CN113025077A - 一种超细白云石粉的制备方法 - Google Patents

一种超细白云石粉的制备方法 Download PDF

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CN113025077A
CN113025077A CN202110223273.2A CN202110223273A CN113025077A CN 113025077 A CN113025077 A CN 113025077A CN 202110223273 A CN202110223273 A CN 202110223273A CN 113025077 A CN113025077 A CN 113025077A
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方伟豹
褚孔建
梁世叙
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Wuxuan Baofeng Mining Co ltd
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Abstract

本发明公开了一种超细白云石粉的制备方法，是将白云石粉碎至粒径大小为0.5‑5.0μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量1‑3%的改性剂球磨进行表面改性，得到改性超细白云石粉，所述改性剂由聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂组成。本发明方法制备的白云石粉不仅能够提高白云石粉的分散性，降低粉体的吸油值，增强白云石超细粉与基体间的相容性，还能使白云石粉体具有良好的机械强度和力学性能；且制备工艺简单，成本较低，容易实现工业化生产。

Description

一种超细白云石粉的制备方法
技术领域
本发明属于无机材料制备技术领域，具体是一种超细白云石粉的制备方法。
背景技术
白云石是一种常见的白色非金属矿物，属于CaCO3和MgCO3的复合碳酸盐矿物，在我国蕴藏量极其丰富，是一种重要的钙镁资源，白云石作为填料已经广泛应用于塑料、橡胶、粘结剂等领域，但大颗粒的白云石粉体在高分子材料中会引起材料本身的机械强度如抗拉伸能力和断裂伸长率等各项指标的恶化，将白云石超细化成为一种必然。
由于超细白云石粉由于粒径较小，粒子之间容易发生团聚现象，分散性较差，导致与基体材料的相容性差，进而影响材料的性能。目前对超细粉体最有效的方法就是对其进行表面改性，从而达到改善粉体物理化学性质、增强填料与基体的相容性、提高分散性、改善界面性质、赋予颗粒新功能的目的。现有技术对白云石粉的改性主要是利用脂肪酸盐进行表面处理，该方法仍然存在出现局部团聚、与基体的相容性及界面结合力相差、力学性能较差等问题。
发明内容
本发明针对上述问题，提供一种超细白云石粉的制备方法。本发明方法不仅能够提高白云石粉的分散性，降低粉体的吸油值，增强白云石超细粉与基体间的相容性，还能使白云石粉体具有良好的机械强度和力学性能；且制备工艺简单，成本较低，容易实现工业化生产。
为了实现以上目的，本发明采用的技术方案如下：
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为0.5-5.0μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量1-3%的改性剂球磨进行表面改性，得到改性超细白云石粉，所述改性剂由聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂组成。
优选的，所述偶联剂为硅烷偶联剂、稀土偶联剂、铝酸酯偶联剂和钛酸酯偶联剂中的一种或多种组合。
优选的，所述改性剂中聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂的质量比为0.1-0.5:1-2:0.1-0.5:1。
优选的，所述球磨机的研磨介质为氧化铝或氧化锆磨球，磨球选用直径为5mm-10mm小球和30-50mm的大球混合，磨球按照球料比为1:15-20的比例加入。
优选的，所述小球和大球的重量比为1:3-5。
优选的，所述表面改性是在转速为300-500r/min下干法处理30-60min。
优选的，所述硅烷偶联剂为KH560、KMB803、KH570、A171型号中的一种。
与现有技术相比，本发明的优点及有益效果为：
本发明方法将白云石粉碎成超细粉后，再用聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂组成的改性剂对白云石进行干法表面改性，不仅能够提高白云石粉的分散性，降低粉体的吸油值，增强白云石超细粉与基体间的相容性，还能使白云石粉体具有良好的机械强度和力学性能；且制备工艺简单，成本较低，容易实现工业化生产。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明。应该强调的是，下述说明仅仅是示例性的，而不是为了限制本发明的范围及其应用。
实施例1
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为0.5μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量2.5%的改性剂，在转速为500r/min下球磨40min进行表面改性，得到改性超细白云石粉。所述改性剂由质量比为0.3:1.5:0.2:1的聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和KH560硅烷偶联剂组成。所述球磨机的所述球磨机的研磨介质为氧化锆磨球，磨球选用直径为5mm小球和40mm的大球混合，小球和大球的重量比为1:3，磨球按照球料比为1:15的比例加入。
实施例2
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为1μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量1.8%的改性剂，在转速为300r/min下球磨60min进行表面改性，得到改性超细白云石粉。所述改性剂由质量比为0.5:1:0.5:1的聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和钛酸酯偶联剂组成。所述球磨机的所述球磨机的研磨介质为氧化锆磨球，磨球选用直径为10mm小球和30mm的大球混合，小球和大球的重量比为1:4，磨球按照球料比为1:20的比例加入。
实施例3
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为5μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量1.2%的改性剂，在转速为400r/min下球磨50min进行表面改性，得到改性超细白云石粉。所述改性剂由质量比为0.3:1.5:0.1:1的聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和铝酸酯偶联剂组成。所述球磨机的所述球磨机的研磨介质为氧化锆磨球，磨球选用直径为10mm小球和40mm的大球混合，小球和大球的重量比为1:3，磨球按照球料比为1:20的比例加入。
实施例4
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为2μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量2.5%的改性剂，在转速为500r/min下球磨40min进行表面改性，得到改性超细白云石粉。所述改性剂由质量比为0.3:1:0.2:1的聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和稀土偶联剂组成。所述球磨机的所述球磨机的研磨介质为氧化锆磨球，磨球选用直径为5mm小球和50mm的大球混合，小球和大球的重量比为1:5，磨球按照球料比为1:20的比例加入。
实施例5
一种超细白云石粉的制备方法，包括如下步骤：将白云石粉碎至粒径大小为2.5μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量3%的改性剂，在转速为300r/min下球磨50min进行表面改性，得到改性超细白云石粉。所述改性剂由质量比为0.4:1.2:0.4:1的聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和KMB803硅烷偶联剂组成。所述球磨机的所述球磨机的研磨介质为氧化锆磨球，磨球选用直径为10mm小球和30mm的大球混合，小球和大球的重量比为1:3，磨球按照球料比为1:15的比例加入。
将本发明实施例1-5制得的改性超细白云石粉按照常规方法测定吸油值，并按照如下配方填充于PVC塑料，其中PVC塑料的配方（重量计）为：PVC树脂100份、白云石粉15份、重质碳酸钙（400目）30份、硅油5份、硬脂酸钠1.5份、钙锌复合稳定剂3份、ACR 5份、DOP增塑剂2.5份和1010抗氧化剂0.5份，按照常规方法制成PVC塑料.填充后测定产品的拉伸强度和抗冲击强度，测定结果如表1，其中对比例为实施例1在同等条件下使用硬脂酸钠进行表面改性得到的超细白云石粉。
表1：本发明提供的超细白云石粉性能测试结果
Figure DEST_PATH_IMAGE002
从上述测试结果得知，本发明制得的超细白云石粉吸油值低，填充PVC塑料后具有很好的拉伸强度和抗冲击强度。
以上内容是结合具体的/优选的实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，其还可以对这些已描述的实施例做出若干替代或变型，而这些替代或变型方式都应视为属于本发明的保护范围。

Claims (7)

1.一种超细白云石粉的制备方法，其特征在于，包括如下步骤：将白云石粉碎至粒径大小为0.5-5.0μm，得白云石粉；再将白云石粉加入球磨机，再加入白云石粉重量1-3%的改性剂球磨进行表面改性，得到改性超细白云石粉，所述改性剂由聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂组成。
2.根据权利要求1所述超细白云石粉的制备方法，其特征在于：所述偶联剂为硅烷偶联剂、稀土偶联剂、铝酸酯偶联剂和钛酸酯偶联剂中的一种或多种组合。
3.根据权利要求2所述超细白云石粉的制备方法，其特征在于：所述改性剂中聚氧乙烯全氟烷基醇醚、氨基葡萄糖月桂酰胺、马来酸单十六醇酯丙基磺酸钠和偶联剂的质量比为0.1-0.5:1-2:0.1-0.5:1。
4.根据权利要求1所述超细白云石粉的制备方法，其特征在于：所述球磨机的研磨介质为氧化铝或氧化锆磨球，磨球选用直径为5mm-10mm小球和30-50mm的大球混合，磨球按照球料比为1:15-20的比例加入。
5.根据权利要求4所述超细白云石粉的制备方法，其特征在于：所述小球和大球的重量比为1:3-5。
6.根据权利要求1所述超细白云石粉的制备方法，其特征在于：所述表面改性是在转速为300-500r/min下干法处理30-60min。
7.根据权利要求1所述超细白云石粉的制备方法，其特征在于：所述硅烷偶联剂为KH560、KMB803、KH570、A171型号中的一种。
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CN101550290A (zh) * 2009-05-04 2009-10-07 广福建材（蕉岭）精化有限公司 改性超细白云石粉的制造方法
CN103804953A (zh) * 2013-12-10 2014-05-21 辽宁亿龙矿业股份有限公司 超细表面改性白云石的制备方法
CN107473657A (zh) * 2017-08-10 2017-12-15 青阳县永诚钙业有限责任公司 一种白云石复合料的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1451695A (zh) * 2003-04-25 2003-10-29 李柏荣 干法生产微米、亚微米有机非金属矿物、功能性母料的方法
CN101098916A (zh) * 2005-01-13 2008-01-02 金文申有限公司 含有碳纳米颗粒的复合材料
CN101550290A (zh) * 2009-05-04 2009-10-07 广福建材（蕉岭）精化有限公司 改性超细白云石粉的制造方法
CN103804953A (zh) * 2013-12-10 2014-05-21 辽宁亿龙矿业股份有限公司 超细表面改性白云石的制备方法
CN107473657A (zh) * 2017-08-10 2017-12-15 青阳县永诚钙业有限责任公司 一种白云石复合料的制备方法

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