CN105797593B - 一种渗透膜的制备方法 - Google Patents
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Classifications
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- B01D67/0081—After-treatment of organic or inorganic membranes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/445—Ion-selective electrodialysis with bipolar membranes; Water splitting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
发明名称：一种渗透膜的制备方法摘要：本发明涉及一种渗透膜的制备方法，将双极膜浸入三烯丙基异三聚氰酸酯，1‑乙烯基‑3‑丁基咪唑双三氟甲烷磺酰亚胺盐,1 4,5‑二氟‑2,2‑二(三氟甲基)‑1,3‑二氧杂环戊烯混合溶液中，经辐照接枝改性制得。
Description
技术领域
本发明涉及一种膜的制备方法，尤其是一种渗透膜的制备方法。
背景技术
膜分离技术的应用之一是对废酸废碱液进行回收处理。随着现代工业（钢铁、冶金、造纸等）的不断发展，生产过程产生的无机酸碱液也不断增加，例如金属矿的提取过程中使用了大量的碱性溶液，会产生大量含有金属酸根离子的废碱液。如果这些废碱液没有做适当的，不仅废液中的有用资源得不到合理的再利用，而且还会对环境和水源、生物造成非常严重的损害。因此如何对这些废酸废碱液进行经济有效的处理，是非常具有理论意义和应用价值的研究课题。研究者曾尝试了一些传统的处理方法（酸-碱中和、浓缩-燃烧、热降解、萃取、离子交换法等），但这些方法的处理效果都不理想，其缺陷在于：酸-碱中和需要耗费大量的酸或碱试剂；萃取方法需外加萃取剂，不但操作不便而且成本高；热降解能耗量较大，不经济；离子交换法与前面几种方法相比具有能耗低的优势，但其弊端在于该过程为间歇操作，运行一段时间后需要再生，且外界的条件（污染、溶胀和降解等）容易影响离子交换树脂运行的稳定性和寿命。所以，人们需要探寻一种既高效又经济环保的新型分离技术，经过长时间的探究，扩散渗析法膜分离技术成为研究者们关注的焦点。
CN103505892A公开了一种盐酸酸洗废液的蒸发浓缩装置，包括蒸发器和再沸器，盐酸酸洗废液在蒸发器中蒸发得到的气相物料，作为所述再沸器的热源。本发明的优点是将盐酸酸洗废液蒸发后的气相物料作为再沸器的热源，提高能源的利用率，减小换热器的换热面积，降低装置成本。
CN103508500A公开了一种盐酸酸洗废液的蒸发浓缩工艺，盐酸酸洗废液依次经过蒸发器和再沸器，所述盐酸酸洗废液在蒸发器中蒸发得到的气相物料，作为再沸器的热源，气相物料的温度为200～300℃。本发明的优点是将盐酸酸洗废液蒸发后的气相物料作为再沸器的热源，工艺过程简单，提高能源的利用率，使每吨废水的蒸发处理直接费用在20元以下，有效控制成本。
现有技术中的盐酸提浓技术以蒸发，蒸馏，萃取蒸馏为主，具有能耗高，流程长的缺点，而电渗析方法只能将1-5%（wt%）的稀盐酸浓缩到10%（wt%）左右的盐酸，现有扩散渗析法以及涉及膜的渗透浓缩技术只能浓缩到10%（wt%）左右的盐酸，不能再进一步提浓。
发明内容
本发明目的在于解决现有技术中存在的上述技术问题，提供一种渗透膜的制备方法。其特征在于制备步骤包括：
按重量份计，将100份双极膜用5-10份丙酮清洗表面，干燥，干膜浸埋在1000-2000份三烯丙基异三聚氰酸酯，0.1-0.5份1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,1-5份4, 5-二氟-2,2-二(三氟甲基)-1,3-二氧杂环戊烯混合溶液中，N2保护，用60Coγ射线照射剂量为10-50kGy左右，辐照时间10-60分钟，将接枝膜取出，用1000-2000份甲苯清洗膜的表面，干燥，并将改性后双极膜阳膜，双极膜阴膜复合使用，即得到可用于盐酸提浓的渗透膜。
所述的双极膜为市售产品，如北京廷润膜技术开发有限公司生产的产品；所述的4,5-二氟-2,2-二(三氟甲基)-1,3-二氧杂环戊烯为市售产品，如杭州安嘉睿化工有限公司生产的产品；所述的1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐为市售产品，如中科院兰州化学物理研究所研制的产品。
所述的三烯丙基异三聚氰酸酯，丙酮，甲苯为市售产品。
本发明由于采用了上述技术方案，具有以下有益效果：
双极膜经过三烯丙基异三聚氰酸酯，1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐，4, 5-二氟-2,2-二(三氟甲基)-1,3-二氧杂环戊烯的接枝改性，复合使用，对盐酸的渗透性能得到提高，1-5%（wt%）的稀盐酸可以浓缩到可以得到质量百分比浓度高于20%的盐酸。
具体实施方式
以下实例仅仅是进一步说明本发明，并不是限制本发明保护的范围。
实施例1
在2000L反应釜中，将100Kg双极膜用8Kg丙酮清洗表面，干燥，干膜浸埋在1500Kg三烯丙基异三聚氰酸酯，0.3Kg1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,3Kg4,5-二氟-2, 2-二(三氟甲基)-1,3-二氧杂环戊烯混合溶液中，N2保护，用60Coγ射线照射剂量为30kGy 左右，辐照时间40分钟，将接枝膜取出，用1500Kg甲苯清洗膜的表面，干燥，并将改性后双极膜阳膜，双极膜阴膜复合使用，即得到可用于盐酸提浓的渗透膜。产品编号B-1。
实施例2
在2000L反应釜中，将100Kg双极膜用5Kg丙酮清洗表面，干燥，干膜浸埋在1000Kg三烯丙基异三聚氰酸酯，0.1Kg1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,1Kg4,5-二氟-2, 2-二(三氟甲基)-1,3-二氧杂环戊烯混合溶液中，N2保护，用60Coγ射线照射剂量为10kGy 左右，辐照时间10分钟，将接枝膜取出，用1000Kg甲苯清洗膜的表面，干燥，并将改性后双极膜阳膜，双极膜阴膜复合使用，即得到可用于盐酸提浓的渗透膜。产品编号B-2。
实施例3
在3000L反应釜中，将100Kg双极膜用10Kg丙酮清洗表面，干燥，干膜浸埋在2000Kg三烯丙基异三聚氰酸酯，0.5Kg1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,5Kg4,5-二氟-2, 2-二(三氟甲基)-1,3-二氧杂环戊烯混合溶液中，N2保护，用60Coγ射线照射剂量为50kGy 左右，辐照时间60分钟，将接枝膜取出，用2000Kg甲苯清洗膜的表面，干燥，并将改性后双极膜阳膜，双极膜阴膜复合使用，即得到可用于盐酸提浓的渗透膜。产品编号B-3。
比较例1三烯丙基异三聚氰酸不加入，其它同实施例1，产品编号B-4。
比较例21-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐不加入，其它同实施例1，产品编号B-5。
比较例3
4,5-二氟-2,2-二(三氟甲基)-1,3-二氧杂环戊烯不加入，其它同实施例1，产品编号B- 6。
比较例4
采用未处理的50Kg双极膜阳膜，50kg双极膜阴膜作为渗透膜，产品编号B-7。
实施例4
质量百分比浓度为5的盐酸放入带有温度控制和电磁搅拌的溶剂为2L的不锈钢渗透池，原料液约400m1．实施例1-3以及比较例1-4制得的的渗透膜共3层在渗透池中均布，在料液中充分浸泡后置于池内,最外层膜下侧压力保持在50Pa，透过物用液氮冷凝收集。采用酸碱滴定法分析原料液及透过液的组成，浓缩后的盐酸浓度见下表：
见下表：
以上仅为本发明的具体实施例，但本发明的技术特征并不局限于此。任何以本发明为基础，为解决基本相同的技术问题，实现基本相同的技术效果，所作出的简单变化、等同替换或者修饰等，皆涵盖于本发明的保护范围之中。
Claims (1)
1.一种渗透膜的制备方法，其特征在于包括以下步骤：
按重量份计，将100份双极膜用5-10份丙酮清洗表面，干燥，干膜浸埋在1000-2000份三烯丙基异三聚氰酸酯，0.1-0.5份1-乙烯基-3-丁基咪唑双三氟甲烷磺酰亚胺盐,1-5份4,5-二氟-2,2-二(三氟甲基)-1,3-二氧杂环戊烯混合溶液中，N2保护，用60Coγ射线照射剂量为10-50kGy，辐照时间10-60分钟，将接枝膜取出，用1000-2000份甲苯清洗膜的表面，干燥，并将改性后双极膜阳膜，双极膜阴膜复合使用，即得到可用于盐酸提浓的渗透膜。
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| US5317035A (en) * | 1990-12-21 | 1994-05-31 | Amoco Corporation | Oriented polymeric microporous films |
| CN1114237A (zh) * | 1994-06-20 | 1996-01-03 | 中国科学院化学研究所 | 聚丙烯微孔膜为基膜的离子交换膜及其制法 |
| CN103804707A (zh) * | 2012-11-09 | 2014-05-21 | 张忠德 | 一种制备用于制备离子交换膜的基膜的方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5317035A (en) * | 1990-12-21 | 1994-05-31 | Amoco Corporation | Oriented polymeric microporous films |
| CN1114237A (zh) * | 1994-06-20 | 1996-01-03 | 中国科学院化学研究所 | 聚丙烯微孔膜为基膜的离子交换膜及其制法 |
| CN103804707A (zh) * | 2012-11-09 | 2014-05-21 | 张忠德 | 一种制备用于制备离子交换膜的基膜的方法 |
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