CN110559876B - 一种新型陶瓷膜 - Google Patents
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Abstract
本发明提供一种新型陶瓷膜，所述陶瓷膜为多层结构，所述陶瓷膜包括支撑层，在支撑层上依次负载有过渡层和膜分离层，每层膜单元的厚度从下向上呈递增的梯度分布，采用了大通量的膜结构，可以保证过滤的效率，同时又能够减少堵塞现象，而且方便对膜进行清洗处理；中心孔设置有支撑柱，同时增强了膜的刚性。
Description
技术领域
本发明涉及陶瓷膜领域，尤其涉及一种新型陶瓷膜。
背景技术
为了应对饮用水质健康风险带来的技术挑战，膜分离技术已经逐渐成为饮用水处理领域研究的热点，目前在饮用水处理中普遍研究和应用的膜技术仍以有机膜为主，虽然其制备成本相对较低，但本身具有局限性，例如耐腐蚀性差、耐氧化能力差、不易清洁、机械强度低、使用寿命短等，上述缺点严重限制了有机膜处理苛刻条件污水的潜在应用价值。
与有机膜相比，陶瓷膜具有显著的材料性能优势。陶瓷膜过滤系统是一种可以广泛应用于各种领域的精密型超级过滤净化设备。其核心组件陶瓷膜具有优良的热稳定性与孔稳定性能，不但强度高、且耐化学腐蚀，清洗再生性能好，兼备有高效过滤与精密过滤的双重优点。
陶瓷膜可用于处理各种生活用水、工艺用水处理，工业废水净化(焦化水、浊环水等)，适用于生产及工业的含油废水处理，水处理行业中工业水处理、工业循环冷却水净化、高纯工艺水净化，生产水处理、超滤、反渗透、电渗析、离子交换树脂前的预过滤，中水回用处理，设备冷冻、冷却循环水的过滤，工业废水过滤、净化，河水、井水、湖水等的精密过滤，但日前市售陶瓷膜均存在成本高、易堵塞等不同程度的缺陷。
为了解决上述技术问题，本发明提供一种新型陶瓷膜。
发明内容
为了解决上述技术问题，在提升污水处理处理效果，本发明提供一种新型陶瓷膜。
本发明是以如下技术方案实现的：
本发明提供一种新型陶瓷膜，所述陶瓷膜为多层结构，所述陶瓷膜包括支撑层，在支撑层上依次负载有过渡层和膜分离层。
进一步地，所述支撑层为一种异型滤孔陶瓷膜。
进一步地，所述异型滤孔陶瓷膜主体结构为多孔道类圆形支撑结构，孔道数量可以为5-9条，优选地为7条，所述孔道自上而下编号1-7，其中1,2,6,7号孔道为无阻隔孔道，每条孔道最高处内径为1mm，3,4,5号孔道每隔两个类圆形孔结构设置有一支撑结构。
进一步地，所述异型滤孔陶瓷膜含有一种新型链式化合物，结构式为
进一步地，所述异型滤孔陶瓷膜的制备方法为：
步骤一、将摩尔比为1.67的Ca(OH)2，和H3PO4混合均匀，通过湿式化学沉淀法制备HAP粉末，在合成期间保持反应环境为pH 11-12，然后将合成的HAP在80℃下烘箱干燥并在800℃下煅烧，之后将HAP粉末化并保存以供进一步使用；
步骤二、制备新型链式化合物。具体地，向60ml 1,2-丙二醇中加入3.25mL，31mmol，6当量的氯化亚砜，0℃反应20分钟；向混合物中加入20mmol L-Gln，室温下置于磁力搅拌器中搅拌178小时，取产物进行薄层层析，验证表明氨基酸完全吸收，获得了一种新型链式化合物，结构式为
步骤三、用Dolapix将步骤一制备的HAP粉末分散在水中，之后加入聚乙二醇及羟乙基纤维素，将上述溶液搅拌至无气泡获得溶液一，将上述溶液一与等体积的新型链式化合物混合并干燥至粉末状态，将其风干过夜，与粘土、氧化铝、成孔剂、抗絮凝剂以质量比为65:20:12:3:1的比例在650℃下以3℃/min的加热速率烧结获得异型滤孔陶瓷膜；
步骤四、用沸水洗涤异型滤孔陶瓷膜，之后用丙酮洗涤异型滤孔陶瓷膜并超声处理，从孔道中除去油状和颗粒状物质，最后将异型滤孔陶瓷膜干燥并吹气以除去灰尘颗粒。
进一步地，所述新型陶瓷膜的制备方法为，将等质量比羟乙基纤维素和氧化石墨烯纤维在聚丙烯酰胺交联固化后沿异型滤孔陶瓷膜内壁延展，将异型滤孔陶瓷膜置于电弧炉烧结中，逐渐升温至880-900℃，烧制1.5h，然后再升温至920-1120℃，烧制0.5h，最后降温至850～870℃，保温2h，冷却，得到二级异型滤孔陶瓷膜；膜分离层为涂覆的纳米银离子(购自大连和建科技发展有限公司)，将纳米银离子通过聚丙烯酰胺交联固化在过渡层上，并于120℃保温3h形成过滤层。
本发明具备下述有益效果：本发明公开了一种分层烧结的陶瓷膜，每层膜单元的厚度从下向上呈递增的梯度分布，采用了大通量的膜结构，可以保证过滤的效率，同时又能够减少堵塞现象，而且方便对膜进行清洗处理；中心孔设置有支撑柱，同时增强了膜的刚性；本发明的制备方法简单方便，采用分层烧结的方法，提高了烧结的成功率。
附图说明
图1为本发明所述新型陶瓷膜的横截面示意图。
图2为本发明所述新型陶瓷膜分层结构示意图，其中111-支撑层、112-过渡层、113-分离层。
图3为本发明所述陶瓷膜过滤器，其中1-陶瓷膜本体、2-第一可拆卸连接头、3-第二可拆卸连接头、11-新型陶瓷膜、12-第一密封圈、13-第二密封圈、14-清洁口、21-第三密封圈、22-出水口、31-第三密封圈、32-出水口。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明作进一步地详细描述。
实施例1：
材料：羟乙基纤维素(购自Sigma，粘度80-125cp)，丙酮(购自Sigma，浓度99.5％)，聚乙二醇(购自Merck，Mw-285-315Da)，Dolapix(购自Merck，CE 64)，正磷酸(购自Merck)，氢氧化钙(购自Merck)，盐酸(HCl，化学纯)，氢氧化钠(NaOH，化学纯)，以下试验所需材料，若无特殊说明，来源均为市售。
步骤一、将摩尔比为1.67的Ca(OH)2，和H3PO4混合均匀，通过湿式化学沉淀法制备HAP粉末，在合成期间保持反应环境为pH11-12，然后将合成的HAP在80℃下烘箱干燥并在800℃下煅烧，之后将HAP粉末化并保存以供进一步使用。
步骤二、制备新型链式化合物。具体地，向60ml 1,2-丙二醇中加入3.25mL，31mmol，6当量的氯化亚砜，0℃反应20分钟；向混合物中加入20mmol L-Gln，室温下置于磁力搅拌器中搅拌178小时，取产物进行薄层层析，验证表明氨基酸完全吸收，获得了一种新型链式化合物，结构式为
步骤三、用Dolapix(1.5wt％)将步骤一制备的HAP粉末(4wt％)分散在水(33wt％)中，之后加入聚乙二醇(5wt％)及羟乙基纤维素(5wt％)，将上述溶液搅拌至无气泡获得溶液一，将上述溶液一与等体积的新型链式化合物混合并干燥至粉末状态，将其风干过夜，与粘土、氧化铝、成孔剂、抗絮凝剂以质量比为65:20:12:3:1的比例在650℃下以3℃/min的加热速率烧结获得异型滤孔陶瓷膜。
步骤四、用沸水洗涤异型滤孔陶瓷膜，之后用丙酮洗涤异型滤孔陶瓷膜并超声处理，从孔道中除去油状和颗粒状物质，最后将异型滤孔陶瓷膜干燥并吹气以除去灰尘颗粒。
所述异型滤孔陶瓷膜如图1，所述异型滤孔陶瓷膜主体结构为多孔道类圆形支撑结构，孔道数量可以为5-9条，优选地为7条，所述孔道自上而下编号1-7，其中1,2,6,7号孔道为无阻隔孔道，每条孔道最高处内径为1mm，3,4,5号孔道每隔两个类圆形孔结构设置有一支撑结构。
实施例2：
以异型滤孔陶瓷膜为基础结构进行下一步制备，如图3所述，所述异型滤孔陶瓷膜为支撑层、在支撑层上还负载有过渡层以及膜分离层，具体地，将等质量比羟乙基纤维素和氧化石墨烯纤维在聚丙烯酰胺交联固化后沿异型滤孔陶瓷膜内壁延展，将异型滤孔陶瓷膜置于电弧炉烧结中，逐渐升温至880-900℃，烧制1.5h，然后再升温至920-1120℃，烧制0.5h，最后降温至850～870℃，保温2h，冷却，得到二级异型滤孔陶瓷膜；膜分离层为涂覆的纳米银离子(购自大连和建科技发展有限公司)，将纳米银离子通过聚丙烯酰胺交联固化在过渡层上，并于120℃保温3h，获得新型陶瓷膜。
实施例3：
为实现陶瓷膜的可置换性能及与其他净化原件的无缝对接，本发明还提供一种陶瓷膜过滤器，结构如图3所示，包括陶瓷膜本体1、第一可拆卸连接头2、第二可拆卸连接头3，所述陶瓷膜本体1包括新型陶瓷膜11、第一密封圈12、第二密封圈13、清洁口14，所述第一可拆卸连接头2包括第三密封圈21和出水口22，所述第二可拆卸连接头3包括第三密封圈31和出水口32。所述陶瓷膜本体1、第一可拆卸连接头2、第二可拆卸连接头3采用常规方式连接，包括但不限于螺纹连接，花键连接，过盈连接，铆接。
利用本实施例制得的陶瓷膜过滤器，进行化工污水小试实验，设每小时2.0kg通量的印染废水过滤；使用20分钟后，测量进出水的COD，结果表明陶瓷膜过滤器对有机物的去除率可达97.88％，原水盐分4.98％，出水可降至0.23％。过滤7天后，使用等比例无机盐及酒精溶液对陶瓷膜进行反冲洗，冲洗30m后，陶瓷膜恢复原色，并且检测表明表面基本无有机物残留，说明了陶瓷膜自清洁功能强，本发明提供的陶瓷膜过滤器有较高的过滤精度(过滤精度最高可达10纳米)和过滤速度，良好的清洗再生性能，适合于各种介质的精密过滤，陶瓷膜表面无毒、无味、具有良好的抗微生物侵蚀能力，除油率达95.12-97.88％，粒径大于0.5μm的悬浮物去除率达99％以上。
以上所揭露的仅为本发明较佳实施例而已，当然不能以此来限定本发明之权利范围，因此依本发明权利要求所作的等同变化，仍属本发明所涵盖的范围。
Claims (2)
1.一种新型陶瓷膜，其特征在于，所述陶瓷膜为多层结构，所述陶瓷膜包括支撑层，在支撑层上依次负载有过渡层和膜分离层，所述支撑层为一种异型滤孔陶瓷膜，所述异型滤孔陶瓷膜主体结构为多孔道类圆形支撑结构，孔道数量为7条，所述孔道自上而下编号1-7，其中1,2,6,7号孔道为无阻隔孔道，每条孔道最高处内径为1mm，3,4,5号孔道每隔两个类圆形孔结构设置有一支撑结构，所述异型滤孔陶瓷膜的制备方法为：
步骤一、将摩尔比为1.67的Ca(OH)2，和H3PO4混合均匀，通过湿式化学沉淀法制备HAP粉末，在合成期间保持反应环境为pH 11-12，然后将合成的HAP在80℃下烘箱干燥并在800℃下煅烧，之后将HAP粉末化并保存以供进一步使用；
步骤二、制备链式化合物，具体地，向60ml 1,2-丙二醇中加入3.25mL，31mmol，6当量的氯化亚砜，0℃反应20分钟；向混合物中加入20mmol L-Gln，室温下置于磁力搅拌器中搅拌178小时，取产物进行薄层层析，验证表明氨基酸完全吸收，获得了一种链式化合物，结构式为
步骤三、用Dolapix将步骤一制备的HAP粉末分散在水中，之后加入聚乙二醇及羟乙基纤维素，将上述溶液搅拌至无气泡获得溶液一，将上述溶液一与等体积的链式化合物混合并干燥至粉末状态，将其风干过夜，与粘土、氧化铝、成孔剂、抗絮凝剂以质量比为65:20:12:3:1的比例在650℃下以3℃/min的加热速率烧结获得异型滤孔陶瓷膜；
步骤四、用沸水洗涤异型滤孔陶瓷膜，之后用丙酮洗涤异型滤孔陶瓷膜并超声处理，从孔道中除去油状和颗粒状物质，最后将异型滤孔陶瓷膜干燥并吹气以除去灰尘颗粒。
2.根据权利要求1所述陶瓷膜，其特征在于，所述新型陶瓷膜的制备方法为，将等质量比羟乙基纤维素和氧化石墨烯纤维在聚丙烯酰胺交联固化后沿异型滤孔陶瓷膜内壁延展，将异型滤孔陶瓷膜置于电弧炉烧结中，逐渐升温至880-900℃，烧制1.5h，然后再升温至920-1120℃，烧制0.5h，最后降温至850～870℃，保温2h，冷却，得到二级异型滤孔陶瓷膜；膜分离层为涂覆的纳米银离子，将纳米银离子通过聚丙烯酰胺交联固化在过渡层上，并于120℃保温3h形成过滤层。
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