CN110105058A - 一种泡沫陶瓷及其在废水处理中的应用 - Google Patents
一种泡沫陶瓷及其在废水处理中的应用 Download PDFInfo
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Abstract
本发明提供了一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:将硅藻土、高岭土、石英、秸秆生物炭和α‑Al2O3微粉混合研磨;加水球磨,烘干得混合粉料;加入明胶溶液,配制浆料,混合球磨;真空脱气,注入模具中,密封固化;干燥后脱模;置于超临界二氧化碳发泡装置中发泡;焙烧;冷却后平铺在低温等离子处理装置中处理得改性泡沫陶瓷;取Al(NO3)3·9H2O和蒸馏水搅拌溶解,回流加热,加铝粉反应;得无色透明溶胶;加入聚乙二醇、硝酸镧和硝酸钡,搅拌溶解;将改性泡沫陶瓷浸入其中,真空浸渍后取出,干燥;取出后焙烧即得。本法所提供的泡沫陶瓷对于COD和氨氮都具有非常好的处理效果,能够有效的应用于废水处理。
Description
技术领域
本发明涉及一种泡沫陶瓷及其在废水处理中的应用。
背景技术
泡沫陶瓷是近年来快速发展起来的以气孔为主要构成部分的一种具有特殊功能的陶瓷材料,是由骨料、造孔剂和粘结剂等组分经过高温烧结而成的。根据孔径大小可分为:大孔材料、介孔材料和微孔材料。泡沫陶瓷材料具有的良好化学稳定性、机械强度高和耐高温等优点。同时,其还具有比表面积大,孔隙率高等特点。其发达的微孔结构,大的比表面积有利于微生物的生长与繁殖;同时在水处理过程中具有截留悬浮固体,改善气水分布的作用。将其进行重塑改性后能够有效的被用于废水处理中,为废水处理提供新的发展方向。
发明内容
要解决的技术问题:提供一种泡沫陶瓷及其在废水处理中的应用,所得泡沫陶瓷对于COD和氨氮都具有非常好的处理效果,能够有效的应用于废水处理。
技术方案:一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将20-30份硅藻土、20-30份高岭土、10-20份石英、5-10份秸秆生物炭和5-10份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为40-45%的浆料,混合球磨5-10min;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度50-80℃、压力10-20MPa下溶胀10-20min,在2s内快速卸压;
(7)放入马弗炉中,在温度1300-1350℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率10-15kHz、工作电压20kV、放电功率70-80W条件下处理10-15min得改性泡沫陶瓷;
(9)取200-250份Al(NO3)3·9H2O和600-650份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入35-40份铝粉反应,反应过程中控制溶液的pH值为3.0-4.0;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入20-25份聚乙二醇、3-6份硝酸镧和4-8份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍0.5-1h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在500-800℃下焙烧5h即得泡沫陶瓷。
进一步的,所述步骤(3)中明胶在混合粉料中的含量为20wt%-30wt%。
进一步的,所述步骤(6)中温度为65℃、压力为15MPa,溶胀时间为15min。
进一步的,所述步骤(8)中电源频率为13kHz,放电功率为75W。
一种泡沫陶瓷在废水处理中的应用。
有益效果:
1.以超临界CO2进行发泡,避免了有机溶剂的使用,节能环保。
2.经低温等离子处理装置处理后,泡沫陶瓷表面介孔数量增加,表面更为粗糙,增加吸附性能。
3.经本发明制备的泡沫陶瓷对于COD和氨氮都具有非常好的处理效果,经处理后,COD和氨氮的去除率都分别高达97.2%和92.1%。
具体实施方式
实施例1
一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将20份硅藻土、20份高岭土、10份石英、5份秸秆生物炭和5份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为40%的浆料,混合球磨5min,其中,明胶在混合粉料中的含量为20wt%;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度50℃、压力10MPa下溶胀10min,在2s内快速卸压;
(7)放入马弗炉中,在温度1300℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率10kHz、工作电压20kV、放电功率70W条件下处理10min得改性泡沫陶瓷;
(9)取200份Al(NO3)3·9H2O和600份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入35份铝粉反应,反应过程中控制溶液的pH值为3.0;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入20份聚乙二醇、3份硝酸镧和4份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍0.5h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在500℃下焙烧5h即得泡沫陶瓷。
实施例2
一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将23份硅藻土、22份高岭土、12份石英、7份秸秆生物炭和7份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为42%的浆料,混合球磨7min,其中,明胶在混合粉料中的含量为22wt%;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度60℃、压力15MPa下溶胀15min,在2s内快速卸压;
(7)放入马弗炉中,在温度1320℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率12kHz、工作电压20kV、放电功率75W条件下处理12min得改性泡沫陶瓷;
(9)取220份Al(NO3)3·9H2O和620份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入36份铝粉反应,反应过程中控制溶液的pH值为3.5;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入22份聚乙二醇、4份硝酸镧和5份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍0.5h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在600℃下焙烧5h即得泡沫陶瓷。
实施例3
一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将25份硅藻土、25份高岭土、15份石英、8份秸秆生物炭和8份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为43%的浆料,混合球磨8min,其中,明胶在混合粉料中的含量为25wt%;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度65℃、压力15MPa下溶胀15min,在2s内快速卸压;
(7)放入马弗炉中,在温度1330℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率13kHz、工作电压20kV、放电功率75W条件下处理13min得改性泡沫陶瓷;
(9)取230份Al(NO3)3·9H2O和630份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入38份铝粉反应,反应过程中控制溶液的pH值为3.5;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入23份聚乙二醇、5份硝酸镧和6份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍1h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在650℃下焙烧5h即得泡沫陶瓷。
实施例4
一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将28份硅藻土、28份高岭土、17份石英、9份秸秆生物炭和9份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为44%的浆料,混合球磨9min,其中,明胶在混合粉料中的含量为28wt%;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度70℃、压力17MPa下溶胀15min,在2s内快速卸压;
(7)放入马弗炉中,在温度1340℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率14kHz、工作电压20kV、放电功率75W条件下处理14min得改性泡沫陶瓷;
(9)取240份Al(NO3)3·9H2O和640份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入39份铝粉反应,反应过程中控制溶液的pH值为4.0;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入24份聚乙二醇、5份硝酸镧和7份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍1h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在700℃下焙烧5h即得泡沫陶瓷。
实施例5
一种泡沫陶瓷,成分按重量份计,制备方法包括以下步骤:
(1)将30份硅藻土、30份高岭土、20份石英、10份秸秆生物炭和10份α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为45%的浆料,混合球磨10min,其中,明胶在混合粉料中的含量为30wt%;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度80℃、压力20MPa下溶胀20min,在2s内快速卸压;
(7)放入马弗炉中,在温度1350℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率15kHz、工作电压20kV、放电功率80W条件下处理15min得改性泡沫陶瓷;
(9)取250份Al(NO3)3·9H2O和650份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入40份铝粉反应,反应过程中控制溶液的pH值为4.0;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入25份聚乙二醇、6份硝酸镧和8份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍1h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在800℃下焙烧5h即得泡沫陶瓷。
将本发明制备的泡沫陶瓷进行污水的处理,污水的COD为484mg/L、氨氮含量为36.3mg/L。
表1经泡沫陶瓷处理后污水的性能指标
产品名称 | COD去除率(%) | 氨氮去除率(%) |
实施例1 | 96.3 | 91.2 |
实施例2 | 96.7 | 91.7 |
实施例3 | 97.2 | 92.1 |
实施例4 | 96.8 | 91.9 |
实施例5 | 96.2 | 91.5 |
注:泡沫陶瓷使用量为3g/L
经本发明制备的泡沫陶瓷对于COD和氨氮都具有非常好的处理效果,经处理后,COD和氨氮的去除率都分别高达97.2%和92.1%。
Claims (5)
1.一种泡沫陶瓷,其特征在于:成分按重量份计,制备方法包括以下步骤:
(1)将硅藻土、高岭土、石英、秸秆生物炭和α-Al2O3微粉混合,研磨至细度<0.1mm;
(2)加水球磨至粒径≤2μm,烘干得混合粉料;
(3)加入明胶溶液,配制总固含量为40-45%的浆料,混合球磨5-10min;
(4)将浆料磁力搅拌后真空脱气,注入模具中,置于85℃恒温干燥箱中密封固化1h;
(5)转移至50℃干燥箱中干燥后脱模;
(6)置于超临界二氧化碳发泡装置的高压釜内,先充入低压二氧化碳将釜内空气置换干净,再充入高压二氧化碳,在温度50-80℃、压力10-20MPa下溶胀10-20min,在2s内快速卸压;
(7)放入马弗炉中,在温度1300-1350℃下焙烧4h;
(8)冷却后均匀地平铺在低温等离子处理装置中的地电极上,在电源频率10-15kHz、工作电压20kV、放电功率70-80W条件下处理10-15min得改性泡沫陶瓷;
(9)取200-250份Al(NO3)3·9H2O和600-650份蒸馏水搅拌溶解,放入水浴锅中,在90℃下进行回流加热,慢慢加入35-40份铝粉反应,反应过程中控制溶液的pH值为3.0-4.0;
(10)离心分离后除去底层灰色沉淀,得无色透明溶胶;
(11)加入20-25份聚乙二醇、3-6份硝酸镧和4-8份硝酸钡,搅拌溶解得淡黄色透明溶胶;
(12)将改性泡沫陶瓷浸入淡黄色透明溶胶中,真空浸渍0.5-1h后取出,放入干燥箱中干燥;
(13)取出后放入马弗炉中在500-800℃下焙烧5h即得泡沫陶瓷。
2.根据权利要求1所述的一种泡沫陶瓷,其特征在于:所述步骤(3)中明胶在混合粉料中的含量为20wt%-30wt%。
3.根据权利要求1所述的一种泡沫陶瓷,其特征在于:所述步骤(6)中温度为65℃、压力为15MPa,溶胀时间为15min。
4.根据权利要求1所述的一种泡沫陶瓷,其特征在于:所述步骤(8)中电源频率为13kHz,放电功率为75W。
5.根据权利要求1-4所述的一种泡沫陶瓷在废水处理中的应用。
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