CN113893706B - 一种多孔亲水的光热海水淡化复合膜及制备方法 - Google Patents
一种多孔亲水的光热海水淡化复合膜及制备方法 Download PDFInfo
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Abstract
本发明涉及太阳能海水淡化技术领域,公开了一种用于太阳能驱动界面蒸发的光热海水淡化复合膜及制备方法。所述光热海水淡化复合膜包括水运输层,热管理层和光吸收层;其中,热管理层设于水运输层和光吸收层之间;所述水运输层为多孔聚丙烯腈薄膜,所述热管理层为掺杂有碳纳米管的多孔水性环氧树脂薄膜,所述光吸收层为碳化硅/氮化硅薄膜。本发明所述光热海水淡化复合膜具有光热转换效率高、生产成本低、耐久稳定、可批量生产等特点,适用于海水淡化处理。
Description
技术领域
本发明涉及太阳能海水淡化和功能表面改性技术领域,涉及一种用于太阳能界面蒸发海水淡化的膜材料及其制备方法。
背景技术
淡水资源是人类最紧缺的资源之一。在地球的全部水资源中,有97%都是不能被人类直接饮用的海水。如何大批量地、成本低廉地将海水转化为淡水,关系到人类的可持续发展。利用太阳能驱动界面蒸发进行海水淡化为此提出了一种解决方案。太阳能是一种丰富的清洁能源,解决了海水淡化的能源问题就在很大程度上解决了成本问题。该技术利用光吸收体的光热吸收能力,使水分子在光吸收体界面蒸发,达到海水淡化的目的。
目前,光热海水淡化膜的主要问题是价格十分昂贵,不具有实际使用的可能性,或是制备方法无法实现工业化。专利CN 109603596A公开了一种金属有机框架材料光热海水淡化膜,其中光热材料层为多级孔结构碳薄膜,由氢氧化物纳米线溶液与单壁碳纳米管制得;专利CN111330451A公开了疏水性碳点改性的正渗透复合膜的制备方法,提出通过共混方式,将聚砜、氧化石墨烯、聚乙二醇、吐温和溶剂加入到烧瓶中,用相转化法制得氧化石墨烯/聚砜支撑层;又如专利CN 111282443A公开了一张用于太阳能界面蒸发海水淡化的膜材料,提出了通过采用静电纺丝技术制备PAA纳米纤维膜,再加温加压对其进行亚胺化得到PI纳米纤维膜,最后激光烧蚀技术对PI膜表面进行烧蚀,使其表面形成多孔蓬松的石墨烯纤维。以上几种制膜方式均存在工艺复杂、原材料昂贵或是材料中含有有毒物质,对人的健康有不利影响等诸多问题。
光热海水淡化膜材料常使用石墨烯、氧化石墨烯(GO)、还原氧化石墨烯(rGO)等二维碳材料或是纳米金、纳米银、纳米铂颗粒等纳米金属颗粒,这也是光热海水淡化膜成本高昂和难以实现工业大规模生产的主要原因。
光热海水淡化膜的另一个问题是基本上没有考虑海洋恶劣天气对膜的影响,在实际使用中常常出现膜剥落或是被腐蚀的现象,严重影响了光热海水淡化膜的正常工作。
综上所述,开发出一种制备光热海水淡化膜的方法,不仅需要增强膜的水运输能力和吸光吸热能力,还应具有绿色环保、便捷简单的工艺方式,同时应考虑使用环境的影响。而目前暂时没有满足以上要求的光热海水淡化膜。
发明内容
本发明所要解决的技术问题是针对上述现有技术存在的不足而提供一种多孔亲水的光热海水淡化复合膜及制备方法。本发明提出的制备方法绿色环保,价格低廉,制备得到的光热海水淡化复合膜具有多孔结构,亲水性强,光吸收率较高,不存在泄露和污染的问题,具有较高的工业应用价值。
本发明为解决上述提出的问题所采用的技术方案为:
一种多孔亲水的光热海水淡化复合膜,包括光吸收层,热管理层和水运输层;其中,热管理层设于水运输层和光吸收层之间;所述水运输层为聚丙烯腈薄膜,所述热管理层为掺杂有碳纳米管的环氧树脂薄膜,所述光吸收层为碳化硅/氮化硅薄膜。
按上述方案,所述光吸收层的厚度为0.1~0.3mm,热管理层的厚度为0.2~0.6mm,水运输层的厚度为0.1~0.3mm。
按上述方案,所述水运输层为多孔聚丙烯腈薄膜,孔隙率为75%~85%;所述热管理层为掺杂有碳纳米管的多孔水性环氧树脂薄膜,孔隙率为65%~80%,接触角为40°~50°,碳纳米管掺杂量为环氧树脂质量的8%~20%(掺杂量以碳纳米管占多孔水性环氧树脂薄膜的质量百分比计);所述光吸收层为碳化硅/氮化硅复合薄膜,其中氮化硅的质量分数为碳化硅的30%~50%,所述多孔聚丙烯腈薄膜购自西安齐岳生物科技有限公司,孔隙率为75%~85%。
按上述方案,所述碳化硅/氮化硅复合薄膜的制备方法包括如下步骤:
ST1:将可膨胀石墨与二氧化硅溶胶混合,经凝胶、烘干、粉碎,得到含可膨胀石墨的二氧化硅干凝胶;其中,所述二氧化硅溶胶的二氧化硅质量分数为30%~50%,pH为9~10;所述可膨胀石墨与二氧化硅的质量比在1:0.6~1:1.1;
ST2:将含可膨胀石墨的二氧化硅干凝胶和硅粉置于管式炉进行烧结,冷却剥离后滚压即得到碳化硅/氮化硅复合薄膜;其中,硅粉的添加质量为所述含可膨胀石墨的二氧化硅干凝胶的60%~65%;所述烧结的工艺为:在氮气气氛下,升温升至1500℃~1800℃,保温4~6h。
按上述方案,掺杂有碳纳米管的环氧树脂薄膜的制备方法包括如下步骤:
ST11:对碳纳米管进行强酸处理、超声处理,洗涤并干燥后备用;
ST22:将氯化铁和硫酸亚铁制成混合水溶液,加入ST11步骤所得碳纳米管,调节混合液pH为8~10,抽滤后得到负载四氧化三铁的碳纳米管粉末,负载量为60~70%(负载量以四氧化三铁占负载四氧化三铁的碳纳米管粉末总质量的质量百分比计);
ST33:在甲基异丁基甲酮中加入环氧树脂、固化剂和乳化剂,并滴加二氧化硅,搅拌均匀得到混合浓乳液;
ST44:向所得浓乳液加入负载四氧化三铁的碳纳米管粉末,刮涂于石英玻璃板上,置于磁场和60℃恒温水浴中共混并预固化,剥离得到各孔径为20~400nm的掺杂有碳纳米管的多孔水性环氧树脂薄膜;
ST55:将ST44步骤所得多孔环氧树脂薄膜浸泡在溶有偶氮二异丁腈的丙酮中进行抽真空处理,取出后干燥,然后浸泡在甲基丙烯酸甲酯中进行抽真空处理,并取出干燥,得到掺杂有碳纳米管的多孔亲水环氧树脂薄膜。
进一步地,所述碳纳米管为多壁碳纳米管;步骤ST11步骤所述的强酸为体积比为3:1的浓硫酸和浓硝酸的混合液;步骤ST33所述的固化剂为650低分子聚酰胺,乳化剂为Span20。其中,乳化剂能降低界面张力,添加一定用量的乳化剂可以制备稳定的环氧树脂浓乳液,但其对多孔化环氧树脂的孔结构可能具有不利影响。为了得到网状孔结构,且孔洞连通性较好、空隙率较高,乳化剂用量应为环氧树脂质量的8%~12%。
进一步地,步骤ST33中,所述环氧树脂为甲基异丁基甲酮质量的65%~72%,固化剂为环氧树脂质量的75%~85%,二氧化硅溶胶为环氧树脂质量的3%~5%。
本发明所述的多孔亲水的光热海水淡化复合膜的制备方法,沿热管理层材料上表面和下表面的边缘一圈涂上环氧粘合剂,将光吸收层,热管理层和水运输层三层依次紧贴复合在一起,形成多孔亲水的光热海水淡化复合膜。
本发明所述的多孔亲水的光热海水淡化复合膜可以在太阳能驱动界面蒸发方面的应用。
本发明中,光吸收层碳化硅/碳化硅薄膜具有明显的二维结构和优异的化学稳定性,以及较高的光吸收率,使光子在其中多次反射形成光学微腔,增强了光吸收。该二维结构的存在使热量不向下方损失,而是向平面扩散,增强了水蒸发速率。而且,碳化硅薄膜价格也比较低廉,适宜工业生产。
热管理层掺杂有碳纳米管的多孔水性环氧树脂薄膜中,环氧树脂和碳纳米管包围空气作为热障,有效的阻止上层热量散失到水面,具有吸热、储热的特性;而且,掺杂碳纳米管后的环氧树脂具有多孔和亲水的特性,便于水分子通过毛细作用向上运输至光吸收界面,同时阻止部分盐离子的扩散,提高了蒸发效率。该膜密度小、质量轻,在因恶劣情况致水运输层脱落后,能为复合膜继续提供浮力和运输水分子使之正常工作。即使光吸收层脱落,该膜因掺有多壁碳纳米管,也具有一定的吸光吸热能力。
水运输层聚丙烯腈的材质密度低,能为上层提供部分浮力,亲水性较好,进行多孔化处理并制成薄膜后,多孔聚丙烯腈薄膜半淹没于海水平面,水分子通过毛细作用运输至上层。
与现有技术相比,本发明有益技术效果是:
(1)本发明所制得的多孔亲水的光热海水淡化复合膜,通过改变微观物理结构来增强单层膜的亲水性,未添加其他亲水物质,符合绿色环保的理念。本发明所述多孔亲水的光热海水淡化复合膜的各层各司其职,协同发挥作用,其中最底层的水运输层提供浮力和运输水分子;中间的热管理层继续向上层运输水分子,同时储存热量,阻止热量逸散到水下;顶层的光吸收层吸收热能,是水蒸发的平台。
(2)本发明考虑了海洋天气可能造成的影响,因意外原因导致光吸收层或水运输层薄膜脱落时,掺有多壁碳纳米管的多孔水性环氧树脂薄膜因含有弥散的碳纳米管,有一定的光吸收作用,且丰富的孔隙能够储存热量;且因其孔隙较多、密度较小,能够为上层提供浮力,亲水化的环氧树脂能发挥水运输的作用。
(3)本发明的制备方法,原材料较为廉价,原料对环境污染小,制成的膜对海洋无污染,工业化生产可能性高。
附图说明
图1为碳化硅(SiC)/碳化硅(Si3N4)薄膜的金相照片(200倍);
图2为碳化硅(SiC)/碳化硅(Si3N4)薄膜的X射线衍射图谱;
图3为掺有多壁碳纳米管的多孔水性环氧树脂薄膜的累积孔体积-孔径关系;
图4为复合膜的水体失重变化曲线;
图5为复合膜的表面升温曲线(100mW/cm2,AM 1.5)。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明不仅仅局限于下面的实施例。
下述实施例中,所述的水运输层的材质为多孔亲水聚丙烯腈薄膜,该膜购自西安齐岳生物科技有限公司(货号24211),具体参数如下:孔隙率为75%~85%,纤维直径:500nm,孔径:30um,厚度:200um;二氧化硅溶胶购自上海麦克林生化科技有限公司(货号S888350),具体参数如下:二氧化硅含量:29%~31%,pH:9~10.5,粘度(25℃):≤6.5mm2/s,粒度:7~10nm;环氧粘合剂购自3M公司(货号EC-2216)。
为更好的理解本发明,下面的实施例是对本发明的进一步说明,但本发明的内容不仅仅局限于下面的实施例。
实施例1
a.纳米碳化硅薄膜的制备
ST1:混合15g可膨胀石墨与50ml二氧化硅溶胶(SiO2含量30%,pH=10),凝胶、烘干、粉碎,得到含可膨胀石墨的二氧化硅干凝胶;
ST2:将含可膨胀石墨的二氧化硅干凝胶混合18g硅粉置于管式炉,在氩气保护环境下,以5℃/min的升温速度升至1500℃,保温4h后取出自然冷却,滴入丙酮溶液,挥发、滚压、剥离即得到碳化硅(SiC)/氮化硅(Si3N4)薄膜,碳化硅(SiC)/氮化硅(Si3N4)的质量比为1:0.4,裁剪为直径40mm的圆形薄膜待用。
所得碳化硅(SiC)/氮化硅(Si3N4)薄膜的金相照片(200倍)、X射线衍射(XRD)图谱分别如图1、2所示。
由图1-2可知:上述方法成功制备了碳化硅(SiC)/氮化硅(Si3N4)薄膜,碳化硅(SiC)/氮化硅(Si3N4)的质量比为1:0.4。
b.掺杂有多壁碳纳米管的多孔水性环氧树脂薄膜的制备
ST11:将0.4g多壁碳纳米管(m-CNTs)加到6mL浓硫酸和2mL浓硝酸的混合液中,超声处理,过滤后用去离子水洗涤至中性,干燥后备用;
ST22:混合0.5g氯化铁(FeCl3·6H20)和0.25g硫酸亚铁(FeSO4·7H2O)并加入20mL去离子水制成水溶液,加入0.2g处理后的多壁碳纳米管,氨水调节混合液pH为9,抽滤后得到负载四氧化三铁的多壁碳纳米管粉末,负载量65%;
ST33:在5.6g甲基异丁基甲酮(MSDS)中混合4g环氧树脂(E-44)、3.2g 650低分子量聚酰胺(LPA650)和0.48g Span20,滴加0.15mL二氧化硅溶胶,搅拌均匀得到混合浓乳液;
ST44:向所得浓乳液加入0.04g负载四氧化三铁的碳纳米管粉末,刮涂于石英玻璃板上,置于磁场和60℃恒温水浴中共混并固化,剥离得到孔径为20~400nm的掺杂有碳纳米管的多孔环氧树脂薄膜,该步骤制得的薄膜样品记为样品ST44;
ST55:将所得掺杂有碳纳米管的多孔环氧树脂薄膜浸泡在溶有1%~2%质量分数偶氮二异丁腈的丙酮中,置于真空烘箱抽3次真空,然后从丙酮中取出后干燥12h,再浸泡在甲基丙烯酸甲酯中置于真空烘箱抽3次真空,得到掺杂有多壁碳纳米管的多孔水性环氧树脂薄膜,掺杂量10%,接触角44.6°,孔隙率75%。该步骤制得的薄膜样品记为样品ST55。
步骤ST55所得掺杂有碳纳米管的多孔环氧树脂薄膜的累积孔体积-孔径关系如图3所示。步骤ST44与步骤ST55处理前后环氧树脂薄膜的接触角如表1所示。
表1
由图3和表1可知:步骤ST55所得掺杂有碳纳米管的多孔环氧树脂薄膜具有多孔的结构,孔径为20~400nm;亲水性良好,接触角为44.6°。
c.一种多孔亲水的光热海水淡化复合膜,包括光吸收层,热管理层和水运输层;其中,热管理层设于水运输层和光吸收层之间;所述水运输层为上述多孔聚丙烯腈薄膜,厚度0.2mm,孔隙率为80%,购自西安齐岳生物科技有限公司;所述热管理层为本实施例制备的掺杂有多壁碳纳米管的多孔水性环氧树脂薄膜,厚度0.4mm,接触角44.6°,掺杂量10%,孔隙率75%;所述光吸收层为本实施例制备的碳化硅/氮化硅复合薄膜,厚度0.3mm。
上述多孔亲水的光热海水淡化复合膜的制备方法,沿热管理层的上表面和下表面的边缘一圈涂上环氧粘合剂(购自3M公司,货号EC-2216)。将光吸收层,热管理层和水运输层三层依次紧贴复合在一起,形成多孔亲水的光热海水淡化复合膜。
所得多孔亲水的光热海水淡化复合膜的水体失重变化曲线、表面升温曲线(100mW/cm2,AM 1.5)如图4、5所示。
由图4-5可知:本实施例所述光热海水淡化复合膜具有良好的光热转换效率,在1个太阳光强度下照射60分钟,有膜情况下水体失重约为1.77kg/m2;而无膜情况下约为0.49kg/m2,提升了3.61倍;在1个太阳光强度下照射450秒,有膜情况下,水体表面温度约为63.3℃,无膜情况下,水体表面温度约为43.2℃,提升了1.47倍。
实施例2
一种多孔亲水的光热海水淡化复合膜,包括光吸收层,热管理层和水运输层;其中,热管理层设于水运输层和光吸收层之间;所述水运输层为多孔聚丙烯腈薄膜,厚度0.2mm;所述热管理层为本实施例制备的掺杂有多壁碳纳米管的多孔水性环氧树脂薄膜,厚度0.5mm;所述光吸收层为本实施例制备的碳化硅/氮化硅复合薄膜,厚度0.2mm。
该多孔亲水的光热海水淡化复合膜的制备方法和复合方式与实施例1相同。
本实施例中,制备碳化硅/氮化硅复合薄膜时取用的可膨胀石墨、二氧化硅溶胶与硅粉分别为15g,60mL,19.8g。所制备的纳米碳化硅/氮化硅复合薄膜厚度为0.2mm,碳化硅(SiC)/氮化硅(Si3N4)的质量比为1:0.5。
本实施例中,制备掺有多壁碳纳米管的多孔水性环氧树脂薄膜时,ST22中取用的氯化铁(FeCl3·6H20)和硫酸亚铁(FeSO4·7H2O)分别为0.4g和0.2g,调节后的pH=10;ST33中取用的环氧树脂(E-44)、650低分子量聚酰胺(LPA650)和Span20分别为4.2g、3.15g和0.5g。制得的掺有多壁碳纳米管的多孔水性环氧树脂薄膜孔径为35~400nm,厚度为0.5mm,掺杂量9.5%,接触角43.5°,孔隙率78%。
实施例3
一种多孔亲水的光热海水淡化复合膜,包括光吸收层,热管理层和水运输层;其中,热管理层设于水运输层和光吸收层之间;所述水运输层为上述多孔聚丙烯腈薄膜,厚度0.2mm;所述热管理层为本实施例制备的掺杂有多壁碳纳米管的多孔水性环氧树脂薄膜,厚度0.6mm;所述光吸收层为本实施例制备的碳化硅/氮化硅复合薄膜,厚度0.2mm。
该多孔亲水的光热海水淡化复合膜的制备方法和复合方式与实施例1相同。
本实施例中,制备碳化硅/氮化硅复合薄膜时升温温度为1600℃,保温时间为5h。所制备的纳米碳化硅薄膜厚度为0.2mm。
本实施例中,制备掺有多壁碳纳米管的多孔水性环氧树脂薄膜时,ST33中取用的环氧树脂(E-44)、650低分子量聚酰胺(LPA650)和Span20分别为4.5g、3.8g和0.54g。制得的掺有多壁碳纳米管的多孔水性环氧树脂薄膜孔径为30~400nm,厚度为0.6mm,掺杂量8.9%,接触角45.4°,孔隙率80%。
以上所述仅是本发明的优选实施方式,应当指出,对于本领域的普通技术人员来说,在不脱离本发明创造构思的前提下,还可以做出若干改进和变换,这些都属于本发明的保护范围。
Claims (7)
1.一种多孔亲水的光热海水淡化复合膜,其特征在于,所述光热海水淡化复合膜包括光吸收层,热管理层和水运输层;其中,热管理层设于水运输层和光吸收层之间,沿热管理层的上表面和下表面的边缘涂抹环氧粘合剂,将水运输层、热管理层和光吸收层三层依次贴合形成所述的光热海水淡化复合膜;所述水运输层为多孔聚丙烯腈薄膜,孔隙率为75%~85%;所述热管理层为掺杂有碳纳米管的环氧树脂薄膜;所述光吸收层为碳化硅/氮化硅薄膜,其中氮化硅的质量分数为碳化硅的30%~50%;
掺杂有碳纳米管的环氧树脂薄膜的制备方法包括如下步骤:
ST11:对碳纳米管进行强酸处理、超声处理,洗涤并干燥后备用;
ST22:将氯化铁和硫酸亚铁制成混合水溶液,加入ST11步骤所得碳纳米管,调节混合液pH为8~10,抽滤后得到负载四氧化三铁的碳纳米管粉末,负载量为60~70%;
ST33:在甲基异丁基甲酮中加入环氧树脂、固化剂和乳化剂,并滴加二氧化硅溶胶,搅拌均匀得到混合浓乳液;
ST44:向所得浓乳液加入负载四氧化三铁的碳纳米管粉末,刮涂于石英玻璃板上,置于磁场和55~65℃恒温水浴中共混并固化,剥离得到孔径为20~400nm的掺杂有碳纳米管的多孔环氧树脂薄膜;
ST55:将ST44步骤所得多孔环氧树脂薄膜浸泡在溶有偶氮二异丁腈的丙酮中进行抽真空处理,取出后干燥,然后浸泡在甲基丙烯酸甲酯中进行抽真空处理,并取出干燥,得到掺杂有碳纳米管的多孔亲水环氧树脂薄膜;
所述碳化硅/氮化硅薄膜的制备方法包括如下步骤:
ST1:将可膨胀石墨与二氧化硅溶胶混合,经凝胶、烘干、粉碎,得到含可膨胀石墨的二氧化硅干凝胶;
ST2:将含可膨胀石墨的二氧化硅干凝胶和硅粉置于氮气氛围下管式炉进行烧结,冷却后收集产物,滚压剥离即得到碳化硅/氮化硅薄膜。
2.根据权利要求1所述的一种多孔亲水的光热海水淡化复合膜,其特征在于,所述光吸收层的厚度为0.1~0.3mm,热管理层的厚度为0.2~0.6mm,水运输层的厚度为0.1~0.3mm。
3.根据权利要求1所述的一种多孔亲水的光热海水淡化复合膜,其特征在于,所述热管理层为掺杂有碳纳米管的多孔水性环氧树脂薄膜,孔隙率为65%~80%,接触角为40°~50°,碳纳米管掺杂量为8%~20%。
4.根据权利要求1所述的一种多孔亲水的光热海水淡化复合膜,其特征在于所述二氧化硅溶胶的二氧化硅质量分数为30%~50%,pH为9~10;所述可膨胀石墨与二氧化硅的质量比在1:0.6~1:1.1;所述硅粉的添加质量为所述含可膨胀石墨的二氧化硅干凝胶的60%~65%;所述烧结的工艺为:在氮气气氛下,升温升至1500℃~1800℃,保温4~6h。
5.根据权利要求1所述的一种多孔亲水的光热海水淡化复合膜,其特征在于所述碳纳米管为多壁碳纳米管;步骤ST33所述的固化剂为650低分子聚酰胺,乳化剂为Span20。
6.根据权利要求1所述的一种多孔亲水的光热海水淡化复合膜,其特征在于步骤ST33中,所述环氧树脂为甲基异丁基甲酮质量的65%~72%,固化剂为环氧树脂质量的75%~85%,乳化剂为环氧树脂质量的8%~12%,二氧化硅溶胶为环氧树脂质量的3%~5%;其中,所述二氧化硅溶胶的二氧化硅含量为30%~50%,pH为9~10。
7.权利要求1所述的多孔亲水的光热海水淡化复合膜在太阳能驱动界面蒸发方面的应用。
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