CN113578281A - 一种玉米芯水热碳@聚多巴胺复合材料的制备及应用 - Google Patents
一种玉米芯水热碳@聚多巴胺复合材料的制备及应用 Download PDFInfo
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Abstract
本发明提供了一种玉米芯水热碳@聚多巴胺复合材料的制备方法，将自然风干的玉米芯破碎、筛分得玉米芯粉末，在玉米芯粉末中加入磷酸溶液，加水稀释并搅拌均匀后，于180~200℃反应15~20h，洗涤，烘干，得到玉米芯水热碳；将玉米芯水热碳超声分散在tris‑HCl溶液里，加入盐酸多巴胺，避光条件下，20~30℃搅拌5~6小时，离心分离，得到玉米芯水热碳@聚多巴胺复合材料。该复合材料制备过程简单，经济效益好、成本低、易降解、绿色环保，且比表面积大，含有丰富的羟基、羧基、儿茶酚基、醌和氨基等活性基团，能提供更多的金属离子吸附位点，对Cu2+具有优异的吸附能力，可用于的Cu2+的吸附。
Description
技术领域
本发明属于材料制备领域，涉及一种玉米芯水热碳@聚多巴胺复合材料的制备方法，本发明同时还涉及玉米芯水热碳@聚多巴胺复合材料在吸附Cu2+中的应用。
背景技术
目前重金属离子吸附材料在提高吸附容量的同时制备过程日益复杂，材料的成本比较高，大面积推广使用存在困难。玉米芯作为玉米加工后的农业废弃物，是一种可再生、易生物降解的环境友好型天然资源。玉米芯具有良好的亲水特异性结构，含有丰富活性基团的天然纤维素，因此能够对重金属离子等进行有效的吸附。
多巴胺在碱性条件和有氧气的环境下，其酚羟基首先发生氧化反应，形成不稳定的多巴胺醌结构，随后进行迈克尔加成反应产生分子成环形成多巴胺中间体，其进一步经过氧化和电子重排形成吲哚，这种吲哚也十分的不稳定，很容易氧化成吲哚醌结构，这两种结构会发生支化反应生成多种二聚体和不同的更加复杂的寡聚物，最后通过多巴胺的邻苯二酚与多巴胺醌的逆向歧化反应形成聚多巴胺结构。聚多巴胺含有丰富的羟基和氨基活性基团，能提供更多的金属离子吸附位点。本发明基于农业废弃物玉米芯和聚多巴胺合成一种用于吸附Cu2+的复合材料。
发明内容
本发明的目的是提供一种玉米芯水热碳@聚多巴胺复合材料的制备方法；
本发明的另一个目的是提供玉米芯水热碳@聚多巴胺复合材料在吸附Cu2+中的应用。
一、玉米芯水热碳@聚多巴胺复合材料的制备
本发明玉米芯水热碳@聚多巴胺复合材料的制备方法，包括以下工艺步骤：
（1）玉米芯水热碳的制备：将自然风干的玉米芯破碎、筛分得玉米芯粉末，在玉米芯粉末中加入磷酸溶液，加水稀释并搅拌均匀后，于180~200 ℃反应15~20h，洗涤，烘干，得到玉米芯水热碳。其中，磷酸溶液的浓度为1.5M；玉米芯粉末与磷酸溶液的质量体积比为0.1~0.2 g/mL。
（2）玉米芯水热碳@聚多巴胺复合材料的制备：将玉米芯水热碳超声分散在tris-HCl溶液里，加入盐酸多巴胺，避光条件下，20~30℃搅拌5~6小时，离心分离，烘干，得到玉米芯水热碳@聚多巴胺复合材料。其中，tris-HCl溶液的pH=8.0~8.5；玉米芯水热碳与盐酸多巴胺的质量比1:2~1:3。
二、玉米芯水热碳@聚多巴胺复合材料的表征
图1 为本发明玉米芯水热碳@聚多巴胺复合材料红外光谱图。从图中可以看到，3418 cm-1、1606 cm-1分别出现了聚多巴胺酚羟基和氨基的特征吸收峰，说明多巴胺发生了聚合，玉米芯水热碳@聚多巴胺制备成功。
图 2为玉米芯水热碳（A）和玉米芯水热碳@聚多巴胺复合材料（B）的扫描电镜图，玉米芯水热碳@聚多巴胺复合材料中可以看到在玉米芯水热碳的表面附着了一层薄膜材料，局部有微小聚多巴胺颗粒存在。
图 3 为玉米芯水热碳@聚多巴胺复合材料的氮气吸附脱附曲线（A）和孔径分布曲线（B），通过氮气吸脱附曲线可以以看出孔道分布不均匀，孔径分布主要集中在7-8 nm，该复合材料的比表面积53.33m2/g。
三、玉米芯水热碳@聚多巴胺复合材料的对Cu2+的吸附性能
将0.06 g功能化水热碳于锥形瓶中，加入15 mL浓度为100 mg/L Cu2+溶液，在温度为298 K、pH=6 静态吸附3 h。图 4为玉米芯水热碳@聚多巴胺复合材料对Cu2+的吸附曲线，玉米芯水热碳@聚多巴胺复合材料开始对Cu2+吸附量增加较快，3 h 时吸附量达到45 mg/g，基本达到吸附平衡。
本发明的有益效果：
1、本发明首先以玉米芯通过水热反应得到玉米芯水热碳，玉米芯水热碳为介孔材料，比表面积大，还有许多活性基团，对金属离子的有一定的吸附性能。基于玉米芯水热碳制备金属离子吸附材料，制备过程简单，经济效益好、成本低、易降解、绿色环保。
2、聚多巴胺的制备过程简单，容易操作，适合大量合成。玉米芯水热碳负载多巴胺后增加了复合材料的吸附位点，提高了对金属离子的吸附容量。
3、玉米芯水热碳@聚多巴胺复合材料含有丰富的羟基、羧基、儿茶酚基、醌和氨基等活性基团，能提供更多的金属离子吸附位点，对Cu2+具有优异的吸附性能。
附图说明
图1 为本发明玉米芯水热碳@聚多巴胺复合材料红外光谱图；
图 2为玉米芯水热碳（A）和玉米芯水热碳@聚多巴胺复合材料（B）的扫描电镜图；
图 3 为玉米芯水热碳@聚多巴胺复合材料的氮气吸附脱附曲线（A）和孔径分布曲线（B）；
图 4为玉米芯水热碳@聚多巴胺复合材料对Cu2+的吸附曲线。
具体实施方式
下面通过具体实例对本发明石墨烯玉米芯水热碳@聚多巴胺复合材料的制备及性能作进一步说明。
实施例1
（1）玉米芯水热碳的制备：将自然风干的玉米芯破碎后过0.25 mm 筛，除去大颗粒玉米芯。将0.5 g玉米芯粉末置于50 ml聚四氟乙烯反应釜，加入5 ml磷酸溶液（1.5M），加水稀释至40 ml，搅拌均匀后在200 ℃保温18h。产物水洗至中性，低温烘干备用。
（2）玉米芯水热碳@聚多巴胺复合材料的制备：0.1 g 玉米芯水热碳超声分散在50ml tris-HCl溶液（pH=8. 5）里，加入0.3 g 盐酸多巴胺，避光条件25℃下磁力搅拌 6小时，多次洗涤除去未反应的多巴胺，离心分离得到产物，低温烘干保存待用。玉米芯水热碳@聚多巴胺复合材料对Cu2+ 3 h 时的吸附量达到45 mg/g。
实施例2
（1）玉米芯水热碳的制备：将自然风干的玉米芯破碎后过0.20 mm 筛，除去大颗粒玉米芯。将1 g玉米芯粉末置于50 ml聚四氟乙烯反应釜，加入5 ml磷酸溶液（1.5M），加水稀释至40 ml，搅拌均匀后在200 ℃保温20h。产物水洗至中性，低温烘干备用。
（2）玉米芯水热碳@聚多巴胺复合材料的制备：0.5 g 玉米芯水热碳超声分散在100 ml tris-HCl溶液（pH=8. 5）里，加入1.0 g 盐酸多巴胺，避光条件下磁力搅拌 6小时，多次洗涤除去未反应的多巴胺，离心分离得到产物，低温烘干保存待用。 玉米芯水热碳@聚多巴胺复合材料对Cu2+3 h 时的吸附量达到42 mg/g。
Claims (5)
1.一种玉米芯水热碳@聚多巴胺复合材料的制备方法，包括以下工艺步骤：
（1）玉米芯水热碳的制备：将自然风干的玉米芯破碎、筛分得玉米芯粉末，在玉米芯粉末中加入磷酸溶液，加水稀释并搅拌均匀后，于180~200℃反应15~20 h，洗涤，烘干，得到玉米芯水热碳；
（2）玉米芯水热碳@聚多巴胺复合材料的制备：将玉米芯水热碳超声分散在tris-HCl溶液里，加入盐酸多巴胺，避光条件下，20~30℃搅拌5~6小时，离心分离，烘干，得到玉米芯水热碳@聚多巴胺复合材料。
2. 如权利要求1所述一种玉米芯水热碳@聚多巴胺复合材料的制备方法，其特征在于：步骤（1）中，磷酸溶液的浓度为1.5M；玉米芯粉末与磷酸溶液的质量体积比为0.1~0.2 g/mL。
3.如权利要求1所述一种玉米芯水热碳@聚多巴胺复合材料的制备方法，其特征在于：步骤（2）中，tris-HCl溶液的pH=8.0~8.5。
4.如权利要求1一种玉米芯水热碳@聚多巴胺复合材料的制备方法，其特征在于：步骤（2）中，玉米芯水热碳与盐酸多巴胺的质量比1:2~1:3。
5.如权利要求1所述方法制备的玉米芯水热碳@聚多巴胺复合材料在吸附Cu2+中的应用。
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| CN116510701A (zh) * | 2023-03-07 | 2023-08-01 | 武汉纺织大学 | 一种三醋酸纤维素/聚多巴胺复合微球的制备方法及产品 |
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