CN111111448A - 一种低压复合纳滤膜 - Google Patents
一种低压复合纳滤膜 Download PDFInfo
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- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007864 aqueous solution Substances 0.000 claims abstract description 31
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims abstract description 24
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- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 1
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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
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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Abstract
Description
技术领域
本发明涉及一种可在较低操作压力下使用的水处理复合纳滤膜,特别涉及带负电荷的复杂有机溶质的去除,属于水处理分离膜材料领域。
背景技术
薄层复合纳滤膜是一种重要的水处理膜,可截留水中溶解的小分子有机物、多价金属盐等,常用在海水淡化、苦咸水淡化、污水处理、酒类及药品的提纯等领域。复合纳滤膜结构主要包括基膜和功能层两部分。基膜常为高聚物多孔膜,功能层通过均苯三甲酰氯(TMC)与哌嗪(PIP)在基膜表面的界面聚合而获得。通常功能层比较致密,操作压力为0.3~0.7Mpa,在苦咸水和海水脱盐应用中表现良好。然而随着污水处理需求的扩大,对可处理复杂污水的纳滤膜的需求越来越多。严重的膜污染和较高的操作压力,是制约这一技术广泛应用的桎梏。TMC-PIP聚酰胺纳滤膜表面较疏水,易与有机分子结合形成滤饼层,造成通量下降。且与TMC-间苯二胺体系制备的反渗透复合膜相比,其表面粗糙度低,不易涂覆亲水高分子物质以获得更高的亲水性。很多含有机污水同时含有无机盐,使用膜过滤这种复杂混合液时浓差极化效应非常明显,膜寿命和膜效率都大大衰减。且操作压力越高,污染速度越快。因此制备较低操作压下的电解质处理膜是一个迫切的行业需求。而获得只截留有机小分子,可允许无机盐类溶质通过的低压疏松纳滤膜更是受到广泛关注。此类膜在处理印染、纺织等领域的高盐、高有机物废水等领域具有广泛的应用前景。将无机盐和染料的混合物分开,实现溶质分别回收、再次利用,可节约生产成本节省能源,实现资源再利用。
本发明通过在哌嗪水溶液中大量添加磺酸基单胺配制混合水溶液,作为水相,与均苯三甲酰氯的有机溶液进行界面聚合,制备复合纳滤膜。水相溶液中,磺酸基单氨与哌嗪发生竞争反应,降低功能层交联密度,提高了膜孔尺寸,降低膜操作压力,亦即降低膜筛分效应。通过调整磺酸基单胺与哌嗪的摩尔比,控制纳滤膜的最低操作压。但在水溶液中,磺酸基单胺与哌嗪存在分子间相互作用,可以活化哌嗪的仲胺基团,使采用混合溶液制备的功能层比同等浓度纯哌嗪水溶液制备的功能层厚,且交联密度高。而且过量磺酸基单氨中的质子化氨基可以与氯离子作用,提高酰氯与哌嗪的反应速度,促进交联反应。同时膜表面引入大量SO3H基团,加强了膜截留中唐南效应的影响,增加高价阴离子盐或带负电荷有机物质的截留。总结果是获得对高价阴离子盐和带负电有机物截留效果更好的低压复合纳滤膜。此系列纳滤膜可高效脱除水中硫酸盐和磷酸盐等高价阴离子盐,并实现对阴离子染料与无机盐的混合水溶液的分馏。当磺酸基单胺与哌嗪在水溶液中的摩尔比为(2.5~3)∶1时,膜的最低操作压力为0.25Mpa,膜对硫酸镁的截留为98%以上;当磺酸基单胺与哌嗪在水溶液中的摩尔比为(60~75)∶1时,膜的最低操作压力为0.1Mpa,可实现多种阴离子染料与氯化钠混合溶液的分馏,截留染料而使大部分氯化钠通过,实现资源的回收利用。
发明内容
此发明的意义在于针对现有技术的不足,制备一种低压水处理复合膜。
本发明的技术方案概述如下:
1.一种低压复合纳滤膜,其特征在于复合膜由大比例磺酸基单胺与哌嗪混合水溶液作为水相原料与均苯三甲酰氯的有机溶液在支撑基膜表面通过界面聚合制备分离功能层而获得;
磺酸基单胺包括牛磺酸(I)、磺酸基苯胺(II)、磺基氨基苯甲酸(III)中的一种,其结构式为:
(II)结构中的SO3H基团为氨基的邻位或间位或对位的任一位置;
(HI)结构中的SO3H基团和COOH基团为氨基的邻位或间位或对位的任一组合位置;
均苯三甲酰氯(IV)和哌嗪(V)的结构式为:
2.根据权利要求书1所述的低压复合膜,磺酸基单胺与哌嗪在水溶液中的摩尔比为(2.5~3)∶1和/或(60~75)∶1,水相混合水溶液的总质量浓度为0.2~5wt%。
3.根据权利要求1和2所述的低压复合膜,所述有机溶剂为正己烷、60~90#石油醚或环己烷中的一种或几种的混合。
4.根据权利要求1和2所述的低压复合膜,所述支撑基膜为聚砜或聚醚砜的平板或中空纤维超滤膜。
5.一种低压复合纳滤膜,由磺酸基单胺与哌嗪混合水溶液作为水相原料与均苯三甲酰氯的有机溶液在支撑基膜表面通过界面聚合制备分离功能层而获得;方法为:按比例配制磺酸基单胺与哌嗪的混合水溶液,将超滤支撑基膜的待涂覆区域与混合水相溶液充分接触,使水相单体吸附于支撑基膜表面,除去多余水相溶液;将超滤支撑基膜吸附过水相单体的部分与均苯三甲酰氯的有机溶液充分接触,在所述基膜表面发生界面聚合反应,获得低压复合膜。
磺基单胺包括牛磺酸(I)、磺酸基苯胺(II)、磺基氨基苯甲酸(III)中的一种,其结构式为:
(II)结构中的SO3H基团为氨基的邻位或间位或对位的任一位置;
(III)结构中的SO3H基团和COOH基团氨基为的邻位或间位或对位的任一组合位置;
均苯三甲酰氯(IV)和哌嗪(V)的结构式为:
磺酸基单胺与哌嗪在水溶液中的摩尔比为(2.5~3)∶1和/或(60~75)∶1,水相混合水溶液的总质量浓度为0.2~5wt%。
根据权利要求1和2所述的低压复合膜,所述有机溶剂为正己烷、60~90#石油醚或环己烷中的一种或几种的混合。
根据权利要求1和2所述的低压复合膜,所述支撑基膜为聚砜或聚醚砜的平板或中空纤维超滤膜。
低压纳滤膜的制备
实施例1
将8mL 2wt%的牛磺酸水溶液与2mL 2wt%的哌嗪水溶液混合,倾注于聚砜平板膜表面,10min后去除过量的水溶液。将10mL 0.1wt%均苯三甲酰氯的正己烷溶液倾注于支撑膜表面,反应30s,弃去过量正己烷溶液,膜表面获得功能层。膜经去离子水清洗后,浸没于去离子水中保存。
实施例2
将0.0168g对磺基苯胺粉末与0.0032g哌嗪粉末溶于10mL去离子水中,配制混合水溶液。将水溶液注入内压聚醚砜中空纤维膜内部,10min后去除过量水溶液。将10mL0.1wt%均苯三甲酰氯的石油醚溶液注入聚醚砜中空纤维膜内部,反应40s,将溶液排出,膜获得内表面功能层。膜经去离子水清洗,置于去离子水中保存。
实施例3
将0.016g哌嗪溶于50mL 4.968wt%的2-磺基-4-氨基苯甲酸水溶液中。将外压聚砜中空纤维膜浸入水溶液中,10min后去除过量的水溶液。将聚醚砜中空纤维膜浸入50mL0.1wt%均苯三甲酰氯的环己烷溶液中,反应25s,将膜提出溶液,获得外表面功能层。膜经去离子水清洗后,置于去离子水中保存。
实施例4
将9.9mL 2wt%的牛磺酸水溶液与0.1mL 2wt%的哌嗪水溶液混合后倾注于聚醚砜平板膜表面,10min后去除过量的水溶液。将10mL 0.1wt%均苯三甲酰氯的正己烷溶液倾注于膜表面,反应30s,弃去过量正己烷溶液,膜表面获得功能层。膜经去离子水清洗后,置于去离子水中保存。
膜截流无机盐
实施例5
将实施例1中的复合膜放置于平板膜评价装置中,进料液为浓度2g/L的硫酸镁水溶液。操作压力0.25MPa,收集出料测的水样,记录每30分钟出料液的收集体积与电导率,经计算,测得膜的水通量为2.89L-1·m-2·h-1·bar-1,截留率为98.34%。
实施例6
将实施例2中的中空纤维复合膜放置于内压式中空纤维膜评价装置中,进料液为浓度2g/L的硫酸镁水溶液。操作压力0.25MPa,收集出料测的水样,记录每30分钟出料液的收集体积与电导率,经计算,测得膜的水通量为8.68L-1·m-2·h-1·bar-1,截留率为93.45%。
膜分馏染料与无机盐
实施例7
将实施例3中的复合膜放置于外压式中空纤维膜评价装置中,进料液为甲基蓝(0.1g/L)-氯化钠(2g/L)混合水溶液。操作压力0.1MPa,收集出料测的水样,记录每30分钟出料液的收集体积与UV-vis吸光度,经计算,测得膜水通量为18.22L-1·m-2·h-1·bar-1,甲基蓝和氯化钠的截留率分别为98.70%和6.38%。
实施例8
将实施例4中的复合膜放置于平板膜评价装置中,进料液为酸性铬蓝K(0.1g/L)-氯化钠(2g/L)混合水溶液。操作压力0.1MPa,收集出料测的水样,记录每30分钟出料液的收集体积与电导率,经计算,测得膜的水通量为20.52L-1·m-2·h-1·bar-1,酸性铬蓝K和氯化钠的截留率分别为97.57%和8.33%。
Claims (5)
2.根据权利要求书1所述的低压复合膜,磺酸基单胺与哌嗪在水溶液中的摩尔比为(2.5~3)∶1和/或(60~75)∶1,水相混合水溶液的总质量浓度为0.2~5wt%。
3.根据权利要求1和2所述的低压复合膜,所述有机溶剂为正己烷、60~90#石油醚或环己烷中的一种或几种的混合。
4.根据权利要求1和2所述的低压复合膜,所述支撑基膜为聚砜或聚醚砜的平板或中空纤维超滤膜。
5.一种低压复合纳滤膜,由大比例的磺酸基单胺与哌嗪混合水溶液作为水相原料与均苯三甲酰氯的有机溶液在支撑基膜表面通过界面聚合制备分离功能层而获得;方法为:按比例配制磺酸基单胺与哌嗪的混合水溶液,将超滤支撑基膜的待涂覆区域与混合水相溶液充分接触,使水相单体吸附于支撑基膜表面,除去多余水相溶液;将超滤支撑基膜吸附过水相单体的部分与均苯三甲酰氯的有机溶液充分接触,在所述基膜表面发生界面聚合反应,获得低压复合膜。
磺基单胺包括牛磺酸(I)、磺酸基苯胺(II)、磺基氨基苯甲酸(III)中的一种,其结构式为:
(II)结构中的SO3H基团为氨基的邻位或间位或对位的任一位置;
(III)结构中的SO3H基团和COOH基团氨基为的邻位或间位或对位的任一组合位置;
均苯三甲酰氯(IV)和哌嗪(V)的结构式为:
磺酸基单胺与哌嗪在水溶液中的摩尔比为(2.5~3)∶1和/或(60~75)∶1,水相混合水溶液的总质量浓度为0.2~5wt%。
根据权利要求1和2所述的低压复合膜,所述有机溶剂为正己烷、60~90#石油醚或环己烷中的一种或几种的混合。
根据权利要求1和2所述的低压复合膜,所述支撑基膜为聚砜或聚醚砜的平板或中空纤维超滤膜。
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