CN116870710A - 一种基于胺单体性质差异制备疏松反渗透膜的方法 - Google Patents
一种基于胺单体性质差异制备疏松反渗透膜的方法 Download PDFInfo
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- 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 description 3
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- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 2
- JDTUPLBMGDDPJS-UHFFFAOYSA-N 2-methoxy-2-phenylethanol Chemical compound COC(CO)C1=CC=CC=C1 JDTUPLBMGDDPJS-UHFFFAOYSA-N 0.000 claims description 2
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- FDQSRULYDNDXQB-UHFFFAOYSA-N benzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC(C(Cl)=O)=C1 FDQSRULYDNDXQB-UHFFFAOYSA-N 0.000 claims description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
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- AASBQTIDAQOQAV-UHFFFAOYSA-N cyclobutane-1,2,3,4-tetracarbonyl chloride Chemical compound ClC(=O)C1C(C(Cl)=O)C(C(Cl)=O)C1C(Cl)=O AASBQTIDAQOQAV-UHFFFAOYSA-N 0.000 claims description 2
- FEUMMORSWUHIPB-UHFFFAOYSA-N cyclohexane-1,2,4,5-tetracarbonyl chloride Chemical compound ClC(=O)C1CC(C(Cl)=O)C(C(Cl)=O)CC1C(Cl)=O FEUMMORSWUHIPB-UHFFFAOYSA-N 0.000 claims description 2
- WMPOZLHMGVKUEJ-UHFFFAOYSA-N decanedioyl dichloride Chemical compound ClC(=O)CCCCCCCCC(Cl)=O WMPOZLHMGVKUEJ-UHFFFAOYSA-N 0.000 claims description 2
- KNPWRSVXYPZCOS-UHFFFAOYSA-N formic acid;piperidine Chemical compound [O-]C=O.C1CC[NH2+]CC1 KNPWRSVXYPZCOS-UHFFFAOYSA-N 0.000 claims description 2
- 150000004676 glycans Chemical class 0.000 claims description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 2
- 125000000468 ketone group Chemical group 0.000 claims description 2
- 239000012621 metal-organic framework Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 claims description 2
- YVOFTMXWTWHRBH-UHFFFAOYSA-N pentanedioyl dichloride Chemical compound ClC(=O)CCCC(Cl)=O YVOFTMXWTWHRBH-UHFFFAOYSA-N 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 229920001282 polysaccharide Polymers 0.000 claims description 2
- 239000005017 polysaccharide Substances 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- SXYFKXOFMCIXQW-UHFFFAOYSA-N propanedioyl dichloride Chemical compound ClC(=O)CC(Cl)=O SXYFKXOFMCIXQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- LXEJRKJRKIFVNY-UHFFFAOYSA-N terephthaloyl chloride Chemical compound ClC(=O)C1=CC=C(C(Cl)=O)C=C1 LXEJRKJRKIFVNY-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 4
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- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 abstract 5
- 125000001240 enamine group Chemical group 0.000 abstract 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 abstract 2
- 239000012071 phase Substances 0.000 abstract 2
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 abstract 2
- 239000006227 byproduct Substances 0.000 abstract 1
- 230000035699 permeability Effects 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 150000003335 secondary amines Chemical class 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 3
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- 238000010612 desalination reaction Methods 0.000 description 2
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- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- B01D61/025—Reverse osmosis; Hyperfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
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- 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
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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Abstract
本发明提出了一种利用水相单体伯胺与仲胺之间的性质差异制备高渗透性反渗透膜的方法。通过在水相中加入仲胺和能与之形成可逆烯胺结构的醛或酮类添加剂对仲胺先进行固定,再加入小分子伯胺作为水相单体。发生界面聚合时,伯胺单体先与有机相单体发生反应生成致密的分离层,并释放出副产物氢离子,被固定的具有烯胺结构的仲胺单体在氢离子环境下被释放出来,继续与有机相单体反应,形成具有疏松结构的分离层。本发明采用简单的方法制备了较为疏松的反渗透膜,为调控界面聚合过程提供了新的思路。
Description
技术领域
本发明涉及一种疏松的反渗透膜的制备方法,适用于家用净水、硬水软化等领域。
背景技术
反渗透(RO)技术是一种是利用渗透压力差为驱动力的膜分离过滤技术,其核心关键就是反渗透膜。作为分离精度最高的水处理膜,反渗透膜几乎可以去除水中所有盐离子,仅对分子量小于100Da且不带电荷的溶质有部分透过性。因此,常规的反渗透膜往往应用于海水淡化、苦咸水脱盐等领域。然而,反渗透膜的通量与选择性之间存在背反效应,即高选择性的膜,通常通量较低,反之亦然。因此,传统的反渗透膜并不适用于一些不需要超高盐截留率,而需要较高渗透性的应用领域,例如家用净水、硬水软化等。
反渗透膜通量较低的原因主要是纯芳香型间苯二胺-均苯三甲酰氯基的聚酰胺分子链紧密排列,导致膜结构致密。因此,引入一些传统的脂肪族仲胺有望解决这一难题。然而,不同的胺单体的扩散速率不同,且在有机相中的溶解度也存在差异,采用多种胺单体制备反渗透膜的结构不可控,寻找一种合适的可以控制不同胺单体的扩散速度的方法,从而有效调控反渗透的微观结构,具有巨大的应用价值和经济效益。
发明内容
本发明通过醛或酮添加剂与水相单体中的仲胺之间的可逆烯胺反应固定了仲胺单体,使其不能直接参与界面聚合反应,从而控制了不同胺单体在同一界面聚合体系下的扩散速率,进而制备出了疏松的反渗透膜。该方法适用范围广,易于放大。通过调控分离层的微观结构,有效提升了反渗透膜的渗透性能。
本发明的技术方案概述如下:
1.一种基于胺单体性质差异制备疏松反渗透膜的方法,包括采用涂覆或浸泡的方式使含有两类水相单体和添加剂的水相溶液进入多孔支撑膜的孔中,再使其与含有酰氯单体的有机相溶液进行界面聚合反应,形成反渗透膜。
2.根据权利要求1所述的疏松反渗透膜的制备方法,其特征是,当形成反渗透膜后,还包括以下步骤:以有机溶剂清洗反渗透膜表面10-120s后,置于40-80℃热处理30s-10min,得到反渗透膜。
3.根据权利要求1所述的疏松反渗透膜的制备方法,其特征是所用多孔支撑膜为聚砜、聚醚砜、聚丙烯腈、水解之后的聚丙烯腈、聚偏氟乙烯等基底膜材料。
4.根据权利要求1所述的反渗透膜的制备方法,其特征是,所述的水相溶液由两类胺单体、添加剂和水相溶剂组成;其中,一类胺单体为能与醛或酮形成可逆烯胺结构且形成的分离层相对疏松的脂肪族仲胺,例如哌嗪、甲级哌啶、二甲基哌啶、哌啶甲酸、吡咯烷等,另一类胺单体是制备传统的反渗透膜的间苯二胺、邻苯二胺、对苯二胺、联苯胺等芳香族伯胺;所述水相溶剂为水。
5.根据权利要求4所述的疏松反渗透膜的制备方法,其特征是所述的添加剂是包括醛基化或含有酮基的多糖、二氧化硅、碳量子点、MOF、分子筛等纳米材料或分子。
6.根据权利要求1所述的疏松反渗透膜制备方法,其特征是,所述有机相溶液由酰氯单体和有机溶剂组成;所述的酰氯单体为均苯三甲酰氯、间苯二甲酰氯、对苯二甲酰氯、环己三酰氯、1,2,3,4-环丁烷四羧酰氯、1,2,4,5-环己烷四甲酰氯、草酰氯、丙二酰氯、丁二酰氯、戊二酰氯、己二酰氯、壬二酰氯、癸二酰氯中的一种或几种混合;所述有机溶剂为正己烷、环己烷、环戊烷、正庚烷、正辛烷和异构烷烃中的一种或几种混合。
本发明具有以下优异效果:
利用伯胺与仲胺之间的性质差异,调控了不同胺单体在同一界面聚合体系下的扩散速率,从而制备出了疏松的反渗透膜。制备的疏松反渗透膜不仅具有优异的渗透性能,还具有优异的二价离子如Ca2+、Mg2+、SO4 2-脱除率,可用于水软化、家庭净水等领域。
具体实施方法
所用基底膜材料均为商品膜。
实施举例
(1)将1.0wt%的哌嗪和0.5wt%的醛基化葡聚糖(Mw=30000)加入到水中搅拌均匀,使其充分反应,随后加入2.0wt%的间苯二胺,搅拌使其溶解。
(2)将水溶液均匀倾倒在聚砜多孔支撑膜上,沉积2min,倒掉多余的溶液,利用风刀除去膜表面未结合的水相单体;
(3)将含有0.15wt%的均苯三甲酰氯的正己烷溶液均匀地分布于步骤(2)获得的膜表面,反应30s后倒掉溶液,用正己烷清洗膜表面15s;
(4)将步骤(3)制备的膜在置于60℃烘箱中热处理2min,得到反渗透膜。
利用高压平板膜装置在25℃,1.55MPa下进行膜分离能力测试,原料液为2000ppm的NaCl溶液,本实例中所制备的反渗透膜对氯化钠的截留率超过94%,通量为70Lm-2h-1。
可以看出,基于本方法制备的疏松反渗透膜具有极高的渗透性,可用于家用净水、硬水软化等领域。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (6)
1.一种基于胺单体性质差异制备疏松反渗透膜的方法,包括采用涂覆或浸泡的方式使含有两类水相单体和添加剂的水相溶液进入多孔支撑膜的孔中,再使其与含有酰氯单体的有机相溶液进行界面聚合反应,形成反渗透膜。
2.根据权利要求1所述的疏松反渗透膜的制备方法,其特征是,当形成反渗透膜后,还包括以下步骤:以有机溶剂清洗反渗透膜表面10-120s后,置于40-80℃热处理30s-10min,得到反渗透膜。
3.根据权利要求1所述的疏松反渗透膜的制备方法,其特征是所用多孔支撑膜为聚砜、聚醚砜、聚丙烯腈、水解之后的聚丙烯腈、聚偏氟乙烯等基底膜材料。
4.根据权利要求1所述的反渗透膜的制备方法,其特征是,所述的水相溶液由两类胺单体、添加剂和水相溶剂组成;其中,一类胺单体为能与醛或酮形成可逆烯胺结构且形成的分离层相对疏松的脂肪族仲胺,例如哌嗪、甲级哌啶、二甲基哌啶、哌啶甲酸、吡咯烷等,另一类胺单体是制备传统的反渗透膜的间苯二胺、邻苯二胺、对苯二胺、联苯胺等芳香族伯胺;所述水相溶剂为水。
5.根据权利要求4所述的疏松反渗透膜的制备方法,其特征是所述的添加剂是包括醛基化或含有酮基的多糖、二氧化硅、碳量子点、MOF、分子筛等纳米材料或分子。
6.根据权利要求1所述的疏松反渗透膜制备方法,其特征是,所述有机相溶液由酰氯单体和有机溶剂组成;所述的酰氯单体为均苯三甲酰氯、间苯二甲酰氯、对苯二甲酰氯、环己三酰氯、1,2,3,4-环丁烷四羧酰氯、1,2,4,5-环己烷四甲酰氯、草酰氯、丙二酰氯、丁二酰氯、戊二酰氯、己二酰氯、壬二酰氯、癸二酰氯中的一种或几种混合;所述有机溶剂为正己烷、环己烷、环戊烷、正庚烷、正辛烷和异构烷烃中的一种或几种混合。
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