CN116219749A - 一种硼酸根离子表面印迹纤维、制备方法及其应用 - Google Patents
一种硼酸根离子表面印迹纤维、制备方法及其应用 Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 143
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229940063013 borate ion Drugs 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229920000098 polyolefin Polymers 0.000 claims abstract description 63
- 239000000178 monomer Substances 0.000 claims abstract description 44
- -1 borate ions Chemical class 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
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- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 claims description 6
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
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- MBBZMMPHUWSWHV-BDVNFPICSA-N N-methylglucamine Chemical compound CNC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO MBBZMMPHUWSWHV-BDVNFPICSA-N 0.000 claims description 2
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- DQJCDTNMLBYVAY-ZXXIYAEKSA-N (2S,5R,10R,13R)-16-{[(2R,3S,4R,5R)-3-{[(2S,3R,4R,5S,6R)-3-acetamido-4,5-dihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy}-5-(ethylamino)-6-hydroxy-2-(hydroxymethyl)oxan-4-yl]oxy}-5-(4-aminobutyl)-10-carbamoyl-2,13-dimethyl-4,7,12,15-tetraoxo-3,6,11,14-tetraazaheptadecan-1-oic acid Chemical compound NCCCC[C@H](C(=O)N[C@@H](C)C(O)=O)NC(=O)CC[C@H](C(N)=O)NC(=O)[C@@H](C)NC(=O)C(C)O[C@@H]1[C@@H](NCC)C(O)O[C@H](CO)[C@H]1O[C@H]1[C@H](NC(C)=O)[C@@H](O)[C@H](O)[C@@H](CO)O1 DQJCDTNMLBYVAY-ZXXIYAEKSA-N 0.000 claims 1
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 8
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
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- 238000011161 development Methods 0.000 description 3
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- 230000020477 pH reduction Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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Abstract
本发明公开了一种硼酸根离子表面印迹纤维、制备方法及其应用,属于吸附技术领域。所述硼酸根离子表面印迹纤维,以聚烯烃纤维为基体,在聚烯烃纤维表面接枝单体A,再由单体B的胺基与单体A的环氧基团发生开环反应相连进行功能化修饰,将功能化修饰后的产物配位负载硼酸根离子,继而与交联剂反应后洗除硼酸根离子,即得到硼酸根离子表面印迹纤维。所述单体A为含有不饱和的烯酸酯基及环氧基的酯类化合物;所述单体B为含有顺式邻位及间位双羟基官能团的分子。该硼酸根离子表面印迹纤维制备条件温和、工艺简单易操作、制备过程中不产生二次污染,适用于大规模生产。
Description
技术领域
本发明属于吸附技术领域,具体涉及一种硼酸根离子表面印迹纤维、制备方法及其应用。
背景技术
硼在玻璃、陶瓷、冶金、农业、医药、半导体、核工业等行业不可或缺,我国是工业用硼大国,但是由于储量和生产能力的限制,每年需要大量进口硼。
矿石和盐湖卤水硼资源丰富,但从矿石中提取硼的操作繁琐,需要经过粉碎、浮选、酸化和分离等步骤,不仅消耗大量化学试剂,还产生环境污染。我国盐湖卤水硼资源丰富,约占硼储量的40%,加强对盐湖卤水中硼资源的有效开发利用,既能降低开发难度满足市场需求,又有利于盐湖卤水资源的综合利用。工业上用于提硼的方法主要有酸化结晶法、沉淀法、溶剂萃取法、吸附法和膜分离法等,其中酸化结晶法是主流的提硼工艺。但是由于回收率较低,需与其他方法结合才能提高从盐湖卤水提硼的效率。同时,世界卫生组织规定饮用水和灌溉水中的硼质量浓度分别不能超过0.5mg/L和1.0mg/L,而工业提硼废水中的硼浓度通常都超过了此标准,若未经净化处理导致饮用水和灌溉水污染,因此需要进一步净化处理。
吸附法提硼是采用吸附剂从卤水中富集硼,再用洗脱剂将硼从树脂上洗脱,得到硼酸产品。吸附法具有吸附效率高、可再生利用和富集效果好等优点,在硼吸附,尤其是低浓度硼酸吸附方面研究较多。吸附剂主要有无机吸附剂和有机吸附剂两大类,常见的无机吸附剂包括金属氢氧化物、活性炭、纤维素衍生物、金属氧化物等,有机吸附剂则主要是离子交换树脂。但是现有的吸附剂在吸附量、吸附速率和吸附选择性等方面存在不足。同时,颗粒状树脂类吸附剂的再生过程比较长而且吸附量损失较大,亟需开发新型吸附材料。
发明内容
现有技术中硼吸附的吸附剂在吸附量、吸附速率和吸附选择性等方面存在不足,为解决该技术问题,本发明提供了一种硼酸根离子表面印迹纤维、制备方法及其应用,在有竞争离子存在的含硼废水中,实现选择性吸附分离含硼废水中的硼酸根离子。
为实现上述目的,本发明提供的技术方案是:
本发明提供了一种硼酸根离子表面印迹纤维,以聚烯烃纤维为基体,在聚烯烃纤维表面接枝单体A,再由单体B的胺基与单体A的环氧基团发生开环反应相连进行功能化修饰,将功能化修饰后的产物配位负载硼酸根离子,继而与交联剂反应后洗除硼酸根离子,即得到硼酸根离子表面印迹纤维。
所述聚烯烃纤维与单体A通过等离子体放电将单体A电离离解产生大量羟基自由基、过氧化物自由基等各类高活性物质,这些活性物质与单体A之间进行加成反应在基体表面形成聚合物相连;功能化修饰后的产物配位负载硼酸根离子与交联剂作用,通过产物与交联剂之间的双键加成反应,使分子之间产生化学键、并使线性分子相互连在一起,形成三维网状结构。
所述聚烯烃纤维为等规聚合物,具有高度结晶性,其平均分子量为18万-30万,一般分子量分布的多分散性系数为4-7,熔融指数为1100-2100g/min,且聚烯烃规度>95%。进一步地,所述聚烯烃纤维选自聚丙烯纤维、聚乙烯纤维、聚氯乙烯纤维、聚苯乙烯纤维等中的一种。
所述单体A为含有不饱和的烯酸酯基及环氧基的酯类化合物;进一步地,所述单体A为甲基丙烯酸缩水甘油酯(GMA)。
所述单体B为含有顺式邻位及间位双羟基官能团的分子,进一步地,所述单体B为葡糖胺(GLU)、葡甲胺(NMDG)、糖类、核苷(NUC)、儿茶酚胺(CA)、聚糖、糖蛋白(GP)、糖肽中的一种。
所述交联剂为多巴胺、苯胺、环氧氯丙烷、N,N-二甲基甲酰胺和戊二醛中的一种。
所述聚烯烃纤维、单体A、单体B、交联剂的质量比为:1:50-200:40-150:50-550。
本发明还提供了一种硼酸根离子表面印迹纤维的制备方法,以聚烯烃纤维为基体,采用低温射频放电等离子体聚合的方式将单体A聚合到聚烯烃纤维表面,得到改性聚烯烃纤维;将单体B与改性聚烯烃纤维上的环氧基团进行开环反应,得到功能化聚烯烃纤维;将功能化聚烯烃纤维配位负载硼酸根离子,继而与交联剂发生交联反应后洗除硼酸根离子,即得到硼酸根离子表面印迹纤维。
所述硼酸根离子表面印迹纤维的制备方法,具体包括如下步骤:
(1)将聚烯烃纤维在单体A改性溶液中充分浸渍,将浸渍后的聚烯烃纤维干燥处理后放入低温等离子体装置中,在单体气氛中正反辐照,使聚烯烃纤维与单体A充分发生等离子体聚合反应,待反应结束后将聚烯烃纤维再次置于单体A改性溶液中,在60-80℃下反应1-3h,得到改性聚烯烃纤维;
(2)将单体B溶于溶剂中,再加入步骤(1)中的改性聚烯烃纤维,在60-80℃下反应6-10h,结束反应后洗涤干燥得到功能化聚烯烃纤维;
(3)将步骤(2)中的功能化聚烯烃纤维置于硼酸根溶液中,使功能化聚烯烃纤维充分配位负载硼酸根离子后,在溶液中加入交联剂,在50-70℃温度下进行交联2-6h;交联反应结束后用碱性溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维。
所述步骤(1)中单体A改性溶液成分组成为单体A、水、乙醇、摩尔盐、H2SO4,其中摩尔盐、GMA、水、乙醇、H2SO4的质量比为1:10-30:10-30:30-50:0.1-1。
所述步骤(1)中单体气氛为氮气、氩气、氦气、二氧化碳、空气、氧气中的一种。
所述步骤(2)中溶剂为水、1,4-二氧六环、异丙醇、二甲基甲酰胺中的一种或两种混合。
本发明的另一方面是提供了如上所述硼酸根离子表面印迹纤维的应用,其中,将所述硼酸根离子表面印迹纤维应用于从含硼废水(如盐湖卤水和工业废水)中吸附提取硼酸根离子。表面印迹纤维经洗脱解吸后循环使用五次,其吸附性能还能达到最初吸附量的85%。
与现有技术相比本发明具有以下有益效果:
(1)以聚烯烃纤维为载体,采用等离子体聚合表面改性赋予其功能基团,结合等离子体聚合改性和表面印迹聚合制备硼酸根离子表面离子印迹纤维,利用基体优异的物化性质、综合两种技术的优点开发出新型的吸附材料,其具有吸附量高、循环使用寿命长、高度选择吸附硼等优点,特别适合含硼废水(盐湖卤水和工业废水)中吸附提取硼酸根离子,丰富含氧酸根阴离子的选择性吸附机理理论体系。
(2)该硼酸根离子表面印迹纤维制备条件温和、工艺简单易操作、制备过程中不产生二次污染,适用于大规模生产。
具体实施方式
为了更好的理解本发明内容,下面结合实施例进一步阐述本发明,但本发明的内容不仅仅限于下面的实施例。凡据本发明方法核心所作的等效变化或修饰,都应涵盖于本发明的保护范围之内。同时,在遵循本发明申请所述工艺参数范围的前提下,可根据各实施例以及其它合乎限定的工艺进行工艺参数调整。
实施例1
将0.1g的PP浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:20:15:40:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氩气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进15mL GMA溶液中,在70℃水浴中加热1h,得到改性聚烯烃纤维PP-g-GMA。将12g GLU溶于10mL纯水、40mL 1,4-二氧六环的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至70℃反应8h,得到功能化聚烯烃纤维PP-g-GMA-GLU。将PP-g-GMA-GLU纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-GLU纤维置于环氧氯丙烷交联剂溶液中,在60℃温度下进行交联4h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-GLU)。
实施例2
将0.1g的PP浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:25:15:35:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯空气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进15mL GMA溶液中,在60℃水浴中加热2h,得到改性聚烯烃纤维PP-g-GMA。将10g NMDG溶于10mL纯水、40mL 1,4-二氧六环的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至80℃反应7h,得到功能化聚烯烃纤维PP-g-GMA-NMDG。将PP-g-GMA-NMDG纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-NMDG纤维置于戊二醛交联剂溶液中,在60℃温度下进行交联3h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-NMDG)。
实施例3
将0.1g的PP浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:15:15:35:1:0.45。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氩气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进5mL GMA溶液中,在70℃水浴中加热3h,得到改性聚烯烃纤维PP-g-GMA。将12g葡萄糖溶于12mL纯水、38mL异丙醇的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至70℃反应8h,得到功能化聚烯烃纤维PP-g-GMA-GLU。将PP-g-GMA-GLU纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-GLU纤维置于环氧氯丙烷交联剂溶液中,在60℃温度下进行交联5h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-GLU)。
实施例4
将0.1g的PVC浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:20:20:35:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氩气氛中正反辐照210s。经等离子体聚合完毕后迅速把纤维放进10mL GMA溶液中,在70℃水浴中加热3h,得到改性聚烯烃纤维PP-g-GMA。将10g半乳糖溶于20mL纯水、30mL 1,4-二氧六环的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至60℃反应8h,得到功能化聚烯烃纤维PP-g-GMA-GAL。将PP-g-GMA-GAL纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-GAL纤维置于环氧氯丙烷交联剂溶液中,在70℃温度下进行交联5h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-GAL)。
实施例5
将0.1g的PVC浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:25:10:35:1:0.36。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氮气氛中正反辐照210s。经等离子体聚合完毕后迅速把纤维放进10mL GMA溶液中,在60℃水浴中加热2h,得到改性聚烯烃纤维PP-g-GMA。将15g NMDG溶于15mL纯水、35mL二甲基甲酰胺的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至80℃反应7h,得到功能化聚烯烃纤维PP-g-GMA-NMDG。将PP-g-GMA-NMDG纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-NMDG纤维置于戊二醛交联剂溶液中,在80℃温度下进行交联4h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-NMDG)。
实施例6
将0.1g的PE浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:20:20:31:1:0.36。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氧气氛中正反辐照150s。经等离子体聚合完毕后迅速把纤维放进20mL GMA溶液中,在60℃水浴中加热1h,得到改性聚烯烃纤维PP-g-GMA。将10g GLU溶于20mL纯水、30mL二甲基甲酰胺的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至80℃反应8h,得到功能化聚烯烃纤维PP-g-GMA-GLU。将PP-g-GMA-GLU纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-GLU纤维置于多巴胺交联剂溶液中,在60℃温度下进行交联5h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-GLU)。
实施例7
将0.1g的PE浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:25:15:35:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氦气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进20mL GMA溶液中,在70℃水浴中加热2h,得到改性聚烯烃纤维PP-g-GMA。将15g GLU溶于15mL纯水、35mL异丙醇的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至70℃反应10h,得到功能化聚烯烃纤维PP-g-GMA-GLU。将PP-g-GMA-GLU纤维置于100mg/L的硼酸根溶液中,在室温下充分振荡2h后,将充分配位后负载硼酸根离子的PP-g-GMA-GLU纤维置于N,N-二甲基甲酰胺交联剂溶液中,在70℃温度下进行交联6h。交联反应结束后用0.1mol/L的NaOH溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维I-(PP-g-GMA-GLU)。
对比例1
市售活性炭。
对比例2
对比例2是基于实施例2设定的,其不同之处在于未对功能化聚烯烃纤维进行后续硼酸根离子表面印迹聚合处理,其他条件均与实施例2一致。
将0.1g的PP浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:25:15:35:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯空气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进15mL GMA溶液中,在60℃水浴中加热2h,得到改性聚烯烃纤维PP-g-GMA。将10g NMDG溶于10mL纯水、40mL 1,4-二氧六环的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至80℃反应7h,得到功能化聚烯烃纤维PP-g-GMA-NMDG。
对比例3
对比例3是基于对比例2设定的,其不同之处在于未对功能化聚烯烃纤维进行后续硼酸根离子表面印迹聚合处理,其他条件均与实施例2一致。
将0.1g的PP浸泡在100mL含GMA、水、乙醇、摩尔盐、H2SO4溶液体系中浸泡24h,GMA、水、乙醇、摩尔盐、H2SO4的质量比为:25:15:35:1:0.3。浸泡过的PP纤维经晾干后放入低温等离子体装置中,在高纯氩气氛中正反辐照180s。经等离子体聚合完毕后迅速把纤维放进15mL GMA溶液中,在60℃水浴中加热2h,得到改性聚烯烃纤维PP-g-GMA。将10g聚乙烯亚胺(PEI)溶于10mL纯水、40mL 1,4-二氧六环的水溶液中,再加入PP-g-GMA。在机械搅拌下,水浴加热至80℃反应7h,得到功能化聚烯烃纤维PP-g-GMA-PEI。
应用实施例1
将实施例1-7及对比例1中的制备样品各0.01g置于10mL溶度为100mg/L的硼酸根溶液中,分别在0.5h、1h、2h和3h测试硼酸根溶液溶度,以此计算硼酸根离子表面印迹纤维对硼酸根的吸附性能,其中硼酸根溶液溶度的测试方法为电感耦合等离子体法(ICP),采用的仪器为电感耦合等离子体发射光谱仪(ICAP6300),其结果如下表1所示:
表1硼酸根离子吸附测试结果
0.5h | 1h | 2h | 3h | |
硼酸根吸附量mg/g | 硼酸根吸附量mg/g | 硼酸根吸附量mg/g | 硼酸根吸附量mg/g | |
实施例1 | 8.43 | 12.56 | 12.56 | 12.56 |
实施例2 | 10.33 | 15.42 | 15.42 | 15.42 |
实施例3 | 7.25 | 10.83 | 10.83 | 10.83 |
实施例4 | 6.93 | 10.16 | 10.16 | 10.16 |
实施例5 | 7.42 | 11.07 | 11.07 | 11.07 |
实施例6 | 8.38 | 12.51 | 12.51 | 12.51 |
实施例7 | 10.73 | 15.88 | 15.88 | 15.88 |
对比例1 | 0.67 | 1.24 | 2.07 | 2.07 |
通过以上实施例及对比例数据对比发现,在硼酸根离子系统中,实施例1-7在0-0.5h时吸附速率比较快,之后吸附速率逐渐下降,在60min左右均达到吸附平衡,最大吸附量达到15.88mg/g,而对比例1中硼吸附剂的吸附速率没有实施例中的快,且需要更长的时间才能达到吸附平衡,最终的吸附量也比实施例中的小。用该专利方法制备的硼吸附剂具有对硼酸根离子吸附速率快、吸附量大、且到达吸附平衡的时间短等优点,这些都是对比例1中的吸附剂达不到的效果。通过实例展现本方法制备的硼吸附剂在吸附量、吸附速率等方面具有一定的优势。
应用实施例2
将实施例2及对比例2-3中的制备样品各0.01g置于10mL含有B(OH)4 -,SO4 2-,Na+,K+,Mg+的各离子浓度均为100mg/L的多离子竞争溶液,2h后测试各样品对溶液中各离子的吸附量,以此计算硼酸根离子表面印迹纤维对硼酸根的选择性吸附能力,其中各离子含量测试方法为电感耦合等离子体法(ICP),采用的仪器为电感耦合等离子体发射光谱仪(ICAP6300)。
通过检测发现,实施例2制备的样品对B(OH)4 -,SO4 2-,Na+,K+,Mg+各离子吸附量分别占总吸附量的76.7%,3.5%,7%,6.8%,6%;而对比例2的样品对B(OH)4 -,SO4 2-,Na+,K+,Mg+各离子的吸附量分别占总吸附量的48.3%,13.2%,14.8%,10.9%,12.8%,对比例3的样品对B(OH)4 -,SO4 2-,Na+,K+,Mg+各离子的吸附量分别占总吸附量的29%,12.9%,20.3%,18.4%,19.4%;由上述结果可知实施例2对硼酸根具有吸附特异性功能,这是因为表面印迹聚合后得到的硼酸根离子表面印迹纤维对多种竞争离子存在的情况下对硼酸根有特异性吸附功能;而对比例3较对比例2对硼酸根特异性弱,这是因为对比例2在制备功能化聚烯烃纤维时引入了带双羟基官能团的NMDG,双羟基官能团有利于对硼酸根特异性吸附。
Claims (10)
1.一种硼酸根离子表面印迹纤维,其特征在于,以聚烯烃纤维为基体,在聚烯烃纤维表面接枝单体A,再由单体B的胺基与单体A的环氧基团发生开环反应相连进行功能化修饰,将功能化修饰后的产物配位负载硼酸根离子,继而与交联剂反应后洗除硼酸根离子,即得到硼酸根离子表面印迹纤维;
所述单体A为含有不饱和的烯酸酯基及环氧基的酯类化合物;
所述单体B为含有顺式邻位及间位双羟基官能团的分子;
所述聚烯烃纤维、单体A、单体B、交联剂的质量比为1:50-200:40-150:50-550。
2.根据权利要求1所述硼酸根离子表面印迹纤维,其特征在于,所述聚烯烃纤维为等规聚合物,其平均分子量为18万-30万。
3.根据权利要求1或2所述硼酸根离子表面印迹纤维,其特征在于,所述聚烯烃纤维选自聚丙烯纤维、聚乙烯纤维、聚氯乙烯纤维、聚苯乙烯纤维中的一种。
4.根据权利要求1所述硼酸根离子表面印迹纤维,其特征在于,所述单体A为甲基丙烯酸缩水甘油酯。
5.根据权利要求1所述硼酸根离子表面印迹纤维,其特征在于,所述单体B为葡糖胺、葡甲胺、糖类、核苷、儿茶酚胺、聚糖、糖蛋白、糖肽中的一种。
6.根据权利要求1所述硼酸根离子表面印迹纤维,其特征在于,所述交联剂为多巴胺、苯胺、环氧氯丙烷、N,N-二甲基甲酰胺和戊二醛中的一种。
7.权利要求1-6中任一项所述硼酸根离子表面印迹纤维的制备方法,其特征在于,具体包括如下步骤:
将聚烯烃纤维在单体A改性溶液中充分浸渍,将浸渍后的聚烯烃纤维干燥处理后放入低温等离子体装置中,在单体气氛中正反辐照,使聚烯烃纤维与单体A充分发生等离子体聚合反应,待反应结束后将聚烯烃纤维再次置于单体A改性溶液中,在60-80℃下反应1-3h,得到改性聚烯烃纤维;
将单体B溶于溶剂中,再加入步骤(1)中的改性聚烯烃纤维,在60-80℃下反应6-10h,结束反应后洗涤干燥得到功能化聚烯烃纤维;
将步骤(2)中的功能化聚烯烃纤维置于硼酸根溶液中,使功能化聚烯烃纤维充分配位负载硼酸根离子后,在溶液中加入交联剂,在50-70°C温度下进行交联2-6 h;交联反应结束后用碱性溶液洗脱除去硼酸根离子,得到硼酸根离子表面印迹纤维。
8.根据权利要求7所述硼酸根离子表面印迹纤维的制备方法,其特征在于,所述步骤(1)中单体A改性溶液成分组成为单体A、水、乙醇、摩尔盐、H2SO4,其中摩尔盐、GMA、水、乙醇、H2SO4的质量比为1:10-30:10-30:30-50:0.1-1。
9.根据权利要求7所述硼酸根离子表面印迹纤维的制备方法,其特征在于,所述步骤(1)中单体气氛为氮气、氩气、氦气、二氧化碳、空气、氧气中一种。
10.根据权利要求7所述硼酸根离子表面印迹纤维的制备方法,其特征在于,所述步骤(2)中溶剂为水、1,4-二氧六环、异丙醇、二甲基甲酰胺中的一种或两种混合。
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