CN114984918A - 用水杨醛肟和Fe3+自组装制备海水提铀木头的制备方法 - Google Patents

用水杨醛肟和Fe3+自组装制备海水提铀木头的制备方法 Download PDF

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CN114984918A
CN114984918A CN202210655875.XA CN202210655875A CN114984918A CN 114984918 A CN114984918 A CN 114984918A CN 202210655875 A CN202210655875 A CN 202210655875A CN 114984918 A CN114984918 A CN 114984918A
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吴铭榜
李天昊
黄祥河
姚菊明
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Zhejiang Sci Tech University ZSTU
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Abstract

本发明公开了一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法。将天然木头通过预处理脱除木质素，在预处理液中高温条件下反应直到变白；清水洗涤后在水浴常温振荡浸渍到醛肟类溶液中，洗涤后水浴常温振荡浸渍到含三价铁离子的溶液中，多次自组装获得海水提铀木头。本发明制备成本低，操作过程简单，反应条件温和，耗能低。

Description

用水杨醛肟和Fe3+自组装制备海水提铀木头的制备方法
技术领域
本发明属于海水提铀领域的一种海水提铀木头的制备方法，涉及一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法。
背景技术
当今社会，随着科技的发展，人类对能源需求与日俱增，伴随着化石燃料的减少以及环境的恶化，发展可再生资源成为能源发展的必然趋势，核能作为清洁能源之一，正逐渐成为实现人类可持续发展的重要保障。
但是，铀红皮书数据显示，已探明的陆地铀矿储量约20万吨，铀资源相对较为贫乏，且铀矿品位不高，开采成本相对较高。洋中含有丰富的铀资源(约4.5×109t)，开发潜力巨大。但由于海水水量庞大，使得铀的浓度极低只有3.3ppb，这就导致了海水提铀的效率低下，极大的限制了核工业的发展。
目前，已开发出多种用于海水提铀的方法，包括吸附法、溶剂萃取分离法、化学沉淀法、生物处理法、离子交换法和超导磁分离法等。其中，吸附法由于制备简单、成本低、效率高的特点成为目前研究最多的方法之一。
公开号为CN112547026A的中国专利文献公开了一种铀吸附材料及其制备方法和在吸附回收海水中铀中的应用，铀吸附材料由非极性大孔树脂负载聚偕胺肟构成。该铀吸附材料利用大孔树脂的超高比表面积和孔隙率充分分散负载偕胺肟，能使偕胺肟的活性基团充分暴露，大大提高对海水中铀的吸附速率和吸附容量，将其应用与海水中的铀提取，具有对铀高选择性吸附，且吸附速率快，容量大，可循环使用，对海水耐受性好等特点，可以重复使用，特别适合海水中铀的富集提取。
公开号为CN113231038A的中国专利文献公开了一种用于海水提铀的半互穿网络水凝胶薄膜材料的制备方法，其特征在于，先按一定质量比将聚丙烯偕胺肟、单体、光引发剂和交联剂溶解在碱性水溶液中获得前驱液，后将前驱液注入到模具中在紫外线或者太阳光下聚合反应制得。本制备方法简单且快速，成本低，通过在碱性条件下的低能耗和环保阳光聚合可用于大规模制造PAO半互穿网络水凝胶薄膜材料。该材料厚度为0.2mm，微级孔径均匀，具有高吸附效率、高选择性、优异的力学性能且可多次重复使用。
公开号为CN109261134A的中国专利文献公开了一种物理与化学协同抗污损型海水提铀吸附剂及其制备方法。首先将二维碳基材料分散于甲醇中，加入化学抗污损剂和中心金属离子，超声处理；然后加入2-甲基咪唑甲醇溶液进行反应；接着将反应产物分别用无水乙醇和甲醇清洗并离心分离；最后进行干燥。本发明的吸附剂对三角褐指藻的抑制率可以达到90％以上，由于二维碳基材料和金属离子掺杂对咪唑酯骨架材料的协同作用，吸附剂饱和吸附量相对于纯的MOF和碳基材料可以提高120～150％，还同步提升了吸附剂整体吸附最佳PH条件，使其更趋向于海水环境，有助于提高吸附效率。
公开号为CN113046857A的中国专利文献公开了一种可自更新活性防污涂层的海水提铀吸附剂的制备方法。包括以下步骤：利用聚丙烯腈和六水合硝酸锌制备六水合硝酸锌-聚丙烯腈纺丝前体溶液；在一定条件下纺丝制备六水合硝酸锌-聚丙烯腈纤维；取六水合硝酸锌-聚丙烯腈纤维加入2-甲基咪唑溶液中反应获得2-甲基咪唑锌盐多孔配位聚合物-聚丙烯复合纤维；利用单宁酸使复合纤维交联获得交联化的2-甲基咪唑锌盐多孔配位聚合物-六水合硝酸锌-聚丙烯复合纤维；最后进行肟化反应获得偕胺肟化的用于海水提铀的纳米级复合纤维材料。通过本方法制备的海水提铀吸附剂，不仅可显著提高其提铀能力，且在循环提铀使用中具有持续自更新的防海洋生物污损能力，不收缩且结构稳定。
以上发明均以化学品合成的物质为主体进行海水提铀，使用较多的化学品已造成污染。
发明内容
为了解决背景技术中存在的问题，本发明提供了一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，使用天然木头为基体，绿色环保、成本低、涉及的化学反应少、操作简单且提铀效果好。
本发明的技术方案如下：
一、一种用水杨醛肟和Fe3+自组装制备海水提铀木头的制备方法，方法包括以下步骤：
(1)将天然木头通过预处理以脱除木质素，在预处理液中于高温条件下反应12-24小时，直至天然木头完全变白；
(2)随后将(1)得到的完全变白的木头取出，在流动的清水条件下洗涤1-12h，直至完全清洗掉预处理液将木头清洗干净，将冲洗干净的木头干燥备用；
(3)将步骤(2)得到的木头浸渍到醛肟类溶液中，水浴常温振荡浸渍10-60min，随后，将木头取出放在纯水中洗涤三次，用滤纸吸取表面多余的水滴；
(4)将步骤(3)得到的木头浸渍到含三价铁离子的溶液中，水浴常温振荡浸渍10-60min，随后，将木头取出在纯水中洗涤三次，用滤纸吸取表面多余的水滴；
(5)依次完成步骤(3)、步骤(4)中的木头浸渍即完成了一次自组装，多次按顺序重复步骤(3)～步骤(4)以完成多次自组装，最终获得海水提铀木头。
所述的天然木头为杉木、樟木、杨木、松木、枫木、榕木、榆木、桦木、椴木中的至少一种。
所述的步骤(1)中，所述的预处理液为亚氯酸钠、氢氧化钠、氢氧化钾、过硫酸钠、次氯酸钠、双氧水、甲醇、乙醇、乙醚、丙酮、甲酸中的至少一种，预处理液浓度为0.2mol/L-1.2mol/L。
步骤(1)中对天然木头进行预处理，高温蒸煮过程中木质素大分子裂开溶出。
所述步骤(1)中，高温条件为50-100℃。
所述步骤(2)中的干燥方式为：自然干燥，加热干燥，冷冻干燥中的一种。
所述步骤(3)中的醛肟类溶液为甲醛肟、乙醛肟、水杨醛肟、二甲基乙二醛肟、丙醛肟中的一种，所述的水浴常温振荡速度为40-120RPM。
所述步骤(4)中的含三价铁离子的溶液为：硝酸铁、硫酸铁、氯化铁、溴化铁溶液中的一种。
所述步骤(3)中的醛肟溶液与所述步骤(4)中的三价铁离子溶液浓度比为10:1-1:1。
所述步骤(5)中，所述的自组装进行1-20次。
二、一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头，由上所述的制备方法制得。
所述的海水提铀木头在海水提铀中应用。
本发明具有如下优点和有益效果：
(1)所需要的原材料、基材种类丰富，来源范围广，成本低。同时，整个操作过程简单，反应条件温和，耗能低。
(2)本方法以木头为基底克服了以化学品合成物为主体，使用较多化学品造成环境污染的问题，本方法制备的木头在使用过程中方便回收，涉及的化学反应少、绿色环保且提铀效果好。本发明提供了一种绿色环保的海水提铀方法，同时为其他研究人员的研究提供了一种可行的参考方法。在海水提铀等领域有着巨大的应用前景。
附图说明
图1为在不同pH下实施例2-7的吸附量结果对比图；
图2为在不同温度下实施例8-11的吸附量结果对比图；
图3为在不同硝酸铀酰浓度下实施例12-14的吸附量结果对比图。
具体实施方式
通过以下实施例对本发明做更详细的描述，但所述实施例不构成对本发明的限制。
本发明的实施例如下：
实施例1：
(1)选用尺寸为4*4cm的巴杉木方形木块，预处理液为0.2mol/L的亚氯酸钠溶液，80℃水浴锅中蒸煮15h，直至木头完全变白，流动的清水条件下洗涤10h。将冲洗干净的木头干燥备用。
(2)将步骤(1)中的木头，在体积100ml的水杨醛肟溶液中水浴常温振荡浸渍50min，随后，将木头取出放在纯水中洗涤三次。用滤纸吸取表面多余的水滴。
(3)将步骤(2)中的木头，在体积20ml的FeCl3·6H2O溶液中水浴常温振荡浸渍60min，随后，将木头取出在纯水中洗涤三次。用滤纸吸取表面多余的水滴。
(4)依次完成步骤(2)、步骤(3)中的木头，即完成了一次自组装。多次按顺序重复步骤(2)、步骤(3)以完成多次自组装。
(5)配制500mg/L的硝酸酰铀溶液100mL，量取10mL将其稀释到250mg/L，用1mol/L盐酸与0.1mol/L氢氧化钠溶液调节pH＝3。将4*4的巴杉木头称量5mg浸入到50mL，pH＝3的250mg/L的硝酸酰铀溶液，水浴振荡器180RPM，温度30℃条件下吸附24小时，用偶氮胂光度法测量铀离子浓度。
实施例2-7
实施例2-7分别用1mol/L盐酸和0.1mol/L氢氧化钠溶液分别调节250mg/L的硝酸酰铀溶液pH到pH＝4、pH＝5、pH＝6、pH＝7、pH＝8、pH＝9。结果如图1所示。图1中可见，在pH＝3至pH＝6时，随着pH的升高铀吸附量变大；在pH＝6至pH＝9时，随着pH的升高铀的吸附量下降，在pH＝6时吸附量达到最高，约为450mg/g。
实施例8-11
实施例8-11分别将4*4的巴杉木头称量5mg浸入到20mL，pH＝6的250mg/L的硝酸酰铀溶液，水浴振荡器180RPM，温度分别为30℃、40℃、50℃、60℃条件下吸附24小时。结果如图2所示。图2中可见，随着温度的升高对铀的平衡吸附量升高，在60℃时达到最高值596.21mg/g。
实施例12-14
实施例12-14分别在PH＝6的条件下，配置不同浓度的硝酸酰铀溶液，浓度分别为300mg/L、250mg/L、200mg/L，测定在相同时间内的吸附量。结果如图3所示。图3中可见，吸附量随着硝酸酰铀溶液的浓度提高而提高，浓度为300mg/L时在相同时间内的吸附量最高。
由此实施可见，本发明制备方法操作简单，可控性强，可应用于海水提铀方面。

Claims (10)

1.一种用水杨醛肟和Fe3+自组装制备海水提铀木头的制备方法，其特征在于：方法包括以下步骤：
(1)将天然木头通过预处理以脱除木质素，在预处理液中于高温条件下反应12-24小时，直至天然木头完全变白；
(2)随后将(1)得到的完全变白的木头取出，在流动的清水条件下洗涤1-12h，直至完全清洗掉预处理液将木头清洗干净，将冲洗干净的木头干燥；
(3)将步骤(2)得到的木头浸渍到醛肟类溶液中，水浴常温振荡浸渍10-60min，随后，将木头取出放在纯水中洗涤三次，用滤纸吸取表面多余的水滴；
(4)将步骤(3)得到的木头浸渍到含三价铁离子的溶液中，水浴常温振荡浸渍10-60min，随后，将木头取出在纯水中洗涤三次，用滤纸吸取表面多余的水滴；
(5)依次完成步骤(3)、步骤(4)中的木头浸渍即完成了一次自组装，多次按顺序重复步骤(3)～步骤(4)以完成多次自组装，最终获得海水提铀木头。
2.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述的天然木头为杉木、樟木、杨木、松木、枫木、榕木、榆木、桦木、椴木中的至少一种。
3.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述的步骤(1)中，所述的预处理液为亚氯酸钠、氢氧化钠、氢氧化钾、过硫酸钠、次氯酸钠、双氧水、甲醇、乙醇、乙醚、丙酮、甲酸中的至少一种，预处理液浓度为0.2mol/L-1.2mol/L。
4.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述步骤(1)中，高温条件为50-100℃。
5.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述步骤(3)中的醛肟类溶液为甲醛肟、乙醛肟、水杨醛肟、二甲基乙二醛肟、丙醛肟中的一种，所述的水浴常温振荡速度为40-120RPM。
6.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述步骤(4)中的含三价铁离子的溶液为：硝酸铁、硫酸铁、氯化铁、溴化铁溶液中的一种。
7.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述步骤(3)中的醛肟溶液与所述步骤(4)中的三价铁离子溶液浓度比为10:1-1:1。
8.根据权利要求1所述的一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头的制备方法，其特征在于：所述步骤(5)中，所述的自组装进行1-20次。
9.一种用水杨醛肟和Fe3+自组装到木头上制备海水提铀木头，其特征在于，由权利要求1～5任一项所述的制备方法制得。
10.权利要求9所述海水提铀木头的应用，其特征在于：在海水提铀中的应用。
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