CN112517069B - 一种光催化活性碳气凝胶材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种光催化活性碳气凝胶材料及其制备方法，属于无机非金属材料领域。所述制备方法为:先将生物质泥炭分别进行碱洗、酸性、过滤去除其中无机矿物质（灰分），在惰性气氛中进行碳化和石墨化煅烧处理，再经洗涤、干燥得到碳微晶材料。以碳微晶的悬浮液进行交联稳定化处理，经冷冻干燥制得三维碳基气凝胶。用光催化剂水溶胶涂覆碳气凝胶表面，得到具有光催化活性的碳气凝胶。与传统的碳气凝胶吸附剂相比，可以将吸附到气凝胶孔洞结构中的有机污染物降解，从而实现复合材料的循环使用，大大降低了治理污染的成本。制备工艺简单，原料廉价易得，制备的碳气凝胶材料具有良好的柔韧性、光催化活性和吸附性能，在环境领域应用前景广阔。
Description
技术领域
本发明涉及一种新型生物质基光催化活性碳气凝胶材料及其制备方法，属于无机非金属材料领域。
背景技术
碳气凝胶作为一种新型碳材料，其结构呈三维网络状，具有质量轻、比表面积大、多孔、吸收可见光、导电性好和化学性能稳定等优点，在环境与能源领域中应用广泛。对碳气凝胶进行功能化是提高其性能、拓展其应用的有效途径，而利用来源丰富的生物质原料，研发简便的、可批量化的功能碳气凝胶制备方法依然是碳材料领域面临的重大挑战。
发明内容
本发明目的在于提供一种新型生物质基光催化活性碳气凝胶材料；另一目的在于提供其制备方法。
为实现本发明目的，技术方案如下：
所述生物质基光催化活性碳气凝胶材料通过以下方法制得：
(1)生物质泥炭预处理：分别采用稀碱、稀酸溶液洗脱，去除泥炭中的无机矿物质；
(2)用高铁酸钾溶液浸渍上述预处理后的泥炭，(使其负载具有催化活化作用的高铁酸钾)，干燥后放入管式炉中，通入氮气(或氩气)作为保护气焙烧；
(3)冷至室温后，加入盐酸溶液搅拌后过滤，用水洗涤至中性；干燥过夜，研磨得到石墨化碳微晶粉末；
(4)在搅拌下将石墨化碳微晶粉末加入交联剂溶液中，交联剂采用聚乙烯醇、聚苯乙烯磺酸盐或二者组合，进行交联稳定化处理后得到水溶胶；
(5)水溶胶进行冷冻干燥处理，得到三维碳微晶气凝胶；
(6)采用旋涂法将g-C3/N4/TiO2光催化剂水溶胶均匀喷涂至三维碳微晶气凝胶表面，干燥后制得具有光催化活性的功能碳气凝胶材料。
所述高铁酸钾(K2FeO4)溶液浓度优选：0.1mol/L；
所述聚交联剂优选质量分数为5％的溶液。
步骤(1)中所述稀碱、稀酸溶液分别为1mol/L氢氧化钠和1mol/L盐酸。
步骤(2)中焙烧温度为800℃-900℃，升温速率3-5℃/min，恒温时间2h。
步骤(3)中所述盐酸溶液浓度为1mol/L。
步骤(5)中所述冷冻干燥前先进行液氮下速冻处理，然后在-40℃下冷冻干燥。
步骤(4)中所述水溶胶的优选制备步骤：将石墨化碳微晶粉末加入到戊二醛、盐酸和聚乙烯醇的混合溶液中，凝胶化处理24h。
步骤(4)中所述水溶胶的优选制备步骤：将石墨化碳微晶粉末加入到交联剂聚苯乙烯磺酸盐溶液中，通过自由基聚合反应24h。
步骤(4)中所述水溶胶的优选制备步骤：将石墨化碳微晶粉末加入到由聚乙烯醇、聚苯乙烯磺酸盐组成的交联剂溶液中，凝胶化处理24h。
本发明构建了一种以碳气凝胶为基的吸附–光催化降解协同作用体系，所得碳微晶材料兼具吸附作用和光催化性能，与传统的碳气凝胶吸附剂相比，可以将吸附到气凝胶孔洞结构中的有机污染物降解，具有长期耐用性，可以实现复合材料的循环使用，大大降低了治理污染的成本，是推进太阳能水净化的一个很有前景的途径。
与现有技术相比，本发明具有如下优点：原材料价格低廉、制备工艺简单、适宜大规模生产。所得碳微晶材料具有良好的柔韧性、具有较大的表面积(215m2/g以上)，良好的孔结构(平均3.5nm以上)，经验证，其表现出优异的吸附性能和显著的光催化活性，在吸附与能量转换与环境领域有潜在应用前景。
附图说明
图1为本发明制备的碳微晶样品的扫描电镜图，其中(a,b)-碳化后，(c,d)-石墨化后；
图2为本发明制备的碳微晶样品的XRD分析图谱；
图3为本发明制备的碳微晶样品的拉曼光谱图；
图4本发明制备的碳微晶气凝胶和光催化碳微晶气凝胶样品实物照图，其中：a-碳微晶气凝胶，b-单面光催化碳微晶气凝胶；
图5为本发明制备的碳微晶气凝胶材料的可见光性能及反应速率常数，其中，a-光催化性能曲线，b–一级反应动力学速率常数。
具体实施方式
为对本发明进行更好地说明，举实施例如下：
实施例1
(1)分别采用浓度为1mol/L的氢氧化钠、盐酸溶液，对泥炭进行洗脱、去除无机矿物质，机械搅拌1-2小时，过滤并干燥；
(2)用0.1mol/L高铁酸钾溶液浸渍上述预处理后的泥炭，干燥后放入管式炉中，通入氮气(或氩气)作为保护气，以3-5℃/分钟速率升温，在800～900℃下焙烧1～2小时；
(3)冷至室温，加入0.1mol/L盐酸溶液搅拌后过滤，用水洗涤至pH＝7.0；在80℃下干燥过夜，研磨得到石墨化的碳微晶材料；
(4)将聚乙烯醇(PVA)交联剂在95℃下溶于水中,制备成质量分数为5％的溶液。在搅拌下加入上述制备的石墨化碳微晶粉末,进行交联稳定化处理得到稳定的水溶胶；
(5)水溶胶在-40℃下进行冷冻干燥处理，得到三维碳微晶气凝胶；
(6)采用旋涂法在碳微晶气凝胶表面均匀负载g-C3/N4/TiO2(光催化剂)水溶胶，80℃下干燥后制得单面具有可见光催化活性的碳气凝胶。
所述生物质碳源泥炭产自河南辉县。
表1本发明制备的碳材料的比表面积及孔径分析
| 样品 | 比表面积(m<sup>2</sup>/g) | 吸附总孔体积(cm<sup>3</sup>/g) | 吸附平均孔径(nm) |
| 碳化(550℃) | 215.605 | 0.195 | 3.579 |
| 石墨化(900℃) | 405.675 | 0.119 | 2.392 |
应用例1：在环境光催化领域应用
性能评价实验：所采用试样为本发明制备的光催化碳微晶气凝胶。利用500W氙灯、420nm滤光片作为可见光源，用1×10-5mol/L的亚甲基蓝(MB)染料溶液作为降解物。性能评价实验在光化学反应仪上完成。
具体操作步骤：准确称量25mg本发明光催化碳微晶气凝胶，将其分散于50mL的MB溶液中，得到悬浮液；将悬浮液进行超声分散10min，避光搅拌30min。然后进行光反应。取样间隔20min，反应时间2h。取样后离心分离，取上清液，在吸收波长λ＝664nm处测量其吸光度。反应性能测试结果见图5。其表现出较强的吸附性能和显著的光催化活性。
Claims (2)
1.一种光催化活性碳气凝胶材料，其特征在于，通过以下方法制得：
（1）生物质泥炭预处理：分别采用稀碱、稀酸溶液洗脱，去除泥炭中的无机矿物质；
（2）用含铁催化剂的溶液浸渍上述预处理后的泥炭，干燥后放入管式炉中，通入氮气或氩气作为保护气，控制升温速率进行焙烧处理；
（3）冷至室温后，加入盐酸溶液搅拌后过滤，用水洗涤至中性；干燥过夜，研磨得到石墨化碳微晶粉末；
（4）在搅拌下将石墨化碳微晶粉末加入交联剂溶液中，进行交联稳定化处理得到水溶胶；
（5）将水溶胶进行冷冻干燥处理，得到三维碳微晶气凝胶；
（6）采用旋涂法将光催化剂g-C3/N4/TiO2水溶胶均匀喷涂至三维碳微晶气凝胶表面，干燥后制得光催化碳气凝胶材料；
所述催化剂选自高铁酸钾；
所述交联剂选自聚乙烯醇、聚苯乙烯磺酸盐或二者组合；
步骤（4）中所述水溶胶的制备步骤：将石墨化碳微晶粉末加入到含有戊二醛、盐酸和聚乙烯醇混合溶液中，凝胶化处理；或将石墨化碳微晶粉末加入到交联剂C溶液中，凝胶化处理；所述交联剂C为聚乙烯醇在聚苯乙烯磺酸盐前驱体溶液中浸泡而得。
2.如权利要求1所述光催化活性碳气凝胶材料，其特征在于，所述高铁酸钾溶液浓度选：0.1mol/L；所述交联剂水溶液选质量分数为5% 的溶液。
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