葡萄糖水热法制备纳米碳球
广州华南农业大学理学院09材化(2)班林勋,200930750211
引言
小鸟画炭微球材料由于其具有高密度、高强度、高比表面积以及在锂离子电池方面的应用前景,已经引起许多研究人员的兴趣。碳微球的形状和大小显著影响着其电学性能。
葡萄糖在水热条件下会发生许多化学反应,实验结果表明:炭微球的增长似乎符合LaMer模型(见图1),当 0.5 mol·L-1 的葡萄糖溶液在低于140 C 或反应时间小于1h
时不会形成炭球,在此条件下反应后溶液呈橙色或红色并且粘度增强,表明有芳香族化合物和低聚糖形成,这是反应的聚合步骤。当反应条件为0.5 mol·L-1、160℃、3h
时开始出现成核现象,这个碳化步骤可能是由于低聚糖之间分子间脱水而引起的交联反应,或者在先前步骤中有其它大分子的形成,然后形成的核在溶液中各向同性生长所致。从现有的研究结果表明,制备过程中的反应条件如葡萄糖的起始浓度、反应温度和反应时间直接影响炭球的粒径分布,其中反应时间对颗粒粒径影响很大,随着反应时间的延长,这些纳米炭球粒径从150nm(最初核的大小,实验所得到的最小的尺寸)生长到1500 nm。
杨士莪由葡萄糖水热法制备纳米炭球具有绿色环保无污染的特点,实验过程中没有引入任何引发剂以及有毒溶剂,制备得到的炭球粒径均匀,大小可控,同时表面含有大量活性官能团,具有优良的亲水性和表面反应活性,可应用于生物化学、生物诊断以及药物传输领域,也可以作为制备核壳结构材料或者多孔材料的模板等等,具有令人欣喜的应用前景。
图1 水热法形成炭球的结构变化示意图
1 实验部分
1.1 实验仪器与试剂
葡萄糖,去离子水,95%乙醇,50mL高压反应釜,鼓风干燥箱,电子天平,抽滤装置(有机滤膜),滤纸,玻璃棒
1.2 纳米碳球的制备
纳米碳球的制备参见文献[1]。用电子天平称取 6g
葡萄糖放入50mL反应釜内衬(图2)中,用移液管准确移取35mL去离子水(葡萄糖溶液的浓度为0.952 mol·L-1
)加入到上述反应釜中,用玻璃棒搅拌溶液,使葡萄糖全部溶解,然后装入反应釜中,用扳手拧紧反应釜,放入烘箱中。设定反应条件为:温度 180 C,反应时间 4~12
h。待反应结束后,降至室温,取出反应釜,将釜内黑褐色溶液抽滤(用40
um有机滤膜),并及时清洗反应釜内衬,抽滤时用去离子水和 95%
乙醇清洗至滤液为无色。将样品用滤纸包好放入干燥箱中70℃干燥
奔跑吧蔷薇
4h。收集样品,称重并计算产率。
图2反应釜实物与结构示意图
1.3 纳米碳球的表征
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do "four", that is, find the problem faster, editorial writing, nd and read faster approval and feedback to implement quickly. To be true and accurate. True mainly reflect the full picture of events, one is one, two, this is the life of the information. Accuracy is primarily qualitative and quantitative questions, quantitative objective of publicQualitative logic. To be reliable and uful. We submit information to have access to decision-making, to guide and promote the work and solve practical problems. Mixed cum. On the negative information and emergency information, rapid escalation in strict accordance with the procedures, firm, newspaper, newspapers, never late, fail to report, fal claim and skimming. Investee 2. supervision and insist on, around and protecting their interests to touch the truth, ek practical results. Adhere to people-oriented, the most important thing is to realize, safeguard and develop the fundamental interests of the overwhelming majority of the people. We carry out inspection, so must go deep among the mass, go deep into the realities, always pay attention to the people's livelihood, to grasp the public ntiment, and earnestly safeguard the benefit, addressing the mass are most concerned about and reflecting the strongest issues, efforts to solve the problem of decisions implemented and not implemented. One is to stick to principles. Right of inspection is one of the most important powers of the Office, should not only dare to u, but also with caution. So-called dared to u, is to hold a number of important issues, bold supervision over supervision, track inspection, problems are not solved do not pass, the blame does not hold did
not miss, dissatisfaction of the mass did not miss, the real right of supervision authority, with the benefits. Call with caution, is supervising departments should strengthen the consciousness of authorized strictly according to procedure, preventing the supervision and excessive to prevent adding burden to grass-roots. To this end, the supervision Department of the Party Committee of supervision must be under city and County party Committee Secretary-General (Office). Second, we should focus on. Is the Governor, tho related to the globalEvent, Governor the protracted difficult, strong Governor during emergency urgent. Not having special departments in charge of the General Governor, under the normal procedure can do good things not Governor, not authorized by County leaders, not the Governor. Third is to solve the problem. The purpo of supervision, to resolve the problem. To adhere to and further improve the
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the party Office around connecting, coordinating internal and external features, contact, rally at all levels, to motivate every aspect, adhere to the truth, strengthening standardized management to achieve coherent, efficient and effective functioning of the daily work of the Party Committee. Is processing messages should strive to streamline, standardize and quality. Streamlining is to control the number of messages, compress messages, reducing procedures, improve message handling efficiency. Specifications, is to strictly enforce the ban issued by the Communist party authorities in document handling regulations and provincial and municipal regulations, conscientiously strengthen and improve communications management to ensure that party documents orderly. High quality, is to improve the quality of message processing, it is necessary to accurately implementing the intention of the Party Committee, clearance, good communications, policy program clod, ensuring that there is no error. Second meeting scheduled to ensure thorough, safe and efficient. Any arrangements for the meetings and events, carefully arranged, item-by-item interface implemented, sure. To vigorously streamline meetings, activities, number of pressure reduction, scale to ensure that leadership emerged from the General Conference and entertainment rvices, focus on big things, matters. Third, reception rvices should lay stress on humane, personal, cultural and human. Reception and work directly with people, reception rvices directly affecting the Office of party Committee The image of the region. At the same time strengtheni
ng the construction of library, improve the reception conditions, more human-oriented, personal, cultural work into the reception, a little more human needs, a little more human care more humane atmosphere, and constantly improve the rvice, improve the quality of rvice. Meanwhile, to further pay special attention to the daily work of the other Office System. Confidential work responsibility system for leading cadres to implement curity as a leader, to improve the confidentiality of classified personnel, especially leading cadres, strengthening party and Government focus on vital ctors of curity management, to advance privacy management standardization, modernization of curity techniques as a means of administration according to law and curity enforcement, ensure the safety of the party and State crets. Confidential work to meet the demands of new technology development
1.3.1 X-射线衍射分析
冬瓜牛肉汤测定所制备碳球的晶型以判断该碳球所属的类型(如普通碳还是石墨型碳)
1.3.2 红外光谱分析
测定碳球的活性官能团,表征不同制备条件下得到的碳球活性官能团变化
2 结果与讨论
2.1 实验数据
实验最终制备得到的纳米碳球的质量为 0.1255 g ,根据下列化学方程式
助学申请书怎么写C 6H 12O 6 6C+6H 2O
可得产率23%.5100%4
.21255.0100%理论产率实际产率ω=⨯=⨯=2.2 纳米碳球的结构表征
2.2.1 纳米碳球的XRD 表征分析
图3、图4给出的是天然石墨和非晶型碳的标准XRD 谱图,图5、图6给出的是在不同样品板上检测实验制备的纳米碳球的XRD 谱图。对比可得,实验制备所得的纳米碳球与非晶型碳更加接近,故而初步判断实验所得的纳米碳球是非晶型碳。
图5为在玻璃样品板上检测所得的XRD 谱图,从图中可以看出在21°附近有一个大的经典词句
“馒头峰”,可以断定纳米碳球是非晶态型结构物质;图6为在铝质样品板上检测所得的XRD 谱
图;可以看出除了有个大的“馒头峰”外,还有两个高而尖锐的峰,即存在晶型结构的物质:Al 2O 3 晶
体,参见文献[2]可知,该晶体为 α-Al 2O 3,属于三方晶系。
图3 天然石墨
图4 非晶型碳
图5 玻璃样品板图6 铝质样品板
家常菜大全菜谱2.2.2 红外光谱分析
图7为碳球的红外光谱图。从图7中可看出:3400cm-1
附近对应为羟基的吸收峰;同时羰基(C=O)振动吸收峰红移到1700 cm-1处;1620cm-
1对应共轭烯烃骨架振动;1500 cm-1到1300 cm-1 峰的存在可能为苯环骨架振动。
由上述官能团存在的可能性表明碳球保留了葡萄糖分子中的大量官能团,葡萄糖在水解过程中可能产生一定程度的芳香化,因为在水热反应过程中糖分子之间发生了分子间脱水交联反应,再脱水、碳化形成碳碳单键和双键,使得产物部分碳化,达到制备碳微球目的,这与制备机理较为符合。综上,碳球的宫能团以―OH、C=O
为主,水热过程中发生了脱水缩合和芳环化过程。
图7 纳米碳球的红外谱图
2.3 水热法制备碳球的优缺点
优点:工艺流程简单、可连续生产、原料便宜、安全无毒;产物粒径小、分布均匀、颗粒团聚轻、晶形好且可控、不需高温烧结,省去了研磨以及由此带来的杂质,避免缺陷。
缺点:反应在密闭容器中进行,无法观察生长过程、对设备要求高(耐高温高压的钢材,耐腐蚀的内衬)、技术难度大(温压控制严格);安全性能差。
2.4 影响碳球形成的因素
葡萄糖的起始浓度、反应温度、反应时间和清洗过程都直接影响碳球的粒径分布,其中反应时
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