粉；所述废橡胶粉选用氟橡胶、硅橡胶或氟硅橡胶中的一种；
所述添加剂为结构式I所示的吡啶盐衍生物离子液体，
，
其中，式中R1选自甲基或乙基；X-为BF4 -或PF6 -,m与n的比值为1～4∶1；
所述发泡剂由偶氮二甲酰胺或N，N-二亚硝基五亚甲基四胺与碳酸氢钠复配得到。
2.如权利要求1所述的改性PVC发泡垫子的制备方法，其特征在于，按重量份计，所述原料分别为80～120份PVC粉、20～30份改性废橡胶粉、5～15份增塑剂、1.5～2份无机填料、2～7份添加剂、1～10份色料、0.5～5.5份发泡剂和50～150份助剂。
3.如权利要求1所述的改性PVC发泡垫子的制备方法，其特征在于，所述增塑剂为邻苯二甲酸二辛酯、邻苯二甲酸二丁酯、邻苯二甲酸二壬酯、邻苯二甲酸丁苄酯中的至少一种。
4.如权利要求1所述的改性PVC发泡垫子的制备方法，其特征在于，所述无机填料为轻质碳酸钙、高岭土、氧化锌、炭黑、云母粉、硅微粉中的至少一种。
5.如权利要求1所述的改性PVC发泡垫子的制备方法，其特征在于，所述色料为钛白粉、玫瑰红、中铬黄、偶氮红、酞青绿、酞青蓝中的至少一种。
6.一种改性PVC发泡垫子，其特征在于，所述改性PVC发泡垫子采用如权利要求1～5任一项所述改性PVC发泡垫子的制备方法制备得到。
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