CN1515157A - Preparation method of imidacloprid microemulsion agent - Google Patents
Preparation method of imidacloprid microemulsion agent Download PDFInfo
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- CN1515157A CN1515157A CNA2003101140025A CN200310114002A CN1515157A CN 1515157 A CN1515157 A CN 1515157A CN A2003101140025 A CNA2003101140025 A CN A2003101140025A CN 200310114002 A CN200310114002 A CN 200310114002A CN 1515157 A CN1515157 A CN 1515157A
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Abstract
The preparation method of imidacloprid microemulsion is that chelating imidacloprid with mixture of monobasis acid and polybasic acid, making them be dissolved in water and using non-ionic surfactant and thickening antifreezing agent to make them be stably dispersed so as to obtain the water base high-concentration imidacloprid microemulsion.
Description
The preparation method that the technical field imidacloprid emulsion is new belongs to the manufacturing technology of pesticides new formulation.
Background technology Imidacloprid (imidacloprid) is to intend nicotinoids biogenic systemic insecticide, efficiently, low toxicity, wide spectrum, pierce-suck type and scratching mouthparts insect to aphid, leafhopper, plant hopper, thrips, aleyrodid etc. and resistant strain thereof have excellent control efficiency, and Lepidoptera and coleopteran pest are also had certain preventive effect.This insecticide is widely used in countries in the world, becomes one of three big insecticides that 21 century attracts people's attention.
Imidacloprid
Normal temperature is the colourless crystallization body down, two kinds of crystal formations are arranged, its fusing point is respectively 143.8 ℃ and 136.4 ℃, except that solvability in dimethyl formamide (about 20%) and carrene (about 10%) is big, be insoluble in other organic solvent, dissolving 0.51 grams per liter in 20 ℃ of water, stable in the PH5-11 scope, in strong acid, decompose.Imidacloprid generally be processed into wetting powder (2,2.5,10,25WP), suspending agent (35,48,70SC), granula (1,2,5GR) use, above-mentioned formulation exists the defective except that environmental protection and production efficiency, its drug effect all is lower than the liquid dosage form with dosage.2%, 5%, 10% missible oil (EC) and 10%, 20% soluble liquid (SL) have appearred, but they all adopt a large amount of benzene,toluene,xylenes and other organic solvent, not only waste industrial resources, strengthened production cost, contaminated environment more seriously, human beings'health is caused potential significant damage, so the Water-borne modification formulation of water replacement hazardous solvent the developing direction and the research focus of the current formulations of pesticide have been become.20% imidacloprid emulsion (Imidacloprid 20%, cosolvent 40%, emulsifier 25%, water 15%) that occurs still needs to use more organic cosolvent and emulsifier in the recent period.
Summary of the invention the objective of the invention is, do not use any organic solvent, produce the Water-borne modification liquid preparation of high concentration Imidacloprid, through repetition test, concentrate on studies, made the 5-45% imidacloprid emulsion (m/m) that do not contain organic solvent or the imidacloprid emulsion (m/v) of 6.5-60% finally.
The inventor has and H according to there being four not N atoms of share electron pair in the Imidacloprid chemical constitution
+Ability Deng the positive charge affinity.Through testing Imidacloprid at 4NHCL or HNO
3, be partly dissolved among the HAeo, but branch parses precipitation after depositing certain hour, but and in phosphoric acid, citric acid, malic acid, tartaric acid, lactic acid minimal amounts of dissolved and do not separate out precipitation, after two kinds of acids are mixed by a certain percentage, solvability multiplication to Imidacloprid, and quite stable, but after in water, diluting, then comparatively fast separate out flakes pin type crystal thing and be insoluble to HCL, if after adding some non-ionic surface active agent and antifreezing agent again in the stoste, then can in dilution, keep relative stability.30% imidacloprid emulsion of final typing, appearance transparent, spontaneous dispersiveness is fabulous in water, elder generation's emulsification then becomes solution, dispersion stabilization is good, and physics and chemical stability after the cold and hot storage are good, the biological effect excellence, for the Imidacloprid Water-borne modification has been opened up a new making route, thereby finished the present invention.
High concentration imidacloprid emulsion of the present invention composed as follows:
Imidacloprid 5-45%
Monoacid 0.08-0.5 mole
Polyacid and organic acid 0.05-0.4 mole
Surfactant 6-20%
Thickening antifreezing agent 0-5%
Running water 30-(surplus) %
The monoacid of indication is among the present invention: in hydrofluoric acid, hydrobromic acid, hydroiodic acid, acid iodide, hydrochloric acid, nitric acid, thiocyanic acid, molybdic acid, formic acid, acetate, dichloroacetic acid, propionic acid, perchloric acid, the hypochlorous acid etc. one or more, working concentration is the 0.08-0.5 mole.
The polyacid of indication and organic acid are among the present invention: in sulfuric acid, sulfurous acid, phosphoric acid, phosphorous acid, pyrophosphoric acid, citric acid, malic acid, tartaric acid, lactic acid, pyruvic acid, oxalic acid, sulfosalicylic acid, alkyl benzene sulphonate, sulfanilic acid, maleic acid, naphthenic acid, ascorbic acid, gluconic acid, DL-alanine, glycine, glutamic acid, succinic acid, L-cystine, nitrilotriacetic acid, the ethylenediamine tetra-acetic acid etc. one or more, working concentration is the 0.05-0.4 mole.
The surfactant of indication is one or more of non-ionic surface active agents such as OP, NP, JFC, 300#, 600#, 700#, 1600#, By, TW-20, TW-80, NP phosphoric acid ester among the present invention, and usage amount is 6-20%.
Thickening antifreezing agent among the present invention is that ethylene glycol, propane diols, glycerine, PEG400, polyvinyl alcohol, its consumption are 0-5%.
The inventor to the understanding of above-mentioned waterborne preparation shaping mechanism is: the mixing acid of different degrees of ionization, respectively with the Imidacloprid structure in loose the combination or chelating of N atom of varying strength negative electrical charge, the molecular compound or the chelate that form can be stablized dissolving in water, but because of the polarization of big water gaging is disintegrated, by the aquation of a plurality of oxygen atoms in non-ionic surface active agent and the thickening antifreezing agent structure, and it is relatively stable that this molecular compound is able to.The formulation of similar water solution among the present invention, since there is no salting liquid like that can with any ratio with water is miscible and can the long-term stability character, but in water after the spontaneous emulsification dissolving and keep relative stability, thereby more approach the characteristic of microemulsion, therefore regard as the novel microemulsion that specific process is made.
Microemulsion of the present invention and preparation method thereof has following characteristics and advantage.
1, compares with microemulsion in the past, need not any organic solvent and distilled water or deionized water, can reduce production costs significantly and use cost, can obtain remarkable economic efficiency, the more important thing is and ensured the safety of producing and using, crops and environment are not had any harmful effect, meet the requirement of environment friendly agricultural.
2, owing to contain the electropositive of recruit's compound (chelate) of acid, help soup and on electronegative blade face, adsorb, opening up and permeate.The emulsifier consumption can reduce and be effective and the longevity of residure is long, be better than general microemulsion, and phosphate radical, citric acid etc. also has facilitation to plant growth in the soup.
3, owing to do not contain organic solvent, safety is good, the flexibility on ground in the time of can enlarging the using method (as spraying, pouring, trunk injection etc.) of Imidacloprid and crop range of application and improve dispenser.
4, production method is simple, and raw material is easy to get, and is beneficial to popularization, and has made the present imidacloprid emulsion of maximum concentration in the world that conventional method can't be made, thereby more has one's own knack.
Embodiment embodiment one: add the 300kg running water in the reactor of 2000 liters, add phosphatase 11 38g, citric acid 2kg, glacial acetic acid 130kg, slowly add 95% Imidacloprid 320kg again, make it to dissolve fully transparent after, add TW-80 50kg again, JFC30kg, polyethylene glycol 30kg promptly gets 30% imidacloprid emulsion (30ME Imidacloprid) 1000kg after stirring.
The physicochemical property of imidacloprid emulsion of the present invention and existing waterborne preparation performance are compared as follows:
Table 1
| Test specimen | Outward appearance | Spontaneous dispersiveness | Dispersion stabilization | Cold storage (0 ℃-week) back phenomenon | Heat storage (54 ± 1 ℃ 14 days) resolution ratio % | The transparency temperature scope |
| 30ME Imidacloprid (the present invention) | Transparent | Excellent | ?????+ | Transparent | ???????2.3 | ??-5-+80℃ |
| The 20ME Imidacloprid | Inferior transparent | Can | ?????± | Small amount of crystalline | ???????3.5 | ??0-+55℃ |
| The 20SL Imidacloprid | Translucent | Difference | ?????++ | Muddy | ???????4.1 | ??0-+60℃ |
Table 2
| Test specimen | Per hectare Imidacloprid working substance consumption, g | To melon thrips control efficiency, % | Production cost (unit/ton) | Use cost (unit/mu) | |||
| 1 day | 3 days | 7 days | 14 days | ||||
| ???30ME | ??????10 | ???95.2 | ???98.4 | ???96.7 | ???95.2 | ???50000 | ????0.5 |
| ???10WP | ??????15 | ???94.8 | ???98.2 | ???97.0 | ???93.0 | ???22000 | ????2.0 |
| ???5EC | ??????12 | ???74.5 | ???89.2 | ???88.9 | ???80.3 | ???15000 | ????2.5 |
Embodiment two
In the reactor of 2000 liters, drop into the 250kg running water, add phosphatase 11 40kg, malic acid 2kg, hydrochloric acid 38kg slowly adds 96% propiconazole 470kg again, make it to dissolve fully transparent after, add agricultural newborn 1600#60kg again, op-10 20kg, polyethylene glycol 20kg promptly gets 45% propiconazole microemulsion 1000kg after stirring.
Claims (6)
- The feature of the preparation method invention that 1, imidacloprid emulsion is new is, to account for the former medicine of component 5-45% Imidacloprid slowly puts into and contains in 0.08-0.5 mole monoacid and 0.05-0.4 mole polyacid and the organic acid mixed aqueous solution, make it the chelating dissolving, add non-ionic surface active agent and thickening antifreezing agent then, make it stable dispersion, made the novel water-based property imidacloprid emulsion that does not contain any organic solvent, this method also is applicable to the making of some nitrogen heterocyclic ring structure microemulsion.
- 2, monoacid according to claim 1, it is characterized in that referring in hydrofluoric acid, hydrobromic acid, hydroiodic acid, acid iodide, hydrochloric acid, nitric acid, thiocyanic acid, molybdic acid, formic acid, acetate, dichloroacetic acid, propionic acid, perchloric acid, the hypochlorous acid etc. one or more, working concentration is the 0.08-0.5 mole.
- 3, polyacid according to claim 1 and organic acid, it is characterized in that referring in sulfuric acid, sulfurous acid, phosphoric acid, phosphorous acid, pyrophosphoric acid, citric acid, malic acid, tartaric acid, lactic acid, pyruvic acid, succinic acid, maleic acid, oxalic acid, sulfosalicylic acid, alkyl benzene sulphonate, sulfanilic acid, naphthenic acid, ascorbic acid, gluconic acid, glycine, DL-alanine, glutamic acid, L-cystine, nitrilotriacetic acid, the ethylenediamine tetra-acetic acid etc. one or more, working concentration 0.05-0.4 mole.
- 4, non-ionic surface active agent according to claim 1, it is characterized in that referring to one or more of OP, NP, JFC, agricultural newborn 300#, agricultural newborn 600#, Nongru-700 #, agricultural newborn 1600#, BY, TW-80, TW-20, NP phosphoric acid ester etc., usage amount is 6-20%.
- 5, thickening antifreezing agent according to claim 1 is characterized in that referring to ethylene glycol, interior glycol, glycerine, PEG400, polyvinyl alcohol, and its consumption is 0-5%.
- 6, some nitrogen heterocyclic ring structure Acetamiprid that agricultural chemicals refers to according to claim 1, Buprofezin, thiophene worm quinoline, pyrazine ketone, fly eradication amine, pyrrole mite glue, chlopyrifos, chlorpyrifos-methyl, Hostathion, quinalphos, diazinon, pirimiphos-methyl, pyridaphethione, triazolone, alkene azoles alcohol, Triadimenol, propiconazole, Tebuconazole, own azoles alcohol, nitrile bacterium azoles, fluorine bacterium azoles, press down mould azoles, the acid amides azoles, Flusilazole, phonetic mould amine, azoles bacterium nitrile, Prochloraz, carbendazim, albendazole, anilazine, Seedvax, MBAMT, pefurazoate, paclobutrazol, uniconazole P, 6-benzyladenine, Feng Ding alcohol, phytocytomine, atrazine, cyanazine, prometryn, symetryne, the piperazine humulone, ametryn, Simanexs etc. are one or more mixture wherein.
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| CNA2003101140025A CN1515157A (en) | 2003-08-28 | 2003-11-05 | Preparation method of imidacloprid microemulsion agent |
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| CN03155965.4 | 2003-08-28 | ||
| CN03155965 | 2003-08-28 | ||
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103621497A (en) * | 2013-11-13 | 2014-03-12 | 江西巴菲特化工有限公司 | Method for processing preparation from raw pesticide structure |
| CN106550940A (en) * | 2015-09-29 | 2017-04-05 | 温菲尔德解决方案公司 | Micronutrient compositions and system and its using method |
| CN108338182A (en) * | 2017-07-27 | 2018-07-31 | 江苏辉丰农化股份有限公司 | Composition pesticide containing cyromazine and organophosphor |
| CN110477000A (en) * | 2019-09-19 | 2019-11-22 | 山东省林业科学研究院 | A kind of liquid formulation for trunk injection and its preparation method and application of Japanese red pine limb portion pest |
| US10807918B2 (en) | 2016-02-25 | 2020-10-20 | Winfield Solutions, Llc | Micronutrient compositions containing zinc and systems and methods of using same |
-
2003
- 2003-11-05 CN CNA2003101140025A patent/CN1515157A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103621497A (en) * | 2013-11-13 | 2014-03-12 | 江西巴菲特化工有限公司 | Method for processing preparation from raw pesticide structure |
| CN106550940A (en) * | 2015-09-29 | 2017-04-05 | 温菲尔德解决方案公司 | Micronutrient compositions and system and its using method |
| US10899675B2 (en) | 2015-09-29 | 2021-01-26 | Winfield Solutions, Llc | Micronutrient compositions and systems and methods of using same |
| US11591273B2 (en) | 2015-09-29 | 2023-02-28 | Winfield Solutions, Llc | Micronutrient compositions and systems and methods of using same |
| US10807918B2 (en) | 2016-02-25 | 2020-10-20 | Winfield Solutions, Llc | Micronutrient compositions containing zinc and systems and methods of using same |
| US12017965B2 (en) | 2016-02-25 | 2024-06-25 | Winfield Solutions, Llc | Micronutrient compositions containing zinc and systems and methods of using same |
| CN108338182A (en) * | 2017-07-27 | 2018-07-31 | 江苏辉丰农化股份有限公司 | Composition pesticide containing cyromazine and organophosphor |
| CN110477000A (en) * | 2019-09-19 | 2019-11-22 | 山东省林业科学研究院 | A kind of liquid formulation for trunk injection and its preparation method and application of Japanese red pine limb portion pest |
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