制备条件对脱乙酰甲壳素性能的影响

我们研究了甲壳素及脱乙酰甲壳素的制备方法,测定了脱乙酰甲壳素的分子量、脱乙酰度及粘度。对不同条件下及用不同原材料制得的脱乙酰甲壳素的性能进行了比较。结果表明,提高反应温度、碱液浓度和延长反应时间,可以提高脱乙酰度,但其分子量和粘度均相应降低。在脱乙酰度基本相同的情况下,由虾壳制得的脱乙酰甲壳素,其分子量和粘度都大于由蟹壳制得的产品。实验表明,脱乙酰甲壳素不适于在极性介质中吸附弱极性物质。     

微波间歇法快速制备高粘均分子量和高脱乙酰度的壳聚糖

使用微波间歇法可快速制备高脱乙酰度和高粘均分子量的壳聚糖. 单因素实验确定的工艺条件为微波功率800 W,将45%(w)的氢氧化钠溶液与250~380 mm的20 g甲壳素粉以8:1的体积比混合,在100℃下反应10 min,洗涤、微波干燥后在相同条件下再反应1次,共20 min,可制得脱乙酰度为94.5%、粘均分子量1.48×106的白色壳聚糖粉末. 其他制备条件相同,使用电加热法间歇处理甲壳素粉3次,反应共5 h,可以得到脱乙酰度为96.2%、粘均分子量为3.8×105的褐色壳聚糖粉末. 微波间歇法所制壳聚糖的结晶度高,内部有规整的有序结构,用它制备的膜致密,性能优于用电加热法所制壳聚糖制备的膜.     

β-甲壳素脱乙酰化及其产物结构表征

由β-甲壳素脱乙酰制备高分子量壳聚糖，利用元素分析方法测定其脱乙酰度（DD），利用梯度稀释法测试特性粘度，利用x-射线衍射（XRD）、傅里叶变换红外光谱（FTIR）、核磁共振（NMR）等现代仪器分析手段分析产物结构。     

微波辐射制备壳聚糖

用质量分数34％的NaOH在微波辐射下对甲壳素进行非均相脱乙酰以快速制备壳聚糖，并测定了不同条件下制得的壳聚糖的相对分子质量和脱乙酰度，该反应时间短，重复性好，产品质量易控制。     

密闭条件下微波场中甲壳素脱乙酰反应的条件研究

密闭条件下微波场中研究反应条件对甲壳素脱乙酰反应的影响。结果表明：120℃时，反应18min，脱乙酰度已超过90％，特性黏度达到440mL／g左右。随料液比的增加，壳聚糖的脱乙酰度及特性黏度增大，但料液比超过1：20，脱乙酰度和黏度反而都有下降的趋势。原料粒径在0．36～0．60mm之间较好。乙醇辅助处理可提高产物脱乙酰度。经红外光谱测定得出，微波处理及常规方法制备得到产物的分子结构基本相似。     

微波条件下甲壳素脱乙酰反应的条件研究

研究了微波处理条件下,甲壳素脱乙酰反应条件对壳聚糖脱乙酰度的影响。结果表明:微波甲壳素颗粒大小选择为0.18～0.3mm(过60～80目筛)较利于反应。在料液比小于1∶12(质量∶体积)时,壳聚糖脱乙酰度几乎不变,粘度逐渐增大,之后脱乙酰度随料液比的增大而下降。脱乙酰度随碱液浓度的增大而增大。随微波处理时间的延长,脱乙酰度上升、特性粘度下降。微波功率越高,相同时间下,产品的脱乙酰度越高。经正交试验得出:粒度为0.18～0.3mm的甲壳素原料,按料液比1∶12(质量∶体积)加入浓度为50%(质量分数)的NaOH溶液,在微波功率320W下处理21min,所得产品的脱乙酰度可达85.65%,特性粘度为394.07mL/g,灰分为0.05%。     

不同虾壳部位中的甲壳素和壳聚糖

用EDTA的方法分别从虾壳的不同部位:虾头、虾身、虾足和虾头内容物三部分制备甲壳素和壳聚糖,对三组试样的性能参数如脱乙酰度和相对分子量等进行分析研究。得出结论:由虾壳不同部位所制得的甲壳素和壳聚糖结构基本一致,但其脱乙酰度和相对分子量有较大差别,其物化性质也有所不同。在三组试样中,以从虾头壳制备的甲壳素和壳聚糖的相对分子质量为最大;而脱乙酰度则以从虾足和虾头内容物中制得试样较高。     

虾壳制备甲壳素和壳聚糖的研究

用EDTA的方法分别从虾壳的不同部位:虾头、虾身、虾足和虾头内容物三部分制备甲壳素和壳聚糖,对三组试样的性能参数如脱乙酰度和相对分子量等进行分析研究。得出结论:由虾壳不同部位所制得的甲壳素和壳聚糖结构基本一致,但其脱乙酰度和相对分子量有较大差别,所以其物化性质也有所不同。特别值得一提的是,在三组试样中,以从虾头壳制备的甲壳素和壳聚糖的相对分子质量为最大;而脱乙酰度则以从虾足和虾头内容物中制得试样较高。     

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。     

壳聚糖的表面性能及分子量与脱乙酰度的影响

应用红外光谱法对四种壳聚糖样品进行了结构表征,同时估算了其脱乙酰度,并用粘度法测定了分子量。根据Washburn的浸渍理论和van Oss-Chaudhury-Good的组合理论,应用柱状灯芯技术,对壳聚糖的表面性能进行了测试。研究发现,壳聚糖的分子量和脱乙酰度都影响其表面性能。当脱乙酰度相同时,分子量与表面能γS及表面能分量γSLW、酸碱比值γS+/γS-成正比,而与其酸性力γS+和碱性力γS-以及极性率γAB/γs成反比;而分子量相近时,表面性能可能主要受脱乙酰度的影响。随着脱乙酰度的增加,壳聚糖的表面能γS及其分量γSLW、酸碱比值γS+/γS-都增大。实验所测得的壳聚糖的表面能数据得到文献的支持。     

酶载体壳聚糖制备的研究

本文分别采用电热法、连续微波法和问歇微波法制备了几种性能不同的壳聚糖,并对产品的脱乙酰度和分子量进行了比较.结果表明,间歇微波法制备的壳聚糖具有制备时间短、产品脱乙酰度高和分子量大等特点,能更好地满足酶载体的要求.     

微波法制备壳聚糖絮凝剂的研究

以虾壳作为原料制得甲壳素后,用NaOH溶液浸润然后在微波作用脱去乙酰基和蛋白质制备壳聚糖;研究了影响壳聚糖脱乙酰度及粘均分子质量的因素;选择c（NaOH）=45%～50%,微波功率400 W,一次微波法反应时间10 min,可得脱乙酰度75%、分子质量（3.5～4） 万的壳聚糖;二次微波法每次反应时间分别为5 min,可得脱乙酰度90%的壳聚糖;与传统方法相比,缩短了反应时间,节约了能耗;将实验制得的壳聚糖作为絮凝剂用于含磷废水,絮凝效果明显,除磷率可达90%.     

Chitosan and modified chitosan membranes I. Preparation and characterisation

Chitosan has been prepared from prawn shell and crab shell chitin. The molecular weight of the material derived from prawn shells is higher than that obtained from crab shell. The molecular weight, tensile strength, elongation at the break, and hydrophilic properties of chitosan are extremely dependent on the degree of deacetylation achieved when chitin is hydrolyzed to chitosan. Graft copolymers have been prepared with chitosan and a series of vinyl monomers using both heterogeneous and homogeneous reaction conditions. The hydrophilic properties of chitosan can be modified by blending with poly(vinyl alcohol).     

Variation in Properties of Chitosan Prepared at Different Alkali Concentrations from Squid Pen and Shrimp Shell

Chitin from squid pen (Loligo sp.) and kiddi shrimp shell (Parapenaeopsis stylifera) were treated at room temperature (30 ± 2°C) with four different concentrations of sodium hydroxide: 20, 30, 40, and 50% w/w. With 50% sodium hydroxide solution, within 108 h, the chitin from squid pen was deacetylated to give chitosan. But it required 126 h at 40% and 144 h at 30% concentration of sodium hydroxide. In the case of chitin from Parapenaeopsis stylifera, complete deacetylation took place after 120 h and 168 h at 50 and 40% concentrations of sodium hydroxide, respectively. But shrimp shell on treatment with 20 and 30% sodium hydroxide solutions and squid pen kept at 20% sodium hydroxide were not sufficiently deacetylated even after 480 h. Properties like degree of deacetylation, viscosity and molecular weight of the prepared chitosan samples were studied. Minimum alkali concentration required for the formation of chitosan at room temperature was found to be 30% for squid chitin and 40% for shrimp chitin. With the increase in the time of deacetylation, decreases in molecular weight and viscosity were observed in chitosan from both sources. Maximum viscosity was recorded by chitosan prepared from squid pen using 30% sodium hydroxide solution at room temperature.     

A New Drying Approach to Enhance Quality of Konjac Glucomannan Extracted from Amorphophallus muelleri

A new drying approach to enhance physical quality of konjac glucomannan extracted from Amorphophallus muelleri was studied. It consisted of a comparison between microwave vacuum drying and conventional hot-air drying. The effects of microwave vacuum drying and hot-air drying on drying kinetics and physical and structural properties such as color, bulk density, particle density, porosity, viscosity, and morphology of konjac glucomannan (KGM) flour were investigated. It can be concluded that microwave vacuum drying significantly reduced drying time and increased porosity of dehydrated products which have a positive effect on the viscosity of the KGM solution. In contrast, it decreased bulk density and particle density when compared with conventional hot-air drying. Microstructure observations revealed the presence of large cavities in the granules of microwave-vacuum-dried KGM samples. However, there was a slight change in color of the microwave-vacuum-dried samples, resulting in a lower whiteness index than the whiteness index of hot-air-dried samples. Hence, microwave vacuum drying was found to have a number of advantages over the conventional hot-air drying method. Therefore, microwave vacuum drying has potential to become a useful drying method for the industrial production of KGM flour.     

胶原蛋白与壳聚糖相容性研究

将胶原蛋白与两种去乙酰度（95％,85％）的壳聚糖分别配成不同质量比的HAc共混溶液,在28℃下测定了共混液的黏度,利用Δb法则比较共混液中两种物质的相容性。结果表明在28℃的HAc溶液中,任何质量比的胶原蛋白和壳聚糖均相容,并且两者相容性不受壳聚糖去乙酰度的影响。     

PET切片干燥过程中的固相缩聚

本文通过测定干燥后PET切片的特性粘度及所纺成纤维的强伸度,研究了直接酯化法生产的PET切片在连续式充填干燥器中干燥过程中所发生的固相缩聚。研究结果表明干燥温度和干燥时间对固化反应的速度和程度都有很大影响,固相缩聚后的干切片粘度和分子量有所提高,并将导致熔体温度和POY强度提高。干燥温度和时间的波动会导致干切片特性粘度的不均,并进一步导致纤维的不匀率提高。     

微波场中KCl浓度对几丁质脱乙酰反应的影响

研究了KCl浓度对几丁质在微波场中脱乙酰反应的影响. 结果表明，引入盐离子促进了反应的进行. 随着反应时间的延长，几丁聚糖的脱乙酰度上升，但上升速度逐渐变慢，呈一级反应特征；分子量随时间延长而降低. 脱乙酰度随KCl浓度上升而减小，但在实验范围内，均高于对照组. 当[KCl]=0.05 mol/L时脱乙酰度达到79.26%，与对照组相比(脱乙酰度=69.84%)提高了13.5%. 随KCl浓度的上升，分子量开始减小，当KCl浓度上升到0.2 mol/L附近时，分子量又呈上升趋势. 这是由于KCl浓度影响体系介质损耗角正切值，在较高KCl浓度时降低了体系对微波的吸收能力.     

Study of the influence of processing parameters on the production of carboxymethylchitin

Carboxymethylchitin was prepared at different reaction temperatures and from alkali chitin with different concentrations of alkali. Properties of the product were studied. Alkali chitin were prepared using freshly prepared sodium hydroxide of 45, 50, 55, 60 and 65% (w/w) concentration and carboxymethylated using monochloroacetic acid at controlled (35-40 °C) and uncontrolled (30-80 °C) temperature conditions. Molecular weight, viscosity, degree of deacetylation, etc. of the resultant product, i.e. carboxymethylchitin were determined. It was found that the reaction temperature has a profound influence on the property of the product than alkali concentration. A hygroscopic and completely water-soluble product was formed. Optimum conditions for the production of carboxymethylchitin were found to be 60% NaOH concentration and at 35-40 °C reaction temperature. At these conditions, it was obtained with a molecular weight of 4.11×10⁶ Da, viscosity 1926 cP and degree of deacetylation 45.02%.