CN115282944B - 硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球及其制备方法 - Google Patents
硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法。该吸附剂以废弃鲍鱼壳为主要原料,通过负载纳米Fe3O4,硬脂酸改性等步骤,制备出硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球,所制备的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球有望成为一种绿色高效吸附剂应用于海洋溢油的处理中。本发明制备工艺简单,材料廉价易获取,在有效减轻环境负担的同时,也发挥了废弃鲍鱼壳的高附加值作用,实现了生态效益和经济价值的双向共赢。
Description
技术领域
本发明属于无机材料制备技术领域,具体涉及一种成本低廉、绿色环保、可以有效吸附海洋溢油的一种硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法。
背景技术
随着海上石油开采和运输的发展以及对工业原材料需求的激增,工业废水的排放和近海油田原油泄漏的频繁发生严重威胁着海洋生态环境。现阶段已有包括原位燃烧,重力分离,生物修复等在内的海洋漏油处理技术,然而这些方法昂贵,效率低,容易对环境造成二次污染。因此,开发成本低廉、工艺简单、绿色环保的高效吸附剂以处理海洋溢油问题显得愈发重要。近年来,具有大表面积,高孔隙率,高吸附性能和特殊润湿性的三维多孔结构吸附剂受到广泛关注。但这些材料仍然具有制造工艺复杂,可回收性差,经济效益低的缺点。
我国是水产大国,海洋贝类资源丰富,但随着贝类养殖加工业的迅速发展,废弃贝壳的大量堆积逐渐造成环境污染问题。由于对贝壳废弃物的利用技术有限,传统的处理方式如焚烧、填埋等,不仅浪费土地资源,而且易对周围环境造成污染,不利于我国沿海地区生态文明建设和可持续发展。
硬脂酸是一种不溶于水的脂肪酸,具有良好的疏水性,价格低廉。Fe3O4磁性纳米粒是一种具有稳定磁导率和超顺磁性的尖晶石铁氧体,Fe3O4磁性纳米粒的制备过程简单便宜。
本发明从解决废弃鲍鱼壳污染的角度出发,以废弃鲍鱼壳为主要原料,通过负载纳米Fe3O4,硬脂酸改性等步骤,制备出硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球,有望作为一种绿色高效吸附剂应用于海洋溢油的处理中。该吸附剂呈介孔微球结构,加入硬脂酸对其表面改性,可以制备成疏水性强、能漂浮于海面的海洋油污吸附材料。其次,Fe3O4磁性纳米粒的加入赋予介孔微球磁响应性,便于回收利用,避免造成二次污染。。
发明内容
本发明目的在于提供一种硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,从解决废弃鲍鱼壳污染的角度出发,以废弃鲍鱼壳为主要原料,通过负载纳米Fe3O4,硬脂酸改性等步骤,制备出硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球,有望作为一种绿色高效吸附剂应用于海洋溢油的处理中。
为实现上述目的,本发明采用如下技术方案:
一种硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,包括以下步骤:
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取一定量鲍鱼壳粉于,加入醋酸溶液对鲍鱼壳粉进行溶解,持续搅拌至无气泡产生;
(3)对步骤(2)中反应溶液离心取上清液,加入超纯水定容,而后在搅拌中缓慢滴加配制好的磷酸溶液;
(4)待磷酸溶液滴加结束,向溶液中添加柠檬酸钠、尿素并持续搅拌一定时间得到澄清前驱体反应液;
(5)向前驱体反应液中加入一定体积已超声分散均匀的纳米Fe3O4分散液,并置于恒温水浴锅中,搅拌数小时;
(6)搅拌完成后,倒入反应釜中并将反应釜置于鼓风干燥箱中,在一定温度下反应数小时;
(7)反应结束后,自然冷却至室温,离心水洗三次,乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球;
(8)称取一定量干燥的鲍鱼壳磁性多孔羟基磷灰石微球粉末,加入适量蒸馏水,使鲍鱼壳磁性多孔羟基磷灰石微球粉末完全润湿后将其放入恒温水浴锅中,使用电动搅拌机,边搅拌边加入一定量硬脂酸粉末,继续搅拌数小时后,倒入抽滤漏斗,利用真空泵进行抽滤,然后置于鼓风干燥箱中烘干,得到所述硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
各步骤的工艺参数如下:
进一步的,步骤(2)中鲍鱼壳粉用量为0.5g,醋酸溶液用量为20mL,浓度为10vol.%。
进一步的,对步骤(3)中离心转速为8000rpm,离心时间为5min;加入超纯水定容至50mL;磷酸溶液的浓度为0.06M,用量为50mL,滴加速度为1 mL /min。
进一步的,步骤(4)中柠檬酸钠用量为0.2358g、尿素用量为6g。
进一步的,步骤(5)纳米Fe3O4分散液用量为5mL,浓度为0.5g/mL。
进一步的,步骤(6)中反应温度为90℃,反应时间为 40h。
进一步的,步骤(8)中鲍鱼壳磁性多孔羟基磷灰石微球粉末用量为0.5g, 硬脂酸粉末用量为0.5g。
如上所述方法制得的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
应用:所述的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球在海洋溢油吸附中的应用。
本发明的显著优点在于:
(1)本发明原材料廉价易获取,制备工艺简单,在减轻鲍鱼壳废弃物造成的环境负担的同时,也开发了废弃鲍鱼壳的高附加价值,具有良好的生态效益和经济价值。
(2)本发明从解决废弃贝壳污染与海洋溢油问题的角度出发,以废弃鲍鱼壳为原料,通过负载纳米Fe3O4,硬脂酸改性等步骤,制备出硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球,微球呈介孔结构,粒径约5μm,孔径约8nm,比表面积高达152.33g/m2,可以作为一种绿色高效吸附剂应用于海洋溢油的处理中。
(3)本发明以废弃鲍鱼壳为原料,通过负载纳米Fe3O4赋予介孔羟基磷灰石微球磁响应性,便于回收和重复利用,避免造成二次污染;通过硬脂酸改性,赋予磁性介孔羟基磷灰石微球优异的疏水性,使其能够漂浮于海面,充分吸附海洋油污。
附图说明
图1、图2为实施例4制备硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球SEM图。从图1中可看出,微球呈花形介孔状,比表面积大、孔径分布均匀,这可以作为一种潜在的绿色高效吸附剂并应用于海洋溢油处理中。
具体实施方式
为了使本发明所述的内容更加便于理解,下面结合具体实施方式对本发明所述的技术方案做进一步的说明,但是下述的实例仅仅是本发明其中的例子而已,并不代表本发明所限定的权利保护范围,本发明的权利保护范围以权利要求书为准。
实施例1(未进行硬脂酸改性)
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取0.5g鲍鱼壳粉末于烧杯中,加入20mL 配制的 10 vol.%醋酸溶液对鲍鱼壳粉进行溶解5h,持续搅拌至无气泡产生;
(3)反应溶液离心(8000r,5min)取上清液,加入超纯水定容至 50mL,而后在搅拌中缓慢滴加配制好的 0.06M 磷酸溶液(50mL,滴加速度1 mL /min);
(4)向溶液中添加0.2358g柠檬酸钠、6g尿素并持续搅拌 0.5h 得到澄清前驱体反应液;
(5)向前驱体反应液中加入1 mL已超声分散均匀的纳米Fe3O4分散液(浓度为0.5g/mL),并将混合溶液置于恒温水浴锅中,利用电动搅拌机反应2h;
(6)搅拌完成后,将混合前驱体反应液倒入反应釜中并将反应釜置于鼓风干燥箱中,90℃水热反应 40h;
(7)反应结束后,自然冷却至室温,离心水洗三次(9000r,5min),乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球。
实施例2
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取0.5g鲍鱼壳粉末于烧杯中,加入20mL 配制的 10 vol.%醋酸溶液对鲍鱼壳粉进行溶解5h,持续搅拌至无气泡产生;
(3)反应溶液离心(8000r,5min)取上清液,加入超纯水定容至 50mL,而后在搅拌中缓慢滴加配制好的 0.06M 磷酸溶液(50mL,滴加速度1 mL /min);
(4)向溶液中添加0.2358g柠檬酸钠、6g尿素并持续搅拌 0.5h 得到澄清前驱体反应液;
(5)向前驱体反应液中加入1 mL已超声分散均匀的纳米Fe3O4分散液(浓度为0.5g/mL),并将混合溶液置于恒温水浴锅中,利用电动搅拌机反应2h;
(6)搅拌完成后,将混合前驱体反应液倒入反应釜中并将反应釜置于鼓风干燥箱中,90℃水热反应 40h;
(7)反应结束后,自然冷却至室温,离心水洗三次(9000r,5min),乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球;
(8)称取0.5g干燥的鲍鱼壳磁性多孔羟基磷灰石微球粉末于250mL烧杯中,加入适量蒸馏水,使鲍鱼壳磁性多孔羟基磷灰石微球粉末完全润湿后将其放入恒温水浴锅中,使用电动搅拌机,边搅拌边加入0.5g硬脂酸粉末,继续搅拌反应2h后,将混合液倒入抽滤漏斗,利用真空泵进行抽滤,然后置于鼓风干燥箱中烘干,得到硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
实施例3
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取0.5g鲍鱼壳粉末于烧杯中,加入20mL 配制的 10 vol.%醋酸溶液对鲍鱼壳粉进行溶解5h,持续搅拌至无气泡产生;
(3)反应溶液离心(8000r,5min)取上清液,加入超纯水定容至 50mL,而后在搅拌中缓慢滴加配制好的 0.06M 磷酸溶液(50mL,滴加速度1 mL /min);
(4)向溶液中添加0.2358g柠檬酸钠、6g尿素并持续搅拌 0.5h 得到澄清前驱体反应液;
(5)向前驱体反应液中加入3 mL已超声分散均匀的纳米Fe3O4分散液(浓度为0.5g/mL),并将混合溶液置于恒温水浴锅中,利用电动搅拌机反应2h;
(6)搅拌完成后,将混合前驱体反应液倒入反应釜中并将反应釜置于鼓风干燥箱中,90℃水热反应 40h;
(7)反应结束后,自然冷却至室温,离心水洗三次(9000r,5min),乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球;
(8)称取0.5g干燥的鲍鱼壳磁性多孔羟基磷灰石微球粉末于250mL烧杯中,加入适量蒸馏水,使鲍鱼壳磁性多孔羟基磷灰石微球粉末完全润湿后将其放入恒温水浴锅中,使用电动搅拌机,边搅拌边加入0.5g硬脂酸粉末,继续搅拌反应2h后,将混合液倒入抽滤漏斗,利用真空泵进行抽滤,然后置于鼓风干燥箱中烘干,得到硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
实施例4
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取0.5g鲍鱼壳粉末于烧杯中,加入20mL 配制的 10 vol.%醋酸溶液对鲍鱼壳粉进行溶解5h,持续搅拌至无气泡产生;
(3)反应溶液离心(8000r,5min)取上清液,加入超纯水定容至 50mL,而后在搅拌中缓慢滴加配制好的 0.06M 磷酸溶液(50mL,滴加速度1 mL /min);
(4)向溶液中添加0.2358g柠檬酸钠、6g尿素并持续搅拌 0.5h 得到澄清前驱体反应液;
(5)向前驱体反应液中加入5 mL已超声分散均匀的纳米Fe3O4分散液(浓度为0.5g/mL),并将混合溶液置于恒温水浴锅中,利用电动搅拌机反应2h;
(6)搅拌完成后,将混合前驱体反应液倒入反应釜中并将反应釜置于鼓风干燥箱中,90℃水热反应 40h;
(7)反应结束后,自然冷却至室温,离心水洗三次(9000r,5min),乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球;
(8)称取0.5g干燥的鲍鱼壳磁性多孔羟基磷灰石微球粉末于250mL烧杯中,加入适量蒸馏水,使鲍鱼壳磁性多孔羟基磷灰石微球粉末完全润湿后将其放入恒温水浴锅中,使用电动搅拌机,边搅拌边加入0.5g硬脂酸粉末,继续搅拌反应2h后,将混合液倒入抽滤漏斗,利用真空泵进行抽滤,然后置于鼓风干燥箱中烘干,得到硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (8)
1.一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:包含以下步骤:
(1)将鲍鱼壳表面刷洗干净后置于阴凉通风处自然干燥,而后使用粉碎机对鲍鱼壳进行粉碎,并使用 200 目筛网进行过筛处理,得到颗粒细小均匀的鲍鱼壳粉;
(2)称取一定量鲍鱼壳粉,加入醋酸溶液对鲍鱼壳粉进行溶解,持续搅拌至无气泡产生;
(3)对步骤(2)中反应溶液离心取上清液,加入超纯水定容,而后在搅拌中缓慢滴加配制好的磷酸溶液;
(4)待磷酸溶液滴加结束,向溶液中添加柠檬酸钠、尿素并持续搅拌一定时间
得到澄清前驱体反应液;
(5)向前驱体反应液中加入一定体积已超声分散均匀的纳米Fe3O4分散液,并置于恒温水浴锅中,搅拌数小时;
(6)搅拌完成后,倒入反应釜中并将反应釜置于鼓风干燥箱中,在一定温度下反应数小时;
(7)反应结束后,自然冷却至室温,离心水洗三次,乙醇洗涤一次,60℃干燥,得到鲍鱼壳磁性多孔羟基磷灰石微球;
(8)称取一定量干燥的鲍鱼壳磁性多孔羟基磷灰石微球粉末,加入适量蒸馏水,使鲍鱼壳磁性多孔羟基磷灰石微球粉末完全润湿后将其放入恒温水浴锅中,边搅拌边加入一定量硬脂酸粉末,继续搅拌数小时后,倒入抽滤漏斗,利用真空泵进行抽滤,然后置于鼓风干燥箱中烘干,得到所述硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
2.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:步骤(2)中鲍鱼壳粉用量为0.5g,醋酸溶液用量为20mL,浓度为10 vol.%。
3.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:对步骤(3)中离心转速为8000rpm,离心时间为5min;加入超纯水定容至 50mL;磷酸溶液的浓度为0.06M,用量为50mL,滴加速度为1 mL /min。
4.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:步骤(4)中柠檬酸钠用量为0.2358g、尿素用量为6g。
5.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:步骤(5)纳米Fe3O4分散液用量为5mL,浓度为0.5g/mL。
6.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:步骤(6)中反应温度为90℃,反应时间为 40h。
7.根据权利要求1所述的一种用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球的制备方法,其特征在于:步骤(8)中鲍鱼壳磁性多孔羟基磷灰石微球粉末用量为0.5g, 硬脂酸粉末用量为0.5g。
8.如权利要求1-7任一项所述方法制得的用于海洋溢油处理的硬脂酸改性鲍鱼壳磁性多孔羟基磷灰石微球。
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