纳米磷酸锌微波辅助制备及应用

发布时间：2018-06-03 03:29

本文选题：磷酸锌 + 棉织物　；参考：《东华大学》2015年硕士论文

【摘要】：磷酸锌具有无毒、环保、分散性好等优点，目前广泛应用于防锈、涂料、微孔材料等领域，随着现代科技的发展，其应用领域亦在不断扩大。本论文尝试使用磷酸锌作为抗紫外、阻燃整理剂，利用微波原位合成法与传统轧焙烘结合，将纳米磷酸锌整理到棉织物上，分别制备具有抗紫外与阻燃作用的棉织物。课题研究的内容主要分三个部分。第一部分研究了利用硝酸锌、醋酸锌、硫酸锌、磷酸二氢钠、磷酸、磷酸氢二铵、尿素、六亚甲基四胺、碳酸胍等为原料，在微波加热的条件下，合成纳米磷酸锌。采用XRD、红外、TG-DTG等测试方法，对产物磷酸锌进行了表征。使用XRD研究了磷酸锌在不同干燥条件下的失水情况，结果表明：80°C干燥条件下得到的是四水合磷酸锌；140°C干燥条件下得到的是四水合磷酸锌与二水合磷酸锌的混合物。第二部分研究了具有抗紫外性能的棉织物的制备。实验中，将棉织物放入含有一定量锌源、磷源及碱剂溶液的三口烧瓶中，80℃条件下微波加热，反应结束后，将棉织物浸轧两次，80℃预烘，140℃焙烘。研究发现：磷酸锌整理后的织物，其UPF值，随Zn2+浓度的增大而增大，随焙烘时间的延长、焙烘温度的升高而增大；但随尿素浓度的提高而降低；而微波反应的温度与时间几乎对其没有明显的影响。未添加尿素整理的织物，虽然具有很好的抗紫外效果，，但其撕破强力很低；通过添加适量的尿素，在保持原有抗紫外性能的同时，还明显提升了织物的撕破强力。抗紫外整理最佳工艺为：Zn2+浓度为0.4mol L-1，尿素浓度为0.7mol L-1，80°C条件下微波加热20min，80°C预烘4分钟，140°C焙烘3分钟。整理后织物UPF值为55.28，与整理前的23.58相比，有了明显的提升；整理后织物的经向撕破强力为1091.01（cN），纬向撕破强力为633.16(cN)，与整理前相比，强力损失很小。第三部分研究了具有阻燃作用的棉织物的制备，实验中，将棉织物放入含有一定量锌源、磷源及碱剂溶液的三口烧瓶中，80℃微波加热反应20min，反应结束后，将棉织物浸轧两次，80℃预烘4min，140℃焙烘3min。研究发现：在不添加尿素时，单独磷酸锌整理后的织物，其阻燃性随Zn2+浓度的增大而增强；添加适量尿素后，织物的阻燃性能获得了进一步的提升，同时也明显提高了织物的撕破强力。TG-DTG分析表明：单独尿素整理的织物几乎没有阻燃作用；在尿素与磷酸锌共同整理的织物中，随尿素浓度增大，整理后织物的起始分解温度和终止分解温度都向高温方向偏移；随Zn2+浓度增大，整理织物的起始分解温度和终止分解温度都向低温方向偏移；与未整理织物相比，整理后织物的起始分解温度、终止分解温度和最大分解速率都有了很大的降低，使织物由高温分解系统转变成了低温分解系统。阻燃最佳工艺为：Zn2+浓度为0.4mol L-1，尿素浓度为1.7mol L-1时，80°C条件下微波加热20min，，80°C预烘4分钟，140°C焙烘3分钟。整理后织物离开火焰后几乎立即熄灭。使用SEM观察整理前后织物的表面形态。结果发现：燃烧测试前，原布表面光滑，并且有一定的扭曲度，燃烧后，其纤维明显变细，扭曲度明显变大，部分纤维甚至发生了断裂；整理后织物的表面均匀分布了较多细小的颗粒，燃烧后，织物表面结构几乎没有发生没变，产生了完整的表面结构。为了测试整理后织物的水洗牢度，将经过洗衣、漂洗、脱水三个过程后的织物，进行了元素分析测试。结果发现，水洗前后，织物上磷酸锌的含量变化不大，说明了磷酸锌与织物的结合比较牢固。最后将充分水洗的织物灼烧完全，进行了XRD测试，结果发现：燃烧后的灰烬为无水磷酸锌。
[Abstract]:Zinc phosphate has the advantages of non-toxic, environmental and good dispersivity. It is widely used in the fields of antirust, coating, microporous materials and so on. With the development of modern science and technology, its application fields are also expanding. This paper tries to use zinc phosphate as anti UV, flame retardant finishing agent, microwave in situ synthesis and traditional rolling roasting, and nano phosphoric acid Zinc finishing was applied to cotton fabrics and cotton fabrics with UV and flame retardant properties were prepared respectively.
The content of the research is divided into three parts. The first part studies the use of zinc nitrate, zinc acetate, zinc sulfate, sodium dihydrogen phosphate, phosphoric acid, diammonium hydrogen phosphate, urea, six methylene four amine, guanidine carbonate, and so on, to synthesize zinc phosphate by microwave heating, using XRD, IR, TG-DTG and so on. The water loss of zinc phosphate under different drying conditions was studied by XRD. The results showed that four hydrated zinc phosphate was obtained under 80 degree C drying condition, and the mixture of four hydrate zinc phosphate and two hydrate zinc phosphate under 140 degree C drying conditions was obtained.
In the second part, the preparation of cotton fabric with anti UV properties was studied. In the experiment, the cotton fabric was placed in three flasks containing a certain amount of zinc source, phosphorus source and alkali solution, microwave heating at 80 degrees centigrade. After the reaction, cotton fabrics were soaked for two times, 80 degrees centigrade and 140 centigrade. The UPF value of the fabric after zinc phosphate treatment was found. With the increase of Zn2+ concentration, it increases with the increase of baking time and baking temperature, but decreases with the increase of urea concentration, but the temperature and time of the microwave reaction almost have no obvious effect on it. The fabric without urea finishing has very good anti UV effect, but its tear strength is very low; The optimum process of anti UV finishing is: Zn2+ concentration is 0.4mol L-1, urea concentration is 0.7mol L-1,80 / C, microwave heating 20min, 80 degree C pre baking for 4 minutes, 140 degree C baking for 3 minutes. The value of UPF value of the finished fabric is 55.28, and before finishing. Compared with 23.58, it has been improved obviously; the warp strength of the finished fabric is 1091.01 (cN) and the weft tear strength is 633.16 (cN), and the strength loss is very small compared with that before the finishing.
In the third part, the preparation of cotton fabric with flame retardancy was studied. In the experiment, the cotton fabric was heated in three flasks containing a certain amount of zinc source, phosphorus source and alkali solution, and 20min was heated by microwave at 80 C. After the reaction, cotton fabric was soaked for two times, 80 centigrade prebaked 4min, and 140 centigrade baking 3min.. The flame retardancy of the fabric treated with zinc phosphate was enhanced with the increase of Zn2+ concentration, and the flame retardancy of the fabric was further enhanced after adding appropriate amount of urea, and the tear strength of the fabric was obviously improved by.TG-DTG analysis. In the fabric, with the increase of urea concentration, the initial decomposition temperature and the termination decomposition temperature of the finished fabric offset to the high temperature direction. With the increase of Zn2+ concentration, the initial decomposition temperature and the termination decomposition temperature of the finished fabric are all offset to the low temperature direction. Compared with the unfinished fabric, the initial decomposition temperature of the finished fabric and the decomposition temperature are terminated. The degree and maximum decomposition rate have been greatly reduced, making the fabric transformed from high temperature decomposition system to low temperature decomposition system. The best flame retardant process is: when the concentration of Zn2+ is 0.4mol L-1 and the urea concentration is 1.7mol L-1, microwave heating 20min under 80 degree C, 80 degree C to bake for 4 minutes and 140 degrees C for 3 minutes. After finishing the fabric, the fabric is almost upright after leaving the flame. That is, to extinguish.
The surface morphology of the fabric before and after the finishing was observed by SEM. It was found that before the combustion test, the surface of the original cloth was smooth and there was a certain distortion. After the combustion, the fiber was obviously thinned, the distortion was obviously larger and some fiber was broken, and the surface of the fabric was evenly distributed more fine particles, after burning, the fabric table was burned. In order to test the washing fastness of the finished fabric, the fabric after three processes of washing, rinsing and dehydrating was tested by elemental analysis. The results showed that the content of zinc phosphate in the fabric changed little before and after washing, indicating the combination of zinc phosphate and fabric. Finally, the water washed fabrics were completely burned and tested by XRD. The results showed that the ashes after burning were anhydrous zinc phosphate.
【学位授予单位】：东华大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ132.41;TB383.1

【参考文献】