CN103804890A - 一种挤出发泡热塑性聚氨酯弹性体粒子及其制备方法 - Google Patents
一种挤出发泡热塑性聚氨酯弹性体粒子及其制备方法 Download PDFInfo
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- CN103804890A CN103804890A CN201410055218.7A CN201410055218A CN103804890A CN 103804890 A CN103804890 A CN 103804890A CN 201410055218 A CN201410055218 A CN 201410055218A CN 103804890 A CN103804890 A CN 103804890A
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- foaming
- thermoplastic elastomer
- polyurethane thermoplastic
- extrusion
- weight part
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- B29B9/02—Making granules by dividing preformed material
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Abstract
本发明涉及一种挤出发泡热塑性聚氨酯弹性体粒子及其制备方法,所述粒子包括以下重量份的成分:100重量份的热塑性聚氨酯弹性体,0.01~0.5重量份的发泡成核剂,0.01~0.2重量份的抗氧剂,所述制备方法为:先将物料混合,然后将混合物投入挤出机造粒得到适于发泡的珠粒原料,最后将上述珠粒投入发泡专用挤出机,经口模发泡后水下切粒,制得产品粒子。本发明利用挤出法制备热塑性聚氨酯发泡粒子,控制发泡工艺条件,得到密度可控的发泡粒子,粒子泡孔密度分布均匀,整体生产方法操作简单,对设备没有特设限制要求,适合工业连续化生产。
Description
技术领域
本发明涉及一种挤出发泡热塑性聚氨酯弹性体粒子及其制备方法,属于发泡材料领域。
背景技术
以塑料为基体,通过物理或化学方法在塑料内部填充大量气泡,得到聚合物发泡材料。泡沫材料具有密度低,隔热隔音、比强度高、缓冲等一列优点,因此在包装业、工业、农业、交通运输业、军事工业、航天工业以及日用品等领域得到广泛应用。常用的泡沫塑料品种有聚氨酯(PU)软质和硬质泡沫塑料,聚苯乙烯(PS)泡沫塑料,聚乙烯(PE)泡沫塑料,聚丙烯(PP)泡沫塑料等。但是聚氨酯泡沫塑料在发泡过程中容易残留异氰酸酯,对人体有害,并且发泡材料无法回收利用。聚苯乙烯泡沫塑料产品降解困难,易产生“白色污染”问题,联合国环境组织已决定停止使用PS泡沫塑料产品。聚乙烯泡沫塑料耐高温性能较差,不适合在高温领域内应用。
热塑性聚氨酯弹性体(TPU)具有较宽泛的硬度范围,优异的耐磨性、机械强度、耐水、耐油、耐化学腐蚀、耐霉菌,可回收利用等优点。采用TPU制备的泡沫材料在保留原基体优异的性能之外,同时具备优异的回弹性,可以在较宽泛的温度范围内使用。基于上述优点,TPU发泡材料在许多工业领域(汽车工业、包装材料)以及日常生活领域(鞋材、地板涂层)具有非常广泛的应用前景。
目前制备发泡热塑性聚氨酯粒子的工艺主要为间歇式釜压发泡。其中,WO2007/082838公开了一种基于热塑性聚氨酯的泡沫,该工艺采用高压釜将TPU颗粒与分散剂,表面活性剂以及正丁烷发泡剂均匀分散在水中,升温至指定温度下保持一定的时间,然后将颗粒迅速卸压至大气压得到发泡热塑性聚氨酯粒子粒,然后经过洗涤烘干等处理,得到水蒸气模压制品的原料。该间歇式釜压发泡工艺较复杂,成本高。
发明内容
本发明所要解决的技术问题是提供一种挤出发泡热塑性聚氨酯弹性体粒子及其制备方法,该方法可连续化生产,发泡材料质量稳定。
本发明解决上述技术问题的技术方案如下:一种挤出发泡热塑性聚氨酯弹性体粒子,包括以下重量份的成分:100重量份的热塑性聚氨酯弹性体(TPU),0.01~0.5重量份的发泡成核剂,0.01~0.2重量份的抗氧剂。
在上述技术方案的基础上,本发明还可以做如下改进。
进一步,所述热塑性聚氨酯弹性体(TPU)的邵氏硬度为55A~95A。
硬度是物质受压变形程度或抗刺穿能力的一种物理度量方式。硬度可分相对硬度和绝对硬度。绝对硬度一般在科学界使用,生产实践中很少用到。我们通常使用硬度体系为相对的硬度,常用有以下几种标示方法:肖氏(也叫邵氏,邵尔,英文SHORE)、洛氏、布氏三种。邵氏一般用于橡胶类材料上。邵氏硬度也称肖氏(SHORE)硬度,常用于度量塑料,橡胶的表面抵抗坚硬物体压入的能力。肖氏硬度(HS)和布氏硬度(BHN)换算关系为HS=BHN/10+12。邵氏硬度的测试方法:用邵氏硬度计插入被测材料,表盘上的指针通过弹簧与一个刺针相连,用针刺入被测物表面,表盘上所显示的数值即为硬度值。
进一步,所述热塑性聚氨酯弹性体(TPU)的熔体流动速率(MI)为5~50g/10分钟。
上述数值是根据ASTM-1238在180℃施加5Kg的重量测得。ASTM指美国材料与试验协会(American Society for Testing and Materials,ASTM)前身是国际材料试验协会(International Association for TestingMaterials,IATM)。19世纪80年代,为解决采购商与供货商在购销工业材料过程中产生的意见和分歧,有人提出建立技术委员会制度,由技术委员会组织各方面的代表参加技术座谈会,讨论解决有关材料规范、试验程序等方面的争议问题。ASTM的宗旨就是促进公共健康与安全,提高生活质量;提供值得信赖的原料、产品、体系和服务;推动国家、地区、乃至国际经济。ASTM-1238是测试塑料熔体流动速率的美国材料协会的标准。
进一步,所述热塑性聚氨酯弹性体(TPU)为基于数均分子量为500~2000g/mol的聚四氢呋喃或数均分子量为800~1200g/mol的聚酯多元醇中的一种或两种的混合。
数均分子量(Number-average Molecular Weight):聚合物是由化学组成相同而聚合度不等的同系混合物组成的,即由分子链长度不同的高聚物混合组成。通常采用平均数分子量表征分子的大小。按分子数目统计平均,则称为数均分子量,符号为(MN)。
聚四氢呋喃,是一种易溶解于醇、酯、酮、芳烃和氯化烃,不溶于酯肪烃和水的白色蜡状固体。当温度超过室温时会变成透明液体。
聚酯多元醇,有机物,通常是由有机二元羧酸(酸酐或酯)与多元醇(包括二醇)缩合(或酯交换)或由内酯与多元醇聚合而成。二元酸有苯二甲酸或苯二甲酸酐或其酯、己二酸、卤代苯二甲酸等。多元醇有乙二醇、丙二醇、一缩二乙二醇、三羟甲基丙烷、季戊四醇等。不同品种的聚酯多元醇由于种类不同或制备工艺不一样,性质也不一样,对于聚酯多元醇比较重要的几个指标是羟值、酸值、水分、粘度、分子量、密度以及色度等。聚酯多元醇的特性及用途:聚酯型聚氨酯因分子内含有较多的酯基、氨基等极性基团,内聚强度和附着力强,具有较高的强度、耐磨性。
进一步,所述发泡成核剂为滑石、二氧化硅、碳酸钙、沸石、石墨粉、氧化铝、氢氧化钙、氢氧化铝、硼酸锌中一种或几种的混合。
进一步,所述抗氧化剂为抗氧剂1010、抗氧剂245、抗氧剂168、抗氧剂Chinox20N中一种或几种的混合。
抗氧剂1010为白色结晶粉末,化学性状稳定,可广泛应用于通用塑料,工程塑料,合成橡胶,纤维,热熔胶,树脂,油品,墨水,涂料等行业中。抗氧剂245,名称是二醇双[β-(3-叔丁基-4-羟基-5-甲基苯基)丙酸酯],该产品作为抗氧剂用于HIPS、MBS、ABS等苯乙烯聚合物,POM、PA等工程塑料以及氨纶等聚氨酯的加工和长期热稳定性的改进。同时在PVC聚合工艺中也是有效的链终止剂。本品对聚合物反应无影响,用于高抗冲聚苯乙烯、聚氯乙烯时,可在聚合前加入单体中。抗氧剂168名称是三[2.4-二叔丁基苯基]亚磷酸酯,本品辅助抗氧剂,与主抗氧剂zm-1010或1076复配,有很好的协同效应,可有效地防止聚丙烯、聚乙烯在基础注塑中的热降解,给聚合物额外的长效保护。抗氧剂Chinox20N是本领域内常规抗氧剂,具有优秀的耐热抗氧化性能,无色污、耐水解性极佳,对于TPU有非常好的效果,还可以应用于POM、PPR水管料等。
本发明解决上述技术问题的另一技术方案如下:一种挤出发泡热塑性聚氨酯弹性体粒子的制备方法,包括以下步骤:取100重量份的热塑性聚氨酯弹性体(TPU)、0.01~0.5重量份的发泡成核剂、0.01~0.2重量份的抗氧剂混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的原料,最后将上述原料投入发泡专用挤出机,并向挤出机中注入挥发性发泡剂,挤出机的机头压力为1~30MPa,熔体经口模发泡后水下切粒,制得挤出发泡热塑性聚氨酯弹性体粒子。
进一步,所述挥发性发泡剂为丙烷、正丁烷、异丁烷、正戊烷、异戊烷一种或几种的混合,所述挥发性发泡剂加入的量为1~40重量份。
进一步,所述发泡专用挤出机为单阶单螺杆挤出机、双阶串联式单螺杆挤出机、同向双螺杆挤出机中的一种。
进一步,所述发泡专用挤出机的机头压力为1MPa~30MPa,机头温度为150~185℃,水下切粒机水温在40~80℃。
所述的挤出发泡热塑性聚氨酯颗粒的发泡密度为0.05~0.5g/cm3。
本发明的性能测试:
根据美国试验材料学会标准ASTM D792-2008测试发泡颗粒发泡密度ρf。
发泡密度计算公式为:
ρf=W1/(W1+W2-W3);
其中,W1为发泡颗粒在空气中的质量,W2是使发泡颗粒浸渍在水中的金属帽的重量,W3发泡颗粒在水中的质量。
本发明的有益效果是:本发明利用挤出法制备热塑性聚氨酯发泡粒子,控制发泡工艺条件,得到密度可控的发泡颗粒,颗粒泡孔密度分布均匀,整体生产方法操作简单,对设备没有特设限制要求,适合工业连续化生产。
具体实施方式
以下对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
下面通过具体实施例对本发明进行具体描述。
所述热塑性聚氨酯弹性体(TPU)采用如表1所示的成分。
表1
其中,TPU的邵氏硬度根据ASTM D2204-05测定的。
实施例1:
将100份表1所示的热塑性聚氨酯(TPU)颗粒A,0.2重量份的滑石,0.05重量份的抗氧剂1010混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入单阶单螺杆挤出机。物料的挤出速度控制在每小时挤出55千克,向挤出机中注入正丁烷的速度控制在每小时5千克,模头压力为13Mpa,模头温度为172℃,水下切粒机水温控制在70℃。可按照上述组分比例连续添加物料,进行连续化生产,得到粒子的发泡密度为0.215g/cm3。
实施例2:
将100份表1所示的热塑性聚氨酯(TPU)颗粒A,0.3重量份的二氧化硅,0.07重量份的抗氧剂245混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入单阶单螺杆挤出机。物料的挤出速度控制在每小时挤出55千克,向挤出机中注入丙烷的速度控制在每小时7千克,模头压力为15Mpa,模头温度为168℃,水下切粒机水温控制在55℃。可按照上述组分比例连续添加物料,进行连续化生产,得到粒子的发泡密度为0.202g/cm3。
实施例3:
将100份表1所示的热塑性聚氨酯(TPU)颗粒B,0.1重量份的碳酸钙,0.1重量份的抗氧剂1010混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入同向双螺杆挤出机。物料的挤出速度控制在每小时挤出40千克,向挤出机中注入正戊烷的速度控制在每小时7千克,模头压力为16Mpa,模头温度为183℃,水下切粒机水温控制在70℃。可按照上述组分比例连续添加物料,进行连续化生产,得到粒子的发泡密度为0.152g/cm3。
实施例4:
将100份表1所示的热塑性聚氨酯(TPU)颗粒B,0.08重量份的硼酸锌,0.1重量份的抗氧剂1010,0.05重量份的抗氧剂Chinox20N混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入同向双螺杆挤出机。物料的挤出速度控制在每小时挤出40千克,向挤出机中注入正戊烷和异戊烷混合气的速度控制在每小时8千克,模头压力为18Mpa,模头温度为175℃,水下切粒机水温控制在65℃。可按照上述组分比例连续添加物料,进行连续化生产,得到粒子的发泡密度为0.132g/cm3。
实施例5:
将100份表1所示的热塑性聚氨酯(TPU)颗粒B,0.08重量份的硼酸锌,0.1重量份的抗氧剂1010,0.05重量份的抗氧剂Chinox20N混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入同向双螺杆挤出机。物料的挤出速度控制在每小时挤出40千克,向挤出机中注入正丁烷和异丁烷混合气的速度控制在每小时10千克,模头压力为20Mpa,模头温度为180℃,水下切粒机水温控制在65℃。可按照上述组分比例连续添加物料,进行连续化生产,得到粒子的发泡密度为0.112g/cm3。
对比例:不添加发泡成核剂热塑性聚氨酯发泡粒子的制备
将100份表1所示的热塑性聚氨酯(TPU)颗粒B,0.1重量份的抗氧剂1010,0.05重量份的抗氧剂Chinox20N混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的颗粒原料,最后将上述原料投入同向双螺杆挤出机。物料的挤出速度控制在每小时挤出40千克,向挤出机中注入正丁烷的速度控制在每小时8千克,模头压力为19Mpa,模头温度为175℃,水下切粒机水温控制在65℃。可按照上述组分比例连续添加物料,进行连续化生产,得到颗粒的发泡密度为0.128g/cm3。
各原料组分的添加比例以及发泡颗粒制备时的模头温度,模头压力,粒子的发泡密度汇总于下表2中。
表2
其中,上述表格中的成核剂、抗氧剂、发泡剂均以重量百分比计(基于TPU颗粒重量份)。
在实施例1~5中,得到的发泡珠粒密度在0.112~0.215g/cm3之间,颗粒表面光亮,在本发明要求范围内。但是在对比例中,在热塑性聚氨酯颗粒中没有未发泡成核剂,得到粒子密度为0.128g/cm3,粒子内部泡孔密度分布不均匀,有明显的大小气孔存在。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,包括以下重量份的成分:100重量份的热塑性聚氨酯弹性体,0.01~0.5重量份的发泡成核剂,0.01~0.2重量份的抗氧剂。
2.根据权利要求1所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述热塑性聚氨酯弹性体的邵氏硬度为55A~95A。
3.根据权利要求1所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述热塑性聚氨酯弹性体的熔体流动速率为5~50g/10分钟。
4.根据权利要求1至3任一项所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述热塑性聚氨酯弹性体为基于数均分子量为500~2000g/mol的聚四氢呋喃或数均分子量为800~1200g/mol的聚酯多元醇中的一种或两种的混合。
5.根据权利要求1所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述发泡成核剂为滑石、二氧化硅、碳酸钙、沸石、石墨粉、氧化铝、氢氧化钙、氢氧化铝、硼酸锌中一种或几种的混合。
6.根据权利要求1所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述抗氧化剂为抗氧剂1010、抗氧剂245、抗氧剂168、抗氧剂Chinox20N中一种或几种的混合。
7.一种挤出发泡热塑性聚氨酯弹性体粒子的制备方法,其特征在于,包括以下步骤:取100重量份的热塑性聚氨酯弹性体、0.01~0.5重量份的发泡成核剂、0.01~0.2重量份的抗氧剂混合均匀,然后将上述混合物投入挤出机造粒得到适于发泡的原料,最后将上述原料投入发泡专用挤出机,并向发泡专用挤出机中注入挥发性发泡剂,熔体经口模发泡后水下切粒,制得挤出发泡热塑性聚氨酯弹性体粒子。
8.根据权利要求7所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述挥发性发泡剂为丙烷、正丁烷、异丁烷、正戊烷、异戊烷一种或几种的混合,所述挥发性发泡剂加入的量为1~40重量份。
9.根据权利要求7所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述发泡专用挤出机为单阶单螺杆挤出机、双阶串联式单螺杆挤出机、同向双螺杆挤出机中的一种。
10.根据权利要求7所述挤出发泡热塑性聚氨酯弹性体粒子,其特征在于,所述发泡专用挤出机的机头压力为1~30MPa,机头温度为150~185℃,水下切粒机水温在40~80℃。
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KR20160124820A (ko) | 2016-10-28 |
EP3109281A4 (en) | 2017-10-18 |
ES2932412T3 (es) | 2023-01-18 |
KR102109392B1 (ko) | 2020-05-12 |
US20170246765A1 (en) | 2017-08-31 |
EP3109281B1 (en) | 2022-10-19 |
MX2016010761A (es) | 2017-02-02 |
PT3109281T (pt) | 2022-11-28 |
CN103804890B (zh) | 2016-01-27 |
EP3109281A1 (en) | 2016-12-28 |
US10137601B2 (en) | 2018-11-27 |
WO2015123961A1 (zh) | 2015-08-27 |
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