納米磷酸鋅微波輔助制備及應(yīng)用
本文選題:磷酸鋅 + 棉織物 ; 參考:《東華大學(xué)》2015年碩士論文
【摘要】:磷酸鋅具有無(wú)毒、環(huán)保、分散性好等優(yōu)點(diǎn),目前廣泛應(yīng)用于防銹、涂料、微孔材料等領(lǐng)域,隨著現(xiàn)代科技的發(fā)展,其應(yīng)用領(lǐng)域亦在不斷擴(kuò)大。本論文嘗試使用磷酸鋅作為抗紫外、阻燃整理劑,利用微波原位合成法與傳統(tǒng)軋焙烘結(jié)合,將納米磷酸鋅整理到棉織物上,分別制備具有抗紫外與阻燃作用的棉織物。 課題研究的內(nèi)容主要分三個(gè)部分。第一部分研究了利用硝酸鋅、醋酸鋅、硫酸鋅、磷酸二氫鈉、磷酸、磷酸氫二銨、尿素、六亞甲基四胺、碳酸胍等為原料,在微波加熱的條件下,合成納米磷酸鋅。采用XRD、紅外、TG-DTG等測(cè)試方法,對(duì)產(chǎn)物磷酸鋅進(jìn)行了表征。使用XRD研究了磷酸鋅在不同干燥條件下的失水情況,結(jié)果表明:80°C干燥條件下得到的是四水合磷酸鋅;140°C干燥條件下得到的是四水合磷酸鋅與二水合磷酸鋅的混合物。 第二部分研究了具有抗紫外性能的棉織物的制備。實(shí)驗(yàn)中,將棉織物放入含有一定量鋅源、磷源及堿劑溶液的三口燒瓶中,80℃條件下微波加熱,反應(yīng)結(jié)束后,將棉織物浸軋兩次,80℃預(yù)烘,140℃焙烘。研究發(fā)現(xiàn):磷酸鋅整理后的織物,其UPF值,隨Zn2+濃度的增大而增大,隨焙烘時(shí)間的延長(zhǎng)、焙烘溫度的升高而增大;但隨尿素濃度的提高而降低;而微波反應(yīng)的溫度與時(shí)間幾乎對(duì)其沒有明顯的影響。未添加尿素整理的織物,雖然具有很好的抗紫外效果,,但其撕破強(qiáng)力很低;通過(guò)添加適量的尿素,在保持原有抗紫外性能的同時(shí),還明顯提升了織物的撕破強(qiáng)力。抗紫外整理最佳工藝為:Zn2+濃度為0.4mol L-1,尿素濃度為0.7mol L-1,80°C條件下微波加熱20min,80°C預(yù)烘4分鐘,140°C焙烘3分鐘。整理后織物UPF值為55.28,與整理前的23.58相比,有了明顯的提升;整理后織物的經(jīng)向撕破強(qiáng)力為1091.01(cN),緯向撕破強(qiáng)力為633.16(cN),與整理前相比,強(qiáng)力損失很小。 第三部分研究了具有阻燃作用的棉織物的制備,實(shí)驗(yàn)中,將棉織物放入含有一定量鋅源、磷源及堿劑溶液的三口燒瓶中,80℃微波加熱反應(yīng)20min,反應(yīng)結(jié)束后,將棉織物浸軋兩次,80℃預(yù)烘4min,140℃焙烘3min。研究發(fā)現(xiàn):在不添加尿素時(shí),單獨(dú)磷酸鋅整理后的織物,其阻燃性隨Zn2+濃度的增大而增強(qiáng);添加適量尿素后,織物的阻燃性能獲得了進(jìn)一步的提升,同時(shí)也明顯提高了織物的撕破強(qiáng)力。TG-DTG分析表明:?jiǎn)为?dú)尿素整理的織物幾乎沒有阻燃作用;在尿素與磷酸鋅共同整理的織物中,隨尿素濃度增大,整理后織物的起始分解溫度和終止分解溫度都向高溫方向偏移;隨Zn2+濃度增大,整理織物的起始分解溫度和終止分解溫度都向低溫方向偏移;與未整理織物相比,整理后織物的起始分解溫度、終止分解溫度和最大分解速率都有了很大的降低,使織物由高溫分解系統(tǒng)轉(zhuǎn)變成了低溫分解系統(tǒng)。阻燃最佳工藝為:Zn2+濃度為0.4mol L-1,尿素濃度為1.7mol L-1時(shí),80°C條件下微波加熱20min,,80°C預(yù)烘4分鐘,140°C焙烘3分鐘。整理后織物離開火焰后幾乎立即熄滅。 使用SEM觀察整理前后織物的表面形態(tài)。結(jié)果發(fā)現(xiàn):燃燒測(cè)試前,原布表面光滑,并且有一定的扭曲度,燃燒后,其纖維明顯變細(xì),扭曲度明顯變大,部分纖維甚至發(fā)生了斷裂;整理后織物的表面均勻分布了較多細(xì)小的顆粒,燃燒后,織物表面結(jié)構(gòu)幾乎沒有發(fā)生沒變,產(chǎn)生了完整的表面結(jié)構(gòu)。為了測(cè)試整理后織物的水洗牢度,將經(jīng)過(guò)洗衣、漂洗、脫水三個(gè)過(guò)程后的織物,進(jìn)行了元素分析測(cè)試。結(jié)果發(fā)現(xiàn),水洗前后,織物上磷酸鋅的含量變化不大,說(shuō)明了磷酸鋅與織物的結(jié)合比較牢固。最后將充分水洗的織物灼燒完全,進(jìn)行了XRD測(cè)試,結(jié)果發(fā)現(xiàn):燃燒后的灰燼為無(wú)水磷酸鋅。
[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.
【學(xué)位授予單位】:東華大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TQ132.41;TB383.1
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