CN114870790B - 一种再生活性炭及其制备方法 - Google Patents
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Abstract
本发明活性炭经过预处理、浸渍、水热、煅烧得到可磁分离光催化再生活性炭复合材料，本发明的活性炭复合材料可磁分离和光催化再生，具有以下优点和有益效果：一、对活性炭的微观结构几乎没有破坏，Fe‑g‑C3N4负载使活性炭具有磁性，在活性炭吸附抗生素后可以通过外磁场进行磁分离，有利于活性炭的回收利用及再生；2）活性炭与Fe‑g‑C3N4复合，增加化学活性点，提高材料的光催化降解能力，在吸附抗生素后可光照催化再生活性炭，使活性炭循环利用；3）本发明的制备方法具有操作简单、环境友好、耗能低等优点，应用于环丙沙星抗生素吸附的条件温和、耗时短、效果优异，活性炭可光催化再生循环利用效率高、效果好。
Description
技术领域
本发明涉及复合材料领域，具体涉及一种可磁分离光催化再生活性炭及其制备方法。
背景技术
活性炭因微孔结构丰富，比表面积大，化学稳定性高和无毒性等优点被广泛应用于水处理、空气净化、食品脱色和药物分离等领域。但其在实际应用中存在分离难和再生难等问题。首先，传统的过滤分离法容易引起筛网堵塞或活性炭的流失。与传统的过滤法相比，磁分离是一种简单高效的分离方法，可分离磁性或可磁化的吸附剂、载体、细胞等物质。而活性炭本身磁化率非常小，需要引入磁性介质才能适用于磁分离。其次，应用后活性炭会产生大量的废弃活性炭，如果这些废弃活性炭不能够再次利用或再生将对环境产生二次污染。常规的活性炭再生技术如热再生，化学再生，生物再生，微波再生等存在处理温度高，化学消耗大，处理周期长，再生效率低等许多缺点。废弃活性炭的光催化再生技术通过将太阳能转化为化学能，光催化降解被吸附的污染物来再生活性炭。由于可以将污染物原位降解，不会对环境产生二次污染。
类石墨相氮化碳 g-C3N4具有优异的可见光反应又不具备毒性，尤其是其独特的二维超薄类石墨烯结构，它的量子限域效应和表面效应使带隙变窄，能够吸收从紫外光到可见光波段光谱，使其成为一种新型热门的光催化材料。但g-C3N4单体比表面积较小，导电性较差，导致参与催化的活性位点少。将g-C3N4进行掺杂改性，并与比表面积较大和导电性较优异的活性炭复合，一方面提高了g-C3N4的光催化活性，另一方面通过了g-C3N4光催化降解活性炭吸附的污染物，使活性炭得到光催化再生。
抗生素因具有的高效光谱、口服活性、完全的交叉抗性等优点，被广泛用于治疗人体、疾病、预防畜禽、水产品的细菌性病害等行业。然而，残留抗生素的数量也随之越来越大，因此急需一种快速、有效的方法来降解掉水体中残留的抗生素。活性炭具有丰富的孔结构，较大的比表面积，可以用来吸附水体中残留的抗生素。然而，单纯的活性炭对特定的抗生素化学活性点不高，抗生素吸附效率不够理想。
发明内容
本发明的目的是制备一种可磁分离光催化再生活性炭，该活性炭为Fe-g-C3N4/活性炭复合材料，同时提供了一种制备该活性炭复合材料的方法。
为实现本发明的目的，采用以下技术方案：
一种可磁分离光催化再生活性炭，其特征在于，所述的活性炭为Fe-g-C3N4/活性炭复合材料，具体包括以下制备步骤：一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入1~5份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品200~500份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在150～200℃下恒温水热处理8～16h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至300~500 ℃保温1~3 h，自然冷却后得到可磁分离光催化再生活性炭。
本发明的有益效果：
1）一、对活性炭的微观结构几乎没有破坏，Fe-g-C3N4负载使活性炭具有磁性，在活性炭吸附抗生素后可以通过外磁场进行磁分离，有利于活性炭的回收利用及再生；2）活性炭与Fe-g-C3N4复合，增加化学活性点，提高材料的光催化降解能力，在吸附抗生素后可光照催化再生活性炭，使活性炭循环利用；3）本发明的制备方法具有操作简单、环境友好、耗能低等优点，应用于环丙沙星抗生素吸附的条件温和、耗时短、效果优异，活性炭可光催化再生循环利用效率高、效果好。
具体实施方式
下面是结合具体实施例，进一步阐述本发明。这些实施例仅用于说明本发明，但不用来限制本发明的范围。
实施例1
一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入1份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品400份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在200℃下恒温水热处理10 h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至500 ℃保温2 h，自然冷却后得到可磁分离光催化再生活性炭。
实施例1制备得到的可磁分离光催化再生活性炭进行磁性能测试，饱和磁化强度为4.27 emu/g，在外磁场下可磁分离；并对环丙沙星抗生素进行吸附，在可见光再生12 h后，经过4次循环活性炭对环丙沙星抗生素的降解率为89%。
实施例2
一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入1份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品200份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在150℃下恒温水热处理16 h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至400 ℃保温3 h，自然冷却后得到可磁分离光催化再生活性炭。
实施例2制备得到的可磁分离光催化再生活性炭进行磁性能测试，饱和磁化强度为6.32 emu/g，在外磁场下可磁分离；并对环丙沙星抗生素进行吸附，在可见光再生12 h后，经过4次循环活性炭对环丙沙星抗生素的降解率为72%。
实施例3
一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入5份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品300份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在180℃下恒温水热处理10 h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至300 ℃保温3 h，自然冷却后得到可磁分离光催化再生活性炭。
实施例3制备得到的可磁分离光催化再生活性炭进行磁性能测试，饱和磁化强度为10.23 emu/g，在外磁场下可磁分离；并对环丙沙星抗生素进行吸附，在可见光再生12 h后，经过4次循环活性炭对环丙沙星抗生素的降解率为62%。
实施例4
一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入3份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品500份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在200℃下恒温水热处理8 h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至300 ℃保温2 h，自然冷却后得到可磁分离光催化再生活性炭。
实施例4制备得到的可磁分离光催化再生活性炭进行磁性能测试，饱和磁化强度为7.88 emu/g，在外磁场下可磁分离；并对环丙沙星抗生素进行吸附，在可见光再生12 h后，经过4次循环活性炭对环丙沙星抗生素的降解率为65%。
实施例5
一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入2份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品400份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在150℃下恒温水热处理12h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至400 ℃保温1 h，自然冷却后得到可磁分离光催化再生活性炭。
实施例5制备得到的可磁分离光催化再生活性炭进行磁性能测试，饱和磁化强度为6.89 emu/g，在外磁场下可磁分离；并对环丙沙星抗生素进行吸附，在可见光再生12 h后，经过4次循环活性炭对环丙沙星抗生素的降解率为84%。
Claims (1)
1.一种可磁分离光催化再生活性炭，其特征在于，所述的活性炭为Fe-g-C3N4/活性炭复合材料，具体包括以下制备步骤：一、将活性炭用研磨机研磨过200目分子筛，在50℃下用NaOH浸泡5h，水洗至中性后过滤并在100℃下烘24 h以备用；二、将1份的三聚氰胺溶于蒸馏水和乙二醇的混合液中搅拌1 h，加入1~5份FeCl3·6H2O继续搅拌1 h，然后逐滴滴加一定量N2H4·H2O，继续搅拌然1 h得到混合溶液A；三、将步骤一得到的样品200~500份加入到混合溶液A中继续搅拌12 h，然后移植到聚四氟乙烯内衬的反应釜中，在150～200℃下恒温水热处理8～16h；四、经磁分离、洗涤及干燥后，将样品移入坩埚，盖好盖子同时保持着较好的密封性，置于管式炉中升温至300~500 ℃保温1~3 h，自然冷却后得到可磁分离光催化再生活性炭。
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