The invention discloses a preparation process of an industrial grade pure ammonium bromide, which belongs to the field of inorganic synthesis. The following steps are as follows: (1) preparation of ammonium bromide aqueous solution, adding deionized water into the ammonium bromide reaction kettle, opening the ammonium bromide solution circulation pump to cycle, controlling the ammonia valve to make the temperature not more than 50, and adding bromine when the pH value reaches 9.5, and keeping the pH value of the solution in the ammonium bromide reactor 8 to 8.5, and the temperature is not super. The solution of ammonium bromide was obtained at 60 C; (2) the solution of ammonium bromide was purified and the discharge valve was opened, and the ammonium bromide solution was purified by the granular activated carbon filter and then concentrated in the flash concentration tank. (3) the pure ammonium bromide was prepared, and the concentrated crystallization liquid was separated into the centrifuge for solid-liquid separation, and then the crystal of ammonium bromide was obtained and then dried. Dry, good grade pure ammonium bromide finished product. The preparation method of advanced grade ammonium bromide is advanced, and has the advantages of large yield, high purity and low production cost, and is suitable for industrial production.
【技术实现步骤摘要】
一种工业化优级纯溴化铵的制备工艺
本专利技术属于无机合成领域,尤其是一种工业化优级纯溴化铵的制备工艺。
技术介绍
溴化铵是一种用途较为广泛的精细化学品,在感光工业上用作照相胶片、相纸和感光乳化剂,在分析化学中用于滴定分析铜的化学分析试剂,在木材工业用作木材防火剂,在医药上用作镇静剂,是神经衰弱及癫痫等的口服药。制备溴化铵的方法很多,可用试级剂溴氢酸与碳酸氢铵合成试剂级和照像用的溴化铵,也可以用工业溴素、工业尿素、工业级碳酸氢铵“一步法”生产试剂级和照像用的溴化铵,但这些方法都难以生产优级纯的溴化铵,而在制药行业却需要使用优级纯的溴化铵。专利201310279842公开了一种优级纯溴化铵的制备方法,该方法包括将蒸馏水放入塑料桶中,通入氨气制得氨水;将溴素在慢慢搅拌下加入制得的氨水中,然后继续通入氨气至PH=7-8,为反应终点,得到澄清溶液;将澄清溶液加热浓缩至一定密度然后通过离心机趁热过滤,得到溴化铵晶体;将得到的溴化铵进行干燥,得到优级纯成品。根据比较,本专利与上述专利文献有较大区别。
技术实现思路
本专利技术的目的在于克服现有技术不足,根据上述
技术介绍
所描述的技术问题,提供一种工艺步骤简单、生产效率高、杂质含量低、纯度高的工业化优级纯溴化铵的制备工艺。本专利技术实现目的技术方案是:一种工业化优级纯溴化铵的制备工艺,包括如下步骤:(1)制备溴化铵水溶液将定量去离子水打入溴化铵反应釜中,然后开启溴化铵溶液循环泵开始进行循环,循环2-5分钟后再开启冷却水和通氨阀门,通过通氨阀门的开启度来控制溴化铵反应釜在测温仪的温度显示数值不超过50℃,当溴化铵反应釜在PH计显示 ...
【技术保护点】
1.一种工业化优级纯溴化铵的制备工艺,其特征在于,步骤如下:(1)制备溴化铵水溶液将定量去离子水打入溴化铵反应釜中,然后开启溴化铵溶液循环泵开始进行循环,循环2‑5分钟后再开启冷却水和通氨阀门,通过通氨阀门的开启度来控制溴化铵反应釜在测温仪的温度显示数值不超过50℃,当溴化铵反应釜在PH计显示PH值达到9.5时开始加入溴素,控制通溴阀门的开度大小,使得溴化铵反应釜中溶液PH值保持在8.0‑8.5,温度不超过60℃,便得到溴化铵水溶液;(2)提纯溴化铵溶液当溴化铵水溶液含量达到要求浓度后,打开出料阀,并控制一定开度,使溴化铵水溶液先通过颗粒活性炭滤芯进行纯化,除去可能存在的溴酸盐、次溴酸盐等,然后再进入闪蒸浓缩罐中进行浓缩结晶;(3)制得优级纯溴化铵当闪蒸浓缩罐中出现大量结晶时,停止浓缩,将浓缩液放入离心机中进行固液分离,得到溴化铵晶体,再将溴化铵晶体进行干燥,得到优级纯溴化铵成品。
【技术特征摘要】
1.一种工业化优级纯溴化铵的制备工艺,其特征在于,步骤如下:(1)制备溴化铵水溶液将定量去离子水打入溴化铵反应釜中,然后开启溴化铵溶液循环泵开始进行循环,循环2-5分钟后再开启冷却水和通氨阀门,通过通氨阀门的开启度来控制溴化铵反应釜在测温仪的温度显示数值不超过50℃,当溴化铵反应釜在PH计显示PH值达到9.5时开始加入溴素,控制通溴阀门的开度大小,使得溴化铵反应釜中溶液PH值保持在8.0-8.5,温度不超过60℃,便得到溴化铵水溶液;(2)提纯溴化铵溶液当溴化铵水溶...
【专利技术属性】
技术研发人员:李迎辉,司林杰,高国杰,肖克强,李迎森,
申请(专利权)人:山西同杰化学试剂有限公司,
类型:发明
国别省市:山西,14
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