CN100450357C - Kresoxim-methyl and nimbin mixed microemulsion and preparation method thereof - Google Patents
Kresoxim-methyl and nimbin mixed microemulsion and preparation method thereof Download PDFInfo
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- CN100450357C CN100450357C CNB2006101235264A CN200610123526A CN100450357C CN 100450357 C CN100450357 C CN 100450357C CN B2006101235264 A CNB2006101235264 A CN B2006101235264A CN 200610123526 A CN200610123526 A CN 200610123526A CN 100450357 C CN100450357 C CN 100450357C
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Abstract
The invention discloses a kresoxim-methyl and nimbin composite microemulsion and its preparing process, wherein the microemulsion comprises the following constituents (by weight percent): kresoxim-methyl 5-40%, nimbin 0.2-20%, emulsifying agent 2-20%, penetrating agent 3-15%, auxiliary solvent 2-25%, deionized water 20-75%. The preparing process comprises the steps of stirring and mixing homogeneously, charging deionized water, stewing 4-11 hrs, heating to 42-56 deg C, and fully agitating.
Description
Technical field
The present invention relates to kresoxim-methyl class mixed pesticide technology, relate to kresoxim-methyl and nimbin mixed bactericidal microemulsion and preparation method thereof particularly.
Background technology
In recent years, developed countries such as Great Britain and America are to an organic solvent restriction increasingly stringent in the pesticidal preparations, and dimethylbenzene is disabled to be the solvent of agricultural chemicals.This is a kind of challenge to cream preparation.And wetting powder and pulvis can bring dust pollution, thereby impel agricultural chemicals to develop along efficient (super-high-efficient), low toxicity, safety, biorational and the good direction of Environmental compatibility.People are when strengthening the novel pesticide research and development, pay attention to research and development more to the formulations of pesticide, it wherein is the direction that the pesticides new formulation of base has become world's formulations of pesticide research and development with water, and as a kind of novel water-based pesticide formulation, a kind of so just environment friendly agricultural preparation of microemulsion.
Kresoxim-methyl (kresoxim-methyl) chemical name is (E)-2-methoxyimino-[2-(o-methyl-benzene oxygen methyl) phenyl] methyl acetate; it is the outstanding kind in the methoxy acrylate series bactericidal agent; its mechanism of action uniqueness; the activity that broad-spectrum high efficacy is arranged; vegetables, apple, pears and cereal class cereal crops now have been widely used in; most of diseases that pathomycetes such as imperfect fungus, sac fungi and oomycetes are caused have protection, treat and root out activity, are specially adapted to control of plant disease such as powdery mildew and scab.The formulation of the kresoxim-methyl sterilizing agent product of using on the agricultural chemicals market mainly contains wetting powder and dry suspending agent at present.Kresoxim-methyl is the same with many efficient germicides, and long-term, continuous, single use all can be developed immunity to drugs, and how to prolong the useful life of this medicament, is the problem that people pay close attention to.
Nimbin (azadirachtin) is a kind of secondary compound of tetracyclic triterpenes that comes from plant seal chinaberry, except having very high insecticidal activity, nimbin also has good bactericidal activity, bibliographical information its can rice sheath blight disease, multiple diseases (Liu Yuerong etc., forestry investigation planning) such as peanut rust, powdery mildew of pea, rose mildew, leaf blight, early blight of tomato, rice blast.The effect that nimbin is prevented and treated disease shows as the control frequency of disease development, reduces degree of disease.The nimbin product of using on the at present domestic and international agricultural chemicals market is many based on nimbin emulsion.
But, how on the basis of environmental protection, be that Fungicidal active substance is mixed and makes the microemulsion that wheat powdery mildew, powdery mildew of pea are had an efficient effect and do not see the correlation technique report as yet with kresoxim-methyl and nimbin.
Summary of the invention
The formulation that the objective of the invention is to overcome kresoxim-methyl sterilizing agent product in the prior art is mainly wetting powder and dry suspending agent, the nimbin product is based on nimbin emulsion, the dust pollution that causes and the toxic effect of cream preparation, with antibacterial substance kresoxim-methyl and nimbin is former medicine, a kind of high-efficiency low-toxicity, low cost, environment amenable nuisanceless bactericide are provided, can be used for the kresoxim-methyl of plant powdery mildew controls such as crops, fruits and vegetables and nimbin mixed microemulsion novel form agricultural chemicals, enrich environmentally friendly pesticide species.Another object of the present invention is to provide the preparation method of above-mentioned kresoxim-methyl and nimbin mixed bactericidal microemulsion.
Purpose of the present invention is achieved through the following technical solutions.
A kind of kresoxim-methyl and nimbin mixed bactericidal microemulsion by weight percentage, comprise following component: kresoxim-methyl 5-40%, nimbin 0.2-20%, emulsifier 2-20%, bleeding agent 3-15%, cosolvent 2-25%, deionized water 20-75%.Described emulsifier is selected from one or more in polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, polyoxyethylene glycol and the benzylphenol APEO of nonionic; Perhaps be selected from calcium dodecyl benzene sulfonate, alkyl benzene sulphonate barium salt and the alkyl diphenyl ether sulfonate of anionic one or more.Described bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, octyl phosphate sodium salt and the azone.Described cosolvent is selected from one or more in isoamyl alcohol, acetone, ethyl acetate and the n-butanol.Kresoxim-methyl of the present invention and nimbin mixed bactericidal microemulsion preparation method comprise the steps: earlier kresoxim-methyl, nimbin, emulsifier, bleeding agent and cosolvent to be mixed in high-speed shearing machine by prescription, add deionized water again, mix, left standstill 4-11 hour, be heated to 42-56 ℃, after fully stirring, promptly can be made into kresoxim-methyl and nimbin mixed pesticide microemulsion.
The microemulsion that is mixed of the present invention is the microemulsion that contains fungicide active ingredient kresoxim-methyl, nimbin.
The present invention utilizes the powder neem seed to carry out lixiviate, and extract becomes the concentrated extract that contains nimbin behind concentrating under reduced pressure.
With respect to prior art, the present invention has following advantage:
1, the present invention is a kind of new high-efficiency fungicide preparation, and plant powdery mildew is had significant drug effect.
2, fungicide preparation of the present invention is difficult for producing poisoning to environment, people and animals and other beneficial organism safety, and disease fungus is difficult for it is developed immunity to drugs.Each composition in the mixture can be worked in coordination with in application and be played a role, and has remedied self deficiency of single agent agricultural chemicals, and has reduced the field pesticides amount of application, has reduced the production cost.
3, fungicide preparation bin stability of the present invention is good, can deposit 1 year more than half.
4, fungicide preparation preparing process of the present invention is simple, is suitable for large scale application.
5, except that having significant bactericidal activity, mixture preparation also has the effect of control pest concurrently.
Embodiment
In order to understand the present invention better, the invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1: take by weighing kresoxim-methyl 5.0kg, nimbin 19.5kg, after mixing in high-speed shearing machine with polyoxyethylene nonylphenol ether 3.0kg, sulfosuccinate di-sec-octyl sodium salt 4.0kg, isoamyl alcohol 3.0kg then, add deionized water 65.5kg at last again, mix, left standstill 4 hours, be heated to 48 ℃, after fully stirring, promptly can be made into microemulsion.Use 2500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 91.3%, 83.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 92.2%, 85.8%.
Embodiment 2: take by weighing kresoxim-methyl 5.5kg, nimbin 20.0kg, after mixing in high-speed shearing machine with benzylphenol APEO 3.0kg, octyl phosphate sodium salt 4.0kg, isoamyl alcohol 2.0kg, acetone 1.0kg then, add deionized water 64.5kg at last again, mix, left standstill 5 hours, be heated to 42 ℃, after fully stirring, promptly can be made into microemulsion.Use 2500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 94.3%, 80.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 93.2%, 86.8%.
Embodiment 3: take by weighing kresoxim-methyl 40.0kg, nimbin 0.3kg, after mixing in high-speed shearing machine with polyoxyethylene nonylphenol ether 3.0kg, phenethyl phenol polyethenoxy ether 2.0kg, polyoxyethylene glycol 1.0kg, azone 3.5kg, isoamyl alcohol 4.0kg, ethyl acetate 3.0kg, n-butanol 1.0kg then, add deionized water 42.2kg at last again, mix, left standstill 6 hours, be heated to 55 ℃, after fully stirring, promptly can be made into microemulsion.Use 5000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 92.6%, 90.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 96.1%, 87.6%.
Embodiment 4: take by weighing kresoxim-methyl 39.5kg, nimbin 0.2kg, after mixing in high-speed shearing machine with polyoxyethylene nonylphenol ether 2.5kg, phenethyl phenol polyethenoxy ether 2.0kg, polyoxyethylene glycol 1.5kg, sulfosuccinate di-sec-octyl sodium salt 3.0kg, acetone 2.0kg, ethyl acetate 2.0kg then, add deionized water 47.3kg at last again, mix, left standstill 8 hours, be heated to 54 ℃, after fully stirring, promptly can be made into microemulsion.Use 5000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 93.7%, 91.4%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 96.1%, 88.6%.
Embodiment 5: take by weighing kresoxim-methyl 20.0kg, nimbin 10.0kg, after mixing in high-speed shearing machine with calcium dodecyl benzene sulfonate 10.0kg, octyl phosphate sodium salt 7.0kg, n-butanol 8.0kg then, add deionized water 45.0kg at last again, mix, left standstill 6 hours, be heated to 48 ℃, after fully stirring, promptly can be made into microemulsion.Use 3500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 92.5%, 89.8%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 91.4%, 87.5%.
Embodiment 6: take by weighing kresoxim-methyl 19.5kg, nimbin 10.5kg, after mixing in high-speed shearing machine with alkyl diphenyl ether sulfonate 10.0kg, octyl phosphate sodium salt 3.5kg, azone 4.0kg, n-butanol 8.5kg then, add deionized water 44.0kg at last again, mix, left standstill 5 hours, be heated to 49 ℃, after fully stirring, promptly can be made into microemulsion.Use 3500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 94.5%, 86.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 93.4%, 88.5%.
Embodiment 7: take by weighing kresoxim-methyl 30.0kg, nimbin 15.0kg, after mixing in high-speed shearing machine with polyoxyethylene glycol 4.0kg, benzylphenol APEO 6.0kg, sulfosuccinate di-sec-octyl sodium salt 5.0kg, azone 3.0kg, ethyl acetate 11.0kg then, add deionized water 26.0kg at last again, mix, left standstill 8 hours, be heated to 53 ℃, after fully stirring, promptly can be made into microemulsion.Use 4200 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 92.3%, 91.6%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 93.4%, 84.5%.
Embodiment 8: take by weighing kresoxim-methyl 31.5kg, nimbin 15.5kg, after mixing in high-speed shearing machine with polyoxyethylene glycol 4.0kg, benzylphenol APEO 6.0kg, octyl phosphate sodium salt 3.5kg, sulfosuccinate di-sec-octyl sodium salt 1.5kg, azone 3.0kg, ethyl acetate 10.0kg then, add deionized water 25.0kg at last again, mix, left standstill 11 hours, be heated to 50 ℃, after fully stirring, promptly can be made into microemulsion.Use 4200 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 5th day and 10 days behind the wheat powdery mildew medicine is respectively 94.5%, 95.6%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 95.2%, 88.5%.
Embodiment 9: take by weighing kresoxim-methyl 10.0kg, nimbin 7.5kg, after mixing in high-speed shearing machine with polyoxyethylene glycol 8.0kg, benzylphenol APEO 9.0kg, octyl phosphate sodium salt 3.0kg, azone 5.0kg, ethyl acetate 4.0kg, n-butanol 2.5kg then, add deionized water 51.0kg at last again, mix, left standstill 11 hours, be heated to 44 ℃, after fully stirring, promptly can be made into microemulsion.Use 2500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 5th day and 10 days behind the wheat powdery mildew medicine is respectively 98.9%, 93.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 97.9%, 87.2%.
Embodiment 10: take by weighing kresoxim-methyl 9.0kg, nimbin 8.0kg, after mixing in high-speed shearing machine with polyoxyethylene glycol 4.0kg, benzylphenol APEO 6.0kg, octyl phosphate sodium salt 5.0kg, azone 10.0kg, ethyl acetate 6.0kg, isoamyl alcohol 2.5kg, acetone 1.5kg then, add deionized water 48.0kg at last again, mix, left standstill 9 hours, be heated to 46 ℃, after fully stirring, promptly can be made into microemulsion.Use 2500 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 5th day and 10 days behind the wheat powdery mildew medicine is respectively 96.8%, 95.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 95.1%, 82.8%.
Embodiment 11: take by weighing kresoxim-methyl 35.0kg, nimbin 17.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 3.0kg, benzylphenol APEO 3.0kg, sulfosuccinate di-sec-octyl sodium salt 1.5kg, octyl phosphate sodium salt 4.5kg, azone 2.0kg, acetone 3.0kg, n-butanol 8.0kg then, add deionized water 23.0kg at last again, mix, left standstill 10 hours, be heated to 42 ℃, after fully stirring, promptly can be made into microemulsion.Use 4000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 12 days behind the wheat powdery mildew medicine is respectively 99.5%, 94.6%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 98.4%, 96.6%.
Embodiment 12: take by weighing kresoxim-methyl 32.0kg, nimbin 12.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 3.0kg, benzylphenol APEO 7.5kg, sulfosuccinate di-sec-octyl sodium salt 1.5kg, octyl phosphate sodium salt 4.5kg, azone 2.5kg, acetone 3.0kg, n-butanol 4.0kg then, add deionized water 30.0kg at last again, mix, left standstill 10 hours, be heated to 45 ℃, after fully stirring, promptly can be made into microemulsion.Use 3200 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 12 days behind the wheat powdery mildew medicine is respectively 99.2%, 94.8%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 97.3%, 94.2%.
Embodiment 13: take by weighing kresoxim-methyl 38.0kg, nimbin 5.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 4.0kg, benzylphenol APEO 3.0kg, polyoxyethylene glycol 2.0kg, polyoxyethylene nonylphenol ether 2.0kg, sulfosuccinate di-sec-octyl sodium salt 2.0kg, azone 5.0kg, acetone 3.0kg, isoamyl alcohol 3.0kg then, add deionized water 33.0kg at last again, mix, left standstill 9 hours, be heated to 49 ℃, after fully stirring, promptly can be made into microemulsion.Use 3000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 6th day and 12 days behind the wheat powdery mildew medicine is respectively 89.1%, 92.7%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 96.5%, 90.4%.
Embodiment 14: take by weighing kresoxim-methyl 25.0kg, nimbin 20.0kg, after mixing in high-speed shearing machine with alkyl benzene sulphonate barium salt 9.0kg, sulfosuccinate di-sec-octyl sodium salt 3.0kg, octyl phosphate sodium salt 6.0kg, azone 5.0kg, acetone 6.0kg then, add deionized water 26.0kg at last again, mix, left standstill 4 hours, be heated to 43 ℃, after fully stirring, promptly can be made into microemulsion.Use 3200 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 93.2%, 87.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 99.8%, 89.7%.
Embodiment 15: take by weighing kresoxim-methyl 7.0kg, nimbin 16.0kg, after mixing in high-speed shearing machine with calcium dodecyl benzene sulfonate 4.5kg, alkyl benzene sulphonate barium salt 3.0kg, octyl phosphate sodium salt 7.5kg, ethyl acetate 13.0kg then, add deionized water 49.0kg at last again, mix, left standstill 10 hours, be heated to 52 ℃, after fully stirring, promptly can be made into microemulsion.Use 2800 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 89.8%, 87.0%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 87.1%, 85.3%.
Embodiment 16: take by weighing kresoxim-methyl 12.0kg, nimbin 13.0kg, after mixing in high-speed shearing machine with calcium dodecyl benzene sulfonate 5.5kg, alkyl benzene sulphonate barium salt 3.0kg, alkyl diphenyl ether sulfonate 2.5kg, azone 6.5kg, n-butanol 12.0kg then, add deionized water 45.5kg at last again, mix, left standstill 5 hours, be heated to 56 ℃, after fully stirring, promptly can be made into microemulsion.Use 3000 times of liquid of said preparation to carry out field control effectiveness test, the control efficiency of the 7th day and 14 days behind the wheat powdery mildew medicine is respectively 88.3%, 83.5%, the control efficiency of the 7th day and 14 days behind the powdery mildew of pea medicine is respectively 89.6%, 82.0%.
The foregoing description shows that kresoxim-methyl of the present invention and nimbin mixed pesticide microemulsion are a kind of new high-efficiency fungicide preparations, to the control efficiency excellence of wheat powdery mildew and powdery mildew of pea.And this microemulsion is base with water, overcome the shortcoming that wetting powder and pulvis bring dust pollution, to environment, people and animals and other beneficial organism safety, be difficult for producing poisoning, and disease fungus is difficult for it is developed immunity to drugs.Each composition in the mixture can be worked in coordination with in application and be played a role, and has remedied self deficiency of single agent agricultural chemicals, and has reduced the field pesticides amount of application, has reduced the production cost.In addition, microemulsion bin stability of the present invention is good, can deposit 1 year more than half, and its preparation technology is simple, is suitable for large scale application.
Claims (2)
1, a kind of kresoxim-methyl and nimbin mixed bactericidal microemulsion is characterized in that by weight percentage, comprise following component: kresoxim-methyl 5-40%, nimbin 0.2-20%, emulsifier 2-20%, bleeding agent 3-15%, cosolvent 2-25%, deionized water 20-75%; Described emulsifier is selected from one or more in polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, polyoxyethylene glycol and the benzylphenol APEO of nonionic; Perhaps be selected from calcium dodecyl benzene sulfonate, alkyl benzene sulphonate barium salt and the alkyl diphenyl ether sulfonate of anionic one or more; Described bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, octyl phosphate sodium salt and the azone; Described cosolvent is selected from one or more in isoamyl alcohol, acetone, ethyl acetate and the n-butanol.
2, described kresoxim-methyl of claim 1 and nimbin mixed bactericidal microemulsion preparation method, it is characterized in that comprising the steps: earlier kresoxim-methyl, nimbin, emulsifier, bleeding agent and cosolvent being mixed in high-speed shearing machine by prescription, add deionized water again, mix, left standstill 4-11 hour, be heated to 42-56 ℃, after fully stirring, promptly can be made into kresoxim-methyl and nimbin mixed bactericidal microemulsion.
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| CN101961018A (en) * | 2010-10-20 | 2011-02-02 | 华南理工大学 | Flubendiamide and azadirachtin compound pesticide microemulsion as well as preparation method thereof |
| CN102047884A (en) * | 2010-10-20 | 2011-05-11 | 华南理工大学 | Aconitine plant source insecticidal micro emulsion and preparation method thereof |
| CN105309488A (en) * | 2014-06-25 | 2016-02-10 | 陕西美邦农药有限公司 | Bactericidal composition containing polygonum cuspidatum extract and azoxystrobin or kresoxim-methyl |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0988790A1 (en) * | 1998-09-25 | 2000-03-29 | American Cyanamid Company | Fungicidal mixtures |
| CN1276161A (en) * | 2000-04-27 | 2000-12-13 | 华南农业大学 | Plant-type nimbin insecticide |
| JP2004010492A (en) * | 2002-06-03 | 2004-01-15 | Nippon Soda Co Ltd | Mixed fungicide composition having reinforced potency and used for agriculture and horticulture |
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2006
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0988790A1 (en) * | 1998-09-25 | 2000-03-29 | American Cyanamid Company | Fungicidal mixtures |
| CN1276161A (en) * | 2000-04-27 | 2000-12-13 | 华南农业大学 | Plant-type nimbin insecticide |
| JP2004010492A (en) * | 2002-06-03 | 2004-01-15 | Nippon Soda Co Ltd | Mixed fungicide composition having reinforced potency and used for agriculture and horticulture |
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