CN111701578A - 一种污水处理用吸附剂及其制备方法 - Google Patents
一种污水处理用吸附剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及污水处理技术领域,具体公开了一种污水处理用吸附剂的制备方法,包括以下步骤:将膨润土、硅藻土和凹凸棒土混合,高温煅烧,然后放入盐酸溶液中超声处理,得到活化无机非金属矿材料;然后加入乙醇配制成悬浮液,加入硅烷偶联剂,在70~80℃搅拌1~2h,收集沉淀物;将淀粉配制成浆液,加入沉淀物混合均匀,加入尿素搅拌反应,添加三聚磷酸钠混合得混合物,干燥至混合物含水量为10~20%,升温至135~150℃反应1~2h,得到改性吸附粉末;将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂。本发明的污水处理用吸附剂具有比表面积大、含有多个吸附活性位点,能吸附去除废水中的重金属、氨氮、磷、有机污染物等多种污染物质,具有好的吸附效果。
Description
技术领域
本发明属于污水处理技术领域,特别涉及一种污水处理用吸附剂及其制备方法。
背景技术
工业污水是指工业生产过程中产生的废水和废液,其中含有随水流失的工业生产用料、中间产物和产品以及生产过程中产生的污染物。随着工业的迅速发展,污水的种类和数量迅猛增加,对水体的污染也日趋广泛和严重,威胁人类的健康和安全。工业污水含有多种污染物质:重金属离子、无机非金属污染物(氨氮、磷等)、有机污染物等等,目前污水处理的方法主要有:化学氧化法、絮凝沉淀法、生物法和物理吸附法等。其中化学氧化法可以污染物的结构实现对污水的处理,但其在处理过程中会产生较多的化学污泥且可能生成毒性更大的中间产物;絮凝沉淀法药剂用量大、操作复杂、污泥量大;生物法需要进行需要控制生化性且占地面积大;吸附法是应用多孔性固体吸附剂,通过范德华力和化学键作用,实现对污水中污染物有效去除的一种水处理技术。吸附法具有操作简单、吸附剂廉价易得、去除效果优、不产生二次污染等优点。寻求吸附量大、低毒无残留、再生能力强的吸附剂成为目前的研究热点。无机非金属矿材料(如膨润土、硅藻土、凹凸棒土等)具有独特的结构而具有良好的吸附和离子交换性能,且其储量大、价格低廉,在污水处理中具有广阔的应用前景。但是无机非金属矿材料原矿存在杂质较多、微孔堵塞、吸附点位较少等缺陷,使得其吸附性能较差,吸附率低。
发明内容
本发明的目的在于提供一种污水处理用吸附剂的制备方法,制得的吸附剂的吸附性能好,对污水中污染物去除效果佳。
为实现上述目的,本发明提供了一种污水处理用吸附剂的制备方法,包括以下步骤:
(1)按重量份计,将膨润土20~30份、硅藻土10~20份和凹凸棒土10~20份混合,在400~500℃下煅烧2~3h,研磨成200~300目粉末,然后放入浓度为3~5mol/L盐酸溶液中,超声1~2h,得到活化无机非金属矿材料;
(2)在步骤(1)的活化无机非金属矿材料中加入乙醇配制成固含量10~20%悬浮液,加入硅烷偶联剂,在70~80℃搅拌1~2h,收集沉淀物,洗涤烘干;
(3)将淀粉加水配制成固含量为5~10%的浆液,然后加入步骤(2)的沉淀物混合均匀,加入尿素搅拌30~60min,添加三聚磷酸钠混合均匀得到混合物,在40~50℃下鼓风干燥至混合物含水量为10~20%,升温至135~150℃反应1~2h,将反应产物进行洗涤,烘干,得到改性吸附粉末;
(4)将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂。
高温煅烧具有清理无机非金属矿材料表面和微孔内的杂质、增加无机非金属矿材料的比表面积和吸附点位,通过酸化处理打通内部孔穴,进一步增大了比表面积;然后通过偶联剂对活化的无机非金属矿材料进行修饰,使得淀粉能够吸附固定在材料表面,加入尿素能够与淀粉大分子上的多个羟基形成氢键,使淀粉交缠的结构舒展,促进淀粉吸附固定在粘土材料上,尿素还具有催化作用,提高后续反应速率,加入三聚磷酸钠,进行热处理后,引入了阴离子基团磷酸酯基和酰胺基团等活性基团,增加了吸附活性位点,提高吸附性能。
优选的,上述制备方法中,所述硅烷偶联剂为氨丙基三乙氧基硅烷,所述硅烷偶联剂的加入量为所述活化无机非金属矿材料质量的0.3~0.6%。
优选的,上述制备方法中,所述步骤(3)中,沉淀物与淀粉的质量比为4~6:1。
优选的,上述制备方法中,所述步骤(3)中,尿素的加入量为淀粉质量的1~2%,三聚磷酸钠的加入量为淀粉质量的3~6%。
优选的,上述制备方法中,所述步骤(4)中,改性吸附粉末与纳米氢氧化钙、活性炭的质量比为5:1~2:0.5~1。
上述的制备方法制得的污水处理用吸附剂。
污水处理用吸附剂的使用方法,调节工业废水pH至5.0~7.0,每1L工业废水加入2~5g,振荡1~2h,静置30min进行废水处理。
与现有的技术相比,本发明具有如下有益效果:
1.本发明的污水处理用吸附剂具有比表面积大、含有多个吸附活性位点,能吸附去除废水中的重金属、氨氮、磷、有机污染物等多种污染物质,具有好的吸附效果,高的吸附效率。
2.本发明的制备方法中结合膨润土、硅藻土和凹凸棒土三种无机非金属矿材料,对其进行改性形成多个吸附点,通过不同吸附作用和吸附点实现对多种污染物进行吸附。通过高温煅烧和酸化处理增加非金属矿材料的比表面积和吸附点位,通过酸化处理打通了内部孔穴,进一步增大了比表面积,然后在非金属矿材料吸附固定淀粉,引入阴离子基团磷酸酯基和酰胺基团等活性基团,增加了吸附活性位点,提高改性吸附粉末吸附性能。
具体实施方式
下面对本发明的具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。
实施例1
一种污水处理用吸附剂的制备方法,具体包括以下步骤:
(1)按重量份计,将膨润土30份、硅藻土15份和凹凸棒土15份混合,在450℃下煅烧3h,研磨成200~300目粉末,然后放入浓度为5mol/L盐酸溶液中,超声2h,得到活化无机非金属矿材料;
(2)在步骤(1)的活化无机非金属矿材料中加入乙醇配制成固含量为18%悬浮液,加入活化无机非金属矿材料质量的0.5%氨丙基三乙氧基硅烷,在70℃搅拌1.5h,离心收集沉淀物,采用乙醇洗涤3次,在90℃烘干;
(3)将淀粉加水配制成固含量为5%的浆液,然后加入步骤(2)的沉淀物混合均匀,沉淀物与淀粉的质量比为4:1,加入淀粉质量的2%尿素搅拌40min,添加淀粉质量的5%三聚磷酸钠混合均匀得到混合物,在50℃下鼓风干燥至混合物含水量为15%,升温至135℃反应2h,将反应产物进行洗涤,100℃下烘干,得到改性吸附粉末;
(4)将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂,改性粉末与纳米氢氧化钙、活性炭的质量比为5:1:0.8。
硅藻土主要成分是硅酸质,表面有大量多级有序排列的微孔,比表面积大,吸附能力强,其Zeta电位较负,吸附正电荷的能力强。膨润土的主要成分为蒙脱石,基本结构单元为两层硅氧四面体夹一层铝氧八面体组成,由于发生同晶取代现象,八面体空隙中的Al3+被Mg2+置换,四面体空隙中的Si4+被Al3+代替,使结构层产生多余的负电荷,使得膨润土具有较强的吸附性和离子交换性。蒙脱石结构单元层边缘上由于Si-O-H键、Al-O-H键的断裂而带正电荷或者负电荷,使得膨润土可以吸附阴离子或者阳离子。凹凸棒土具有独特的链式结构,使得凹凸棒土具有大量的微孔道和很大的比表面积,具有很强的吸附能力,凹凸棒土的吸附主要为电荷不平衡引起的吸附和Si-O-Si中氧硅键的断裂可以与被吸附的物质形成共价键,产生较强的吸附能力。结合这三种无机非金属矿材料,对其进行改性,通过不同吸附作用和多个吸附点实现对多种污染物进行吸附。
实施例2
一种污水处理用吸附剂的制备方法,具体包括以下步骤:
(1)按重量份计,将膨润土22份、硅藻土20份和凹凸棒土18份混合,在450℃下煅烧3h,研磨成200~300目粉末,然后放入浓度为3mol/L盐酸溶液中,超声2h,得到活化无机非金属矿材料;
(2)在步骤(1)的活化无机非金属矿材料中加入乙醇配制成固含量为10%悬浮液,加入活化无机非金属矿材料质量的0.6%氨丙基三乙氧基硅烷,在70℃搅拌1.5h,离心收集沉淀物,采用乙醇洗涤3次,在90℃烘干;
(3)将淀粉加水配制成固含量为10%的浆液,然后加入步骤(2)的沉淀物混合均匀,沉淀物与淀粉的质量比为5:1,加入淀粉质量的1.5%尿素搅拌40min,添加淀粉质量的6%三聚磷酸钠混合均匀得到混合物,在50℃下鼓风干燥至混合物含水量为15%,升温至140℃反应2h,将反应产物进行洗涤,100℃下烘干,得到改性吸附粉末;
(4)将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂,改性粉末与纳米氢氧化钙、活性炭的质量比为5:2:0.5。
实施例3
一种污水处理用吸附剂的制备方法,具体包括以下步骤:
(1)按重量份计,将膨润土25份、硅藻土10份和凹凸棒土15份混合,在500℃下煅烧2h,研磨成200~300目粉末,然后放入浓度为3.5mol/L盐酸溶液中,超声2h,得到活化无机非金属矿材料;
(2)在步骤(1)的活化无机非金属矿材料中加入乙醇配制成固含量为15%悬浮液,加入活化无机非金属矿材料质量的0.3%氨丙基三乙氧基硅烷,在80℃搅拌1h,离心收集沉淀物,采用乙醇洗涤3次,在100℃烘干;
(3)将淀粉加水配制成固含量为8%的浆液,然后加入步骤(2)的沉淀物混合均匀,沉淀物与淀粉的质量比为6:1,加入淀粉质量的1%尿素搅拌40min,添加淀粉质量的4%三聚磷酸钠混合均匀得到混合物,在50℃下鼓风干燥至混合物含水量为20%,升温至150℃反应1h,将反应产物进行洗涤,100℃下烘干,得到改性吸附粉末;
(4)将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂,改性粉末与纳米氢氧化钙、活性炭的质量比为5:1:1。
对比例1
一种污水处理用吸附剂,按重量份计,将膨润土30份、硅藻土15份和凹凸棒土15份混合,在450℃下煅烧3h,研磨成200~300目粉末,然后放入浓度为5mol/L盐酸溶液中,超声2h制得的。
对比例2
本对比例的污水处理用吸附剂的制备方法与实施例1不同之处在于:采用乙烯基三乙氧基硅烷替换氨丙基三乙氧基硅烷作为硅烷偶联剂,其他步骤和参数与实施例1完全相同。
将本发明实施例1~3和对比例1~2制得的污水处理用吸附剂用于废水处理,废水为随机采样的工业废水,工业废水中含有重金属离子、有机废物等污染物,重金属的含量为71.5mg/L,氨氮含量为145.8mg/L,磷含量为6.2mg/L,COD(化学需氧量)为630.1mg/L。调节工业废水pH至5.0,每1L工业废水加入3g,振荡2h,静置30min进行废水处理,过滤沉淀,完成对废水净化。
表1污水处理用吸附剂对废水中的污染物去除效果
表1为各处理药剂对废水中的污染物去除效果,由表可知,本发明的复合污水处理药剂具有高效净化能力,对重金属离子的去除率达到98%以上,氨氮去除率达到94%以上,磷去除率在91%以上,COD去除率在93%以上。本发明的污水处理用吸附剂能够吸附多种污染物,对污水的处理效果好,时间短,效率高。
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式,并且很显然,根据上述教导,可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用,从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。
Claims (7)
1.一种污水处理用吸附剂的制备方法,其特征在于,包括以下步骤:
(1)按重量份计,将膨润土20~30份、硅藻土10~20份和凹凸棒土10~20份混合,在400~500℃下煅烧2~3h,研磨成200~300目粉末,然后放入浓度为3~5mol/L盐酸溶液中,超声1~2h,得到活化无机非金属矿材料;
(2)在步骤(1)的活化无机非金属矿材料中加入乙醇配制成固含量为10~20%悬浮液,加入硅烷偶联剂,在70~80℃搅拌1~2h,收集沉淀物,洗涤烘干;
(3)将淀粉加水配制成固含量为5~10%的浆液,然后加入步骤(2)的沉淀物混合均匀,加入尿素搅拌30~60min,添加三聚磷酸钠混合均匀得到混合物,在40~50℃下鼓风干燥至混合物含水量为10~20%,升温至135~150℃反应1~2h,将反应产物进行洗涤,烘干,得到改性吸附粉末;
(4)将改性吸附粉末与纳米氢氧化钙、活性炭混合得到污水处理用吸附剂。
2.根据权利要求1所述的制备方法,其特征在于,所述硅烷偶联剂为氨丙基三乙氧基硅烷,所述硅烷偶联剂的加入量为所述活化无机非金属矿材料质量的0.3~0.6%。
3.根据权利要求1所述的制备方法,其特征在于,所述步骤(3)中,沉淀物与淀粉的质量比为4~6:1。
4.根据权利要求1所述的制备方法,其特征在于,所述步骤(3)中,尿素的加入量为淀粉质量的1~2%,三聚磷酸钠的加入量为淀粉质量的3~6%。
5.根据权利要求1所述的制备方法,其特征在于,所述步骤(4)中,改性吸附粉末与纳米氢氧化钙、活性炭的质量比为5:1~2:0.5~1。
6.如权利要求1~5任一项所述的制备方法制得的污水处理用吸附剂。
7.如权利要求6所述的污水处理用吸附剂的使用方法,其特征在于,调节工业废水pH至5.0~7.0,每1L工业废水加入2~5g,振荡1~2h,静置30min进行废水处理。
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