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低能耗制备硫酸羟胺的生产工艺特性
来源:http://www.jnjrh.com 日期:2019-10-01 发布人:admin
硫酸羟胺( (NH2OH)2·H2SO4)作为一种重要的化工中间体,主要用于合成抗癌药(羟基脲)、磺胺类药(新诺明)和农药(灭多威),有着很大的市场需求量及普遍的应用价值[1]。目前,硫酸羟胺传统消费工艺主要有硝基甲烷道路、自然气硝化法、二磺酸铵盐水解法、一氧化氮催化复原道路[5]以及酮肟水解道路,各工艺优缺陷如下:
Hydroxylamine sulphate ((NH2OH) 2. H2SO4), as an important chemical intermediate, is mainly used for the synthesis of anticancer drugs (Qiang Jiniao), sulfonamides (sulfamethoxazole) and pesticide (Do-win), which has great market demand and universal application value [1]. At present, the traditional consumption processes of hydroxylamine sulfate mainly include nitromethane road, natural gas nitration, ammonium disulfonate hydrolysis, nitric oxide catalytic recovery road [5] and ketoxime hydrolysis road. The advantages and disadvantages of each process are as follows:
随着化工行业对消费平安、产质量量请求及环保认识的进步,传统消费工艺中存在的弊端愈创造显,肟水解法近年来遭到研讨者的关注。
With the progress of the chemical industry's understanding of safety of consumption, quality of production and environmental protection, the drawbacks of traditional consumption process are more and more obvious. Oxime hydrolysis method has attracted the attention of researchers in recent years.
氨基磺酸
第一次细致报道了丙酮肟水解反响制备盐酸盐;但酮肟水解反响是典型的受热力学限制的反响,其均衡转化率普通只要10%~20%,需求经过将反响—别离和反响—结晶耦合技术对过程停止强化,移除生成的酮与硫酸羟胺,突破热力学均衡限制,进步反响转化率。
The reaction of acetone oxime hydrolysis to prepare hydrochloride is reported in detail for the first time. However, the reaction of ketone oxime hydrolysis is a typical reaction restricted by thermodynamics. Its equilibrium conversion rate is usually only 10%~20%. It is necessary to stop the process by coupling reaction-separation and reaction-crystallization technology, remove the ketone and hydroxylamine sulfate produced, break through the thermodynamic equilibrium restriction and improve the reaction conversion rate.
反响—别离耦合强化技术主要有离子交流、反响—萃取[8]、反响—蒸馏、反响—精馏、反响—吸收、反响—降解、反响—结晶、反响—膜别离[应用反响—精馏耦合方式制备羟胺盐,但所用硫酸浓度较低,大量水的充裕直接招致精馏能耗及废水排放增加。
Reaction-separation coupling technology mainly includes ion exchange, reaction-extraction [8], reaction-distillation, reaction-distillation, reaction-absorption, reaction-degradation, reaction-crystallization, reaction-membrane separation [hydroxylamine salt is prepared by reaction-distillation coupling method, but the concentration of sulfuric acid used is low, abundant water directly leads to the increase of distillation energy consumption and wastewater discharge.
为进一步降低硫酸羟胺消费能耗及废水排放量,针对肟水解制备羟胺盐中反响液中含水量较大这一问题,本文经过计算不同硫酸浓度下酮肟水解在一定转化率下理论剩余水量及生成硫酸羟胺质量,并分离常压下硫酸羟胺在水中的溶解度的测定结果,提出将反响—精馏与反响—结晶两种反响别离技术耦合用于酮肟水解制备硫酸羟胺工艺,经过将产物硫酸羟胺以及副产物酮的连续原位移出以进步反响转化率,同时防止反响液因黏渡过高而影响传质和传热,避免部分过热,防止副反响发作,完成高浓度硫酸反响体系下制备硫酸羟胺。同时本文调查了不同酸肟比及初始参加硫酸浓度对工艺影响。
In order to further reduce the consumption of hydroxylamine sulfate and the discharge of wastewater, aiming at the problem of high water content in the reaction liquid of hydroxylamine sulfate prepared by oxime hydrolysis, this paper calculates the theoretical residual water volume and the quality of hydroxylamine sulfate produced by ketoxime hydrolysis at a certain conversion rate under different sulfuric acid concentration, and separates the determination results of the solubility of hydroxylamine sulfate in water under normal pressure, and puts forward the idea of reflex-refining. The reaction separation technology of distillation and reaction-crystallization was coupled to prepare hydroxylamine sulfate by hydrolysis of ketoxime. The reaction conversion rate was improved by moving the product hydroxylamine sulfate and by-product ketone in situ continuously. At the same time, the reaction fluid was prevented from affecting mass transfer and heat transfer due to excessive viscosity, partial overheating was avoided, and side reaction occurred. The hydroxyl sulfate was prepared in high concentration sulfuric acid reaction system. Amine. At the same time, the effects of acid oxime ratio and initial concentration of sulfuric acid on the process were investigated.