CN115121218B - 一种制备吸附pb2+的污泥基改性陶粒的方法 - Google Patents

一种制备吸附pb2+的污泥基改性陶粒的方法 Download PDF

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CN115121218B
CN115121218B CN202210717828.3A CN202210717828A CN115121218B CN 115121218 B CN115121218 B CN 115121218B CN 202210717828 A CN202210717828 A CN 202210717828A CN 115121218 B CN115121218 B CN 115121218B
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程星星
方伟成
张云
孙常荣
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Abstract

本发明提供一种制备吸附pb2+的污泥基改性陶粒的方法,属于污水处理技术领域。该方法首先将陶粒原料研成粉末,置于三颈烧瓶中并加入超纯水和氢氧化钠粉末;然后在室温下,将三颈烧瓶置于磁力搅拌器中搅拌并加入甲醛溶液;再将三颈烧瓶置于KI2型的烧瓶加热器中反应;到达预设反应时间后,将三颈烧瓶取出并自然冷却,将二硫化碳溶液和NaOH粉末同时加入三颈烧瓶中搅拌均匀,自然反应;到达预设反应时间后,加入盐酸,搅拌均匀后静置,出现棕黑色沉淀;将得到的沉淀用超纯水冲洗后,将沉淀物用冷冻干燥机收集,即得到改性陶粒。该方法能够实现改性污泥陶粒对Pb2+的吸附率达到90%以上,解决了现有污泥陶粒难以有效吸附Pb2+的技术难题。

Description

一种制备吸附pb2+的污泥基改性陶粒的方法
技术领域
本发明涉及污水处理技术领域,特别是指一种制备吸附pb2+的污泥基改性陶粒的方法。
背景技术
污水治理是一项长期工程,多年来用于污水处理的技术层出不穷,但如何低成本、高效率地处理污水则是关键所在,尤其是如何实现以污治污更是科学界与工程领域的研究热点,污泥基陶粒在污水处理中正在发挥重要作用[7]
在处理污水过程中,重金属离子能否有效吸附和固化是衡量处理效果的核心指标。现有技术中提及了污泥基陶粒对废水中的污染物具备广泛的消解能力,但其对于重金属离子的吸附效果不甚理想,尤其是对于Pb2+的吸附效果更弱;同时,现有技术中制备的普通污泥基陶粒粉对Cu2+的去除率仅为15%,对Pb2+的吸附效果更差。
现有技术中公开了一种生物质污泥陶粒及其制备方法和应用,该生物质污泥陶粒由生物质混烧灰、污泥粉等组成,不消耗任何页岩、高岭土、粘土等不可再生自然资源,其孔径大小均匀,具有较低的吸水率及较好的吸附效果,是一种很好的重金属污水处理材料。但该方法所制备的生物质污泥陶粒对Pb2+的最大吸附率仅为39.94%,而对Zn、Cd、Cu、As等重金属的吸附率均不超过20%。
现有技术中提出了一种用于重金属废水处理的污泥陶粒及制备方法,所述污泥陶粒是将河道底泥及矿物粉料烧结制得多孔陶粒,同时将腐殖酸、异丙醇等混合制成混合浆液,并将多孔陶粒在浆状液中反复浸泡-烘干而制得。该方法提供的改性污泥陶粒,比表面积大,对重金属Pb、Cd、Cu等具有很强的吸附性且吸附率稳定,同时可多次回收利用,无二次污染,可广泛用于重金属废水处理。但其对Cu2+和Pb2+的最大吸附率分别仅为61%和57%,远远达不到我国污水处理中重金属离子的处理要求。
现有的关于污泥陶粒制备方法虽有不少,但均未考虑如何提高污泥陶粒对重金属离子的吸附性能。
可见,理论界和工程界普遍未关注或未能提出如何通过制备改性污泥陶粒从而实现对重金属离子,特别是pb2+的有效吸附,而造成这一现状的核心原因有两条:(1)污泥陶粒在微观层面对Pb2+的吸附机制未被充分揭示;(2)目前缺乏科学地评估污泥基陶粒吸附Pb2+性能的方法,这给陶粒改性工作带来困难。
由此,本发明研究设计了一种全新的制备吸附pb2+的污泥基改性陶粒的方法,实现对Pb2+具备较强吸附特性的污泥基改性陶粒的制备。
发明内容
本发明基于污水处理领域目前缺乏科学、环保、经济的去除重金属离子尤其是Pb2+的技术和工艺,提供一种制备吸附pb2+的污泥基改性陶粒的方法,通过在碱性条件下于分子层面为普通污泥陶粒颗粒表面附着含硫官能团的方法,有效提升污泥基陶粒对Pb2+的吸附特性。
本发明方法充分发挥含硫官能团存在易与金属离子结合的活性位点这一特征,在分子层面对污泥基陶粒进行改性,使其颗粒表面附着多种含硫官能团,从而有效提升污泥基陶粒对Pb2+的吸附特性。
该方法包括步骤如下:
S1:将陶粒原料研成粉末后,置于三颈烧瓶中并加入超纯水,再取氢氧化钠粉末加入三颈烧瓶中,将溶液的pH值调节为12~13;
S2:在室温下,将三颈烧瓶置于磁力搅拌器中搅拌10~15分钟,随后加入甲醛溶液,搅拌均匀;
S3:将KI2型的烧瓶加热器温度设定为90℃,将三颈烧瓶置于其中,使其自然反应2.5~3小时;
S4:到达预设反应时间后,将三颈烧瓶取出并自然冷却,待温度降到40~45℃以下时,将二硫化碳溶液和NaOH粉末同时加入三颈烧瓶中并搅拌均匀,自然反应2~3小时;
S5:到达预设反应时间后,向三颈烧瓶中加入0.1-0.2mol/L的盐酸,搅拌均匀后静置4.5~6小时,三颈烧瓶中出现棕黑色沉淀;
S6:将S5中得到的沉淀用超纯水冲洗3~5分钟,待滤液颜色接近透明且滤液的pH值为7.0~7.3时,将沉淀物用冷冻干燥机收集,即得到改性陶粒。
上述,陶粒原料化学成分SiO2、Al2O3、氧化物溶剂总和满足Riley相图;陶粒比表面积大于48700cm2/g;
其中,氧化物溶剂为CaO+MgO+Fe2O3+Na2O+K2O。
上述S1中陶粒原料粉末粒度小于80目。
S1中陶粒原料和超纯水的质量比为1:3~1:4。
S2中甲醛溶液的加入量为2mL-3mL/g陶粒。
S4中二硫化碳溶液和NaOH粉末的0.025-0.05g/g陶粒。
S5中盐酸加入量保证溶液pH为中性。
S5中得到的改性陶粒对Pb2+的吸附率达到90%以上。
本发明的上述技术方案的有益效果如下:
上述方案中,能够实现改性污泥陶粒对Pb2+的吸附率达到90%以上,较好地解决了现有污泥陶粒难以有效吸附Pb2+的技术难题,拓展了污泥基陶粒的工业和生态用途,同时为污水、土壤中重金属固化技术的发展提供了新的技术思路。
附图说明
图1为本发明的制备吸附pb2+的污泥基改性陶粒的方法流程图;
图2为本发明实施例中改性前后陶粒表面官能团分析;
图3为本发明实施例中两种材料对Pb2+的吸附性能评估。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚,下面将结合附图及具体实施例进行详细描述。
本发明提供一种制备吸附pb2+的污泥基改性陶粒的方法。
如图1所示,该方法包括步骤如下:
S1:将陶粒原料研成粉末后,置于三颈烧瓶中并加入超纯水,再取氢氧化钠粉末加入三颈烧瓶中,将溶液的pH值调节为12~13;
S2:在室温下,将三颈烧瓶置于磁力搅拌器中搅拌10~15分钟,随后加入甲醛溶液,搅拌均匀;
S3:将KI2型的烧瓶加热器温度设定为90℃,将三颈烧瓶置于其中,使其自然反应2.5~3小时;
S4:到达预设反应时间后,将三颈烧瓶取出并自然冷却,待温度降到40~45℃以下时,将二硫化碳溶液和NaOH粉末同时加入三颈烧瓶中并搅拌均匀,自然反应2~3小时;
S5:到达预设反应时间后,向三颈烧瓶中加入0.1-0.2mol/L的盐酸,搅拌均匀后静置4.5~6小时,三颈烧瓶中出现棕黑色沉淀;
S6:将S5中得到的沉淀用超纯水冲洗3~5分钟,待滤液颜色接近透明且滤液的pH值为7.0~7.3时,将沉淀物用冷冻干燥机收集,即得到改性陶粒。
在具体制备中,所用陶粒原料化学成分SiO2、Al2O3、氧化物溶剂总和满足Riley相图;陶粒比表面积大于48700cm2/g;
其中,氧化物溶剂为CaO+MgO+Fe2O3+Na2O+K2O。
S1中陶粒原料粉末用80目筛子筛分取粒度小于80目的筛下物。
S5中得到的改性陶粒对Pb2+的吸附率达到90%以上。
在具体实施过程中,按如下步骤:
S1:将10g陶粒原料研成粉末(粒度小于80目)后,置于三颈烧瓶中并加入超纯水30mL,再取氢氧化钠粉末加入三颈烧瓶中,将溶液的pH值调节为12~13;
S2:在室温下,将三颈烧瓶置于磁力搅拌器中搅拌10~15分钟,随后加入20mL甲醛溶液,搅拌均匀;
S3:将KI2型的烧瓶加热器温度设定为90℃,将三颈烧瓶置于其中,使其自然反应2.5~3小时;
S4:到达预设反应时间后,将三颈烧瓶取出并自然冷却,待温度降到40~45℃以下时,将20mL二硫化碳溶液和0.5gNaOH粉末同时加入三颈烧瓶中并搅拌均匀,自然反应2~3小时;
S5:到达预设反应时间后,向三颈烧瓶中加入0.1mol/L的盐酸,直至溶液pH为中性,搅拌均匀后静置4.5~6小时,三颈烧瓶中出现棕黑色沉淀;
S6:将S5中得到的沉淀用超纯水冲洗3~5分钟,待滤液颜色接近透明且滤液的pH值为7.0~7.3时,将沉淀物用冷冻干燥机收集,即得到改性陶粒。
改性陶粒分为改性后陶粒1和改性后陶粒2两组,在试验过程中,为确保结果的准确,改性后陶粒1和改性后陶粒2采用不同的样品量进行分析,如图2所示,分别为改性前陶粒颗粒表面的官能团红外光谱分析情况、改性后陶粒1(pH调节为12-13)颗粒表面的官能团红外光谱分析情况和改性后陶粒2(pH调节为12-13)颗粒表面的官能团红外光谱分析情况。在光谱735cm-1时,改性后陶粒1和2均比改性前陶粒多出了O-S官能团,在光谱649cm-1时,改性后陶粒1和2均比改性前陶粒多出了C-S官能团,因此表明改性后陶粒的表面成功携带了含S官能团。
如图3所示,为改性前后陶粒对Pb2+的吸附平衡曲线,改性前陶粒对Pb2+的平衡吸附量为0.283mg/g,改性后的吸附量可达0.55mg/g。吸附效率也可从47%提高到92%。
以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明所述原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。

Claims (3)

1.一种制备吸附pb2+的污泥基改性陶粒的方法,其特征在于,包括步骤如下:
S1:将陶粒原料研成粉末后,置于三颈烧瓶中并加入超纯水,再取氢氧化钠粉末加入三颈烧瓶中,将溶液的pH值调节为12~13;
S2:在室温下,将三颈烧瓶置于磁力搅拌器中搅拌10~15分钟,随后加入甲醛溶液,搅拌均匀;
S3:将KI2型的烧瓶加热器温度设定为90℃,将三颈烧瓶置于其中,使其自然反应2.5~3小时;
S4:到达预设反应时间后,将三颈烧瓶取出并自然冷却,待温度降到40~45℃以下时,将二硫化碳溶液和NaOH粉末同时加入三颈烧瓶中并搅拌均匀,自然反应2~3小时;
S5:到达预设反应时间后,向三颈烧瓶中加入0.1-0.2mol/L的盐酸,搅拌均匀后静置4.5~6小时,三颈烧瓶中出现棕黑色沉淀;
S6:将S5中得到的沉淀用超纯水冲洗3~5分钟,待滤液颜色接近透明且滤液的pH值为7.0~7.3时,将沉淀物用冷冻干燥机收集,即得到改性陶粒,改性陶粒表面附着含硫官能团,从而有效提升污泥基陶粒对Pb2+的吸附特性;
所述陶粒原料化学成分SiO2、Al2O3、氧化物溶剂总和满足Riley相图;陶粒比表面积大于48700cm2/g;
其中,氧化物溶剂为CaO+MgO+Fe2O3+Na2O+K2O;
所述S5中得到的改性陶粒对Pb2+的吸附率达到90%以上;
所述S1中陶粒原料和超纯水的质量比为1:3~1:4;
所述S2中甲醛溶液的加入量为2mL-3mL/g陶粒;
所述S4中二硫化碳溶液的加入量为2mL-3mL/g陶粒,NaOH粉末的加入量为0.025-0.05g/g陶粒。
2.根据权利要求1所述的制备吸附pb2+的污泥基改性陶粒的方法,其特征在于,所述S1中陶粒原料粉末粒度小于80目。
3.根据权利要求1所述的制备吸附pb2+的污泥基改性陶粒的方法,其特征在于,所述S5中加入盐酸,直至溶液为中性。
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