CN107032758B - 一种利用污泥和牛粪制备气体净化多孔陶瓷的方法 - Google Patents
一种利用污泥和牛粪制备气体净化多孔陶瓷的方法 Download PDFInfo
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Abstract
一种利用污泥和牛粪制备气体净化多孔陶瓷的方法，该方法包括如下步骤：取剩余污泥、畜禽粪便、双氧水、硅藻土和硝酸溶液，加热，得到固体A和液体A；将固体A浸泡并加热，调整溶液的pH值，得到固体B和液体B；将液体A调pH值，得到固体C和液体C；将固体C和B混合，烘干球磨，烘干煅烧，得到多孔陶瓷材料；将多孔陶瓷材料浸泡于液体B中，浓缩干燥，浸泡于浓磷酸中，静置，取出，炭化活化，得到载炭多孔陶瓷；将液体C浓缩，加入催化剂，加入脲和乙烯脲，将多孔陶瓷浸泡于该悬浊液中，超声振荡，静置吸附，取出多孔陶瓷，烘干，得到多孔陶瓷，回收浸泡液即为复合肥。本发明节能环保，具有很高的环境效益和经济效益。
Description
技术领域
本发明属于环境生态技术领域，具体涉及一种利用污泥和牛粪制备气体净化多孔陶瓷的方法。
背景技术
污水处理厂排放的大量的剩余污泥和养殖业排放的畜禽粪便都是富含有机物和重金属等有害物质的固体废弃物。目前，各国对于污泥，常采用卫生填埋、焚烧和堆肥等方法处理；而畜禽粪便常用于生产有机肥料。但是卫生填埋需要大量的土地，也存在着环境安全隐患，焚烧法成本高，污染空气，堆肥和制作有机肥料难以解决重金属污染问题。李志光等采用双氧水等为氧化剂，金属氧化物和粉煤灰等的混合物为氧化导向剂，对污泥进行处理，降低了污泥的水分和化学需氧量，但是该方法没有彻底解决污泥的污染问题，污泥中的有用物质没有回收利用(发明专利，申请号201210562724.6，一种处理污泥的方法)；污泥的资源化利用是最理想的方案，将污泥作为一种成分添加烧制建筑用砖，制水泥，制陶瓷和制备活性炭等(李鸿江等，污泥资源化利用技术，冶金工业出版社，2010年；周中德，发明专利，污泥环保砌块，授权公告号CN 102627433 B)。在烧制水泥、制砖和烧制陶粒应用技术中，都是将干缩污泥直接加入，这样受产品有害物质限量的影响，使用过程中污泥的添加量有限，而且污泥中有用的蛋白质类物质直接烧掉，没有得到利用；污泥制活性炭杂质高，产率低。而在畜禽粪便利用方面，曹进(发明专利，申请号：201310511848.6，一种利用畜禽粪便生产有机肥料的方法)采用向畜禽粪便中添加吸附剂，混合后发酵的方法，制备有机肥；李荣华(李荣华，西北农林科技大学，博士学位论文，添加重金属钝化剂对猪粪好氧堆肥的影响研究，2013)采用玉米秸秆为调理剂，以工业废弃物粉煤灰、风化煤和膨润土为重金属钝化剂，发酵处理畜禽粪便，等等。这些仅仅依靠发酵的方法不能有效去除抗生素等有害物质，对重金属的钝化只是临时改变了重金属的状态，重金属依然存在粪肥中，依然存在着环境风险。近年来，一些养牛企业，将牛粪焚烧发电，但是，牛粪中含水率较高，需要干燥处理，耗费能源，同时，牛粪中含有的纤维素、木质素、蛋白质和胶体物质以及金属等物质都被烧掉，探索综合利用这些有用成分，是处理牛粪的最佳选择。
发明内容
本发明的目的是，提供一种利用污泥和牛粪制备气体净化多孔陶瓷的方法。污泥中含有以微生物残体为主的有机物，还含有一定量的重金属等有害物质；牛粪中含有大量的纤维素和木质素以及蛋白质和胶体物质，也含有一定量的金属，将污泥和牛粪混合后用催化氧化法消灭微生物等有害物质，破坏污泥微生物细胞壁，充分提取氨基酸类物质，再通过酸提取金属，并生成氢氧化物沉淀，由于牛粪胶体物质的络合絮凝作用，使得牛粪和污泥中的重金属离子沉淀更为彻底；将各步骤提取的剩余物混合即可烧制多孔陶瓷材料，再将提取液中的催化剂等有效成分修饰于多孔陶瓷上，即可得到气体净化材料，可用于吸附分解净化甲醛和氮氧化物。处理和利用污泥和牛粪的同时制备高性能除甲醛和氮氧化物材料，污泥和牛粪中的各组分均得以充分利用，无二次污染，节能环保，具有很高的环境效益和经济效益。
采用的技术方案是
一种利用污泥和牛粪制备气体净化多孔陶瓷的方法，该方法包括如下步骤：
1)取新鲜的含水率均为80-85％的剩余污泥和牛粪，等质量混合，依次加入污泥和粪便总质量的10％-20％的质量百分含量为30％的双氧水、10％-30％的硅藻土，再按污泥和牛粪总质量与酸溶液体积比为1Kg:1L的比例，加入0.5-1mol/L的硝酸溶液，搅拌均匀，加热微沸10-20min，固液分离，得到固体A和液体A；
2)向固体A中加水至刚好浸没，用氢氧化钾调pH值11-12，并加热微沸30min，期间，调整溶液的pH值为11-12，固液分离，得到固体B和液体B；
3)将液体A用氨水调pH值为8-9，搅拌均匀，静置12h，固液分离，得到固体C和液体C；
4)将固体C和固体B混合，105-150℃烘干，球磨6-8h，润湿加压10-20MPa成型，60-90℃烘干，于1000-1250℃下煅烧，得到多孔陶瓷材料；
5)将步骤四得到的多孔陶瓷材料浸泡于步骤二得到的液体B中，超声振荡10min，加热继续浓缩，蒸发，干燥，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，隔绝空气条件下，于400-500℃炭化活化1h，得到载炭多孔陶瓷；
6)将液体C加热浓缩至近饱和，加入占液体C质量的1-5％纳米催化剂粉体，光辐照下搅拌60-120min后，加入液体C质量5-10％的脲和5-10％的乙烯脲，超声分散成悬浊液，将步骤五得到的载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡20-30min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去外表面残液，50℃真空烘干，得到去除甲醛和氮氧化物的多孔陶瓷，回收浸泡液即为农用复合肥。
所述的污泥为城市污水处理厂排放的剩余污泥。
所述的步骤四中煅烧方法为：以3.6℃/min的升温速度升到360℃,并在此温度下保温30min。再以5℃/min的速度继续升温到烧成温度,并保温10-20min，炉内冷却到室温。
所述的步骤六中加入的纳米催化剂粉体为纳米钛酸钙、纳米钛酸锶、纳米钒酸铋和纳米二氧化钛中的一种或几种。
本发明的优点在于，综合处理和利用污泥和牛粪的同时制备高性能除甲醛和氮氧化物材料，污泥和牛粪中的各组分均得以充分利用，无二次污染，节能环保，具有很高的环境效益和经济效益。
附图说明
图1为本方法的工艺流程图。
具体实施方式
本发明实施例中所用纳米钛酸钙粉体为本实验室按文献(张东,侯平.纳米钛酸钙粉体的制备及其对水中铅和镉的吸附行为[J].化学学报,2009,(12):1336-1342)方法合成；所用的纳米钒酸铋粉体是本实验室按文献(张东，等，一种高活性N-F共掺杂钒酸铋可见光光催化材料的合成方法，发明专利，ZL 201210105621.7)方法合成；所用纳米钛酸锶粉体为本实验室按文献(Dong zhang,etal,Synthesis of Strontium Titanate Microtubuleand Their Photocatalytic Activity for Degradation of Furfural in AqueousSolutions,J.Adv.Oxid.Technol.Vol.18,No.2,2015:221-226)方法合成；所用纳米二氧化钛是市售p25。
实施例1
取新鲜的含水率为81％的城市污水处理厂的剩余污泥1Kg与1Kg含水率为80％新鲜牛粪混合，依次加入300g质量百分含量为30％的双氧水、400g的硅藻土、1mol/L的硝酸溶液2L，搅拌均匀，加热微沸20min，抽滤，得到固体A和液体A；向固体A中加水至刚好浸没，用氢氧化钾调pH值11，并加热微沸30min，期间，调整并保持溶液的pH值11，抽滤，得到固体B和液体B；将液体A用氨水调pH值为8，搅拌均匀，静置12h，固液分离，得到固体C和液体C；将固体C和固体B混合，105℃烘干，球磨8h，润湿，加压10MPa成型，制成直径40mm，厚为3mm的圆片，80℃烘干，置于马弗炉中，以3.6℃/min的升温速度升到360℃,并在此温度下保温30min。再以5℃/min的速度继续升温到1050℃,并保温10min，炉内冷却到室温，得到多孔陶瓷材料；将多孔陶瓷材料浸泡于液体B中，超声振荡10min，加热继续浓缩，105℃烘干，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，置于真空马弗炉内，于450℃炭化活化1h，得到载炭多孔陶瓷；将液体C加热浓缩至近饱和，加入液体C质量的3％的纳米钛酸钙粉体，置于波长为254nm，辐照强度为100μW/cm2紫外光辐照下，搅拌120min后，加入液体C质量8％的脲和8％的乙烯脲，超声分散成悬浊液，将载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡20min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去表面残液，50℃真空烘干，得到可净化空气中甲醛和氮氧化物的多孔陶瓷1。
实施例2
取新鲜的含水率为85％的城市污水处理厂的剩余污泥1Kg与1Kg含水率为80％新鲜牛粪混合，依次加入200g质量百分含量为30％的双氧水、200g的硅藻土、0.5mol/L的硝酸溶液2L，搅拌均匀，加热微沸10min，抽滤，得到固体A和液体A；向固体A中加水至刚好浸没，用氢氧化钾调pH值12，并加热微沸30min，期间，调整并保持溶液的pH值为12，抽滤，得到固体B和液体B；将液体A用氨水调pH值为9，搅拌均匀，静置12h，固液分离得到固体C和液体C；将固体C和固体B混合，150℃烘干，球磨6h，润湿加压15MPa成型，制成直径40mm，厚为3mm的圆片，60℃烘干，置于马弗炉中，以3.6℃/min的升温速度升到360℃,并在此温度下保温30min,再以5℃/min的速度继续升温到1000℃,并保温10min，炉内冷却到室温，得到多孔陶瓷材料；将步骤四得到的多孔陶瓷材料浸泡于液体B中，超声振荡10min，加热继续浓缩，105℃烘干，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，置于真空马弗炉内，于450℃炭化活化1h，得到载炭多孔陶瓷；将液体C加热浓缩至近饱和，加入液体C质量的5％纳米钛酸锶粉体，置于波长为254nm，辐照强度为100μW/cm2紫外光辐照下，搅拌60min后，加入液体C质量5％的脲和5％的乙烯脲，超声分散成悬浊液，将载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡30min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去表面残液，50℃真空烘干，得到可净化空气中甲醛和氮氧化物的多孔陶瓷2。
实施例3
取新鲜的含水率为80％的城市污水处理厂的剩余污泥1Kg与1Kg含水率为85％新鲜牛粪混合，依次加入400g质量百分含量为30％的双氧水、300g的硅藻土、2L的0.8mol/L的硝酸溶液，搅拌均匀，加热微沸20min，抽滤，得到固体A和液体A；向固体A中加水至刚好浸没，用氢氧化钾调pH值11，并加热微沸30min，期间，调整并保持溶液的pH值为11，抽滤，得到固体B和液体B；将液体A用氨水调pH值为8，搅拌均匀，静置12h，固液分离得到固体C和液体C；将固体C和固体B混合，110℃烘干，球磨6h，润湿加压10MPa成型，制成直径40mm，厚为3mm的圆片，80℃烘干，置于马弗炉中，以3.6℃/min的升温速度升到360℃,并在此温度下保温30min，再以5℃/min的速度继续升温到1100℃,并保温10min，炉内冷却到室温，得到多孔陶瓷材料；将多孔陶瓷材料浸泡于液体B其中，超声振荡10min，加热继续浓缩，105℃烘干，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，置于真空马弗炉内，于400℃炭化活化1h，得到载炭多孔陶瓷；将液体C加热浓缩至近饱和，加入液体C质量的1％纳米钒酸铋粉体和1％的纳米钛酸钙粉体，置于250W的金属卤化物灯下，辐照强度为200LUX的光照条件下搅拌120min后，加入液体C质量10％的脲和10％的乙烯脲，超声分散成悬浊液，将载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡30min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去表面残液，50℃真空烘干，得到可净化空气中甲醛和氮氧化物的多孔陶瓷3。
实施例4
取新鲜的含水率为85％的城市污水处理厂的剩余污泥1Kg与1Kg含水率为85％新鲜牛粪混合，依次加入200g质量百分含量为30％的双氧水、600g的硅藻土、2L的0.5mol/L的硝酸溶液，搅拌均匀，加热微沸10min，抽滤，得到固体A和液体A；向固体A中加水至刚好浸没，用氢氧化钾调pH值12，并加热微沸30min，期间，调整并保持溶液的pH值为12，抽滤，得到固体B和液体B；将液体A用氨水调pH值为8，搅拌均匀，静置12h，固液分离得到固体C和液体C；将固体C和固体B混合，135℃烘干，球磨6h，润湿加压20MPa成型，制成直径40mm，厚为3mm的圆片，85℃烘干，置于马弗炉中，以3.6℃/min的升温速度升到360℃,并在此温度下保温30min，再以5℃/min的速度继续升温到1200℃，并保温10min，炉内冷却到室温，得到多孔陶瓷材料；将多孔陶瓷材料浸泡于液体B中，超声振荡10min，加热继续浓缩，105℃烘干，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，置于真空马弗炉内，于500℃炭化活化1h，得到载炭多孔陶瓷；将液体C加热浓缩至近饱和，加入液体C质量的2％纳米二氧化钛粉体，置于波长为254nm，辐照强度为100μW/cm2紫外光辐照下，搅拌120min后，加入液体C质量5％的脲和10％的乙烯脲，超声分散成悬浊液，将载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡30min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去表面残液，50℃真空烘干，得到可净化空气中甲醛和氮氧化物的多孔陶瓷4。
实施例5
取新鲜的含水率为80％的城市污水处理厂的剩余污泥1Kg与1Kg含水率为80％新鲜牛粪混合，依次加入300g质量百分含量为30％的双氧水、500g的硅藻土、2L的0.5mol/L的硝酸溶液，搅拌均匀，加热微沸10min，抽滤，得到固体A和液体A；向固体A中加水至刚好浸没，用氢氧化钾调pH值11，并加热微沸30min，期间，调整并保持溶液的pH值为11，抽滤，得到固体B和液体B；将液体A用氨水调pH值为8，搅拌均匀，静置12h，固液分离得到固体C和液体C；将固体C和固体B混合，145℃烘干，球磨8h，润湿加压15MPa成型，制成直径40mm，厚为3mm的圆片，90℃烘干，置于马弗炉中，以3.6℃/min的升温速度升到360℃,并在此温度下保温30min，再以5℃/min的速度继续升温到1250℃,并保温10min，炉内冷却到室温，得到多孔陶瓷材料；将多孔陶瓷材料浸泡于液体B中，超声振荡10min，加热继续浓缩，105℃烘干，浸泡于质量百分浓度为85％的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，置于真空马弗炉内，于450℃炭化活化1h，得到载炭多孔陶瓷；将液体C加热浓缩至近饱和，加入液体C质量的2％纳米钛酸钙粉体，置于波长为254nm，辐照强度为100μW/cm2紫外光辐照下，搅拌100min后，加入液体C质量10％的脲和5％的乙烯脲，超声分散成悬浊液，将载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡20min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去表面残液，50℃真空烘干，得到可净化空气中甲醛和氮氧化物的多孔陶瓷5。
实施例6：多孔陶瓷对空气中甲醛的净化性能
分别取实施例1-5制备的复合多孔陶瓷圆片装嵌于内径为40mm的玻璃管中，将玻璃管的一端通过变径与吸气泵连接，制成简易空气净化装置，将该空气净化装置置于长×宽×高为1250mm×800mm×1000mm的全玻璃空气试验箱内，调整箱内甲醛的初始浓度为0.5mg/m3，开启吸气泵，以1m3/min的速度循环吸气，室内自然光条件下，运行12h，根据GB/T18204.26-2000“空气质量-甲醛的测定-酚试剂分光光度法”，测定箱内甲醛浓度。按公式(1)计算甲醛的去除率，同时做空白实验，结果见表1
η为去除率％，C0为初始浓度，Ce为处理后浓度。
表1.多孔陶瓷1-5对空气中甲醛的净化性能
| 净化后甲醛浓度(mg/m<sup>3</sup>) | 去除率(％) | |
| 多孔陶瓷1 | 0 | 100 |
| 多孔陶瓷2 | 0.012 | 97.6 |
| 多孔陶瓷3 | 0 | 100 |
| 多孔陶瓷4 | 0.017 | 96.6 |
| 多孔陶瓷5 | 0 | 100 |
| 空白 | 0.481 | 3.8 |
实施例7：多孔陶瓷对氮氧化物的净化性能
按实施例6同样方法，分别取实施例1-5制备的复合多孔陶瓷圆片3片，装嵌于内径为40mm的玻璃管中，多孔陶瓷片间距离为20mm，将玻璃管的一端通过变径与吸气泵连接，制成简易空气净化装置，将该空气净化装置置于长×宽×高为1250mm×800mm×1000mm的全玻璃空气试验箱内，在箱内用铜片和硝酸反应，生成氮氧化物，根据HJ 479—2009“环境空气氮氧化物的测定-盐酸萘乙二胺分光光度法”测定箱内空气中氮氧化物的浓度为1.837mg/m3，开启吸气泵，以1m3/min的速度循环吸气，室内自然光条件下，运行12h，测定箱内氮氧化物的浓度。按公式(1)计算去除率，同时做空白实验，结果见表2.
表2.多孔陶瓷1-5对空气中氮氧化物的净化性能
| 12h后氮氧化物浓度(mg/m<sup>3</sup>) | 去除率(％) | |
| 多孔陶瓷1 | 0.014 | 99.2 |
| 多孔陶瓷2 | 0.035 | 98.1 |
| 多孔陶瓷3 | 0.024 | 98.7 |
| 多孔陶瓷4 | 0.053 | 97.1 |
| 多孔陶瓷5 | 0.017 | 99.1 |
| 空白 | 1.764 | 3.97 |
以上数据表明,本发明方法制备的多孔陶瓷对空气中甲醛和氮氧化物均具有较好的净化能力。
Claims (2)
1.一种利用污泥和牛粪制备气体净化多孔陶瓷的方法，其特征在于，该方法包括如下步骤：
1）取新鲜的含水率均为80-85%的剩余污泥和牛粪，等质量混合，依次加入污泥和粪便总质量的10%-20%的质量百分含量为30%的双氧水、10%-30%的硅藻土，再按污泥和牛粪总质
量与酸溶液体积比为1Kg:1L的比例，加入0.5-1mol/L的硝酸溶液，搅拌均匀，加热微沸10-20min，固液分离，得到固体A和液体A；
2）向固体A中加水至刚好浸没，用氢氧化钾调pH值11-12，并加热微沸30min，期间，调整并保持溶液的pH值为11-12，固液分离，得到固体B和液体B；
3）将液体A用氨水调pH值为8-9，搅拌均匀，静置12h，固液分离，得到固体C和液体C；
4）将固体C和固体B混合，105-150℃烘干，球磨6-8h，润湿加压10-20MPa成型，60-90℃烘干，于1000-1250℃下煅烧，得到多孔陶瓷材料；
5）将步骤4）得到的多孔陶瓷材料浸泡于步骤2）得到的液体B中，超声振荡10min，加热继续浓缩，蒸发，干燥，浸泡于质量百分浓度为85%的浓磷酸中，超声振荡吸附10min，静置浸泡12h，取出，隔绝空气条件下，于400-500℃炭化活化1h，得到载炭多孔陶瓷；
6）将液体C加热浓缩至近饱和，加入占液体C质量的1-5%纳米催化剂粉体，光辐照下搅
拌60-120min后，加入液体C质量5-10%的脲和5-10%的乙烯脲，超声分散成悬浊液，将步骤5）得到的载炭多孔陶瓷浸泡于该悬浊液中，继续超声振荡20-30min，静置吸附，将悬浊液反复滤过多孔陶瓷，待液体澄清，取出载炭多孔陶瓷，用压缩空气轻轻吹去外表面残液，50℃真空烘干，得到去除甲醛和氮氧化物的多孔陶瓷，回收浸泡液即为农用复合肥；
所述的污泥为城市污水处理厂排放的剩余污泥；
所述的步骤6）中加入的纳米催化剂粉体为纳米钛酸钙粉体、纳米钛酸锶粉体、纳米钒酸铋粉体和纳米二氧化钛粉体中的一种或几种。
2.根据权利要求1所述的一种利用污泥和牛粪制备气体净化多孔陶瓷的方法，其特征在于，所述的步骤4）中煅烧方法为：以3.6℃/min的升温速度升到360 ℃, 并在此温度下保温30 min，再以5℃/min的速度继续升温到烧成温度, 并保温10-20 min，炉内冷却到室温。
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