环氧衍生物开环法制备壳聚糖季铵盐的工艺研究

采用异丙醇为溶剂,以壳聚糖(CTS)、2,3-环氧丙基三甲基氯化铵(GTA)为原料,用环氧衍生物开环法制备了壳聚糖季铵盐(HACC).通过单因素实验,研究了反应物摩尔比、反应时间、反应温度等因素对产物取代度的影响.结果表明,制备壳聚糖季铵盐的最优工艺为:ncrs∶nGrA =1∶4,反应时间8h,反应温度75℃,反应pH值为7,碱化时间14h,壳聚糖分子量3.2×105,反应体系含水率20％.通过红外光谱、扫描电镜、热重仅对壳聚糖、壳聚糖季铵盐的结构、外观形貌以及热稳定性进行了表征与分析,结果表明壳聚糖季铵化改性以N-取代为主,改性后外貌和粒度有了明显变化,且热稳定性降低.     

环氧衍生物开环法制备壳聚糖季铵盐

采用异丙醇为溶剂,以壳聚糖(CTS)、2,3-环氧丙基三甲基氯化铵(GTA)为原料,用环氧衍生物开环法制备了壳聚糖季铵盐(HACC),通过单因素实验,考察了反应物摩尔比、反应时间、反应温度等因素对产物取代度的影响,结果表明,制备壳聚糖季铵盐的最优工艺条件为:n(CTS):n(GTA)=1∶4,壳聚糖相对分子质量(简称分子量,下同)3.2×105,碱化时间14h,预处理壳聚糖含水率20％,反应pH =7,反应温度75℃,反应时间8h.通过红外光谱、扫描电镜、热重分析对壳聚糖、壳聚糖季铵盐的结构、外观形貌、热稳定性进行了表征与分析,结果表明,壳聚糖季铵化改性以N取代为主,改性后外貌和粒度有了明显变化,并且热稳定性降低.     

环氧衍生物开环法制备壳聚糖季铵盐的工艺研究

采用异丙醇为溶剂,以壳聚糖(CTS)、2,3-环氧丙基三甲基氯化铵(GTA)为原料,用环氧衍生物开环法制备了壳聚糖季铵盐(HACC),通过单因素实验,考察了反应物摩尔比,反应时间,反应温度等因素对产物取代度的影响,结果表明,制备壳聚糖季铵盐的最优工艺为：nCTS: nGTA=1: 4,壳聚糖相对分子质量3.2×105,碱化时间14h,预处理壳聚糖含水率20%,反应pH值7,反应温度75℃,反应时间8h。通过红外光谱、扫描电镜、热重分析对壳聚糖、壳聚糖季铵盐的结构、外观形貌、热稳定性进行了表征与分析,结果表明壳聚糖季铵化改性以N取代为主,改性后外貌和粒度有了明显变化,并且热稳定性降低。     

不同取代度壳聚糖季铵盐的制备及其热稳定性研究

制备了不同取代度的壳聚糖季铵盐(羟丙基三甲基氯化铵壳聚糖),利用单因素实验分析了制备条件,采用热重分析探讨了壳聚糖季铵盐的热降解温度。结果表明,壳聚糖季铵盐的最佳制备条件为环氧丙基三甲基氯化铵(ETA)与壳聚糖的比为3,水与异丙醇的比为3,反应温度为80℃,反应体系的pH值为6.0。壳聚糖季铵盐与壳聚糖相比,热稳定性下降,随着壳聚糖季铵盐取代度的增加,初始降解温度(T0)、最大降解速率温度(Tp)和终止降解温度(Tf)均逐渐降低。同时,从初始降解温度到最大降解速率温度的时间也随着取代度的增加而减少。     

O-季铵化低聚壳聚糖芳香醛席夫碱衍生物的制备及其抑菌活性

以低聚壳聚糖为对象,苯甲醛、水杨醛、香草醛为改性试剂,设计合成了一系列O-季铵盐低聚壳聚糖芳香醛席夫碱衍生物。产物元素分析发现其席夫碱取代度接近100%,电位滴定确定产物的季铵盐接枝率在35%左右。抑菌活性研究表明,合成的各种O-季铵盐低聚壳聚糖芳香醛席夫碱衍生物抑菌活性明显增强,活性大小依次为香草醛改性物水杨醛改性物苯甲醛改性物低聚壳聚糖。抑菌活性构效关系分析表明,低聚壳聚糖通过芳香醛席夫碱改性引入了酚羟基抑菌活性中心,但酚羟基的抑菌活性受空间位阻影响较大。     

壳聚糖季铵盐改性物的制备工艺优化及产品的抑菌性

壳聚糖季铵盐(HTCC)是以壳聚糖为基本原料,将壳聚糖与2,3-环氧丙基三甲基氯化铵(GTA)发生醚化反应的产物。壳聚糖季铵化改性后,不仅提高了壳聚糖的溶解性,而且在一定程度上增加了其抑菌性。优化了制备壳聚糖季铵盐的几项基本工艺参数,确定了壳聚糖季铵盐制备的最佳工艺参数为:GTA与壳聚糖的质量比为4∶1,反应温度为70℃,反应时间为9h,p H值为7.0,产物取代度最高可达85.1%。将制备的壳聚糖季铵盐产品用于咸鸭蛋和草莓的保鲜,取得了较好的保鲜效果。     

壳聚糖季铵盐铜配合物的热降解行为研究

采用热重分析(TG)研究壳聚糖季铵盐铜配合物在30℃～600℃的温度范围内的热降解行为,探讨壳聚糖季铵盐铜配合物的热稳定性。研究结果表明:壳聚糖季铵盐铜配合物的热降解为一步反应,取代度对壳聚糖季铵盐的热降解有明显的影响,壳聚糖季铵盐铜配合物的特征降解温度都随取代度的增加而降低。     

壳聚糖季铵盐研究进展

壳聚糖是应用广泛的天然多糖,资源丰富,壳聚糖化学改性后得到的衍生物改善了壳聚糖的功能,并保留了壳聚糖本身的可生物降解性、生物相容性等优点.其中壳聚糖的季铵盐改性明显提高了其抑菌、抗氧化等活性,并增强了壳聚糖的水溶性,近年来研究较多,介绍了壳聚糖季铵盐的化学改性及应用研究进展,这些化学改性方式均在一定程度上提高了壳聚糖的...     

新型壳聚糖季铵盐抗菌剂的合成及其性能

先用两步法合成了无O-甲基化 N,N,N-三甲基壳聚糖季铵盐（TMC）,再通过相转移催化合成了N,N,N-三甲基O-辛基壳聚糖季铵盐（TMOC）,用 FTIR、1H NMR、EA、TG 等方法对产物进行表征,并研究其抗菌性能。结果表明,TMOC在pH值为5.5的抗菌活性优于pH值为7.2的抗菌活性;TMOC对革兰阳性菌S. aureus的抗菌活性比革兰阴性菌E. coli强。在不影响水溶性的前提下,O-烷基化改性能有效提高壳聚糖季铵盐的抗菌活性,并且抗菌活性随着O-烷基化度的提高而提高。研究结果为壳聚糖基抗菌剂的改性和制备提供了依据。     

海因改性N-季铵化壳聚糖衍生物的合成及其抗菌性能

在酸性条件下,以壳聚糖与环氧季铵盐为原料反应得到水溶性良好的产物N-(2-羟丙基三甲基氯化铵)壳聚糖(HTCC),再用实验室自制的环氧海因改性,得到O-羟丙基(5,5-二甲基海因)-N-(2-羟丙基三甲基氯化铵)壳聚糖衍生物(GH-HTCC),用 FTIR、¹H NMR、UV-VIS和EA 等对产物进行表征。抗菌实验结果表明,产物对两种菌种都有一定的抗菌活性,对金黄色葡萄球菌的抗菌活性优于大肠杆菌;GH-HTCC的抗菌活性优于HTCC,并随环氧海因取代度的增加而增强;低浓度的乙二胺四乙酸(EDTA)增强了HTCC和GH-HTCC的抗菌活性,而高浓度的EDTA在一定程度上抑制了二者的抗菌活性。     

Preparation of Chitosan and Water-Soluble Chitosan Microspheres via Spray-Drying Method to Lower Blood Lipids in Rats Fed with High-Fat Diets

This experiment aimed to investigate the effects of the chitosan (CTS) and water-soluble chitosan (WSC) microspheres on plasma lipids in male Sprague-Dawley rats fed with high-fat diets. CTS microspheres and WSC microspheres were prepared by the spray-drying technique. Scanning electron microscopy (SEM) micrographs showed that the microspheres were nearly spherical in shape. The mean size of CTS microspheres was 4.07 μm (varying from 1.50 to 7.21 μm) and of WSC microspheres was 2.00 μm (varying from 0.85 to 3.58 μm). The rats were classified into eight groups (n = 8) and were fed with high-fat diets for two weeks to establish the hyperlipidemic condition and were then treated with CTS microspheres and WSC microspheres, CTS and WSC for four weeks. The results showed that CTS and WSC microspheres reduced blood lipids and plasma viscosity and increased the serum superoxide dismutase (SOD) levels significantly. This study is the first report of the lipid-lowering effects of CTS and WSC microspheres. CTS and WSC microspheres were found to be more effective in improving hyperlipidemia in rats than common CTS and WSC.     

氨基硫脲壳聚糖与碘的配合物抑菌性质研究

壳聚糖(CTS)与硫氰酸铵在乙醇中反应制得氨基硫脲壳聚糖(ATU-CTS)。制备ATU-CTS和碘的配合物(ATU-CTS-I2),用红外光谱和热重分析对CTS、ATU-CTS和ATU-CTS-I2进行表征。讨论了ATU-CTS与碘配合物的抑菌性质,结果表明ATU-CTS-I2对大肠杆菌和金黄色葡萄球菌抑菌敏感度为高度敏感。     

Influence of 2-hydroxypropyltrimethyl ammonium chloride chitosan on sedimentation and volume change behavior of cohesive soil sediments

The 2-hydroxypropyltrimethyl ammonium chloride chitosan (HACC), introducing the functional quaternary ammonium group to the structure of Chitosan, has greatly broadened the application prospect. The influence on natural cohesive soil has rarely been considered. The sedimentation tests for the natural soil in HACC solutions and the HACC-treated soils in distilled water are considered to analyze the change of sedimentation behaviors in this paper. Moreover, the potential change on the surface of soil particles, the change in particle size distribution, X-ray diffraction of Ca-montmorillonite/HACC, and scanning electron microscopy images are investigated to explain the reasons for the results. Results indicate that the surface potential of soil particles achieved reversal, and the particle size had significant agglomeration. The adsorption of HACC results in the rapid sedimentation of the treated soils in water. HACC has a significant influence on setting time and final volume. HACC cannot inhibit the interlayer swelling of Ca-montmorillonite. The dehydration process can promote the aggregation effect of the treated soils. The specific effects provided an essential train of thought to solve soil problems.     

羟丙基三甲基氯化铵壳聚糖在化妆品中的应用研究

用2，3-环氧丙基三甲基氯化铵对壳聚糖进行改性，采用不同反应条件制备了一系列不同取代度的羟丙基三甲基氯化铵壳聚糖（HACC），通过红外光谱，核磁共振光谱对结构进行表征，IR谱图证实以N上取代为主。研究了产物的取代度，吸湿与保湿性、抗菌性，pH稳定性，与表面活性剂的配伍性。     

降解壳聚糖与水杨醛改性衍生物对Ca~(2+)、Fe~(3+)的螯合性质

过氧化氢对壳聚糖氧化降解反应适宜条件为:温度70～80℃;pH=4～7;w(H2O2)=5%。对降解产物(CTS′)与水杨醛进行化学改性得相应衍生物S CTS′(H)、S CTS′(Na)和还原产物RS CTS′(H)、RS CTS′(Na)。在pH=10～11的水溶液中对Ca2+的螯合(吸附)能力为RS CTS′(Na)∽S CTS′(Na)>RS CTS′(H)∽S CTS′(H)。同时给出S CTS′(H)在c(HCl)=0 10mol/L的介质中对Fe3+螯合的UV吸收光谱。     

Study on superabsorbent composites. XXI. Synthesis,characterization and swelling behaviors of chitosan‐g‐poly(acrylic acid)/organo‐rectorite nanocomposite superabsorbents

A novel chitosan‐g‐poly(acrylic acid)/organo‐rectorite (CTS‐g‐PAA/OREC) nanocomposite superabsorbent was synthesized by aqueous polymerization using N, N′‐methylenebisacrylamide as a crosslinker and ammonium persulfate as an initiator. Rectorite was organified with four different degree of hexadecyltrimethyl ammonium bromide, and the organification of rectorite was proved by FTIR and XRD. The effect of organification degree of rectorite on water absorbency of CTS‐g‐PAA/OREC with different organo‐rectorite content was investigated. The swelling behaviors in distilled water and various pH solutions were also studied. The results from IR spectroscopy and XRD data show that acrylic acid had been grafted polymerization with chitosan and organo‐rectorite and formed nanocomposite. Introducing organo‐rectorite into the CTS‐g‐PAA polymeric network can improved water absorbency and swelling rate of CTS‐g‐PAA/OREC. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Mechanical properties and drug release of microcapsules containing quaternized‐chitosan‐modified reduced graphene oxide in the capsular wall

Reduced graphene oxide (rGO) sheets were first modified with 2‐hydroxypropyltrimethyl ammonium chloride chitosan (HACC), and these modified rGO sheets (named HACC–rGO) were used as reinforcement materials and introduced to the walls of chitosan (CS) microcapsules. All of the monodisperse microcapsules were conveniently generated by a gas–liquid microfluidic technique. The results of scanning electron microscopy, X‐ray diffraction, and thermogravimetric analysis all demonstrate that the HACC–rGO sheets existed and were dispersed in the capsular shell. The HACC–rGO‐reinforced CS microcapsules showed better mechanical strength and better chemical stability with an α‐cyclodextrin solution than the CS microcapsules without HACC–rGO. Importantly, the HACC–rGO‐reinforced CS microcapsules exhibited a slower drug‐release behavior and provide a method for the control of the release rate of drug‐loaded microcapsules. In an in vitro cytotoxicity evaluation by a 3‐(4,5‐dimethyl‐2‐thiazolyl)‐2,5‐diphenyl‐2‐H‐tetrazolium bromide assay, the Schwann cells still showed good cell viability after they were treated by extracts of the CS/HACC–rGO microcapsules with concentrations ranging from 0.02 to 2000 μg/mL. Therefore, the HACC–rGO‐reinforced CS microcapsules are promising for applications in the fields of drug delivery and controlled release. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44549.     

Synthesis and characterization of grafting β‐cyclodextrin with chitosan

Two new adsorbents [β‐cyclodextrin–chitosan (β‐CD–CTS) and β‐cyclodextrin‐6–chitosan (β‐CD‐6‐CTS)] were synthesized by the reaction of β‐cyclodextrin (β‐CD) with epoxy‐activated chitosan (CTS) and the sulfonation of the C‐6 hydroxyl group of β‐cyclodextrin with CTS, respectively. Their structures were confirmed by IR spectral analysis and X‐ray diffraction analysis, and their apparent amount of grafting was determined by ultraviolet spectroscopy. The adsorption properties of β‐CD‐CTS and β‐CD‐6‐CTS for p‐dihydroxybenzene were studied. The experimental results showed that the two new adsorbents exerted adsorption on the carefully chosen target. The highest saturated capacity of p‐dihydroxybenzene of β‐CD‐CTS and β‐CD‐6‐CTS were 51.68 and 46.41 mg/g, respectively. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 94: 860–864, 2004     

琥珀酰壳聚糖季铵盐的合成及絮凝性能

壳聚糖由于水溶性差、电荷密度低等缺点,使其在絮凝应用方面受到限制。对壳聚糖进行化学改性,可以改善其水溶性和絮凝性能。本文采用苯甲醛保护壳聚糖氨基,然后与丁二酸酐反应合成琥珀酰壳聚糖（SACTS）,进一步与二甲基二烯丙基氯化铵（DMDAAC）反应合成琥珀酰壳聚糖季铵盐（SAQCS）。采用FTIR、¹H NMR、XRD、ESEM等方法对SAQCS的结构和形貌进行表征。探讨了引发剂用量、单体配比、反应温度、反应时间对SAQCS阳离子度的影响。结果表明,SAQCS较优合成工艺条件为：引发剂用量（占单体的质量分数） 2%,m（DMDAAC）/m（SACTS）=5.4,反应温度70℃,反应时间7h。此工艺条件下合成的SAQCS的阳离子度为42.26%。将SAQCS、壳聚糖、聚丙烯酰胺与配制的高岭土模拟废水进行絮凝实验,考察了pH、投加量、温度对絮凝效果的影响。结果表明,当絮凝条件为pH=2～5、投加量3~9mg/L、温度25～50℃范围内,使用SAQCS絮凝后上清液浊度去除率均在96%以上。