万吨级草铵膦中间体甲基亚磷酸二乙酯的工业装置

万吨级草铵膦中间体甲基亚磷酸二乙酯的工业装置李强雷青菊摘要：以三氯化磷为起始原料，生产氯基亚磷酸二乙酯，再与格式试剂发生烷基化反应后，粗品经固液分离，精馏后得到高纯度的甲基亚磷酸二乙酯。

由于大生产装置的安全性、复杂性、环保要求等，致使国内化工装置普遍偏小、简陋、安全隐患突出。

因此，有必要建设万吨级高度安全、自控、环保的大型装置。

Abstract:：with phosphorus trichloride as raw materials, production of chlorine radical phosphorous acid e t hyl ester two, and alkylation reactionwith Grignard reagent, the crude product by the solid-liquid separation,rectified to obtain high purity methyl phosphorous acid ethyl ester two.The production device security, complexity, environmental requirements,resulting in the domestic chemical device generally small, simple, security risks outstanding. Therefore, it is necessary to build large device million ton high security, environmental protection, automatic control.关键词：甲基氯化镁烷基化精馏甲基亚磷酸二乙酯装置生产随着草甘膦与百草枯部分剂型产品的禁用，以及转基因技术的发展，灭生性除草剂草铵膦即将成为全球第一大除草剂。

With the disabled glyphosate and paraquat part product formulations, as well as the development of transgenic technology, herbicide glufosinatewill become the world's first major herbicide.在国内，生产草铵膦所需的原料成本六成以上来自中间体甲基亚磷酸二乙酯。

In China, the production of glufosinate required raw materials cost sixmore than from the intermediate methyl phosphorous acid ethyl ester two.为降低草铵膦的使用成本，迫使厂家不断优化生产工艺，启用新技术新装备，所以降低甲基亚磷酸二乙酯的生产成本尤为关键。

In order to reduce the use cost of glufosinate, forcing manufacturers toconstantly optimize the production process, the opening of the newtechnology and new equipment, so reducing the methyl phosphorous acid ethyl ester two production cost is crucial.一、粗品的合成（1）歧化装置。

来自亚磷酸三乙酯贮罐的三乙酯，经计量后与一定量的溶剂、催化剂进入混合釜，搅拌降温一定时间后，转入歧化釜内。

来自三氯化磷贮罐的三磷经泵打计量后，进入高位槽备用。

歧化装置采用高通量快速反应器，整个歧化反应时间为1小时，保温时间2小时，取样器选用安策管道密封式的，具有安全、简单等优点。

合格后，物料转入烷基化釜备用。

Disproportionation unit. Three ethyl ester from phosphorous acid ethyl ester three tanks, the measurement after with a certain amount ofsolvent, catalyst into the mixing tank, stirring cooling after a certain period of time, to disproportionation reactor. From phosphorus trichloridetank three phosphorus by pump metering, into the high groove standby.Disproportionation unit using high throughput fast reactor, thedisproportionation reaction time 1 hours, 2 hours holding time, the selection of pipeline sampler an CE sealing type, has the advantages ofsafety, simple etc.. After passing the material into the alkylation reactorstandby.（2）格式装置。

来自四氢呋喃贮罐的呋喃与回收的溶剂，经计量后进入格式釜。

由投料仓加入称量准确的镁条，启动搅拌，温度控制温度后，开始通入氯甲烷气体。

Format device. Furan and tetrahydrofuran solvent recovery fromthetank, the measurement into the format kettle.By adding magnesium castsilo weighing, accurate start stirring, temperature control temperature,began to pass into the chlorine methane gas.在冷凝器内部，设计了末端捕集器等构件及外部附件，可以使四氢呋喃的回收率提高5%以上。

与国内其它装置比较，在全部达产的前提下，每月可以节约近200万的四氢呋喃消耗。

In the condenser internal, designed a terminal collector and other components and external accessories, can make the tetrahydrofuranrecovery rate increased more than 5%. Compared with other devices indomestic, all production under the premise, a month can save nearly 2000000 of the tetrahydrofuran consumption.反应合格后，在“赶气”釜内通入惰性气体将残余的氯甲烷“赶走”，保证格式反应的淬灭。

最后将物料转入格式试剂高位槽冷却备用。

整个批次操作时间较长，因此，共设计了20套装置。

The reaction of qualified, in "drive gas" kettle, introducing inert gas into methane chloride "residual away", guarantee format responsequenching. Finally thematerial into the Grignard reagent high slotcooling standby. The whole batch operation time is longer, therefore, a total of 20 sets of device design.为保证装置的安全性与连续性，应设计如下措施：In order to ensure safety and continuity of the device design, the following measures should be:1、氯甲烷通气管道上设计了切断阀。

一旦格式釜压力过高，氯甲烷气体自动停止通气。

1, methane chloride ventilation pipeline design cut off valve. Once theformat pressure is too high, automatic stop aeration chlorine methane gas.2、格式釜的尾气管道上设计了爆破膜片。

2. Tail gas piping format kettle on the design of blasting diaphragm.3、设计了一台5倍格式釜体积的事故应急罐。

一旦格式釜内温度异常时，底部事故排放阀自动开启，釜内物料排放至应急罐内。

3, design the emergency tank a 5 times the volume of the format reactoraccident. Once the temperature in the kettle bottom format when abnormal, accidental discharge valve automatically opens, kettle materialdischarge to the emergency tank.4、现场设计了运行监视屏。

工业机器人可以参与巡回检查。

远程DCS监控与SIS安全防护（嵌入紧急停车按钮）是必不可少的。

4, the site is designed to run the monitor screen. Industrial robots can participatein the tour of inspection. Remote DCS monitoring and SIS security (embeddedin the emergency stop button) is essential.（3）烷基化装置。

打开搅拌并控制好温度后，打开格式试剂高位槽滴加阀门。