研究优化电解还原对硝基苯胂酸(p-A)合成对氨基苯胂酸(p-ASA)的工艺条件.实验表明:硫酸浓度、添加剂量、反应温度、投料量等工艺参数对合成产率有显著影响.初步得出比较适宜的电解合成条件为:硫酸浓度10%(bymass,下同)、添加剂量1%(bymass)NaCl、反应温度80℃、投料量71.4g/L、电流密度10A·dm-2.在上述工艺条件下,电解合成产率可达65.8%.
The electrochemical reduction of p-nitrophenyl arsonit acid to p-aminobenzenearsenic acid was studied using controlled-current electrolysis.The results showed that the yield of p-aminobenzenearsenic acid was determinated by the following factors:the concentrations of sulphuric acid,the amount of additive,temperature and the concentrations of p-nitrophenyl arsenic acid.The optimum electrolytic conditions were obtained to be is 10% H2SO4,1% NaCl,80 ℃,25 g/350 mL p-nitrophenyl arsenic acid and 10 A·dm-2.The yield of arsanilic acid could be reached 64.7% under the optimum electrolytic conditions.
[1]Guo Xiaozhong(郭效忠),Liu Tianyu(刘天余).The research process of nutrition effect of organic arsenical on livestock and birds[J].Feed Reseach(饲料研究),2000,(10)1:15-17.
[2]Qiu yixiu(邱亦秀).The application of organic arsenical in feed industry[J].Jiangxi Feed(江西饲料),2006,(5):3-4,13.
[3]http://www.chemyq.com/xz/xz11/101312otdff.htm.
[4]Wang zhifeng(王志峰).The use and production of ar-sanilic acid[J].Si Chuan Hua Gong Yu Fu Shi Kong Zhi(四川化工与腐蚀控制),1998,4(1):34-36.
[5]Zhong guoqing(钟国清).Synthesize and application of organic arsenical feed additive[J].Feed Industry(饲料工业),1995,16(7):27-28.
[6]Hermann Hoffmann,Harry E Creen.Production of arsa-nilic acid:US,3763201[P].1973.
[7]Lu Guiqing(卢桂琴),Hong zehu(洪泽湖),Tao Xian-jian(陶贤鉴),et al.The preparation of para-amino-benzenearsenic acid by solvent process[J].Hunan Chemical Industry(湖南化工).1998,28(2):23-24.
[8]Ma Chun-an(马淳安).Introduction to synthetic organ-ic electrochemistry[M].Beijing:Science Press,2002.