CN105964231B - 一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法 - Google Patents
一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法 Download PDFInfo
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Abstract
一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,本发明属于材料表面改性、吸附新材料技术领域。本发明要解决现有超疏水/超亲油与磁性油吸附材料,大多通过水热合成法方法制备,存在设备要求高耐温耐压的钢材,耐腐蚀的内衬、温压控制严格、成本高;安全性差,加热时密闭反应釜中流体体积膨胀,能产生极大的压强,存在安全隐患,高温会破坏原料基材的内部结构,影响最终所制备的吸附剂吸附效果的问题。方法:一、木粉的预处理;二、制备磁性木粉;三、制备改性液;四、磁性木粉改性,即完成一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法。本发明用于一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法。
Description
技术领域
本发明属于材料表面改性、吸附新材料技术领域。
背景技术
在环境污染中,油污染是一直是关系人民生活和可持续发展的重要课题。其中,涉及到油处理的问题主要为溢油的处理与含油废水的处理,而吸附法处理是目前最有效的方法。为避免对环境的二次污染,且高效可回收的分离油污,生物质材料由于廉价易得,可降解,易处理等特点逐渐成为材料研究的热点。
目前,已开发的吸油材料主要分为两种类型,即:无机吸油材料和有机吸油材料。由于天然有机吸油材料吸收液体后会下沉、疏水性较差、不易回收且难以处理油水乳液的缺点,限制了在油水体系中的应用。以木粉为原料合成磁性可回收超疏水吸附剂,是一类新兴的石油吸附材料,特别适用于水面浮油回收,同时还具有吸油种类多,吸油不吸水的优点。目前已知的同时具备超疏水/超亲油与磁性油吸附材料,大多通过水热合成法方法制备,而此类方法存在以下问题:首先,设备要求高耐温耐压的钢材,耐腐蚀的内衬、温压控制严格、成本高;其次,安全性差,加热时密闭反应釜中流体体积膨胀,能产生极大的压强,存在极大的安全隐患;最后,高温会破坏原料基材的内部结构,从而影响最终所制备的吸附剂吸附效果的问题。
发明内容
本发明要解决现有超疏水/超亲油与磁性油吸附材料,大多通过水热合成法方法制备,存在设备要求高耐温耐压的钢材,耐腐蚀的内衬、温压控制严格、成本高;安全性差,加热时密闭反应釜中流体体积膨胀,能产生极大的压强,存在极大的安全隐患,高温会破坏原料基材的内部结构,从而影响最终所制备的吸附剂吸附效果的问题,而提供一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法。
一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,具体是按照以下步骤进行的:
一、木粉的预处理:
将木粉依次过60目和100目筛子,得到粒径均匀的木粉,将粒径均匀的木粉浸入到过氧化氢、氢氧化钠和蒸馏水的混合溶液中,在室温下搅拌10h~15h,得到反应体系,用质量百分数为30%~37%的盐酸调节反应体系pH至中性,用蒸馏水洗涤反应后的木粉2次~4次,然后将洗涤后的木粉置于温度为40℃~70℃的烘箱下干燥至质量恒定,得到干燥后的木粉;
所述的氢氧化钠与过氧化氢的质量比为1:(1~10);所述的氢氧化钠与蒸馏水的质量比为1:(10~200);
二、制备磁性木粉:
将单组份聚氨酯与正己烷混合并磁力搅拌均匀,然后将四氧化三铁纳米颗粒与干燥后的木粉加入到单组份聚氨酯与正己烷的混合溶液中,并在转速为400r/min~800r/min的条件下,搅拌反应10h~20h,得到混合物,将混合物静置并弃上层清液,然后向弃上层清液后的混合物中加入丙三醇水溶液,得到磁性木粉复合物,最后将磁性木粉复合物过滤取出,并用无水乙醇洗涤,然后在温度为50℃~60℃的条件下干燥至恒重,得到磁性木粉;
所述的丙三醇水溶液中丙三醇与水的体积比为1:(0.1~2);所述的单组份聚氨酯的质量与正己烷的体积比为1g:(10~100)mL;所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:(0.1~1);所述的单组份聚氨酯与干燥后的木粉的质量比为1:(0.1~1);所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:(100~200)mL;
三、制备改性液:
将正己烷与十八烷基三氯硅烷混合均匀,得到改性液;
所述的十八烷基三氯硅烷与正己烷的体积比为1:(10~100);
四、磁性木粉改性:
将磁性木粉加入到改性液中,在室温搅拌条件下,反应4h~8h,反应后过滤并用蒸馏水和无水乙醇洗涤,然后在温度为40℃~60℃的烘箱中干燥,得到磁性可回收超疏水超亲油吸附剂;
所述的磁性木粉的质量与改性液的体积比为1g:(10~100)mL。
本发明的有益效果是:
1、使用木粉作为原材料,是一种天然可降解的生物质材料,具有储量丰富,廉价易得,且环境友好,易于回收等特点。
2、本发明制备得到的磁性可回收超疏水超亲油吸附剂,与水的接触角为150°~152°,与油的接触角为0°,是一种新型的吸油剂,具备高效的油水分离性能。对汽油的吸油容量为10g/g~20g/g,对柴油的吸油容量为10g/g~20g/g,对四氯化碳的吸油容量为10g/g~20g/g。
3、本发明制备得到的磁性可回收超疏水超亲油吸附剂,可以广泛应用于海洋溢油处理、工业污水净化、食品废油处理等方面。
4、本发明实验方案可行性高,操作工艺简单,资金投入少,制备周期短,反应条件温和,不需要大型仪器设备,可以实现大规模的工业化生产加工,具有很广泛的应用前景。
本发明用于以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备。
附图说明
图1为实施例一步骤一中所述的木粉电镜照片;
图2为实施例一制备的磁性可回收超疏水超亲油吸附剂放大1000倍的电镜照片;
图3为实施例一制备的磁性可回收超疏水超亲油吸附剂放大2000倍的电镜照片;
图4为实施例一制备的磁性可回收超疏水超亲油吸附剂放大5000倍的电镜照片;
图5为实施例一步骤一中所述的木粉与水的接触角照片;
图6为实施例一制备的磁性可回收超疏水超亲油吸附剂与水的接触角照片;
图7为实施例一制备的磁性可回收超疏水超亲油吸附剂与正己烷的接触角照片;
图8为实施例一制备的磁性可回收超疏水超亲油吸附剂吸附柴油后用磁石回收的照片;
图9为水与汽油混合溶液经超声分散所得到的水油乳液;
图10为实施例一制备的磁性可回收超疏水超亲油吸附剂,在离心搅拌的条件下吸附油水乳液中的油后用磁石回收的照片;
图11为实施例一制备的磁性可回收超疏水超亲油吸附剂被完全除去后所得到的溶液照片。
具体实施方式
本发明技术方案不局限于以下所列举的具体实施方式,还包括各具体实施方式之间的任意组合。
具体实施方式一:本实施方式所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,具体是按照以下步骤进行的:
一、木粉的预处理:
将木粉依次过60目和100目筛子,得到粒径均匀的木粉,将粒径均匀的木粉浸入到过氧化氢、氢氧化钠和蒸馏水的混合溶液中,在室温下搅拌10h~15h,得到反应体系,用质量百分数为30%~37%的盐酸调节反应体系pH至中性,用蒸馏水洗涤反应后的木粉2次~4次,然后将洗涤后的木粉置于温度为40℃~70℃的烘箱下干燥至质量恒定,得到干燥后的木粉;
所述的氢氧化钠与过氧化氢的质量比为1:(1~10);所述的氢氧化钠与蒸馏水的质量比为1:(10~200);
二、制备磁性木粉:
将单组份聚氨酯与正己烷混合并磁力搅拌均匀,然后将四氧化三铁纳米颗粒与干燥后的木粉加入到单组份聚氨酯与正己烷的混合溶液中,并在转速为400r/min~800r/min的条件下,搅拌反应10h~20h,得到混合物,将混合物静置并弃上层清液,然后向弃上层清液后的混合物中加入丙三醇水溶液,得到磁性木粉复合物,最后将磁性木粉复合物过滤取出,并用无水乙醇洗涤,然后在温度为50℃~60℃的条件下干燥至恒重,得到磁性木粉;
所述的丙三醇水溶液中丙三醇与水的体积比为1:(0.1~2);所述的单组份聚氨酯的质量与正己烷的体积比为1g:(10~100)mL;所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:(0.1~1);所述的单组份聚氨酯与干燥后的木粉的质量比为1:(0.1~1);所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:(100~200)mL;
三、制备改性液:
将正己烷与十八烷基三氯硅烷混合均匀,得到改性液;
所述的十八烷基三氯硅烷与正己烷的体积比为1:(10~100);
四、磁性木粉改性:
将磁性木粉加入到改性液中,在室温搅拌条件下,反应4h~8h,反应后过滤并用蒸馏水和无水乙醇洗涤,然后在温度为40℃~60℃的烘箱中干燥,得到磁性可回收超疏水超亲油吸附剂;
所述的磁性木粉的质量与改性液的体积比为1g:(10~100)mL。
未经处理的木粉表面存在蜡烛物质,表面含有许多毛刺与毛球,经步骤一的操作降低木粉中的半纤维素和木质素的组分,可以去除纤维表面的杂质及灰尘,除掉纤维表面的蜡状物质,使纤维表面变得膨松粗糙,有利于其与四氧化三铁胶的结合。四氧化三铁通过单组份聚氨酯胶液与木粉的表面吸附共同,进而实现四氧化三铁负载于木粉表面的目的。
本具体实施方式创新点在于,通过胶黏剂粘结包覆的方法将四氧化三铁与木粉粘合,从而得到单组份聚氨酯胶黏剂包覆的木粉复合颗粒。区别于其它胶黏剂仅有的粘合作用,本具体实施方式制备的复合物表面的单组份聚氨酯胶黏剂在丙三醇水溶液的作用下固化形成微纳米颗粒,在四氧化三铁与单组份聚氨酯纳米粒子的共同作用下木粉复合物表面具备良好的微纳米粗糙结构。在随后的硅烷偶联剂改性过程中,由于单组份聚氨酯固化剂表面富含多种极性基团,该基团通过与硅烷偶联剂发生键合,进而达到超疏水/超亲油的目的。而后的溢油吸附和水油乳液吸附实验证明,本具体实施方式所制备的吸附剂解决了现有吸附材料天然有机吸油材料吸收液体后会下沉、疏水性较差、不易回收且难以处理水油乳液等问题,且解决的技术手段不是常规物理操作或本领域人员所公知的。
本实施方式的有益效果是:
1、使用木粉作为原材料,是一种天然可降解的生物质材料,具有储量丰富,廉价易得,且环境友好,易于回收等特点。
2、本实施方式制备得到的磁性可回收超疏水超亲油吸附剂,与水的接触角为150°~152°,与油的接触角为0°,是一种新型的吸油剂,具备高效的油水分离性能。对汽油的吸油容量为10g/g~20g/g,对柴油的吸油容量为10g/g~20g/g,对四氯化碳的吸油容量为10g/g~20g/g。
3、本实施方式制备得到的磁性可回收超疏水超亲油吸附剂,可以广泛应用于海洋溢油处理、工业污水净化、食品废油处理等方面。
4、本实施方式实验方案可行性高,操作工艺简单,资金投入少,制备周期短,反应条件温和,不需要大型仪器设备,可以实现大规模的工业化生产加工,具有很广泛的应用前景。
具体实施方式二:本实施方式与具体实施方式一不同的是:步骤二中所述的四氧化三铁纳米颗粒的粒径为100nm~500nm。其它与具体实施方式一相同。
具体实施方式三:本实施方式与具体实施方式一或二之一不同的是:步骤一中所述的氢氧化钠与过氧化氢的质量比为1:7。其它与具体实施方式一或二相同。
具体实施方式四:本实施方式与具体实施方式一至三之一不同的是:步骤一中所述的氢氧化钠与蒸馏水的质量比为1:100。其它与具体实施方式一至三相同。
具体实施方式五:本实施方式与具体实施方式一至四之一不同的是:步骤二中所述的丙三醇水溶液中丙三醇与水的体积比为7:3。其它与具体实施方式一至四相同。
具体实施方式六:本实施方式与具体实施方式一至五之一不同的是:步骤二中所述的单组份聚氨酯的质量与正己烷的体积比为1g:20mL。其它与具体实施方式一至五相同。
具体实施方式七:本实施方式与具体实施方式一至六之一不同的是:步骤二中所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:0.1。其它与具体实施方式一至六相同。
具体实施方式八:本实施方式与具体实施方式一至七之一不同的是:步骤二中所述的单组份聚氨酯与干燥后的木粉的质量比为1:0.4;步骤二中所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:100mL。其它与具体实施方式一至七相同。
具体实施方式九:本实施方式与具体实施方式一至八之一不同的是:步骤二中所述的单组份聚氨酯为718系单组份无溶剂潮气固化聚氨酯。其它与具体实施方式一至八相同。
具体实施方式十:本实施方式与具体实施方式一至九之一不同的是:步骤三中所述的十八烷基三氯硅烷与正己烷的体积比为1:100。其它与具体实施方式一至九相同。
采用以下实施例验证本发明的有益效果:
实施例一:
一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法是按以下步骤进行:
一、木粉的预处理:
将木粉依次过60目和100目筛子,得到粒径均匀的木粉,将粒径均匀的木粉浸入到过氧化氢、氢氧化钠和蒸馏水的混合溶液中,在室温下搅拌10h,得到反应体系,用质量百分数为36%的盐酸调节反应体系pH至中性,用蒸馏水洗涤反应后的木粉3次,然后将洗涤后的木粉置于温度为50℃的烘箱下干燥至质量恒定,得到干燥后的木粉;
所述的氢氧化钠与过氧化氢的质量比为1:7;所述的氢氧化钠与蒸馏水的质量比为1:100;
二、制备磁性木粉:
将单组份聚氨酯与正己烷混合并磁力搅拌均匀,然后将四氧化三铁纳米颗粒与干燥后的木粉加入到单组份聚氨酯与正己烷的混合溶液中,并在转速为600r/min的条件下,搅拌反应10h,得到混合物,将混合物静置并弃上层清液,然后向弃上层清液后的混合物中加入丙三醇水溶液,得到磁性木粉复合物,最后将磁性木粉复合物过滤取出,并用无水乙醇洗涤,然后在温度为50℃的条件下干燥至恒重,得到磁性木粉;
所述的丙三醇水溶液中丙三醇与水的体积比为7:3;所述的单组份聚氨酯的质量与正己烷的体积比为1g:20mL;所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:0.1;所述的单组份聚氨酯与干燥后的木粉的质量比为1:0.4;所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:100mL;
三、制备改性液:
将正己烷与十八烷基三氯硅烷混合均匀,得到改性液;
所述的十八烷基三氯硅烷与正己烷的体积比为1:100;
四、磁性木粉改性:
将磁性木粉加入到改性液中,在室温搅拌条件下,反应4h,反应后过滤并用蒸馏水和无水乙醇洗涤,然后在温度为50℃的烘箱中干燥,得到磁性可回收超疏水超亲油吸附剂;
所述的磁性木粉的质量与改性液的体积比为1g:100mL;
本实施例步骤二中所述的单组份聚氨酯为长城牌718系单组份无溶剂潮气固化聚氨酯。
图1为实施例一步骤一中所述的木粉电镜照片。由图可知,原始木粉纤维表面是相对光滑的,且疏松多孔。
图2为实施例一制备的磁性可回收超疏水超亲油吸附剂放大1000倍的电镜照片;与原始木粉相比,磁性可回收超疏水超亲油吸附剂表面是粗糙的。
图3为实施例一制备的磁性可回收超疏水超亲油吸附剂放大2000倍的电镜照片;图4为实施例一制备的磁性可回收超疏水超亲油吸附剂放大5000倍的电镜照片;由图3和图4可知,可以看出木粉表面负载大量的胶团,即为经过水固化后的单组份聚氨酯,同时说明由于木粉的吸附作用和胶黏剂的粘附作用,使得四氧化三铁粒子或沉积在木粉纤维表面或被胶黏剂团聚到一起,这些粒子的直径为0.2~5um,粒子之间相互交联,从而构建了较高的表面粗糙度。
图5为实施例一步骤一中所述的木粉与水的接触角照片;图6为实施例一制备的磁性可回收超疏水超亲油吸附剂与水的接触角照片;图5说明原始木粉样品与水滴的接触角大小为0°,能够被水完全润湿,是超亲水的;图6说明本实施例制备的吸附剂对水的接触角为152°,水滴在样品表现呈现球形,是超疏水的;
图7为实施例一制备的磁性可回收超疏水超亲油吸附剂与正己烷的接触角照片;图7说明本实施例制备的吸附剂对油的接触角为0°,是超亲油的。
图8为实施例一制备的磁性可回收超疏水超亲油吸附剂吸附柴油后用磁石回收的照片;由图可知,包覆塑料袋的磁石底部将本实施方式制备的吸附剂全部吸附出来,说明本实施方式制备的吸附剂良好磁性效果,易于回收。
图9为水与汽油混合溶液经超声分散所得到的水油乳液;由图可知油水混合物最终形成了良好的水油乳液。
图10为实施例一制备的磁性可回收超疏水超亲油吸附剂,在离心搅拌的条件下吸附油水乳液中的油后用磁石回收的照片;由图可知,在离心的条件下吸附剂与水油乳液接触充分,且包覆塑料袋的磁石底部将本实施方式制备的吸附剂吸附出来。
图11为实施例一制备的磁性可回收超疏水超亲油吸附剂被完全除去后所得到的溶液照片;由图可知,经吸附剂处理后的溶液具有良好的透光性。
综合图6、图7和图8可知,根据本实施例成功获得了磁性可回收超疏水超亲油功能的吸附剂。综合图9、图10和图11可知,本实施例成功获得的磁性可回收超疏水超亲油功能的吸附剂可以被应用在水油乳液处理方面。
本实施例制备的磁性可回收超疏水超亲油吸附剂的吸油性能研究:对汽油的吸油容量为10.3g/g,对柴油的吸油容量为10.7g/g,对四氯化碳的吸油容量为11.4g/g。
Claims (10)
1.一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于所述吸附剂的制备方法是按照以下步骤进行的:
一、木粉的预处理:
将木粉依次过60目和100目筛子,得到粒径均匀的木粉,将粒径均匀的木粉浸入到过氧化氢、氢氧化钠和蒸馏水的混合溶液中,在室温下搅拌10h~15h,得到反应体系,用质量百分数为30%~37%的盐酸调节反应体系pH至中性,用蒸馏水洗涤反应后的木粉2次~4次,然后将洗涤后的木粉置于温度为40℃~70℃的烘箱下干燥至质量恒定,得到干燥后的木粉;
所述的氢氧化钠与过氧化氢的质量比为1:(1~10);所述的氢氧化钠与蒸馏水的质量比为1:(10~200);
二、制备磁性木粉:
将单组份聚氨酯与正己烷混合并磁力搅拌均匀,然后将四氧化三铁纳米颗粒与干燥后的木粉加入到单组份聚氨酯与正己烷的混合溶液中,并在转速为400r/min~800r/min的条件下,搅拌反应10h~20h,得到混合物,将混合物静置并弃上层清液,然后向弃上层清液后的混合物中加入丙三醇水溶液,得到磁性木粉复合物,最后将磁性木粉复合物过滤取出,并用无水乙醇洗涤,然后在温度为50℃~60℃的条件下干燥至恒重,得到磁性木粉;
所述的丙三醇水溶液中丙三醇与水的体积比为1:(0.1~2);所述的单组份聚氨酯的质量与正己烷的体积比为1g:(10~100)mL;所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:(0.1~1);所述的单组份聚氨酯与干燥后的木粉的质量比为1:(0.1~1);所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:(100~200)mL;
三、制备改性液:
将正己烷与十八烷基三氯硅烷混合均匀,得到改性液;
所述的十八烷基三氯硅烷与正己烷的体积比为1:(10~100);
四、磁性木粉改性:
将磁性木粉加入到改性液中,在室温搅拌条件下,反应4h~8h,反应后过滤并用蒸馏水和无水乙醇洗涤,然后在温度为40℃~60℃的烘箱中干燥,得到磁性可回收超疏水超亲油吸附剂;
所述的磁性木粉的质量与改性液的体积比为1g:(10~100)mL。
2.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的四氧化三铁纳米颗粒的粒径为100nm~500nm。
3.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤一中所述的氢氧化钠与过氧化氢的质量比为1:7。
4.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤一中所述的氢氧化钠与蒸馏水的质量比为1:100。
5.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的丙三醇水溶液中丙三醇与水的体积比为7:3。
6.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的单组份聚氨酯的质量与正己烷的体积比为1g:20mL。
7.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的单组份聚氨酯与四氧化三铁纳米颗粒的质量比为1:0.1。
8.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的单组份聚氨酯与干燥后的木粉的质量比为1:0.4;步骤二中所述的干燥后的木粉的质量与丙三醇水溶液的体积比为1g:100mL。
9.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤二中所述的单组份聚氨酯为718系单组份无溶剂潮气固化聚氨酯。
10.根据权利要求1所述的一种以木粉为原料的磁性可回收超疏水超亲油吸附剂的制备方法,其特征在于步骤三中所述的十八烷基三氯硅烷与正己烷的体积比为1:100。
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