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CN113522030B - 一种光热膜蒸馏用三层膜的制备方法 - Google Patents

一种光热膜蒸馏用三层膜的制备方法 Download PDF

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CN113522030B
CN113522030B CN202110993248.2A CN202110993248A CN113522030B CN 113522030 B CN113522030 B CN 113522030B CN 202110993248 A CN202110993248 A CN 202110993248A CN 113522030 B CN113522030 B CN 113522030B
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康卫民
刘梦瑶
王春艳
鞠敬鸽
黄宇婷
史佳丽
胡伟
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Binzhou Cornell New Material Technology Co ltd
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Abstract

本发明涉及一种光热膜蒸馏用三层膜的制备方法，属于膜蒸馏技术领域。所述三层膜是由聚四氟乙烯纳米纤维膜作为疏水基层，聚偏氟乙烯纳米纤维膜作为中间粘结层，炭黑/聚乙烯醇复合纳米纤维膜作为亲水光热层，所述亲水光热层利用中间粘结层负载于疏水基层。其特征包括：(1)静电溶吹聚四氟乙烯纳米纤维膜的制备；(2)静电纺聚偏氟乙烯纳米纤维膜的制备；(3)静电纺炭黑/聚乙烯醇复合纳米纤维膜的制备；(4)三层膜的复合四个步骤。采用本发明制备的光热膜蒸馏用三层膜具有优异的光热转化性能、较高的水通量、抗盐性和防污性能，在处理高盐废水方面具有广阔的应用前景。

Description

一种光热膜蒸馏用三层膜的制备方法
技术领域
本发明属于光热膜蒸馏技术领域，具体涉及一种光热膜蒸馏用三层膜的制备方法。
背景技术
随着工业的高速发展和人口膨胀，水资源短缺已成为全球面临的严重挑战。海水储量丰富，占全球地表含水量的97％，通过海水淡化技术利用海水资源是解决水资源问题的有效途径。目前，海水淡化工艺主要包括多级闪蒸(MSF)、多效蒸馏(MED)、机械蒸汽压缩(MVC)、反渗透(RO)、纳滤(NF)和膜蒸馏(MD)等。其中，MD是一种膜技术与传统热蒸馏相结合的技术，因出水水质高、运行压力低和运行温度低等优点备受关注。然而，尽管膜蒸馏技术优势显著，但膜蒸馏技术迄今为止仍未实现产业化，这是由于传统膜蒸馏技术仍存在一些局限性，包括给水加热需要损耗大量电能，以及疏水膜与有机污染物之间的强相互作用导致膜污染和膜润湿问题。
为此，采用低品位或可再生能源作为热源替代电能成为膜蒸馏工艺优化的重要举措之一。其中，太阳能因其分布广、成本低而成为MD的理想能源。太阳能驱动MD过程消除了通过外部方式加热水的能源成本，从而为高效的水处理开辟了新的机会。太阳能驱动MD成功的关键是太阳能的高效收集和转移，若采用太阳光直接加热水源，水对太阳光的吸收能力差效率低；若设置太阳能集热装置必然会增加膜蒸馏系统的复杂性。因此，通过制备光热膜成为利用太阳能的优选方案之一。等离子体金属、半导体、碳基材料等纳米粒子已被证明可以有效吸收太阳能，其中碳基材料因其固有的优异性能而被选为优良的光热转换材料，可广泛应用于日常生活中。良好的光热效应、高吸光度和低反射率是碳基材料作为光热材料的关键因素。常用的碳基材料包括炭黑、石墨、石墨烯、碳纳米管、碳复合材料、无定形碳等。
另一方面，针对光热MD膜的膜润湿和膜污染问题，近年来，科学家利用油水分离及抗生物粘附材料的知识和理论，得到亲水材料与污染物之间可以形成水层，可用作有机污染物附着的坚固屏障，赋予MD膜优异防污染和防润湿性能。
本发明探讨出一种光热膜蒸馏用三层膜的制备方法，采用高效的静电溶吹技术开发了一种简单、低成本、高效率的光热膜蒸馏用三层膜，PTFE纳米纤维膜作为疏水基层，其较低的导热率可以减少热量损失，PVDF纳米纤维膜作为中间粘结层，表面能介于PTFE和PVA之间，可有效改善两层之间的附着力，以成本低廉的炭黑纳米颗粒和PVA为原料制备亲水光热层，具有优异的光热性能和亲水性，三层协同具有优异的耐久性，同时实现了高效的局部加热和出色的长期稳定运行，在处理海水淡化方面具有广阔的应用前景。
发明内容
本发明涉及一种光热膜蒸馏用三层膜的制备方法，通过太阳能照射引发光热层的高效局部加热，取代了通过外部加热整个给水系统的需要，消除了传统MD固有的效率限制和巨大的功率需求。基层PTFE高疏水低导热率可以起到了疏水和减少热量损失的作用，中间层PVDF起到紧密粘结作用，表层C/PVA起到了光热防污作用。三层膜具有互相贯通的开孔结构，显著减小蒸汽传质阻力，提高水通量，三层协同具有优异的耐久性，实现了高效的局部加热和出色的长期稳定运行。本发明所制备的光热膜蒸馏用三层膜在膜蒸馏领域具有广阔的应用前景。
1、一种光热膜蒸馏用三层膜的制备方法，其特征在于，包括以下步骤：
(1)静电溶吹聚四氟乙烯(PTFE)纳米纤维膜的制备：将一定量的聚四氟乙烯溶液和一定量聚乙烯醇溶液按照一定比例混合，在室温搅拌0.5～3h，得到纺丝液，采用静电溶吹技术对上述溶液进行纺丝，经煅烧，制得PTFE纳米纤维膜。
(2)静电纺聚偏氟乙烯(PVDF)纳米纤维膜的制备：将一定量的聚偏氟乙烯粉末加入到N，N-二甲基甲酰胺溶剂中，40～60℃下搅拌6～12h至溶质溶解，得到纺丝液，采用静电纺丝技术对上述溶液进行纺丝，制得PVDF纳米纤维膜。
(3)静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备：将一定量的炭黑加入到聚乙烯醇溶液中，室温超声3～5h使炭黑分散均匀，得到纺丝液，采用静电纺丝技术对上述溶液进行纺丝，制得C/PVA复合纳米纤维膜。
(4)三层膜的复合：上述步骤(1)制备的PTFE膜作为基层，步骤(2)制备得PVDF膜作为中间粘结层，步骤(1)制备的C/PVA膜作为光热表层，将三者进行热压复合，制备出光热膜蒸馏用三层膜。图1是本发明光热膜蒸馏用三层膜的制备流程图。
优选的，步骤(1)中所述聚四氟乙烯溶液的质量分数为60％，聚乙烯醇溶液的质量分数为8～12％，两者的混合质量比为5∶2。
优选的，步骤(1)中静电溶吹纺丝参数为纺丝液供给速率25～35ml/h，电压35～45kV，气压0.06～0.12MPa，接收距离60～90cm，煅烧温度360～400℃。
优选的，步骤(2)中聚偏氟乙烯溶液的质量分数为9％。
优选的，步骤(3)中聚乙烯醇溶液的质量分数为10％，炭黑占聚乙烯醇的质量比为0～30％。
优选的，步骤(2)和(3)中静电纺丝参数电压为15～25kV，接收距离为15～20cm，纺丝速度0.5～1.0mL/h。
优选的，步骤(4)中热压温度为170～190℃，时间为0.5～2h。
三层膜的亲水层聚乙烯醇PVA固有的亲水性和良好的可纺性使其成为一种有吸引力的防污聚合物。考虑到PVA聚合物的水溶性，在水处理应用过程中，有必要进行交联处理，以防止静电纺丝亲水涂层膨胀，高温热压不仅能使三层膜紧密复合，还可同时进行PVA的热交联处理。
与现有的技术相比，本发明的优点如下：(1)以高效的静电溶吹技术制备PTFE膜作为基膜，具有优异的隔热性能和疏水性，可有效减少热量损失和防止渗透侧被冷水浸润。(2)PVDF膜的表面能介于PTFE和PVA之间，可以有效改善两层之间的附着力，起到粘合剂的作用。(3)C/PVA光热层中混入低成本高效光热材料炭黑纳米粒子，使表层具有良好的光热转化性能，通过太阳能照射引发光热层的高效局部加热，取代了通过外部加热整个给水系统的需要，消除了传统MD固有的效率限制和巨大的功率需求。在疏水膜上加一层PVA亲水层，膜对表面活性剂、油和腐殖酸表现出良好的防污染性能，可以有效防止膜被含低表面张力污染物所润湿和污染，具有较高的水通量、抗盐性和防污性能，可长期稳定运行，本发明所制备的三层膜在光热膜蒸馏海水淡化领域具有广阔的应用前景。
附图说明
图1是本发明光热膜蒸馏用三层膜的制备流程图。
图2是利用本发明实施例1制备的PTFE纳米纤维膜的电镜图。
图3是利用本发明实施例1制备的PVDF纳米纤维膜的电镜图。
图4是利用本发明实施例1制备的C/PVA纳米纤维膜的电镜图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
(1)取一定量的聚乙烯醇粉末溶于水中，室温搅拌3h，90℃搅拌4h，配置成10％的聚乙烯醇水溶液，冷却待用。
(2)静电溶吹PTFE纳米纤维膜的制备：将60％的PTFE溶液和10％PVA溶液按照比例5∶2混合，在室温搅拌1h，得到纺丝液；采用静电溶吹技术(纺丝液供给速率30ml/h，电压40kV，气压0.1MPa，接收距离80cm)对上述溶液进行纺丝，经390℃高温煅烧，制得PTFE纳米纤维膜。
(3)静电纺PVDF纳米纤维膜的制备，将一定量的PVDF粉末加入到N，N-二甲基甲酰胺溶剂中，50℃下搅拌6h至溶质完全溶解，配置成9％的PVDF纺丝液，采用静电纺丝技术(参数电压15kV，接受距离20cm，纺丝速度0.6mL/h)对上述溶液进行纺丝，制得PVDF纳米纤维膜。
(4)静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备，取一定量的10％的PVA溶液，加入(占PVA含量)10％的炭黑，室温超声3-5h使炭黑分散均匀，得到纺丝液，采用静电纺丝技术(参数电压15-25kV，接受距离15-20cm，纺丝速度0.5-1mL/h)对上述溶液进行纺丝，制得C/PVA复合纳米纤维膜。
(5)三层膜的复合，上述步骤(1)制备的PTFE膜作为基层，步骤(2)制备得PVDF膜作为中间粘结层，步骤(1)制备的C/PVA膜作为光热表层，将三者进行180℃热压复合，制备出光热膜蒸馏用三层膜。
(6)上述制得的三层膜，三者厚度比为10∶1∶4进行复合，膜的总厚度为160-180μm。图2是利用本发明实施例1制备的PTFE纳米纤维膜的电镜图，图3是利用本发明实施例1制备的PVDF纳米纤维膜的电镜图，图4是利用本发明实施例1制备的C/PVA纳米纤维膜的电镜图。
(7)光热膜蒸馏测试：由太阳模拟器、玻璃模具、电子天平、电导率仪、蠕动泵与恒温水箱组成的直接接触式膜蒸馏系统测试所制备膜的光热膜蒸馏性能。渗透液和进料液的温度始终由恒温水箱保持在20℃。进料液和渗透液均由蠕动泵循环，恒定流量为0.25L/min，模拟海水浓度为3.5wt％NaCl，设定光照强度为1kW/m2，测试面积2×2cm2。抗污染性能测试中，进料液是由3.5％NaCl、3g/L CaCl2、10mg/L SDS、10mg/L HA组成的混合液。由电导率仪与天平测量，膜蒸馏软件记录渗透液的电导率变化以及渗透通量变化。采用红外热成像仪测量膜表面的温度变化。渗透通量J通过渗透液的重量变化计算，由以下公式计算得到：
J＝ΔM/(ΔT×S)
式中：J为通量(kg/m2h)，ΔM渗透液增重(kg)，ΔT运行时间(h)，S膜有效面积(cm2)
截盐率R通过渗透液的电导率计算，由以下公式计算得到：
R＝[(Cf-Cp)/Cf]×100％
式中：R截留率，Cf进料液的浓度(g/L)，Cp渗透液的浓度(g/L)。可根据电导率和浓度的线性关系，由电导率计算出溶液浓度。
所制备得到的三层膜测试结果如表1所示，在模拟一个太阳光照条件下，经90s光照后，膜表面温度最高可达47.1℃，运行10h渗透通量可达1.15kg/m2h，截留率高达99.9％以上。三层膜在处理含各种污染物的盐水时具有良好的稳定性，截留率仍可保持在99.99％以上，而商业膜PVDF、PTFE基膜在此过程中污染严重，产生膜润湿和膜污染现象。
实施例2
(1)同实施例1。
(2)同实施例1。
(3)同实施例1。
(4)静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备，取一定量的10％的PVA溶液，加入(占PVA含量)20％的炭黑，室温超声3-5h使炭黑分散均匀，得到纺丝液，采用静电纺丝技术(参数电压15-25kV，接受距离15-20cm，纺丝速度0.5-1mL/h)对上述溶液进行纺丝，制得C/PVA复合纳米纤维膜。
(5)同实施例1。
(6)同实施例1。
(7)同实施例1。
所制备得到的三层膜测试结果如表1所示，在模拟一个太阳光照条件下，经90s光照后，膜表面温度最高可达52.6℃，运行10h渗透通量可达1.54kg/m2h，截盐率高达99.9％以上。
实施例3
(1)同实施例1。
(2)同实施例1。
(3)同实施例1。
(4)静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备，取一定量的10％的PVA溶液，加入(占PVA含量)30％的炭黑，室温超声3-5h使炭黑分散均匀，得到纺丝液，采用静电纺丝技术(参数电压15-25kV，接受距离15-20cm，纺丝速度0.5-1mL/h)对上述溶液进行纺丝，制得C/PVA复合纳米纤维膜。
(5)同实施例1。
(6)同实施例1。
(7)同实施例1。
所制备得到的三层膜测试结果如表1所示，在模拟一个太阳光照条件下，经90s光照后，膜表面温度最高可达53℃，运行10h渗透通量1.60kg/m2h，截盐率高达99.9％以上。
表1光热膜蒸馏用三层膜的性能
Figure BSA0000250963660000061

Claims (1)

1.一种光热膜蒸馏用三层膜的制备方法，其特征在于，包括以下步骤：
(1)静电溶吹聚四氟乙烯(PTFE)纳米纤维膜的制备：将一定量的聚四氟乙烯溶液和一定量聚乙烯醇溶液按照一定比例混合，在室温下搅拌0.5～3h，得到纺丝液；采用静电溶吹技术对上述溶液进行纺丝，经煅烧，制得PTFE纳米纤维膜；
(2)静电纺聚偏氟乙烯(PVDF)纳米纤维膜的制备：将一定量的聚偏氟乙烯粉末加入到N，N-二甲基甲酰胺溶剂中，40～60℃下搅拌6～12h至溶质溶解，得到纺丝液，采用静电纺丝技术对上述溶液进行纺丝，制得PVDF纳米纤维膜；
(3)静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备：将一定量的炭黑加入到聚乙烯醇溶液中，室温超声3～5h使炭黑分散均匀，得到纺丝液，采用静电纺丝技术对上述溶液进行纺丝，制得C/PVA复合纳米纤维膜；
(4)三层膜的复合，上述步骤(1)制备的PTFE膜作为基层，步骤(2)制备得PVDF膜作为中间粘结层，步骤(1)制备的C/PVA膜作为光热表层，将三者进行热压复合，制备出光热膜蒸馏用三层膜；
所述静电溶吹聚四氟乙烯(PTFE)纳米纤维膜的制备中，聚四氟乙烯溶液的质量分数为60％，聚乙烯醇溶液的质量分数为8～12％，两者的混合质量比为5∶2；静电溶吹纺丝参数为纺丝液供给速率25～35ml/h，电压35～45kV，气压0.06～0.12MPa，接收距离60～90cm；煅烧温度360～400℃；
所述静电纺聚偏氟乙烯(PVDF)纳米纤维膜和静电纺炭黑/聚乙烯醇(C/PVA)复合纳米纤维膜的制备中，聚偏氟乙烯溶液的质量分数为9％，聚乙烯醇溶液的质量分数为10％，炭黑占聚乙烯醇的质量为0～30％；静电纺丝参数电压为15～25kV，接收距离为15～20cm，纺丝速度0.5～1.0mL/h；
所述三层膜的复合过程中，热压温度为170～190℃，时间为0.5～2h。
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