CN102234292B - 敌百虫提纯工艺 - Google Patents

敌百虫提纯工艺 Download PDF

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CN102234292B
CN102234292B CN 201010160539 CN201010160539A CN102234292B CN 102234292 B CN102234292 B CN 102234292B CN 201010160539 CN201010160539 CN 201010160539 CN 201010160539 A CN201010160539 A CN 201010160539A CN 102234292 B CN102234292 B CN 102234292B
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trichlorphon
drying
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CN102234292A (zh
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肖尚发
胥敏一
李永
滕军
陈亮
孙奇峰
王峰
李晓竞
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Shandong Dacheng Biological Chemical Co Ltd
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Abstract

本发明涉及一种敌百虫提纯新工艺，其特征在于以敌百虫原药为溶质，以三氯乙烯为溶剂，经混合、溶解、重结晶、过滤、干燥后制得精制敌百虫。过滤后的滤液可用来进行加碱处理，用来生产敌敌畏。本发明使得敌百虫的含量提高，含量提高以后其价格也相应提升，溶剂也可以回收利用，采用三氯乙烯作为溶剂敌百虫的收率可以达到80％以上。为公司带来了良好的经济效益；过滤后的滤液可用来进行加碱处理，制作敌敌畏，大大提高了敌百虫的利用率。

Description

敌百虫提纯工艺
技术领域
本发明涉及一种敌百虫提纯新工艺，术语农药化工领域。 
技术背景
敌百虫，化学名称：O，O-二甲基-(2，2，2-三氯-1-羟基乙基)磷酸酯。 
英文名称：O，O-Dimethyl-(2，2，2-trichloro-1-hydroxhethyl-)phosohonate， 
分子式：C4H8O4PCl3
结构式： 
Figure GDA0000021022410000011
分子量：257.43。纯品敌百虫在常温下为白色结晶粉末，具有芳香气味，熔点83～84℃，密度1.73(20℃)，10％的水溶液折光率为1.3439，蒸气压7.8μPa(20℃)。挥发度极小，在20℃时为0.11毫克/米。敌百虫易溶于水，在25℃时100毫升可溶解15.4克。温度升高，敌百虫在水中的溶解度增大。25℃时在有机溶剂中溶解度为：正己烷0.08克/100毫升；乙醚17.0克/100毫升；三氯甲烷75克/100毫升；苯15.2克/100毫升。 
工业品敌百虫为白色或淡黄色结晶固体，工业品有氯醛气味，熔点78～80℃。 
敌百虫广泛用于农业、园艺、森林、畜牧以及家庭和环境卫生等方面。对多种害虫有较好的防治作用。 
同行业中敌百虫的提纯工艺均采用水作为溶剂，收率不高，一股在65％～70％。 
发明内容
本发明要解决的技术问题是：提供一种敌百虫提纯新工艺，使敌百虫的纯度大幅提高，提升其价值，溶剂也可以回收利用。 
本发明解决其技术问题所采用的技术方案是：提供一种敌百虫提纯新工艺，其特征在于以敌百虫原药为溶质，以三氯乙烯为溶剂，经混合、溶解、重结晶、过滤、干燥后制得精制敌百虫。 
所述的敌百虫原药与三氯乙烯的质量比为1∶0.8～1.5。 
所述的重结晶温度为15～22℃。 
所述的过滤后的滤液可用来进行加碱处理，用来生产敌敌畏。 
所述的干燥温度为35～55℃，干燥时间为5～15min。 
本发明所具有的有益效果是：本发明使得敌百虫的含量提高，含量提高以后其价格也相应提升，溶剂也可以回收利用，采用三氯乙烯作为溶剂敌百虫的收率可以达到80％以上，为公司带来了良好的经济效益；过滤后的滤液可用来进行加碱处理，制作敌敌畏，大大提高了敌百虫的利用率。 
具体实施方式
实施例1 
投1000kg三氯乙烯到结晶釜，开启搅拌到高速状态；加入含量为90％液体敌百虫800kg；开结晶釜夹套蒸汽，将混合物料温度升高至60℃；半小时后，开启夹套冷却水，缓慢降低物料温度；降至30℃时，开始结晶，观察釜内物料开始发白；2h后，温度降至15℃时，关闭夹套冷却水；将过滤机定位到过滤状态，调节结晶釜搅拌速度至低速状态；开启打料泵将物料打入过滤机；开启抽滤真空泵，将滤液抽滤完毕，所得滤液重量为1050g；开启过滤机出料阀，将滤饼倒入加料器；开启干燥机、热水系统、加料器，调节干燥速度，控制干燥温度为35℃，对滤饼进行干燥，干燥回收三氯乙烯86kg；干燥机排出的敌百虫称重为615kg，分析含量为98.1％，所得敌百虫达到优等品标准，其收率为83.8％。滤液用蒸汽加热增浓回收三氯乙烯515kg，增浓后的滤液送敌敌畏工序副产敌敌畏102kg。 
实施例2 
投1000g三氯乙烯到结晶釜，开启搅拌到高速状态；加入含量为89.6％液体敌百虫1000kg；开结晶釜夹套蒸汽，将混合物料温度升高至60℃；半小时后，开启夹套冷却水，缓慢降低物料温度；降至30℃时，开始结晶，观察釜内物料开始发白；2h后，温度降至18℃时，关闭夹套冷却水；将过滤机定位到过滤状态，调节结晶釜搅拌速度至低速状态；开启打料泵将物料打入过滤机；开启抽滤真空泵，将滤液抽滤完毕，所得滤液重量为1210kg；开启过滤机出料阀，将滤饼倒入加料器；开启干燥机、热水系统、加料器，调节干燥速度，控制干燥温度为45℃，对滤饼进行干燥，干燥回收三氯乙烯91kg；干燥机排出的敌百虫称重为758kg，分析含量为98.5％，所得敌百虫达到优等品标准，其收率为83.3％。滤液用蒸汽加热增浓回收三氯乙烯554kg，增浓后的滤液送敌敌畏工序副产敌敌畏148kg。 
实施例3 
投1000kg三氯乙烯到结晶釜，开启搅拌到高速状态；加入含量为90.2％液体敌百虫1500kg；开结晶釜夹套蒸汽，将混合物料温度升高至60℃；半小时后，开启夹套冷却水，缓慢降低物料温度；降至30℃时，开始结晶，观察釜内物料开始发白；2h后，温度降至22℃ 时，关闭夹套冷却水；将过滤机定位到过滤状态，调节结晶釜搅拌速度至低速状态；开启打料泵将物料打入过滤机；开启抽滤真空泵，将滤液抽滤完毕，所得滤液重量为1164kg；开启过滤机出料阀，将滤饼倒入加料器；开启干燥机、热水系统、加料器，调节干燥速度，控制干燥温度为55℃，对滤饼进行干燥，干燥回收三氯乙烯84kg；干燥机排出的敌百虫称重为1138kg，分析含量为97.6％，所得敌百虫达到优等品标准，其收率为82.1％。滤液用蒸汽加热增浓回收三氯乙烯499kg，增浓后的滤液送敌敌畏工序副产敌敌畏116kg。 

Claims (2)

1.一种敌百虫提纯工艺，其特征在于以敌百虫原药为溶质，以三氯乙烯为溶剂，经混合、溶解、重结晶、过滤、干燥后制得精制敌百虫；敌百虫原药与三氯乙烯的质量比为1：0.8～1.5；重结晶温度为15～22℃。 
2.根据权利要求1所述的敌百虫提纯工艺，其特征在于干燥温度为35～55℃，干燥时间为5～15min。 
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SU586180A1 (ru) * 1975-05-12 1977-12-30 Предприятие П/Я А-7411 Способ получени смачивающегос порошка хлорофоса
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DD290890A5 (de) * 1984-05-08 1991-06-13 Fettchemie Karl-Marx-Stadt,De Gewinnung von hochwirksamen trichlorphon
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