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作 者:刘豆 强西怀 户滢 LIU Dou;QIANG Xi-huai;HU Wing(College of Bioresources Chemical and Materials Engineering,Shaanxi University of Science and Technology,Xi'an 710021,Shaanxi,China;National Demonstration for Experimental Light Chemistry Engineering Education,Xi'an 710021,Shaanxi,China;Key Laboratory of Leather Cleaner Production,China National Light Industry,Xi'an 710021,Shaanxi,China)
机构地区:[1]陕西科技大学轻工科学与工程学院,陕西西安710021 [2]轻化工程国家级实验教学示范中心,陕西西安710021 [3]中国轻工业皮革清洁生产重点实验室,陕西西安710021
出 处:《精细化工》2019年第1期136-141,148,共7页Fine Chemicals
基 金:国家重点研发计划项目(2017YFB0308500);陕西科技大学创新科研团队(TD12-04);陕西科技大学研究生创新基金~~
摘 要:在水为介质的条件下,以三聚氯氰(TCT)与赖氨酸(Lys)为原料,经缩合反应制备N,N?-二-(4,6-二氯-[1,3,5]-三嗪基)-2,6-二氨基己酸(简称DTDHA),利用FTIR和1HNMR对其结构进行了表征。通过正交实验考察了原料物质的量之比、缚酸剂种类、反应时间对产物收率的影响,得出较适宜的反应条件为:n(三聚氯氰)∶n(赖氨酸)=3.0∶1.0,KOH做缚酸剂,反应时间6 h,在该条件下DTDHA产率为91%。并将产物应用于生皮鞣制,以鞣制坯革的收缩温度为考察指标,采用单因素实验对鞣制工艺条件进行了优化。得到适宜的鞣制工艺条件为:鞣剂用量20%(以灰皮质量为基准,下同),温度从25℃开始每隔2 h阶梯上升15℃,最终达到55℃,鞣制总时间8h,在该条件下,坯革的收缩温度为85.6℃。该鞣制工艺下合成产物具有良好的鞣制效应,是一种新型的有机合成鞣剂。N,N’-Bis-(4,6-dichloro-[1,3,5]-triazin-2-yl)-2,6-diaminohexanic acid(DTDHA) was synthesized by condensation reaction of cyanuric chloride(TCT) and lysine(Lys) in the presence of water,and was characterized by FTIR and 1 HNMR.The effects of molar ratio of raw material,type of acid-binding agent and reaction time on the yield of product were investigated by orthogonal experiment.The suitable reaction conditions were obtained as followed:the molar ratio of cyanuric chloride to lysine was 3.0∶1.0,potassium hydroxide was used as acid binding agent,and the reaction time was 6 h.Under these optimized conditions,the yield of product was 91%.The product was then applied to the tanning of raw hides.The single factor test method was used to optimize the technical conditions of the tanning process by using the shrinkage temperature of tanned leather as an inspection index.The results showed that the optimum tanning process conditions were that tanning agent dosage 20%(based on the mass of raw hide,the same below),temperature rising from 25 ℃,stepwise control rising by 15 ℃ every 2 hours,finally reaching to 55 ℃,total tanning time 8 hours.Under the above-mentioned conditions,the shrinkage temperature of crust leather was 85.6 ℃.The synthetic product has a good tanning effect and belongs to a new type of organic synthesis tanning agent.
关 键 词:三聚氯氰 赖氨酸 N N′-二-(4 6-二氯-[1 3 5]-三嗪基)-2 6-二氨基己酸 无铬鞣剂 鞣制 皮革化学品
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