加入收藏| 关于我们 您好,欢迎来到济南金日和化工用品生产厂家,免费售后,欢迎咨询!

全国咨询热线:13386411819
0531-81762771

当前位置:首页>>热门资讯>>技术支持>>硫酸羟胺在纯度制备上的生产研究
联系我们
联系我们

咨询热线:13386411819

QQ:

联系地址:济南市新材料化工市场北区536

硫酸羟胺在纯度制备上的生产研究
来源:http://www.jnjrh.com 日期:2019-10-01 发布人:admin
丁酮肟,纯度99.5%,山东西亚化工有限公司;硫酸,纯度98%,北京化工厂,与去离子水配置成一定浓度的硫酸水溶液;乙醇,纯度 > 99.7%,北京化工厂;氢氧化钠,纯度 > 96%,配置成0.2 mol·L-1的氢氧化钠溶液。紫外分光光度计(岛津公司)用于丈量反响液及馏出液中酮肟含量;智能真空泵(成都气海机电制造有限公司)用于减压反响精馏过程。
Ding Tongwo, the purity is 99.5%, the Western Asia Chemical Co., Ltd., the sulfuric acid, the purity 98%, the chemical factory, and the deionized water is allocated to a certain concentration of sulfuric acid solution; the purity of ethanol is 99.7%, the chemical factory, the sodium hydroxide, the purity > 96%, and the sodium hydroxide solution is 0.2 mol L-1. The ultraviolet spectrophotometer (SHIMADZU) is used to measure the content of ketoxime in the reflux liquid and distillate. The intelligent vacuum pump (Chengdu gas sea electromechanical Manufacturing Co., Ltd.) is used in the vacuum repercussion distillation process.
2 实验步骤
2 experimental steps
为实验工艺流程表示图,其中精馏塔为课题组自行设计组装的填料精馏塔。实验步骤如下:
The distillation column is a packed distillation column designed and assembled by our team. The experimental steps are as follows:
氨基磺酸
(1) 取酮肟和硫酸溶液备用,将硫酸配置成40%(wt) ~60%(wt)的硫酸水溶液;
(1) Ketoxime and sulphuric acid solution were taken for reserve, and sulphuric acid was prepared into 40% (wt) to 60% (wt) sulphuric acid aqueous solution.
(2) 将酮肟、硫酸水溶液按酮肟和H2SO4以一定摩尔比参与到反响釜中,控制反响液温度在80℃左右,经过调理真空度调理上升蒸汽量,从精馏塔塔顶将馏出的酮/水混合物采出,当反响液有硫酸羟胺晶体析出后,将反响液快速过滤,也可将反响液快速降温过滤,过滤后的反响液循环并继续反响;
(2) The ketoxime and sulfuric acid aqueous solution were added into the reactor at a certain molar ratio of ketoxime and H2SO4. The temperature of the reactor was controlled at about 80 C. The rising steam volume was regulated by vacuum. The distilled ketone/water mixture was extracted from the top of the distillation column. When hydroxylamine sulfate crystals were precipitated from the reactor, the reactor was filtered quickly, and the reactor was filtered quickly. The reverberant circulates and continues to reverberate.
(3) 反响终了后将釜液中止降温、结晶、过滤、洗濯、单调后得到硫酸羟胺固体,过滤后的母液可投入下一批反响循环套用;经过对反响液及晶体中止剖析得到硫酸羟胺收率。
(3) After the reaction, hydroxylamine sulfate solids were obtained by stopping and cooling, crystallization, filtration, washing and monotony. The filtered mother liquor could be used in the next batch of reaction cycle. The yield of hydroxylamine sulfate was obtained by discontinuing the analysis of the reaction liquor and crystals.