CN101606521B - Synergic acaricide - Google Patents
Synergic acaricide Download PDFInfo
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- CN101606521B CN101606521B CN 200910108818 CN200910108818A CN101606521B CN 101606521 B CN101606521 B CN 101606521B CN 200910108818 CN200910108818 CN 200910108818 CN 200910108818 A CN200910108818 A CN 200910108818A CN 101606521 B CN101606521 B CN 101606521B
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- hesperidene
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Abstract
The invention provides a synergic acaricide which contains an effective amount of spiromesifen, an effective amount of a solvent capable of dissolving the spiromesifen and an effective amount of an emulsifier, and the solvent contains d-hesperidene at least. The synergic acaricide makes use of dissolubility characteristic of stronger dissolving capacity of the d-hesperidene, takes the d-hesperidene as the solvent of the spiromesifen to replace an aromatic solvent with high toxicity and without environmental protection, thus reducing pollution of the acaricide to the environment.In addition, the d-hesperidene as the solvent of the spiromesifen plays functions of dissolving and breaking a waxiness layer on a surface of a destructive acarid body, allows the acaricide to infiltrate into the acarid body more easily and increases quick availability of the spiromesifen, thus improving acarid killing effect. Moreover, the synergic acaricide can be processed to emulsifiable solution, micellar emulsion, aqueous emulsion formulations and the like dosage forms.
Description
Technical field
The invention belongs to pesticide field, relate in particular to a kind of synergic acaricide.
Background technology
Spiral shell mite ester is tetronic acid class miticide (tetronic acid), chemical name: 3-(2,4 dichloro benzene base)-2-oxo-1-oxaspiro [4,5]-last of the ten Heavenly stems-3-alkene 4-base-2,2-dimethyl butyl ester; Molecular formula: C
21H
24C
12O
4Relative molecular weight: 411.32.Spiral shell mite ester has following characteristics:
1, the mechanism of action is unique: mainly suppress the lipogenesis in the pest mite body, it with existing miticide between do not have cross resistance, be applicable to be used for preventing and treating pest mite class to existing miticide generation resistance.
2, the mite spectrum is wide extremely, adaptability is strong.Spirodiclofen against red spider, yellow spider, rust Pi lice, yellow tea mite, carmine spider mite and two-spotted spider mite, etc. have a good control effect, can be used for citrus, grapes and other fruit trees and eggplant, peppers, tomatoes and other tomato Section crops mites treatment.In addition, spiral shell mite ester also has the well double effect of controlling to insects such as pear sucker, oystershell scale and leafhopper classes.
3, the ovum children is double kills: kill ovum effect excellence especially, simultaneously the children is also had good action of contace poison as if mite, though can not kill female one-tenth mite quickly, female one-tenth mite is had good sterilisation-effect.Female one-tenth mite touches the ovum that is produced behind the medicine has 96% can not hatch, and dies from late embryogenesis.
4, the lasting period is long: the lasting period of spiral shell mite ester is long, reaches 40～50 days with 5000 times of full pawls of dilution fluid power control citrus in the production.Spiral shell mite ester sprays application to back resistance of rainwater washing against on the crop leaf, and the spray medicine is met the normal performance that moderate rain does not influence drug effect after 2 hours.
5, low toxicity, low-residual, safety are good.As safe as a house to crop under different temperature conditions, to people and animals and crop safety, low toxicity, be suitable for nuisanceless production.
6, no transreactance property: can use with existing the mixing at present of most of agricultural chemicals (except strong basicity agricultural chemicals and the copper agent).Both can improve the quick-acting of spiral shell mite ester, help the resistance management of mite evil again.
Spiral shell mite ester solvability in water very little (0.05g/1000ml, 20 ℃) is all wanted when therefore being processed into emulsifiable concentrates for agricultural chemicals, aqueous emulsion, microemulsion to use dissolution with solvents to spiral shell mite ester earlier.Therefore, solvent is to produce the essential auxiliary agent of these formulations.At present, spiral shell mite ester mainly is processed into missible oil and uses, and missible oil need be used a large amount of aromatic hydrocarbon solvent production, and environmental pollution is more serious, is all seeking the alternative aromatic hydrocarbon solvent of new environmentally friendly solvent both at home and abroad.Though and present spiral shell mite ester formulation lasting period long (length can reach 60 days), quick-acting is relatively poor relatively.
D-hesperidene (d-limonene) has another name called the D-limonene, hesperidene, citrene or limonene; It is in natural plant essential oils, to have the most a kind of monocycle tangerine terpene; How from the higher orange peel of content, to extract, belong to food additives, have strong volatility and permeability; Use as domestic hygiene insecticide and tea place hesperidene insecticide in the U.S., the wax coat that can destroy the insect body surface causes body fluid outflow dehydration and death.
At present, also do not occur spiral shell mite ester and d-hesperidene are mixed the report that uses.
Summary of the invention
The purpose of the embodiment of the invention is to provide a kind of synergic acaricide, is intended to solve the serious environmental pollution that existing spiral shell mite ester agricultural chemicals uses a large amount of aromatic hydrocarbon solvent production to bring, and the relatively poor problem of quick-acting.
The embodiment of the invention is achieved in that a kind of synergic acaricide, wherein contains: the spiral shell mite ester of effective dose; The solvent that can dissolve spiral shell mite ester of effective dose, this solvent comprises the d-hesperidene at least; And the emulsifier of effective dose.
Compared with prior art, the synergic acaricide of the embodiment of the invention utilizes the strong dissolution characteristics of the solvability of d-hesperidene, the d-hesperidene both as the solvent of spiral shell mite ester, alternative toxicity greatly, the aromatic hydrocarbon solvent of not environmental protection, reduce the pollution of miticide to environment.
In addition, with the solvent of d-hesperidene as spiral shell mite ester, the wax coat surperficial to the polypide of harmful mite has dissolving, destruction, makes miticide get into polypide inside more easily, increased the quick-acting of spiral shell mite ester, thereby improved acaricidal action.Therefore, be used to prevent and treat the mite class with d-hesperidene Compositional acaricide and have obvious synergistic effect.
And, behind d-hesperidene dissolving spiral shell mite ester, can as required miticide be processed into formulations such as missible oil, microemulsion, aqueous emulsion.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
It is compared with prior art a kind of that the embodiment of the invention provides, and not only environmental protection but also quick-acting synergic acaricides particularly, wherein contain:
The spiral shell mite ester of effective dose;
The solvent that can dissolve spiral shell mite ester of effective dose, said solvent comprises the d-hesperidene at least; And
The emulsifier of effective dose.
The emulsifier of the embodiment of the invention does not have special restriction, is the emulsifier that this area is used always, for example can select the mixture of one or more materials in alkylbenzenesulfonate, phosphoric acid ester, the polyethers.
Also comprise the environmental protection organic solvent that except that the d-hesperidene, can dissolve spiral shell mite ester in the solvent of the embodiment of the invention, for example can be selected from ethanol, isopropyl alcohol, glycerine, pyrrolidones, dibasic ester, vegetable oil and the vegetable oil esters class one or more mixture.
The synergic acaricide of the embodiment of the invention can add this area various auxiliary agents commonly used as required, is mixed with the various formulations of pesticide, for example missible oil, microemulsion or aqueous emulsion.If above-mentioned synergic acaricide is when being mixed with missible oil, and wherein solvent can be merely the d-hesperidene, and perhaps d-hesperidene and other can dissolve the mixture of the organic solvent of spiral shell mite ester; If be mixed with microemulsion or aqueous emulsion, also comprise the water that it is mixed with microemulsion or aqueous emulsion requirement in this synergic acaricide.When being mixed with microemulsion, can also add this area cosurfactant commonly used, a kind of or both mixture in ethanol, the isopropyl alcohol for example is to enlarge the warm area scope.When being mixed with aqueous emulsion, can also add this area antifreeze, for example glycerine, isopropyl alcohol etc. commonly used.
More specifically, the synergic acaricide of the embodiment of the invention is mixed with missible oil; In the synergic acaricide gross weight, wherein contain spiral shell mite ester 2～25%, d-hesperidene 3～50%; Emulsifier 3～25%, and 0～92% except that the d-hesperidene, can dissolve spiral shell mite ester other organic solvent.Further; Wherein emulsification dosage is preferably 5～25% (weight); Other organic solvent that except that the d-hesperidene, can dissolve spiral shell mite ester is preferably 0～90% (weight), and this organic solvent can be selected from the mixture of one or more materials in ethanol, isopropyl alcohol, glycerine, pyrrolidones, dibasic ester, vegetable oil and the vegetable oil esters class.This emulsifier is with the mixture of alkyl benzene calcium sulfonate, styrenated phenol APEO, alkyl phenol formaldehyde resin polyoxyethylene ether; Or other emulsifier monomer of knowing with industry technical staff or composite emulsifier all can, in above-mentioned scope, carry out suitable adjustment for reaching emulsifiability to emulsifier proportion preferably the time.The compound method of missible oil is: in the preparation still, add earlier the d-hesperidene, add spiral shell mite ester again, stir about dissolving in 20 minutes back fully adds emulsifier and also supplies solvent, continues to stir to accomplish spiral shell mite emulsifiable concentrate product of the present invention in about 15 minutes.
When the synergic acaricide of the embodiment of the invention is mixed with microemulsion or aqueous emulsion, in the synergic acaricide gross weight, wherein contain spiral shell mite ester 2～25%, d-hesperidene 3～50%, emulsifier 3～25%, 0～92% water.
More specifically, when producing microemulsion, preferably use spiral shell mite ester 5～20% by weight percentage, d-hesperidene 10～30%, emulsifier 5～25%, 0～10% cosurfactant, 15～80% water are prepared.Emulsifier is with the mixture of alkyl benzene calcium sulfonate, styrenated phenol polyoxyethylene ether phosphate and alkyl phenol formaldehyde resin polyoxyethylene ether, or all can with other emulsifier monomer or composite emulsifier that industry technical staff knows.Can enlarge the transparent warm area scope of microemulsion through adding cosurfactant (for example ethanol, isopropyl alcohol etc.) (promptly adds cosurfactant and also can prepare the completion microemulsion; When not with cosurfactant, the transparent warm area of the microemulsion of formation is 10～30 ℃, and when adding cosurfactant, the transparent warm area of the microemulsion of formation is-5～60 ℃, can be in most places of China room temperature storage throughout the year).The compound method of microemulsion is: in the preparation still, add the d-hesperidene earlier; Add spiral shell mite ester again; Add or do not add ethanol or isopropyl alcohol, about fully 20 minutes of stirring and dissolving adds emulsifier then and continued to stir about 10 minutes; Water is supplied the liquid that the continued stir about obtained homogeneous phase transparent in 15 minutes, accomplishes spirodiclofen microemulsion product of the present invention.
More specifically, when producing aqueous emulsion, preferably use spiral shell mite ester 5～20% by weight percentage, d-hesperidene 10～30%, emulsifier 5～25%, antifreeze 0～10%, water 15～80%.Emulsifier adopts the styrenated phenol polyoxyethylene ether phosphate, or other emulsifier monomer of knowing with industry technical staff or composite emulsifier all can, be uniformly dispersed for reaching aqueous emulsion emulsification, in above-mentioned scope, carry out suitable adjustment to emulsifier proportion.The compound method of aqueous emulsion is: in the preparation still, add the d-hesperidene earlier, add spiral shell mite ester again, about fully 20 minutes of stirring and dissolving; Back adding emulsifier continues to stir and accomplished the preparation of oil phase in about 10 minutes, in mixing kettle, adds entry, under agitation slowly adds oil phase; Make oil phase be dispersed in aqueous phase and form the milky aqueous emulsion; Be antifreeze needs, can also add above-mentioned antifreezing agent (for example glycerine), stir and accomplish spirodiclofen water emulsion product of the present invention.
Embodiment 1
Press embodiment 1 prescription in the table 1; In the preparation still, add the d-hesperidene earlier, add spiral shell mite ester again, stir about dissolving in 20 minutes adds emulsifier and supplies solvent in the back fully; Continuing to stir was mixed with 5% spiral shell mite emulsifiable concentrate preparation in about 15 minutes, and each components contents all by percentage to the quality in the prescription.The preparation for preparing is sealed in the 10ml ampere bottle, and each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
Comparative Examples 1
Make solvent with xylol; Be made into 5% spiral shell mite emulsifiable concentrate by Comparative Examples in the table 11 prescription with the method for embodiment 1; The preparation for preparing is sealed in the 10ml ampere bottle; Each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
Embodiment 2
Press embodiment 2 prescriptions in the table 1, in the preparation still, add the d-hesperidene earlier, add spiral shell mite ester again; About fully 20 minutes of stirring and dissolving; The back adds emulsifier continued to stir about 10 minutes, and water is supplied the liquid that the continued stir about obtained homogeneous phase transparent in 15 minutes, is mixed with 5% spirodiclofen microemulsion.The preparation for preparing is sealed in the 10ml ampere bottle, and each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
Comparative Examples 2
Make solvent with xylol; Be made into 5% spirodiclofen microemulsion by Comparative Examples in the table 12 prescription with the method for embodiment 2; The preparation for preparing is sealed in the 10ml ampere bottle; Each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
Embodiment 3
Press embodiment 3 prescriptions in the table 1, in the preparation still, add the d-hesperidene earlier, add spiral shell mite ester again; About fully 20 minutes of stirring and dissolving; Back adding emulsifier continues to stir and accomplished the preparation of oil phase in about 10 minutes, in mixing kettle, adds entry, under agitation slowly adds oil phase; Make oil phase be dispersed in aqueous phase and form the milky aqueous emulsion, the adding antifreezing agent stirs and is mixed with 5% spirodiclofen water emulsion.The preparation for preparing is sealed in the 10ml ampere bottle, and each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
Comparative Examples 3
Make solvent with xylol; Be made into 5% spirodiclofen water emulsion by Comparative Examples in the table 13 prescription with the method for embodiment 3; The preparation for preparing is sealed in the 10ml ampere bottle; Each medicament approved sample was stored 14 days in 0 ℃ of refrigerator and 54 ℃ of baking ovens respectively for 2 bottles, and the analysis content that expires is tried to achieve resolution ratio, and the result is referring to table 1.
The concrete consumption of table 1 embodiment and Comparative Examples
Can find out that from table 1 synergic acaricide of the embodiment of the invention has good stability.
Embodiment 4
Press embodiment 1 method, accomplish 25% spiral shell mite emulsifiable concentrate preparation by following formulated.
Spiral shell mite ester 25%, d-hesperidene 50%, alkyl benzene calcium sulfonate 10%, alkyl phenol formaldehyde resin polyoxyethylene ether 10%, EO/PO block polyether 5%.
Embodiment 5
Press embodiment 1 method, accomplish 20% spiral shell mite emulsifiable concentrate preparation by following formulated.
Spiral shell mite ester 20%, d-hesperidene 15%, dimethyl succinate 30%, ethanol 10%, alkyl benzene calcium sulfonate 8%, alkyl phenol formaldehyde resin polyoxyethylene ether 10%, EO/PO block polyether 7%.
Embodiment 6
Press embodiment 2 methods, accomplish 20% spirodiclofen microemulsion by following formulated.
Spiral shell mite ester 20%, d-hesperidene 20%, ethanol 10%, alkyl benzene calcium sulfonate 11%, alkyl phenol formaldehyde resin polyoxyethylene ether 9%, EO/PO block polyether 8%, water supply 100%.
Embodiment 7
Press embodiment 2 methods, accomplish 15% spirodiclofen microemulsion by following formulated.
Spiral shell mite ester 15%, d-hesperidene 20%, isopropyl alcohol 3%, alkyl phenol formaldehyde resin polyoxyethylene ether 5%, EO/PO block polyether phosphate 18%, water supply 100%.
Embodiment 8
Press embodiment 2 methods, accomplish 2% spirodiclofen microemulsion by following formulated.
Spiral shell mite ester 2%, d-hesperidene 10%, isopropyl alcohol 3%, alkyl phenol formaldehyde resin polyoxyethylene ether 2%, EO/PO block polyether phosphate 8%, water supply 100%.
Embodiment 9
Press embodiment 3 methods, accomplish 25% spirodiclofen water emulsion by following formulated.
Spiral shell mite ester 25%, d-hesperidene 30%, EO/PO block polyether phosphate emulsifier 8%, glycerine 5%, water supply 100%.
Embodiment 10
Press embodiment 3 methods, accomplish 2% spirodiclofen water emulsion by following formulated.
Spiral shell mite ester 2%, d-hesperidene 20%, EO/PO block polyether phosphate emulsifier 5%, water supply 100%.
The virulence test
Use the running water dilution to be certain concentration each medicament of 1～3 in embodiment 1～3 and the Comparative Examples, adopt the virulence of leaf dipping method test medicament tomato Tetranychus cinnabarinus adult.Whole tomato leaf was flooded for 5 seconds in the soup for preparing; Pull the back out and blot the soup of blade rapidly with filter paper; Choosing 20 tomato Tetranychus cinnabarinus adults with little writing brush is placed on and soaks on the tomato leaf that dries behind the medicine; Put into the 9cm culture dish that is lined with filter paper (drip to go up on the filter paper several drip wetting), each culture dish a slice tomato leaf covers the culture dish lid.Each handles 3 repetitions, examines under a microscope result such as table 2 after 72 hours.Death standard: motionless with polypide at microscopically is standard.
Table 2: spiral shell mite ester different dosage form different solvents comparative test result
Find out from table 2, in spiral shell mite ester formulation, introduce the d-hesperidene, greatly improved the mite quick-acting extremely of spiral shell mite ester formulation, have obvious synergistic effect as synergist.Thereby, thereby the consumption that can reduce spiral shell mite ester further reduces production and use cost.In addition; The d-hesperidene can dissolve spiral shell mite ester in the synergic acaricide of the embodiment of the invention, therefore can be fully without the aromatic hydrocarbons organic solvent, and all to adopt the d-hesperidene be solvent or only add a spot of ethanol or other environmentally friendly solvent; Environmental protection, the basic nontoxic pollution-free of solvent.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. synergic acaricide, formulation is a missible oil, in the synergic acaricide gross weight, wherein contains:
2. synergic acaricide, formulation is a microemulsion, in the synergic acaricide gross weight, wherein contains:
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| CN 200910108818 CN101606521B (en) | 2009-07-20 | 2009-07-20 | Synergic acaricide |
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| CN 200910108818 CN101606521B (en) | 2009-07-20 | 2009-07-20 | Synergic acaricide |
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| CN101606521B true CN101606521B (en) | 2012-12-05 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102696655B (en) * | 2012-05-24 | 2013-11-27 | 永农生物科学有限公司 | Compound pesticide composition containing spirodiclofen and its preparation |
| CN106359444A (en) * | 2016-08-20 | 2017-02-01 | 广东中迅农科股份有限公司 | Pesticide adopting D-limonene as synergist |
| CN109221109A (en) * | 2018-09-17 | 2019-01-18 | 福建新农大正生物工程有限公司 | A kind of Synergistic mite killing composition containing avermectin |
| CN109392922A (en) * | 2018-12-11 | 2019-03-01 | 深圳诺普信农化股份有限公司 | A kind of Synergistic mite killing composition containing etoxazole |
| GB202301368D0 (en) * | 2023-01-31 | 2023-03-15 | Upl Mauritius Ltd | Insecticidal composition |
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| WO2007112845A1 (en) * | 2006-03-29 | 2007-10-11 | Bayer Cropscience Ag | Active ingredient combinations with insecticidal and acaricidal properties |
| CN101406185A (en) * | 2008-10-31 | 2009-04-15 | 淄博新农基农药化工有限公司 | Compositional agent for killing insects and mites with synergistic interaction containing spirodiclofen |
| CN101690481A (en) * | 2009-07-07 | 2010-04-07 | 深圳诺普信农化股份有限公司 | Spirodiclofen multiple emulsion and preparation method thereof |
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2009
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007112845A1 (en) * | 2006-03-29 | 2007-10-11 | Bayer Cropscience Ag | Active ingredient combinations with insecticidal and acaricidal properties |
| CN101406185A (en) * | 2008-10-31 | 2009-04-15 | 淄博新农基农药化工有限公司 | Compositional agent for killing insects and mites with synergistic interaction containing spirodiclofen |
| CN101690481A (en) * | 2009-07-07 | 2010-04-07 | 深圳诺普信农化股份有限公司 | Spirodiclofen multiple emulsion and preparation method thereof |
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