本文主要研究内容
作者牛芊(2019)在《相转移催化制备5-硝基愈创木酚钠及工程数据的测定》一文中研究指出:中国作为农业大国,怎样在单位土地面积上提高农作物产量的话题一直备受关注,在生态环保的理念下促进作物新陈代谢、增强植物免疫力、提高作物产品质量就成了突出问题。因此,研究并发展毒性低、效率高的新型植物生长调节剂就至关重要。新型植物生长调节剂复硝酚钠具有低毒、高效、无残留、无公害等特点,可以广泛应用于农作物的整个生命周期,其最主要的成分是5-硝基愈创木酚钠。本文选用三步反应法合成5-硝基愈创木酚钠:将愈创木酚经乙酰化、硝化和水解来得到目的产物。对合成工艺中水解反应时,相转移催化剂的使用进行了研究考察,并测定了5-硝基愈创木酚钠的工程数据。首先,用更安全的浓硝酸替换发烟硝酸同冰乙酸混合作为硝化剂,制备水解反应所需原料5-硝基乙酰愈创木酚,并采用单因素法和正交试验设计探索乙酰愈创木酚硝化反应的最优化方案:乙酰愈创木酚与硝酸的摩尔配比为1:8.1,乙酰愈创木酚与冰乙酸的摩尔配比为1:6.4,硝酸用量35 mL、冰乙酸用量35 mL、反应温度50℃、反应时间2.0 h,受硝酸浓度的限制,5-硝基乙酰愈创木酚产率最高仅可达35.37%,纯度为93.09%。提高了实验的安全性,减小了使用发烟硝酸产生危险的概率。第二步,从常见的聚醚类和季铵盐类相转移催化剂中,筛选出了4000目聚乙二醇,促进了水解反应的有效进行,并通过响应面分析法确定了以5-硝基愈创木酚钠的产率为响应值的较佳反应条件为:催化剂用量为水解原料5-硝基乙酰愈创木酚质量的7%、反应温度42.16℃、反应时间为2.52 h。在上述条件下,5-硝基愈创木酚钠的产率达91.36%。然后,对5-硝基愈创木酚钠的工程数据进行了测定。使用汽液双循环釜法(ROSE)测定了制备5-硝基愈创木酚钠过程中涉及到的愈创木酚+乙酰愈创木酚二元物系在压力为13.50(±0.5)kPa时的汽液平衡数据,用Aspen Plus流程模拟软件对实测数据进行模拟,结果表明NRTL、UNIQUAC和Wilson三种溶液模型均可以用来预测愈创木酚+乙酰愈创木酚二元物系的汽液平衡数据。最后,用热分析仪(DSC和TG-DTA)考察了5-硝基愈创木酚钠的非等温热分解现象,并用Flynn–Wall–Ozawa(FWO),Kissinger和?atava-?esták三种热分析方法对5-硝基愈创木酚钠扫描数据进行数学分析,确定出该物质的非等温热分解的机理,其机理函数的积分形式为:g(α)=[-ln(1-α)]2,同时根据热力学性质的计算原理,计算得到5-硝基愈创木酚钠热分解反应过程中的活化能E=0.1448 kJ·mol-1,指前因子的对数lgAk=13.91 min-1,焓变ΔH≠、熵变ΔS≠和吉布斯自由能变ΔG≠分别为-5.079 kJ·mol-1,1.136 J·mol-1·K-1和708.404 kJ·mol-1。用氧弹量热仪测定并计算出5-硝基愈创木酚钠的标准摩尔燃烧焓4719.10 kJ·mol-1、标准摩尔生成焓8331.21 kJ·mol-1。用DSC热分析仪测定了温度在295.15-433.15 K范围内的比热容,并根据扫描数据用最小二乘法进行回归计算得到5-硝基愈创木酚钠的比热容与温度间的关系式为:Cp/J·mol-1·K-1=0.1060T+53.8477,(R2=0.9993)。以上研究填补了5-硝基愈创木酚钠在工程数据方面的空白,为工业化应用发展奠定了基础。
Abstract
zhong guo zuo wei nong ye da guo ,zen yang zai chan wei tu de mian ji shang di gao nong zuo wu chan liang de hua ti yi zhi bei shou guan zhu ,zai sheng tai huan bao de li nian xia cu jin zuo wu xin chen dai xie 、zeng jiang zhi wu mian yi li 、di gao zuo wu chan pin zhi liang jiu cheng le tu chu wen ti 。yin ci ,yan jiu bing fa zhan du xing di 、xiao lv gao de xin xing zhi wu sheng chang diao jie ji jiu zhi guan chong yao 。xin xing zhi wu sheng chang diao jie ji fu xiao fen na ju you di du 、gao xiao 、mo can liu 、mo gong hai deng te dian ,ke yi an fan ying yong yu nong zuo wu de zheng ge sheng ming zhou ji ,ji zui zhu yao de cheng fen shi 5-xiao ji yu chuang mu fen na 。ben wen shua yong san bu fan ying fa ge cheng 5-xiao ji yu chuang mu fen na :jiang yu chuang mu fen jing yi xian hua 、xiao hua he shui jie lai de dao mu de chan wu 。dui ge cheng gong yi zhong shui jie fan ying shi ,xiang zhuai yi cui hua ji de shi yong jin hang le yan jiu kao cha ,bing ce ding le 5-xiao ji yu chuang mu fen na de gong cheng shu ju 。shou xian ,yong geng an quan de nong xiao suan ti huan fa yan xiao suan tong bing yi suan hun ge zuo wei xiao hua ji ,zhi bei shui jie fan ying suo xu yuan liao 5-xiao ji yi xian yu chuang mu fen ,bing cai yong chan yin su fa he zheng jiao shi yan she ji tan suo yi xian yu chuang mu fen xiao hua fan ying de zui you hua fang an :yi xian yu chuang mu fen yu xiao suan de ma er pei bi wei 1:8.1,yi xian yu chuang mu fen yu bing yi suan de ma er pei bi wei 1:6.4,xiao suan yong liang 35 mL、bing yi suan yong liang 35 mL、fan ying wen du 50℃、fan ying shi jian 2.0 h,shou xiao suan nong du de xian zhi ,5-xiao ji yi xian yu chuang mu fen chan lv zui gao jin ke da 35.37%,chun du wei 93.09%。di gao le shi yan de an quan xing ,jian xiao le shi yong fa yan xiao suan chan sheng wei xian de gai lv 。di er bu ,cong chang jian de ju mi lei he ji an yan lei xiang zhuai yi cui hua ji zhong ,shai shua chu le 4000mu ju yi er chun ,cu jin le shui jie fan ying de you xiao jin hang ,bing tong guo xiang ying mian fen xi fa que ding le yi 5-xiao ji yu chuang mu fen na de chan lv wei xiang ying zhi de jiao jia fan ying tiao jian wei :cui hua ji yong liang wei shui jie yuan liao 5-xiao ji yi xian yu chuang mu fen zhi liang de 7%、fan ying wen du 42.16℃、fan ying shi jian wei 2.52 h。zai shang shu tiao jian xia ,5-xiao ji yu chuang mu fen na de chan lv da 91.36%。ran hou ,dui 5-xiao ji yu chuang mu fen na de gong cheng shu ju jin hang le ce ding 。shi yong qi ye shuang xun huan fu fa (ROSE)ce ding le zhi bei 5-xiao ji yu chuang mu fen na guo cheng zhong she ji dao de yu chuang mu fen +yi xian yu chuang mu fen er yuan wu ji zai ya li wei 13.50(±0.5)kPashi de qi ye ping heng shu ju ,yong Aspen Plusliu cheng mo ni ruan jian dui shi ce shu ju jin hang mo ni ,jie guo biao ming NRTL、UNIQUAChe Wilsonsan chong rong ye mo xing jun ke yi yong lai yu ce yu chuang mu fen +yi xian yu chuang mu fen er yuan wu ji de qi ye ping heng shu ju 。zui hou ,yong re fen xi yi (DSChe TG-DTA)kao cha le 5-xiao ji yu chuang mu fen na de fei deng wen re fen jie xian xiang ,bing yong Flynn–Wall–Ozawa(FWO),Kissingerhe ?atava-?estáksan chong re fen xi fang fa dui 5-xiao ji yu chuang mu fen na sao miao shu ju jin hang shu xue fen xi ,que ding chu gai wu zhi de fei deng wen re fen jie de ji li ,ji ji li han shu de ji fen xing shi wei :g(α)=[-ln(1-α)]2,tong shi gen ju re li xue xing zhi de ji suan yuan li ,ji suan de dao 5-xiao ji yu chuang mu fen na re fen jie fan ying guo cheng zhong de huo hua neng E=0.1448 kJ·mol-1,zhi qian yin zi de dui shu lgAk=13.91 min-1,han bian ΔH≠、shang bian ΔS≠he ji bu si zi you neng bian ΔG≠fen bie wei -5.079 kJ·mol-1,1.136 J·mol-1·K-1he 708.404 kJ·mol-1。yong yang dan liang re yi ce ding bing ji suan chu 5-xiao ji yu chuang mu fen na de biao zhun ma er ran shao han 4719.10 kJ·mol-1、biao zhun ma er sheng cheng han 8331.21 kJ·mol-1。yong DSCre fen xi yi ce ding le wen du zai 295.15-433.15 Kfan wei nei de bi re rong ,bing gen ju sao miao shu ju yong zui xiao er cheng fa jin hang hui gui ji suan de dao 5-xiao ji yu chuang mu fen na de bi re rong yu wen du jian de guan ji shi wei :Cp/J·mol-1·K-1=0.1060T+53.8477,(R2=0.9993)。yi shang yan jiu tian bu le 5-xiao ji yu chuang mu fen na zai gong cheng shu ju fang mian de kong bai ,wei gong ye hua ying yong fa zhan dian ding le ji chu 。
论文参考文献
论文详细介绍
论文作者分别是来自郑州大学的牛芊,发表于刊物郑州大学2019-07-03论文,是一篇关于硝基愈创木酚钠论文,相转移催化剂论文,汽液平衡论文,非等温热分解动力学论文,热力学性质论文,郑州大学2019-07-03论文的文章。本文可供学术参考使用,各位学者可以免费参考阅读下载,文章观点不代表本站观点,资料来自郑州大学2019-07-03论文网站,若本站收录的文献无意侵犯了您的著作版权,请联系我们删除。
标签:硝基愈创木酚钠论文; 相转移催化剂论文; 汽液平衡论文; 非等温热分解动力学论文; 热力学性质论文; 郑州大学2019-07-03论文;