脱胶对蚕丝纤维的溶解及丝素蛋白性能的影响

为探究脱胶对蚕丝溶解及丝素蛋白的影响,分别将碳酸钠和尿素脱胶的蚕丝溶解在氯化钙/乙醇/ 水体系中,借助颜色光谱、红外光谱、X 射线衍射、十二烷基硫酸钠聚丙烯酰胺凝胶电泳、扫描电子显微镜等方法对蚕丝脱胶率、脱胶蚕丝结构、溶解进程以及丝素蛋白的流变、成膜及成球性能进行测试。结果表明：相对于尿素脱胶,碳酸钠脱胶可溶解部分丝素蛋白,脱胶率较高,脱胶蚕丝白度低;碳酸钠脱胶对蚕丝结晶度影响大,且对丝素蛋白重链分子单元破坏严重,有助于溶解体系中钙离子对丝素蛋白的渗透,使脱胶蚕丝较易溶解,但丝素蛋白分子量低,蛋白液黏度较小;碳酸钠脱胶降低了丝素蛋白膜的力学性能和透光率,制备的丝素蛋白空白微球粒径较小,分布较为集中。     

基于钙醇体系的丝素蛋白提取工艺

采用尿素对蚕丝进行脱胶,在钙醇体系下对丝素进行溶解得到丝素蛋白,对蚕丝的脱胶率、丝素蛋白化学结构、丝素蛋白含量和相对分子质量进行测试.结果表明:当尿素为9 mol/L,处理温度90～100℃,处理时间2 h时,蚕丝脱胶所用时间最短.在CaCl2-EtOH-H2O(物质的量之比1:2:8)体系下,溶解温度90℃,溶解时间...     

酸-醇体系丝素蛋白水凝胶制备与性能表征

针对再生丝素蛋白水凝胶形貌不可控、凝胶速度慢、压缩性能差的问题,提出了一种乙酸-乙醇体系共同促进丝素蛋白快速凝胶的方法。通过研究相同酸性条件下,不同质量分数乙醇对水凝胶形貌、聚集态结构、热稳定性、压缩性能等的影响,探索水凝胶内部纤维结构的成形条件以及不同形貌下水凝胶的结构与性能差异。结果表明:相同酸性条件下随着乙醇质量分数的提高,水凝胶的结构与性能均得到改善,凝胶时间由12~14 h缩减到1 h 左右,水凝胶形貌逐渐由几十到几百微米的孔洞结构向纤维结构转变,水凝胶中丝素蛋白结构以β-折叠为主;当乙醇质量分数为5.0%时,纤维直径为(1.09±0.5) μm,在干态下应变为60%时的压缩强度为(75.16±3.79) kPa,在湿态下压缩回复率达到伸长的63%。     

脱胶工艺对蚕丝溶解及再生丝素蛋白纤维性能的影响

为探究脱胶工艺与蚕丝溶解及纤维成形之间的关系,讨论了脱胶溶液质量分数、脱胶次数对蚕丝脱胶率、蚕丝表面形貌、丝素溶解度以及再生丝素蛋白纤维结构及性能的影响。结果表明：蚕丝脱胶率随 Na2CO3 溶液质量分数与脱胶次数的增加而增加,当 Na2CO3 溶液质量分数为0.1%、脱胶3次时,脱胶丝素纤维表面出现明显劈裂的微原纤结构,纤维的断裂强度下降了27.6%。丝胶的去除程度对丝素溶解及再生丝素纤维的结构有所影响,溶解时间随 Na2CO3 溶液质量分数、脱胶次数的增加而减少,再生丝素蛋白纤维的力学性能随脱胶程度的加深而降低,当 Na2CO3 溶液质量分数为0.05%、脱胶3次时,再生丝素蛋白纤维直径均匀、表面光滑、结构紧密且力学性能较好。     

再生丝素蛋白水凝胶的制备与改性

近年来,水凝胶材料在生物医学等领域异军突起,受到了国内外学者的重视。丝素蛋白材料生物相容性良好、可被降解性且无生物毒性,现已被广泛应用在生物医学领域,许多研究水凝胶材料的学者将其研究原料锁定为丝素蛋白材料。本文以蚕丝丝素蛋白结构为基础,详细叙述了从蚕丝脱胶、丝素蛋白溶解到凝胶形成的丝素蛋白水凝胶的制备全过程。并从凝胶形成的角度,介绍了通过物理、化学、基因工程等方法对丝素蛋白水凝胶改性的实例,为丝素蛋白水凝胶的研究提供了新方向。     

丝素蛋白溶液的制备工艺研究

从丝素蛋白的功能活性角度出发,对工业废蚕丝进行进行脱胶处理,选择安全、廉价的碳酸钠作为脱胶剂,并采用正交试验对脱胶条件进行了优化,得出最佳脱胶工艺条件为:Na2CO3质量分数为0.5%,脱胶时间为30 min,废蚕丝与Na2CO3溶液的固液比为1∶50(g/m L),此时脱胶率最高,可达23.1%,同时对脱胶的蚕丝进行了盐溶处理,得出脱胶丝素以Ca Cl2质量分数为40%,溶解时间为5 min进行溶解时,其效果最好。     

海藻酸钠/丝素蛋白复合水凝胶的制备及性能研究

将海藻酸钠与丝素蛋白共混制备海藻酸钠/丝素蛋白水凝胶,探讨水凝胶成形过程及不同参数对水凝胶凝胶时间的影响及药物在海藻酸钠/丝素蛋白水凝胶中的缓释情况。试验表明:氯化钙/甲酸溶剂体系溶解脱胶蚕丝可以获得纳米原纤结构的再生丝素溶液,在凝胶过程中,复合水凝胶的凝胶时间随海藻酸钠的含量增加而延长,丝素蛋白/海藻酸钠比例为50/50时,凝胶时间需要89 min;当凝胶温度由15℃升至55℃时,凝胶时间由150 min缩短到55 min,因此可以通过调整海藻酸钠的比例、凝胶温度来调节复合水凝胶的凝胶时间;载药复合水凝胶释药曲线表明,药物释放过程呈先快后慢规律。     

丝素蛋白在生物医用材料中的应用

总结蚕丝蛋白纤维的组成与结构、蚕茧脱胶与丝素蛋白溶液的制备、丝素蛋白在单一结构和多级结构的生物医用材料中的应用和发展现状,以及丝素蛋白纤维的溶解方法和纺丝方法。     

丝素蛋白/海藻酸钠水凝胶的制备及其释药性能

为提高水凝胶的负载率和缓释率，以N-羟基丁二酰亚胺和乙基(3-二甲基氨基丙基)碳酰二亚胺盐为催化剂，柠檬酸为交联剂，将丝素蛋白和海藻酸钠交联制备得到丝素蛋白/海藻酸钠水凝胶，测试了水凝胶的结构、形貌、溶失率、吸水率、载药率和释药率。结果显示：丝素蛋白/海藻酸钠水凝胶的最佳制备工艺条件为丝素质量分数2.5%,柠檬酸质量分数2.5%,海藻酸钠质量分数4.5%,催化剂(质量比为1∶1)质量分数为0.5%。红外光谱图显示，在该条件下制备的水凝胶中含有丝素蛋白和海藻酸钠的特征吸收峰，其形貌为多孔结构，24 h后溶失率为11.4%,吸水率约70%,其最大载药率约50%,在pH=7.4的缓冲溶液中缓释8 h后，其释药率接近75%,表现出良好的释药性能。     

超疏水弹性丝素蛋白纤维气凝胶的制备及其吸油性能

为提升丝素蛋白(SF)气凝胶力学弹性，以SF微-纳米纤维(SMNF)为前驱体，通过冷冻干燥和硅烷改性策略成功构筑了超疏水高弹性SMNF气凝胶(简称MS气凝胶),并对其微观结构和力学性能进行测试表征，系统研究了MS气凝胶的吸油性能。结果表明：MS气凝胶的网络骨架由微-纳米纤维组装而成，并具有分级多孔的胞腔结构，这赋予气凝胶超低的密度(5.36 mg/cm³)和超高的孔隙率(99.63%);此外，MS气凝胶还表现出优异的力学性能，在80%纵向压缩应变下的最大应力为15.72 kPa, 100次循环压缩后气凝胶保留了81%以上的初始相对高度。能量色散光谱和红外光谱分析证实：硅烷改性后气凝胶的表面形成了硅氧烷网络结构，使其具有超疏水特征(水接触角为150.9°);MS气凝胶对氯仿的吸收能力为188.75 g/g,并具有优良的循环使用性能。     

Effect of silk degumming on the structure and properties of silk fibroin

Two different silk fibroin samples were obtained by the Na₂CO₃ and urea degumming methods of silk fibers in the same fiber dissolution system, respectively. The molecular weight and viscosity of the fibroin samples were analyzed by the methods of SDS-PAGE, rheological, and etc. Then, different silk fibroin membranes (SFMs) and blank microspheres were prepared, and the effects of degumming methods on the silk fibroin were studied via analyzing the differences of SFMs and blank microspheres of the two samples. The experimental results showed that the viscosity of fibroin solution was positively correlated with its molecular weight. The fibroin prepared by the Na₂CO₃ degumming was lower than the one prepared by the urea degumming in the viscosity of the fibroin solution under the same mass concentration. Degumming with Na₂CO₃ exhibited the obvious effects on the thermal stability and mechanical properties of SFM, tensile strength decreased almost 10% and breaking elongation reduced more than 50%. Blank microspheres prepared from silk fibroin degummed with the different methods showed different particle sizes and its distribution. The microspheres prepared from silk fibroin degummed with the Na₂CO₃ had the smaller particle sizes and more concentrated distribution compared with those with the urea.     

Experimental study on hydrogen peroxide-free processing machine-made silk floss北大核心CSCD

Silk is a kind of natural fiber with good luster strength elasticity dyeability hygroscopicity and other advantages. Silk products are quite popular to the customers because of their excellent performance such as heat preservation air permeability and so on which make them comfortable to use. Silk floss which is made from pupa lining secondary cocoon etc. can be used as floc and filler materials and is an important part of silk products. According to its production mode silk floss can be divided into manual silk floss and machine-made silk floss and the latter has become the main processing mode of silk floss production due to its high production efficiency. In terms of composition silk flossing generally contains 20% - 30% sericin pupa oil and impurities so in the degumming process in addition to adding sodium carbonate and other degumming agents to remove sericin a large amount of hydrogen peroxide with strong oxidation property is also used to increase the cleanliness and smoothness. Unfortunately hydrogen peroxide is highly flammable and explosive and poses a risk in transportation and storage causing potential safety hazards to the silk processing industry. In order to solve this problem we innovatively propose two hydrogen peroxide-free processing methods of machine-made silk floss by using sodium percarbonate degumming or sodium carbonate-ozone. As an environmentally friendly solid oxidant sodium percarbonate can produce hydrogen peroxide and sodium carbonate after decomposition and is often used to degrade organic harmful substances. Similarly ozone is a common strong oxidant with broad-spectrum antibacterial properties and because ozone can be produced instantly by ozone generators there is no risk of transport and storage. Silk is composed of silk fibroin and sericin. Among them silk fibroin is fibrous protein which will swell in hot water while sericin is globular protein which is easy to dissolve in hot water. As a result in this paper heated sodium percarbonate solution and sodium carbonate-ozone system were used to deglue silk floss. The methods were as follows silk floss was degummed three times in boiling 0. 78 g / L sodium percarbonate solution for 30 minutes each time or was degummed three times in boiled 0. 5 g / L Na2 CO3 solution with ozone continuously flow at a rate of 100 mg / L - h for 30 minutes each time. After cleaning and drying the degummed silk floss can be obtained. After the experiment the apparent morphology sericin residual efficiency impurity rate compression resilience whiteness and other silk floss quality indexes of the two methods were analyzed and compared with superior machine-made silk floss processed by commercial way with hydrogen peroxide. The results show that both two processing methods got uniform degumming effect of silk floss and the surface of the single fiber was smooth and the degumming effect was basically the same as that of commercial products prepared with hydrogen peroxide. The sericin residual rate of silk floss was between 3% - 4% which was in line with the requirements of less than 5% of superior silk floss. There was no significant difference between silk floss obtained and commercial superior products in smoothness and whiteness. In conclusion the performance of silk floss in all aspects has reached the standard of superior products that is the sericin content is not more than 5% the impurity content is not more than 0. 1% the compression rate is not less than 45% and the response rate is not less than 92% . Based on the experimental results and analysis it can be concluded that the machine-made silk floss with good performance can be prepared without hydrogen peroxide showing the feasibility of processing machine-made silk floss without hydrogen peroxide which is of great significance to the research and development of a safe and reliable oxidant system for the removal of impurities in silk floss and to further improve the safety of machine-made silk floss production process. © 2022 China Silk Association. All rights reserved.     

再生蓖麻蚕丝素蛋白静电纺丝的结构研究

采用碳酸钠溶液对蓖麻蚕丝纤维脱胶,将脱胶后的蓖麻蚕丝素溶解于一定浓度的硫氰酸锂溶液中,透析成膜.然后将丝素膜溶解于六氟异丙醇,利用静电纺丝法制得再生蓖麻蚕丝素蛋白非织造网.通过扫描电镜观察非织造网的形态结构,红外光谱、X-射线衍射、热分析(DTA/TG)分析纤维的聚集态结构变化.研究结果表明,再生蓖麻蚕丝素蛋白非织造网纤维直径大约在几微米,与天然丝素相比其聚集态结构有较大变化.     

丝素蛋白/壳聚糖微球制备及其抗菌性能

为开发一种对人体有益且天然无害的抗菌整理剂,采用乳液聚合法制备丝素蛋白/壳聚糖抗菌微球,分析了不同比例下丝素蛋白和壳聚糖制备微球的微观形貌、粒径、二级结构、晶体结构、热稳定性和抗菌性能。结果表明:丝素蛋白质量分数为6%,壳聚糖溶液的质量分数为3%,壳聚糖溶液与丝素蛋白溶液的体积配比为1∶2,所制备的微球形态规整圆滑,粒径均匀分布在0.4~1.4 μm之间;其抗菌效果优异,对大肠杆菌和金黄色葡萄球菌的抑菌率分别为(82±4.2)%和(80±2.6)%;在该比例条件下制备的微球的二级结构由silk I型转变为silk II型,热分解起始温度大于250 ℃,具有良好的热稳定性。     

Studies on degumming of eri silk cocoons

Degumming of eri silk cocoons was carried out using three different concentrations of sodium carbonate and neutral soap along with three different duration of boiling following Box and Behnken design of experiment. Higher amount of degumming loss was observed with more sodium carbonate concentration and duration of boiling for both white and brick red eri silk cocoons. Single fibre tenacity decreases with increase of sodium carbonate concentration as well as duration of boiling. Breaking elongation is affected only by sodium carbonate. Presence of neutral soap has no impact on degumming loss and single fibre tensile characteristics. About 10% sodium carbonate and neutral soap concentration each along with 1-h boiling time facilitates uniform degumming of eri silk cocoons. Degumming loss of about 10% was found without any significant deterioration of single fibre tensile characteristics.     

蚕丝的柠檬酸脱胶

将柠檬酸用到蚕丝的脱胶处理中,研究了酸的质量浓度、反应温度和时间等对脱胶效果的影响,得出了最佳工艺:柠檬酸质量浓度15g/L,温度98℃,浴比1∶60,处理时间30min.研究了酸脱胶后蚕丝的机械性能和表面形态结构的变化,结果表明:对丝素的损伤较小,脱胶后丝的表面变得平滑.