CN100478056C - 耐氧化复合反渗透膜 - Google Patents
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Abstract
本发明公开了一种耐氧化复合反渗透膜。它包括无纺布层和聚砜支撑层，其特点是：在聚砜支撑层上有一个用多元胺与改性多酰氯溶液、或用多元胺与均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液制备的聚酰胺层。本发明通过在聚砜支撑层上制备一个改性的聚酰胺层，提高了反渗透膜的耐氧化性能和抗有机污染的性能，延长了反渗透膜的使用寿命。本发明还具有易于制备和操作，脱盐率高及水通量大，清洗间隔周期长的特点。本发明不但可以应用于水处理过程中，还可为反渗透膜的应用拓展更广泛的领域。
Description
技术领域
本发明属于水处理领域，特别是一种用于水处理的反渗透膜。
背景技术
反渗透技术是在一定的压力作用下，借助于反渗透膜的选择截留作用将溶液中的溶质与溶剂分开的分离方法，它被广泛应用于污水处理以及液体的提纯与浓缩，其中最普遍的应用是在水处理工艺中，用反渗透技术将原水中的无机离子、细菌、病毒、有机物及胶体等杂质去除，以获得高质量的纯净水。但反渗透膜在净化水的过程中，也会被水中的一些有机物或者无机物污染，如原水中的无机离子、细菌、病毒、有机物及胶体等杂质会吸附在反渗透膜上，造成胶体颗粒污染和生化污染。使反渗透膜的水通量下降；另外普通的聚酰胺反渗透膜对氯很敏感，很低浓度的氯就会破坏膜的性能，让膜在很短的时间失去脱盐率。而目前的水源大多是受过污染的，还有些是经过处理后的废水，水源中含有大量的氧化性杀菌剂，因此现有的反渗透膜使用寿命很短，需要经常更换，既增加了运行费用，也降低了膜的运行效率。
发明内容
本发明的目的是，提供一种耐氧化复合反渗透膜。提高反渗透膜的耐氧化性能和抗有机污染的性能，延长反渗透膜的使用寿命。
本发明是这样实现的。耐氧化复合反渗透膜，包括无纺布层和聚砜支撑层，其特点是：在聚砜支撑层上有一个用多元胺与改性多酰氯溶液、或用多元胺与均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液制备的聚酰胺层。
上述的耐氧化复合反渗透膜中，所述的均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯5～100份和改性多酰氯0～95份混匀构成的酰基氯有机溶液；所述份为重量份。
前述的耐氧化复合反渗透膜中，均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯20～95份和改性多酰氯5～80份混匀构成的酰基氯有机溶液。
前述的耐氧化复合反渗透膜中，均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯30～80份和改性多酰氯20～70份混匀构成的酰基氯有机溶液。
前述的耐氧化复合反渗透膜中，改性多酰氯，是5-碘-间苯二甲酰氯、2-碘-对苯二甲酰氯、5-溴-间苯二甲酰氯或2-溴-对苯二甲酰氯。
前述的耐氧化复合反渗透膜中，将制备好的聚酰胺层，在浓度0.5-10％、pH为7.5～8.5的过硫酸盐溶液中，浸泡10～120分钟，然后烘干。
前述的耐氧化复合反渗透膜中，更好地是将制备好的聚酰胺层，在浓度0.5-3％、pH为7.5～8.5的过硫酸盐溶液中，浸泡10～120分钟，然后烘干。
前述的耐氧化复合反渗透膜中，所述的过硫酸盐，是过硫酸钾、过硫酸铵或过硫酸钠。
与现有技术比较，本发明通过在聚砜支撑层上制备一个改性的聚酰胺层，提高了反渗透膜的耐氧化性能和抗有机污染的性能，延长了反渗透膜的使用寿命。本发明还通过用过硫酸盐溶液对改性的聚酰胺层作进一步处理，使得复合反渗透膜的耐氯性能和抗污染性能更强。本发明还具有易于制备和操作，脱盐率高及水通量大，清洗间隔周期长的特点。本发明不但可以应用于水处理过程中，还可为反渗透膜的应用拓展更广泛的领域。
具体实施方式
下面的例子用于阐明本发明并不用于解释限制本发明的保护范围。
比较例1：现有技术制备的有无纺布层、聚砜支撑层和聚酰胺层的反渗透膜。
使用含有16％聚砜的DMF溶液组成的多孔聚砜支撑膜(即聚砜支撑层)，放入2.5％的间苯二胺(MPDA)溶液约1分钟。胺溶液均含有0.1wt％的十二烷基磺酸钠(SDBS)表面活性剂。经MDPA(A)浸泡后的支撑膜放在纸巾上用橡胶辊滚动去除正面及背面多余的溶液。然后将这种支撑层与均苯三甲酰氯(B)的有机溶液接触50秒，形成聚酰胺层，接着放入40℃～100℃烘箱中保持10分钟，形成聚酰胺复合反渗透膜。
用含氯化钠2000ppm的水溶液，pH为7.5，在225psi的条件下检测膜的初始性能，之后用2000ppmNaClO溶液浸泡30小时后再在上述条件下检测膜的性能，所得结果如下：膜的初始脱盐率为99.3％，水通量为24.8GFD，经过NaClO(次氯酸钠)氧化处理后其脱盐率为5.8％，水通量为562GFD。
实施例1-6
使用含有16％聚砜的DMF溶液组成的多孔聚砜支撑膜，放入2.5％的间苯二胺(MPDA)溶液约1分钟。胺溶液均含有0.1wt％的十二烷基磺酸钠(SDBS)表面活性剂。经MDPA浸泡后的支撑膜放在纸巾上用橡胶辊滚动去除正面及背面多余的溶液。以上步骤和多元胺的用量，与现有技术制备聚酰胺层的情况相同。然后将这种支撑层与表1中所列含有0.1％(wt/v％)的酰基氯(-COCl)有机溶液接触50秒，接着放入40℃烘箱中保持10分钟，形成聚酰胺层。取出后用浓度1％的过硫酸钾溶液，在磷酸钾缓冲溶液pH为8的时候处理30分钟。然后在140℃烘箱中保持5分钟，得到最终的复合反渗透膜。
用含氯化钠2000ppm的水溶液，pH为7.5，在225psi的条件下检测膜的初始性能，之后用2000ppmNaClO溶液浸泡30小时后再在上述条件下检测膜的性能，所得结果如表1。
表1实施例1--6
| 实施例 | 1 | 2 | 3 | 4 | 5 | 6 |
| 酰基氯的总浓度TMC占酰基氯的相对浓度(％)5-碘-间苯二甲酰氯(％)脱盐率(％)水通量(GFD)NaClO浸泡后脱盐率(％)水通量(GFD) | 0.1010098.620.597.341.2 | 0.1802099.32498.134.3 | 0.1703099.323.598.432.1 | 0.1505099.223.398.828.7 | 0.1406099.122.198.628.2 | 0.1307099.021.598.128.8 |
从表1可以看出，加入5-碘-间苯二甲酰氯，膜的脱盐率和水通量在NaClO浸泡后变化较小，膜的耐氧化能力明显提高。
实施例7
除用2-碘-对苯二甲酰氯苯代替5-碘-间苯二甲酰氯外，采用与实施例4相同的操作制备得到复合反渗透膜。然后采用与实施例4相同的测试方法，膜的初始脱盐率为99.1％，水通量为25.3GFD，经过NaClO氧化处理后其脱盐率为98.5％，水通量为33.4GFD。
实施例8
除用5-溴-间苯二甲酰氯代替5-碘-间苯二甲酰氯外，采用与实施例4相同的操作制备得到复合反渗透膜。然后采用与实施例4相同的测试方法，膜的初始脱盐率为98.7％，水通量为22.8GFD，经过NaClO氧化处理后其脱盐率为97.0％，水通量为34.4GFD。
实施例9
除用3-二氨基环己烷代替间苯二胺之外，采用与实施例4相同的操作制备得到复合反渗透膜。然后采用与实施例4相同的测试方法，膜的初始脱盐率为98.9％，水通量为26.8GFD，经过NaClO氧化处理后其脱盐率为96.1％，水通量为44.9GFD。
实施例10-15
除了过硫酸钾处理时间不同外，采用与实施例4相同的操作制备得到复合反渗透膜。然后采用与实施例4相同的测试方法，其结果见表2。
表2实施例10--15
| 实施例 | 10 | 11 | 12 | 13 | 14 | 15 |
| 过硫酸钾处理时间(min)脱盐率(％)水通量(GFD)NaClO浸泡后脱盐率(％)水通量(GFD) | 099.022.072.545.8 | 1099.221.898.628.3 | 2099.123.798.430.1 | 4099.224.398.729.7 | 8099.024.198.332.4 | 12099.025.598.235.8 |
从表2中可以看出，采用过硫酸钾进行处理后，膜的耐氧化性能有明显提高。
实施例16-21
除了过硫酸钾溶液浓度不同外，采用与实施例4相同的操作制备得到复合反渗透膜。然后采用与实施例4相同的测试方法，其结果见表3。
表3实施例16-21
| 实施例 | 16 | 17 | 18 | 19 | 20 | 21 |
| 过硫酸钾溶液浓度(％)脱盐率(％)水通量(GFD)NaClO浸泡后脱盐率(％)水通量(GFD) | 0.598.821.198.530.8 | 1.598.923.898.432.3 | 3.099.124.798.630.5 | 5.099.225.398.332.7 | 8.099.025.898.232.9 | 10.099.025.598.036.3 |
将表3与表2进行比较，可以看出，采用不同浓度的过硫酸钾进行处理，膜的耐氧化性能均可以提高，其中浓度0.5-3.0％效果最好。
Claims (8)
1、耐氧化复合反渗透膜，包括无纺布层和聚砜支撑层，其特征在于：在聚砜支撑层上有一个用多元胺与改性多酰氯或均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液制备的聚酰胺层。
2、根据权利要求1所述的耐氧化复合反渗透膜，其特征在于：所述的均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯5～100份和改性多酰氯0～95份混匀构成的酰基氯有机溶液；所述份为重量份。
3、根据权利要求2所述的耐氧化复合反渗透膜，其特征在于：所述的均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯20～95份和改性多酰氯5～80份混匀构成的酰基氯有机溶液。
4、根据权利要求3所述的耐氧化复合反渗透膜，其特征在于：所述的均苯三甲酰氯和改性多酰氯构成的酰基氯有机溶液，是用均苯三甲酰氯30～80份和改性多酰氯20～70份混匀构成的酰基氯有机溶液。
5、根据权利要求4所述的耐氧化复合反渗透膜，其特征在于：所述的改性多酰氯，是5-碘-间苯二甲酰氯、2-碘-对苯二甲酰氯、5-溴-间苯二甲酰氯或2-溴-对苯二甲酰氯。
6、根据权利要求1至5中任一权利要求所述的耐氧化复合反渗透膜，其特征在于：将制备好的聚酰胺层，在浓度0.5-10％、pH为7.5～8.5的过硫酸盐溶液中，浸泡10～120分钟，然后烘干。
7、根据权利要求6所述的耐氧化复合反渗透膜，其特征在于：将制备好的聚酰胺层，在浓度0.5-3％、pH为7.5～8.5的过硫酸盐溶液中，浸泡10～120分钟，然后烘干。
8、根据权利要求7所述的耐氧化复合反渗透膜，其特征在于：所述的过硫酸盐，是过硫酸钾、过硫酸铵或过硫酸钠。
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| CNB2006100512005A CN100478056C (zh) | 2006-08-25 | 2006-08-25 | 耐氧化复合反渗透膜 |
| EP07114714A EP1894614A1 (en) | 2006-08-25 | 2007-08-21 | Oxidation-resistant composite reverse osmosis membrane |
| PCT/CN2007/002576 WO2008025259A1 (en) | 2006-08-25 | 2007-08-27 | Oxidation-resistant composite reverse osmosis membrane |
| KR1020070086147A KR100910899B1 (ko) | 2006-08-25 | 2007-08-27 | 내산화성 복합체 역삼투막 |
| US11/845,238 US20080203013A1 (en) | 2006-08-25 | 2007-08-27 | Oxidation-resistant composite reverse osmosis membrane |
| TW096131690A TWI368536B (en) | 2006-08-25 | 2007-08-27 | Oxidation-resistant composite reverse osmosis membrane |
| JP2007220441A JP2008100214A (ja) | 2006-08-25 | 2007-08-27 | 耐酸化性の複合逆浸透膜 |
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| CN109647224A (zh) * | 2018-12-28 | 2019-04-19 | 南京理工大学 | 耐氯聚酰胺复合反渗透膜及其制备方法 |
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| DE102009022513A1 (de) * | 2009-05-25 | 2010-12-02 | Qiagen Gmbh | Verfahren zum Schutz von Membranen |
| CN102527253A (zh) * | 2012-01-11 | 2012-07-04 | 杭州天创环境科技股份有限公司 | 一种抑菌抗氧化复合反渗透膜 |
| JP5923793B2 (ja) * | 2012-05-31 | 2016-05-25 | エルジー・ケム・リミテッド | カルボジイミド系化合物を含む高透過逆浸透膜及びこれを製造する方法 |
| KR101430066B1 (ko) * | 2012-10-30 | 2014-08-14 | 경희대학교 산학협력단 | 라디컬 그라프팅법을 이용한 역삼투막의 표면개질 방법 |
| CN103386263A (zh) * | 2013-08-06 | 2013-11-13 | 浙江理工大学 | 一种表面矿化的高亲水性复合反渗透膜 |
| JP6305729B2 (ja) * | 2013-11-05 | 2018-04-04 | 日東電工株式会社 | 複合半透膜 |
| US10384167B2 (en) | 2013-11-21 | 2019-08-20 | Oasys Water LLC | Systems and methods for improving performance of osmotically driven membrane systems |
| CN105080368B (zh) * | 2014-04-25 | 2017-05-31 | 中国石油化工股份有限公司 | 一种反渗透膜及其制备方法 |
| CN104437110B (zh) * | 2014-12-15 | 2016-09-28 | 湖南澳维环保科技有限公司 | 一种大通量聚酰胺复合膜 |
| JP6456671B2 (ja) * | 2014-12-16 | 2019-01-23 | 日東電工株式会社 | 多孔性支持体、複合半透膜、及びスパイラル型分離膜エレメント |
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| WO2008025259A1 (en) | 2008-03-06 |
| KR100910899B1 (ko) | 2009-08-05 |
| US20080203013A1 (en) | 2008-08-28 |
| TW200909044A (en) | 2009-03-01 |
| CN101130155A (zh) | 2008-02-27 |
| EP1894614A1 (en) | 2008-03-05 |
| JP2008100214A (ja) | 2008-05-01 |
| TWI368536B (en) | 2012-07-21 |
| KR20080018854A (ko) | 2008-02-28 |
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