CN101288409A - Fipronil, chlopyrifos and production method thereof - Google Patents

Fipronil, chlopyrifos and production method thereof Download PDF

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Publication number
CN101288409A
CN101288409A CNA2007100143471A CN200710014347A CN101288409A CN 101288409 A CN101288409 A CN 101288409A CN A2007100143471 A CNA2007100143471 A CN A2007100143471A CN 200710014347 A CN200710014347 A CN 200710014347A CN 101288409 A CN101288409 A CN 101288409A
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China
Prior art keywords
worm nitrile
fluorine worm
add
chlorpyrifos
emulsifier
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CNA2007100143471A
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Chinese (zh)
Inventor
姜伟
冯尊岗
张明勇
李任凯
穆香明
孔波
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Individual
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Individual
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Priority to CNA2007100143471A priority Critical patent/CN101288409A/en
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Abstract

The invention relates to the technical field of new dosage form of microemulsion for fipronil and chlorpyrifos composite mixed insecticide, in particular to the fipronil and the chlorpyrifos mixed microemulsion and a production method thereof. The invention aims at providing a composite mixed microemulsion preparation with the fipronil and the chlorpyrifos serving as effective components and a preparation method thereof. The microemulsion preparation of the invention synthesizes and mixes the insecticides of the fipronil and the chlorpyrifos has the advantages that the readily availability and durable effectiveness are enhanced, and the drug resistance that is generated by the continuous use of a single dose to the injurious insects is weakened. The composite mixed microemulsion preparation can be used for comprehensive control of the injurious insects to a plurality of crops such as paddy rice, fruit trees, corns, cottons, tobacco, vegetables, etc.

Description

A kind of fluorine worm nitrile, chlopyrifos and production method thereof
Technical field:
Fluorine worm nitrile, chlorpyrifos mixture insecticide and the microemulsion novel form that the present invention relates to, detailed say so fluorine worm nitrile, chlorpyrifos mixture microemulsion and production method thereof.
Background technology:
Fluorine worm nitrile is wide spectrum, the efficient pesticides of at first being developed by French Rhone-Poulenc, chemical name is: (R, S)-5-amino-1-(2,6-dichloromethyl phenyl)-4-trifluoromethanesulpacidc acidc benzene pyridine-3-nitrile, general (Fipronil) by name, commodity are called Regent (sharp strength spy), are a kind of phenylpyridine insecticides.The product of external registration has: 5% suspending agent, 0.3% granule, 5% seed dressing, 80% water dispersion granule, fluorine worm nitrile preparation have tag, stomach toxicity and systemic action, insecticidal spectrum is wide, can be widely used in the control of insect of various crop such as paddy rice, fruit tree, corn, cotton, tobacco, vegetables, Semiptera, Lepidoptera, coleoptera, thrips insect are had high preventive effect.And there is not cross resistance with conventional organophosphorous pesticide, pyrethrin pesticide, methyl carbamate class agricultural chemicals.But its quick-acting is relatively poor, and single agent uses continuously and be easy to generate resistance, to as shortcomings such as insect effects such as paddy stem borer are undesirable.
Chlopyrifos is wide spectrum, the efficient organophosphorus insecticide of at first being developed by LG-DOW, and chemical name is: zero, zero-diethyl-zero-3,5,6-two chloro-2-pyridine radicals phosphorothioates, its adopted name is: chlorpyrifos, commodity are called Le Siben.External registration has 48.8% missible oil (weight/capacity), chlopyrifos have tag, stomach toxicity and stronger infiltration and fumigation action, insecticidal spectrum is wide, also can be widely used in the control of insect of various crop such as paddy rice, fruit tree, corn, cotton, tobacco, vegetables, Semiptera, Lepidoptera, coleoptera, thrips insect are had high preventive effect.Though drug effect speed is fast, uses continuously and produced resistance for many years.
With above two kinds of pesticide compositionals, both improved quick-acting, increase lasting effect again, alleviated insect is used generation continuously to single agent pesticide resistance simultaneously.Can be used as the integrated control of various crop insects such as paddy rice, fruit tree, corn, cotton, tobacco, vegetables.
Microemulsion is to be matrix with water, and by former medicine dissolving, the microemulsified process forms the stabilising system of even phase.Micella particle diameter in the system is less than optical wavelength, grain fineness is little, because of its auxiliary agent content height, the opening up of its soup, infiltration, wetting, filming function all has and cream preparation and suspending agent, the effective rate of utilization height of its soup, drug effect be missible oil and suspending agent under the same dose 1.2-1.5 doubly.Microemulsion is matrix with water, has also reduced the production cost of agricultural chemicals, helps alleviating the pressure of environmental pollution, to the development green agriculture, keeps ecology and is of great importance.
Summary of the invention:
The purpose of this invention is to provide a kind of is the preparation and preparation method thereof of the complex microemulsion of active ingredient with fluorine worm nitrile, chlopyrifos.
The main technical schemes that the present invention adopts is: replace a large amount of inflammable benzene class organic solvents with water, reduce product toxicity and production cost; Improve the safety of producing and storing and transporting; Make two kinds of mutual synergy of insecticide by prescription screening, by surfactant and add synergist and improve the opening up of medicament, wetting, infiltration, film forming, improve the availability of agricultural chemicals, reduce actual dosage.
Fluorine worm nitrile of the present invention, chlorpyrifos micro emulsion, wherein fluorine worm nitrile, chlopyrifos are main component, mass content in preparation is respectively 1-10% and 20-50%, and other compositions comprise that emulsifier 5-25%, cosolvent 1-15%, synergist 1-10%, stabilizing agent 1-10%, surplus are water.
The emulsifier that the present invention is fit to is one or more the compound that is selected from alkylphenol polyoxyethylene series, agricultural emulsifier NO series, castor oil polyoxyethylene ether series, phenethyl phenol polyethenoxy ether yuban, the dodecyl benzene sulfonate.(newborn BRT-1 emulsifier)
The cosolvent that the present invention is fit to is to be selected from aromatic solvent as toluene, dimethylbenzene etc.; C1-5-unit alcohol as: methyl alcohol, ethanol, n-butanol etc.; Acetone, cyclohexanone, dimethyl sulfoxide (DMSO) or have similar features or the material of performance in any one or two kinds of above compositions.
The synergist that the present invention is fit to be selected from Butacide, synergy phosphorus, Octachlorodipropyl Ether, azone, thiophene ketone, fast T, fatty alcohol-polyoxyethylene ether have similar features or the surface reactive material of performance in one or more composition.
The stabilizing agent that the present invention is fit to be selected from ethylene glycol, polyethylene glycol, glycerine, urea have similar characteristic or the material of performance in any one or two kinds of above compositions.
The water that the present invention is fit to is to be selected from running water, underground water, deionized water, the distilled water any one.
This microemulsion can be with known preparation method preparation, and chlopyrifos, fluorine worm nitrile are dissolved in the middle of the flux, adds emulsifier, add or do not add synergist, add or do not add stabilizing agent, stir, slowly add excess water, be stirred well to even phase transparency liquid, both got fluorine worm nitrile, chlorpyrifos micro emulsion.The method that this microemulsion uses is spraying, and working concentration regards thing as and controlling object uses 100-500ppm usually.Below in conjunction with embodiment the present invention is made more specific description, but embodiment does not limit the present invention, the percentage among the embodiment is mass percent.
Embodiment 1
12% fluorine worm nitrile, chlorpyrifos micro emulsion
Fluorine worm nitrile 2%
Chlopyrifos 10%
Toluene 5%
DMF 5%
BRT-1 15%
Water adds to 100%
Preparation method: after fluorine worm nitrile, the former medicinal toluene of chlopyrifos and DMF dissolving, add the BRT-1 emulsifier, stir, slowly add excess water, be stirred well to even phase transparency liquid.
Embodiment 2
22% fluorine worm nitrile, chlorpyrifos micro emulsion
Fluorine worm nitrile 2%
Chlopyrifos 20%
Toluene 15%
DMF 5%
BRT-1 18%
Water adds to 100%
Preparation method: after fluorine worm nitrile, the former medicinal toluene of chlopyrifos and DMF dissolving, add the BRT-1 emulsifier, stir, slowly add excess water, be stirred well to even phase transparency liquid.
Embodiment 3
45% fluorine worm nitrile, chlorpyrifos micro emulsion
Fluorine worm nitrile 5%
Chlopyrifos 40%
Toluene 5%
DMF 15%
N-butanol 5%
BRT-1 18%
Water adds to 100%
Preparation method: after fluorine worm nitrile, the former medicinal toluene of chlopyrifos, DMF and n-butanol dissolving, add the BRT-1 emulsifier, stir, slowly add excess water, be stirred well to even phase transparency liquid.
The microemulsion physicochemical property of preparation is as follows:
Outward appearance: light yellow or pale brown look is spared the phase transparency liquid
Transparency temperature zone :-5-60 ℃
Ageing stability: seasoning was stablized in 2 years under the normal temperature
Low-temperature stability :-10-0 ℃ of two weeks are not stratified, do not separate out, and are haze-free
Stability of emulsion: qualified (200 times of liquid)
Microemulsion of the present invention has the following advantages with missible oil and suspending agent ratio:
1, a large amount of minimizing organic solvent has reduced production cost and to the pollution of environment, product is not Inflammable, non-explosive, produce storing safety.
2, active ingredient size ratio cream preparation was little more than 100 times after medicament was converted water, to wearing of target Ability is stronger thoroughly; The wettability of soup improves 20-30 doubly than missible oil, the plate-out ability of soup is good, Effective rate of utilization height, drug effect are better than missible oil and suspension formulation. Through field test, 30% chlopyrifos micro emulsion Agent, 40% chlorpyrifos ec are done the test of pesticide effectiveness to 1500 times of apple tree woolly aphids, and behind the medicine 15 days, preventive effect Quite, illustrate that preventive effect is still suitable in the situation of active constituent content than missible oil low 25%.
3, product composite after, slowed down to a great extent the resistance to the action of a drug of insect, improved insecticidal spectrum, More be conducive to the integrated control of insect.
4, micro emulsion is take water as matrix, alleviated in the cream preparation organic solvent to the wound of young fruit and tender leaf Evil has improved safety in utilization.

Claims (6)

1, a kind of fluorine worm nitrile, its feature of chlorpyrifos micro emulsion comprise following composition and content (by mass)
Fluorine worm nitrile 1-10%
Chlopyrifos 20-50%
Emulsifier 5-25%
Cosolvent 0-15%
Synergist 0-10%
Stabilizing agent 0-10%
Excess water
2, a kind of microemulsion according to claim 1, it is characterized in that described emulsifier is selected from one or more the compound in alkylphenol polyoxyethylene series, agricultural emulsifier NO series, castor oil polyoxyethylene ether series, phenethyl phenol polyethenoxy ether yuban, the dodecyl benzene sulfonate.(newborn BRT-1 emulsifier)
3, microemulsion according to claim 1 is characterized in that, described cosolvent is selected from aromatic solvent as toluene, dimethylbenzene etc.; The C1-5 monohydric alcohol is as methyl alcohol, ethanol, n-butanol etc.; Acetone, cyclohexanone, any one or two kinds of above compositions of dimethyl sulfoxide (DMSO).
4, fluorine worm nitrile according to claim 1, chlorpyrifos micro emulsion, it is characterized in that described synergist is selected from one or more the composition in Butacide, synergy phosphorus, Octachlorodipropyl Ether, azone, thiophene ketone, fast T, organic silicon surfactant, the fatty alcohol-polyoxyethylene ether active substance.
5, fluorine worm nitrile according to claim 1, chlorpyrifos micro emulsion is characterized in that, described stabilizing agent is selected from ethylene glycol, polyethylene glycol, interior triol, any one or two kinds of above compositions.
6, a kind of fluorine worm nitrile, chlorpyrifos micro emulsion production method, it is characterized in that, chlopyrifos and fluorine worm nitrile are dissolved in the middle of the cosolvent, add emulsifier, add or do not add synergist, add or do not add stabilizing agent, stir, slowly add excess water, be stirred well to even phase transparency liquid, both got fluorine worm nitrile, chlorpyrifos micro emulsion.
CNA2007100143471A 2007-04-21 2007-04-21 Fipronil, chlopyrifos and production method thereof Pending CN101288409A (en)

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CNA2007100143471A CN101288409A (en) 2007-04-21 2007-04-21 Fipronil, chlopyrifos and production method thereof

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CN101288409A true CN101288409A (en) 2008-10-22

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2464449A (en) * 2008-09-05 2010-04-21 Norbrook Lab Ltd A topical ectoparasiticide composition
US8404735B2 (en) 2009-03-18 2013-03-26 Omnipharm Limited Parasiticidal formulation
CN103271082A (en) * 2013-06-19 2013-09-04 北京燕化永乐农药有限公司 Insect killing composition
CN107751238A (en) * 2017-11-17 2018-03-06 青海省农林科学院 One kind preventing and treating rape flea beetle, stem weevil seed coat agent
CN108208015A (en) * 2018-02-08 2018-06-29 武汉楚强生物科技有限公司 A kind of agricultural chemicals suspension agent and its preparation method and application

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2464449A (en) * 2008-09-05 2010-04-21 Norbrook Lab Ltd A topical ectoparasiticide composition
GB2464449B (en) * 2008-09-05 2011-10-12 Norbrook Lab Ltd A topical ectoparasticide composition
US8404735B2 (en) 2009-03-18 2013-03-26 Omnipharm Limited Parasiticidal formulation
US8580837B2 (en) 2009-03-18 2013-11-12 Fidopharm, Inc. Parasiticidal formulation
US8829038B2 (en) 2009-03-18 2014-09-09 Velcera, Inc. Parasiticidal formulation
CN103271082A (en) * 2013-06-19 2013-09-04 北京燕化永乐农药有限公司 Insect killing composition
CN107751238A (en) * 2017-11-17 2018-03-06 青海省农林科学院 One kind preventing and treating rape flea beetle, stem weevil seed coat agent
CN108208015A (en) * 2018-02-08 2018-06-29 武汉楚强生物科技有限公司 A kind of agricultural chemicals suspension agent and its preparation method and application

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Open date: 20081022