ATRP法接枝卤胺分子制备纤维素共聚物抗菌材料

以氯化1-烯丙基-3-甲基咪唑([AMIM]Cl)离子液体为溶剂,采用原子转移自由基聚合法(ATRP)在微晶纤维素上接枝功能单体N-羟甲基丙烯酰胺,制备了卤胺化合物中间体,应用卤化法将接枝共聚物中的N—H转化为N—Cl键获得具有抗菌性的共聚物材料,并对其抗菌性能进行研究。通过FT-IR、1H NMR、SEM以及抗菌测试等分析手段表征分析了聚合物的结构、表面形貌和抗菌性能等。结果表明该工艺合成了纤维素接枝N-羟甲基丙烯酰胺共聚物,接枝后表面明显变得粗糙,有利于材料与细菌的接触进而充分发挥其抗菌性能,制备的材料对金黄色葡萄球菌和大肠杆菌均表现出良好抗菌性能,在抗菌材料领域具有较好的应用前景。     

ATRP法均相制备纤维素/甲基丙烯酸丁酯接枝聚合物

在纤维素LiCl/DMAc均相溶液中,通过氯乙酰氯(ClC2OCl)与纤维素的均相酰化反应制得纤维素氯乙酸酯(Cellulose-ClAc)后,将其溶解在DMAc中,在FeCl2/4-二甲氨基吡啶(DMAP)的催化作用下,引发甲基丙烯酸丁酯(BMA)的均相ATRP聚合反应,制备了纤维素/BMA接枝共聚物(Cellulose-g-PBMA),考察了反应时间、反应温度、反应物配比等对酰化及接枝聚合反应的影响,并通过测试Cellulose-g-PBMA薄膜的接触角,对最终产物的疏水性能进行了研究;采用FTIR、NMR、SEM、TEM、AFM等分析手段对Cellulose-ClAc及Cellulose-g-PBMA的结构进行了表征;利用GPC分析了接枝聚合反应的活性特征。     

ATRP法均相制备纤维素/甲基丙烯酸丁酯接枝聚合物

在纤维素LiCl/DMAc均相溶液中,通过氯乙酰氯（ClC₂OCl）与纤维素的均相酰化反应制得纤维素氯乙酸酯（Cellulose-ClAc）后,将其溶解在DMAc中,在FeCl₂/4-二甲氨基吡啶（DMAP）的催化作用下,引发甲基丙烯酸丁酯（BMA）的均相ATRP 聚合反应,制备了纤维素/BMA接枝共聚物（Cellulose-g-PBMA）,考察了反应时间、反应温度、反应物配比等对酰化及接枝聚合反应的影响,并通过测试Cellulose-g-PBMA薄膜的接触角,对最终产物的疏水性能进行了研究;采用FTIR、NMR、SEM、TEM、AFM等分析手段对Cellulose-ClAc及Cellulose-g-PBMA的结构进行了表征;利用GPC分析了接枝聚合反应的活性特征。     

离子液体中采用AGET ATRP法制备MCC-g-PGMA

在氯化1-烯丙基-3-甲基咪唑([AMIM]Cl)离子液体中, 采用AGET ATRP技术, 以VC为还原剂、CuBr₂/乙二胺为催化体系, 成功制备了微晶纤维素接枝聚甲基丙烯酸缩水甘油酯(MCC-g-PGMA)分子。研究表明:[AMIM]Cl对微晶纤维素有较好的溶解性, 最佳反应条件为GMA/乙二胺/CuBr₂/VC摩尔比为100:4:1:1, 反应温度25℃, 反应时间4 h, 接枝效率可达54.56%, 分子量分布较窄为1.48。通过FT-IR、TEM和SEM测试表明:成功合成了MCC-g-PGMA接枝共聚物分子, PGMA接枝微晶纤维素后表面形态变得粗糙, 接枝共聚物在丙酮溶液中可自组装成150～200 nm的球形结构, 在药物载体领域具有良好的应用潜能。     

[AMIM]Cl离子液体中纤维素接枝PDEAEMA分子刷的均相可控聚合

在氯化1-烯丙基-3-甲基咪唑([AMIM]Cl)离子液体中,采用原子转移自由基(ATRP) 法接枝改性微晶纤维素,合成了微晶纤维素-g-甲基丙烯酸二乙氨基乙酯(MCC-g-PDEAEMA)聚合物分子刷。通过加入助溶剂形成均相反应体系,解决了功能性单体甲基丙烯酸二乙氨基乙酯(DEAEMA)在[AMIM]Cl离子液体中的溶解问题。分别研究了离子液体中均相与非均相的反应机理,结果表明:在均相体系中,生成的反应副产物PDEAEMA较少,聚合物分子刷的接枝效率较高,分子量分布窄,ATRP反应可控性好。实验确定了均相体系最佳反应条件:CuBr/PMDETA/DEAEMA/乙醇的摩尔比为1:15:150:300, MCC-g-PDEAEMA的接枝效率可达78.1%。通过红外、核磁和GPC对聚合物表征发现,侧链PDEAEMA成功地接枝到微晶纤维素骨架上,生成的聚合物分子刷的分子量分布均匀。     

ATRP法制备PVDF-g-PS共聚物及其表征

采用ATRP法制备了聚偏氟乙烯(PVDF)接枝苯乙烯共聚物(PVDF-g-PS),对产物的结构与性能进行了表征。结果表明:随着接枝率的提高,接枝共聚物的熔点和熔融焓下降,且PVDF在接枝后表面由光滑转变为凹凸不平的形貌。     

纤维素与MBA接枝共聚物在离子液体中的制备

以N,N’-亚甲基双丙烯酰胺(MBA)为单体,过硫酸钾为引发剂,研究了MBA与纤维素在离子液体中的接枝共聚反应。通过正交单因素实验,研究了反应时间、单体用量、反应温度、引发剂用量对接枝效果的影响。实验结果表明:当反应时间为2 h,单体与纤维素质量比为3∶1,反应温度为50℃,引发剂用量为0.05 g时,接枝效果最好。此条件下,MBA与纤维素的接枝率可达38.06%。     

纤维素均相接枝丙烯酸球形吸附剂的制备与性能

以离子液体1-烯丙基-3-甲基氯代咪唑（[AMIM] CI）为反应介质,采用丙烯酸为单体,过硫酸铵为引发剂,N,N＇-亚甲基双丙烯酰胺为交联剂,利用接枝共聚方法合成纤维素-丙烯酸接枝共聚物.以轻液体石蜡为分散相,经反相悬浮过程将接枝物球化.通过正交实验法探索了最佳合成条件：单体的用量为4g/g CE,引发剂的用量为0.15g/g CE,交联剂的用量为0.05g/g CE,反应温度为60℃,反应时间为1.5h.采用傅里叶变换红外光谱（FT-IR）、透射电子显微镜（TEM）、热重分析仪对纤维素-丙烯酸接枝共聚物进行了表征.结果表明,聚合物微球对Cu＋2离子有较好的吸附效果,最佳吸附量为198.6 mg/g.     

离子液体溶剂法制备再生纤维素纤维

离子液体是纤维素的有效溶剂,可以实现快速溶解。以离子液体生产的再生纤维素纤维较多地保留了纤维素的天然特性,易于生物降解,产品性能优于传统的粘胶工艺。介绍了离子液体的物性、作为纤维素溶剂的优点、对纤维素的溶解机理、纺丝原液制备及纺丝工艺。     

纤维素接枝反应的研究进展

纤维素是世界上最丰富的天然可再生资源。离子液体是一种新型的绿色溶剂,在纤维素的均相接枝研究中正起着越来越重要的作用。文章介绍了纤维素接枝反应尤其是均相接枝反应的研究进展。     

Preparation and characterization of quaternary bacterial cellulose composites for antimicrobial oil-absorbing materials

The treatment of various types of oily wastewater is paramount for environmental protection. Bacterial cellulose (BC) stands out as a highly promising material for oil/water separation, owing to its exceptional mechanical properties and three-dimensional porous structures. However, excessive hydroxyl groups on BC make it highly hydrophilic, reducing oil absorption and promoting bacterial growth, affecting its stability. To address these challenges, we developed a straightforward in situ polymerization method for the preparation of BC-DMC composites. The innovation lies in the concurrent enhancement of BC's hydrophobicity and antimicrobial properties only through the addition of 2-(Methacryloyloxy)ethyltrimethylammonium chloride (DMC), considerably simplifying the synthesis of materials possessing oil-absorbing and antimicrobial properties. Morphological and structural characterization results confirmed the successful combination of DMC onto BC while maintaining its porous structure. After process parameter optimization, the BC-DMC composites exhibited a remarkable increase in contact angle (117.7° compared with pure BC's 19.5°). It also demonstrated excellent oil absorption performance, with maximum capacities exceeding 30 g/g for different oils, maintaining values above 20 g/g even after eight cycles. In addition, the BC-DMC composites exhibited strong antibacterial activity, with rates of 82.4% against Escherichia coli and 97.5% against Staphylococcus aureus. The antibacterial mechanism of the BC-DMC composites was also discussed. Our novel BC-DMC composites provides excellent oil absorption and antibacterial properties, making it highly applicable in the field of oily wastewater treatment and serving as a valuable reference for other researchers.     

离子液体法制备再生细菌纤维素纤维

以离子液体(氯化1-甲基-3-正丁基咪唑)溶解高聚合度细菌纤维素(BC),采用湿法纺丝制备再生细菌纤维素(RBC)初生纤维;通过红外光谱分析(FTIR)、广角X射线衍射(WAXD)分析、热失重(TG)分析、扫描电镜( SEM)、单丝强度拉伸等表征了RBC初生纤维的结构和性能.结果表明:该溶剂体系通过10 h的快速搅拌溶...     

Preparation of antibacterial cellulose with s‐triazine‐based quaternarized N‐halamine

To reduce the neutral salt used in the textile finishing with s‐triazine derivatives, a novel s‐triazine‐based quaternarized N‐halamine precursor was synthesized by two simple steps and characterized by H‐NMR and FT‐IR. This compound can be effectively coated onto cellulose by nucleophilic substitution process without neutral salt. The treated cellulose was rendered with powerful biocidal efficacy after transferring to an N‐halamine structure by exposing to dilute sodium hypochlorite solution through the synergistic antimicrobial effect quaternary ammonium salt and N‐halamine. The chlorinated samples could inactivate 6‐logs of Staphylococcus aureus and Escherichia coli O157:H7 within 1 min and 5 min, respectively. In addition, about 50% of oxidant chlorine remained after 50 washing cycles and 30 days storage, and all of the lost active chlorines in the N‐halamine molecules recovered after exposing to bleach solution. With these advantages, the as‐prepared antimicrobial fabrics will have potential application, especially in the medical and healthcare textiles. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44998.     

季铵盐型抗菌纤维素纤维的辐射接枝聚合

固相表面接触抗菌材料应用于水的表面接触消毒是一项新的水处理技术,提高材料表面抗菌基团含量将有利于抗菌性能的提高。本研究采用直接辐射接枝和预辐射接枝两种方法,在纤维素纤维表面引入具有抗菌功能的季铵盐聚合物,详细探讨了两种辐射接枝聚合技术以及温度、时间、单体浓度、辐射剂量等具体辐射接枝聚合工艺参数对接枝聚合反应的影响。利用红外光谱（FTIR）、扫描电子显微镜（SEM）对接枝纤维素纤维进行了表征。结果表明,采用预辐射接枝技术可制得接枝率55%以上的高接枝率抗菌纤维素纤维。     

Preparation,characterization, and antibacterial activities of quaternarized N‐halamine‐grafted cellulose fibers

A viable method for coating of cellulose fiber with quaternarized N‐halamine is reported in this article. The use of quaternary ammonium salt group in combination with N‐halamine group can reinforce the antibacterial activity. The chemical structure of as‐synthesized N‐halamine precursor 4‐(Bromo‐acetic acid methylester)‐4‐ethyl‐2‐ oxazolidinone (BEO) was characterized by ¹H‐NMR. The cellulose fibers were characterized by Fourier transform infrared spectra and X‐ray photoelectron spectra. The spectra data confirmed that the quaternarized N‐halamine‐grafted cellulose fibers were successfully obtained. The antibacterial properties of functional fibers were challenged with both Gram positive and Gram negative bacteria. The antibacterial tests and showed that the as‐prepared antibacterial cellulose fibers exhibited powerful and rapid bactericidal performance against both Gram negative E. coli and Gram positive S. aureus. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42702.     

离子液体中天然纤维素的溶解研究进展

纤维素是广泛存在的自然资源,普遍应用于石油、医药、电子等行业。但是由于纤维素的本身化学性质使其难以加工。传统的黏胶法与铜氨法由于其生产条件严苛,污染环境,已经不再适合新时代对于绿色化学的要求。近年来,绿色高效的离子液体得到研究开发,为纤维素的发展提供一个新的平台。本文综述了当前纤维素的几种溶解体系及其概况,探讨了各个体系优缺点,并着重介绍了近年来离子液体的研究进展,提出了今后离子液体应用于纤维素的几个方向,以期为今后纤维素溶解及开发更多纤维素材料提供参考。