CN106699997A - 一种磁性聚合物复合材料及其制备方法和应用 - Google Patents
一种磁性聚合物复合材料及其制备方法和应用 Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/26—Synthetic macromolecular compounds
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Abstract
本发明涉及一种磁性聚合物复合材料及其制备方法和应用,属于复合材料技术领域。本发明将磁性物质Fe3O4加入甲苯中,然后加入氨丙基三甲氧基硅烷,氮气保护条件下,回流反应得到产物A;将产物A放入乙腈中,加入3‑氯丙烯,氮气保护条件下,回流反应得到产物B;将产物B放入蒸馏水中,然后加入苯并‑18‑冠‑6‑醚‑丙烯酰胺和丙烯酸、再加入引发剂,在氮气保护条件下反应,然后反应产物离心分离烘干后得到磁性聚合物复合材料。本发明方法制备的磁性聚合物复合材料对铯离子有很高的吸附能力,且有很高的选择性,可广泛用于工业废水中铯离子的回收利用。
Description
技术领域
本发明涉及一种磁性聚合物复合材料及其制备方法和应用,属于复合材料技术领域。
背景技术
铯是一种银色的金属,主要应用于电子、陶瓷、医药、核工业等领域,特别是在核工业中,放射性铯作为铀核裂变的产物之一,大量出现在核废水当中。铯具有38 个同位素,除了铯-133 为稳定同位素外,其余均为放射性同位素,特别是铯-137 危害巨大。目前核能作为一种清洁能源被越来越广泛的使用,从而会产生大量的低中放固体废物进入到生态系统中。铯不是动植物的必须组分,环境中的铯若通过食物链被植物、动物和人吸收,会对生物体产生巨大的危害。
为降低水环境中铯的生态风险,需要去除污水或地表水体中的铯。目前常规的水处理方法有物理、化学、生物法以及上述方法的组合处理方法。与传统的复杂工艺相比,吸附法具有工艺简单、处理效果稳定、价格相对低等优点。目前,还未研究出能有效吸附脱除水中污染物,且具有分散性好、吸附速率快、吸附效果好、且回收容易的特点的吸附剂。
发明内容
本发明的目的是提供一种磁性聚合物复合材料,其化学结构式为:
。
本发明的另一目的提供所述磁性聚合物复合材料的制备方法,具体包括以下步骤:
(1)将磁性物质Fe3O4加入甲苯中,然后加入氨丙基三甲氧基硅烷,氮气保护条件下,回流反应得到产物A,标记为APTMS- Fe3O4;
(2)将步骤(1)得到的产物A(APTMS- Fe3O4)放入乙腈中,加入3-氯丙烯,氮气保护条件下,回流反应得到产物B,标记为CP- Fe3O4;
(3)将步骤(2)得到的产物B(CP- Fe3O4)放入蒸馏水中,然后加入苯并-18-冠-6-醚-丙烯酰胺和丙烯酸,再加入引发剂,在氮气保护条件下反应,然后反应产物离心分离烘干后得到磁性聚合物复合材料,标记为BC-Fe3O4。
所述步骤(1)中甲苯与磁性Fe3O4的液固比mL:mg为5:1~15:1;
所述步骤(1)中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为1:1~3:1;
所述步骤(1)中回流反应的温度为60~80℃,回流反应时间为16~24h;
所述步骤(2)中乙腈与产物A(APTMS- Fe3O4)的液固比mL:mg为5:1~15:1;
所述步骤(2)中3-氯丙烯与产物A(APTMS- Fe3O4)的液固比mL:mg为2:1~4:1;
所述步骤(2)中回流反应的温度为60~80℃,回流反应时间为16~24h;
所述步骤(3)中蒸馏水与磁性Fe3O4的液固比mL:mg为5:1~15:1;
所述步骤(3)中苯并-18-冠-6-醚-丙烯酰胺参照文献Cation Binding Properties ofPolymethacrylamide Derivatives of Crown Ethersa,K. Yagi, J. A. Ruiz, M. C.Sanchez, Makromol. Chem. Rapid. Commun. 1980, 1, 263制备而得;
所述步骤(3)中苯并-18-冠-6-醚-丙烯酰胺与产物B(CP- Fe3O4)的液固比mL:mg为1:1~3:1;
所述步骤(3)中丙烯酸与产物B(CP- Fe3O4)的液固比mL:mg为3:1~9:1;
所述步骤(3)中引发剂与产物B的质量比为1:100~3:100;
所述步骤(3)中引发剂为偶氮二异丁脒盐酸盐、偶氮二异丁腈或偶氮二异庚腈;
所述步骤(3)中反应的温度为60~80℃,反应时间为8~12h;
本发明所述的磁性聚合物复合材料BC-Fe3O4可用作铯离子吸附剂。
本发明的有益效果:
(1)本发明的磁性聚合物复合材料对铯离子有很高的吸附能力,且有很高的选择性,可广泛用于工业废水中铯离子的回收利用;
(2)本发明的磁性聚合物复合材料制备方法简单,流程短,易于制备;
(3)本发明的磁性聚合物复合材料使用性好,方法操作简单,富集率高,易于实现。易与水溶液分离,对环境不造成二次污染,具有广泛的应用价值和经济价值。
附图说明
图1 为实施例1 制备的磁性聚合物复合材料的红外光谱图。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
苯并-18-冠-6-醚-丙烯酰胺制备:参照文献Cation Binding Properties ofPolymethacrylamide Derivatives of Crown Ethersa,K. Yagi, J. A. Ruiz, M. C.Sanchez, Makromol. Chem. Rapid. Commun. 1980, 1, 263,将4-硝基苯并-18-冠-6醚与丙烯酰氯加入到四氢呋喃中,并加入三乙胺,在40℃条件下反应2h,得到苯并-18-冠-6-醚-丙烯酰胺,产率为86%。
实施例1:一种磁性聚合物复合材料的制备方法,具体步骤如下:
(1)将磁性物质Fe3O4加入甲苯中,其中甲苯与磁性Fe3O4的液固比mL:mg为5:1;然后加入氨丙基三甲氧基硅烷,其中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为1:1;在温度为60℃、氮气保护条件下,回流反应16h得到产物A,标记为APTMS- Fe3O4;
(2)将步骤(1)得到的产物A(APTMS- Fe3O4)放入乙腈中,其中乙腈与产物A(APTMS-Fe3O4)的液固比mL:mg为5:1;加入3-氯丙烯,其中3-氯丙烯与产物A(APTMS- Fe3O4)的液固比mL:mg为2:1;在温度为60℃、氮气保护条件下,回流反应16h得到产物B,标记为CP- Fe3O4;
(3)将步骤(2)得到的产物B(CP- Fe3O4)放入蒸馏水中,其中蒸馏水与步骤(1)中的磁性物质Fe3O4液固比mL:mg为5:1;然后加入苯并-18-冠-6-醚-丙烯酰胺(苯并-18-冠-6-醚-丙烯酰胺与产物B(CP- Fe3O4)的液固比mL:mg为1:1)和丙烯酸(丙烯酸与产物B(CP- Fe3O4)的液固比mL:mg为3:1);再加入引发剂(引发剂为偶氮二异丁脒盐酸盐(V50),其中偶氮二异丁脒盐酸盐(V50)与产物B(CP- Fe3O4)的质量比为1:100);在温度为60℃、氮气保护条件下反应8h,然后反应产物离心分离烘干后得到磁性聚合物复合材料,标记为BC-Fe3O4,磁性聚合物复合材料的产率为95%。
本实施例制备得到的磁性聚合物复合材料的红外光谱见图1,从图1 中看到,样品在620cm-1处的吸收峰对应Fe-O的吸收峰,在3430 cm-1处的宽峰对应于-NH的吸收峰,在1110 cm-1处的峰对应于Si-O的吸收峰,1516cm-1处的峰对应于C=C的吸收峰,1695cm-1处的峰对应于-COOH的吸收峰,从而证明了磁性聚合物复合材料的成功合成。
对铯离子的吸附实验:分别配制离子浓度均为50mg/L的含有钠、钾、锂或铯离子的离子水溶液,取0.02 g 磁性聚合物复合材料(BC-Fe3O4)吸附剂分别投入10 ml含有钠、钾、锂或铯离子的离子水溶液中,震荡吸附1h,然后磁分离吸附剂,用原子吸收法分别测定上清液中剩余金属的离子浓度,其中钠离子浓度为48mg/L、钾离子浓度为34mg/L、锂离子浓度为46mg/L、铯离子浓度为 4mg/L,结果表明吸附剂对铯离子有较高的吸附率,对其他金属离子吸附能力非常弱,表明BC-Fe3O4对铯离子的选择性吸附效果较好。
实施例2:一种磁性聚合物复合材料的制备方法,具体步骤如下:
(1)将磁性物质Fe3O4加入甲苯中,其中甲苯与磁性Fe3O4的液固比mL:mg为10:1;然后加入氨丙基三甲氧基硅烷,其中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为2:1;在温度为70℃、氮气保护条件下,回流反应20h得到产物A,标记为APTMS- Fe3O4;
(2)将步骤(1)得到的产物A(APTMS- Fe3O4)放入乙腈中,其中乙腈与产物A(APTMS-Fe3O4)的液固比mL:mg为10:1;加入3-氯丙烯,其中3-氯丙烯与产物A(APTMS- Fe3O4)的液固比mL:mg为3:1;在温度为70℃、氮气保护条件下,回流反应20h得到产物B,标记为CP- Fe3O4;
(3)将步骤(2)得到的产物B(CP- Fe3O4)放入蒸馏水中,其中蒸馏水与步骤(1)中的磁性物质Fe3O4液固比mL:mg为10:1;然后加入苯并-18-冠-6-醚-丙烯酰胺(苯并-18-冠-6-醚-丙烯酰胺与产物B(CP- Fe3O4)的液固比mL:mg为2:1)和丙烯酸(丙烯酸与产物B(CP- Fe3O4)的液固比mL:mg为6:1);再加入引发剂(引发剂为偶氮二异丁腈,其中偶氮二异丁腈与产物B(CP- Fe3O4)的质量比为2:100);在温度为70℃、氮气保护条件下反应10h,然后反应产物离心分离烘干后得到磁性聚合物复合材料,标记为BC-Fe3O4,磁性聚合物复合材料的产率为92%。
对铯离子的吸附实验:分别配制离子浓度均为50mg/L的含有钠、钾、锂或铯离子的离子水溶液,取0.02 g 磁性聚合物复合材料(BC-Fe3O4)吸附剂分别投入10 ml含有钠、钾、锂或铯离子的离子水溶液中,震荡吸附1h,然后磁分离吸附剂,用原子吸收法分别测定上清液中剩余金属的离子浓度,其中钠离子浓度为46mg/L、钾离子浓度为33mg/L、锂离子浓度为45mg/L、铯离子浓度为 3mg/L,结果表明吸附剂对铯离子有较高的吸附率,对其他金属离子吸附能力非常弱,表明BC-Fe3O4对铯离子的选择性吸附效果较好。
实施例3:一种磁性聚合物复合材料的制备方法,具体步骤如下:
(1)将磁性物质Fe3O4加入甲苯中,其中甲苯与磁性Fe3O4的液固比mL:mg为12:1;然后加入氨丙基三甲氧基硅烷,其中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为3:2;在温度为75℃、氮气保护条件下,回流反应22h得到产物A,标记为APTMS- Fe3O4;
(2)将步骤(1)得到的产物A(APTMS- Fe3O4)放入乙腈中,其中乙腈与产物A(APTMS-Fe3O4)的液固比mL:mg为12:1;加入3-氯丙烯,其中3-氯丙烯与产物A(APTMS- Fe3O4)的液固比mL:mg为3:1;在温度为75℃、氮气保护条件下,回流反应22h得到产物B,标记为CP- Fe3O4;
(3)将步骤(2)得到的产物B(CP- Fe3O4)放入蒸馏水中,其中蒸馏水与步骤(1)中的磁性物质Fe3O4液固比mL:mg为12:1;然后加入苯并-18-冠-6-醚-丙烯酰胺(苯并-18-冠-6-醚-丙烯酰胺与产物B(CP- Fe3O4)的液固比mL:mg为3:2)和丙烯酸(丙烯酸与产物B(CP- Fe3O4)的液固比mL:mg为8:1);再加入引发剂(引发剂为偶氮二异庚腈,其中偶氮二异庚腈与产物B(CP- Fe3O4)的质量比为2:100);在温度为75℃、氮气保护条件下反应11h,然后反应产物离心分离烘干后得到磁性聚合物复合材料,标记为BC-Fe3O4,磁性聚合物复合材料的产率为94%。
对铯离子的吸附实验:分别配制离子浓度均为50mg/L的含有钠、钾、锂或铯离子的离子水溶液,取0.02 g 磁性聚合物复合材料(BC-Fe3O4)吸附剂分别投入10 ml含有钠、钾、锂或铯离子的离子水溶液中,震荡吸附1h,然后磁分离吸附剂,用原子吸收法分别测定上清液中剩余金属的离子浓度,其中钠离子浓度为45mg/L、钾离子浓度为31mg/L、锂离子浓度为45mg/L、铯离子浓度为3mg/L,结果表明吸附剂对铯离子有较高的吸附率,对其他金属离子吸附能力非常弱,表明BC-Fe3O4对铯离子的选择性吸附效果较好。
实施例4:一种磁性聚合物复合材料的制备方法,具体步骤如下:
(1)将磁性物质Fe3O4加入甲苯中,其中甲苯与磁性Fe3O4的液固比mL:mg为15:1;然后加入氨丙基三甲氧基硅烷,其中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为3:1;在温度为80℃、氮气保护条件下,回流反应24h得到产物A,标记为APTMS- Fe3O4;
(2)将步骤(1)得到的产物A(APTMS- Fe3O4)放入乙腈中,其中乙腈与产物A(APTMS-Fe3O4)的液固比mL:mg为15:1;加入3-氯丙烯,其中3-氯丙烯与产物A(APTMS- Fe3O4)的液固比mL:mg为4:1;在温度为80℃、氮气保护条件下,回流反应24h得到产物B,标记为CP- Fe3O4;
(3)将步骤(2)得到的产物B(CP- Fe3O4)放入蒸馏水中,其中蒸馏水与步骤(1)中的磁性物质Fe3O4液固比mL:mg为15:1;然后加入苯并-18-冠-6-醚-丙烯酰胺(苯并-18-冠-6-醚-丙烯酰胺与产物B(CP- Fe3O4)的液固比mL:mg为3:1)和丙烯酸(丙烯酸与产物B(CP- Fe3O4)的液固比mL:mg为9:1);再加入引发剂(引发剂为偶氮二异庚腈,其中偶氮二异庚腈与产物B(CP- Fe3O4)的质量比为3:100);在温度为80℃、氮气保护条件下反应12h,然后反应产物离心分离烘干后得到磁性聚合物复合材料,标记为BC-Fe3O4,磁性聚合物复合材料的产率为94%。
对铯离子的吸附实验:分别配制离子浓度均为50mg/L的含有钠、钾、锂或铯离子的离子水溶液,取0.02 g 磁性聚合物复合材料(BC-Fe3O4)吸附剂分别投入10 ml含有钠、钾、锂或铯离子的离子水溶液中,震荡吸附1h,然后磁分离吸附剂,用原子吸收法分别测定上清液中剩余金属的离子浓度,其中钠离子浓度为44mg/L、钾离子浓度为32mg/L、锂离子浓度为43mg/L、铯离子浓度为3mg/L,结果表明吸附剂对铯离子有较高的吸附率,对其他金属离子吸附能力非常弱,表明BC-Fe3O4对铯离子的选择性吸附效果较好。
Claims (15)
1.一种磁性聚合物复合材料,其特征在于,化学结构式为:
。
2.权利要求1所述磁性聚合物复合材料的制备方法,其特征在于,具体步骤如下:
(1)将磁性物质Fe3O4加入甲苯中,然后加入氨丙基三甲氧基硅烷,氮气保护条件下,回流反应得到产物A;
(2)将步骤(1)得到的产物A放入乙腈中,加入3-氯丙烯,氮气保护条件下,回流反应得到产物B;
(3)将步骤(2)得到的产物B放入蒸馏水中,然后加入苯并-18-冠-6-醚-丙烯酰胺和丙烯酸、再加入引发剂,在氮气保护条件下反应,然后反应产物离心分离烘干后得到磁性聚合物复合材料。
3.根据权利要求2所述磁性聚合物复合材料的制备方法,其特征在于:步骤(1)中甲苯与磁性Fe3O4的液固比mL:mg为5:1~15:1。
4.根据权利要求2或3所述磁性聚合物复合材料的制备方法,其特征在于:步骤(1)中氨丙基三甲氧基硅烷与磁性Fe3O4的液固比mL:mg为1:1~3:1。
5.根据权利要求4所述磁性聚合物复合材料的制备方法,其特征在于:步骤(1)中回流反应的温度为60~80℃,回流反应时间为16~24h。
6.根据权利要求2所述磁性聚合物复合材料的制备方法,其特征在于:步骤(2)中乙腈与产物A的液固比mL:mg为5:1~15:1。
7.根据权利要求2或6所述磁性聚合物复合材料的制备方法,其特征在于:步骤(2)中3-氯丙烯与产物A的液固比mL:mg为2:1~4:1。
8.根据权利要求7所述磁性聚合物复合材料的制备方法,其特征在于:步骤(2)中回流反应的温度为60~80℃,回流反应时间为16~24h。
9.根据权利要求2所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中蒸馏水与Fe3O4的液固比mL:mg为5:1~15:1。
10.根据权利要求9所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中苯并-18-冠-6-醚-丙烯酰胺与产物B的液固比mL:mg为1:1~3:1。
11.根据权利要求9或10所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中丙烯酸与产物B的液固比mL:mg为3:1~9:1。
12.根据权利要求11所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中引发剂与产物B的质量比为1:100~3:100。
13.根据权利要求1或12所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中引发剂为偶氮二异丁脒盐酸盐、偶氮二异丁腈或偶氮二异庚腈。
14.根据权利要求12所述磁性聚合物复合材料的制备方法,其特征在于:步骤(3)中反应的温度为60~80℃,反应时间为8~12h。
15.权利要求1所述磁性聚合物复合材料作为铯离子吸附剂的应用。
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