CN110372330A - 一种基于市政污泥的多孔磁性陶粒及其制备方法和应用 - Google Patents
一种基于市政污泥的多孔磁性陶粒及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开一种基于市政污泥的多孔磁性陶粒及其制备方法和应用,包括以下重量份原料:市政污泥100份、铝矾土6‑10份、硅藻土4‑8份、粉煤灰2‑6份、环戊二烯基铁0.01‑0.1份、硅酸镁锂1‑2份、硝酸铁0.1‑1份、硝酸钴0.1‑0.3份、硝酸镍0.1‑1份、造孔剂1‑3份;其制备方法如下:(1)酸浸煮市政污泥、铝矾土等原料;(2)氨水调节PH至8.4‑9.2,加入硝酸盐进行陈化;(3)制陶粒生料;(4)烧结陶粒。本发明采用一步法直接制备磁性纳米Fe2O3/Co3O4/NiO负载的多孔陶粒,不需要采用铁盐、镍盐、钴盐复合的前驱体溶液预先浸渍,方法简单,操作便捷,负载量更高,适宜大规模工业生产,同时可使纳米颗粒稳定分布于陶粒网络结构中,形成均一体系,避免纳米颗粒的分层、脱落。
Description
技术领域
本发明属于污泥资源化再生利用技术领域,还涉及功能型陶粒领域,具体涉及一种基于市政污泥的多孔磁性陶粒及其制备方法和应用。
背景技术
市政污泥是市政污水处理过程产生的副产物,随着我国经济的快速增长和城镇化进程的不断推进,市政污泥的产量逐年递增,到2020年,我国市政污泥年产量预计达6000-9000万吨。目前,市政污泥的资源化利用水平较低,其处理手段主要包括焚烧、卫生填埋、农业堆肥、消化制沼气等,焚烧和卫生填埋对空气和土壤均带来不同程度的二次污染,难以真正实现市政污泥的无公害、无污染、资源化利用,由于市政污泥的有机质含量较低,仅25%左右,应用于堆肥化技术和燃料化技术,产品产率极低。
陶粒是一种在回转窑中经发泡生产的轻骨料,内部呈蜂窝状,密度低、热导率低、强度高,多以煤、黏土、亚黏土、黏土质页岩等为原料,为不可再生资源,若以市政污泥为原料烧结陶粒,不仅实现污泥的减量化、资源化、无害化处理,同时,大大减少了不可再生资源的开采与浪费。
纳米磁性材料是一种特殊的磁学性质的材料,纳米粒子尺寸小,具有单磁畴结构和矫顽力很高的特性,在生物医药、光催化、宽频吸收、电声器件、阻尼器件、旋转密封及润滑和选矿等领域都有重要的应用,因此,利用纳米磁性材料对陶粒进行修饰,可赋予陶粒特殊功能及磁分离性质,具有较高的经济和生态环境效应。
发明内容
针对现有技术的不足之处,本发明的目的在于提供一种基于市政污泥的多孔磁性陶粒及其制备方法和应用。
本发明的技术方案概述如下:
一种基于市政污泥的多孔磁性陶粒,包括以下重量份原料:市政污泥100份、铝矾土6-10份、硅藻土4-8份、粉煤灰2-6份、环戊二烯基铁0.01-0.1份、硅酸镁锂1-2份、硝酸铁0.1-1份、硝酸钴0.1-0.3份、硝酸镍0.1-1份、造孔剂1-3份。
优选的是,所述造孔剂由碳酸锌、三氮化钠、方解石粉按1:0.5:1.5的质量比混合而成。
一种基于市政污泥的多孔磁性陶粒的制备方法,包括以下步骤:
(1)将市政污泥压滤至含水量为55-60%,加入铝矾土、硅藻土、粉煤灰,搅拌均匀后,加酸调节PH至5-6,60-80℃浸煮2-6h,得预处理混合料;
(2)向预处理混合料中加入氨水,调节PH至8.4-9.2,再加入硝酸铁、硝酸钴、硝酸镍,35-40℃搅拌反应2-6h,再静置陈化12-24h,得陈化混合料;
(3)向陈化混合料中加入环戊二烯基铁、硅酸镁锂、发泡剂,混合均匀后,挤压成粒径为1-6mm的陶粒生料;
(4)80-100℃干燥陶粒生料至含水量≦10%,升温至300-320℃,预热0.5h,以完成发泡剂的初步分解及氧化还原过程,再升温至400-450℃,保温1-1.5h,以完成氢氧化铁、氢氧化钴、氢氧化镍的热解过程,再升温至950-1250℃烧结0.5-1h,以完成发泡剂的二次分解,自然冷却至室温后,制得成品多孔磁性陶粒。
优选的是,所述氨水浓度为25-28%。
优选的是,所述挤压压力为10-25MPa。
优选的是,所述升温速率为5-10℃/min。
一种基于市政污泥的多孔磁性陶粒在废水处理中的应用。
一种基于市政污泥的多孔磁性陶粒在土壤改良中的应用。
一种基于市政污泥的多孔磁性陶粒在催化剂载体的应用。
本发明的有益效果:
(1)本发明采用一步法直接制备磁性纳米Fe2O3/Co3O4/NiO负载的多孔陶粒,不需要采用铁盐、镍盐、钴盐复合的前驱体溶液预先浸渍,方法简单,操作便捷,负载量更高,适合大规模工业生产,同时,浸渍法主要将纳米磁性颗粒固定于陶粒表面或孔洞中,结构稳定性较差,纳米颗粒易脱落,直接掺杂的方式可使纳米颗粒稳定分布于陶粒网络结构中,进而形成均一体系,避免纳米颗粒的分层、脱落。
(2)本发明以市政污泥为主料,以铝矾土、硅藻土和粉煤灰为辅料,生产多孔磁性陶粒,原料来源广,成本低廉,减少不可再生资源的开发与浪费,制出的功能型陶粒可应用于废水处理、土壤改良、催化剂载体等领域,以废制废,环境友好,不会造成二次污染,具有极高的经济和生态环境效应。
(3)本发明的造孔剂通过不同组分的合理复配使多孔磁性陶粒完成两个阶段造孔过程,极大地提高了多孔磁性陶粒的孔隙率和比表面积。在烧结过程中,300-330℃预热陶粒生料时,碳酸锌发生热分解反应,释放CO2,与此同时,三氮化钠与空气中的氧气发生氧化还原反应,生成大量N2,完成造孔剂的第一次造孔过程,之后950-1250℃焙烧,完成方解石的热分解反应,产生CO2,完成发泡剂的第二次造孔过程。
具体实施方式
下面结合实施例对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。
本发明提供一实施例的基于市政污泥的多孔磁性陶粒,该多孔磁性陶粒以100份市政污泥为主料,以6-10份铝矾土、4-8份硅藻土和2-6份粉煤灰为辅料,原料来源广,成本低廉,减少不可再生资源的开发与浪费,制出的功能型陶粒可应用于废水处理、土壤改良、催化剂载体等领域,以废制废,环境友好,不会造成二次污染,具有极高的经济和生态环境效应;
该多孔磁性陶粒还包括环戊二烯基铁,作为消烟添加剂,减少在烧结过程中有毒烟雾及飞灰的产生,同时作为陶粒膨胀剂,提高陶粒烧结过程的发泡效率,其较优的重量份区间为0.01-0.1份;
该多孔磁性陶粒还包括硅酸镁锂,作为增稠剂,提高原料间的粘结强度,进而加强陶粒的结构强度,并提高陶粒的吸附性能,其较优的重量份区间为1-2份;
该多孔磁性陶粒以硝酸铁、硝酸钴、硝酸镍作为纳米磁性材料的前体物质,一步法直接制备磁性纳米Fe2O3/Co3O4/NiO负载的多孔陶粒,不需要采用铁盐、镍盐、钴盐复合的前驱体溶液预先浸渍,方法简单,操作便捷,负载量更高,适合大规模工业生产,同时,浸渍法主要将纳米磁性颗粒固定于陶粒表面或孔洞中,结构稳定性较差,纳米颗粒易脱落,直接掺杂的方式可使纳米颗粒稳定分布于陶粒网络结构中,进而形成均一体系,避免纳米颗粒的分层、脱落,三者存在的较优的重量份区间分别为0.1-1份、0.1-0.3份、0.1-1份;
该多孔磁性陶粒还包括1-3份造孔剂,所述造孔剂由碳酸锌、三氮化钠、方解石粉按1:0.5:1.5的质量比混合而成,通过不同组分的合理复配使多孔磁性陶粒完成两个阶段造孔过程,极大地提高了多孔磁性陶粒的孔隙率和比表面积;在烧结过程中,300-330℃预热陶粒生料时,碳酸锌发生热分解反应,释放CO2,与此同时,三氮化钠与空气中的氧气发生氧化还原反应,生成大量N2,完成造孔剂的第一次造孔过程,之后950-1250℃焙烧,完成方解石的热分解反应,产生CO2,完成发泡剂的第二次造孔过程。
所述基于市政污泥的多孔磁性陶粒的制备方法,包括以下步骤:
(1)将市政污泥压滤至含水量为55-60%,加入铝矾土、硅藻土、粉煤灰,搅拌均匀后,加酸调节PH至5-6,60-80℃浸煮2-6h,得预处理混合料;
(2)向预处理混合料中加入25-28%氨水,调节PH至8.4-9.2,再加入硝酸铁、硝酸钴、硝酸镍,35-40℃搅拌反应2-6h,再静置陈化12-24h,得陈化混合料;
(3)向陈化混合料中加入环戊二烯基铁、硅酸镁锂、造孔剂,混合均匀后,以10-25MPa压力挤压成粒径为1-6mm的陶粒生料;
(4)80-100℃干燥陶粒生料至含水量≦10%,以5-10℃/min速率升温至300-320℃,预热0.5h,以完成造孔剂的初步分解及氧化还原过程,以5-10℃/min速率再升温至400-450℃,保温1-1.5h,以完成氢氧化铁、氢氧化钴、氢氧化镍的热解过程,以5-10℃/min速率再升温至950-1250℃烧结0.5-1h,以完成发泡剂的二次分解,自然冷却至室温后,制得成品多孔磁性陶粒。
实施例1制备陶粒生料
S1:按1:0.5:1.5的质量比混合碳酸锌、三氮化钠、方解石粉,得造孔剂;
S2:将100份市政污泥压滤至含水量为55%,加入8份铝矾土、6份硅藻土、4份粉煤灰,搅拌均匀后,加酸调节PH至5.5,70℃浸煮4h,得预处理混合料;
S3:向所得预处理混合料中加入27%氨水,调节PH至8.8,再加入0.5份硝酸铁、0.2份硝酸钴、0.5份硝酸镍,38℃搅拌反应4h,再静置陈化18h,得陈化混合料;
S4:向陈化混合料中加入0.05份环戊二烯基铁、1.5份硅酸镁锂、2份造孔剂,混合均匀后,以18MPa挤压成粒径为3.5mm的陶粒生料。
实施例2烧结多孔磁性陶粒
90℃干燥陶粒生料至含水量≦10%,以7.5℃/min的速率进行升温,先升温至310℃,预热0.5h,以完成造孔剂的初步分解及氧化还原过程,再升温至425℃,保温1.5h,以完成氢氧化铁、氢氧化钴、氢氧化镍的热解过程,再升温至1100℃烧结1h,以完成发泡剂的二次分解,自然冷却至室温后,制得成品多孔磁性陶粒。
实施例3对实施例2制出的多孔磁性陶粒进行性能检测
试验结果如下所示:磁性纳米颗粒的平均粒径为12.7nm、堆积密度为358.2kg/m3、抗压强度为29.4MPa、孔隙率为76.3%、吸水率为7.5%,可广泛应用于废水处理、土壤改良及催化剂载体领域。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。
Claims (9)
1.一种基于市政污泥的多孔磁性陶粒,其特征在于,包括以下重量份原料:市政污泥100份、铝矾土6-10份、硅藻土4-8份、粉煤灰2-6份、环戊二烯基铁0.01-0.1份、硅酸镁锂1-2份、硝酸铁0.1-1份、硝酸钴0.1-0.3份、硝酸镍0.1-1份、造孔剂1-3份。
2.根据权利要求1所述一种基于市政污泥的多孔磁性陶粒,其特征在于,所述造孔剂由碳酸锌、三氮化钠、方解石粉按1:0.5:1.5的质量比混合而成。
3.一种基于市政污泥的多孔磁性陶粒的制备方法,其特征在于,包括以下步骤:
(1)将市政污泥压滤至含水量为55-60%,加入铝矾土、硅藻土、粉煤灰,搅拌均匀后,加酸调节PH至5-6,60-80℃浸煮2-6h,得预处理混合料;
(2)向预处理混合料中加入氨水,调节PH至8.4-9.2,再加入硝酸铁、硝酸钴、硝酸镍,35-40℃搅拌反应2-6h,再静置陈化12-24h,得陈化混合料;
(3)向陈化混合料中加入环戊二烯基铁、硅酸镁锂、造孔剂,混合均匀后,挤压成粒径为1-6mm的陶粒生料;
(4)80-100℃干燥陶粒生料至含水量≦10%,升温至300-320℃,预热0.5h,以完成造孔剂的初步分解及氧化还原过程,再升温至400-450℃,保温1-1.5h,以完成氢氧化铁、氢氧化钴、氢氧化镍的热解过程,再升温至950-1250℃烧结0.5-1h,以完成发泡剂的二次分解,自然冷却至室温后,制得成品多孔磁性陶粒。
4.根据权利要求3所述一种基于市政污泥的多孔磁性陶粒的制备方法,其特征在于,所述氨水浓度为25-28%。
5.根据权利要求3所述一种基于市政污泥的多孔磁性陶粒的制备方法,其特征在于,所述挤压压力为10-25MPa。
6.根据权利要求3所述一种基于市政污泥的多孔磁性陶粒的制备方法,其特征在于,所述升温速率为5-10℃/min。
7.一种基于市政污泥的多孔磁性陶粒在废水处理中的应用。
8.一种基于市政污泥的多孔磁性陶粒在土壤改良中的应用。
9.一种基于市政污泥的多孔磁性陶粒在催化剂载体的应用。
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Application publication date: 20191025 |