CN104529846A - Method for increasing yield of produced methomyl - Google Patents
Method for increasing yield of produced methomyl Download PDFInfo
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- CN104529846A CN104529846A CN201410819834.5A CN201410819834A CN104529846A CN 104529846 A CN104529846 A CN 104529846A CN 201410819834 A CN201410819834 A CN 201410819834A CN 104529846 A CN104529846 A CN 104529846A
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- methomyl
- aqueous solution
- yield
- producing
- filtration
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Abstract
The invention provides a method for increasing yield of produced methomyl. The method comprises the steps of reacting by virtue of methomyl oxime and methyl isocyanate to prepare a methomyl water solution; after the reaction is finished and the temperature of the methomyl water solution is controlled to 5-10 DEG C, adding NaCl to separate methomyl, and filtering, so as to obtain solid methomyl. According to the method, methomyl in the water solution is seperated by virtue of a salting-out method, so that the yield of methomyl is increased, furthermore, the emission load of pollutants in wastewater is reduced, and the environment is protected. The method is easy, the cost is low; furthermore, an obtained methomyl product is high in purity, good in quality and has very high practicability.
Description
Technical field
The present invention relates to method for producing agricultural field, specifically a kind of method improving production methomyl yield.
Background technology
The method of domestic production methomyl is generally adopt many oximes that goes out to react with different ester, directly synthesis target product methomyl.But methomyl has certain water-soluble, and due to the dissolving of methomyl in water in production process, make the yield of chemosynthesis reaction not high, pollutant discharge amount is large.
Summary of the invention
The object of the invention is to provide a kind of according to the deficiencies in the prior art and improve the method for producing methomyl yield, the method technique is simple, and cost is low, can improve the yield of methomyl production by the method.
The present invention is achieved through the following technical solutions: a kind of method improving production methomyl yield, described methomyl is by many oximes and the obtained methomyl aqueous solution of methyl isocyanate reaction of going out, its step comprises: the temperature of the methomyl aqueous solution controlled after having reacted to add after 5-10 DEG C after NaCl makes methomyl separate out and filter, the solid after filtration is methomyl.
Preferably, the filtrate after described filtration recovery continues to join in the methomyl aqueous solution as NaCl.
Preferably, the methomyl solid after described filtration is that then first recrystallization obtains after drying.
Preferably, charcoal absorption impurity is added in the described methomyl aqueous solution.
The present invention utilizes the method for saltouing that the methomyl in the aqueous solution is separated out, and improves the yield that methomyl is produced, and reduces the quantity discharged of Pollutants in Wastewater, be beneficial to environmental protection.Method is simple, and cost is low, and the methomyl product purity obtained is high, and quality is good, has very strong practicality.
Embodiment
By the following specific examples further illustrate the invention:
Embodiment 1
By many oximes and the obtained methomyl aqueous solution of methyl isocyanate reaction of going out, charcoal absorption impurity is added after having reacted, then utilizing icy salt solution methomyl aqueous temperature to be controlled after 5 DEG C, add NaCl makes methomyl separate out rear filtration, and the filtrate after filtration recovery continues to join in the methomyl aqueous solution as NaCl.The methomyl that then the first recrystallization of solid after filtration obtains after drying, yield has brought up to 93% from 90%.
Embodiment 2
By many oximes and the obtained methomyl aqueous solution of methyl isocyanate reaction of going out, charcoal absorption impurity is added after having reacted, then utilizing icy salt solution methomyl aqueous temperature to be controlled after 10 DEG C, add NaCl makes methomyl separate out rear filtration, and the filtrate after filtration recovery continues to join in the methomyl aqueous solution as NaCl.The methomyl that then the first recrystallization of solid after filtration obtains after drying, yield has brought up to 92% from 88%.
Embodiment 3
By many oximes and the obtained methomyl aqueous solution of methyl isocyanate reaction of going out, charcoal absorption impurity is added after having reacted, then utilizing icy salt solution methomyl aqueous temperature to be controlled after 8 DEG C, add NaCl makes methomyl separate out rear filtration, and the filtrate after filtration recovery continues to join in the methomyl aqueous solution as NaCl.The methomyl that then the first recrystallization of solid after filtration obtains after drying, yield has brought up to 92% from 90%.
The methomyl purity purity that the inventive method obtains can reach more than 98%, and has fully reclaimed the methomyl in the methomyl aqueous solution, improves yield.Meanwhile, reduce the contaminative of waste water, be conducive to environmental protection, there is very strong practicality.
For those skilled in the art, under the prerequisite not departing from embodiment of the present invention principle, can also make some improvements and modifications, these improvements and modifications are also considered as the protection domain of the embodiment of the present invention.
Claims (4)
1. one kind is improved the method for producing methomyl yield, described methomyl is by many oximes and the obtained methomyl aqueous solution of methyl isocyanate reaction of going out, its step comprises: the temperature of the methomyl aqueous solution controlled after having reacted to add after 5-10 DEG C after NaCl makes methomyl separate out and filter, the solid after filtration is methomyl.
2. improve the method for producing methomyl yield according to claim 1, it is characterized in that: the filtrate after described filtration recovery continues to join in the methomyl aqueous solution as NaCl.
3. improve the method for producing methomyl yield according to claim 1, it is characterized in that: the methomyl solid after described filtration is that then first recrystallization obtains after drying.
4. improve the method for producing methomyl yield according to claim 1, it is characterized in that: in the described methomyl aqueous solution, add charcoal absorption impurity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410819834.5A CN104529846A (en) | 2014-12-25 | 2014-12-25 | Method for increasing yield of produced methomyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410819834.5A CN104529846A (en) | 2014-12-25 | 2014-12-25 | Method for increasing yield of produced methomyl |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104529846A true CN104529846A (en) | 2015-04-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410819834.5A Pending CN104529846A (en) | 2014-12-25 | 2014-12-25 | Method for increasing yield of produced methomyl |
Country Status (1)
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| CN (1) | CN104529846A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529847A (en) * | 2014-12-25 | 2015-04-22 | 湖北沙隆达股份有限公司 | Method for producing methomyl |
| CN111187192A (en) * | 2019-12-27 | 2020-05-22 | 安道麦股份有限公司 | Method for improving yield of methomyl |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3890362A (en) * | 1972-06-19 | 1975-06-17 | Du Pont | Preparation of thiohydroximate carbamates |
| CN1257655A (en) * | 1999-12-17 | 2000-06-28 | 温沛宏 | Methomyl and cyfluthrin microemulsion as insecticide-miticide |
| CN102924354A (en) * | 2012-10-23 | 2013-02-13 | 海利贵溪化工农药有限公司 | Synthetic method of methomyl |
| CN103524389A (en) * | 2013-10-22 | 2014-01-22 | 沙隆达集团公司 | Method for preparing pesticide methomyl |
-
2014
- 2014-12-25 CN CN201410819834.5A patent/CN104529846A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3890362A (en) * | 1972-06-19 | 1975-06-17 | Du Pont | Preparation of thiohydroximate carbamates |
| CN1257655A (en) * | 1999-12-17 | 2000-06-28 | 温沛宏 | Methomyl and cyfluthrin microemulsion as insecticide-miticide |
| CN102924354A (en) * | 2012-10-23 | 2013-02-13 | 海利贵溪化工农药有限公司 | Synthetic method of methomyl |
| CN103524389A (en) * | 2013-10-22 | 2014-01-22 | 沙隆达集团公司 | Method for preparing pesticide methomyl |
Non-Patent Citations (2)
| Title |
|---|
| 成四喜 等: "灭多威及其中间体合成路线述评", 《湖南化工》 * |
| 李成未: "提高灭多威收率的有效途径", 《河南化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104529847A (en) * | 2014-12-25 | 2015-04-22 | 湖北沙隆达股份有限公司 | Method for producing methomyl |
| CN111187192A (en) * | 2019-12-27 | 2020-05-22 | 安道麦股份有限公司 | Method for improving yield of methomyl |
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Application publication date: 20150422 |