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。     

壳聚糖季铵化衍生物结构表征及特性研究

采用壳聚糖(CTS)与2,3-环氧丙基三甲基氯化铵(GTA)制备了不同取代度的水溶性壳聚糖季铵盐(HACC),通过红外、扫描电镜对壳聚糖、壳聚糖季铵盐结构进行表征,同时测试了壳聚糖季铵盐的水溶性、表面张力.结果表明:取代主要发生在壳聚糖的氨基上,改性后产物外观与粒度有很大变化;壳聚糖季铵化改性产物具有比壳聚糖更优良的水溶性、表面活性,且随着取代度的增加而提高.     

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。     

离子液体中制备壳聚糖季铵盐及其絮凝效果研究

采用一步合成法制备了离子液体甘氨酸盐酸盐,以其水溶液为反应介质,壳聚糖与2,3-环氧丙基三甲基氯化铵进行季铵化反应,得到壳聚糖季铵盐,并将其用于中药废水的絮凝处理.考察了温度、时间、反应物配比及离子液体浓度对季铵盐取代度的影响,以及季铵盐加入量、pH、搅拌时间对絮凝效果的影响.实验结果表明,在离子液体中进行的季铵化反应效率及产品取代度均高于常规的非均相反应,壳聚糖季铵盐能够有效去除中药废水的浊度和COD.     

壳聚糖季铵盐用于银杏叶水提液絮凝工艺研究

[目的]研究壳聚糖季铵盐用于银杏叶水提液除杂纯化的效果。[方法]采用壳聚糖改性产物壳聚糖季铵盐对银杏叶水提液进行絮凝处理,以芦丁保留率和药物浊度作为指标,考察了絮凝剂用量、絮凝温度、静置时间对絮凝效果的影响,并通过正交试验确定出最佳工艺条件。[结果]壳聚糖季铵盐对银杏叶水提液絮凝的最佳工艺条件:水提液p H=4.9,水提液温度40℃,壳聚糖季铵盐用量0.4g/L,静置时间3h。[结论]壳聚糖季铵盐絮凝法澄清效果好,经济实用,可用于银杏叶水提液的絮凝纯化。     

水溶性壳聚糖季铵盐的制备工艺及絮凝性能研究

采用壳聚糖（CTS）为原料,NaOH为催化剂,与3-氯-2-羟丙基三甲基氯化铵（CTA）进行季铵化反应,得到了取代度较高的壳聚糖接枝物,确定最佳反应工艺条件为：n（NaOH）／n（CTA）=1．1：1,n（CTA）／n（CTS）=5：1,反应时间为8h,反应温度为78℃。合成的产物能完全溶于水,并将产物对马铃薯淀粉厂废水进行了絮凝性能测试,结果表明水溶性壳聚糖季铵盐对污水的絮凝效果良好。     

降解壳聚糖季铵盐的制备及其在亚麻染色中的应用

降解壳聚糖季铵盐是将降解壳聚糖的氨基通过引入基团转换成季铵盐或者把一个低分子季铵盐接到氨基上而得到的一类降解壳聚糖衍生物。降解壳聚糖季铵盐在亚麻织物染色中的应用研究表明其具有一定的助染作用。国外对壳聚糖季铵盐的合成已有报道,如1985年国外报道了碘化壳聚糖季铵盐的合成方法,但得到的碘化N-三甲基壳聚糖季铵盐是不溶于水的。     

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.     

壳聚糖季铵盐超声波催化合成

用超声波催化荣典聚糖季铵盐的合成反应，考察了不同反应条件对合成取代度和反应速度的影响，并对反应产物进行相应的结构表征。实验结果表明，超声波催化可以显著白蚁同壳聚糖季铵化异相反应速度，增加反应取代度；本实验反应条件下，壳聚糖的季铵衍生化反应主要发生于亲核中心C2位氮基上，所合成的壳聚糖季铵盐衍生物易溶解于水，具有显著的吸湿与保湿作用     

季铵盐壳聚糖的制备及影响因素

以2,3-环氧丙基三甲基氯化铵(GTA)为醚化剂,与壳聚糖(CS)反应制备了季铵盐壳聚糖。研究了GTA的添加比例,即GTA与CS的物质的量比,以及反应时间、温度、pH值对产物取代度的影响。结果表明:当r(GTA)∶r(CS)为5∶1、反应时间为13 h、温度为80℃、pH值为6～7时,产物取代度最高。     

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.     

Effect of cupric ion on thermal degradation of chitosan

The thermal degradation of chitosan and chitosan–cupric ion compounds in nitrogen was studied by thermogravimetry analysis and differential thermal analysis (DTA) in the temperature range 30–600°C. The effect of cupric ion on the thermal degradation behaviors of chitosan was discussed. Fourier transform-infrared (FTIR) and X-ray diffractogram (XRD) analysis were utilized to determine the micro-structure of chitosan–cupric ion compounds. The results show that FTIR absorbance bands of  N H,  C N ,  C O C etc. groups of chitosan are shifted, and XRD peaks of chitosan located at 11.3, 17.8, and 22.8° are gradually absent with increasing weight fraction of cupric ion mixed in chitosan, which show that there are coordinating bonds between chitosan and cupric ion. The results of thermal analysis indicate that the thermal degradation of chitosan and chitosan–cupric ion compounds in nitrogen is a two-stage reaction. The first stage is the deacetylation of the main chain and the cleavage of glycosidic linkages of chitosan, and the second stage is the thermal destruction of pyranose ring of chitosan and the decomposition of residual carbon, in which both are exothermic. The effect of cupric ion on the thermal degradation of chitosan is significant. In the thermal degradation of chitosan–cupric ion compounds, the temperature of initial weight loss (T_st), the temperature of maximal weight loss rate (T_max), that is, the peak temperature on the DTG curve, and the peak temperature (T_p) on the DTA curve decrease, and the reaction activation energy (E_a) varies with increasing weight fraction of cupric ion. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

The impact of cupric ion on thermo‐oxidative degradation of chitosan

The thermal degradation of chitosan and chitosan–cupric ion compounds in air was studied using thermogravimetric and differential thermal analyses in the temperature range 30–600 °C. The impact of cupric ion on the thermo‐oxidative degradation of chitosan was investigated. Fourier transform infrared and X‐ray diffraction analyses were utilized to determine the microstructure of the chitosan–cupric ion compounds. Kinetic parameters such as activation energy, pre‐exponential factor, Gibbs energy, and enthalpy and entropy of activation were determined using the Coats–Redfern equation. The results show that the thermo‐oxidative degradation of chitosan and chitosan–cupric ion compounds is a two‐stage reaction. The impact of cupric ion on the thermo‐oxidative degradation of chitosan is significant, and all thermodynamic parameters indicate that the thermo‐oxidative degradation of chitosan and chitosan–cupric ion compounds is a non‐spontaneous process and proceeds via a mechanism involving nucleation and growth, with an Avrami–Erofeev function (A₄) with the integral form [?ln(1 ? α)]⁴. Copyright © 2010 Society of Chemical Industry     

气氛对壳聚糖及其铜离子混合物热降解的影响

利用热重分析(TGA)和差热分析(DTA)研究了壳聚糖及其铜离子混合物在氮气气氛和空气气氛中的热降解行为,探讨了气氛对壳聚糖及其铜离子混合物热降解的影响,并采用FTIR、X-射线衍射对壳聚糖铜离子混合物进行了表征.结果显示,壳聚糖及其铜离子混合物的热降解和热氧降解分三个阶段进行:第一阶段为材料失水,为吸热反应;第二阶段为主链脱乙酰和糖苷键的裂解,为放热反应;第三阶段为吡喃环的裂解和炭化残渣的分解,为放热反应.气氛对壳聚糖第一、第二阶段的降解影响较小,对第三阶段的降解影响较大.     

壳聚糖季铵盐阳离子改性亚麻织物染色

采用羟甲基二甲基氯化铵与伯羟基酰化N-乙酰化壳聚糖合成了低聚合度季铵型阳离子壳聚糖季铵盐(HBCC)。采用HBCC对亚麻织物整理后染色,研究结果表明,HBCC处理的亚麻织物上染率为41.0%,固色率为75.9%,水洗牢度达到5级,耐摩擦牢度达到5级。     

Synthesis and characterization of chitosan alkyl carbamates

The synthesis of chitosan methylcarbamate (ChMC) and ethylcarbamate (ChEC) is described by using a new methodology. Polymers with substitution degrees up to 63% for ChEC and 68.5% for ChMC were obtained. Derivatives with lower substitutions were acid soluble but those with higher ones were completely insoluble. This could be due to the loss in hydrophilic sites when the substitution degree increases. The reaction conditions and degree of substitution obtained for both derivatives were also described. A complete chemical characterization was carried out by spectroscopic techniques. The thermal degradation of chitosan and derivatives were studied in the range 25–500°C and both derivatives were shown to be thermally less stable than chitosan. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 2742–2747, 2002