Name: preparation of hollow polystyrene particles and microcapsules by radical polymerization of janus droplets consisting of hydrocarbon and fluorocarbon oils
Uploaded: 2018-01-25T13:30:00
Duration: 7 min 1 s
Description: Watch this Scientific Journal Video about Preparation of Hollow Polystyrene Particles and Microcapsules by Radical Polymerization of Janus Droplets Consisting of Hydrocarbon and Fluorocarbon Oils at J

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1. 制备由苯乙烯/PFO/水溶液混合液组成的乳液
<ol><li>为制备5毫米的水 sds 溶液, 在高纯度 H2O 10 毫升中溶解14.5 毫克 sds。 注: 高纯度 H2O 已被使用 (电阻率 (R) = 18 ω cm, 表面张力 (γ) = 72.0 mN m-1在25° c)。</li>
	<li>加入1.5 克苯乙烯, 0.6 克 PFO, 0.9 克5毫米的水溶液 SDS 溶液到10毫升玻璃小瓶与搅拌棒。 注: 在扫描共聚焦荧光显微镜观察, 添加2.6 毫克香豆素102和0.062 毫克的素的混合物。</li>
	<li>在室温下搅动60分钟 1150 rpm 的混合物, 然后将温度升高到80° c。</li>
	<li>搅拌的混合物为60分钟, 在 1150 rpm 和80° c。</li>
</ol>2. 用苯乙烯/PFO/水溶液混合物组成的乳液制备聚合物微粒
<ol><li>添加3.9 毫克的钾硫酸钾, 2 毫克的芘, 1.5 克苯乙烯, 0.6 克 PFO, 0.9 克5毫米的水溶液 SDS 溶液到10毫升玻璃小瓶与搅拌棒和密封它与橡胶隔膜。</li>
	<li>通过注射器针将氮气 Deoxygenate 30 分钟。 注意: 缓慢流动的氮气不会产生大量的泡沫。</li>
	<li>准备乳液, 搅拌60分钟的混合物在 1150 rpm 和室温, 然后提高温度到80° c。</li>
	<li>搅拌的混合物为30分钟, 在 1150 rpm 和80° c。</li>
	<li>将所产生的溶液 (3 毫升) 中的多云部分 (1.8 毫升) 转移到试管中, 然后加入30% 乙醇溶液以完全终止聚合反应。</li>
	<li>几种 (功率: 130 W, 频率: 4.2 赫), 10 分钟洗涤产生的聚合物粒子, 然后离心10分钟, 在 2300 x g。</li>
	<li>要获得聚合物粒子, 从试管中除去上清溶液。</li>
	<li>在试管中加入3毫升的水到所产生的固体中。几种 (功率: 130 W, 频率: 4.2 赫) 为10分钟和离心机为 10 min 在 2300 x g. 从试管中取出上清液。</li>
	<li>重复洗涤过程 (步骤 2.8), 直到没有从上清溶液生成泡沫。蒸发水获得固体的空心高分子颗粒。</li>
</ol>3. 利用空心高分子微粒制备微胶囊
<ol><li>加入1毫克的空心聚苯乙烯颗粒 (步骤 2.9) 和4毫升的水到一个10毫升玻璃小瓶与搅拌棒。</li>
	<li>几种 (功率: 130 W, 频率: 4.2 赫), 用于在水中分散空心粒子10分钟。</li>
	<li>在室温下, 将0.1 毫升的甲苯添加到水中分散的颗粒, 然后搅拌1小时 100 rpm。将液体转移到试管。 注意: 如果每分钟的自转增加, 粒子的形态就会变形。</li>
	<li>离心液体为10分钟在 2300 x g 分离微囊形成它。从试管中取出上清液。</li>
</ol>

<ol>
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A., Chang, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic-Assisted+Synthesis+of+Polymer+Particles.">Microfluidic-Assisted Synthesis of Polymer Particles.</a> Chem Eng Tech. 31 (8), 1099-1115 (2008).</li><li>Higuchi, T., Yabu, H., Shimomura, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simple+preparation+of+hemispherical+polystyrene+particles.">Simple preparation of hemispherical polystyrene particles.</a> Colloids Surf A. 284, 250-253 (2006).</li><li>Sun, Z. Q., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonspherical+Colloidal+Crystals+Fabricated+by+the+Thermal+Pressing+of+Colloidal+Crystal+Chips.">Nonspherical Colloidal Crystals Fabricated by the Thermal Pressing of Colloidal Crystal Chips.</a> Langmuir. 21 (20), 8987-8991 (2005).</li><li>Deng, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+novel+approach+to+the+construction+of+3-D+ordered+macrostructures+with+polyhedral+particles.">A novel approach to the construction of 3-D ordered macrostructures with polyhedral particles.</a> J Mater Chem. 18 (4), 408-415 (2008).</li><li>Hyuk Im, S., Jeong, U., Xia, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+hollow+particles+with+controllable+holes+in+their+surfaces.">Polymer hollow particles with controllable holes in their surfaces.</a> Nat Mater. 4 (9), 671-675 (2005).</li><li>Saito, N., Kagari, Y., Okubo, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+Colloidal+Stabilizer+on+the+Shape+of+Polystyrene/Poly(methyl+methacrylate)+Composite+Particles+Prepared+in+Aqueous+Medium+by+the+Solvent+Evaporation+Method.">Effect of Colloidal Stabilizer on the Shape of Polystyrene/Poly(methyl methacrylate) Composite Particles Prepared in Aqueous Medium by the Solvent Evaporation Method.</a> Langmuir. 22 (22), 9397-9402 (2006).</li><li>Cai, P. -. j., Tang, Y. -. j., Wang, Y. -. t., Cao, Y. -. j. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fabrication+of+polystyrene+hollow+spheres+in+W/O/W+multiple+emulsions.">Fabrication of polystyrene hollow spheres in W/O/W multiple emulsions.</a> Mater Chem Phys. 124 (1), 10-12 (2010).</li><li>Liang, S. -. S., Chen, S. -. L., Chen, S. -. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Diverse+macroporous+spheres+synthesized+by+multiple+emulsion+polymerization+for+protein+analyses.">Diverse macroporous spheres synthesized by multiple emulsion polymerization for protein analyses.</a> Chem Commun. 47 (29), 8385-8387 (2011).</li><li>Kondo, Y., Yoshino, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hybrid+fluorocarbon/hydrocarbon+surfactants.">Hybrid fluorocarbon/hydrocarbon surfactants.</a> Curr Opin Colloid Interface Sci. 10 (3-4), 88-93 (2005).</li><li>Takahashi, Y., Kondo, Y., Schmidt, J., Talmon, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Self-Assembly+of+a+Fluorocarbon-Hydrocarbon+Hybrid+Surfactant:+Dependence+of+Morphology+on+Surfactant+Concentration+and+Time.">Self-Assembly of a Fluorocarbon-Hydrocarbon Hybrid Surfactant: Dependence of Morphology on Surfactant Concentration and Time.</a> J Phys Chem B. 114 (42), 13319-13325 (2010).</li><li>Takahashi, Y., Nasu, Y., Aramaki, K., Kondo, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Unusual+viscoelastic+behavior+of+aqueous+solutions+of+fluorocarbon-hydrocarbon+hybrid+surfactant+and+its+morphological+transformations.">Unusual viscoelastic behavior of aqueous solutions of fluorocarbon-hydrocarbon hybrid surfactant and its morphological transformations.</a> J Fluor Chem. 145, 141-147 (2013).</li><li>Yoshino, N., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Syntheses+of+Hybrid+Anionic+Surfactants+Containing+Fluorocarbon+and+Hydrocarbon+Chains.">Syntheses of Hybrid Anionic Surfactants Containing Fluorocarbon and Hydrocarbon Chains.</a> Langmuir. 11 (2), 466-469 (1995).</li><li>Zarzar, L. 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在水 SDS 浓度和苯乙烯、PFO 的重量分数的 10% 以上, 得到了含苯乙烯和 PFO 的乳液。当含有该液滴的乳液的各种重量分数被聚合为30分钟时, 可以获得所有成分的空心聚苯乙烯颗粒。这些结果表明, 此处所示的协议很简单。此外, 本文所述方法中的聚合时间可以控制空心聚苯乙烯颗粒的直径、孔径大小和孔体积。
我们建议以下的机制来制造空心聚苯乙烯颗粒。在80° c 的含水 SDS 溶液、苯乙烯和 PFO 混合物的 O/W 乳液中形成了由苯乙烯和 PFO 组成的两面油滴。PFO 液滴位于苯乙烯滴的表面。由于作为聚合的引发剂的科索沃警察部队在水相中是可溶的, 聚合将在苯乙烯/水溶液 SDS 溶液的界面上进行。在80° c 时, 三元乳液中苯乙烯聚合成聚苯乙烯, 而 PFO 没有聚合基团, 在该温度下仍留在乳液中。聚合终止后, 通过去除 PFO, 形成聚苯乙烯颗粒上的孔。因此, 在表面上有孔的中空杯状聚苯乙烯颗粒是任何苯乙烯和 PFO 的重量分数和所有聚合时间的产物。
在90分钟内, 将少量的甲苯加入到由自由基聚合制备的空心聚苯乙烯颗粒上, 就会使空心聚苯乙烯颗粒上的孔洞得到密封。这一现象与赫 al.9报告的是一致的。封装法可以在微粒中含有水的物质。
在本文中, 我们展示了一种使用由苯乙烯和 PFO 组成的含油滴的中空聚合物颗粒的制备方法, 它们是相互不相容的。非球形高分子颗粒的制备方法, 由于其在各种应用中的潜在用途, 已经得到了广泛的研究。该策略采用烃油和氟碳油的两面油滴, 适用于不同类型单体和药物输送系统的非球形聚合物颗粒的制备。

虽然球形高分子颗粒已广泛应用于各种工业应用, 但众所周知, 酒窝粒子, 半球, 磁盘, 和椭球, 已准备通过播种聚合1,2,3, 使用具有特定几何形状的微的非球形单体液滴的光聚合,4,5, 使用聚合物再的自组织6, 以及球形聚合物的变形微粒由机械外部力量7,8。特别是, 由溶剂9,10 , 用多乳剂聚合而成的球形高分子颗粒的好溶剂蒸发制备了微米级的中空聚合物颗粒。11,12。
在这项工作中, 我们关注的是烃类和氟碳油的相互溶在聚合物微粒的制造中的应用。混合表面活性剂在分子中有一个碳氢化合物链和一个氟碳链。此前, 我们报告了在常规表面活性剂中未观察到的混合表面活性剂的独特特性13,14,15。我们还研究了使用烃类油、氟碳油和表面活性剂溶液的乳液, 它们是相互不相容的16。然而, 对乳剂的研究很少有17。这些研究描述了由烃油和氟碳油组成的油滴在表面活性剂溶液中的形貌。
在这里, 我们展示了一个详细的协议制造空心聚合物颗粒的基础聚合使用油滴的乳液由烃油, 氟碳油, 和水钠硫酸钠 (SDS) 溶液。本文提出了一种新的非球形高分子颗粒制备方法, 它有别于常规的工艺。该方法能在短时间内简单地制备空心高分子颗粒。此外, 还显示了通过空心高分子微粒制备微胶囊的协议。

<table>
	<tbody>
		<tr>
			<td>Material</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Sodium dodecylsulfate, 95.0%</td>
			<td>Wako Pure Chemical Industries, Ltd.</td>
			<td>192-08672</td>
			<td></td>
		</tr>
		<tr>
			<td>Styrene, 99.0%</td>
			<td>Tokyo Chemical Industry Co. Ltd.</td>
			<td>S0095</td>
			<td></td>
		</tr>
		<tr>
			<td>Perfluorooctane, 99%</td>
			<td>Fluorochem Ltd.</td>
			<td>8706</td>
			<td></td>
		</tr>
		<tr>
			<td>Coumarin 102, 97.0%</td>
			<td>Tokyo Chemical Industry Co. Ltd.</td>
			<td>C2267</td>
			<td></td>
		</tr>
		<tr>
			<td>Calcein</td>
			<td>Dojindo Molecular Technologies, Inc.</td>
			<td>C001</td>
			<td></td>
		</tr>
		<tr>
			<td>Potassium peroxodisulfate, 98.0%</td>
			<td>Kanto Chemical Co., Inc.</td>
			<td>32375-30</td>
			<td></td>
		</tr>
		<tr>
			<td>Pyrene, 97.0%</td>
			<td>Wako Pure Chemical Industries, Ltd.</td>
			<td>167-05302</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol, 99.5%</td>
			<td>Kanto Chemical Co., Inc.</td>
			<td>14033-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Toluene, 99.5%</td>
			<td>Kanto Chemical Co., Inc.</td>
			<td>40180-00</td>
			<td></td>
		</tr>
		<tr>
			<td>Name</td>
			<td>Company</td>
			<td>Catalog Number</td>
			<td>Comments</td>
		</tr>
		<tr>
			<td>Equipment</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope</td>
			<td>Hitachi High-Technologies Corporation</td>
			<td>S-4800</td>
			<td></td>
		</tr>
		<tr>
			<td>Scanning Transmission Electron Microscope</td>
			<td>Hitachi High-Technologies Corporation</td>
			<td>S-4800</td>
			<td></td>
		</tr>
		<tr>
			<td>Ultrasonic cleaner</td>
			<td>Branson Ultrasonics, Emerson Japan, Ltd.</td>
			<td>Model 3510</td>
			<td></td>
		</tr>
		<tr>
			<td>Centrifuge</td>
			<td>AS ONE Corporation</td>
			<td>CN-1050</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation of hollow polystyrene particles and microcapsules by radical polymerization of janus droplets consisting of hydrocarbon and fluorocarbon oils

在这篇文章中, 我们已经演示了一种方法, 生产空心颗粒和微胶囊使用油滴由烃油 (苯乙烯) 和氟碳油 (氟-n-辛烷, PFO) 在水表面活性剂 (钠硫酸钠,SDS) 解决方案。由于氟碳油与烃类油不相容, 这两种油分离。乳液是由搅拌苯乙烯/PFO/水 SDS 溶液混合物在80° c。用光学显微镜和扫描共聚焦荧光显微镜观察了乳液的类型和液滴的形貌。结果表明, 在 SDS 溶液中形成了由相互不相容的苯乙烯和 PFO 组成的油滴。聚苯乙烯颗粒是由苯乙烯/PFO/水 SDS 溶液在80° c 的三元混合物的自由基聚合制备的。通过扫描电子显微镜和扫描透射电镜观察, 证实了聚苯乙烯的形貌。这些观察表明, 表面上有一个孔的聚苯乙烯空心颗粒的制备。根据我们的知识, 这种方法是一种新的战略使用溶烃和氟碳油。空心颗粒也可用于微胶囊的制备。

光和扫描共聚焦荧光显微镜观察, 以确定的形态和组成的液滴在乳液由苯乙烯, PFO, 和5毫米水溶液 SDS (图 1)。扫描电子显微镜 (SEM) 和扫描透射电镜 (词干) 观察显示空心粒子和微胶囊的形成 (图 2)。
由苯乙烯/PFO/水 sds 溶液三元混合物组成的乳剂的 DIC 和共聚焦荧光显微图像表明, 连续相是水 sds 溶液, 因为在素中观察到的绿色荧光连续相, 因此, 油内水型乳剂形成 (图 1a和1b)。这些图像还表明, 油滴包括苯乙烯和 PFO, 这是相互不相容的。含香豆素102乳剂的 DIC 和共焦荧光显微图像显示, PFO 液滴位于水与苯乙烯滴之间的界面上。苯乙烯、PFO 和水 SDS 溶液的三元混合物, 其5毫米的乳液含有由苯乙烯和 PFO 组成的两面油滴。
styrene/PFO/5 毫米水溶液的乳液自由基聚合制备的聚合物粒子的扫描电镜和干图表明, 表面有孔的空心非球形聚苯乙烯颗粒 (图 2a和2b). 通过扫描电镜和茎秆观察200粒子, 评价空心聚苯乙烯颗粒的形成速率、直径和孔径。平均直径估计从 SEM 观察是1.3 µm。尺寸与由动态光散射测量估计的聚合物颗粒的直径一致。形成率约为100%。空心颗粒中孔的平均孔径和体积分别为0.8 ±0.4 µm 和0.9 ±0.4 µm3。因此, 在乳液中含有苯乙烯的同液滴的自由基聚合, 制备出具有0.8 µm 孔的空心聚苯乙烯颗粒。
<img alt="Figure 1" class="xfigimg" src="/files/ftp_upload/56922/56922fig1.jpg"> 图1。由苯乙烯、PFO 和5毫米水溶液 SDS 溶液组成的乳液中的液滴形态.(a)差分干扰对比 (DIC) 和(b)共焦荧光显微图像的乳液含有水荧光素。(c) DIC 和(d)含有油溶性荧光香豆素102的乳剂的共焦荧光显微图像。<a href="//cloudflare.jove.com/files/ftp_upload/56922/56922fig1large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>
<img alt="Figure 2" class="xfigimg" src="/files/ftp_upload/56922/56922fig2.jpg"> 图2。采用苯乙烯、PFO 和5毫米水溶液 SDS 的乳液组成的空心聚苯乙烯颗粒和微胶囊的形貌。(a) SEM 和(b)空心聚苯乙烯颗粒的茎图像。(c) SEM 和(d)微胶囊的茎图像。<a href="//cloudflare.jove.com/files/ftp_upload/56922/56922fig2large.jpg" target="_blank">请单击此处查看此图的较大版本.</a>

Watch this Scientific Journal Video about Preparation of Hollow Polystyrene Particles and Microcapsules by Radical Polymerization of Janus Droplets Consisting of Hydrocarbon and Fluorocarbon Oils at J

Preparation of Hollow Polystyrene Particles and Microcapsules by Radical Polymerization of Janus Droplets Consisting of Hydrocarbon and Fluorocarbon Oils

由烃类和氟碳油组成的同液滴的自由基聚合制备空心聚苯乙烯颗粒和微胶囊

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In this article, we have demonstrated a method for producing hollow particles and microcapsules using oil droplets consisting of hydrocarbon oil (styrene) ...

Research

JoVE Journal

Chemistry

Origami Inspired Self-assembly of Patterned and Reconfigurable Particles

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科研

化学

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Using Polystyrene-block-poly(acrylic acid)-coated Metal Nanoparticles as Monomers for Their Homo- and Co-polymerization

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Atom Transfer Radical Polymerization of Functionalized Vinyl Monomers Using Perylene as a Visible Light Photocatalyst

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A Simple and Efficient Protocol for the Catalytic Insertion Polymerization of Functional Norbornenes

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Norbornene can be polymerized by a variety of mechanisms, including insertion polymerization whereby the double bond is polymerized and the bicyclic ...