聚芳醚砜酮基分离膜在环丁砜溶液浓缩中应用
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摘要
有机物质的有效回收与再利用是工业废水处理中一个不可缺少的部分,膜法水处理技术受到越来越广泛的应用。含二氮杂萘酮结构的聚芳醚砜酮(PPESK)材料具有较高的玻璃化转变温度,良好的溶解性、机械性能和化学稳定性,是一类优良的分离膜制备材料。本文以含二氮杂萘酮结构PPESK为膜材料制备了不同类型的分离膜,分别对环丁砜水溶液进行分离浓缩尝试,为膜法浓缩技术在类似体系中应用进行了探索。
以PPESK为基膜,以TMC为油相单体,PIP与MPD分别为水相单体,采用界面聚合工艺制备复合膜,考察了PPESK超滤基膜、单体浓度、界面聚合时间等因素对复合膜性能的影响。在20℃、1.0MPa下,分别选用对1g·L~(-1)Na_2SO_4溶液截留率为96%的PPA/PPESK膜和对2g·L~(-1)KCl溶液截留率为94%的PA/PPESK膜对环丁砜水溶液进行分离截留尝试,它们对环丁砜的截留率分别达到64%、84%,对溶液中盐的截留率分别为72%、90%,渗透通量为16.8L·m~(-2)·h~(-1)和6.5L·m~(-2)·h~(-1)。选取两种复合膜浸入100 g·L~(-1)环丁砜溶液中进行为期90天的静态浸泡考察表明PA/PPESK膜在环丁砜溶液中的稳定性更好。
采用PA/PPESK膜在静态平板膜测试仪中模拟膜法二级浓缩环丁砜浴液过程,将一级膜分离渗透液作为二级浓缩进料液,确定一级、二级浓缩比例分别为50%和90%,在50℃、1.5MPa下,浓度为10g·L~(-1)、电导率为2×10~3μS·cm~(-1)的环丁砜溶液经二级浓缩后,两级浓缩液环丁砜浓度分别为20g·L~(-1)和18.5g·L~(-1),二级浓缩渗透液环丁砜浓度约为0.2g·L~(-1),电导率约为0.01×10~3μS·cm~(-1)。PA/PPESK膜在24h连续分离20g·L~(-1)、电导率约为3×10~3μS·cm~(-1)的环丁砜浓缩液过程运行稳定。
将PPESK材料氯甲基化,采用相转化法制备CMPPESK非对称膜,再进行季铵化改性制备了QAPPESK纳滤膜,考察铸膜液溶剂与添加剂种类与含量、聚合物浓度、胺化试剂组成、胺化温度等工艺条件对膜性能的影响,优化工艺条件制制得QAPPESK纳滤膜在0.4MPa下对1 g·L~(-1)MgCl_2溶液的截留率可达93%,溶液渗透通量为15L·m~(-2)·h~(-1)。
选取QAPPESK纳滤膜进行环丁砜分离尝试,考察操作温度与压力对膜性能的影响,确定该膜分离环丁砜溶液的最佳条件是50℃、1.0MPa,在该条件下PPESK纳滤膜连续分离环丁砜溶液,发现当浓缩比例小于60%时,膜对环丁砜的截留率从44%增加到54%,渗透通量在14.8L·m~(-2)·h~(-1)至14L·m~(-2)·h~(-1),在此过程中膜运行平稳。对该类膜分离浓缩环丁砜的长期稳定性还需进一步探索。
The effective recycling and reuse of organic compounds have always been an indispensable part in wastewater treatment realm,the membrane separation techniques of treating industrial wastewater had been utilized on many application realms. Poly(phthalazinone ether sulfone ketone)(PPESK) is a novel membrane material for filtration membrane with high glass-transition temperature,good solubility,good mechanical performance and chemical stability,in this thesis a series of different membranes were made by PPESK material and were used to separate and concentrate a water sample containing sulfolanc and inorganic salts.This research provided a good reference of membrane separation wastewater treatment in similar solution system.
A series of poly(phthalazinone ether sulfone ketone) composite membranes were prepared by piperazine(PIP) and m-phenylenediamine(MPD) with trimesoylchloride(TMC) respectively through the interfacial polymerization technique on the poly(phthalazinone ether sulfone ether ketone)(PPESK) supporting membrane.The effect of the structure of substrate membrane,the content of monomer and the time of interfacial polymerization on the surface morphology and separation pcrformancc of the composite membrane were studied.A PPA/PPESK membrane with 96%rejection to 1g·L~(-1)Na_2SO_4 solution and a PA/PPESK membrane with 94%rejection to 2g·L~(-1)KCI solution were used to separate the sulfolane solution at 20℃and 1.0Mpa,the results showed that the rejections to the sulfolanc were respectively 64%and 84%,and the rejections to the salts solved in the solution were 72%and 90%,and the permeation flux were 16.8L·m~(-2)·h~(-1) and 6.5L·m~(-2)·h(-1).The PA/PPESK membrane had a better stability performance than the PPA/PPESK membrane when dipped into the 100 g·L~(-1) sulfolane solution with 90 day captive test.
A flat membrane test device was used to simulate the two-stage separation and concentration process using PA/PPESK membrane.The permeate solution of the first stage entered the second stage as a feed.It turned out that the suitable concentration ratio of the two stage separation was separately 50%and 90%.Under the condition of 50℃and 1.5MPa,the PA/PPESK membrane was used to separate the 10 g·L~(-1) sulfolane solution,
The result indicated that the contents of sulfolane in the two stage concentration solution were about 20g·L~(-1) and 18.5g·L~(-1) when the feed containing 10g·L~(-1) sulfolane and the conductivity was 2×10~3μS·cm~(-1),the second permeate had 0.2g·L~(-1) sulfolane content and the conductivity was 0.01×10~3μS·cm~(-1).The PA/PPESK membrane showed a good performance through a 24h constant separation opcration in the concentrated suifolane solution with a 20g·L~(-1) sulfolane content and 3×10~3μS·cm~(-1) conductivity. CMPPESK was acquired from PPESK through chloromethylation;CMPPESK asymmetric membrane was prepared form CMPPESK membrane material by phase inversion method. And quaternized poly(phthalazinone ether sulfone ketone)(QAPPESK) nanofiltration(NF) membranes were prepared from CMPPESK asymmetric membrane by quaternized modification.The effects of preparation conditions,such as the content and sorts of solvents and non-solvent additives,the concentration of polymer,the composition of quaternization reagent and the temperature of quaternization were investigated.QAPPESK NF membranes were obtained by optimal technology conditions,which had a rejection of 93%and 15L·m~(-2)·h~(-1) permeation flux to the 1g·L~(-1) MgCl_2 solution at 20℃and 0.4MPa.
A series of QAPPESK NF membranes were used to separate the sulfolane solution,the effects of the operation temperaturc and pressure were investigated.A constant separation trial to the sulfolane solution procecded at 50℃and 1.0MPa,it was found that the rejection to the sulfolane was from 44%to 54%and the permcation flux was from 14.8L·m~(-2)·h~(-1) to 14L·m~(-2)·h~(-1) when the concentration ratio was 60%below.In this course the performance of membrane was stable.The long time separating pertormancc of the QAPPESK NF mcmbrane in the sulfolane solution needs to be researched further.
以PPESK为基膜,以TMC为油相单体,PIP与MPD分别为水相单体,采用界面聚合工艺制备复合膜,考察了PPESK超滤基膜、单体浓度、界面聚合时间等因素对复合膜性能的影响。在20℃、1.0MPa下,分别选用对1g·L~(-1)Na_2SO_4溶液截留率为96%的PPA/PPESK膜和对2g·L~(-1)KCl溶液截留率为94%的PA/PPESK膜对环丁砜水溶液进行分离截留尝试,它们对环丁砜的截留率分别达到64%、84%,对溶液中盐的截留率分别为72%、90%,渗透通量为16.8L·m~(-2)·h~(-1)和6.5L·m~(-2)·h~(-1)。选取两种复合膜浸入100 g·L~(-1)环丁砜溶液中进行为期90天的静态浸泡考察表明PA/PPESK膜在环丁砜溶液中的稳定性更好。
采用PA/PPESK膜在静态平板膜测试仪中模拟膜法二级浓缩环丁砜浴液过程,将一级膜分离渗透液作为二级浓缩进料液,确定一级、二级浓缩比例分别为50%和90%,在50℃、1.5MPa下,浓度为10g·L~(-1)、电导率为2×10~3μS·cm~(-1)的环丁砜溶液经二级浓缩后,两级浓缩液环丁砜浓度分别为20g·L~(-1)和18.5g·L~(-1),二级浓缩渗透液环丁砜浓度约为0.2g·L~(-1),电导率约为0.01×10~3μS·cm~(-1)。PA/PPESK膜在24h连续分离20g·L~(-1)、电导率约为3×10~3μS·cm~(-1)的环丁砜浓缩液过程运行稳定。
将PPESK材料氯甲基化,采用相转化法制备CMPPESK非对称膜,再进行季铵化改性制备了QAPPESK纳滤膜,考察铸膜液溶剂与添加剂种类与含量、聚合物浓度、胺化试剂组成、胺化温度等工艺条件对膜性能的影响,优化工艺条件制制得QAPPESK纳滤膜在0.4MPa下对1 g·L~(-1)MgCl_2溶液的截留率可达93%,溶液渗透通量为15L·m~(-2)·h~(-1)。
选取QAPPESK纳滤膜进行环丁砜分离尝试,考察操作温度与压力对膜性能的影响,确定该膜分离环丁砜溶液的最佳条件是50℃、1.0MPa,在该条件下PPESK纳滤膜连续分离环丁砜溶液,发现当浓缩比例小于60%时,膜对环丁砜的截留率从44%增加到54%,渗透通量在14.8L·m~(-2)·h~(-1)至14L·m~(-2)·h~(-1),在此过程中膜运行平稳。对该类膜分离浓缩环丁砜的长期稳定性还需进一步探索。
The effective recycling and reuse of organic compounds have always been an indispensable part in wastewater treatment realm,the membrane separation techniques of treating industrial wastewater had been utilized on many application realms. Poly(phthalazinone ether sulfone ketone)(PPESK) is a novel membrane material for filtration membrane with high glass-transition temperature,good solubility,good mechanical performance and chemical stability,in this thesis a series of different membranes were made by PPESK material and were used to separate and concentrate a water sample containing sulfolanc and inorganic salts.This research provided a good reference of membrane separation wastewater treatment in similar solution system.
A series of poly(phthalazinone ether sulfone ketone) composite membranes were prepared by piperazine(PIP) and m-phenylenediamine(MPD) with trimesoylchloride(TMC) respectively through the interfacial polymerization technique on the poly(phthalazinone ether sulfone ether ketone)(PPESK) supporting membrane.The effect of the structure of substrate membrane,the content of monomer and the time of interfacial polymerization on the surface morphology and separation pcrformancc of the composite membrane were studied.A PPA/PPESK membrane with 96%rejection to 1g·L~(-1)Na_2SO_4 solution and a PA/PPESK membrane with 94%rejection to 2g·L~(-1)KCI solution were used to separate the sulfolane solution at 20℃and 1.0Mpa,the results showed that the rejections to the sulfolanc were respectively 64%and 84%,and the rejections to the salts solved in the solution were 72%and 90%,and the permeation flux were 16.8L·m~(-2)·h~(-1) and 6.5L·m~(-2)·h(-1).The PA/PPESK membrane had a better stability performance than the PPA/PPESK membrane when dipped into the 100 g·L~(-1) sulfolane solution with 90 day captive test.
A flat membrane test device was used to simulate the two-stage separation and concentration process using PA/PPESK membrane.The permeate solution of the first stage entered the second stage as a feed.It turned out that the suitable concentration ratio of the two stage separation was separately 50%and 90%.Under the condition of 50℃and 1.5MPa,the PA/PPESK membrane was used to separate the 10 g·L~(-1) sulfolane solution,
The result indicated that the contents of sulfolane in the two stage concentration solution were about 20g·L~(-1) and 18.5g·L~(-1) when the feed containing 10g·L~(-1) sulfolane and the conductivity was 2×10~3μS·cm~(-1),the second permeate had 0.2g·L~(-1) sulfolane content and the conductivity was 0.01×10~3μS·cm~(-1).The PA/PPESK membrane showed a good performance through a 24h constant separation opcration in the concentrated suifolane solution with a 20g·L~(-1) sulfolane content and 3×10~3μS·cm~(-1) conductivity. CMPPESK was acquired from PPESK through chloromethylation;CMPPESK asymmetric membrane was prepared form CMPPESK membrane material by phase inversion method. And quaternized poly(phthalazinone ether sulfone ketone)(QAPPESK) nanofiltration(NF) membranes were prepared from CMPPESK asymmetric membrane by quaternized modification.The effects of preparation conditions,such as the content and sorts of solvents and non-solvent additives,the concentration of polymer,the composition of quaternization reagent and the temperature of quaternization were investigated.QAPPESK NF membranes were obtained by optimal technology conditions,which had a rejection of 93%and 15L·m~(-2)·h~(-1) permeation flux to the 1g·L~(-1) MgCl_2 solution at 20℃and 0.4MPa.
A series of QAPPESK NF membranes were used to separate the sulfolane solution,the effects of the operation temperaturc and pressure were investigated.A constant separation trial to the sulfolane solution procecded at 50℃and 1.0MPa,it was found that the rejection to the sulfolane was from 44%to 54%and the permcation flux was from 14.8L·m~(-2)·h~(-1) to 14L·m~(-2)·h~(-1) when the concentration ratio was 60%below.In this course the performance of membrane was stable.The long time separating pertormancc of the QAPPESK NF mcmbrane in the sulfolane solution needs to be researched further.
引文
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