Name: synthesis of hydrogels with antifouling properties as membranes for water purification
Uploaded: 2017-04-07T14:00:00.000+00:00
Duration: 7 min 32 s
Description: Watch this Scientific Journal Video about Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification at JoVE.com

We gratefully acknowledge the financial support of this work by the Korean Carbon Capture and Sequestration R&amp;D Center (KCRC).

1.预聚物溶液的制备<ol><li> 使用水作为溶剂制备 <ol><li> 10.00克去离子（DI）水添加到玻璃瓶中有磁力搅拌棒。 </li><li>测量2.00克SBMA的，并将其转移至含有水的玻璃瓶中。搅拌30分钟的溶液中，直到SBMA完全溶解。 </li><li>在一个单独的瓶中，加入20.00克PEGDA的（m×n个 = 700克/摩尔）。 </li><li>添加20.0毫克1-羟基环己基苯酮（HCPK），光引发剂，给PEGDA溶液。让溶液搅拌至少30分钟。 </li><li>使用一次性吸管，转移8.00克的PEGDA-HCPK解决SBMA水溶液。连续地搅拌混合物，直到该溶液均匀。 </li></ol></li><li> 使用水/乙醇混合物作为溶剂制备 <ol><li>添加6.00克DI水和4.00g的乙醇成琥珀色玻璃瓶有磁力搅拌棒。搅拌溶液，以便充分混合。 </li><li> 2.00克SBMA添加到水/乙醇混合物。搅拌溶液，并允许SBMA完全溶解。 </li><li>使用移液管〜8.00克PEGDA-HCPK溶液转移到SBMA混合物。搅拌至溶液充分混合。 </li></ol></li></ol> 2.独立式膜的制备<ol><li>放置两个间隔件用干净的石英盘上的已知厚度;间隔件的厚度来控制所获得的聚合物薄膜19的厚度。 </li><li>转移预聚物溶液的少量（〜1.0mL）中，使用一个一次性吸石英光盘。 </li><li>放置在液体顶部另一个石英盘，并确保有在液膜没有气泡。 </li><li>放置在紫外线（UV）的交联剂的样品和照射了使用UV光以254纳米19的波长5分钟。 注:另类照射时间S和波长可根据光引发剂的类型来使用。 </li><li>使用锋利的刀片的石英盘分离的聚合物膜。用镊子将膜转印到DI水浴。第一个24小时期间换水两次以从膜除去溶剂，未反应的单体/交联剂，和溶胶。 注意:所述的聚合物膜应保持在去离子水以保持孔结构，如果有的话。 </li><li>制备用于ATR-FTIR和DSC分析干燥的膜。 <ol><li>从水浴中取出薄膜，并允许它在空气中干燥24小时。 </li><li>放置膜在真空烘箱中在80℃下在真空下干燥过夜。 </li></ol></li></ol> 3.浸渍膜的制备<ol><li>的多孔性支撑体的片材放置到石英盘。 </li><li>使用泡沫刷，涂覆支撑的每一侧两次基于水/乙醇混合物4的预聚物溶液。 注意:因为T他支持是疏水性的，含有乙醇的预聚物溶液可以很容易地浸湿载体。 </li><li>将另一石英盘上的支持之上。 </li><li>将样品在UV交联剂和照射用于使用UV光的254nm波长的5分钟。 </li><li>以除去从石英盘上的含浸膜，浸泡在DI水浴整个组件5分钟，并小心地取出用锋利的刀片和镊子的膜。 </li><li>请去离子水的膜。换水两次以除去溶剂，未反应的单体/交联剂，并从膜的溶胶。 </li><li>制备干燥的，浸渍的膜为ATR-FTIR和DSC分析。 <ol><li>取下水浴膜。允许该膜在环境条件下干燥24小时。 </li><li>在真空中干燥该膜烘箱中过夜，在真空下80℃。 </li></ol></li></ol> 4.表征独立式薄膜和浸渍的Membranes <ol><li> ATR-FTIR分析 <ol><li>制备预聚物溶液的样品，如在步骤1.1所述，用于FTIR分析。 </li><li>扫描样品之前执行后台扫描。波数范围内设定为600 -1至4,500厘米-1处测量的4 -1分辨率。 </li><li>将样品在FTIR机进行分析。 </li><li>取出样品。清洁晶体并用合适的溶剂的尖端。 </li><li>重复步骤4.1.1 - 4.1.4下列样品:多孔质支撑体，预聚物溶液，干燥独立膜，并干燥浸渍的膜。 </li></ol></li><li> 差扫描量热法（DSC） <ol><li>将DSC盘中，并盖在天平称量并记录自己的体重。 </li><li>放置盘内样品（5-10毫克）少量，用盖子关闭它。 </li><li>称量含有样品的盘。从邻之间的重量差ccupied锅和盖子和未占用的锅和盖，计算样品的重量。 </li><li>使用压力机，气密密封所述盘内部的样品。 </li><li>放置在其中的惰性参考位于DSC单元内的密封盘。 </li><li>进入未占据盘和盖，并在程序中的样本的重量的重量。 </li><li>用-80℃的DSC至160℃以10℃/ min的加热速率进行扫描。 </li><li>执行使用制造商的协议DSC分析。 </li><li>重复以下的上述步骤不同样品的DSC实验。 </li></ol></li><li> 使用悬滴法接触角的测定 <ol><li>切膜样品（约30毫米×6mm）的的矩形条。 </li><li>浸泡在去离子水中这条10分钟，然后晾干5分钟。 </li><li>放置在样本夹持器干燥样品。 </li><li>浸没样品架中的透明含有去离子水20的环境室中。 </li><li>使用微升注射器用不锈钢针，分配Ñ -癸烷（约1μL）滴在膜样品。 </li><li>离开不受干扰2分钟的设置，以确保液滴的稳定化。 </li><li>使用适当的图像分析软件通过测量在膜表面上的分配的液滴的角度，以确定样品的接触角。 </li><li>采取的各种液滴获得的接触角值的平均值。 </li></ol></li><li> 使用死端过滤系统的水渗透性的表征 <ol><li>用锤子驱动打孔器与适当的直径切割独立膜和浸渍的膜的优惠券。 </li><li>放置一个制备优惠券上的死端过滤单元内的多孔载体上。 </li><li>放在样品的顶部上的O形环。拧两半渗透细胞的一起。 </li><li>添加约50mL DI水到渗透细胞。拧上盖子，并将渗透细胞在磁力搅拌器上。组300和900的转速之间搅拌速度。 </li><li>放在天平上的覆盖烧杯收集渗透水。去皮。 </li><li>打开气瓶阀。顺时针压力调节阀打开，直到达到所需的压力（45psig下为独立式膜和35 psig的用于浸渍的膜）。 </li><li>打开释放阀以递送压力，以渗透细胞。 </li><li>监测和记录时间的烧杯的重量。 </li><li>计算水的渗透率（A W）和渗透性（P w）的与所述溶液-扩散模型下面4所示，21 <img alt="方程" src="/files/ftp_upload/55426/55426eq1.jpg" /> 其中，A w是第È水渗透率（L / m 2的HBAR或LMH /巴），P w是水渗透率（LMH厘米/巴），ρw是水的密度（克/升），A是膜的有效面积（m 2），ΔM为在水渗透物（克）在时间周期Δt（H）的质量变化，ΔP是穿过膜（巴的压力差），并且l是溶胀膜（厘米）的厚度。 </li><li>使用含有在pH = 7.4的磷酸盐缓冲盐水（PBS）溶液0.5g / L的BSA一个BSA溶液来评价膜的防污性和废品率。 </li><li>重复步骤4.4.5 - 4.4.10确定BSA存在的水通量。计算与下面的等式22中的BSA废品率 <img alt="方程" src="/files/ftp_upload/55426/55426eq2.jpg" /> 其中R BSA是膜（％）的BSA排斥率，中c p是BSA在渗透物（克/升）的浓度，和C F是BSA的进料（克/升）的浓度; BSA的浓度可通过UV光谱法来确定。 </li></ol></li></ol>

<ol>
	<li>Qasim, M., Darwish, N. A., Sarp, S., Hilal, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Water+desalination+by+forward+(direct)+osmosis+phenomenon:+A+comprehensive+review.">Water desalination by forward (direct) osmosis phenomenon: A comprehensive review.</a> Desalination. , 47-69 (2015).</li><li>Geise, G. M., 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=Water+purification+by+membranes:+The+role+of+polymer+science.">Water purification by membranes: The role of polymer science.</a> J. Polym. Sci. Part B Polym. Phys. 48 (15), 1685-1718 (2010).</li><li>Miller, D. J., Dreyer, D., Bielawski, C., Paul, D. R., Freeman, B. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+modification+of+water+purification+membranes:+A+review.">Surface modification of water purification membranes: A review.</a> Angew Chem Int Ed Engl. , (2016).</li><li>Zhao, S. Z., Huang, K. P., Lin, H. Q. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Impregnated+Membranes+for+Water+Purification+Using+Forward+Osmosis.">Impregnated Membranes for Water Purification Using Forward Osmosis.</a> Ind. Eng. Chem. Res. 54 (49), 12354-12366 (2015).</li><li>Ostuni, E., Chapman, R. G., Holmlin, R. E., Takayama, S., Whitesides, G. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+survey+of+structure-property+relationships+of+surfaces+that+resist+the+adsorption+of+protein.">A survey of structure-property relationships of surfaces that resist the adsorption of protein.</a> Langmuir. 17 (18), 5605-5620 (2001).</li><li>Jiang, S., Cao, Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultralow-fouling,+functionalizable,+and+hydrolyzable+zwitterionic+materials+and+their+derivatives+for+biological+applications.">Ultralow-fouling, functionalizable, and hydrolyzable zwitterionic materials and their derivatives for biological applications.</a> Adv Mat. 22 (9), 920-932 (2010).</li><li>Shah, S., 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=Transport+properties+of+small+molecules+in+zwitterionic+polymers.">Transport properties of small molecules in zwitterionic polymers.</a> J. Polym. Sci. Part B Polym. Phys. 54 (19), 1924-1934 (2016).</li><li>Shao, Q., Jiang, S. Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Molecular+Understanding+and+Design+of+Zwitterionic+Materials.">Molecular Understanding and Design of Zwitterionic Materials.</a> Adv Mat. 27 (1), 15-26 (2015).</li><li>Zhang, Z., Chao, T., Chen, S., Jiang, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Superlow+Fouling+Sulfobetaine+and+Carboxybetaine+Polymers+on+Glass+Slides.">Superlow Fouling Sulfobetaine and Carboxybetaine Polymers on Glass Slides.</a> Langmuir. 22 (24), 10072-10077 (2006).</li><li>Chen, S., Li, L., Zhao, C., Zheng, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+hydration:+principles+and+applications+toward+low-fouling/nonfouling+biomaterials.">Surface hydration: principles and applications toward low-fouling/nonfouling biomaterials.</a> Polymer. 51 (23), 5283-5293 (2010).</li><li>Bengani, P., Kou, Y. M., Asatekin, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Zwitterionic+copolymer+self-assembly+for+fouling+resistant,+high+flux+membranes+with+size-based+small+molecule+selectivity.">Zwitterionic copolymer self-assembly for fouling resistant, high flux membranes with size-based small molecule selectivity.</a> J Membr Sci. 493, 755-765 (2015).</li><li>Chiang, Y. C., Chang, Y., Chuang, C. J., Ruaan, R. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+facile+zwitterionization+in+the+interfacial+modification+of+low+bio-fouling+nanofiltration+membranes.">A facile zwitterionization in the interfacial modification of low bio-fouling nanofiltration membranes.</a> J Membr Sci. 389, 76-82 (2012).</li><li>Mi, Y. F., Zhao, Q., Ji, Y. L., An, Q. F., Gao, C. J. <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+route+for+surface+zwitterionic+functionalization+of+polyamide+nanofiltration+membranes+with+improved+performance.">A novel route for surface zwitterionic functionalization of polyamide nanofiltration membranes with improved performance.</a> J Membr Sci. 490, 311-320 (2015).</li><li>Shafi, H. Z., Khan, Z., Yang, R., Gleason, K. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+modification+of+reverse+osmosis+membranes+with+zwitterionic+coating+for+improved+resistance+to+fouling.">Surface modification of reverse osmosis membranes with zwitterionic coating for improved resistance to fouling.</a> Desalination. 362, 93-103 (2015).</li><li>Yang, R., Goktekin, E., Gleason, K. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Zwitterionic+Antifouling+Coatings+for+the+Purification+of+High-Salinity+Shale+Gas+Produced+Water.">Zwitterionic Antifouling Coatings for the Purification of High-Salinity Shale Gas Produced Water.</a> Langmuir. 31 (43), 11895-11903 (2015).</li><li>Yang, R., Jang, H., Stocker, R., Gleason, K. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synergistic+Prevention+of+Biofouling+in+Seawater+Desalination+by+Zwitterionic+Surfaces+and+Low-Level+Chlorination.">Synergistic Prevention of Biofouling in Seawater Desalination by Zwitterionic Surfaces and Low-Level Chlorination.</a> Adv Mat. 26 (11), 1711-1718 (2014).</li><li>Azari, S., Zou, L. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Using+zwitterionic+amino+acid+L-DOPA+to+modify+the+surface+of+thin+film+composite+polyamide+reverse+osmosis+membranes+to+increase+their+fouling+resistance.">Using zwitterionic amino acid L-DOPA to modify the surface of thin film composite polyamide reverse osmosis membranes to increase their fouling resistance.</a> J Membr Sci. 401, 68-75 (2012).</li><li>Chang, C., 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=Underwater+Superoleophobic+Surfaces+Prepared+from+Polymer+Zwitterion/Dopamine+Composite+Coatings.">Underwater Superoleophobic Surfaces Prepared from Polymer Zwitterion/Dopamine Composite Coatings.</a> Adv Mater Inter. , (2016).</li><li>Lin, H., Kai, T., Freeman, B. D., Kalakkunnath, S., Kalika, D. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Effect+of+Cross-Linking+on+Gas+Permeability+in+Cross-Linked+Poly(Ethylene+Glycol+Diacrylate).">The Effect of Cross-Linking on Gas Permeability in Cross-Linked Poly(Ethylene Glycol Diacrylate).</a> Macromolecules. 38 (20), 8381-8393 (2005).</li><li>Sagle, A. C., Ju, H., Freeman, B. D., Sharma, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=PEG-based+hydrogel+membrane+coatings.">PEG-based hydrogel membrane coatings.</a> Polymer. 50 (3), 756-766 (2009).</li><li>Wu, Y. -. H., Park, H. B., Kai, T., Freeman, B. D., Kalika, D. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Water+uptake,+transport+and+structure+characterization+in+poly(ethylene+glycol)+diacrylate+hydrogels.">Water uptake, transport and structure characterization in poly(ethylene glycol) diacrylate hydrogels.</a> J Membr Sci. 347 (1-2), 197-208 (2010).</li><li>Rahimpour, A., 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=Novel+functionalized+carbon+nanotubes+for+improving+the+surface+properties+and+performance+of+polyethersulfone+(PES)+membrane.">Novel functionalized carbon nanotubes for improving the surface properties and performance of polyethersulfone (PES) membrane.</a> Desalination. 286, 99-107 (2012).</li><li>Gulmine, J. V., Janissek, P. R., Heise, H. M., Akcelrud, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polyethylene+characterization+by+FTIR.">Polyethylene characterization by FTIR.</a> Polym Testing. 21 (5), 557-563 (2002).</li><li>Ara&#250;jo, J. R., Waldman, W. R., De Paoli, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+properties+of+high+density+polyethylene+composites+with+natural+fibres:+Coupling+agent+effect.">Thermal properties of high density polyethylene composites with natural fibres: Coupling agent effect.</a> Polym. Degrad. Stab. 93 (10), 1770-1775 (2008).</li><li>McCloskey, B. D., 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=Influence+of+polydopamine+deposition+conditions+on+pure+water+flux+and+foulant+adhesion+resistance+of+reverse+osmosis,+ultrafiltration,+and+microfiltration+membranes.">Influence of polydopamine deposition conditions on pure water flux and foulant adhesion resistance of reverse osmosis, ultrafiltration, and microfiltration membranes.</a> Polymer. 51 (15), 3472-3485 (2010).</li></ol>

The authors declare that they have no competing financial interests.

我们已经证明了一个浅显的方法来制备独立电影和基于两性离子水凝胶浸渍膜。三（甲基）丙烯酸酯的特征峰的消失（ 即 ，810，1190，和1410厘米-1）在所得到的聚合物膜的红外光谱和含浸膜（ 图2）表示的单体和交联剂4的良好的转化率， 19，21。此外，该SO 3的外观-在光谱的膜和膜振动峰证实了两性离子基团已被成功地引入到水凝胶。将所得到的共聚物具有可忽略的溶胶部分，表明该共聚物的组合物是非常相似的预聚物溶液中7。 S30的Tg值和S50是相似的，这表明在预聚物溶液中的溶剂类型对的Tg的影响最小。对于含浸膜，熔融峰归因于多孔载体（聚乙烯），这表明该膜的承诺，以维持高温和高压穿过膜。 通过悬滴法接触角测量是只适用于多孔载体。该方法不能用于在这项工作中所制造的自支撑膜和薄膜，因为样品从样品架中的水腔室浸没时脱离自己。因此，对于这些样品的接触角测量，通过简单地在样品表面的顶部滴加水（1.0-5.0μL）小液滴进行测定。用于支撑接触角比那些自支撑膜和含浸膜的，这证实了更大的亲水性在这些zwitterioni高得多Ç水凝胶。 各样品的透水通过死端过滤系统来确定。水合S50薄膜厚度为471吨微米的展品的最低水渗透率（0.085 LMH /巴），而S30膜和IMS30膜表现出较高的水渗透率。 本文介绍了一种简便的方法通过光聚合用于水净化以制造基于水凝胶的独立式膜和浸渍膜。含有PEGDA和SBMA与亲水性水凝胶是合成的，并且它们可以增强浸渍膜的多孔载体的亲水性。该报告提供了在准备这些材料和鉴定它们的物理特性，包括水的传输性能实用的指导。该方法和材料也可用于制备气体分离膜，如CO 2捕获。

有一个非常需要开发低成本和高效节能技术，以满足日益增长的需求，产生干净的水。聚合物膜已成为一个领先的技术水净化由于其固有的优点，诸如它们的高的能量效率，成本低，简单并在操作1。膜允许纯水渗透通过而拒绝该污染物。然而，膜往往受到由在进料水中的污染物，其可以被吸附在膜表面上从它们的有利的相互作用2,3结垢。结垢可显着通过膜减少的水通量，增加所需要的薄膜面积和水净化的成本。 以减轻结垢的有效途径是修改膜表面以增加亲水性，从而降低在有利膜表面和污物之间teractions。一种方法是使用薄膜涂层具有超亲水3倍的水凝胶。水凝胶通常具有高的水渗透性;因此，薄膜涂层可以增加通过膜的长期水渗透率由于减轻的结垢，尽管在整个膜中的略微增加输送阻力。水凝胶也可以直接制作成用于水净化的浸渍膜渗透压应用4。 两性离子物质同时含有正和负电荷的官能团，具有净中性电荷，并且具有通过静电诱导的氢键5，6，7，8，9强表面水化。紧密结合的水化层用作物理和能垒，从而防止污物附着在表面上，因此证明优异的防污性10。两性离子聚合物，如聚（磺基甜菜碱甲基丙烯酸酯）（PSBMA）和聚（羧基甜菜碱甲基丙烯酸酯）（PCBMA），已被用于修饰膜表面通过涂布11，12，13，14，15，16，17，18，以增加表面亲水性，因此防污性。 我们在这里表明了容易的方法，以制备使用经由光聚合，这是使用聚（乙二醇）交联的磺基甜菜碱甲基丙烯酸酯（SBMA）两性离子水凝胶丙烯酸酯（PEGDA，m×n个 = 700克/摩尔），以改善机械强度。我们还提出一个过程通过在光聚合前的高度多孔疏水性载体含浸于单体和交联剂以构建健壮膜。独立式膜和浸渍膜的物理和水输送性质彻底特征在于阐明用于水净化的结构/性质关系。所制备的水凝胶可用于作为表面涂层，以提高膜的分离性能。通过调整交联密度或通过浸渍到疏水性多孔载体，这些材料也能形成薄膜，与用于渗透过程，诸如正向渗透或压力延迟渗透4足够的机械强度。

<table><tbody><tr><td>Poly(ethylene glycol) diacrylate&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp;&amp;nbsp; M&lt;sub&gt;n&lt;/sub&gt; = 700 (PEGDA)</td><td>Sigma Aldrich</td><td>455008</td><td></td></tr><tr><td>1-Hydroxycyclohexyl phenyl ketone, 99% (HCPK)</td><td>Sigma Aldrich</td><td>405612</td><td></td></tr><tr><td>[2-(Methacrloyloxy)ethyl dimethyl-(3-sulfopropyl) ammonium hydroxide, 97%</td><td>Sigma Aldrich</td><td>537284</td><td>Acutely Toxic</td></tr><tr><td>Ethanol, 95%</td><td>Koptec, VWR International</td><td>V1101</td><td>Flamable</td></tr><tr><td>Decane, anhydrous, 99%</td><td>Sigma Aldrich</td><td>457116</td><td></td></tr><tr><td>Solupor Membrane</td><td>Lydall</td><td>7PO7D</td><td></td></tr><tr><td>Micrometer&amp;nbsp;</td><td>Starrett</td><td>2900-6</td><td></td></tr><tr><td>ATR-FTIR</td><td>Vertex 70</td><td></td><td></td></tr><tr><td>DSC: TA Q2000</td><td>TA Instruments</td><td></td><td></td></tr><tr><td>Rame&amp;rsquo;-hart Goniometer: Model 190</td><td>Rame&amp;rsquo;-hart Instruments</td><td></td><td></td></tr><tr><td>Ultraviolet Crosslinker: CX-2000</td><td>Ultra-Violet Products</td><td></td><td>UV radiation&amp;nbsp;</td></tr><tr><td>Permeation Cell: Model UHP-43</td><td>Advantec MFS</td><td></td><td></td></tr><tr><td>Deionized Water: Milli-Q Water</td><td>EMD Millipore</td><td></td><td></td></tr></tbody></table>

synthesis of hydrogels with antifouling properties as membranes for water purification

水凝胶已被广泛利用，以提高水的净化膜的表面亲水性，增加了防污性，从而通过膜随时间获得稳定的水渗透性。在这里，我们报告一个浅显的方法来制备基于两性离子的膜应用的水凝胶。独立式的薄膜可以由磺基甜菜碱甲基丙烯酸酯（SBMA）通过光聚合的聚交联剂（乙二醇）二丙烯酸酯（PEGDA）来制备。水凝胶也可通过浸渍制备成疏水性的多孔载体，以提高机械强度。这些膜可以通过衰减全反射傅立叶来表征变换红外光谱（ATR-FTIR）来确定（甲基）丙烯酸酯基团的转化程度，使用亲水性和差示扫描量热法（DSC）对聚合物链的动态测角器。我们还报告的协议，以确定死胡同FILTRA的透水性灰系统和污垢对膜性能的影响（牛血清白蛋白，BSA）。

随着在步骤1.1和1.2中指定的预聚物溶液制备自立式膜分别称为S50和S30。详细信息显示在表1中 。在步骤1.2中指定的预聚物溶液也用于制造浸渍膜，其被表示为IMS30。由于多孔性支撑体是由疏水性的聚乙烯的，仅含有乙醇的预聚物溶液可以浸渍到载体并形成透明膜， 如图1 4。 在PEGDA和SBMA的（甲基）丙烯酸酯基团的转化率通过ATR-FTIR光谱证实。 图2呈现的多孔载体的红外光谱，预聚物溶液，干燥的聚合物膜（S50和S30），并干燥浸渍的膜（IMS30）。在SP的多孔性支撑体的（a）示出了ectrum围绕1460厘米-1，其与弯曲变形23相关联的特征峰。该预聚物溶液（b）的红外光谱显示在810处的三个峰丙烯酸酯基团的特性，1190，和1410厘米-1 19,21。这些峰在S50薄膜（C）的红外光谱消失，S30薄膜（D），以及IMS30膜（e）中，表示（甲基）丙烯酸酯的完全转化。此外，在1035厘米的特征峰-1为SO 3的振动-基团，SBMA出现在所有IR光谱，除了多孔载体的光谱。 图3比较了干燥S50膜的DSC结果（a）中，S30薄膜（B），和IMS30膜（C）。的DSC曲线被用来确定玻璃化转变温度（T每个样品的克）。所述的Tg值是一致的，比文献值（ 即 ，-33℃），用于与类似SBMA和PEGDA含量7膜略低。对于IMS30的DSC曲线还示出了在132℃的高密度聚乙烯，这与文献中报道的24的值的熔融峰。 水接触角在图4中给出，用来阐明的表面的亲水性。较低的接触角表明更强亲水性。所述多孔载体具有92°的接触角，这是比26°为S50膜，18°为S30膜和37°为IMS30膜的值高得多。该结果表明，在膜和含浸膜比多孔载体更亲水性的。 表格1 </强&gt;总结物理性能和S50薄膜，S30膜和IMS30膜的水输送特性，以及用于制造膜和膜预聚物溶液中的组合物。水渗透率计算，并使用数字测微计测量膜的厚度。用471微米的厚度SM50膜具有0.085 LMH /巴的水渗透率。较薄SM30膜显示出0.16 LMH /巴的水渗透性，并且IMS30膜，其厚度类似于SM30薄膜，还示出了0.15 LMH /巴的可比水渗透性。在厚度测量中示出的不确定性是多次测量的标准偏差。 <img alt="图1" src="/files/ftp_upload/55426/55426fig1.jpg" /> 图1:（a）一种自立式膜（S30，厚度= 152微米）（b）一种多孔载体，以及（c的照片）浸渍膜（IMS30）。 <a href="https://ecsource-jove-com.bdigitaluss.remotexs.co/files/ftp_upload/55426/55426fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/55426/55426fig2.jpg" /> 图2:ATR-FTIR光谱（a）的所述多孔载体的比较，（b）该预聚物溶液，（c）该S50自立式膜，（d）该S30自立式膜，和（e）的IMS30含浸膜。 <img alt="图3" src="/files/ftp_upload/55426/55426fig3.jpg" /> 图3:（a）所述S50自立式膜，（b）该S30自立式膜，和（c）的IMS30含浸膜DSC曲线。 图4: 接触角测量和水滴的图片在多孔载体上，独立电影，和浸渍膜的表面。误差棒是多次测量的标准偏差。注:悬滴法25; b。正常滴法25。 <table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always"><tbody><tr><td rowspan="2"> 样品 </td><td colspan="4"> 预聚物溶液含量（wt。％） </td><td colspan="2"> 的Tg </td><td colspan="2" rowspan="2"> 厚度（μm） </td><td colspan="2" rowspan="2"> 透水（LMH /条） </td><td colspan="2" rowspan="2"> 水渗透（厘米2 / s）的 </td></tr><tr><td> SBMA </td><td> PEGDA </td><td> H 2ö </td><td> 乙醇 </td><td colspan="2"> （C） </td></tr><tr><td> S50 </td><td> 10 </td><td> 40 </td><td> 50 </td><td> 0 </td><td colspan="2"> -37 </td><td colspan="2"> 471±3 </td><td colspan="2"> 0.085 </td><td colspan="2"> 1.5×10 -6 </td></tr><tr><td> S30 </td><td> 10 </td><td> 40 </td><td>三十</td><td> 20 </td><td colspan="2"> -38 </td><td colspan="2"> 110±7 </td><td colspan="2"> 0.16 </td><td colspan="2"> 6.6×10 -5 </td></tr><tr><td> IMS30 </td><td> 10 </td><td> 40 </td><td>三十</td><td> 20 </td><td colspan="2"> -38 </td><td colspan="2"> 94±11 </td><td colspan="2"> 0.15 b </td><td colspan="2"> 5.3×10 -5 </td></tr><tr><td colspan="13"> 水通量在45psi下测量用350rpm的搅拌速率。 </td></tr><tr><td colspan="13"> B水混合物在35psi下测量用350rpm的搅拌速率。 </td></tr></tbody></table> 表1:独立式电影和含浸膜的物理和水输运性质的总结。

Watch this Scientific Journal Video about Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification at JoVE.com

Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

This paper reports practical methods to prepare hydrogels in freestanding films and impregnated membranes and to characterize their physical properties, including water transport properties.

水凝胶的合成与防污性能作为膜的净水

Hydrogels have been widely utilized to enhance the surface hydrophilicity of membranes for water purification, increasing the antifouling properties and ...

synthesis-hydrogels-with-antifouling-properties-as-membranes-for

Universidad San Sebastian

Research

JoVE Journal

Bioengineering

9.3K 次观看.  The State University of New York at Buffalo. This paper reports practical methods to prepare hydrogels in freestanding films and impregnated membranes and to characterize their physical properties, including water transport properties. 

视频: Synthesis of Hydrogels with Antifouling Properties As Membranes for Water Purification

Electrophoretic Crystallization of Ultrathin High-performance Metal-organic Framework Membranes

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and non-porous supports (polymer, ceramic, metal, carbon, and graphene). We developed a novel crystallization technique, which is termed the ENACT approach: the electrophoretic nuclei assembly for the crystallization of highly intergrown thin films (ENACT). This approach allows for a high density of heterogeneous nucleation of MOFs on a chosen substrate via the electrophoretic deposition (EPD) directly from the precursor sol. The growth of well-packed MOF nuclei leads to a highly intergrown polycrystalline MOF film. We show that this simple approach can be used for the synthesis of thin, intergrown zeolite imidazole framework (ZIF)-7 and ZIF-8 films. The resulting 500 nm-thick ZIF-8 membranes show a considerably high H2 permeance (8.3 x 10-6 mol m-2 s-1 Pa-1) and ideal gas selectivities (7.3 for H2/CO2, 15.5 for H2/N2, 16.2 for H2/CH4, and 2655 for H2/C3H8). An attractive performance for C3H6/C3H8 separation is also achieved (a C3H6 permeance of 9.9 x 10-8 mol m-2 s-1 Pa-1 and a C3H6/C3H8 ideal selectivity of 31.6 at 25 &#176;C). Overall, the ENACT process, owing to its simplicity, can be extended to synthesize intergrown thin films of a wide range of nanoporous crystalline materials.

A simple, reproducible, and versatile approach for the synthesis of intergrown, polycrystalline metal-organic framework membranes on a wide range of unmodified porous and non-porous supports is presented.

超薄高性能金属-有机骨架膜的电泳结晶

We report the synthesis of thin, highly intergrown, polycrystalline metal-organic framework (MOF) membranes on a wide range of unmodified porous and ...

科研

化学

Fabricating Superhydrophobic Polymeric Materials for Biomedical Applications

Superhydrophobic materials, with surfaces possessing permanent or metastable non-wetted states, are of interest for a number of biomedical and industrial applications. Here we describe how electrospinning or electrospraying a polymer mixture containing a biodegradable, biocompatible aliphatic polyester (e.g., polycaprolactone and poly(lactide-co-glycolide)), as the major component, doped with a hydrophobic copolymer composed of the polyester and a stearate-modified poly(glycerol carbonate) affords a superhydrophobic biomaterial. The fabrication techniques of electrospinning or electrospraying provide the enhanced surface roughness and porosity on and within the fibers or the particles, respectively. The use of a low surface energy copolymer dopant that blends with the polyester and can be stably electrospun or electrosprayed affords these superhydrophobic materials. Important parameters such as fiber size, copolymer dopant composition and/or concentration, and their effects on wettability are discussed. This combination of polymer chemistry and process engineering affords a versatile approach to develop application-specific materials using scalable techniques, which are likely generalizable to a wider class of polymers for a variety of applications.

Two- and three-dimensional superhydrophobic polymeric materials are prepared by electrospinning or electrospraying biodegradable polymers blended with a lower surface energy polymer of similar composition.

制造超疏水高分子材料生物医学应用

Superhydrophobic materials, with surfaces possessing permanent or metastable non-wetted states, are of interest for a number of biomedical and industrial ...

生物工程

Three-Dimensionally Printed Microfluidic Cross-flow System for Ultrafiltration/Nanofiltration Membrane Performance Testing

Minimization and management of membrane fouling is a formidable challenge in diverse industrial processes and other practices that utilize membrane technology. Understanding the fouling process could lead to optimization and higher efficiency of membrane based filtration. Here we show the design and fabrication of an automated three-dimensionally (3-D) printed microfluidic cross-flow filtration system that can test up to 4 membranes in parallel. The microfluidic cells were printed using multi-material photopolymer 3-D printing technology, which used a transparent hard polymer for the microfluidic cell body and incorporated a thin rubber-like polymer layer, which prevents leakages during operation. The performance of ultrafiltration (UF), and nanofiltration (NF) membranes were tested and membrane fouling could be observed with a model foulant bovine serum albumin (BSA). Feed solutions containing BSA showed flux decline of the membrane. This protocol may be extended to measure fouling or biofouling with many other organic, inorganic or microbial containing solutions. The microfluidic design is especially advantageous for testing materials that are costly or only available in small quantities, for example polysaccharides, proteins, or lipids due to the small surface area of the membrane being tested. This modular system may also be easily expanded for high throughput testing of membranes.&#160;

Design and fabrication of a three-dimensionally (3-D) printed microfluidic cross-flow filtration system is demonstrated. The system is used to test performance and observe fouling of ultrafiltration and nanofiltration (thin film composite) membranes.

超滤/纳滤膜性能测试三维印刷微流控横流系统

Minimization and management of membrane fouling is a formidable challenge in diverse industrial processes and other practices that utilize membrane ...

Proof-of-Concept for Gas-Entrapping Membranes Derived from Water-Loving SiO2/Si/SiO2 Wafers for Green Desalination

Desalination through direct contact membrane distillation (DCMD) exploits water-repellent membranes to robustly separate counterflowing streams of hot and salty seawater from cold and pure water, thus allowing only pure water vapor to pass through. To achieve this feat, commercial DCMD membranes are derived from or coated with water-repellent perfluorocarbons such as polytetrafluoroethylene (PTFE) and polyvinylidene difluoride (PVDF). However, the use of perfluorocarbons is limiting due to their high cost, non-biodegradability, and vulnerability to harsh operational conditions. Unveiled here is a new class of membranes referred to as gas-entrapping membranes (GEMs) that can robustly entrap air upon immersion in water. GEMs achieve this function by their microstructure rather than their chemical make-up. This work demonstrates a proof-of-concept for GEMs using intrinsically wetting SiO2/Si/SiO2 wafers as the model system; the contact angle of water on SiO2 is &#952;o &#8776; 40&#176;. Silica-GEMs had 300 &#956;m-long cylindrical pores whose diameters at the (2 &#956;m-long) inlet and outlet regions were significantly smaller; this geometrically discontinuous structure, with 90&#176; turns at the inlets and outlets, is known as the &#34;reentrant microtexture&#34;. The microfabrication protocol for silica-GEMs entails designing, photolithography, chrome sputtering, and isotropic and anisotropic etching. Despite the water loving nature of silica, water does not intrude silica-GEMs on submersion. In fact, they robustly entrap air underwater and keep it intact even after six weeks (&#62;106 seconds). On the other hand, silica membranes with simple cylindrical pores spontaneously imbibe water (&#60; 1 s). These findings highlight the potential of the GEMs architecture for separation processes. While the choice of SiO2/Si/SiO2 wafers for GEMs is limited to demonstrating the proof-of-concept, it is expected that the protocols and concepts presented here will advance the rational design of scalable GEMs using inexpensive common materials for desalination and beyond.

Proof-of-Concept for Gas-Entrapping Membranes Derived from Water-Loving SiO2/Si/SiO2 Wafers for Green Desalination

Presented here is a stepwise protocol for realizing gas-entrapping membranes (GEMs) from SiO2/Si wafers using integrated circuit microfabrication technology. When silica-GEMs are immersed in water, the intrusion of water is prevented, despite the water-loving composition of silica.

气体夹膜的概念验证，源自爱水的SiO 2/Si/SiO2晶圆，用于绿色海水淡化

Desalination through direct contact membrane distillation (DCMD) exploits water-repellent membranes to robustly separate counterflowing streams of hot and ...

工程学

Fabricating Degradable Thermoresponsive Hydrogels on Multiple Length Scales via Reactive Extrusion, Microfluidics, Self-assembly, and Electrospinning

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), their ultimate clinical use has been hampered by the lack of biologically-relevant degradation observed for most smart materials. This is particularly true for temperature-responsive hydrogels, which are almost uniformly based on polymers that are functionally non-degradable (e.g., poly(N-isopropylacrylamide) (PNIPAM) or poly(oligoethylene glycol methacrylate) (POEGMA)). As such, to effectively translate the potential of thermoresponsive hydrogels to the challenges of remote-controlled or metabolism-regulated drug delivery, cell scaffolds with tunable cell-material interactions, theranostic materials with the potential for both imaging and drug delivery, and other such applications, a method is required to render the hydrogels (if not fully degradable) at least capable of renal clearance following the required lifetime of the material. To that end, this protocol describes the preparation of hydrolytically-degradable hydrazone-crosslinked hydrogels on multiple length scales based on the reaction between hydrazide and aldehyde-functionalized PNIPAM or POEGMA oligomers with molecular weights below the renal filtration limit. Specifically, methods to fabricate degradable thermoresponsive bulk hydrogels (using a double barrel syringe technique), hydrogel particles (on both the microscale through the use of a microfluidics platform facilitating simultaneous mixing and emulsification of the precursor polymers and the nanoscale through the use of a thermally-driven self-assembly and cross-linking method), and hydrogel nanofibers (using a reactive electrospinning strategy) are described. In each case, hydrogels with temperature-responsive properties similar to those achieved via conventional free radical cross-linking processes can be achieved, but the hydrazone cross-linked network can be degraded over time to re-form the oligomeric precursor polymers and enable clearance. As such, we anticipate these methods (which may be generically applied to any synthetic water-soluble polymer, not just smart materials) will enable easier translation of synthetic smart materials to clinical applications.

Protocols are described for the fabrication of degradable thermoresponsive hydrogels based on hydrazone cross-linking of polymeric oligomers on the bulk scale, microscale, and nanoscale, the latter for preparation of both gel nanoparticles and nanofibers.

通过反应挤出、微流体、自组装和电纺丝制备多长尺度可降解 Thermoresponsive 水凝胶

While various smart materials have been explored for a variety of biomedical applications (e.g., drug delivery, tissue engineering, bioimaging, etc.), ...

Ultrathin Porated Elastic Hydrogels As a Biomimetic Basement Membrane for Dual Cell Culture

The basement membrane is a critical component of cellular bilayers that can vary in stiffness, composition, architecture, and porosity. In vitro studies of endothelial-epithelial bilayers have traditionally relied on permeable support models that enable bilayer culture, but permeable supports are limited in their ability to replicate the diversity of human basement membranes. In contrast, hydrogel models that require chemical synthesis are highly tunable and allow for modifications of both the material stiffness and the biochemical composition via incorporation of biomimetic peptides or proteins. However, traditional hydrogel models are limited in functionality because they lack pores for cell-cell contacts and functional in vitro migration studies. Additionally, due to the thickness of traditional hydrogels, incorporation of pores that span the entire thickness of hydrogels has been challenging. In the present study, we use poly-(ethylene-glycol) (PEG) hydrogels and a novel zinc oxide templating method to address the previous shortcomings of biomimetic hydrogels. As a result, we present an ultrathin, basement membrane-like hydrogel that permits the culture of confluent cellular bilayers on a customizable scaffold with variable pore architectures, mechanical properties, and biochemical composition.

Current bilayer culture models do not allow for functional in vitro studies that mimic in vivo microenvironments. Using polyethylene glycol and a zinc oxide templating method, this protocol describes the development of an ultrathin biomimetic basement membrane with tunable stiffness, porosity, and biochemical composition that closely mimics in vivo extracellular matrices.

超薄 Porated 弹性水凝胶作为双细胞培养的仿生基底膜

The basement membrane is a critical component of cellular bilayers that can vary in stiffness, composition, architecture, and porosity. In vitro studies ...

An Additive Manufacturing Technique for the Facile and Rapid Fabrication of Hydrogel-based Micromachines with Magnetically Responsive Components

Polyethylene glycol (PEG)-based hydrogels are biocompatible hydrogels that have been approved for use in humans by the FDA. Typical PEG-based hydrogels have simple monolithic architectures and often function as scaffolding materials for tissue engineering applications. More sophisticated structures typically take a long time to fabricate and do not contain moving components. This protocol describes a photolithography method that allows for facile and rapid microfabrication of PEG structures and devices. This strategy involves an in-house developed fabrication stage that allows for the rapid fabrication of 3D structures by building upwards in a layer-by-layer fashion. Independent moving components can also be aligned and assembled onto support structures to form integrated devices. These independent components are doped with superparamagnetic iron oxide nanoparticles that are sensitive to magnetic actuation. In this manner, the fabricated devices can be actuated using external magnets to yield movement of the components within. Hence, this technique allows for the fabrication of sophisticated MEMS-like devices (micromachines) that are composed entirely out of a biocompatible hydrogel, able to function without an onboard power source, and respond to a contact-less method of actuation. This manuscript describes the fabrication of both the fabrication set-up as well as the step-by-step method for the microfabrication of these hydrogels-based MEMS-like devices.

An additive manufacturing strategy for processing UV-crosslinkable hydrogels has been developed. This strategy allows for the layer-by-layer assembly of microfabricated hydrogel structures as well as the assembly of independent components, yielding integrated devices containing moving components that are responsive to magnetic actuation.

一种简便快速制备磁响应元件的水凝胶基微型机械的添加剂制造技术

Polyethylene glycol (PEG)-based hydrogels are biocompatible hydrogels that have been approved for use in humans by the FDA. Typical PEG-based hydrogels ...

Photodegradable Hydrogel Interfaces for Bacteria Screening, Selection, and Isolation

Biologists have long attempted to understand the relationship between phenotype and genotype. To better understand this connection, it is crucial to develop practical technologies that couple microscopic cell screening with cell isolation at high purity for downstream genetic analysis. Here, the use of photodegradable poly(ethylene glycol) hydrogels for screening and isolation of bacteria with unique growth phenotypes from heterogeneous cell populations is described. The method relies on encapsulating or entrapping cells with the hydrogel, followed by culture, microscopic screening, then use of a high-resolution light patterning tool for spatiotemporal control of hydrogel degradation and release of selected cells into a solution for retrieval. Applying different light patterns allows for control over the morphology of the extracted cell, and patterns such as rings or crosses can be used to retrieve cells with minimal direct UV light exposure to mitigate DNA damage to the isolates. Moreover, the light patterning tool delivers an adjustable light dose to achieve various degradation and cell release rates. It allows for degradation at high resolution, enabling cell retrieval with micron-scale spatial precision. Here, the use of this material to screen and retrieve bacteria from both bulk hydrogels and microfabricated lab-on-a-chip devices is demonstrated. The method is inexpensive, simple, and can be used for common and emerging applications in microbiology, including isolation of bacterial strains with rare growth profiles from mutant libraries and isolation of bacterial consortia with emergent phenotypes for genomic characterizations.

The use of photodegradable hydrogels to isolate bacterial cells by utilizing a high-resolution light pattering tool is reported. Essential experimental procedures, results, and advantages of the process are reviewed. The method enables rapid and inexpensive isolation of targeted bacteria showing rare or unique functions from heterogeneous communities or populations.

用于细菌筛选、选择和分离的可光降解水凝胶接口

Biologists have long attempted to understand the relationship between phenotype and genotype. To better understand this connection, it is crucial to ...

Synthesis of Strong Adhesive Hydrogel, Gelatin O-Nitrosobenzaldehyde

Adhesive materials have become popular biomaterials in the field of biomedical and tissue engineering. In our previous work, we presented a new material - gelatin o-nitrosobenzaldehyde (gelatin-NB) - which is mainly used for tissue regeneration and has been validated in animal models of corneal injury and inflammatory bowel disease. This is a novel hydrogel formed by modifying biological gelatin with o-nitrosobenzaldehyde (NB). Gelatin-NB was synthesized by activating the carboxyl group of NB-COOH and reacting with gelatin through 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) and N-hydroxysuccinimide (NHS). The obtained compound was purified to generate the final product, which can be stably stored for at least 18 months. NB has a strong adhesion to -NH2 on the tissue, which can form many C = N bonds, thus increasing the adhesion of gelatin-NB to the tissue interface. The preparation process comprises steps for the synthesis of the NB-COOH group, modification of the group, synthesis of gelatin-NB, and purification of the compound. The goal is to describe the specific synthesis process of gelatin-NB in detail and to demonstrate the application of gelatin-NB to damage repair. Moreover, the protocol is presented to further strengthen and expand the nature of the material produced by the scientific community for more applicable scenarios.

The protocol presented here shows the synthesis of a strong adhesive hydrogel gelatin o-nitrosobenzaldehyde (gelatin-NB). Gelatin-NB has rapid and efficient tissue adhesion ability, which can form a strong physical barrier to protect wound surfaces, so it is expected to be applied to the field of injury repair biotechnology.

强粘性水凝胶明胶O-亚硝基苯甲醛的合成

Adhesive materials have become popular biomaterials in the field of biomedical and tissue engineering. In our previous work, we presented a new material - ...

将 CFPS 反应包埋在各种水凝胶基质中

Methods for Embedding Cell-Free Protein Synthesis Reactions in Macro-Scale Hydrogels

Synthetic gene networks provide a platform for scientists and engineers to design and build novel systems with functionality encoded at a genetic level. While the dominant paradigm for the deployment of gene networks is within a cellular chassis, synthetic gene networks may also be deployed in cell-free environments. Promising applications of cell-free gene networks include biosensors, as these devices have been demonstrated against biotic (Ebola, Zika, and SARS-CoV-2 viruses) and abiotic (heavy metals, sulfides, pesticides, and other organic contaminants) targets. Cell-free systems are typically deployed in liquid form within a reaction vessel. Being able to embed such reactions in a physical matrix, however, may facilitate their broader application in a wider set of environments. To this end, methods for embedding cell-free protein synthesis (CFPS) reactions in a variety of hydrogel matrices have been developed. One of the key properties of hydrogels conducive to this work is the high-water reconstitution capacity of hydrogel materials. Additionally, hydrogels possess physical and chemical characteristics that are functionally beneficial. Hydrogels can be freeze-dried for storage and rehydrated for use later. Two step-by-step protocols for the inclusion and assay of CFPS reactions in hydrogels are presented. First, a CFPS system can be incorporated into a hydrogel via rehydration with a cell lysate. The system within the hydrogel can then be induced or expressed constitutively for complete protein expression through the hydrogel. Second, cell lysate can be introduced to a hydrogel at the point of polymerization, and the entire system can be freeze-dried and rehydrated at a later point with an aqueous solution containing the inducer for the expression system encoded within the hydrogel. These methods have the potential to allow for cell-free gene networks that confer sensory capabilities to hydrogel materials, with the potential for deployment beyond the laboratory.

作者聚焦:一种在水凝胶中包埋无细胞蛋白质合成反应的新方法 

Here, we present two protocols for embedding cell-free protein synthesis reactions in macro-scale hydrogel matrices without the need for an external liquid phase.

在宏观水凝胶中包埋无细胞蛋白质合成反应的方法

Synthetic gene networks provide a platform for scientists and engineers to design and build novel systems with functionality encoded at a genetic level. ...