CN109603302B - 一种防污改性核桃壳滤料及其制备方法和应用 - Google Patents
一种防污改性核桃壳滤料及其制备方法和应用 Download PDFInfo
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Abstract
一种防污改性核桃壳滤料及其制备方法和应用，将核桃壳滤料用水洗涤后干燥备用；将亲水微纳米颗粒、硅烷偶联剂分散在水中，搅拌得到混合溶液；向上述混合液中加入水性树脂和助剂，搅拌混匀后获得所需的改性溶液；将洗净的核桃壳滤料加入到改性溶液中，搅拌滤出后烘干即可得所述防污改性核桃壳滤料。本发明通过表面改性，使核桃壳滤料在空气中对水和油的接触角为0°，具有超亲水性和超亲油性，同时在水下具有超疏油性，具有对油滴低粘附的特性，从而具备防污特性，优化过滤效果，提升反冲洗能力。
Description
技术领域
本发明属于含油污水处理领域，具体属于亲水水性疏油涂层领域，尤其涉及一种防污改性核桃壳滤料及其制备方法和应用。
背景技术
核桃壳滤料作为一种废弃再生资源，由于本身硬度高、耐磨损、抗压性好、化学性能稳定、吸附截污能力强且来源广泛等优点，被作为油水分离器的填充滤料，广泛应用在油田含油污水处理、工业废水处理以及民用水处理等领域，是取代石英砂滤料，提高水质，大幅度降低水处理成本的新一代滤料。虽然核桃壳滤料在过滤初始阶段吸附截污能力较强，但吸附的油污粘附在滤料表面将会使滤料粘结，使得过滤通道减少，从而导致过滤器截污能力降低、过滤效果变差、反冲洗效果变差。久而久之，核桃壳滤料结块，对过滤器内部结构件产生破坏，出现跑料的现象。
发明内容
解决的技术问题：本发明提供一种防污改性核桃壳滤料及其制备方法和应用，通过表面改性，使核桃壳滤料在空气中对水和油的接触角为0°，具有超亲水性和超亲油性，同时在水下具有超疏油性，具有对油滴低粘附的特性，从而具备防污特性，优化过滤效果，提升反冲洗能力。
技术方案：一种防污改性核桃壳滤料的制备方法，包括如下步骤：（1）将核桃壳滤料用水洗涤后干燥备用；（2）以重量计，将1-10份级配的亲水微纳米颗粒、0.5-5份硅烷偶联剂分散在20-200份水中，搅拌得到混合溶液；所述级配的亲水微纳米颗粒为SiO2、TiO2、CaO颗粒中的至少一种，由1-10μm的微米颗粒和10-500nm的纳米颗粒按质量比1:1~1:2组成；（3）向上述混合液中加入1-10份水性树脂和0.01-1份助剂，搅拌混匀后获得所需的改性溶液；（4）将洗净的核桃壳滤料加入到改性溶液中，核桃壳滤料的浓度为10wt.%-100wt.%，搅拌滤出后烘干即可得所述防污改性核桃壳滤料。
优选的，上述核桃壳滤料颗粒的粒径为1-5mm，清洗干燥流程为在室温下用清水搓洗3-5次，或用开水煮沸30min，随后于60-80℃下烘干至恒重。
优选的，上述硅烷偶联剂为KH-550、KH-560、KH-570、KH-590、KH-792中的任一种。
优选的，上述水性树脂为水性氟碳树脂或水性氟硅树脂、水性有机硅树脂和水性环氧树脂、水性聚乙烯醇树脂、水性聚氨酯树脂、水性丙烯酸树脂中的至少两种。
优选的，上述助剂为分散剂和增稠剂，分散剂:增稠剂的质量比为1:1；所述分散剂为三聚磷酸钠、六偏磷酸钠或焦磷酸钠，所述增稠剂为聚乙烯吡咯烷酮、聚乙烯醇或聚丙烯酰胺。
上述防污改性核桃壳滤料在空气中具有超亲水性和超亲油性，对水和食用油的接触角为0°，5μL水滴和油滴吸收速度小于0.1s，饱和吸水增加的重量百分比与未处理核桃壳滤料相比增加30-50%，饱和吸食用油增加的重量百分比与未处理核桃壳滤料相比增加30-50%；在水下具有超疏油性，石油、食用油的接触角大于150°，滚动角小于10°。
上述防污改性核桃壳滤料在油水混合物过滤处理中的应用。
有益效果：（1）本发明所制备的改性核桃壳滤料在空气中对水的接触角为0°，具有超亲水性，微纳米颗粒级配形成粗糙的多孔结构，增大了核桃壳滤料的吸水能力，同时在水下具有超疏油性，具有对石油等油滴低粘附的特性，不易被油污粘附，具备一定的防污性；
（2）本发明所制备的改性核桃壳滤料可应用于油水混合物的过滤处理，高温环境下亦有效，耐高温可达150℃；
（3）本发明所使用的主要原材料为水性树脂和亲水颗粒，廉价易得，无需使用有机溶剂，无需固化剂，无毒副作用，不会产生二次污染，环境友好；
（4）助剂的加入，不仅有效改善了颗粒的分散效果，放置大颗粒的沉降，同时提高了涂层的强度；
（5）本发明方法所用设备及工艺简单，操作简便易于实现，且能耗小，成本低，重复性好，可大范围大规模生产。
附图说明
图1为实施例1所得改性核桃壳在空气中超亲水的过程图。
图2为实施例1所得改性核桃壳的饱和吸附能力，其中每组左侧数据柱为饱和吸水能力，右侧数据柱为饱和吸油能力。
图3为实施例1所得改性核桃壳水下油滴的接触角测示图。
图4为实施例2所得改性核桃壳表面形貌扫描电镜图。
图5为实施例3改性前后核桃壳滤料进行油田污水过滤处理图，其中a为油田含油污水处理装置，b为过滤前的油田含油污水，c为未改性的核桃壳滤料的过滤效果，d为改性核桃壳滤料的过滤效果。
具体实施方式
实施例1
（1）室温下，将核桃壳滤料用清水搓洗3次，去除表面灰尘及杂质，干燥备用；（2）分别将0.5g粒径为10-40nm和1μm的SiO2纳米颗粒、0.5gKH-550分散在40g水中，搅拌其形成均匀的混合溶液；（3）向上述混合液中分别加入0.5g水性氟碳树脂、0.5g水性环氧树脂和0.5mg三聚磷酸、0.5mg聚乙烯醇，混匀后获得所需的改性溶液；（4）将20g洗净的核桃壳滤料加入到所得的改性溶液中，在800r/min的转速下经机械搅拌2h后置于60℃下烘干8h即可得所述改性核桃壳滤料。图1为改性核桃壳在空气中超亲水的过程，从图中可以看出，水滴刚一接触到核桃壳表面就立即铺展开，并在重力和毛细吸附力的作用下快速渗透到空隙内部，展现出了很好的超亲水性能。图2为未改性核桃壳和改性核桃壳饱和吸水能力和吸油能力，经测算，饱和吸水增加的重量百分比与未处理核桃壳滤料相比增加30-50%，饱和吸食用油增加的重量百分比与未处理核桃壳滤料相比增加30-50%。图3为制得的改性核桃壳水下油滴的接触角测量图，测试液滴为液态石油，改性核桃壳粒在水下可有效包裹石油液滴，展现出很好的水下疏油性，且油滴小于10°即可轻易滚动，没有粘附现象产生。
实施例2
（1）室温下，将核桃壳滤料用清水搓洗5次，去除表面灰尘及杂质，干燥备用；（2）分别将1g粒径为10-40nm和1μm的SiO2纳米颗粒、1gKH-570分散在60g水中，搅拌其形成均匀的混合溶液；（3）向上述混合液中加入1g水性丙烯酸树脂、1g水性聚乙烯醇树脂和0.5mg三聚磷酸、0.5mg聚丙烯酰胺，混匀后获得所需的改性溶液；（4）将30g洗净的核桃壳滤料加入到所得的改性溶液中，600r/min的转速下经机械搅拌2h后置于80℃下烘干5h，即可得所述改性核桃壳滤料。图4为改性核桃壳表面形貌扫描电镜图。从图中可以看出在表面包覆有树脂和SiO2颗粒杂化的微米级聚合物包覆层，同时在包覆层上多层次均匀分布着微米尺度的球形突起，在微米尺度突起之上和微米突起间隔里均匀分布着纳米尺度的球形乳突，形成了微米-纳米粗糙的多孔结构，为空气中超亲水和水下疏油提供了必要的条件，同时增强了滤料的吸水能力。
实施例3
（1）室温下，将核桃壳滤料用清水搓洗5次，去除表面灰尘及杂质，干燥备用；（2）分别将1g粒径为100-200nm和1μm的TiO2纳米颗粒、2gKH-570分散在60g水中，搅拌其形成均匀的混合溶液；（3）向上述混合液中加入1g水性聚氨酯树脂、1g水性氟硅树脂和0.5mg焦磷酸钠、0.5mg聚丙烯酰胺，混匀后获得所需的改性溶液；（4）将40g洗净的核桃壳滤料加入到所得的改性溶液中，600r/min的转速下搅拌2h后置于60℃下烘干5h，即可得所述改性核桃壳滤料。油田含油污水处理装置如图5（a）所示，其中玻璃管内径为3cm，滤料的填充高度为5cm，利用该装置过滤含油污水0.5L，污水含油量为213mg/L，过滤完毕后测定滤液含油量，且滤料使用0.5L去离子水浸泡搅拌，测定反洗水含油量。对比图5（c）和图5（d）可以看出，油田含油污水经过改性核桃壳过滤处理后，滤液的含油量为34mg/L，其含油量显著降低，作为对比，未改性核桃壳滤料过滤处理后滤液的含油量为90mg/L，改性核桃壳滤料的过滤效果（图5（d））明显优于未改性的核桃壳滤料的过滤效果（图5（c））。过滤完毕后滤料使用0.5L去离子水浸泡搅拌，测定反洗水含油量，未改性核桃壳滤料所得反洗水含油量为97 mg/L ，而改性核桃壳滤料所得反洗水含油量为158 mg/L ，滤料经过改性后，可以用去离子水从滤料表面反洗下更多的油滴，说明改性核桃壳滤料具备一定的防污性。
实施例4
（1）室温下，将核桃壳滤料用清水搓洗5次，去除表面灰尘及杂质，干燥备用；（2）分别将0.5g粒径为10-40nm和1μm的SiO2纳米颗粒、1gKH-590分散在40g水中，搅拌其形成均匀的混合溶液；（3）向上述混合液中加入水性有机硅树脂和水性环氧树脂各1g和0.5mg焦磷酸钠、0.5mg聚乙烯醇，混匀后获得所需的改性溶液；（4）将40g洗净的核桃壳滤料加入到所得的改性溶液中，500r/min的转速下搅拌2h后置于70℃下烘干5h，即可得所述改性核桃壳滤料。将所得改性核桃壳滤料置于150℃高温环境下12h，随后用于油田污水过滤处理，油田含油污水处理装置如图5（a），处理结果为：含油污水过滤前含油量为232mg/L，过滤后滤液含油量为31mg/L，滤完毕后滤料使用0.5L去离子水浸泡搅拌，测定反洗水含油量，所得反洗水含油量为161mg/L。可以看出，本发明所制备的改性核桃壳滤料可应用于油水混合物的过滤处理，高温环境下亦有效，耐高温可达150℃。
Claims (2)
1.一种防污改性核桃壳滤料的制备方法，其特征在于包括如下步骤：（1）将核桃壳滤料用水洗涤后干燥备用，所述核桃壳滤料颗粒的粒径为1-5mm，清洗干燥流程为在室温下用清水搓洗3-5次，或用开水煮沸30min，随后于60-80℃下烘干至恒重；（2）以重量计，将1-10份级配的亲水微纳米颗粒、0.5-5份硅烷偶联剂分散在20-200份水中，所述硅烷偶联剂为KH-550、KH-560、KH-570、KH-590、KH-792中的任一种，搅拌得到混合溶液；所述级配的亲水微纳米颗粒为SiO2、TiO2、CaO颗粒中的至少一种，由1-10μm的微米颗粒和10-500nm的纳米颗粒按质量比1:1~1:2组成；（3）向上述混合液中加入1-10份水性树脂和0.01-1份助剂，所述水性树脂为水性氟碳树脂、水性氟硅树脂、水性有机硅树脂、水性环氧树脂、水性聚乙烯醇树脂、水性聚氨酯树脂、水性丙烯酸树脂中的至少两种；搅拌混匀后获得所需的改性溶液；所述助剂为分散剂和增稠剂，分散剂:增稠剂的质量比为1:1；所述分散剂为三聚磷酸钠、六偏磷酸钠或焦磷酸钠，所述增稠剂为聚乙烯吡咯烷酮、聚乙烯醇或聚丙烯酰胺；（4）将洗净的核桃壳滤料加入到改性溶液中，核桃壳滤料的浓度为10wt.%-100wt.%，搅拌滤出后烘干即可得所述防污改性核桃壳滤料，所述防污改性核桃壳滤料在空气中具有超亲水性和超亲油性，对水和食用油的接触角为0°，5μL水滴和油滴吸收速度小于0.1s，饱和吸水增加的重量百分比与未处理核桃壳滤料相比增加30-50%，饱和吸食用油增加的重量百分比与未处理核桃壳滤料相比增加30-50%；在水下具有超疏油性，石油、食用油的接触角大于150°，滚动角小于10°。
2.权利要求1所述防污改性核桃壳滤料在油水混合物过滤处理中的应用。
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