CN108636372B - 一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备及应用 - Google Patents

一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备及应用 Download PDF

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CN108636372B
CN108636372B CN201810544659.1A CN201810544659A CN108636372B CN 108636372 B CN108636372 B CN 108636372B CN 201810544659 A CN201810544659 A CN 201810544659A CN 108636372 B CN108636372 B CN 108636372B
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魏东
刘英瑞
房亚南
乔一明
丁祥伟
杜斌
魏琴
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Abstract

本发明涉及一种好氧颗粒污泥‑Fe3O4‑腐殖酸复合生物吸附剂的制备及应用。所述生物吸附剂是由好氧颗粒污泥、磁性Fe3O4和腐殖酸三种原材料制备而成的,其制备过程是将磁性Fe3O4与腐殖酸按4:1~5:1的质量比混合,溶液体系的pH控制在7以上,于80~100℃搅拌30~40 min,于40~80℃烘干得Fe3O4‑腐殖酸黑色粉末;将Fe3O4‑腐殖酸与好氧颗粒污泥干重按1:5~2:5的质量比混合,加入100~150 mL、25%的戊二醛,在25℃下搅拌12~18 h,搅拌速度为100 r/min,经冷冻真空干燥48 h后制得好氧颗粒污泥‑Fe3O4‑腐殖酸复合生物吸附剂。本发明应用于重金属的吸附,成本低廉、吸附容量和去除率高、可重复利用且不造成二次污染。

Description

一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备及 应用
技术领域
本发明涉及一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备及应用,适用于重金属离子的去除,属于污水处理技术领域。
背景技术
随着社会经济的飞速发展,工业和农业用水量日趋增加,污水排放总量逐渐增大,导致许多地区的地下水资源都受到不同程度的重金属污染。医药制造厂、电镀厂、金属冶炼厂、采矿厂、造纸厂和制革厂等大量的工厂在运转过程中会对重金属进行不同量的排放。重金属化学性质稳定,不易被生物降解。且重金属进入到人体后会迅速与蛋白质结合对酶产生抑制作用,使酶活性降低甚至失活,严重危害人体健康。因为,水环境中的重金属污染问题是亟待解决的。
好氧颗粒污泥是微生物通过自凝聚作用形成的一种特殊的生物聚集体,具有结构致密、沉降性能优异、抗冲击负荷能力强、多功能微生物分区定殖等特点,其在废水重金属去除方面具有明显的技术优势。腐植酸的组成元素极其复杂,化学结构复杂多样,含有羧基、醇羟基、酚羟基、醌型羰基和酮型羰基等多种活性官能团,具有很高的反应活性,能与环境中的金属离子、矿物质、有机质、氧化物、氢氧化物和有毒活性污染物等发生吸附、络合和氧化还原作用。腐殖酸的这些基团和功能使其成为较好的吸附材料。申请号为201410026441.9的发明专利公开了一种磁性腐殖酸纳米材料的制备方法和应用,但复合材料较少,功能化较低。本发明将好氧颗粒污泥、磁性Fe3O4和腐殖酸复合制得好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,成功地将三种有效吸附材料进行结合,得到了更加高效的复合吸附剂,用于重金属离子的去除。该吸附方法简单,操作方便,不造成二次污染,再生后的吸附剂可循环利用。
发明内容
针对现有技术近一步改进的需求,本发明提供了一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备方法,用于重金属离子的吸附。
本发明的技术方案如下:
1.一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备,其特征包括以下步骤:
(1)Fe3O4-腐殖酸的制备:称取4 ~ 5 g Fe3O4粉末于100 ~ 200 mL蒸馏水中,超声15 ~ 30 min;依次加入30 mL一水合氨使得溶液体系的pH控制在7以上,1 g腐殖酸粉末和100 mL NaCl溶液;置于80 ~ 100℃水浴搅拌30 ~ 40 min,冷却至室温,用蒸馏水或无水乙醇清洗直至上清液清澈,用外加磁铁进行分离,于烘箱中进行40 ~ 80℃烘干,制得Fe3O4-腐殖酸的黑色粉末;
(2)好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备:称取1 ~ 2 g Fe3O4-腐殖酸粉末置于200 mL蒸馏水中,超声20 ~ 30 min,依次加入5 g好氧颗粒污泥和100 ~150mL、25%的戊二醛,在25℃下搅拌12 ~ 18 h,搅拌速度为100 r/min,经冷冻真空干燥48h直至完全干燥后,制得好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂。
2.所述的一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备,其特征在于所述好氧颗粒污泥粒径为1.0 ~ 3.0 mm,形状近球形,沉降速度30 ~ 60 m/min,使用前用蒸馏水清洗6 ~ 8次。
3.所述的一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备,应用于重金属的吸附,其步骤如下:取20 ~ 40 mL、20 ~ 50 mg/L、pH=6的重金属溶液于50 mL锥形瓶中,投加5 ~ 50 mg的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,在20 ~ 35℃,转速为150r/min的水浴摇床中震荡8 ~ 12 h,取出静置后过滤;采用原子吸收分光光度计测量溶液中的重金属离子浓度,计算重金属的去除率。
4. 所述的一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备,重金属选其中之一:铜、镍、镉。
本发明的有益成果
1. 本发明以好氧颗粒污泥、磁性Fe3O4和腐殖酸为原材料制备的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂是一种新型高效的吸附剂材料,使好氧颗粒污泥得到了资源化利用。
2. 本发明制备的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,其具有良好的磁性和化学性能,且好氧颗粒污泥比表面积大、吸附性能好;好氧颗粒污泥和腐殖酸中含有丰富的官能团,对重金属的吸附量大,吸附效率高,有良好的应用前景。
3. 本发明制备的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,条件易于控制,合成成本低,易操作。
附图说明
图1一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的合成制备示意图。
具体实施方式
实施例1一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备方法
(1)将实验室SBR反应器中培养的好氧颗粒污泥用蒸馏水清洗6 ~ 8次,随后用筛网筛选出粒径为1.0 mm的好氧颗粒污泥;
(2)称取4 g磁性Fe3O4黑色粉末,将其溶解于100 mL蒸馏水中,水浴加热至80℃;依次加入30 mL一水合氨、1 g腐殖酸粉末和100 mL NaCl溶液,在80℃下水浴搅拌30 min;冷却至室温后,用蒸馏水或无水乙醇清洗直至上清液清澈,用外加磁铁进行分离,在烘箱中进行40℃烘干,制得Fe3O4-腐殖酸黑色粉末;
(3)称取1 g Fe3O4-腐殖酸粉末置于200 mL蒸馏水中,超声20 min;依次加入5 g好氧颗粒污泥和100 mL、25%的戊二醛,在25℃下搅拌12 h,搅拌速度为100 r/min,经冷冻干燥48 h直至完全干燥,最终制得好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂。
实施例2一种好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂的制备方法
(1)将实验室SBR反应器中培养的好氧颗粒污泥用超纯水清洗6 ~ 8次,随后用筛网筛选出粒径为1.0 mm的好氧颗粒污泥;
(2)称取5 g磁性Fe3O4黑色粉末,将其溶解于200 mL蒸馏水中,水浴加热至90℃;依次加入30 mL一水合氨、1 g腐殖酸粉末和100 mL NaCl溶液,在90℃下水浴搅拌40 min;冷却至室温后,用蒸馏水或无水乙醇清洗直至上清液清澈,用外加磁铁进行分离,在烘箱中进行60℃烘干,制得Fe3O4-腐殖酸黑色粉末;
(3)称取2 g Fe3O4-腐殖酸粉末置于200 mL蒸馏水中,超声20 min;依次加入5 g好氧颗粒污泥和150 mL、25%的戊二醛,在25℃下搅拌18 h,搅拌速度为100 r/min,经冷冻干燥48 h直至完全干燥,最终制得好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂。
实施例3铜离子的去除
取30 mL、40 mg/L、pH=6的铜溶液于50 mL锥形瓶中,投加6 mg的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,在25℃,转速为150 r/min的水浴摇床中震荡8 h,取出静置后过滤;采用原子吸收分光光度计测量溶液中的重金属离子浓度,计算得到离子的出水浓度为0.92 mg/L,去除率为97.7%。
实施例4镍离子的去除
取35 mL、45 mg/L、pH=6的镍溶液于50 mL锥形瓶中,投加8 mg的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,在25℃,转速为150 r/min的水浴摇床中震荡10 h,取出静置后过滤;采用原子吸收分光光度计测量溶液中的重金属离子浓度,计算得到离子的出水浓度为2.12 mg/L,去除率为95.3%。
实施例5镉离子的去除
取40 mL、50 mg/L、pH=6的镉溶液于50 mL锥形瓶中,投加10 mg的好氧颗粒污泥-Fe3O4-腐殖酸复合生物吸附剂,在25℃,转速为的水浴摇床中震荡12 h,取出静置后过滤;采用原子吸收分光光度计测量溶液中的重金属离子浓度,计算得到离子的出水浓度为0.75mg/L,去除率为98.5%。

Claims (4)

1.一种好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂的制备,其特征包括以下步骤:
(1)Fe3O4 -腐殖酸的制备:称取4~5g Fe3O4 粉末于100~200mL蒸馏水中,超声15~30min;依次加入30mL一水合氨使得溶液体系的pH控制在7以上,1g腐殖酸粉末和100mLNaCl溶液;置于80~100℃水浴搅拌30~40min,冷却至室温,用蒸馏水或无水乙醇清洗直至上清液清澈,用外加磁铁进行分离,于烘箱中进行40~80℃烘干,制得Fe3O4 -腐殖酸的黑色粉末;
(2)好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂的制备:称取1~2g Fe3O4 -腐殖酸粉末置于200mL蒸馏水中,超声20~30min,依次加入5g好氧颗粒污泥和100~150mL、25%的戊二醛,在25℃下搅拌12~18h,搅拌速度为100r/min,经冷冻真空干燥48h直至完全干燥后,制得好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂。
2.根据权利要求1所述的一种好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂的制备,其特征在于所述好氧颗粒污泥粒径为1.0~3.0mm,形状近球形,沉降速度30~60m/min,使用前用蒸馏水清洗6~8次。
3.根据权利要求1所述的一种好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂的制备,应用于重金属的吸附,其步骤如下:取20~40mL、20~50mg/L、pH=6的重金属溶液于50mL锥形瓶中,投加5~50mg的好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂,在20~35℃,转速为150r/min的水浴摇床中震荡8~12h,取出静置后过滤;采用原子吸收分光光度计测量溶液中的重金属离子浓度,计算重金属的去除率。
4.根据权利要求3所述的一种好氧颗粒污泥-Fe3O4 -腐殖酸复合生物吸附剂的制备,重金属选其中之一:铜、镍、镉。
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