CN102090397B - High-purity imidazolone weedicide ammonium salt raw powder and production process thereof - Google Patents
High-purity imidazolone weedicide ammonium salt raw powder and production process thereof Download PDFInfo
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- CN102090397B CN102090397B CN 201010610830 CN201010610830A CN102090397B CN 102090397 B CN102090397 B CN 102090397B CN 201010610830 CN201010610830 CN 201010610830 CN 201010610830 A CN201010610830 A CN 201010610830A CN 102090397 B CN102090397 B CN 102090397B
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- imidazolinone herbicide
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Abstract
The invention particularly discloses high-purity imidazolone weedicide ammonium salt raw powder and a production process thereof, which belong to the field of application of weedicides. The process comprises the following steps of: mixing an imidazolone weedicide active compound, amine (ammonia) and double solvents; completely salifying; evaporating a low-boiling-point solvent for pelletizing; filtering; and drying under the reduced pressure to obtain a product. By adopting the method, the product has the advantages of high content, good medicament effect, high mixing performance, short production period, simple production process, wide application range and broad market prospect.
Description
(1) technical field
The invention belongs to the weed killer herbicide application, particularly a kind of high-purity imidazolinone herbicide ammonium salt raw powder and production technology thereof.
(2) background technology
Imidazolinone herbicide is to absorb by plant roots and cauline leaf, in xylem and phloem conduction, accumulates in meristematic tissue.After cauline leaf was handled, susceptible weeds stopped growing immediately, and after the soil treatment, root absorption upwards conducts to the meristematic tissue on weeds top, it was stopped growing and necrosis.That at present, drops into that commercialization produces has imidazoles nicotinic acid.Miaow oxalate, imazaquin, imazethapyr etc.The former liquid medicine dissolubility of imidazolinone herbicide is poor, and the universal method of dealing with problems is salify, and the formulation of common usefulness is to be the theme with isopropyl amine salt and ammonium salt on the market now, and that uses for many years facts have proved that ammonium salt is generally accepted for users at home and abroad.
At present, the main technique of synthetic imidazolinone herbicide ammonium salt raw powder is single solvent method, and synthetic ammonium salt is vitreum, need leave standstill for a long time to become solid, could beat powder after thoroughly pulverizing, and the production cycle is long, complex manufacturing.
(3) summary of the invention
The present invention provides a kind of drug effect is remarkable, the performance that is mixed is good high-purity imidazolinone herbicide ammonium salt raw powder and production technology thereof in order to remedy the deficiencies in the prior art.
The present invention is achieved through the following technical solutions:
A kind of high-purity imidazolinone herbicide ammonium salt raw powder is characterized in that: the parts by weight that contain the imidazolinone herbicide ammonium salt in the former powder are 95～99%, and loss on drying≤0.1% during its high level, can reach 98～99%.
The former medicine of imidazolinone herbicide, amine (ammonia) and solvent pairs are mixed, behind the salify, steam low boiling point solvent and carry out granulation fully, the oven dry of reducing pressure after filtering more namely obtains product; Wherein, the former medicine of imidazolinone herbicide is
R is hydrogen, methyl, ethyl, methoxyl methyl or phenyl; The mol ratio of the former medicine of imidazolinone herbicide and amine (ammonia) is 1: 1～3, with the weight proportion of solvent pairs be 1: 1～6.
Described amine (ammonia) is organic amine or liquefied ammonia such as methylamine, n-propylamine, isopropylamine.
Described solvent pairs is the organic solvent that two kinds of materials in methyl alcohol, ethanol, acetone, ethyl acetate, carrene, dichloroethane, n-hexane, cyclohexane, ether, benzinum and the dioxane are formed by 1: 1 weight proportion.
The mol ratio of the former medicine of described imidazolinone herbicide and amine (ammonia) is 1: 1.5, with the weight proportion of solvent pairs be 1: 4.
Because the too high meeting of bake out temperature causes the product ammonium salt partly to decompose, and causes product water-soluble bad, therefore oven dry needs the decompression oven dry.
Product purity of the present invention adopts efficient liquid phase chromatographic analysis, and analyzing and testing result shows that the product purity of the inventive method can reach more than 98%.
Product content height of the present invention, good drug efficacy, the performance that is mixed is good, and is with short production cycle, and production technology is simple, is widely used, and market prospects are wide.
(4) embodiment
Embodiment 1;
The former medicine 500kg of the Imazethapyr of purity 98% (1.70kmol), 43.2kg (2.54kmol) liquefied ammonia, 1000kg acetone, 1000kg cyclohexane are reacted in the enamel reaction still of 3000L, after stirring reaction is transparent, steam acetone, cooling is filtered, solid can obtain high-purity Imazethapyr ammonium salt raw powder 482kg (1.56kmol) thus with the decompression oven for drying.In the resulting Imazethapyr ammonium salt raw powder, contain the Imazethapyr ammonium salt more than 98%, loss on drying≤1.0%.
State high-purity Imazethapyr ammonium salt raw powder product, be solid powdery, can be used as a kind of good composite female powder, mix with solid, or mix with liquid, all do not have bad physical phenomenons such as precipitation, layering, muddiness, the industrialization that very easy realization is mixed.Can be widely used.The present invention not only can directly use and be configurable, and female powder of holding concurrently, preparation are to use in the present Imazethapyr and the level that disposes in the preparation is the highest, product the most easily.
Embodiment 2:
The former medicine 500kg of the weed eradication cigarette of purity 98% (1.88kmol), 166kg (2.82kmol) isopropylamine, 1000kg carrene, 1000kg benzinum are reacted in the enamel reaction still of 3000L, after stirring reaction is transparent, steam carrene, cooling is filtered, solid can obtain the high-purity weed eradication cigarette former powder 558kg of isopropyl amine salt (1.73kmol) thus with the decompression oven for drying.In the former powder of resulting weed eradication cigarette isopropyl amine salt, contain weed eradication cigarette isopropyl amine salt more than 98%, loss on drying≤1.0%.。
Embodiment 3:
The former medicine 500kg of the imazapic of purity 98% (1.78kmol), 158kg (2.67kmol) isopropylamine, 1000kg methyl alcohol, 1000kg cyclohexane are reacted in the enamel reaction still of 3000L, after stirring reaction is transparent, steam methyl alcohol, cooling is filtered, solid can obtain the former powder 553kg of high-purity methyl Imazethapyr isopropyl amine salt (1.64kmol) thus with the decompression oven for drying.In the former powder of resulting imazapic isopropyl amine salt, contain the imazapic isopropyl amine salt more than 98%, loss on drying≤1.0%.
Embodiment 4:
The former medicine 500kg of the weed eradication quinoline of purity 98% (1.58kmol), 40.2kg (2.36kmol) liquefied ammonia, 1000kg acetone, 1000kg benzinum are reacted in the enamel reaction still of 3000L, after stirring reaction is transparent, steam acetone, cooling is filtered, solid can obtain high-purity weed eradication quinoline ammonium salt raw powder 480kg (1.45kmol) thus with the decompression oven for drying.In the resulting weed eradication quinoline ammonium salt raw powder, contain weed eradication quinoline ammonium salt salt more than 98%, loss on drying≤1.0%.
Claims (4)
1. high-purity imidazolinone herbicide ammonium salt raw powder, it is characterized in that: the parts by weight that contain the imidazolinone herbicide ammonium salt in the former powder are 95 ~ 99%, loss on drying≤0.1%, its production craft step is, the former medicine of imidazolinone herbicide, amine (ammonia) and solvent pairs are mixed, behind the salify, steam low boiling point solvent and carry out granulation fully, the oven dry of reducing pressure after filtering more namely obtains product; Wherein, the former medicine of imidazolinone herbicide is
, R is hydrogen, methyl, ethyl, methoxyl methyl or phenyl; The mol ratio of the former medicine of imidazolinone herbicide and amine (ammonia) is 1:1 ~ 3, with the weight proportion of solvent pairs be 1:1 ~ 6; Described amine (ammonia) is methylamine, n-propylamine, isopropylamine or liquefied ammonia; Described solvent pairs is the organic solvent that two kinds of materials in methyl alcohol, ethanol, acetone, ethyl acetate, carrene, dichloroethane, n-hexane, cyclohexane, ether, benzinum and the dioxane are formed by the weight proportion of 1:1.
2. high-purity imidazolinone herbicide ammonium salt raw powder according to claim 1, it is characterized in that: the parts by weight that contain the imidazolinone herbicide ammonium salt in the described former powder are 98 ~ 99%.
3. the production technology of high-purity imidazolinone herbicide ammonium salt raw powder according to claim 1, it is characterized in that: the former medicine of imidazolinone herbicide, amine (ammonia) and solvent pairs are mixed, fully behind the salify, steam low boiling point solvent and carry out granulation, the oven dry of reducing pressure after filtering more namely obtains product; Wherein, the former medicine of imidazolinone herbicide is
, R is hydrogen, methyl, ethyl, methoxyl methyl or phenyl; The mol ratio of the former medicine of imidazolinone herbicide and amine (ammonia) is 1:1 ~ 3, with the weight proportion of solvent pairs be 1:1 ~ 6; Described amine (ammonia) is methylamine, n-propylamine, isopropylamine or liquefied ammonia; Described solvent pairs is the organic solvent that two kinds of materials in methyl alcohol, ethanol, acetone, ethyl acetate, carrene, dichloroethane, n-hexane, cyclohexane, ether, benzinum and the dioxane are formed by the weight proportion of 1:1.
4. according to the production technology of the described high-purity imidazolinone herbicide of claim 3 ammonium salt raw powder, it is characterized in that: the mol ratio of the former medicine of described imidazolinone herbicide and amine (ammonia) is 1:1.5, with the weight proportion of solvent pairs be 1:4.
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| CN 201010610830 CN102090397B (en) | 2010-12-29 | 2010-12-29 | High-purity imidazolone weedicide ammonium salt raw powder and production process thereof |
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| CN 201010610830 CN102090397B (en) | 2010-12-29 | 2010-12-29 | High-purity imidazolone weedicide ammonium salt raw powder and production process thereof |
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| CN102090397B true CN102090397B (en) | 2013-08-07 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101636084A (en) * | 2007-03-16 | 2010-01-27 | 组合化学工业株式会社 | Herbicidal composition |
| CN101671076A (en) * | 2009-09-01 | 2010-03-17 | 山东先达化工有限公司 | Oxidative degradation process for imidazolinone herbicide wastewater |
| TW201018399A (en) * | 2008-09-26 | 2010-05-16 | Basf Se | Liquid, water-emulsifiable active ingredient concentrates |
| CN101856036A (en) * | 2010-06-13 | 2010-10-13 | 南京农业大学 | Biological weed control compound and preparation method thereof |
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2010
- 2010-12-29 CN CN 201010610830 patent/CN102090397B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101636084A (en) * | 2007-03-16 | 2010-01-27 | 组合化学工业株式会社 | Herbicidal composition |
| TW201018399A (en) * | 2008-09-26 | 2010-05-16 | Basf Se | Liquid, water-emulsifiable active ingredient concentrates |
| CN101671076A (en) * | 2009-09-01 | 2010-03-17 | 山东先达化工有限公司 | Oxidative degradation process for imidazolinone herbicide wastewater |
| CN101856036A (en) * | 2010-06-13 | 2010-10-13 | 南京农业大学 | Biological weed control compound and preparation method thereof |
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Effective date of registration: 20211130 Address after: 261000 East 2nd house, Lingang chemical park, Binhai Economic Development Zone, Weifang City, Shandong Province Patentee after: WEIFANG CYNDA CHEMICAL Co.,Ltd. Patentee after: Shandong Xianda agrochemical Co., Ltd Address before: 261000 Lingang Chemical Park, Weifang Binhai Economic Development Zone, Shandong Province Patentee before: WEIFANG CYNDA CHEMICAL Co.,Ltd. |
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