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 from

thetank, 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。