【作者】 张勇；

【导师】 阎克路；

【作者基本信息】 东华大学 ， 纺织化学与染整工程， 2011， 硕士

【摘要】 纤维素是地球上储藏量很大的天然高分子,很多农作物废弃物中含有大量的纤维素,近几年来,将农业废弃物等可再生资源用于工业生产已经成为一种新的发展趋势。纳米微晶纤维素(NCC)作为一种多羟基化合物,可与聚氨酯(PU)采用一定方式复合生成纳米纤维素-聚氨酯(NCC/PU)复合材料,增强其在羊毛纤维基质材料上的成膜性,从而赋予羊毛纺织品更好的防毡缩性能。本文的研究工作主要涉及以下内容：纳米微晶纤维素的制各和表征、水性聚氨酯合成工艺改进、纳米微晶纤维素与封端型水性聚氨酯复配及在羊毛防毡缩工艺应用方面的研究。首先,采用硫酸酸解微晶纤维素(MCC)的方法来制备纳米微晶纤维素,通过单因素实验确定工艺条件范围,再通过正交实验和利用对水解液的外观评价,优化制备NCC的工艺条件。在此基础上,借助粒径和产率测试,研究了硫酸浓度、处理时间和温度对NCC粒径和产率的影响,提出制备NCC的最佳酸解条件。然后通过傅立叶红外光谱(FITR)、透射电镜(TEM)、X射线衍射图谱(XRD)、热重分析(TG)以及元素分析测试技术,对NCC的性能进行表征和分析。同时,在课题组前期研究工作的基础上,对水性聚氨酯(PU)合成工艺作了改进。聚氨酯合成工艺一般采用有机锡催化剂,其毒性较大；另外,合成反应的终点采用滴定法测量异氰酸酯基含量,在大生产中比较难控制。针对这些问题,本文筛选了3种非锡催化剂,最终确定了一种非锡催化剂替代了毒性较大的有机锡催化剂。研究了非锡催化剂的用量、反应温度对反应速率的影响。同时,研究了预聚体粘度与对应异氰酸酯基(NCO)之间的关系,证明了可以用测试预聚体粘度来确定合成反应终点的简易测试方法,并考察了聚氨酯乳液的稳定性。通过傅立叶红外光谱表征了预聚反应过程。最后,将制备的纳米微晶纤维素与水性聚氨酯进行复配实验,确定了NCC的添加量,制备了纳米纤维素-聚氨酯(NCC/PU)复合乳液。并用NCC/PU复合乳液对羊毛进行防毡缩整理,提出了NCC/PU复合乳液防毡缩整理的合适浓度。通过扫描电镜(SEM)、手感测试等对处理过的羊毛织物进行表征和评价,并与纯PU对羊毛织物的整理效果作了比较。研究结果表明,经NCC/PU复合乳液处理的羊毛织物比纯PU整理剂处理的有更好的防毡缩性能。更多还原

【Abstract】 Cellulose is a natural polymer with big reserves on earth. A lot of crop waste contains abundant cellulose. In recent years, it has become a new trend that renewable resources such as agricultural waste are used for industrial production. As a polyol, nanocrystalline cellulose(NCC) can be used with polyurethane(PU) to produce a composite material NCC/PU in a certain way, to enhance the membrane on wool fibers and obtain a better wool shrink-proofing performance.This research mainly involves the followings:the preparation and characterization of nanocrystalline cellulose, optimization of synthetic process of water-soluble polyurethane, the preparation of NCC/PU and its application of anti-felting finishing on wool.Nanocrystalline cellulose was prepared with microcrystalline cellulose by hydrolysis with sulfuric acid. The conditions of acid hydrolysis process were discussed by measuring the clarity degree of hydrolyzed solutions through single factor and orthogonal experiments. And then we discussed the effect of sulfuric acid concentration, treatment time and temperature on the size and yield of NCC. The properties of the NCC were analyzed and characterized by FITR, TEM, WXRD, TG and element analysis.Meanwhile, on the basis of previous studies on water-soluble polyurethane, synthetic process was optimized. Generally, organotin catalyst is used in polyurethane synthesis, but it is toxic. In addition, the end of pre-polymerization is measured by titration of NCO content which is inconvenient to control production process. In this paper, an amine catalyst (triethylene diamine) was selected to replace toxic dibutyltin dilaurate. The amount of the catalyst and the optimum reaction temperature were discussed. The relationship between the viscosity of the pre-polymer and the corresponding content of NCO was studied. We developed an easy viscosity test method to control the pre-polymerization. We also studied the stability of polyurethane emulsion. The pre-polymerization process was characterized by FITR.Finally, NCC was mixed with PU to prepare NCC/PU. We discussed the content of NCC. And we treated wool with NCC/PU emulsion for anti-felting finish. The optimum concentration was discussed also. The wool fabric treated with NCC/PU was characterized and evaluated through SEM and hand testing and compared with that treated with only PU. The result showed that wool treated with NCC/PU had a better performance on anti-felting.更多还原