CN104072843A - 一种多尺度复合功能母粒及其制备方法 - Google Patents

一种多尺度复合功能母粒及其制备方法 Download PDF

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CN104072843A
CN104072843A CN201410255528.3A CN201410255528A CN104072843A CN 104072843 A CN104072843 A CN 104072843A CN 201410255528 A CN201410255528 A CN 201410255528A CN 104072843 A CN104072843 A CN 104072843A
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whisker
talcum powder
parts
multiple dimensioned
functional agglomerate
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CN104072843B (zh
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丁鹏
施利毅
唐圣福
刘枫
宋娜
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University of Shanghai for Science and Technology
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DONGGUAN-SHU INSTITUTE OF NANOTECHNOLOGY
University of Shanghai for Science and Technology
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Abstract

本发明公开了一种多尺度复合功能母粒，其由如下重量份数的原料而制成：滑石粉：20～80份；晶须：10～70份；载体：8～40份；所述的滑石粉粒径为50nm-3μm；所述的晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的一种或两种，晶须长度为5-100μm，平均直径为20nm-3μm；所述的载体为塑料、热塑性弹性体的一种或两种。本发明还公开了上述的多尺度复合功能母粒的制备方法，包括备料、加料、预混合、双螺杆挤出、风冷、切粒等步骤。本发明实现了粒径小于3μm，填充量大于75wt％的超微细无机粉体母粒用的连续生产，解决了高填充母粒制备过程中超微细无机粉体喂料难、计量不准确的问题，还可以减少粉尘飞扬，提高母粒和树脂基体间的相容性。

Description

一种多尺度复合功能母粒及其制备方法
技术领域
本发明涉及塑料工业技术领域，尤其涉及一种多尺度复合功能母粒及其制备方法。
背景技术
塑料母粒是指由超出常规添加量(多为50wt％以上)的塑料助剂加入载体树脂中而制得的一种新型塑料成型加工助剂。在成型塑料制品时，可直接加入母粒，使制品达到预定的性能。使用塑料母粒可以简化生产工艺，减少粉尘飞扬，减小设备的磨损，节省原料，使原料混合方便、混炼质量均匀，从而提高生产效率及制品的性能指标。因此，塑料母粒对推动塑料工业的迅猛发展起了很大作用。
滑石粉，其结构呈片状或鳞片状，属单斜晶系，在已知矿物中滑石粉的硬度最小，对塑料加工设备使用寿命有利。滑石粉应用于塑料改性，在提高刚性的同时，耐热性能也有相应的提高，从而提高热变形温度。但是滑石粉的添加含量增大，复合材料的拉伸强度会下降，此外，复合材料的冲击韧性和光泽也有明显的下降。
晶须是一种纤维状的单晶材料，其晶体结构完整，内部缺陷较少，纯度高，直径细小，具有高强度、高模量、耐高温、耐磨、耐腐蚀、轻量等特性，而且在电、光、磁学等方面也表现出不同的性能，广泛应用于各种高性能先进复合材料。亚微观尺寸的晶须填充聚合物，不但与聚合物能产生显著的增强效果，而且对聚合物基体的成型加工影响较小，加工流动性好，可以实现聚合物的显微增强、各向同性、高表面质量等。
近年来，由于无机超微细滑石粉及晶须状无机填料，尤其是纳米尺寸填料可以大幅改善塑料制品的性能同时降低原料成本，其使用得到了改性塑料行业的极大重视，且使用量越来越大。
然而，目前超微细无机填充改性塑料，大多都是直接添加，或者首先通过密炼-单螺杆挤出工艺制备超微细无机母粒，然后添加。这两种方式都会带来粉体飞扬对环境形成二次污染的问题，并且还存在着工艺不连续、计量不准确、产品性能不稳定等问题。
现有的双螺杆制备工艺是工业上最常用的塑料复合加工手段，可以实现产品的连续生产、精确计量等，但是在高填充母粒制备过程中，由于超微细无机粉体的松装密度极小，采用一般的双螺杆挤出机，高填充的喂料将是一个大问题，难以实现填充量大于75wt％的超微细无机功能母粒的制备。
然而，随着现代工业的发展,对生产环境及超微细无机填料综合性能提出了越来越高的要求，特别是高细度、高品质的超微细无机功能母粒，有着更加广泛的应用，在国内外市场上供不应求。
现有的产品、制备方法，均不能满足市场的需求，所以攻破高细度、高品质的超微细无机复合功能母粒的制备的关键技术已经迫在眉睫。
发明内容
针对现有技术的上述不足，本发明的目的在于提供一种以滑石粉及金属氧化物须晶为主要成分、并可提高母粒和应用树脂载体间的相容性、产品性能稳定的多尺度复合功能母粒。
本发明的目的还在于提供该多尺度复合功能母粒的制备方法，以解决高填充喂料、计量及连续生产的问题，减少粉尘飞扬，并容易产业化。
本发明的上述目的是通过如下技术方案来实现的：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  20～80份
晶须    10～70份
载体    8～40份；
所述的滑石粉粒径为50nm-3μm。
所述的晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的一种或两种，晶须长度为5-100μm，平均直径为20nm-3μm。
所述的载体为塑料、热塑性弹性体的一种或两种。
所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种。
所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
一种上述的多尺度滑石粉/晶须功能母粒的制备方法，其包括以下步骤：
(1)按照设定比例准确称量原料，备料：
滑石粉  20～80份
晶须    10～70份
载体    8～40份
(2)加料、预混合：将40-100％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将剩下的滑石粉和0-50％晶须通过第一侧喂料口喂料，之后将剩下的晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
(3)挤出、造粒：将步骤(2)所制得的混合物在双螺杆挤出机中进行塑化挤出，之后风冷热切造粒，得到多尺度滑石粉/晶须功能母粒。
所述步骤(3)中双螺杆挤出机的挤出温度为175～245℃。
所述的滑石粉粒径为50nm-3μm；晶须为Al2O3、CaSO4、ZnO、MgSO4等无级晶须的任意一种，晶须长度为5-100μm，平均直径为20nm-3μm；所述的载体为塑料、热塑性弹性体的一种或两种；所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种；所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
与现有技术相比，本发明的有益效果是：
(1)本发明制备的复合型功能母粒，提高了母粒和应用树脂载体间的相容性能，解决了单一组分母粒造成性能提升的单一化、性能不稳定等问题；本发明提供的多尺度复合母粒能更好的实现母粒多功能化、稳定化，该母粒作为尼龙、聚丙烯、聚乙烯等塑料的改性填料，可以有效的提高复合材料的强度及化学稳定性，同时具有良好的加工性能。
(2)本发明提供的制备方法，采用独特的喂料方式、双螺杆挤出机挤出造粒，解决了超微细无机粉体母粒制备的一个重大难题，实现了粒径小于3μm(大于5000目)，填充量大于75wt％的超微细无机粉体母粒用的连续生产，是超微细无机粉体母粒制备技术的一个重大的突破。
(3)本发明克服了因为超微细无机粉体的松装密度极小，一般的双螺杆挤出机会遇到高填充喂料的难题，难以实现填充量大于75wt％的超微细无机功能母粒的制备的问题；本发明解决了高填充母粒制备过程中超微细无机粉体喂料难、计量不准确的问题，同时还可以减少粉尘飞扬，提高母粒和树脂基体间的相容性。
(4)本发明提供的制备方法，步骤较少、原料少，，降低成本，工艺合理、操作方便、控制精确，易于产业化。
下面结合具体实施例来详细描述本发明，但并不是对本发明的进一步限制。
具体实施方式
实施例1：
本实施例提供的多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  20～80份
晶须    10～70份
载体    8～40份；
所述的滑石粉粒径为50nm-3μm。
所述的晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的一种或两种，晶须长度为5-100μm，平均直径为20nm-3μm。
所述的载体为塑料、热塑性弹性体的一种或两种。
所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种。
所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：
(1)按照设定比例准确称量原料，备料：
滑石粉  20～80份
晶须    10～70份
载体    8～40份；
(2)加料、预混合：将40-100％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将剩下的滑石粉和0-50％晶须通过第一侧喂料口喂料，之后将剩下的晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
(3)挤出、造粒：将步骤(2)所制得的混合物在双螺杆挤出机中进行塑化挤出，之后风冷热切造粒，得到多尺度滑石粉/晶须功能母粒。
所述步骤(3)中双螺杆挤出机的挤出温度为175～245℃。
所述的滑石粉粒径为50nm-3μm；晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的任意一种，晶须长度为5-100μm，平均直径为20nm-3μm；所述的载体为塑料、热塑性弹性体的一种或两种；所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种；所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
实施例2：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  50份
晶须    30份
载体    20份；
所述的滑石粉粒径为200nm；
所述的晶须为ZnO晶须，晶须长度为35μm，平均直径为2μm。
所述的载体为聚乙烯。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：
(1)按照设定比例准确称量原料，备料：
滑石粉  50份
晶须    30份
载体    20份
(2)加料、预混合：将40％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将剩下的60％滑石粉通过第一侧喂料口喂料，之后将全部晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
(3)挤出、造粒：将步骤(2)所制得的混合物在双螺杆挤出机中进行塑化挤出，之后风冷热切造粒，得到多尺度滑石粉/晶须功能母粒。
所述步骤(3)中双螺杆挤出机的挤出温度为205～245℃。
所述的滑石粉粒径为200nm；晶须为ZnO，晶须长度为35μm，平均直径为2μm；所述的载体为聚乙烯。
该实施例所得的复合功能母粒可以作为尼龙、聚丙烯、聚乙烯等塑料的改性功能填料，特别适合聚乙烯的改性过程中使用，能有效提高复合材料的强度和模量。
实施例3：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1、2基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  35份
晶须    35份
载体    8份
所述的滑石粉粒径为2μm；
所述的晶须为Al2O3晶须，晶须长度为20μm，平均直径为3μm。
所述的载体为热塑性弹性体；
所述的热塑性弹性体为聚氨酯类弹性体TPU。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：不同之处在于，步骤(2)加料、预混合：将50％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将剩下的50％滑石粉和25％ZnO晶须通过第一侧喂料口喂料，之后将剩余75％ZnO晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
所述步骤(3)中双螺杆挤出机的挤出温度为205～245℃。
该实施例所得的功能母粒可以作为弹性体的改性功能填料，特别适合聚氨酯类弹性体TPU的改性过程中使用，能有效提高复合材料的强度和模量。
实施例4：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1、2、3均基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  20份
晶须    60份
载体    12份；
所述的滑石粉粒径为500nm；
所述的晶须为CaSO4晶须，晶须长度为5μm，平均直径为1μm。
所述的载体为热塑性烯烃类弹性体。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：不同之处在于，步骤(2)加料、预混合：将70％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将剩下的30％滑石粉和50％CaSO4晶须通过第一侧喂料口喂料，之后将剩下的50％晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
所述步骤(3)中双螺杆挤出机的挤出温度为175～195℃。
本实施例所得的功能母粒可以作为弹性体的改性功能填料，特别适合热塑性烯烃类弹性体的改性过程中使用，能有效提高复合材料的强度和模量。
实施例5：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1、2、3、4均基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  50份
晶须    40份
载体    16份；
所述的滑石粉粒径为1.5μm；
所述的晶须为CaSO4晶须，晶须长度为25μm，平均直径为20nm。
所述的载体为尼龙。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：不同之处在于，步骤(2)加料、预混合：将100％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将40％CaSO4晶须通过第一侧喂料口喂料，之后将剩下的60％晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
所述步骤(3)中双螺杆挤出机的挤出温度为175～195℃。
该实施例所得的功能母粒可以作为尼龙、聚丙烯、聚乙烯等塑料的改性功能填料，特别适合尼龙的改性过程中使用，能有效提高复合材料的强度和模量。
实施例6：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1、-5之一均基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  80份
晶须    10份
载体    24份；
所述的滑石粉粒径为3μm；
所述的晶须为MgSO4晶须，晶须长度为100μm，平均直径为800nm。
所述的载体为聚丙烯。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：不同之处在于，步骤(2)加料、预混合：将60％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将40％滑石粉和15％MgSO4晶须通过第一侧喂料口喂料，之后将剩余的85％晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
所述步骤(3)中双螺杆挤出机的挤出温度为175～195℃。
本实施例所得的功能母粒可以作为尼龙、聚丙烯、聚乙烯等塑料的改性功能填料，特别适合聚丙烯的改性过程中使用，能有效提高复合材料的强度和模量，所得复合材料适合汽车行业对聚丙烯材料性能要求。
实施例7：
本实施例提供的多尺度复合功能母粒及其制备方法，与实施例1、2、3、4、5、6基本相同，其不同之处在于：
一种多尺度复合功能母粒，其由如下重量份数的原料而制成：
滑石粉  65份
晶须    70份
载体    40份
所述的滑石粉粒径为50nm；
所述的晶须为Al2O3晶须，晶须长度为50μm，平均直径为1.5μm。
所述的载体为热塑性氯乙烯类弹性体。
一种上述的多尺度复合功能母粒的制备方法，其包括以下步骤：不同之处在于，步骤(2)加料、预混合：将100％滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将45％Al2O3晶须通过第一侧喂料口喂料，之后将剩余55％Al2O3晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合。
所述步骤(3)中双螺杆挤出机的挤出温度为205～245℃。
本实施例所得的功能母粒可以作为热塑性弹性体的改性功能填料，特别适合热塑性氯乙烯类弹性体的改性过程中使用，能有效提高复合材料的强度和模量。
本发明提供的产品及制备方法，采用独特的喂料方式、双螺杆挤出机挤出造粒，解决了超微细无机粉体母粒制备的一个重大难题，实现了粒径小于3μm(大于5000目)，填充量大于75wt％的超微细无机粉体母粒用的连续生产，是超微细无机粉体母粒制备技术的一个重大的突破。克服了因为超微细无机粉体的松装密度极小，一般的双螺杆挤出机会遇到高填充喂料的难题，难以实现填充量大于75wt％的超微细无机功能母粒的制备的问题；解决了高填充母粒制备过程中超微细无机粉体喂料难、计量不准确的问题，同时还可以减少粉尘飞扬，提高母粒和树脂基体间的相容性。
本发明制备的复合型功能母粒能解决单一组分母粒造成性能提升的单一化问题，本发明的多尺度复合母粒能更好的实现母粒功能化，该母粒作为尼龙、聚丙烯、聚乙烯等塑料的改性填料，可以有效的提高复合材料的强度及化学稳定性，同时具有良好的加工性能。另外。
本发明提供的制备方法，步骤较少、原料少，降低成本，工艺合理、操作方便、控制精确，易于产业化。
本发明并不限于上述实施方式，采用与本发明上述实施例相同或近似的原料及制备方法，而得到的其他类似的多尺度滑石粉/晶须功能母粒，均在本发明的保护范围之内。

Claims (10)

1.一种多尺度复合功能母粒，特征在于，其由如下重量份数的原料制成：
滑石粉  20～80份
晶须    10～70份
载体    8～40份。
2.根据权利要求1所述的多尺度滑石粉/晶须功能母粒，特征在于，所述的滑石粉粒径为50nm-3μm。
3.根据权利要求1所述的多尺度滑石粉/晶须功能母粒，特征在于，所述的晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的一种或两种，晶须长度为5-100μm，平均直径为20nm-3μm。
4.根据权利要求1所述的多尺度滑石粉/晶须功能母粒，特征在于，所述的载体为塑料、热塑性弹性体的一种或两种。
5.根据权利要求4所述的多尺度滑石粉/晶须功能母粒，特征在于，所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种。
6.根据权利要求4所述的多尺度滑石粉/晶须功能母粒，特征在于，所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
7.一种制备权利要求1-6之一所述的多尺度复合功能母粒的方法，特征在于，其包括以下步骤：
(1)按照设定比例准确称量原料，备料：
滑石粉  20～80份
晶须    10～70份
载体    8～40份；
(2)加料、预混合：将40-100％的滑石粉和全部载体通过双螺杆挤出机的主喂料口喂料，之后将其余的滑石粉和0-50％的晶须通过第一侧喂料口喂料，之后将剩下全部的晶须通过第二侧喂料口喂料，完成喂料后在高速混合机中进行预混合；
(3)挤出、造粒：将步骤(2)所制得的混合物在双螺杆挤出机中进行塑化挤出，之后风冷热切造粒，得到多尺度滑石粉/晶须功能母粒。
8.根据权利要求7所述的多尺度复合功能母粒的制备方法，特征在于，所述步骤(3)中双螺杆挤出机的挤出温度为175～245℃。
9.根据权利要求7所述的多尺度复合功能母粒的制备方法，特征在于，所述的滑石粉粒径为50nm-3μm；晶须为Al2O3、CaSO4、ZnO、MgSO4晶须的任意一种，晶须长度为5-100μm，平均直径为20nm-3μm。
10.根据权利要求7所述的多尺度复合功能母粒的制备方法，特征在于，所述的载体为塑料、热塑性弹性体的一种或两种；所述的塑料为聚丙烯、聚乙烯、尼龙的一种或两种；所述的热塑性弹性体为聚氨酯类弹性体TPU、烯烃类弹性体、氯乙烯类弹性体中的一种或两种。
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