基于脲醛树脂模板构建磁性微球
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摘要
磁性纳米晶体和微球推动了生物技术、医药科技、催化、核磁造影、数据存储及环境治理等领域的技术革新,并发挥着日益重要的作用。虽然目前已经发展了一些方法来制造磁性微球和纳米晶体,但是可用于生产高质量、可扩大制备的方法并不多。因此,急需开发新的制备方法来批量制备新型、高质量、低成本的磁性微球来满足日益增长的使用需求。
为此,我们开发了一系列基于脲醛树脂模板的磁性微球制备技术,制备出一系列新型的磁性微球,并用SEM、TEM、VSM、XRD、BET、TGA、FTIR、DLS等手段进行表征,并对微球的形成做了较为系统的研究。取得成果如下:
1)开发了室温一锅法制备磁性微球的新方法,直接将磁性纳米粒子包埋于脲醛树脂制得单分散超顺磁性微球,并将其成功的应用于人血基因组DNA的提取。在聚合过程中加入荧光物质可以得到高荧光强度的双功能磁性微球。并对脲醛树脂微球的形成机理做了系统的研究,并采用吸光度法实时监控了聚合反应浊度变化过程。
2)开发了水热还原制备磁性微球新方法,将磁性前驱体包埋于脲醛树脂制得非磁性复合微球再通过水热还原得到磁性微球,该方法可获得磁性更强的单分散磁性微球,并被成功的应用于酵母和玉米基因组DNA的提取。还阐述了水热还原羟基铁氧化物的机理。
3)开发了制备多孔四氧化三铁磁性微球新方法,该方法通过灼烧将脲醛树脂基质从复合微球中除去,得到多孔的三氧化二铁微球再通过水热还原得到多孔纯四氧化三铁微球。所制备得磁性微球为立方型四氧化三铁纳米粒子堆砌而成的多孔四氧化三铁微球,饱和磁化强度高达72 emu/g。该种微球对砷吸附模型证实该微球对砷有较强的吸附,可以用于水中砷处理。
4)对氢气还原法制备碳包覆磁性微球进行了初探,用氢气法还原羟基铁氧化物/UF微球时,得到磁性微球及结构新颖的四氧化三铁纳米管。用化学气相沉积法(CVD)制备磁性微球时,得到碳包覆磁性微球和碳纤维棒。在用CVD法制备碳包覆磁性二氧化硅微球时,可以发现硅球表面生成碳纳米管的生长点,还意外的得到单分散纳米石墨微球。
基于脲醛树脂为模板用四种方法构建了四种新型磁性微球,并将水热还原制备高磁化强度磁性纳米粒子,这四种制备方法都具有易于实施、低成本、环境友好、易于放大生产的特点。本论文在这种背景下展开研究,具有很大的理论意义和实用价值。
Magnetic microspheres and nanocrystals are of great interest for researchers from a wide range of hot research field including biotechnology/biomedicine, catalysis, magnetic resonance imaging, data storage, and environmental remediation.
Although a number of suitable methods have been developed for the synthesis of magnetic nanoparticles of various different compositions, few of them are capable of producing high quality magnetic microspheres with large quantity. Therefore, it’s of great urgency to develop methods for large scale production of these materials to meet growing demands from the above fields.
Our research is focused on the development of methods for preparation of magnetic microspheres based on the urea-formaldehyde templates and production of a series of novel functional magnetic microspheres. Those novel magnetic microspheres fully characterized by SEM, TEM, VSM, XRD, BET, TGA, FTIR, DLS have been successfully applied to the DNA extraction and arsenic removal. The results are list as follows:
1) Development of novel method for one pot preparation of magnetic microspheres at room temperature. By this method, magnetic nano particles were embedded by UF to form the microspheres with sphereical like morphology and 8 emu/g magnetic saturation. The microspheres were applied to extraction of DNA from human blood. Also, the fluorescent compounds can be added during the polymerization to form the bi-functional microspheres. The mechanism of UF microspheres were studied systematically.
2) Development of novel method for two-step preparation of magnetic microspheres. The method is based on the formation of iron hydroxide/polymer composite microspheres followed by in situ conversion to strong magnetizable them to magnetite nanocrystals by reaction with sodium borohydride under hydrothermal conditions. The obtained magnetic crystals embedded in the polymer matrix are of cubic shape and highly crystalline structure. The magnetic particles were used as adsorbents for isolation of genomic DNA from biological samples, with results comparable to those obtained by magnetic silica microspheres.
3) Development of a novel method for three-step preparation of porous magnetite microspheres. As for two-step method, the ironhydroxide/UF microspheres were stablized by condensation polymerization and then subjected to heating treatment to remove polymer template. The porous iron-oxide was transferred into magnetite by thermal reduction. The porous magnetite microspheres were proved be an effective adsorbent for removal of arsenic from the water.
4) Investigation on high temperature reduction of magnetic precursors embedded in UF matrix at H2 atmospheres in attempt to preparation of carbon coated magnetic microspheres. The reduction of hydroxide/UF microspheres by H2 produces the magnetite nano tubes along with magnetic microspheres. A CVD procedure applied for hydroxide/UF produces magnetic microspheres and carbon fiber, and for iron coated microspheres produced the highly uniform graphite nanospheres with magnetic microspheres.
Incorporation of iron hydroxide colloids into polymer microspheres coupled with chemically induced phase transformation represents a new cost-effective approach to the preparation of uniform magnetic microspheres that is more controllable with respect to particle properties and more amenable to large-scale production.
The above results confirm that the novel system of magnetic microspheres preparation based on urea formaldehyde polymerization is facile, cost-effective, environmentally benign, and readily scaled up for mass production.
为此,我们开发了一系列基于脲醛树脂模板的磁性微球制备技术,制备出一系列新型的磁性微球,并用SEM、TEM、VSM、XRD、BET、TGA、FTIR、DLS等手段进行表征,并对微球的形成做了较为系统的研究。取得成果如下:
1)开发了室温一锅法制备磁性微球的新方法,直接将磁性纳米粒子包埋于脲醛树脂制得单分散超顺磁性微球,并将其成功的应用于人血基因组DNA的提取。在聚合过程中加入荧光物质可以得到高荧光强度的双功能磁性微球。并对脲醛树脂微球的形成机理做了系统的研究,并采用吸光度法实时监控了聚合反应浊度变化过程。
2)开发了水热还原制备磁性微球新方法,将磁性前驱体包埋于脲醛树脂制得非磁性复合微球再通过水热还原得到磁性微球,该方法可获得磁性更强的单分散磁性微球,并被成功的应用于酵母和玉米基因组DNA的提取。还阐述了水热还原羟基铁氧化物的机理。
3)开发了制备多孔四氧化三铁磁性微球新方法,该方法通过灼烧将脲醛树脂基质从复合微球中除去,得到多孔的三氧化二铁微球再通过水热还原得到多孔纯四氧化三铁微球。所制备得磁性微球为立方型四氧化三铁纳米粒子堆砌而成的多孔四氧化三铁微球,饱和磁化强度高达72 emu/g。该种微球对砷吸附模型证实该微球对砷有较强的吸附,可以用于水中砷处理。
4)对氢气还原法制备碳包覆磁性微球进行了初探,用氢气法还原羟基铁氧化物/UF微球时,得到磁性微球及结构新颖的四氧化三铁纳米管。用化学气相沉积法(CVD)制备磁性微球时,得到碳包覆磁性微球和碳纤维棒。在用CVD法制备碳包覆磁性二氧化硅微球时,可以发现硅球表面生成碳纳米管的生长点,还意外的得到单分散纳米石墨微球。
基于脲醛树脂为模板用四种方法构建了四种新型磁性微球,并将水热还原制备高磁化强度磁性纳米粒子,这四种制备方法都具有易于实施、低成本、环境友好、易于放大生产的特点。本论文在这种背景下展开研究,具有很大的理论意义和实用价值。
Magnetic microspheres and nanocrystals are of great interest for researchers from a wide range of hot research field including biotechnology/biomedicine, catalysis, magnetic resonance imaging, data storage, and environmental remediation.
Although a number of suitable methods have been developed for the synthesis of magnetic nanoparticles of various different compositions, few of them are capable of producing high quality magnetic microspheres with large quantity. Therefore, it’s of great urgency to develop methods for large scale production of these materials to meet growing demands from the above fields.
Our research is focused on the development of methods for preparation of magnetic microspheres based on the urea-formaldehyde templates and production of a series of novel functional magnetic microspheres. Those novel magnetic microspheres fully characterized by SEM, TEM, VSM, XRD, BET, TGA, FTIR, DLS have been successfully applied to the DNA extraction and arsenic removal. The results are list as follows:
1) Development of novel method for one pot preparation of magnetic microspheres at room temperature. By this method, magnetic nano particles were embedded by UF to form the microspheres with sphereical like morphology and 8 emu/g magnetic saturation. The microspheres were applied to extraction of DNA from human blood. Also, the fluorescent compounds can be added during the polymerization to form the bi-functional microspheres. The mechanism of UF microspheres were studied systematically.
2) Development of novel method for two-step preparation of magnetic microspheres. The method is based on the formation of iron hydroxide/polymer composite microspheres followed by in situ conversion to strong magnetizable them to magnetite nanocrystals by reaction with sodium borohydride under hydrothermal conditions. The obtained magnetic crystals embedded in the polymer matrix are of cubic shape and highly crystalline structure. The magnetic particles were used as adsorbents for isolation of genomic DNA from biological samples, with results comparable to those obtained by magnetic silica microspheres.
3) Development of a novel method for three-step preparation of porous magnetite microspheres. As for two-step method, the ironhydroxide/UF microspheres were stablized by condensation polymerization and then subjected to heating treatment to remove polymer template. The porous iron-oxide was transferred into magnetite by thermal reduction. The porous magnetite microspheres were proved be an effective adsorbent for removal of arsenic from the water.
4) Investigation on high temperature reduction of magnetic precursors embedded in UF matrix at H2 atmospheres in attempt to preparation of carbon coated magnetic microspheres. The reduction of hydroxide/UF microspheres by H2 produces the magnetite nano tubes along with magnetic microspheres. A CVD procedure applied for hydroxide/UF produces magnetic microspheres and carbon fiber, and for iron coated microspheres produced the highly uniform graphite nanospheres with magnetic microspheres.
Incorporation of iron hydroxide colloids into polymer microspheres coupled with chemically induced phase transformation represents a new cost-effective approach to the preparation of uniform magnetic microspheres that is more controllable with respect to particle properties and more amenable to large-scale production.
The above results confirm that the novel system of magnetic microspheres preparation based on urea formaldehyde polymerization is facile, cost-effective, environmentally benign, and readily scaled up for mass production.
引文
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