CN102550549A - Butane fipronil water emulsion and its preparation method - Google Patents
Butane fipronil water emulsion and its preparation method Download PDFInfo
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- CN102550549A CN102550549A CN2012100190933A CN201210019093A CN102550549A CN 102550549 A CN102550549 A CN 102550549A CN 2012100190933 A CN2012100190933 A CN 2012100190933A CN 201210019093 A CN201210019093 A CN 201210019093A CN 102550549 A CN102550549 A CN 102550549A
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- butene
- fipronil
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Abstract
The invention relates to a butene-fipronil water emulsion and its preparation method, which belongs to environmentally friendly pesticide technical field. The butene fipronil water emulsion comprises the following components by weight percentage: 1-30% of butene fipronil, 5-15% of solvent, 5-15%of cosolvent, 3-15% of emulsifier, 3-5% of antifreeze, 0.1-1% of defoamer, 0.01 to 0.5%of thickener and the balance of water. The water emulsion is environmentally friendly, safe and pollution-free, which belongs to the environmentally friendly pesticide formulation. The active ingredient butene fipronil uses a reasonable process to obtain the water emulsion products with stable quality, good dispersion property and storage resistance. Compared with the registered suspending agents, the butene-fipronil water emulsion has the following advantages that: 1, the requirement for the devices is low, the production processing cycle is short, the preparation cost is low; 2, the water emulsion is stable, and difficult to generate the phenomena of agglomeration, lamination and sedimentation, and has the characteristic of storage resistance; 3, the water emulsion has the merits of smaller liquid particles, better dispersibility, stronger adhesion, and equivalent or higher field efficacy than that of the existed suspending agents. The butane fipronil water emulsion can be used for effectively preventing and controlling Chilo suppressalis and other pests in agriculture.
Description
Technical field
The present invention relates to a kind of butene-fipronil aqueous emulsion and preparation method thereof, belong to the environment-protection pesticide technical field.
Background technology
Butene-fipronil is Ruize Farm-Chemicals Co., Ltd., Dalian's independent research and a kind of super-high-efficient novel pesticide that has independent intellectual property right (Chinese patent of the patent No. 02128312.5 has been done detailed disclosing to the general structure and the synthesis preparation method thereof of butene-fipronil).This insecticide is mainly used in the control of paddy rice, fruit tree and vegetable-crop pest-insect, can effectively prevent and treat various pests such as the snout moth's larva of rice, plant hopper, and the mu usage amount is 2～2.5 grams only.
Its mechanism of action is different from main insecticide such as pyrethroid, organic phosphor, carbamate, does not almost produce the chance of cross resistance with the existing insecticide of majority.Therefore, it is the desirable kind of resistance management, can be mixed with other chemical pesticide, is used alternatingly.
Becoming more and more important of the raising of Along with people's quality of life and environmental protection, environment-friendly pesticide preparation will become the main developing direction of agricultural chemicals.
Summary of the invention
The purpose of this invention is to provide agricultural insecticide butene-fipronil aqueous emulsion of a kind of safer, environmental protection and preparation method thereof.
The technical scheme that the present invention adopts is: a kind of component and weight percent content thereof of butene-fipronil aqueous emulsion are: butene-fipronil is 1～30%; Solvent is 5～15%, and cosolvent is 5～15%, and emulsifier is 3～15%; Antifreezing agent is 3～5%; Antifoaming agent is 0.1～1%, and thickener is 0.01～0.5%, and all the other are water.
The said solvent of filling a prescription is selected from one or more in xylol, trimethylbenzene, solvent naphtha, the methylated vegetable oil, and methylated vegetable oil comprises: esterification soybean oil, esterification castor oil, esterification palm wet goods.
The said cosolvent of filling a prescription is selected from one or more in cyclohexanone, phosphate, the pyrrolidones.
The said emulsifier of filling a prescription is selected from one or more the mixture in styryl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether, APES formaldehyde condensation products, AEO, sorbitan fatty acid ester APEO, castor oil polyoxyethylene ether, APES phosphate, calcium dodecyl benzene sulfonate, the EO/PO block polyether phosphate.
The said antifreezing agent of filling a prescription is selected from one or more in ethylene glycol, propane diols, urea, the glycerine.
The said antifoaming agent of filling a prescription is selected from one or more in tributyl phosphate, octanol, the silicone defoaming agent.
Thickener described in the prescription is selected from one or more in gelatin, sodium carboxymethylcellulose, gum Arabic, xanthans, starch phosphate sodium, the hydroxypropul starch ether.
Water is running water or deionized water in the prescription.
The preparation method of above-mentioned butene-fipronil aqueous emulsion: take by weighing the former medicine of butene-fipronil of aequum, be dissolved to clear solution, add emulsifier for mixing more evenly as oil phase with solvent, cosolvent; Taking by weighing suitable quantity of water and in water, adding antifreezing agent is water, under shear conditions, water is slowly added oil phase, shears to form emulsion liquid, adds thickener again, stirs and processes described aqueous emulsion.
The technical indicator that the employing technique scheme obtains product is following:
Butene-fipronil content % 1～30
PH value 4.0～7.0
Pourability is toppled over back residue %≤5
Washing back residue %≤2
Stability of emulsion is qualified
Lasting foaming characteristic (behind the 1min) ml≤50
Low-temperature stability is qualified
Heat storage stability (54 ± 2 ℃, 14d) resolution ratio %≤5
Stability of emulsion test is undertaken by method among the GB/T 1603, with sample with 200 times of standard hard water dilutions, go up behind the 30min no oil slick, down do not have sink oily and be precipitated as qualified.
Above-mentioned butene-fipronil aqueous emulsion is used for cultural control rice-stem borer insect.
The invention has the beneficial effects as follows: this butene-fipronil aqueous emulsion is with water as solvent, and is environmentally friendly, and safety non-pollution belongs to the environment-protection pesticide formulation.The active ingredient butene-fipronil adopts reasonable process technology can access that steady quality, dispersive property are good, the aqueous emulsion product of anti-storage.This butene-fipronil aqueous emulsion relatively has following advantage with the suspending agent that existing registration is used:
1. low for equipment requirements, the production and processing cycle is short, low processing cost.
2. preparation stabilization is difficult for producing phenomenons such as caking, layering, deposition, anti-storage.
3. aqueous emulsion soup particle is littler, and is dispersed better, and adhesion is stronger, and field efficacy quite or be higher than existing suspending agent product.
Embodiment
Specify the present invention with embodiment below.
One: 5% butene-fipronil aqueous emulsion of embodiment
Butene-fipronil 5%, trimethylbenzene 6%, pyrrolidones 9%, styryl phenol polyethenoxy polyethenoxy ether 3%, AEO 2%, ethylene glycol 2%, isooctanol 0.5%, xanthans 0.05%, water supplies 100%.
The preparation method: take by weighing 95% the former medicine 52.8g of butene-fipronil, add trimethylbenzene 60g respectively, pyrrolidones 90g, stirring and dissolving adds styryl phenol polyethenoxy polyethenoxy ether 30g to transparent, AEO 20g, stirring is oil phase; Take by weighing the 726.65g deionized water, ethylene glycol 20g, isooctanol 5g, stirring is water; Under 4000～5000 rev/mins of conditions, water is slowly added oil phase, shear and formed emulsion liquid in 30 minutes, add xanthans 0.5g, stir and process 5% butene-fipronil aqueous emulsion.
Through check analysis: residue 2.7% after toppling over, washing back residue 1.1%, and stability of emulsion is qualified, lasting foaming characteristic 17ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.7% to heat storage stability.
Two: 10% butene-fipronil aqueous emulsions of embodiment
Take by weighing the former medicine 105.6g of 95% butene-fipronil, xylol 60g, N-Methyl pyrrolidone 90g, stirring and dissolving adds styryl phenol polyethenoxy polyethenoxy ether 30g to transparent, APES phosphate 40g, stirring is oil phase; Take by weighing the 590.4g deionized water, propane diols 30g, silicone defoaming agent 4g stir and are water; Under 4000～5000 rev/mins of conditions, water is slowly added oil phase, shear and formed emulsion liquid in 30 minutes, add sodium carboxymethylcellulose 8g, stir and process 10% butene-fipronil aqueous emulsion.
Three: 20% butene-fipronil aqueous emulsions of embodiment
Take by weighing the former medicine 211g of 95% butene-fipronil, 200# solvent naphtha 160g, cyclohexanone 30g stirring and dissolving is extremely transparent, EO/PO block polyether phosphate 60g, alkyl phenol formaldehyde resin polyoxyethylene ether 15g, polyoxyethylene polyoxypropylene glycerin ether 5g, stirring is oil phase; Take by weighing 389g, deionized water, glycerine 40g, stirring is water; Under 3000～4000 rev/mins of conditions, water is slowly added oil phase, shear and formed emulsion liquid in 20～30 minutes, adding hydroxypropul starch ether 10g stirs and processes 20% butene-fipronil aqueous emulsion.
Through check and analysis: residue 2.3% after toppling over, washing back residue 0.8%, and stability of emulsion is qualified, lasting foaming characteristic 13ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.0% to heat storage stability.Prevent that with the butene-fipronil aqueous emulsion among the embodiment one to three the rice-stem borer preventive effect is following:
Show that through test under unit are effective ingredient consumption same case, the preventive effect of the embodiment of the invention butene-fipronil aqueous emulsion control rice-stem borer of participating in the experiment is suitable with the preventive effect of 5% butene-fipronil missible oil.
Claims (9)
1. butene-fipronil aqueous emulsion, it is characterized in that: its component and weight percent content thereof are: butene-fipronil is 1～30%, solvent is 5～15%; Cosolvent is 5～15%; Emulsifier is 3～15%, and antifreezing agent is 3～5%, and antifoaming agent is 0.1～1%; Thickener is 0.01～0.5%, and all the other are water.
2. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said solvent is selected from one or more in xylol, trimethylbenzene, solvent naphtha, the methylated vegetable oil.
3. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said cosolvent is selected from one or more in cyclohexanone, phosphate, the pyridine alkane ketone.
4. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said emulsifier is selected from one or more the mixture in styryl phenol polyethenoxy polyethenoxy ether, phenethyl phenol polyethenoxy ether, APES formaldehyde condensation products, AEO, sorbitan fatty acid ester APEO, castor oil polyoxyethylene ether, APES phosphate, calcium dodecyl benzene sulfonate, the EO/PO block polyether phosphate.
5. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said antifreezing agent is selected from one or more in ethylene glycol, propane diols, urea, the glycerine.
6. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said antifoaming agent is selected from one or more in tributyl phosphate, octanol, the silicone defoaming agent.
7. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said thickener is selected from one or more in gelatin, sodium carboxymethylcellulose, gum Arabic, xanthans, starch phosphate sodium, the hydroxypropul starch ether.
8. the preparation method of butene-fipronil aqueous emulsion according to claim 1; It is characterized in that: comprise the steps: to take by weighing the former medicine of needed butene-fipronil; Be dissolved to clear solution with solvent, cosolvent, add emulsifier for mixing more evenly as oil phase; Taking by weighing suitable quantity of water and in water, adding antifreezing agent is water; Under shear conditions, water slowly added and form emulsion liquid in the oil phase, add thickener again and stir and process said aqueous emulsion.
9. butene-fipronil aqueous emulsion according to claim 1 is characterized in that: said aqueous emulsion is used for cultural control rice-stem borer insect.
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| CN2012100190933A CN102550549A (en) | 2012-01-20 | 2012-01-20 | Butane fipronil water emulsion and its preparation method |
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Cited By (2)
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| CN104642401A (en) * | 2015-02-03 | 2015-05-27 | 沈阳农业大学 | Flufiprole oily agent for preventing and controlling locusts and preparation method thereof |
| CN106879585A (en) * | 2017-03-10 | 2017-06-23 | 上海交通大学 | Trichoderma brassin lactones wettable powder and its preparation method and application |
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| CN104642401A (en) * | 2015-02-03 | 2015-05-27 | 沈阳农业大学 | Flufiprole oily agent for preventing and controlling locusts and preparation method thereof |
| CN106879585A (en) * | 2017-03-10 | 2017-06-23 | 上海交通大学 | Trichoderma brassin lactones wettable powder and its preparation method and application |
| CN106879585B (en) * | 2017-03-10 | 2020-11-17 | 上海交通大学 | Trichoderma brassinolide wettable powder and preparation method and application thereof |
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Application publication date: 20120711 |