不同脱乙酰度壳聚糖的制备及其聚集行为研究

壳聚糖的脱乙酰度直接影响壳聚糖的物理化学和生物特性。在乙酸-水-甲醇体系中研究壳聚糖的乙酰化反应工艺,考察了反应时间、壳聚糖质量浓度对乙酰化反应的影响,优化了反应条件。研究表明,反应时间为6h时,壳聚糖乙酰化反应基本完全,乙酰化反应后,相对重均分子质量基本不变,壳聚糖相对分子质量分布变宽。在优化后的反应条件下,改变乙酸酐加入量分别制备了脱乙酰度为76%,64%和54%的不同脱乙酰度的壳聚糖。芘荧光光谱研究表明,壳聚糖的临界聚集浓度(CSC)随脱乙酰度的降低而增加。     

不脱蛋白质壳聚糖制备工艺

采用D -近似最优设计法系统地研究了NaOH质量分数、碱处理时间及碱处理温度这三个主要因素对制备壳聚糖的影响 :当碱液质量分数增加时 ,壳聚糖的脱乙酰度增加 ,但其速度却在减小 ,当碱液质量分数达到 40 %时 ,脱乙酰度出现峰值 ,约为 90 % ,而后增加碱液质量分数时 ,脱乙酰度反而下降 ;随着反应温度的升高 ,其脱乙酰度几乎线性递增 ,当温度达到 2 0 0℃附近时 ,曲线趋于平直并且脱乙酰度达到最大 ;随着反应时间的增加 ,脱乙酰度开始呈线性增加 ,当反应时间超过 5 0min后 ,脱乙酰度有下降趋势 ;在一定碱液质量分数 (4 0 % )条件下 ,脱乙酰度随着温度的增加而增加 ,因此 ,若需获得较高质量的壳聚糖 ,必须提高反应温度     

止血性壳聚糖的制备及其凝血效果的研究

在温和均相条件下,对较高脱乙酰度的壳聚糖进行乙酰化,制备不同脱乙酰度的壳聚糖;测试不同脱乙酰度和分子量的壳聚糖醋酸溶液的凝血效果。中药—壳聚糖复合止血材料的制备及其止血功能的研究。     

壳聚糖制备工艺研究

为了制备不同脱乙酰度的壳聚糖,采用正交试验方法进行实验设计,考查了醇浓度、碱浓度、物料比和反应时间在不同水平下对脱乙酰度的影响。通过SAS计算机软件进行数据处理,回归得到方程E=3.18A-3.78B＋21.42C-0.036A^2＋0.089B^2-1.71C^2-0.59D^2,具有高度统计显著性,可为工业化生产制备不同脱乙酰度的壳聚糖提供工艺指导。     

紫外测定壳聚糖脱乙酰度方法的探讨

分别采用直接、一阶导数、多波长和双内标等4种紫外分光光度法测定壳聚糖的脱乙酰度,评价4种紫外测定方法,并与胶体滴定、电位滴定和氢核磁3种测定方法进行了比较。结果表明,采取上述紫外法测定壳聚糖脱乙酰度值均高于胶体滴定和氢核磁测定值。故准确测定高脱乙酰度壳聚糖的脱乙酰度,紫外法非首选方法。     

壳聚糖在醋酸溶液中的溶解行为及动力学模型

用电导和粒度测试两种方法研究了壳聚糖在醋酸溶液中的溶解行为。结果显示:醋酸浓度、溶解温度和壳聚糖样品本身的脱乙酰度及分子量都会影响壳聚糖的溶解,但溶解初期壳聚糖因吸附醋酸根离子而产生聚集现象。一般情况下,温度高有利于壳聚糖的溶解。当壳聚糖脱乙酰度非常高,分子量差距又并不是非常大时,前者将对溶解起主导作用,同时脱乙酰度越高越有利于其溶解。     

醇溶剂法制备高脱乙酰度壳聚糖

采用戊醇-氢氧化钠反应体系,通过对投料比、反应温度、反应时间等影响因素研究了甲壳素的脱乙酰反应,结果表明在四流温度．反应时间1．5h,壳聚糖：NaOH：醇=1：5：11(质量比)条件下制得脱乙酰度为99．7％的壳聚糖,而传统水溶剂脱乙酰度小于50％。     

高脱乙酰度壳聚糖的制备

以甲壳素为原料,以异丁醇为溶剂,氢氧化钠为亲核试剂,探讨了一种制备高脱乙酰度壳聚糖的新方法.研究了投料比、反应温度、反应时间、反应方法等对脱乙酰度的影响.结果表明,在反应温度为110℃,反应时间2.5h,壳聚糖∶NaOH∶醇=1∶5∶12(质量比)条件下制得脱乙酰度为93.2%的壳聚糖,而传统水溶剂脱乙酰度小于50%.另外间歇法处理样品可以在较短的时间里制备出脱乙酰度较高的壳聚糖,并用红外谱图对壳聚糖进行了表征.     

壳聚糖脱乙酰度测定方法的总结与比较

测定壳聚糖脱乙酰度(DD)的方法主要分为三类:①光谱法:紫外、红外光谱和核磁法;②破坏样品法:色谱法、差示扫描量热和元素分析法;③滴定法:酸碱、电位和胶体滴定等方法。对壳聚糖脱乙酰度测定方法进行总结与比较,为研究者选择最佳的壳聚糖脱乙酰度测定方法提供理论依据。     

N-乙酰化制备水溶性壳聚糖研究

以高脱乙酰度壳聚糖为原料,在不使用吡啶的无水乙醇均相体系中用乙酸酐通过N-乙酰化制备了水溶性壳聚糖,采用酸碱滴定、XRD、IR对壳聚糖原料和所制得水溶性壳聚糖的脱乙酰度、结晶状态、红外光谱分别进行了测试分析,并探讨了水溶性壳聚糖的结构与水溶性机理。     

The effect of the degree of deacetylation of chitosan on its dispersion of carbon nanotubes

The effect of the degree of deacetylation (DD) of chitosan biopolymer on the noncovalent surface modification of multiwall carbon nanotubes (MWCNTs) is presented. MWCNTs were modified by chitosan having different degree of deacetylation (61%, 71%, 78%, 84%, 90% and 93%) and UV-Visible spectroscopy was used to evaluate their dispersion efficiency as a function of chitosan concentration and degree of deacetylation. Results showed that the dispersion of MWCNTs could be dramatically improved when using chitosan with the lowest degree of deacetylation (61%DD) possibly due to a higher surface coverage of the MWCNTs. Zeta potential measurements were used to confirm that the chitosan surface coverage on the MWCNTs was twice as high when modifying the nanotubes surface with the 61%DD than when using the 93%DD chitosan. These results suggest that the dispersion of MWCNTs with chitosan can be improved when using chitosan having a degree of deacetylation of 61%. These results are of interest in particular for the improved dispersion of MWCNTs in aqueous solutions such as in drug delivery applications.     

溶解沉淀法制备高脱乙酰度壳聚糖

以乙醇为反应介质,采用溶解沉淀法制备了高脱乙酰壳聚糖。在反应温度８０℃,反应时间３ｈ,壳聚糖与氢氧化钠和乙醇的质量比为１∶３∶１６的条件下,获得了脱乙酰度达９０％的壳聚糖,而传统方法只有８０％。     

Effect of Deacetylation Degree in Chitosan Composite Membranes on Pervaporation Performance

ABSTRACT

The effect of the degree of deacetylation in chitosan composite membranes on their pervaporation performance for ethanol dehydration was investigated. The degree of deacetylation of chitosans was measured by using an infrared spectroscopic method and elemental analysis. The chitosan composite membranes were prepared by coating a chitosan solution onto a microporous polyethersulfone membrane with 3–7 nm pore sizes. Then the surface of the top layer (chitosan) of well-dried membranes was crosslinked with sulfuric acid, and pervaporation experiments for binary mixtures (water—ethanol) were carried out at various conditions. In the case of a chitosan membrane with a high degree of deacetylation, the flux increases while the separation factor decreases compared with membranes with a low degree of deacetylation.     

Influence of chitosan characteristics on coagulation and flocculation of organic suspensions

Several samples of chitosan with different degrees of deacetylation and of different molecular weights were tested for the coagulation–flocculation of organic suspensions. Organic suspensions were prepared by mixing mushroom powder with tap water. Experiments were carried out at pH 5, pH 7, and pH 9. Because decreasing the pH reduced the amount of chitosan required to reach the required turbidity, at pH 9, a high concentration of chitosan was required to achieve the required treatment levels, whereas the difference was less significant between pH 7 and pH 5 (the required concentration of chitosan was halved). Though viscosity, correlated to the molecular weight of chitosan, affected treatment performance, its influence on the efficiency of coagulation–flocculation could be substantially reduced by slightly increasing the concentration of the polymer. This is of importance in the processing of industrial effluents: the aging of a chitosan solution, which may cause partial depolymerization, and loss of viscosity, will have a limited impact on process efficiency. The degree of deacetylation also has a limited effect on treatment performance, especially when the degree of deacetylation exceeds 90%. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 98: 2070–2079, 2005     

Effect of molecular weight and degree of deacetylation of chitosan on urea adsorption properties of copper chitosan

Copper chitosan complexes prepared by different specifications of chitosan and copper sulfate were used as urea sorbents. Experimental results showed that the adsorption capacity for urea of copper chitosan increased with an increasing degree of deacetylation and decreasing molecular weight of chitosan. The urea adsorption capacity of copper chitosan was 120.0 mg/g, when 1.0 g of copper chitosan was admitted to 100 mL of a 1300 mg/mL (pH 6.0) urea solution, with chitosan degree of deacetylation of 84.3% and viscosity molecular weight of 6.5 × 10⁵, at 37°C for 8 h. No elution of the copper from the copper chitosan could be detected under the optimal conditions. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 1520–1523, 2003     

壳聚糖降解探索

本文着重讨论了壳聚糖的主要降解方法及使用氧化降解法制备低聚壳聚糖的方法,采用正交设计,探讨降解条件对产物脱乙酰度、特性粘度等的影响。     

Chitosan as Scaffold Materials: Effects of Molecular Weight and Degree of Deacetylation

In this study, we investigated in vitro the role of the degree of deacetylation and molecular weight on some biological properties of chitosan films. The influence of different degree of deacetylation and molecular weight of chitosan on the hydrophilicity, degradation, mechanical properties and biocompatibility were evaluated. The results showed that the degree of deacetylation affected the hydrophilicity and biocompatibility of the chitosan films. The molecular weight, on the other hand, affected the rate of degradation and the mechanical properties. Chitosan with higher degree of deacetylation and molecular weight was more suitable for tissue engineering applications. Alginate could be added into chitosan to modify the rigidity and hydrophilicity of chitosan. Higher hydrophilicity, biocompatibility, and elongation were found after modification.     

壳聚糖在活性染料染羊毛织物上的应用工艺探讨

本文对壳聚糖处理过的羊毛织物用活性蓝BET染色工艺进行了探讨.讨论了壳聚糖脱乙酰度、壳聚糖浓度对羊毛染色性能的影响,并比较了经壳聚糖处理与未处理羊毛染色性能的差异.结果表明,提高处理液中壳聚糖的浓度或脱乙酰度都能提高活性染料的固色率,提高织物表面色深值K/S,而且对染色样的各项牢度影响不大.