CN108579796B - 一种可分解有机污染物的活化沸石滤料的制备方法 - Google Patents
一种可分解有机污染物的活化沸石滤料的制备方法 Download PDFInfo
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Abstract
一种可分解有机污染物的活化沸石滤料的制备方法，属于环境净化功能材料领域，包括下述工艺步骤：制备硼镧钛三元复合前驱体，以乙醇、乙二醇、钛酸异丙酯、硼酸三丁酯、乙酰丙酮、硝酸镧水溶液和活化沸石滤料经搅拌和超声处理制得；热反应挂膜，将上述前驱体在不锈钢反应釜中设定温度和压力反应，过滤清洗；固化成膜，将滤饼干燥、煅烧即制得可分解有机污染物的活化沸石滤料，具有在光照条件下分解有机污染物的活性。
Description
技术领域：
本发明属于环境净化功能材料领域，具体涉及一种可分解有机污染物的活化沸石滤料的制备方法。
背景技术：
沸石是一种极性物质，是极性很强的吸附剂，对极性分子和不饱和分子有机物，如卤代烃有很强的吸附效果，对非极性分子中极化率大的分子也有较高的选择吸附优势。活化沸石是天然沸石经过多种特殊工艺活化而成，其吸附性能比天然沸石更强，离子交换性能也更好，不仅能去除水中的浊度、色度、异味，而且对水中有害的重金属，如：铬、镉、镍、锌、汞、铁离子及有机物：酚、六六六、滴滴涕、三氮、氨氮、磷酸根离子等物质具有吸附交换作用，也有利于去除水中各种微污染物且水浸出液不含有毒、有害人体物质，去除水中铁、氟效果更为显著。因此活化沸石是工业给水、废水处理及自来水过滤的新型理想滤料。典型活化沸石的密度1.8~2.2 g/cm3，空隙率≥50%，比表面积500~800 m2/g。然而，活化沸石滤料不具有分解有机污染物的性能，在吸附饱和后即不具有持续的吸附能力。如果在活化沸石表面附着具有光催化净化分解活性的材料，即可使该型活化沸石在光照射下分解在表面吸附的有机污染物，达到持续净化污水的能力。此类新型活化沸石滤料在各种水净化领域具有广泛的用途。
发明内容：
针对现有技术存在的问题，本发明旨在提供一种可分解有机污染物的活化沸石滤料的制备方法。此种活化沸石滤料表面附着具有光催化净化分解活性的材料，可用于各种水污染净化领域。
本发明采用的技术方案是：
一种可分解有机污染物的活化沸石滤料的制备方法，包括下述工艺步骤：
步骤1：制备硼镧钛三元复合前驱体
1.1 取500 mL烧杯1只，依次加入210~220 mL乙醇、33~36 mL乙二醇、16~18 mL钛酸异丙酯、3.5~4.5 mL硼酸三丁酯和6~8 mL乙酰丙酮，上述材料为纯料，搅拌均匀；
1.2 向烧杯中加入23~27 mL 0.2mol/L硝酸镧水溶液，搅拌均匀；
1.3 向烧杯中加入活化沸石滤料30~40g，将混合物置于功率100W超声波清洗机中，在40MHz下处理30 min，即制得硼镧钛三元复合前驱体，备用。
步骤2：热反应挂膜
2.1 将步骤1.3中的硼镧钛三元复合前驱体倒入不锈钢反应釜中，将反应釜密闭，保持反应釜中温度160~190℃，压力2.5~3.5 MPa，反应72 h，然后自然冷却；
2.2 将所得产物通过滤纸过滤，用去离子水清洗滤饼。
步骤3：固化成膜
3.1 将滤饼置于电热鼓风干燥箱中，在210℃干燥24 h，在瓷研钵中充分研磨成粉末；
3.2 将粉末置于程控箱式电炉中，保持煅烧温度410~560℃，煅烧3h，待电炉冷却后，即制得可分解有机污染物的活化沸石滤料。
上述步骤1.3中活化沸石滤料的密度1.8~2.2g/cm3，空隙率≥50%，比表面积500~800 m2/g。
与现有技术相比，本发明的优点在于：
本发明通过合理地控制反应条件，能够成功地在活化沸石滤料表面附着硼镧钛复合涂层。该新型材料不仅保留活化沸石滤料低密度、高比表面积的特点，还具有在光照条件下分解有机污染物的活性，从而使该新型材料能够持续地吸附分解水中的有机污染物，具有长寿命、高效率的特点，适于多种形式的水治理过程。
具体实施方式：
实施例1
一种可分解有机污染物的活化沸石滤料的制备方法，包括下述工艺步骤：
步骤1：制备硼镧钛三元复合前驱体
1.1 取500 mL烧杯1只，依次加入210 mL乙醇、33 mL乙二醇、16 mL钛酸异丙酯、3.5 mL硼酸三丁酯和6 mL乙酰丙酮，上述材料为纯料，搅拌均匀；
1.2 向烧杯中加入23 mL 0.2mol/L硝酸镧水溶液，搅拌均匀；
1.3 向烧杯中加入活化沸石滤料30g，将混合物置于功率100W超声波清洗机中，在40MHz下处理30 min，即制得硼镧钛三元复合前驱体，备用。
步骤2：热反应挂膜
2.1 将步骤1.3中的硼镧钛三元复合前驱体倒入不锈钢反应釜中，将反应釜密闭，保持反应釜中温度160℃，压力2.5 MPa，反应72 h，然后自然冷却；
2.2 将所得产物通过滤纸过滤，用去离子水清洗滤饼。
步骤3：固化成膜
3.1 将滤饼置于电热鼓风干燥箱中，在210℃干燥24 h，在瓷研钵中充分研磨成粉末；
3.2 将粉末置于程控箱式电炉中，保持煅烧温度410℃，煅烧3h，待电炉冷却后，即制得可分解有机污染物的活化沸石滤料。
上述步骤1.3中的活化沸石滤料的密度2.2g/cm3，空隙率60%，比表面积500 m2/g。
实施例2
一种可分解有机污染物的活化沸石滤料的制备方法，包括下述工艺步骤：
步骤1：制备硼镧钛三元复合前驱体
1.1 取500 mL烧杯1只，依次加入215 mL乙醇、34 mL乙二醇、17 mL钛酸异丙酯、3.9 mL硼酸三丁酯和7 mL乙酰丙酮，上述材料为纯料，搅拌均匀；
1.2 向烧杯中加入25 mL 0.2mol/L硝酸镧水溶液，搅拌均匀；
1.3 向烧杯中加入活化沸石滤料35g，将混合物置于功率100W超声波清洗机中，在40MHz下处理30 min，即制得硼镧钛三元复合前驱体，备用。
步骤2：热反应挂膜
2.1 将硼镧钛三元复合前驱体倒入不锈钢反应釜中，将反应釜密闭，保持反应釜中温度170℃，压力3 MPa，反应72 h，然后自然冷却；
2.2 将所得产物通过滤纸过滤，用去离子水清洗滤饼。
步骤3：固化成膜
3.1 将滤饼置于电热鼓风干燥箱中，在210℃干燥24 h，在瓷研钵中充分研磨成粉末；
3.2 将粉末置于程控箱式电炉中，保持煅烧温度480℃，煅烧3h，待电炉冷却后，即制得可分解有机污染物的活化沸石滤料。
上述步骤1.3中的活化沸石滤料的密度2g/cm3，空隙率65%，比表面积600 m2/g。
实施例3
一种可分解有机污染物的活化沸石滤料的制备方法，包括下述工艺步骤：
步骤1：制备硼镧钛三元复合前驱体
1.1 取500 mL烧杯1只，依次加入220 mL乙醇、36 mL乙二醇、18 mL钛酸异丙酯、4.5 mL硼酸三丁酯和8 mL乙酰丙酮，上述材料为纯料，搅拌均匀；
1.2 向烧杯中加入27 mL 0.2mol/L硝酸镧水溶液，搅拌均匀；
1.3 向烧杯中加入活化沸石滤料40g，将混合物置于功率100W超声波清洗机中，在40MHz下处理30 min，即制得硼镧钛三元复合前驱体，备用。
步骤2：热反应挂膜
2.1 将步骤1.3中的硼镧钛三元复合前驱体倒入不锈钢反应釜中，将反应釜密闭，保持反应釜中温度190℃，压力3.5 MPa，反应72 h，然后自然冷却；
2.2 将所得产物通过滤纸过滤，用去离子水清洗滤饼。
步骤3：固化成膜
3.1 将滤饼置于电热鼓风干燥箱中，在210℃干燥24 h，在瓷研钵中充分研磨成粉末；
3.2 将粉末置于程控箱式电炉中，保持煅烧温度560℃，煅烧3h，待电炉冷却后，即制得可分解有机污染物的活化沸石滤料。
上述步骤1.3中的活化沸石滤料的密度1.8g/cm3，空隙率70%，比表面积800 m2/g。
Claims (2)
1.一种可分解有机污染物的活化沸石滤料的制备方法，其特征在于，包括下述工艺步骤：
步骤1：制备硼镧钛三元复合前驱体
1.1 取500 mL烧杯1只，依次加入210~220 mL乙醇、33~36 mL乙二醇、16~18 mL钛酸异丙酯、3.5~4.5 mL硼酸三丁酯和6~8 mL乙酰丙酮，上述材料为纯料，搅拌均匀；
1.2 向烧杯中加入23~27 mL 0.2mol/L硝酸镧水溶液，搅拌均匀；
1.3 向烧杯中加入活化沸石滤料30~40g，将混合物置于功率100W超声波清洗机中，在40MHz下处理30 min，即制得硼镧钛三元复合前驱体，备用；
步骤2：热反应挂膜
2.1 将步骤1.3中的硼镧钛三元复合前驱体倒入不锈钢反应釜中，将反应釜密闭，保持反应釜中温度160~190℃，压力2.5~3.5 MPa，反应72 h，然后自然冷却；
2.2 将所得产物通过滤纸过滤，用去离子水清洗滤饼；
步骤3：固化成膜
3.1 将滤饼置于电热鼓风干燥箱中，在210℃干燥24 h，在瓷研钵中充分研磨成粉末；
3.2 将粉末置于程控箱式电炉中，保持煅烧温度410~560℃，煅烧3h，待电炉冷却后，即制得可分解有机污染物的活化沸石滤料。
2.根据权利要求1所述的一种可分解有机污染物的活化沸石滤料的制备方法，其特征在于：上述步骤1.3中的活化沸石滤料的密度1.8~2.2g/cm3，空隙率≥50%，比表面积500~800 m2/g。
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