CN106732110A - 一种重金属污水处理剂的制备方法 - Google Patents
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Abstract
本发明公开了一种重金属污水处理剂的制备方法，其采用微流控技术，结合乳化和交联反应，并添加纳米二氧化钛和γ‑三氧化二铁制成蔗渣纤维素黄原酸醋微球吸附剂。本发明利用蔗渣纤维素作为吸附剂的原料，成本低，不会对环境造成二次污染，本发明含有纳米二氧化钛和γ‑三氧化二铁对重金属污水中的重金属离子具有很强的吸附作用，同时可分解污水中的有机物，兼具吸附性能和光催化性能，依照本发明制成的吸附剂分散性好，吸附容量好，污水处理效果好。
Description
技术领域
本发明涉及废水处理技术领域，具体涉及一种重金属污水处理剂的制备方法。
背景技术
目前国内外重金属污水的处理的方法主要有化学沉淀法、离子交换法、生物法、电解法、膜分离技术、吸附法等，化学沉淀法是比较成熟的重金属污水处理方法之一操作简单，处理速度快，但污水重金属离子浓度高，沉渣量大，含水率高，成本高，且容易造成二次污染，活性炭吸附法和离子交换法材料成本高，工艺复杂，电解法重金属离子对离子浓度要求高，成本大，耗能大处理量小，但符合社会低碳的要求，生物法微生物菌种培养困难，处理时间长，且易造成生物污染，现阶段的重金属处理方法中，各有利弊，因此，再此基础上改进废水处理剂的生产方法，研制出环境污染小、成本低、污水处理效果好的污水处理剂具有重要意义。
发明内容
本发明的目的在于，针对现有技术的不足，提供了一种重金属污水处理剂的制备方法。
为实现上述目的，本发明采取以下技术方案：
一种重金属污水处理剂的制备方法，其包括如下步骤：
(1)微流控芯片的制备：芯片采用三板式结构，三板厚均为1mm，基板主通道宽度在3mm，聚焦通道宽度在500μm，上盖板和下底板开孔直径为3mm；
(2)结合反相乳化法采用油包水(O/W)体系，水相体系为将质量分数为2％的蔗渣纤维素溶于0.1～0.5mol/L的氢氧化钠溶液中搅拌反应1～3h，静置，除去多余的氢氧化钠溶液，将氢氧化钠处理后的蔗渣纤维素加入二硫化碳反应得到蔗渣纤维素黄原醋酸水溶物，同时加入0.1％的纳米二氧化钛和0.2～1％的γ-三氧化二铁混匀；油相体系为含有十八烷的石蜡乳液；
(3)将水相与油相用注射泵推入微流控芯片中，在聚焦处界面张力和外相流体剪切力及压力作用下内相被剪断与剥离，形成规整的乳液液滴；
(4)采用交联反应对蔗渣纤维素乳液进行固化，交联剂为戊二醛饱和的甲苯溶液，交联转速控制在300r/min，交联在25℃室温下完成，得到固化后的蔗渣纤维素黄原酸醋微球；
(5)固化后的蔗渣纤维素黄原酸醋微球用石油醚抽滤后用去离子水反复清洗，直至表面油相完全被清除，从而避免残余油相导致颗粒团聚。
(6)将清洗后蔗渣纤维素黄原酸醋微球在50℃烘干3h制得成品。
其中，所述的步骤(2)中，蔗渣纤维素与氢氧化钠的比例为每1g蔗渣纤维素溶于10ml氢氧化钠溶液。
其中，所述的步骤(2)中蔗渣纤维素与二硫化碳的质量比为1：1～5。
其中，所述的步骤(3)所述的石蜡乳液中，十八烷的质量百分比为1～10％。
其中，本发明将蔗渣纤维素碱处理后与二硫化碳反应生成蔗渣纤维素黄原酸醋，将蔗渣纤维黄原酸醋加入纳米二氧化钛和γ-三氧化二铁制成蔗渣纤维素黄原酸醋微球，本发明中得到的蔗渣纤维素黄原酸醋微球对水中的重金属具有很强的吸附作用，添加入纳米二氧化钛可加速污水中有机物的降解。
本发明的有益效果是：
1、本发明利用蔗渣纤维素作为吸附剂的原料，成本低，不会对环境造成二次污染；
2、本发明的重金属污水处理剂具含有纳米二氧化钛和γ-三氧化二铁对重金属污水中的重金属离子具有很强的吸附作用，同时可分解污水中的有机物，兼具吸附性能和光催化性能；
3、依照本发明制成的重金属污水处理剂分散性好，吸附容量好，污水处理效果好。
具体实施方式
下面结合具体实施例，对本发明进一步的说明。
实施例1
一种重金属污水处理剂的制备方法，其包括如下步骤：
(1)微流控芯片的制备：芯片采用三板式结构，三板厚均为1mm，基板主通道宽度在3mm，聚焦通道宽度在500μm，上盖板和下底板开孔直径为3mm；
(2)结合反相乳化法采用油包水(O/W)体系，水相体系为将质量分数为2％的蔗渣纤维素按蔗渣纤维素与氢氧化钠的比例为每1g蔗渣纤维素溶于10ml氢氧化钠溶液的比例溶于0.3mol/L的氢氧化钠溶液中搅拌反应2h，静置，除去多余的氢氧化钠溶液，将氢氧化钠处理后的蔗渣纤维素按蔗渣纤维素与二硫化碳的质量比1：4加入二硫化碳反应得到蔗渣纤维素黄原醋酸水溶物，同时加入0.1％的纳米二氧化钛和0.8％的γ-三氧化二铁混匀；油相体系为含有十八烷的质量百分比为5％的石蜡乳液；
(3)将水相与油相用注射泵推入微流控芯片中，在聚焦处界面张力和外相流体剪切力及压力作用下内相被剪断与剥离，形成规整的乳液液滴；
(4)采用交联反应对蔗渣纤维素乳液进行固化，交联剂为戊二醛饱和的甲苯溶液，交联转速控制在300r/min，交联在25℃室温下完成，得到固化后的蔗渣纤维素黄原酸醋微球；
(5)固化后的蔗渣纤维素黄原酸醋微球用石油醚抽滤后用去离子水反复清洗，直至表面油相完全被清除，从而避免残余油相导致颗粒团聚。
(6)将清洗后蔗渣纤维素黄原酸醋微球在50℃烘干3h制得成品。
实施例2
一种重金属污水处理剂的制备方法，其包括如下步骤：
(1)微流控芯片的制备：芯片采用三板式结构，三板厚均为1mm，基板主通道宽度在3mm，聚焦通道宽度在500μm，上盖板和下底板开孔直径为3mm；
(2)结合反相乳化法采用油包水(O/W)体系，水相体系为将质量分数为2％的蔗渣纤维素按蔗渣纤维素与氢氧化钠的比例为每1g蔗渣纤维素溶于10ml氢氧化钠溶液的比例溶于0.1mol/L的氢氧化钠溶液中搅拌反应3h，静置，除去多余的氢氧化钠溶液，将氢氧化钠处理后的蔗渣纤维素按蔗渣纤维素与二硫化碳的质量比1：1加入二硫化碳反应得到蔗渣纤维素黄原醋酸水溶物，同时加入0.1％的纳米二氧化钛和0.2％的γ-三氧化二铁混匀；油相体系为含有十八烷的质量百分比为1％的石蜡乳液；
(3)将水相与油相用注射泵推入微流控芯片中，在聚焦处界面张力和外相流体剪切力及压力作用下内相被剪断与剥离，形成规整的乳液液滴；
(4)采用交联反应对蔗渣纤维素乳液进行固化，交联剂为戊二醛饱和的甲苯溶液，交联转速控制在300r/min，交联在25℃室温下完成，得到固化后的蔗渣纤维素黄原酸醋微球；
(5)固化后的蔗渣纤维素黄原酸醋微球用石油醚抽滤后用去离子水反复清洗，直至表面油相完全被清除，从而避免残余油相导致颗粒团聚。
(6)将清洗后蔗渣纤维素黄原酸醋微球在50℃烘干3h制得成品。
实施例3
一种重金属污水处理剂的制备方法，其包括如下步骤：
(1)微流控芯片的制备：芯片采用三板式结构，三板厚均为1mm，基板主通道宽度在3mm，聚焦通道宽度在500μm，上盖板和下底板开孔直径为3mm；
(2)结合反相乳化法采用油包水(O/W)体系，水相体系为将质量分数为2％的蔗渣纤维素按蔗渣纤维素与氢氧化钠的比例为每1g蔗渣纤维素溶于10ml氢氧化钠溶液的比例溶于0.5mol/L的氢氧化钠溶液中搅拌反应1h，静置，除去多余的氢氧化钠溶液，将氢氧化钠处理后的蔗渣纤维素按蔗渣纤维素与二硫化碳的质量比1：5加入二硫化碳反应得到蔗渣纤维素黄原醋酸水溶物，同时加入0.1％的纳米二氧化钛和1％的γ-三氧化二铁混匀；油相体系为含有十八烷的质量百分比为10％的石蜡乳液；
(3)将水相与油相用注射泵推入微流控芯片中，在聚焦处界面张力和外相流体剪切力及压力作用下内相被剪断与剥离，形成规整的乳液液滴；
(4)采用交联反应对蔗渣纤维素乳液进行固化，交联剂为戊二醛饱和的甲苯溶液，交联转速控制在300r/min，交联在25℃室温下完成，得到固化后的蔗渣纤维素黄原酸醋微球；
(5)固化后的蔗渣纤维素黄原酸醋微球用石油醚抽滤后用去离子水反复清洗，直至表面油相完全被清除，从而避免残余油相导致颗粒团聚。
(6)将清洗后蔗渣纤维素黄原酸醋微球在50℃烘干3h制得成品。
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。
Claims (4)
1.一种重金属污水处理剂的制备方法，其特征在于，其包括如下步骤：
(1)微流控芯片的制备：芯片采用三板式结构，三板厚均为1mm，基板主通道宽度在3mm，聚焦通道宽度在500μm，上盖板和下底板开孔直径为3mm；
(2)结合反相乳化法采用油包水(O/W)体系，水相体系为将质量分数为2％的蔗渣纤维素溶于0.1～0.5mol/L的氢氧化钠溶液中搅拌反应1～3h，静止，除去多余的氢氧化钠溶液，将氢氧化钠处理后的蔗渣纤维素加入二硫化碳反应得到蔗渣纤维素黄原醋酸水溶物，同时加入0.1％的纳米二氧化钛和0.2～1％的γ-三氧化二铁混匀；油相体系为含有十八烷的石蜡乳液；
(3)将水相与油相用注射泵推入微流控芯片中，在聚焦处界面张力和外相流体剪切力及压力作用下内相被剪断与剥离，形成规整的乳液液滴；
(4)采用交联反应对蔗渣纤维素乳液进行固化，交联剂为戊二醛饱和的甲苯溶液，交联转速控制在300r/min，交联在25℃室温下完成，得到固化后的蔗渣纤维素黄原酸醋微球；
(5)固化后的蔗渣纤维素黄原酸醋微球用石油醚抽滤后用去离子水反复清洗，直至表面油相完全被清除，从而避免残余油相导致颗粒团聚。
(6)将清洗后蔗渣纤维素黄原酸醋微球在50℃烘干3h制得成品。
2.根据权利要求1所述的一种重金属污水处理剂的制备方法，其特征在于，所述的步骤(2)中，蔗渣纤维素与氢氧化钠的比例为每1g蔗渣纤维素溶于10ml氢氧化钠溶液。
3.根据权利要求1所述的一种重金属污水处理剂的制备方法，其特征在于，所述的步骤(2)中蔗渣纤维素与二硫化碳的质量比为1：1～5。
4.根据权利要求1所述的一种重金属污水处理剂的制备方法，其特征在于，所述的步骤(3)所述的石蜡乳液中，十八烷的质量百分比为1～10％。
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