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CN113462044B - 一种复合压花柔性发泡材料及其制备方法 - Google Patents

一种复合压花柔性发泡材料及其制备方法 Download PDF

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CN113462044B
CN113462044B CN202110788011.0A CN202110788011A CN113462044B CN 113462044 B CN113462044 B CN 113462044B CN 202110788011 A CN202110788011 A CN 202110788011A CN 113462044 B CN113462044 B CN 113462044B
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CN113462044A (zh
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高贺勇
高贺昌
吴华明
何兵
郭超
崔建坡
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Huamei Energy Saving Technology Jiangxi Co ltd
Huamei Energy Saving Technology Group Co ltd
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Abstract

本发明公开了一种复合压花柔性发泡材料及其制备方法，复合压花柔性发泡材料由压花层和保温层构成，包括骨架材料、填料、发泡剂、交联剂、促进剂、活性剂、增塑剂、润滑剂、阻燃剂、相容剂、补强剂和颜料等。所述骨架材料是由丁腈橡胶、聚氯乙烯糊树脂、氯化聚乙烯以及抗撕裂聚合物构成。本发明复合压花柔性发泡材料采用两台挤出机共混挤出和硫化发泡一体成型连续生产工艺，其生产制作工艺简便，效率高；此外，在保证原有发泡材料的保温性能以外，其抗撕裂压花层通过选用撕裂性能好的原材料或调整配方比例，以此赋予抗撕裂压花层相应的功能，从而满足了美观以及施工过程中不容易划伤裂开的需求。

Description

一种复合压花柔性发泡材料及其制备方法
技术领域
本发明属于高分子材料发泡技术领域，具体涉及一种复合压花柔性发泡材料及其制备方法。
背景技术
传统的NBR/PVC橡塑发泡保温材料，目前已很难满足不同客户和一些工程上及施工方面的需求，如外观美观性、色彩、表皮撕裂强度等。目前应用的产品有以下两种，一种是传统的单一颜色、单一胶料成型的发泡制品，如CN103102533A，其存在结构单一，整体美观程度不足，表皮撕裂性较差等缺点。另外一种是在传统橡塑保温材料的表层，通过胶粘的方式贴上一层其它色彩的复合层，这种方式加工成本高、工序繁杂、贴面不规整，并且复合强度低，所用粘结剂对环境危害较大，进而影响了橡塑绝热保温材料整体美观性和环保性。
专利CN203974373U和CN204236121 U中分别公布了“一种浮雕工艺橡塑保温板”和“一种浮雕图形柔性橡塑发泡保温板”，但一般型橡塑浮雕板在某些特定应用领域中仍存在表面撕裂强度差，外观不鲜艳靓丽、美观视觉差的缺点。CN108892825A中公布了“一种多层复合橡塑发泡保温材料及制备方法”，此工艺方法制备的复合橡塑发泡保温材料存在表面无凹凸层次，不美观，影响装饰和吸音效果等缺点；且制作成型为烘箱发泡，不是连续成型，生产效率低。
发明内容
针对现有技术中传统橡塑发泡保温材料的不足，本发明目的在于提供一种表面撕裂强度高，外观鲜艳靓丽、美观视觉好的复合压花柔性发泡材料，本发明的另一目的在于提供一种通过两台挤出机共混挤出并经连续硫化发泡生产的复合压花柔性发泡材料的制备方法。
本发明复合压花柔性发泡材料为板材。
本发明复合压花柔性发泡材料由压花层和保温层构成，压花层和保温层为整体结构。
本发明复合压花柔性发泡材料，包括骨架材料、填料、发泡剂、交联剂、促进剂、活性剂、增塑剂、润滑剂、阻燃剂、相容剂、补强剂和颜料等。
所述骨架材料包括丁腈橡胶、聚氯乙烯糊树脂和氯化聚乙烯。
本发明采用的聚氯乙烯糊树脂更有利于材料发泡，其具有较低的塑化温度，较好的分散效果，使得最终产品撕裂强度高，柔性好，表观质量好。并且，不同于现有技术的NBR/PVC体系，聚氯乙烯糊树脂的配方体系加工条件温和，加工过程更加节能，降低能源消耗。
所述保温层聚氯乙烯糊树脂以重量份计为复合压花柔性发泡材料中保温层配方的6-11。
所述压花层聚氯乙烯糊树脂以重量份计为复合压花柔性发泡材料中压花层配方的4-8。
所述保温层氯化聚乙烯以重量份计为复合压花柔性发泡材料中保温层配方的4-9。
所述压花层氯化聚乙烯以重量份计为复合压花柔性发泡材料中压花层配方的3-7。
进一步地，压花层骨架材料还包括抗撕裂聚合物，抗撕裂压花层根据产品要求调整抗撕裂聚合物比例。
所述压花层抗撕裂聚合物以重量份计为复合压花柔性发泡材料中压花层配方的10-25。
所述抗撕裂聚合物为环氧化天然橡胶ENR、氯丁橡胶CR，以及聚酯型热塑性弹性体TPEE或聚氨酯橡胶PUR中的一种。
所述抗撕裂聚合物中各组分重量份计为：环氧化天然橡胶ENR：20-90、氯丁橡胶CR：5-30，以及聚酯型热塑性弹性体TPEE或聚氨酯橡胶PUR：5-50。
优选抗撕裂聚合物中各组分重量份计环氧化天然橡胶ENR：50-60、氯丁橡胶CR：10-20，以及聚酯型热塑性弹性体TPEE或聚氨酯橡胶PUR：20-30。
所述填料选自滑石粉、氢氧化铝和碳酸钙等。
所述发泡剂为偶氮二甲酰胺等。
所述交联剂为硫磺等。
所述促进剂为二甲基二硫代氨基甲酸锌(PZ)、四硫化双戊撑秋兰姆(DPTT)、促进剂D(二苯胍)和促进剂M(2一巯基苯并噻唑)中的2-3种。
所述活性剂是由纳米氧化锌和对甲苯亚磺酸锌等组成。
所述增塑剂为环氧大豆油，以及氯化石蜡油和癸二酸二辛酯(DOS)中的一种组成。
所述压花层癸二酸二辛酯(DOS)以重量份计为复合压花柔性发泡材料中压花层配方的18-24。
所述润滑剂是选自全精炼石蜡、硬脂酸和聚乙二醇等。
所述阻燃剂为三氧化二锑等。
所述相容剂能够增强聚合物之间的相容性，增加复合材料间的界面粘合力，从而提高压花层材料的抗撕裂强度。所述相容剂为马来酸酐接枝PE等，所述保温层不添加相容剂，抗撕裂压花层根据产品要求调整相容剂用量。
所述压花层马来酸酐接枝PE以重量份计为复合压花柔性发泡材料中压花层配方的1-3。
所述补强剂为炭黑或钛白粉等。
所述颜料为无机颜料或者有机颜料，且只在压花层中加入颜料。
本发明复合压花柔性发泡材料，其保温层和压花层配比组成如下表1所示，按重量份计：
表1：保温层和压花层配方表
Figure BDA0003159752180000031
Figure BDA0003159752180000041
进一步地，本发明提供一种上述复合压花柔性发泡材料的制备方法，包括以下步骤：
a)保温层和压花层胶料的制备。
①保温层胶料制备。
按比例称取原料，并将填料和增塑剂分别分成两份，第一份填料与第二份填料的重量比为1-3:1，第一份增塑剂与第二份增塑剂的重量比为1-3:1。
优选所述第一重量份的填料、第二重量份填料的重量比是2:1，第一份增塑剂与第二份增塑剂的重量比为2:1。
所述填料选自滑石粉和氢氧化铝等。
所述第一份填料优选氢氧化铝。
所述增塑剂为环氧大豆油和氯化石蜡油等。
所述第一份增塑剂优选氯化石蜡油。
将按比例称取的骨架材料、第一份填料和增塑剂以及其它填料、增塑剂、润滑剂、阻燃剂、补强剂等进行混合，将混合后的原料投入密炼机进行密炼，密炼时间为5-10min，然后再加入第二份的填料和增塑剂继续炼胶，时间为3-5min；密炼炼胶温度为140-170℃。最后将密炼完成的胶料投入开炼机进行开炼，开炼时间为5-15min，然后冷却切片得到1号胶料。
将按比例称取的发泡剂、交联剂、促进剂、活性剂以及1号胶料投入开炼机进行开炼，时间为8-15min，开炼炼胶温度为35-60℃，然后冷却切条得到保温层胶料。
②压花层胶料制备。
按比例称取原料，并将填料和增塑剂分别分成两份，第一份填料与第二份填料的重量比为1-3:1，第一份增塑剂与第二份增塑剂的重量比为1-3:1。
优选所述第一重量份的填料、第二重量份填料重量比是2:1，第一份增塑剂与第二份增塑剂的重量比为2:1。
所述填料选自滑石粉、氢氧化铝和碳酸钙等。
所述第一份填料优选氢氧化铝。
所述增塑剂为环氧大豆油和癸二酸二辛酯(DOS)等。
所述第一份增塑剂优选癸二酸二辛酯(DOS)。
将按比例称取的骨架材料、第一份填料和增塑剂以及其它填料、增塑剂、润滑剂、阻燃剂、相容剂、补强剂以及颜料等进行混合，将混合后的原料投入密炼机进行密炼，密炼时间为5-10min，然后再加入第二份的填料和增塑剂继续炼胶，时间为3-5min；密炼炼胶温度为150-190℃。最后将密炼完成的胶料投入开炼机进行开炼，开炼时间为5-15min，开炼炼胶温度为35-60℃，然后冷却切片得到2号胶料。
将按比例称取的发泡剂、交联剂、促进剂、活性剂以及2号胶料投入开炼机进行开炼，时间为8-15min，然后冷却切条得到压花层胶料。
b)将所述保温层和压花层胶料分别喂入挤出机一体化复合装置中挤出成型，然后经浮雕印花辊进行压花处理。所述挤出机一体化复合装置为两台挤出机连接一个口模的整体装置。
c)经压花处理后的成型胶片进入自动化流水线进行连续发泡生产。
d)最后，经过冷却架进行冷却定型得到复合压花柔性发泡材料。
根据上述制备方法，所述步骤b)中，在共混挤出时，抗撕裂压花美观层和保温层均为平板状。
根据上述制备方法，所述步骤b)中，挤出机参数如下：挤出机螺杆温度为25-50℃，其中喂料段温度为25-40℃，塑化段温度为40-50℃，机头段温度为35-50℃。
所述挤出机压力通常控制为0.2-0.6MPa，具体优选为：喂料段压力为0.2-0.4MPa，塑化段压力为0.5-0.6MPa，机头压力为0.5-0.6MPa。
所述步骤b)中成型模具包括第一模和第二模，所述第一模挤出保温层胶料，第二模挤出抗撕裂压花层，所述第一模和第二模之间通过模具流道形成材料贴合结构。所述模具中第一模和第二模为复合一体化结构，复合结构中共有流道和成型区，使压花层和保温层形成无分隔的整体结构。
所述步骤b)中浮雕印花辊为经过嵌刻加工的双辊结构，浮雕压花图案可根据需要特殊设计。
所述步骤c)中，所述发泡炉发泡温度优选控制入炉温度60-100℃，出口温度155-160℃。
所述步骤c)中，发泡过程是将挤出成型的胶片连续进入发泡炉中，依次经过6个发泡区进行发泡处理，其中传输速度为一区1-1.4m/min，二区1.2-1.5m/min，三区1.5-1.7m/min，四区2.5-3.2m/min，五区3.7-4.7m/min，六区5.0-7.0m/min。
所述发泡炉各区温度分别为：一区80-110℃，二区100-115℃，三区110-125℃，四区120-135℃，五区130-145℃，六区145-160℃。
本发明的复合压花柔性发泡材料及其制备方法与现有技术相比，具有以下优势：
1、复合压花柔性发泡材料配方中引入聚氯乙烯糊树脂更有利于材料发泡，其具有较低的塑化温度，较好的分散效果，使得最终产品撕裂强度高，柔性好，表观质量好。
2、复合压花柔性发泡材料配方中引入氯化聚乙烯CPE基材，使得橡塑复合发泡体系综合性能大大提高。硫化特性方面，随着CPE的添加，橡塑共混胶的弹性、粘性和交联效果都有所提高，对比不加CPE的配方，胶料门尼值可以提高1-3，硫化值提高0.1-0.3，并且更有利于配方胶料发泡性能的提高；力学性能方面，随着CPE的添加，橡塑发泡材料的压缩弹性以及撕裂强度等均有所提高。
3、本发明一种复合压花柔性发泡材料除了选择橡塑共混材料发泡外，还选择添加撕裂强度高的弹性体材料发泡，超出了现有技术均选定橡塑共混材料进行发泡的局限性。
4、本发明压花层采用癸二酸二辛酯(DOS)作为增塑剂使用，使产品增塑效果好，挥发性低，产品柔性好。
5、本发明复合压花柔性发泡材料配方中加入相容剂马来酸酐接枝PE，解决了本发明选用撕裂强度较好的非极性聚合物时，其与原有基材的相容性会降低的问题，添加相容剂马来酸酐接枝PE后明显改善了各基材间的粘结力，产品综合性能大大提高。
6、与现有技术一般多层复合制作工艺相比较，本发明复合压花柔性发泡材料制备方法中，抗撕裂压花层和保温层胶料制备工艺相同，并且压花层和保温层胶料采用两台螺杆挤出机复合挤出一体化制作工艺，因此，本发明发泡材料既能多层复合，又实现在线连续生产，提升了本发明压花产品技术性能。
7、本发明通过优化配方，实现复合压花柔性发泡材料制备过程中开炼炼胶温度较低，发泡炉入口出口温度低，加工条件温和，加工过程更加节能，降低能源消耗。
具体实施方式
下文将结合具体实施方式和实施例，具体阐述本发明，本发明的优点和各种效果将由此更加清楚地呈现。本领域技术人员应理解，这些具体实施方式和实施例是用于说明本发明，而非限制本发明。
本发明复合压花柔性发泡材料由抗撕裂压花层和保温层构成，所述抗撕裂压花层和保温层均为柔性发泡材料，所述抗撕裂压花层和保温层通过共混挤出、硫化发泡一体成型，所述抗撕裂压花美观层和保温层为整体结构。
可根据需要，在抗撕裂压花层添加各种不同色彩的颜料，以满足不同需求。
对比例1采用CN108892825A实施例2的配方，采用本发明的制备方式制备复合压花柔性发泡材料。
各实施例的配方如下表2所示。
表2：实施例1-4配方，按重量份计。
Figure BDA0003159752180000071
Figure BDA0003159752180000081
表2中，抗撕裂聚合物种类及用量比例如表3所示。
表3：实施例1-4抗撕裂聚合物种类及用量比例。
种类 实施例1 实施例2 实施例3 实施例4
ENR 60％ 60％ 50％ 50％
TPEE 20％ 30％ - -
PUR - - 30％ 30％
CR 20％ 10％ 20％ 20％
表4：实施例1-4和对比例1性能测试结果。
Figure BDA0003159752180000091
从表4可知，本发明通过优化配方，解决了选用撕裂强度较好的非极性聚合物时，其与原有基材的相容性会降低的问题，保证了产品具有较高的撕裂强度、压缩回弹率和湿阻因子，产品综合性能大大提高。

Claims (11)

1.一种复合压花柔性发泡材料，由压花层和保温层构成，所述压花层和保温层通过共混挤出、硫化发泡一体成型，所述压花层和保温层为整体结构，所述压花层和保温层包括骨架材料、填料、发泡剂、交联剂、促进剂、活性剂、增塑剂、润滑剂、阻燃剂、补强剂，其特征在于，骨架材料为丁腈橡胶、聚氯乙烯糊树脂和氯化聚乙烯；所述压花层还包括相容剂和颜料；所述相容剂为马来酸酐接枝PE；所述压花层增塑剂为癸二酸二辛酯；压花层骨架材料还包括抗撕裂聚合物，抗撕裂聚合物为环氧化天然橡胶ENR、氯丁橡胶CR、聚酯型热塑性弹性体TPEE，或抗撕裂聚合物为环氧化天然橡胶ENR、氯丁橡胶CR、聚氨酯橡胶PUR；抗撕裂聚合物中各组分重量份计为：环氧化天然橡胶ENR：20-90、氯丁橡胶CR：5-30，以及聚酯型热塑性弹性体TPEE或聚氨酯橡胶PUR：5-50。
2.根据权利要求1所述复合压花柔性发泡材料，其特征在于，抗撕裂聚合物中各组分重量份计为；环氧化天然橡胶ENR：50-60、氯丁橡胶CR：10-20，以及聚酯型热塑性弹性体TPEE或聚氨酯橡胶PUR：20-30。
3.根据权利要求1所述复合压花柔性发泡材料，其特征在于，保温层聚氯乙烯糊树脂以重量份计为复合压花柔性发泡材料中保温层配方的6-11。
4.根据权利要求1所述复合压花柔性发泡材料，其特征在于，压花层聚氯乙烯糊树脂以重量份计为复合压花柔性发泡材料中压花层配方的4-8。
5.根据权利要求3所述复合压花柔性发泡材料，其特征在于，压花层聚氯乙烯糊树脂以重量份计为复合压花柔性发泡材料中压花层配方的4-8。
6.根据权利要求1-5任意一项所述复合压花柔性发泡材料，其特征在于，压花层抗撕裂聚合物以重量份计为复合压花柔性发泡材料中压花层配方的10-25。
7.根据权利要求1-5任意一项所述复合压花柔性发泡材料，其特征在于，促进剂为二甲基二硫代氨基甲酸锌、四硫化双戊撑秋兰姆、促进剂D和促进剂M中的2-3种。
8.根据权利要求6所述复合压花柔性发泡材料，其特征在于，促进剂为二甲基二硫代氨基甲酸锌、四硫化双戊撑秋兰姆、促进剂D和促进剂M中的2-3种。
9.根据权利要求1-5任意一项所述复合压花柔性发泡材料，其特征在于，压花层马来酸酐接枝PE以重量份计为复合压花柔性发泡材料中压花层配方的1-3。
10.根据权利要求6所述复合压花柔性发泡材料，其特征在于，压花层马来酸酐接枝PE以重量份计为复合压花柔性发泡材料中压花层配方的1-3。
11.根据权利要求7所述复合压花柔性发泡材料，其特征在于，压花层马来酸酐接枝PE以重量份计为复合压花柔性发泡材料中压花层配方的1-3。
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