CN107502003B - 一种疏水无机粉体材料的制备方法 - Google Patents

一种疏水无机粉体材料的制备方法 Download PDF

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CN107502003B
CN107502003B CN201610415981.5A CN201610415981A CN107502003B CN 107502003 B CN107502003 B CN 107502003B CN 201610415981 A CN201610415981 A CN 201610415981A CN 107502003 B CN107502003 B CN 107502003B
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inorganic powder
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CN107502003A (zh
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吴敏
黄勇
赵猛猛
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Technical Institute of Physics and Chemistry of CAS
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Abstract

本发明公开了一种疏水无机粉体材料的制备方法，该制备方法包括如下步骤：将无机粉末材料和疏水材料混合研磨；经研磨，无机粉末材料表面均匀包覆疏水材料，将多余的疏水材料分离除去，得疏水无机粉体材料。该制备方法简单、成本低、且绿色环保。本发明还公开了用此方法制备得到的疏水无机粉体材料，材料的粒径尺寸为0.01～500μm，疏水性能优异，与水的接触角可达150°。

Description

一种疏水无机粉体材料的制备方法
技术领域
本发明涉及无机粉体材料的技术领域。更具体地，涉及一种疏水无机粉体材料的制备方法。
背景技术
无机粉体材料在化工、医药、颜料、染料等领域有着广泛的应用。近年来在化工和新材料方面的应用更加活跃。但是由于粉体材料比表面能和表面极性大，粒子间极易团聚，与有机物质之间的亲和性差，不能在有机高聚物本体或有机溶剂中良好分散。研究发现在无机粉体材料表面包覆一层无机或有机物质可以很好地改善材料的分散性及耐温、耐候、耐化学性等。如发明专利CN104140692A陈国术等通过添加氧化性无机防水成分和有机防水成分对纳米二氧化钛进行表面改性，制备了疏水性好，光稳定性优异的纳米二氧化钛粉体。CN101367548A姚超等在二氧化钛的核体表面先包覆一层磷酸铝，再包覆一层氧化硅水合物，然后包覆一层氧化铝水合物，最后用表面活性剂进行有机表面处理，得到疏水性纳米二氧化钛粉体。CN101932661A将氟代烷基硅烷共价接枝到无机颗粒表面，获得疏水疏油的无机颗粒。但上述制备方法有的需使用溶剂、有的不环保且制备方法复杂。
因此，需提供一种制备方法简单的、环保的且能实现高效生产的疏水无机粉体材料的制备方法。
发明内容
本发明的第一个目的在于提供一种疏水无机粉体材料的制备方法，该制备方法简单、成本低、绿色环保，可获得性能稳定的、疏水性能优异的无机粉体材料，得到的疏水无机粉体材料的水接触角可达120°～150°。
本发明的第二个目的在于提供上述制备方法得到的一种疏水无机粉体材料，该疏水无机粉体材料性能稳定，疏水性好，且粒径横向尺寸可控制在0.01～500μm之间。
为达到上述第一个目的，本发明采用下述技术方案：
一种疏水无机粉体材料的制备方法，包括如下步骤：
将无机粉末材料和疏水材料混合研磨；
经研磨，无机粉末材料表面均匀包覆疏水材料，将多余的疏水材料分离除去，得疏水无机粉体材料。
上述制备方法中，所述无机粉末材料可为金属及其化合物、非金属及其化合物、无机矿物等无机材料。进一步地，所述金属选自铁、铝、钛、锌、钙、铜、锰、钡、锆、铅、镁、铬、镍中的一种或几种；所述金属化合物选自相应金属的氧化物、金属盐中的一种或几种；所述非金属及化合物选自金刚石、硅、碳化硅、碳化硼或氮化硼中的一种或几种；所述无机矿物选自高岭土、蒙脱土、云母、矿石或人造硅酸盐中的一种或几种。
优选地，所述金属选自铁、铝、钛、锌、钙中的一种或几种；相应的，所述金属的氧化物可为氧化铁、氧化铝、二氧化钛、氧化锌、所述非金属化合物选自金刚石、碳化硅、碳化硼或氮化硼中的一种或几种；所述无机矿物选自高岭土、蒙脱土或云母中的一种或几种。
进一步地，上述制备方法中，所述疏水材料为低表面能的材料，选自含氟的聚合物、聚烯烃及其衍生物、聚酯、聚酰胺中的一种或几种；
进一步地，上述含氟的聚合物选自聚四氟乙烯、聚偏氟乙烯、氟化乙烯丙烯共聚物、乙烯三氟氯乙烯或氟代烷基硅烷中的一种或几种；
优选地，所述聚烯烃选自聚乙烯、聚丙烯或聚苯乙烯中的一种或几种；
优选地，所述聚酯选自聚对苯二甲酸乙二醇酯、聚甲基丙烯酸甲酯、聚丁二酸丁二醇酯、聚碳酸酯中的一种或几种；
优选地，所述聚酰胺选自尼龙66或尼龙1010中的一种或两种。
进一步地，所述研磨是在球磨机或研磨仪中进行，所述研磨速度为200～540rpm，研磨时间为2～30h。
进一步地，所述球磨机或研磨仪选自行星式球磨机、振动式球磨机或臼式研磨仪。
进一步地，本发明制备方法中的分离去除多余的疏水物质的方法为用尼龙或不锈钢筛将多余疏水材料分离除去。
本发明的制备方法中，结合机械化学的方法，将无机粉末材料和疏水材料共研磨，使粉碎、研磨、摩擦等机械力应用于本发明中的无机粉末材料和疏水材料，无机粉末材料表面激活，促进粉体与疏水材料发生化学反应或者相互附着，从而达到表面疏水改性的目的。且本发明发明人经过大量的实验还发现，该方法对本发明中的无机粉末材料的疏水性处理效果最为明显。且整个制备方法中避免了溶剂的使用，制备方法绿色环保。
为达到上述第二个目的，本发明采用下述技术方案：
本发明还保护上述制备方法制备得到的疏水无机粉体材料，该疏水无机粉体材料的粒径尺寸为0.01～500μm；水接触角为120°～150°。
优选地，所述疏水无机粉体材料的粒径尺寸为0.1～10μm；更优选地，所述疏水无机粉体材料的粒径大小为0.1～5μm。
本发明中的疏水无机粉体材料的种类和形态、混合比例，本领域技术人员可根据经验掌握。
本发明的有益效果如下：
本发明通过将无机粉体和疏水物质经过简单的机械复合，方法简单、环保、易操作，使得到的疏水无机粉体材料疏水性好、性能稳定。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明。
图1示出实施例1的金刚石微粉研磨前后的形貌图。
图2示出实施例1的疏水金刚石微粉在水中的分散图。
图3示出实施例1的金刚石微粉疏水改性前后的水接触角。
具体实施方式
为了更清楚地说明本发明，下面结合优选实施例和附图对本发明做进一步的说明。附图中相似的部件以相同的附图标记进行表示。本领域技术人员应当理解，下面所具体描述的内容是说明性的而非限制性的，不应以此限制本发明的保护范围。
实施例1
一种疏水金刚石微粉的制备方法，步骤如下：
将金刚石微粉80℃真空干燥4h，取干燥后的金刚石微粉4g，与PTFE在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度500r/min。将复合后的金刚石微粉与多余PTFE用尼龙或者不锈钢筛分离，得到疏水的金刚石微粉。
图1示出金刚石微粉球磨前后的形貌图，球磨前金刚石颗粒的尺寸为15～20微米，球磨后为0.1～7微米。图2为实施例1的疏水金刚石微粉在水中的分散图，不同于未疏水改性的金刚石微粉在水中沉降，疏水改性后的金刚石微粉在水中斥水。将金刚石微粉在10MPa压制成厚度为1mm的薄片，用于水接触角测试，图3为实施例1的金刚石微粉疏水改性前后的水接触角，可以看出疏水改性前水接触角为0°，疏水改性后水接触角可达142°。
实施例2
疏水碳化硅微粉的制备方法，步骤如下：
将碳化硅微粉80℃真空干燥4h，取干燥后的碳化硅微粉4g，按照实例1的方法得到疏水碳化硅微粉。所得疏水碳化硅微粉的尺寸为0.1-0.5微米。将碳化硅微粉在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达136°。
实施例3
疏水氧化铝粉末的制备方法，步骤如下：
将氧化铝粉末80℃真空干燥4h，取干燥后的氧化铝粉末4g，按照实例1的方法得到疏水的氧化铝粉末。所得疏水氧化铝粉末的颗粒尺寸为0.1-1微米。将氧化铝粉末在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达150°。
实施例4
疏水纳米二氧化钛的制备方法，步骤如下：
将纳米二氧化钛80℃真空干燥4h，取干燥后的二氧化钛粉末4g，按照实例1的方法得到疏水纳米二氧化钛。所的疏水二氧化钛的颗粒尺寸为0.1-0.2微米。将二氧化钛粉末在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达143°。
实施例5
疏水还原铁粉的制备方法，步骤如下：
将还原铁粉80℃真空干燥4h，取干燥后的还原铁粉粉末4g，按照实例1的方法得到疏水铁粉。所得疏水铁粉的颗粒尺寸为0.5-5微米。将铁粉在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为17.8°，疏水改性后水接触角可达138°。
实施例6
疏水碳酸钙粉末的制备方法，步骤如下：
将碳酸钙粉末80℃真空干燥4h，取干燥后的碳酸钙粉末4g，按照实例1的方法得到疏水的碳酸钙粉末。所得疏水碳酸钙粉末的颗粒尺寸为0.1-5微米。将碳酸钙粉末在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达124°。
实施例7
疏水高岭土的制备方法，步骤如下：
将高岭土80℃真空干燥4h，取干燥后的高岭土4g，照实例1的方法得到疏水的高岭土。所得疏水高岭土的颗粒尺寸为0.1-0.5微米。将高岭土在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达120°。
实施例8
疏水金刚石微粉的制备方法，步骤如下：
将金刚石微粉80℃真空干燥4h，取干燥后的金刚石微粉4g，与PVDF在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度540r/min。将复合后的金刚石微粉与多余PVDF用不锈钢筛分离，得到疏水的金刚石微粉。所得疏水金刚石微粉的尺寸为0.1-1微米。将金刚石微粉在10Mpa压制成厚度为1mm的薄片，疏水改性后水接触角可达135°。
实施例9
疏水氧化铝粉的制备方法，步骤如下：
将氧化铝粉80℃真空干燥4h，取干燥后的氧化铝粉4g，与PP在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度540r/min。将复合后的氧化铝与多余PP用不锈钢筛分离，得到疏水的氧化铝粉末。所得疏水的氧化铝粉的尺寸为0.4-2微米。将氧化铝粉在10Mpa压制成厚度为1mm的薄片，疏水改性后水接触角可达122°。
实施例10
疏水高岭土的制备方法，步骤如下：
将高岭土80℃真空干燥4h，取干燥后的高岭土4g，与HDPE在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度540r/min。将复合后的氧化铝与多余HDPE用不锈钢筛分离，得到疏水的高岭土。所得疏水高岭土的颗粒尺寸为0.1-1微米。将高岭土在10Mpa压制成厚度为1mm的薄片，进行接触角测试，疏水改性前水接触角为0°，疏水改性后水接触角可达134°。
对比例1
将二氧化硅粉末80℃真空干燥4h，取干燥后的二氧化硅粉4g，与PTFE在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度500r/min。将复合后的二氧化硅粉与多余PTFE用尼龙或不锈钢筛分离。将二氧化硅粉末在10Mpa压制成厚度为1mm的薄片，进行接触角测试，球磨前水接触角为0°，与PTFE复合研磨后水接触角为0°。疏水性并未提高。
对比例2
将石墨80℃真空干燥4h，取干燥后的石墨4g，与PTFE在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度500r/min。将复合后的石墨与多余PTFE用尼龙或不锈钢筛分离。将石墨在10Mpa压制成厚度为1mm的薄片，进行接触角测试，球磨前水接触角为70.3°，与PTFE复合研磨后水接触角为38.4°。疏水性并未提高。
对比例3
将硅藻土80℃真空干燥4h，取干燥后的硅藻土4g，与PTFE在行星式球磨机上球磨复合12h，研磨球为直径8cm，质量为130g的氧化锆球，研磨速度500r/min。将复合后的硅藻土与多余PTFE用尼龙或者不锈钢筛分离。将硅藻土在10Mpa压制成厚度为1mm的薄片，进行接触角测试，球磨前水接触角为0°，与PTFE复合研磨后水接触角为7.1°，疏水性几乎没有提高。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定，对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动，这里无法对所有的实施方式予以穷举，凡是属于本发明的技术方案所引伸出的显而易见的变化或变动仍处于本发明的保护范围之列。

Claims (5)

1.一种疏水无机粉体材料的制备方法，其特征在于，包括如下步骤：
将无机粉末材料和疏水材料混合研磨；
经研磨，无机粉末材料表面均匀包覆疏水材料，将多余的疏水材料分离除去，得疏水无机粉体材料；
所述无机粉末材料选自金刚石、碳化硅、氧化铝、二氧化钛、铁、碳酸钙、高岭土中的一种；
所述疏水材料选自含氟的聚合物、聚烯烃及其衍生物中的一种或几种；
所述含氟的聚合物选自聚四氟乙烯、聚偏氟乙烯、氟化乙烯丙烯共聚物、乙烯三氟氯乙烯或氟代烷基硅烷中的一种或几种；
所述聚烯烃选自聚乙烯、聚丙烯或聚苯乙烯中的一种或几种；
所述研磨是在球磨机或研磨仪中进行，所述研磨速度为200~540rpm，研磨时间为2~30h；
所述疏水无机粉体材料的粒径尺寸为0.01~500μm；所述疏水无机粉体材料的水接触角为120°~150°。
2.根据权利要求1所述的制备方法，其特征在于，所述球磨机或研磨仪选自行星式球磨机、振动式球磨机或臼式研磨仪。
3.根据权利要求1所述的制备方法，其特征在于，分离去除多余的疏水物质的方法为用尼龙或不锈钢筛将多余疏水材料分离除去。
4.根据权利要求1所述的制备方法，其特征在于，所述疏水无机粉体材料的粒径尺寸为0.1~10μm。
5.根据权利要求4所述的制备方法，其特征在于，所述疏水无机粉体材料的粒径大小为0.1~5μm。
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