CN102742582A - Phenylpyrazole water-based hygienic insecticide and preparation method thereof - Google Patents
Phenylpyrazole water-based hygienic insecticide and preparation method thereof Download PDFInfo
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- CN102742582A CN102742582A CN2012102406275A CN201210240627A CN102742582A CN 102742582 A CN102742582 A CN 102742582A CN 2012102406275 A CN2012102406275 A CN 2012102406275A CN 201210240627 A CN201210240627 A CN 201210240627A CN 102742582 A CN102742582 A CN 102742582A
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Abstract
The invention relates to a phenylpyrazole water-based hygienic insecticide, and particularly relates to a fipronil emulsion hygienic insecticide and a preparation method thereof. In percentage by weight, the phenylpyrazole water-based hygienic insecticide comprises the following components: 6-30% of phenylpyrazole insecticide original medicine, 10-40% of organic solvent, 15-20% of emulsifier, 0-5% of cosolvent and the balance of water. The phenylpyrazole water-based hygienic insecticide is prepared in an emulsification kettle via the following processing steps of: firstly dissolving the insecticide original medicine in the solvent; then adding the emulsifier and the cosolvent to mix evenly; slowly pouring the solution into a certain amount of water; mixing the oil phase and the water phase in the emulsification kettle; and stirring at a speed of 100-200r/min for 10-30minutes to obtain the phenylpyrazole water-based hygienic insecticide. Compared with the missible oil products, the phenylpyrazole water-based hygienic insecticide has the advantages of decreasing the environment pollution, decreasing the toxicity of pesticide, improving the flash point of the product and improving the safety of production, transportation and use personnel.
Description
Technical field
The present invention relates to a kind of water baseization of phenyl pyrazoles hygienic insecticide, specifically is fluorine worm nitrile hygienic insecticide and preparation method thereof.
Background technology
Fluorine worm nitrile, it is special to call sharp strength, CAS numbering: 120068-37-3, chemical name: (RS)-5-amino-1-(2,6-dichlor-4-trifluoromethyl phenyl)-4-trifluoromethyl sulfinyl pyrazole-3-nitrile.Be that a kind of Phenylpyrazole insecticides, insecticidal spectrum are wide; Is main to insect with stomach poison function; Have concurrently and tag and certain systemic function, its mechanism of action is to hinder the chloride metabolism of insect GABA control, therefore sanitary insect pests such as mosquito, fly, flea, cockroach, bedbug is had very high insecticidal activity; To people's low toxicity, belong to the lower toxicity insecticide.
Summary of the invention
To the technical problem that exists in the prior art, the object of the present invention is to provide good water baseization of the phenyl pyrazoles hygienic insecticide of a kind of insecticidal effect.
The technical scheme that the present invention adopted is:
A kind of water baseization of phenyl pyrazoles hygienic insecticide is characterized in that, by weight percentage, comprising: phenyl pyrazoles raw insecticide medicine 6-30%, and organic solvent 10-40%, emulsifier 15-20%, cosolvent 0-5%, surplus is a water.
Further, said phenyl pyrazoles raw insecticide medicine is a fluorine worm nitrile.
Further, said organic solvent is toluene, xylol, mixed benzene, 1,2,3-trimethylbenzene, kerosene, methyl alcohol, N, one or several compositions in N dimethyl formamide, cyclohexanone, the dimethyl sulfoxide (DMSO).
Further; Said emulsifier is that dibenzyl connects phenyl APEO (agricultural newborn 300#), calcium dodecyl benzene sulfonate (agricultural newborn 500#), styryl phenol APEO (agricultural newborn 600#), one or more compositions in alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700 #), OPEO (OP-10), NPE (NP-10), castor oil and the ethylene oxide condensate (By-125, By-140).
Further, said cosolvent is n-butanol and/or ethylene glycol.
In the technique scheme, fluorine worm nitrile is the active ingredient of this water baseization of invention phenyl pyrazoles hygienic insecticide, act as desinsection; Organic solvent is used for fluorine worm nitrile is dissolved; Emulsifier is used to make oil phase and water to form micro emulsion; The effect of cosolvent is to help the former medicine of dissolving, improves the transparency temperature scope.
The preparation method of water baseization of phenyl pyrazoles hygienic insecticide is dissolved in the former medicine of fluorine worm nitrile in the organic solvent earlier, adds emulsifier then and cosolvent mixes; Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 10-30 minute, promptly get with 100-200 rev/min of rotating speed.
Beneficial effect of the present invention shows as:
1, fluorine worm nitrile is processed water baseization formulation, raw material is simple and easy to, and processing method is simple, improved drug effect simultaneously.
2, reduce environmental pollution, compare the organic solvent of practicing thrift 30%-60% with the missible oil product.
3, having reduced the toxicity of agricultural chemicals, is that per os LD50 is greater than 5000mg/kg through toxicology test fluorine worm nitrile microemulsion toxicity.
4, improved safety, because water instead of part solvent is not flammable, no thermal explosion property, no flash-point below the boiling point has improved safety greatly.
Embodiment
Below will combine embodiment, the present invention will be carried out comparatively detailed explanation.
Embodiment 1
Fluorine worm nitrile microemulsion hygienic insecticide insecticide, fluorine-containing worm nitrile 30%, xylol 20%, calcium dodecyl benzene sulfonate (agricultural newborn 500#) 10%, dibenzyl connect phenyl APEO (agricultural newborn 300#) 10%, and n-butanol is 5%, and surplus is a water.
The preparation method is: earlier the former medicine of fluorine worm nitrile is dissolved in the xylol, adds calcium dodecyl benzene sulfonate (agricultural newborn 500#) then, dibenzyl connects phenyl APEO (agricultural newborn 300#) and n-butanol mixes.Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 10 minutes, promptly get fluorine worm nitrile microemulsion hygienic insecticide with 100 rev/mins of rotating speeds.
Embodiment 2
Fluorine worm nitrile microemulsion hygienic insecticide insecticide, fluorine-containing worm nitrile 6%, xylol 10%, mixed benzene 10%, calcium dodecyl benzene sulfonate (agricultural newborn 500#) 10%, styryl phenol APEO (agricultural newborn 600#) 10%, n-butanol is 5%, surplus is a water.
The preparation method is: earlier the former medicine of fluorine worm nitrile is dissolved in xylol and the mixed benzene, adds calcium dodecyl benzene sulfonate (agricultural newborn 500#), styryl phenol APEO (agricultural newborn 600#) and n-butanol then and mix.Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 15 minutes, promptly get fluorine worm nitrile microemulsion hygienic insecticide with 100 rev/mins of rotating speeds.
Embodiment 3
Fluorine worm nitrile microemulsion hygienic insecticide insecticide, fluorine-containing worm nitrile 8%, xylol 15%, N; N dimethyl formamide 15%, calcium dodecyl benzene sulfonate (agricultural newborn 500#) 15%, alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700 #) 10%; Ethylene glycol is 5%, and surplus is a water.
The preparation method is: earlier the former medicine of fluorine worm nitrile is dissolved in xylol and N, in the N dimethyl formamide, adds calcium dodecyl benzene sulfonate (agricultural newborn 500#), alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700 #) and ethylene glycol then and mix.Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 20 minutes, promptly get fluorine worm nitrile microemulsion hygienic insecticide with 100 rev/mins of rotating speeds.
Embodiment 4
Fluorine worm nitrile microemulsion hygienic insecticide insecticide, fluorine-containing worm nitrile 10%, xylol 15%, N, N dimethyl formamide 15%, calcium dodecyl benzene sulfonate (agricultural newborn 500#) 15%, OPEO (OP-10) 10%, ethylene glycol are 5%, surplus is a water.
The preparation method is: earlier the former medicine of fluorine worm nitrile is dissolved in xylol and N, in the N dimethyl formamide, adds calcium dodecyl benzene sulfonate (agricultural newborn 500#), OPEO (OP-10) and ethylene glycol then and mix.Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 20 minutes, promptly get fluorine worm nitrile microemulsion hygienic insecticide with 150 rev/mins of rotating speeds.
Embodiment 5
Fluorine worm nitrile microemulsion hygienic insecticide insecticide, fluorine-containing worm nitrile 12%, xylol 15%, dimethyl sulfoxide (DMSO) 20%; Calcium dodecyl benzene sulfonate (agricultural newborn 500#) 15%; NPE (NP-10) 15%, n-butanol 2.5%, ethylene glycol are 2.5%, surplus is a water.
The preparation method is: earlier the former medicine of fluorine worm nitrile is dissolved in xylol and the dimethyl sulfoxide (DMSO), adds calcium dodecyl benzene sulfonate (agricultural newborn 500#), NPE (OP-10) and n-butanol, ethylene glycol then and mix.Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 20 minutes, promptly get fluorine worm nitrile microemulsion hygienic insecticide with 200 rev/mins of rotating speeds.
The quality control project indicator of the fluorine worm nitrile microemulsion hygienic insecticide of embodiment 1-5 preparations is seen table 1.
The table 1 fluorine worm nitrile microemulsion quality control project indicator
| Index | 1 | 2 | 3 | 4 | 5 |
| Outward appearance | Transparency liquid | Transparency liquid | Transparency liquid | Transparency liquid | Transparency liquid |
| The transparency temperature scope | 0～50 | 0～50 | 0～50 | 0～50 | 0～50 |
| Low-temperature stability | Qualified | Qualified | Qualified | Qualified | Qualified |
| Heat storage stability | Qualified | Qualified | Qualified | Qualified | Qualified |
| Lasting foaming characteristic ml | 9 | 12 | 11 | 10 | 14 |
| Acidity | 0.2 | 0.3 | 0.2 | 0.1 | 0.3 |
Annotate:
1, transparency temperature scope assay method: get the 10mL sample in the 25mL test tube, stir up and down, cooling gradually on ice bath with stirring rod; Till becoming turbid or freezing, the temperature of this turning point is transparency temperature lower limit t1, again test tube is placed water-bath; Speed with 2 ℃ of per minutes is slowly heated; The temperature of record when becoming turbid, i.e. transparency temperature upper limit t2, then the transparency temperature scope is t1-t2.
2, low-temperature stability assay method GB/T 19137-2003.
3, heat storage stability assay method GB/T 19136-2003.
4, the lasting foaming characteristic assay method of agricultural chemicals HG/T 2467.5-2003.
6, the mensuration of agricultural chemicals acidity value: standard solution of sodium hydroxide titration.
The fluorine worm nitrile microemulsion hygienic insecticide evaluation of pesticide effectiveness data of embodiment 1-5 preparations are seen table 2.
Table 2 fluorine worm nitrile microemulsion hygienic insecticide simulated field drug effect (housefly) is measured the result
| Index | 1 | 2 | 3 | 4 | 5 |
| Indoor harmacological effect KT 50(min) | 1.74 | 1.89 | 1.54 | 1.61 | 1.93 |
| Indoor harmacological effect 24h lethality | 100% | 100% | 100% | 100% | 100% |
| Simulated field 1h rate of knockdown | 98% | 100% | 100% | 100% | 100% |
| Simulated field 24h lethality | 100% | 100% | 100% | 100% | 100% |
| Extension rate | 40 | 40 | 40 | 40 | 40 |
Assay method:
1, GB/T13917.1-2009 " agriculture chemical registration is with the hygienic insecticide indoor pharmacodynamic test and estimate part 1: propellant ".
2, GB/T13917.10-2009 " agriculture chemical registration is with the hygienic insecticide indoor pharmacodynamic test and estimate the 10th part: simulated field ".
The fluorine worm nitrile microemulsion hygienic insecticide of the present invention's preparation through reducing the consumption of organic solvent, replaces with part water, has improved flash-point, has improved safety, has improved Transport Safety.Fluorine worm nitrile microemulsion hygienic insecticide indoor harmacological effect 24h lethality, simulated field 1h rate of knockdown, simulated field 24h lethality are respectively 100% or approach 100%, and drug effect is good.
Above content only is giving an example and explanation that the present invention is done; Under the technical staff in present technique field described specific embodiment is made various modifications or replenish or adopt similar mode to substitute; Only otherwise depart from the design of invention or surmount the defined scope of these claims, all should belong to protection scope of the present invention.
Claims (6)
1. water baseization of a phenyl pyrazoles hygienic insecticide is characterized in that, by weight percentage, comprising: phenyl pyrazoles raw insecticide medicine 6-30%, and organic solvent 10-40%, emulsifier 15-20%, cosolvent 0-5%, surplus is a water.
2. a kind of water baseization of phenyl pyrazoles hygienic insecticide according to claim 1 is characterized in that said phenyl pyrazoles raw insecticide medicine is a fluorine worm nitrile.
3. a kind of water baseization of phenyl pyrazoles hygienic insecticide according to claim 1; It is characterized in that; Said organic solvent is toluene, xylol, mixed benzene, 1; 2,3-trimethylbenzene, kerosene, methyl alcohol, N, one or several compositions in N dimethyl formamide, cyclohexanone, the dimethyl sulfoxide (DMSO).
4. a kind of water baseization of phenyl pyrazoles hygienic insecticide according to claim 1; It is characterized in that; Said emulsifier is that dibenzyl connects phenyl APEO, calcium dodecyl benzene sulfonate, styryl phenol APEO, one or more compositions in alkyl phenol formaldehyde resin polyoxyethylene ether, OPEO, NPE, castor oil and the ethylene oxide condensate.
5. a kind of water baseization of phenyl pyrazoles hygienic insecticide according to claim 1 is characterized in that said cosolvent is n-butanol and/or ethylene glycol.
6. like the preparation method of each described a kind of water baseization of phenyl pyrazoles hygienic insecticide of claim 1-5, it is characterized in that, earlier the former medicine of fluorine worm nitrile is dissolved in the organic solvent, add emulsifier then and cosolvent mixes; Above-mentioned solution is slowly poured in the gauge water, oil phase and water are mixed in the emulsification still, stirred 10-30 minute, promptly get with 100-200 rev/min of rotating speed.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101044858A (en) * | 2007-04-24 | 2007-10-03 | 海南博士威农用化学有限公司 | Compound agricultural chemical containing fipronil, soluble agent and microemulsion |
| JP2008505121A (en) * | 2004-07-01 | 2008-02-21 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Synergistic mixture of anthranilamido invertebrate pest control agents |
| WO2009103901A2 (en) * | 2007-12-21 | 2009-08-27 | Virbac | Pharmaceutical composition containing an n‑phenylpyrazole derivative and glycofurol, use for the preparation of a topical veterinary medicament for combating fleas |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008505121A (en) * | 2004-07-01 | 2008-02-21 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニー | Synergistic mixture of anthranilamido invertebrate pest control agents |
| CN101044858A (en) * | 2007-04-24 | 2007-10-03 | 海南博士威农用化学有限公司 | Compound agricultural chemical containing fipronil, soluble agent and microemulsion |
| WO2009103901A2 (en) * | 2007-12-21 | 2009-08-27 | Virbac | Pharmaceutical composition containing an n‑phenylpyrazole derivative and glycofurol, use for the preparation of a topical veterinary medicament for combating fleas |
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Application publication date: 20121024 |