CN108607607A - 一种功能性细菌纤维素的制备方法 - Google Patents
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Abstract
本发明公开了一种功能性细菌纤维素的制备方法，涉及功能纤维素技术领域，该制备方法以细菌纤维素、纳米TiO2和Ag离子为原料，采用添加纳米TiO2的营养液进行细菌纤维素的培养，然后将培养出的细菌纤维素进行水洗、碱煮、在水洗和冷冻干燥处理后，最后冷冻干燥后的细菌纤维素采用磁控溅射技术进行Ag离子溅射，制备的功能性细菌纤维素相对于纯细菌纤维素具有良好的光催化性能，采用磁控溅射技术将银离子沉积在细菌纤维素表面，使银离子均匀且牢固负载在细菌纤维素上，有效提高Ag沉积的TiO2量子产率。
Description
技术领域
本发明属于功能材料技术领域，涉及细菌纤维素技术领域，具体涉及一种功能性细菌纤维素的制备方法。
背景技术
自然界中有少数细菌可以产生纤维素，其中木醋菌属中的木醋杆菌合成纤维素的能力最强，具有大规模生产的能力。为了区别于植物来源的纤维素,称微生物合成的纤维素为细菌纤维素(Bacterial cellulose，简称BC)。它是一种多孔性网状纳米级生物高分子聚合物，具有独特的超精细纳米网络结构、良好的持水性和吸水性以及优异的机械性能和生物相容性等特点。基于以上优点，细菌纤维素开始被应用于光催化领域，但是由于其本身功能性的不足而需要进行进一步的功能整理。
纳米TiO2是一种白色、无毒的粉末。它的优点主要有抗化学和光腐蚀、光催化活性高、对废水中的有机物降解无选择性、无二次污染等优点，是目前被称为拥有广阔应用前景的光催化剂。研究表明，在TiO2材料中掺杂其他物质对其改性，如有机染料，聚合物和金属等，此类掺杂物质可成为光生电子和空穴的捕获阱，能够降低电子和空穴对的复合几率，同时降低TiO2禁带宽度，从而增强TiO2对光的利用。贵金属沉积所形成的金属－半导体电极，能使光生电子在Ag岛上富集，光生空穴向TiO2晶粒表面迁移，从而促进光生电子和空穴的有效分离。
磁控溅射是由二极溅射基础上发展而来，在靶材表面建立与电场正交磁场，解决了二极溅射沉积速率低，等离子体离化率低等问题，成为目前镀膜工业主要方法之一。磁控溅射与其它镀膜技术相比具有如下特点：可制备成靶的材料广，几乎所有金属，合金和陶瓷材料都可以制成靶材；在适当条件下多元靶材共溅射方式，可沉积配比精确恒定的合金；在溅射的放电气氛中加入氧、氮或其它活性气体，可沉积形成靶材物质与气体分子的化合物薄膜；通过精确地控制溅射镀膜过程，容易获得均匀的高精度的膜厚；通过离子溅射靶材料物质由固态直接转变为等离子态，溅射靶的安装不受限制，适合于大容积镀膜室多靶布置设计；溅射镀膜速度快，膜层致密，附着性好等特点，很适合于大批量，高效率工业生产。
发明内容
根据以上现有技术的不足，本发明所要解决的技术问题是提出一种将细菌纤维素、磁控溅射技术、银离子与纳米TiO2的优点相结合，使纳米TiO2有效地负载在细菌纤维素这样载体上，提高光的利用率，进而有效提升光催化效率的功能性细菌纤维素的制备方法，为了解决上述技术问题，本发明采用的技术方案为：
一种功能性细菌纤维素的制备方法，具体步骤如下：
1)将胰蛋白胨、酵母粉和甘露醇配置成营养液，将营养液分装并加入纳米TiO2颗粒，最后将营养液进行高温灭菌，无菌冷却，在细菌纤维素培养中加入纳米TiO2颗粒，将细菌纤维素作为纳米TiO2的载体，防止纳米TiO2颗粒发生集聚、失活，提高对光的利用率，使其能够更好的应用于光催化领域；
2)将原菌液加入冷却后的营养液中进行接种，将接种好的营养液进行静态培养；
3)将培养的细菌纤维素取出，依次进行去离子水冲洗、碱煮、去离子水冲洗至中性、去离子水水洗和冷冻干燥；
4)对冷冻干燥后的细菌纤维素进行银离子的磁控溅射，得功能性细菌纤维素，在细菌纤维素表面沉积银离子，对TiO2产生协同促进作用，从而提高其光催化活性，扩大其光吸收波长范围，进而提高光量子效率。
优选的，所述营养液中胰蛋白胨、酵母粉和甘露醇的质量比为5:3:25。
优选的，所述纳米TiO2颗粒的添加量为0.01-0.03g。
优选的，所述碱煮的碱液为浓度0.1-0.2moL/L的NaOH溶液，时长为6-12h；所述去离子水洗时长为6-12h。
优选的，所述磁控溅射参数为：真空度为7×10-4-9×10-4Pa，工作气体为99.999％的氩气，气体流量为15-25mL/min，工作压强为2-4Pa，溅射功率为50-80w，溅射时间为30-90s，采用磁控溅射技术将银离子沉积在细菌纤维素表面，使银离子均匀且牢固负载在细菌纤维素上，有效提高Ag沉积的TiO2量子产率。
与现有技术相比，本发明的有益效果：
1.本发明采用细菌纤维作为纳米TiO2的粉末的载体，细菌纤维素作为一种新型的环境友好性能优异的材料，具有防止纳米TiO2颗粒发生集聚、失活，提高对光的利用率，使其能够更好的应用于光催化领域。
2.本发明采用在细菌纤维素表面沉积银离子，对TiO2产生协同促进作用，从而提高其光催化活性，扩大其光吸收波长范围，进而提高光量子效率。
3.本发明采用磁控溅射技术将银离子沉积在细菌纤维素表面，使银离子均匀且牢固负载在细菌纤维素上，有效提高Ag沉积的TiO2量子产率，制备的磁控溅射Ag/原位生长纳米TiO2细菌纤维素应用于有机染料光催化降解领域，具有显著的功能性。
附图说明
1.图1是细菌纤维素SEM图片；
2.图2是原位生长纳米TiO2细菌纤维素SEM图片；
3.图3是磁控溅射Ag/原位生长纳米TiO2细菌纤维素SEM图片。
具体实施方式
下面通过对实施例的描述，作进一步详细的说明，以帮助本领域技术人员对本发明的发明构思、技术方案有更完整、准确和深入的理解。
实施例1
本实施例中功能性细菌纤维素的制备方法，具体步骤如下：
1)将胰蛋白胨、酵母粉和甘露醇按质量比为5:3:25配置成营养液，将配置的营养液按体积200mL分装到培养瓶中，并向培养瓶中加入0.01g的纳米TiO2颗粒，最后将装有营养液的培养瓶置于高压灭菌锅中在温度126℃，压力0.15MPa进行高温灭菌55min，然后进行无菌冷却；
2)在生物安全柜中，利用移液枪移取10mL木醋杆菌原菌液加入冷却后的营养液中进行接种，将接种好的营养液放置于摇床培养箱中进行静态培养7天；
3)将培养出的细菌纤维素取出，先用去离子水冲洗，去除培养好的细菌纤维素表面的可见残留培养基固体物质,然后置于浓度为0.1moL/L的NaOH溶液中进行碱煮6h，碱煮结束后将细菌纤维素用去离子水冲洗至中性，最后再放入去离子水中进行水洗6h，将用去离子水清洗后的细菌纤维素后放入冷冻干燥机中，在真空度为70pa、冷阱温度为-67℃、样品温度为15℃条件下进行冷冻干燥16h；
4)对冷冻干燥后的细菌纤维素在真空度为8×10-4Pa，纯度99.999％氩气工作气体，流量为20mL/min，工作压强为2Pa，溅射功率为50w进行银离子磁控溅射30s，得功能性细菌纤维素。
实施例2
本实施例同实施例1，不同的是本实施例中分装营养液体积为150mL，碱煮的碱液为浓度0.11moL/L的NaOH溶液，去离子水水洗时长为12h。
实施例3
本实施例同实施例1，不同的是本实施例中原菌液体积为15mL，静态培养5天，碱煮的碱液为浓度0.11moL/L的NaOH溶液，碱煮时长12h，去离子水水洗时长为12h。
实施例4
光催化性能测试
配置浓度为0.5mol/L的亚甲基蓝溶液，在4个试管中分别放入50mL亚甲基蓝溶液，将质量为10mg的纯细菌纤维素和实施例1-3制备的细菌纤维素放入试管中，在功率为300w的汞灯照射下，经过120min催化降解反应后，取一定量的亚甲基蓝溶液，测试其在664nm波长处的吸光度大小，由公式(1)计算得到亚甲基蓝降解率。测试结果如表1所示。由表1可知，磁控溅射Ag/原位生长纳米TiO2细菌纤维素具有良好的光催化性能。
表1亚甲基蓝降解率
| 亚甲基蓝降解率 | |
| 纯细菌纤维素 | 29.1％ |
| 实施例1 | 46.9％ |
| 实施例2 | 48.2％ |
| 实施例3 | 47.6％ |
上面结合具体实施例对本发明进行了示例性描述，显然本发明具体实现并不受上述方式的限制，只要采用了本发明的方法构思和技术方案进行的各种非实质性的改进，或未经改进将本发明的构思和技术方案直接应用于其它场合的，均在本发明的保护范围之内。本发明的保护范围应该以权利要求书所限定的保护范围为准。
Claims (5)
1.一种功能性细菌纤维素的制备方法，其特征在于，具体步骤如下：
1)将胰蛋白胨、酵母粉和甘露醇配置成营养液，将营养液分装并加入纳米TiO2颗粒，最后将营养液进行高温灭菌，无菌冷却；
2)将原菌液加入冷却后的营养液中进行接种，将接种好的营养液进行静态培养；
3)将培养的细菌纤维素取出，依次进行去离子水冲洗、碱煮、去离子水冲洗至中性、去离子水水洗和冷冻干燥；
4)对冷冻干燥后的细菌纤维素进行银离子的磁控溅射，得功能性细菌纤维素。
2.根据权利要求1所述的功能性细菌纤维素的制备方法，其特征在于，所述营养液中胰蛋白胨、酵母粉和甘露醇的质量比为5:3:25。
3.根据权利要求1所述的功能性细菌纤维素的制备方法，其特征在于，所述纳米TiO2颗粒的添加量为0.01-0.03g。
4.根据权利要求1所述的功能性细菌纤维素的制备方法，其特征在于，所述碱煮的碱液为浓度0.1-0.2moL/L的NaOH溶液，时长为6-12h；所述去离子水洗时长为6-12h。
5.根据权利要求1所述的功能性细菌纤维素的制备方法，其特征在于，所述磁控溅射参数为：真空度为7×10-4-9×10-4Pa，工作气体为99.999％的氩气，气体流量为15-25mL/min，工作压强为2-4Pa，溅射功率为50-80w，溅射时间为30-90s。
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