![2,4-二氯苯氧乙酸连续反应结晶粒度控制方法](/CN/2014/1/93/images/201410468544.jpg)
基本信息:
- 专利标题: 2,4-二氯苯氧乙酸连续反应结晶粒度控制方法
- 专利标题(英):Method for controlling continuous reaction crystal size of 2,4-dichlorphenoxyacetic acid
- 申请号:CN201410468544.0 申请日:2014-09-15
- 公开(公告)号:CN104276944A 公开(公告)日:2015-01-14
- 发明人: 王彦飞 , 沙作良 , 朱亮 , 许史杰 , 黄艳敏 , 杨静 , 刘安平 , 殷宏 , 薛光才 , 刘建华 , 熊金华 , 范文涛
- 申请人: 天津科技大学 , 湖北沙隆达股份有限公司
- 申请人地址: 天津市经济技术开发区第三大街翠亨村C-10-601
- 专利权人: 天津科技大学,湖北沙隆达股份有限公司
- 当前专利权人: 天津科技大学,湖北沙隆达股份有限公司
- 当前专利权人地址: 天津市经济技术开发区第三大街翠亨村C-10-601
- 主分类号: C07C59/70
- IPC分类号: C07C59/70 ; C07C51/02 ; C07C51/43
The invention relates to a method for controlling a continuous reaction crystal size of a herbicide 2,4-dichlorphenoxyacetic acid. The method comprises the following steps: (1) preparing a 80-100 DEG C saturated or nearly saturated solution of a 2,4-dichlorphenoxyacetic acid salt, and 10-38% hydrochloric acid respectively; (2) in a crystallizer, continuously adding the 2,4-dichlorphenoxyacetic acid salt solution and the hydrochloric acid prepared in the step (1), wherein a molar ratio of the 2,4-dichlorphenoxyacetic acid salt to hydrochloric acid is 1 to (1-1.2), controlling the crystallization temperature at 20-60 DEG C, controlling the retention time to 2-10 hours, continuously discharging the material to an after-treatment process to obtain the 2,4-dichlorphenoxyacetic acid product. According to the crystal size control method disclosed by the invention, the 2,4-dichlorphenoxyacetic acid salt is dissolved at a high temperature, the 2,4-dichlorphenoxyacetic acid salt solution and hydrochloric acid are subjected to a continuous reaction crystallization process in the crystallizer at a low temperature, so that the problems that the 2,4-dichlorphenoxyacetic acid product produced by the process of performing acidification reaction at a high temperature and then cooling for crystallizing is low in purity and small in crystal size and easily causes equipment corrosion are solved. The method has the advantages that the prepared produce has a great crystal size and a high purity, energy consumption is low, equipment corrosion is hardly caused, the operation is simplified and the process is easily controlled automatically.
公开/授权文献:
- CN104276944B 2,4-二氯苯氧乙酸连续反应结晶粒度控制方法 公开/授权日:2018-05-01
IPC结构图谱:
C | 化学;冶金 |
--C07 | 有机化学 |
----C07C | 无环或碳环化合物 |
------C07C59/00 | 羧基连接在非环碳原子上的化合物,含羟基(—OH)、氧—金属基、醛基(—CHO)、酮基、醚基、COOC基、COOCOC基或COOCOCOC基中任何基团的化合物 |
--------C07C59/01 | .只有1个羧基和含有羟基或氧—金属基的饱和化合物 |
----------C07C59/42 | ..含羟基或氧—金属基 |
------------C07C59/64 | ...含六元芳环 |
--------------C07C59/66 | ....醚的无羧基部分含六元芳环 |
----------------C07C59/68 | .....醚基的氧原子连接非稠合六元芳环 |
------------------C07C59/70 | ......羟基乙酸的醚 |