无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ
工业技术

微反应制备三氯化磷研究

  • 陈韬 ,
  • 高慧敏
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  • 1.云南招标股份有限公司, 云南 昆明 650032
    2.昆明理工大学, 云南 昆明 650031
    3.云南云天化以化磷业研究技术有限公司, 云南 昆明 650028
陈韬(1977— ),男,硕士,工程师,主要研究方向为化工工艺及节能减排技术;E-mail:14425510@qq.com

收稿日期: 2022-06-21

  网络出版日期: 2023-04-13

Study on preparation of phosphorus trichloride by microreaction

  • CHEN Tao ,
  • GAO Huimin
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  • 1. Yunnan Tendering Co. ,Ltd. ,Kunming 650032,China
    2. Kunming University of Science and Technology,Kunming 650031,China
    3. Yunnan ICL YTH Phosphate Research and Technology Center Co. ,Ltd. ,Kunming 650028,China

Received date: 2022-06-21

  Online published: 2023-04-13

摘要

针对传统三氯化磷生产存在工艺控制复杂、安全性差、对设备腐蚀严重等问题,研究了一种以黄磷和液氯为原料,通过微反应技术直接合成三氯化磷的新方法。该方法通过使用微反应技术对反应的影响因素实现精确控制,来保证磷氯的瞬间混合和高效的传质传热,从而达到在反应安全可控的条件下大幅提高反应速率的目标。对反应物料配比、温度、停留时间、回流比等因素进行了单因素条件实验,得到磷氯配料比为0.35∶1(质量比)、反应环境介质温度为75 ℃、反应停留时间为60 s和回流比为2是比较适宜的条件。新方法将反应停留时间缩短至60 s,而且收率达到90%以上,产品质量满足优级品标准,并且可以实现产品的安全、连续化生产。

关键词: 三氯化磷; 黄磷; ; 微反应

本文引用格式

陈韬 , 高慧敏 . 微反应制备三氯化磷研究[J]. 无机盐工业, 2023 , 55(4) : 72 -75 . DOI: 10.19964/j.issn.1006-4990.2022-0379

Abstract

In view of the problems of traditional phosphorus trichloride production,such as complex process control,poor safety and serious corrosion to equipment,a new method for directly synthesizing phosphorus trichloride by micro reaction technology was studied by using yellow phosphorus and liquid chlorine as raw materials.The influencing factors could be accurately controlled by using micro-reaction technology in this method to ensure the instantaneous mixing of phosphorus and chlorine and efficient mass and heat transfer,so as to achieve the goal of getting greatly increased reaction rate under safe and controllable reaction conditions.The single factor condition experiments were carried out on factors such as reaction material ratio,temperature,residence time,reflux ratio,etc.The preferable conditions were the ratio of phosphorus and chlorine of 0.35∶1,the ambient medium temperature of 75 ℃,the reaction residence time of 60 s and the reflux ratio of 2.The new method shortened the reaction residence time to 60 s,and the yield reached more than 90%,the product quality met the standard of premium product and the safe and continuous production of the product could be realized.

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