CN107162565B - 一种高强度地聚合物空心微球及其制备方法 - Google Patents

一种高强度地聚合物空心微球及其制备方法 Download PDF

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CN107162565B
CN107162565B CN201710473085.9A CN201710473085A CN107162565B CN 107162565 B CN107162565 B CN 107162565B CN 201710473085 A CN201710473085 A CN 201710473085A CN 107162565 B CN107162565 B CN 107162565B
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步玉环
马睿
柳华杰
郭胜来
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China University of Petroleum East China
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Abstract

本发明公开了一种高强度地聚合物空心微球及其制备方法，将氢氧化钠（NaOH）、硅酸钠（Na2SiO3·9H2O）及成球助剂溶解于水中形成溶液A，将活性粉末加入溶液A中搅拌混合均匀后形成浆体B，将浆体加入油相中搅拌分散成球，搅拌一定时间后，过滤得到地聚合物微球Ⅰ，将微球洗净后，进行高温煅烧后得到高强度中空地聚合微球Ⅱ。和传统制备空心微球的方法相比，该方法工艺简单，原材料价格便宜来源广泛，成球率高，生产成本低，空心微球强度高，可以大规模生产。

Description

一种高强度地聚合物空心微球及其制备方法
技术领域
本发明属于微球材料技术领域，具体涉及一种高强度地聚合物空心微球及制备方法。
背景技术
空心微球是一种中空微小球形材料。它是一种性能独特而稳定的中空颗粒，由于其特殊的形态及中空，被广泛应用于石油固井，建筑载体，封装材料，吸波材料及轻质高强混凝土外加材料等领域。
目前，空心微球主要有空心玻璃微珠，空心陶瓷微珠，ZnO掺杂TiO2复合空心球（CN101905153A）及轻质铝锆空心微球（CN 103803952 A）。目前除了空心玻璃微珠生产工艺较为成熟，其他空心微球生产工艺都较为复杂，微球生产过程中很容易引入杂质。此外，虽然空心玻璃微珠生产工艺较为成熟，但是空心玻璃微球的抗压强度低。
发明内容
本发明的目的在于为了解决上述现有技术中存在问题之一，提供一种高强度地聚合物空心微球及其制备方法。
本发明解决其技术问题所采用的技术方案是：
本发明一方面提供一种高强度地聚合物多孔微球制备方法，将氢氧化钠（NaOH）、硅酸钠（Na2SiO3·9H2O）及成球助剂溶解于水中形成溶液A，将活性粉末加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入油相中搅拌分散成球，搅拌后，过滤得到地聚合物微球Ⅰ，将微球洗净后，进行高温煅烧后得到高强度多孔地聚合微球Ⅱ；其中所述氢氧化钠（NaOH）、硅酸钠（Na2SiO3·9H2O）和成球助剂的质量百分比为(10~40%):(20~60%):(20~60%)，所述水和活性粉末质量比为1：2~1，所述浆体B占所述油相分散介质体积的5%~50%；所述高温煅烧温度800-1500℃，煅烧时间1-8h。
优选的，所述氢氧化钠（NaOH）、硅酸钠（Na2SiO3·9H2O）和成球助剂的质量百分比为(12~20%):(40~60%):(30~50%)，所述水和活性粉末质量比为1：1.5~1，所述浆体B占所述油相分散介质体积的10%~40%。
优选的，所述高温煅烧温度850-1200℃，煅烧时间1-2h。
优选的，所述氢氧化钠（NaOH）、硅酸钠（Na2SiO3·9H2O）、成球助剂和水的质量份数比为(12~20):(40~60):(30~50):100。
优选的，所述成球助剂为钠盐和钾盐。
优选的，所述钠盐包括碳酸钠、氯化钠、硝酸钠、硫酸钠中的一种或几种。
优选的，所述钾盐包括氯化钾、碳酸钾、硫酸钾中的一种或者几种。
优选的，活性粉末包括粉煤灰、偏高岭土和矿渣中的一种或者几种。
优选的，所述活性粉末目数为500~1000目。
优选的，所述油相为玉米油或大豆油或花生油或煤油或蓖麻油或菜籽油。
优选的，所述油相温度为50-90℃。
优选的，所述将浆体B分散到油相中的搅拌速度为400-1000r/min，搅拌时间0.5-3h。
优选的，所述高温煅烧温度800-1500℃，煅烧时间1-8h。
优选的，所述采用本发明制备方法所得的地聚合物空心微球的粒径范围为50~300μm，壁厚10-50μm，密度0.5-0.8g/cm3，抗压强度≥20MPa。
本发明还提供了由上述的高强度地聚合物空心微球制备方法制备的高强度地聚合物多孔微球。
本发明的有益效果是：和传统制备空心微球的方法相比，该方法工艺简单，原材料价格便宜来源广泛，成球率高，生产成本低，空心微球强度高，可以大规模生产。
附图说明
本发明的上述和或附加的方面和优点从结合下面附图对实施例的描述中将变得明显和容易理解，其中：
图1是本发明地聚合物空心微球的显微图，粒径范围50-100 μm；
图2为选取有破裂的微球，表明其为空心。
从图中可以明显看出微球以及微球内部的空腔。
具体实施方式
下面通过参考附图描述的实施例是示例性的，旨在用于解释本发明，而不能理解为对本发明的限制。
实施例1 高强度地聚合物多孔微球及其制备方法
氢氧化钠（NaOH）1.5g 、硅酸钠（Na2SiO3·9H2O）5g及氯化钠（NaCl）3g溶解于10g水中形成溶液A，将10g偏高岭土加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入玉米油中，浆体B占玉米油体积的10%，搅拌使浆体B分散成球，搅拌速度600 r/min，搅拌0.5h，玉米油温度55℃，过滤得到地聚合物微球Ⅰ，将微球洗净后，850℃高温煅烧2h后得到高强度多孔地聚合微球（M 1），微球粒径范围50-100 μm，微球抗压强度23MPa，壁厚10μm，密度0.60 g/cm3。
实施例2高强度地聚合物多孔微球及其制备方法
氢氧化钠（NaOH）2g 、硅酸钠（Na2SiO3·9H2O）6g及氯化钠4.5g溶解于10g水中形成溶液A，将15g偏高岭土加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入大豆油中，浆体B占大豆油体积的15%，搅拌使浆体B分散成球，搅拌速度400 r/min，搅拌1.5h，玉米油温度65℃，过滤得到地聚合物微球Ⅰ，将微球洗净后，1000℃高温煅烧1.5h后得到高强度多孔地聚合微球（M 2），微球粒径范围250-300 μm，微球抗压强度27MPa，壁厚45μm，密度0.65 g/cm3。
实施例3高强度地聚合物多孔微球及其制备方法
氢氧化钠（NaOH）1.2g 、硅酸钠（Na2SiO3·9H2O）4g及氯化钠5g溶解于10g水中形成溶液A，将12g偏高岭土加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入玉米油中，浆体B占玉米油体积的40%，搅拌使浆体B分散成球，搅拌速度500 r/min，搅拌2.0 h，玉米油温度75℃，过滤得到地聚合物微球Ⅰ，将微球洗净后，1200℃高温煅烧1h后得到高强度多孔地聚合微球（M 3），微球粒径范围250-300 μm，微球抗压强度24MPa，壁厚30μm，密度0.70 g/cm3。
实施例4高强度地聚合物多孔微球及其制备方法
氢氧化钠（NaOH）1.4g 、硅酸钠（Na2SiO3·9H2O）6g及氯化钠4g溶解于10g水中形成溶液A，将12g偏高岭土加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入玉米油中，浆体B占玉米油体积的30%，搅拌使浆体B分散成球，搅拌速度700 r/min，搅拌0.5 h，玉米油温度85℃，过滤得到地聚合物微球Ⅰ，将微球洗净后，900℃高温煅烧2h后得到高强度多孔地聚合微球（M 4），微球粒径范围100-200 μm，微球抗压强度26 MPa，壁厚25μm，密度0.65 g/cm3。
尽管已经示出和描述了本发明的实施例，本领域的普通技术人员可以理解：在不脱离本发明的原理和宗旨的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由权利要求及其等同物限定。

Claims (8)

1.一种高强度地聚合物空心微球制备方法，其特征在于，将氢氧化钠、硅酸钠及成球助剂溶解于水中形成溶液A，将活性粉末加入溶液A中搅拌混合均匀后形成浆体B，将浆体B加入油相中搅拌分散成球，搅拌后，过滤得到地聚合物微球Ⅰ，将微球洗净后，进行高温煅烧后得到高强度多孔地聚合微球Ⅱ；其中所述氢氧化钠、硅酸钠和成球助剂的质量百分比为(10～40％):(20～60％):(20～60％)，所述水和活性粉末质量比为1：2～1，所述浆体B占所述油相分散介质体积的5％～50％；所述高温煅烧温度800-1500℃，煅烧时间1-8h；所述成球助剂为钠盐和钾盐；所述钠盐包括碳酸钠、氯化钠、硝酸钠、硫酸钠中的一种或几种；所述钾盐包括氯化钾、碳酸钾、硫酸钾中的一种或者几种。
2.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，所述氢氧化钠、硅酸钠和成球助剂的质量百分比为(12～20％):(40～60％):(30～50％)，所述水和活性粉末质量比为1：1.5～1，所述浆体B占所述油相分散介质体积的10％～40％。
3.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，所述高温煅烧温度850-1200℃，煅烧时间1-2h。
4.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，活性粉末包括粉煤灰、偏高岭土和矿渣中的一种或者几种，所述活性粉末目数为500～1000目。
5.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，所述油相为玉米油或大豆油或花生油或煤油或蓖麻油或菜籽油。
6.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，所述油相温度为50-90℃。
7.根据权利要求1所述的高强度地聚合物空心微球制备方法，其特征在于，所述将浆体B分散到油相中的搅拌速度为400-1000r/min，搅拌时间0.5-3h。
8.权利要求1-7任一项所述的高强度地聚合物空心微球制备方法制备的高强度地聚合物空心微球。
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