CN102432512A - Purification method of clethodim technical pesticide - Google Patents
Purification method of clethodim technical pesticide Download PDFInfo
- Publication number
- CN102432512A CN102432512A CN201110433414XA CN201110433414A CN102432512A CN 102432512 A CN102432512 A CN 102432512A CN 201110433414X A CN201110433414X A CN 201110433414XA CN 201110433414 A CN201110433414 A CN 201110433414A CN 102432512 A CN102432512 A CN 102432512A
- Authority
- CN
- China
- Prior art keywords
- clethodim
- former medicine
- organic
- polar solvent
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a purification method of clethodim technical pesticide, which comprises the following steps: adding diluted alkali liquor into partially decomposed clethodim technical pesticide (the effective ingredient content is about 50%), sufficiently stirring and mixing at room temperature, standing to stratify, discarding the understratum tarry impurity, and extracting out some other impurities respectively with organic non-polar solvent and polar solvent; after acidifying the water layer, extracting with organic polar solvent, washing the organic extract with water to neutrality, and drying with a drying agent; and finally, removing the solvent to obtain the high-purity clethodim technical pesticide. The content is up to higher than 85%, and the total yield is up to higher than 90%.
Description
Technical field
The invention belongs to technical field of pesticide, relate in particular to the method for purification of the former medicine of a kind of clethodim.
Background technology
Clethodim is a kind of cyclohexyl diketone weedicide with good weeding activity.Because contain two non-conterminous carbon-carbon double bonds in this structure of matter formula, thereby have multiple cis-trans-isomer to exist, what have weeding activity mainly is (E, E) formula.Configuration reversal externally can take place under the Conditioning in clethodim, and clethodim is unstable under ultraviolet ray, strong acid, highly basic condition, poor heat stability, so the former medicine of clethodim is easy to take place decomposing phenomenon in storage process.Clethodim just can not be reprocessed into formulation and use in case the content reduction is decomposed in generation, re-uses after therefore must purifying.There is not bibliographical information at present, the method that the former medicine of decomposed clethodim is purified.
Summary of the invention
The object of the invention is to provide a kind of convenience simple and direct, and through the purify method of the former medicine of clethodim of extraction+single flash, its working method is: adding sig water in the former medicine of clethodim (active constituent content about 50%) that part is decomposed; After thorough mixing stirred under the room temperature, standing demix discarded lower floor's tarry impurity; Extract other impurity respectively with organic non-polar solvent and polar solvent then, with after the water layer acidifying, extract with organic polar solvent more then; With organic layer washing to neutral, with the siccative drying, remove solvent at last after; Get the former medicine of highly purified clethodim, content reaches more than 85%, and total recovery reaches more than 90%.
This method is simple to operate, implements easily.Advantages such as it is short to have a treatment time, and service temperature is low.
Embodiment
Embodiment: the method for purification of the former medicine of a kind of clethodim, operate as follows:
In the 500ml beaker, add the former medicine of clethodim (active constituent content about 50%) of 100g, add the dilute alkaline aqueous solution of 250ml again, mix 30 minutes with magnetic stirrer under the room temperature after; Pour in the separating funnel, standing demix discards the dark tarry matters of lower floor, water layer is poured into the sherwood oil that adds 100ml in the beaker; After the magnetic agitation 30 minutes, standing demix, discard organic layer (recyclable applying mechanically) after, add the 100ml methylene dichloride again; After the magnetic agitation 30 minutes, standing demix, discard organic layer (recyclable applying mechanically) after, water layer is acidified to pH1-2 with diluted acid; Extract at twice with the 300ml methylene dichloride, combining extraction liquid is washed with water to washing water and is neutral, after dichloromethane extraction liquid adds anhydrous magnesium sulfate drying again; Underpressure distillation removes methylene dichloride, gets the former medicine of clethodim, content 85.6%.The recovery is 90.8%.
Claims (3)
1. the method for purification of the former medicine of clethodim is characterized in that: in the former medicine of clethodim (active constituent content about 50%) that part is decomposed, add sig water, after fully mixing under the room temperature; Standing demix discards lower floor's tarry impurity, extracts other impurity respectively with organic non-polar solvent and polar solvent then; With after the water layer acidifying, extract with organic polar solvent more then, then that the organic extract liquid washing is extremely neutral; Dry with siccative, remove solvent at last after, the former medicine of highly purified clethodim; Content reaches more than 85%, and total recovery reaches more than 90%.
2. the method for purification of the former medicine of clethodim according to claim 1 is characterized in that: this method is dissolved the former medicine of decomposed clethodim with sig water earlier, thereby separablely falls most of insoluble tarry impurity.
3. the method for purification of clethodim according to claim 1; It is characterized in that: use polar organic (as: methylene dichloride) and nonpolar (as: sherwood oil) solvent under alkaline condition, to extract different impurity respectively respectively, and staple is not extracted out basically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110433414XA CN102432512A (en) | 2011-12-21 | 2011-12-21 | Purification method of clethodim technical pesticide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110433414XA CN102432512A (en) | 2011-12-21 | 2011-12-21 | Purification method of clethodim technical pesticide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102432512A true CN102432512A (en) | 2012-05-02 |
Family
ID=45980907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110433414XA Pending CN102432512A (en) | 2011-12-21 | 2011-12-21 | Purification method of clethodim technical pesticide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102432512A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831416A (en) * | 2016-12-29 | 2017-06-13 | 淮安国瑞化工有限公司 | A kind of preparation method of high content TrinexAN_SNacethyl active compound |
| CN111233720A (en) * | 2018-11-28 | 2020-06-05 | 沈阳科创化学品有限公司 | Method for purifying trione and method for preparing clethodim |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575307A (en) * | 2009-06-11 | 2009-11-11 | 江苏长青农化股份有限公司 | Synthetic method of clethodim |
| US20100304971A1 (en) * | 2007-10-24 | 2010-12-02 | Bayer Cropscience Ag | Herbicidal combination |
-
2011
- 2011-12-21 CN CN201110433414XA patent/CN102432512A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100304971A1 (en) * | 2007-10-24 | 2010-12-02 | Bayer Cropscience Ag | Herbicidal combination |
| CN101575307A (en) * | 2009-06-11 | 2009-11-11 | 江苏长青农化股份有限公司 | Synthetic method of clethodim |
Non-Patent Citations (3)
| Title |
|---|
| QIN YU等: "Diversity of Acetyl-Coenzyme A Carboxylase Mutations in Resistant Lolium Populations: Evaluation Using Clethodim1", 《PLANT PHYSIOLOGY》 * |
| 孙光强等: "环己烯酮类除草剂-烯草酮的合成", 《现代农药》 * |
| 郭林华等: "除草剂烯草酮的合成研究进展", 《现代农药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831416A (en) * | 2016-12-29 | 2017-06-13 | 淮安国瑞化工有限公司 | A kind of preparation method of high content TrinexAN_SNacethyl active compound |
| CN106831416B (en) * | 2016-12-29 | 2019-11-08 | 淮安国瑞化工有限公司 | A kind of preparation method of high-content TrinexAN_SNacethyl raw medicine |
| CN111233720A (en) * | 2018-11-28 | 2020-06-05 | 沈阳科创化学品有限公司 | Method for purifying trione and method for preparing clethodim |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101381298B (en) | Method for preparing conjugate linolic acid using idesia polycarpa maxim. var. vestita diels oil | |
| CN102342307B (en) | Pollution-free biopesticide | |
| CN111773910B (en) | Fulvic acid sterilization deodorant as well as preparation method and application thereof | |
| CN103193598A (en) | Oriented synthesis preparation process of cis-form p-menthane-3,8-diol | |
| CN103113195A (en) | Novel method for rapidly preparing hydroxytyrosol | |
| CN101492579A (en) | Printing ink cleaning agent | |
| CN102432512A (en) | Purification method of clethodim technical pesticide | |
| CN104255815A (en) | Preparation method of botanical insecticide | |
| CN102558379A (en) | Method for extraction and deproteinization of hop polysaccharide | |
| CN104592067A (en) | Method for recycling dimethyl sulfoxide waste residue through multi-stage extraction | |
| CN100569717C (en) | The method for preparing sclareol by sclareol medicinal extract | |
| CN105198029A (en) | Extraction treatment method for 2, 4-dichloro-3, 5-dimethylphenol waste water | |
| CH250524A (en) | Process for the production of penicillin salts of alkali and alkaline earth metals. | |
| CN102805990A (en) | System for washing and recycling tail gas generated during production of urea | |
| CN105153434A (en) | Process for extracting humic acid from coarse slime | |
| CN106588620A (en) | Method for extracting and separating 6-paradol from aframomum melegueta | |
| WO2004108848A1 (en) | Method for processing vegetable raw materials | |
| CN103483232A (en) | Refining method of valnemulin hydrochloride | |
| CN1113846C (en) | Process for producing terephthalic acid | |
| CN116712476B (en) | Hypericum perforatum extract and preparation method thereof | |
| Ho | Ketone regeneration from oximes with alkaline hydrogen peroxide | |
| CN105983122A (en) | Preparation method of natural plant-source environment-friendly deodorant | |
| CN109439452A (en) | A kind of lavatory deodorization scale remover and preparation method | |
| CN103588843A (en) | Method for extracting ergosterol from waste mycelium of fermented citric acid | |
| CN104402857B (en) | Method for purifying cyclohexanedione monoethylene ketal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120502 |