CN101700017B - Ethiprole emulsion in water and preparation method thereof - Google Patents

Ethiprole emulsion in water and preparation method thereof Download PDF

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Publication number
CN101700017B
CN101700017B CN2009101644946A CN200910164494A CN101700017B CN 101700017 B CN101700017 B CN 101700017B CN 2009101644946 A CN2009101644946 A CN 2009101644946A CN 200910164494 A CN200910164494 A CN 200910164494A CN 101700017 B CN101700017 B CN 101700017B
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water
emulsion
ethiprole
solvent
phosphate
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CN101700017A (en
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仇晓锋
景辉
刘晓明
宁昭宇
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Shenzhen Noposion Agrochemicals Co Ltd
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Shenzhen Noposion Agrochemicals Co Ltd
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Abstract

The invention relates to an ethiprole emulsion in water which is characterized by comprising the components by weight percent: 1-30% of ethiprole, 5-15% of solvent, 5-15% of cosolvent, 3-15% of emulsifying agent, 3-5% of antifreeze, 0.1-1% of defoaming agent, 0.01-0.5% of thickening agent and water supplementing 100%. A preparation method of the ethiprole emulsion in water comprises the steps of: weighing raw ethiprole with the required quantity, and dissolving into transparent solution by the solvent and the cosolvent; adding emulsifying agent into the obtained solution and evenly stirring, and taking the product as oil phase; weighing right amount of water, and adding the antifreeze into the water to be taken as water phase; and finally, under the high shearing condition, slowly adding the oil phase into the water phase to form emulsion, and then adding the thickening agent and evenly stirring to prepare the emulsion in water. The ethiprole emulsion in water can be used for agricultural control of pests such as rice planthopper, etc.

Description

A kind of ethiprole emulsion in water and preparation method thereof
Technical field
The present invention relates to a kind of agricultural insecticide waterborne preparation and preparation method thereof, relate in particular to a kind of aqueous emulsion that contains second worm nitrile.
Background technology
Second worm nitrile, English general Ethiprole by name.It is a kind of novel Insecticidal pyrazolines, insecticidal spectrum light.Disturbing chloride channel through GABA (GABA), is that insect causes death thereby destroy the central nervous system normal activity.This medicine is tightr to the constraint comparison vertebrate of insect GABA chloride channel, thereby very high selection toxicity is arranged.Be mainly used in control thrips, stinkbug, beet tops moth, aphid, plant hopper and locust etc., some aleyrodid is also shown activity, particularly the rice grub green rice bug to extremely difficult control has very strong activity.
Its mechanism of action is different from main insecticide families 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.
The second worm nitrile preparation of China's registration now all is 100 grams per liter suspending agents.Second worm nitrile water-emulsion preparation product does not appear in the newspapers as yet.
Summary of the invention
The purpose of this invention is to provide agricultural insecticide ethiprole emulsion in water of a kind of safer, environmental protection and preparation method thereof.
The ethiprole emulsion in water prescription is formed (by weight percentage):
Second worm nitrile 1~30%, solvent 5~15%, cosolvent 5~15%, emulsifier 3~15%, antifreezing agent 3~5%, antifoaming agent 0.1~1%, thickener 0.01~0.5%, water supplies 100%.
The said solvent of filling a prescription comprises one or more in xylol, trimethylbenzene, solvent naphtha S-200, the methylated vegetable oil, and methylated vegetable oil comprises for example esterification soybean oil, esterification castor oil, esterification palm wet goods.
The said cosolvent of filling a prescription comprises one or more in cyclohexanone, phosphate, the above alcohol of C4, the pyrrolidones.
The said emulsifier of filling a prescription is one or more a composition 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 comprises at least a in ethylene glycol, propane diols, urea, the glycerine.
Antifoaming agent described in the prescription is at least a in tributyl phosphate, octanol, polyoxypropylene oxygen Ethylene Glycol ether, the silicone defoaming agent.
Thickener described in the prescription is at least a in gelatin, sodium carboxymethylcellulose, sodium alginate, carragheen, gum Arabic, xanthans, sodium carboxymethyl starch, starch phosphate sodium, the hydroxypropul starch ether.
Water is running water or deionized water in the prescription.
The preparation method of ethiprole emulsion in water of the present invention: take by weighing the former medicine of second worm nitrile 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, oil phase is slowly added water, shear to form emulsion liquid, add thickener again and stir and process described aqueous emulsion.
Technical target of the product is following:
Second worm nitrile content % 1~30
PH value 4.0~7.0
Pourability: topple 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.
The low-temperature stability test is undertaken by 2.1 " emulsion and homogeneous liquid preparations " among the GB/T 19137-2003.Sample takes out after storing 7d under 0 ± 1 ℃ of condition, returns to room temperature, through mild agitation, should not have visible particle and grease, and then the low-temperature stability of sample is qualified.
The preparation that the present invention obtains is made solvent with water, and is environmentally friendly, and safety non-pollution belongs to the environment-protection pesticide formulation.Active ingredient second worm nitrile of the present invention adopts reasonable process technology can access that steady quality, dispersive property are good, the aqueous emulsion product of anti-storage.
The ethiprole emulsion in water that the present invention obtains compares with the suspending agent that existing registration is used, and following advantage is arranged: 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% ethiprole emulsion in water of embodiment
Second worm nitrile 5%, trimethylbenzene 5%, pyrrolidones 10%, styryl phenol polyethenoxy polyethenoxy ether 3%, AEO 2%, ethylene glycol 2%, isooctanol 0.5%, xanthans 0.05%, water supplies 100%.
Preparation method: take by weighing 92% the former medicine 54.5g of second worm nitrile, add trimethylbenzene 50g, pyrrolidones 100g stirring and dissolving respectively, add styryl phenol polyethenoxy polyethenoxy ether 30g, AEO 20g stirs and is oil phase to transparent; Take by weighing the 724.95g deionized water, ethylene glycol 20g, isooctanol 5g, stirring is water; Under 4000~5000 rev/mins of conditions, oil phase is slowly added water, shear and formed emulsion liquid in 15~20 minutes, add xanthans 0.5g, stir and process 5% ethiprole emulsion in water.
Through check and analysis: residue 3.2% after toppling over, washing back residue 1.3%, and stability of emulsion is qualified, lasting foaming characteristic 21ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 3.5% to heat storage stability.
Two: 10% ethiprole emulsion in water of embodiment
Take by weighing the former medicine 109g of 92% second worm nitrile, xylol 100g, cyclohexanone 60g stirring and dissolving adds styryl phenol polyethenoxy polyethenoxy ether 50g to transparent, and APES phosphate 50g stirs and is oil phase; Take by weighing the 587g deionized water, propane diols 30g, silicone defoaming agent 6g stir and are water; Under 4000~5000 rev/mins of conditions, oil phase is slowly added water, shear and formed emulsion liquid in 20~30 minutes, add sodium carboxymethylcellulose 8g, stir and process 10% ethiprole emulsion in water.
Through check and analysis: residue 2.4% after toppling over, washing back residue 1.7%, and stability of emulsion is qualified, lasting foaming characteristic 18ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.9% to heat storage stability.
Three: 15% ethiprole emulsion in water of embodiment
Take by weighing the former medicine 161.5g of 93% second worm nitrile; Solvent naphtha S-200120g, phosphate 30g, pyrrolidones 30g stirring and dissolving is to transparent; Add sorbitan fatty acid ester APEO 60g; Phenethyl phenol polyethenoxy ether 30g, castor oil polyoxyethylene ether 30g, calcium dodecyl benzene sulfonate 10g stir and are oil phase; Take by weighing the 488.5g deionized water, glycerine 30g stirs and is water; Under 3000~4000 rev/mins of conditions, oil phase is slowly added water, shear and formed emulsion liquid in 20~30 minutes, add the methyl starch sodium 10g that contracts, stir and process 15% ethiprole emulsion in water.
Through check and analysis: residue 2.7% after toppling over, washing back residue 1.3%, and stability of emulsion is qualified, lasting foaming characteristic 13ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.5% to heat storage stability.Four: 20% ethiprole emulsion in water of embodiment
Take by weighing the former medicine 215.5g of 93% second worm nitrile, solvent naphtha S-200160g, n-butanol 30g stirring and dissolving is to transparent; Add N-Methyl pyrrolidone 80g; EO/PO block polyether phosphate 60g, alkyl phenol formaldehyde resin polyoxyethylene ether 15g, polyoxyethylene polyoxypropylene glycerin ether 5g stir and are oil phase; Take by weighing the 384.5g deionized water, glycerine 40g stirs and is water; Under 3000~4000 rev/mins of conditions, oil phase is slowly added water, shear and formed emulsion liquid in 20~30 minutes, adding hydroxypropul starch ether 10g stirs and processes 20% ethiprole emulsion in water.
Through check and analysis: residue 2.5% after toppling over, washing back residue 1.2%, and stability of emulsion is qualified, lasting foaming characteristic 14ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.2% to heat storage stability.Five: 30% ethiprole emulsion in water of embodiment
Take by weighing the former medicine 323g of 93% second worm nitrile; Esterification castor oil 120g, cyclohexanone 100g stirring and dissolving adds pyrrolidones 30g to transparent; Sorbitan fatty acid ester APEO 30g; Polyoxyethylene polyoxypropylene glycerin ether 30g, phenethyl phenol polyethenoxy ether phosphate 20g, castor oil polyoxyethylene ether 10g stir and are oil phase; Take by weighing the 302g deionized water, glycerine 25g stirs and is water; Under 3500~4500 rev/mins of conditions, oil phase is slowly added water, shear and formed emulsion liquid in 30~40 minutes, adding hydroxypropul starch ether 10g stirs and processes 30% ethiprole emulsion in water.
Through check and analysis: residue 3.8% after toppling over, washing back residue 1.7%, and stability of emulsion is qualified, lasting foaming characteristic 19ml, low-temperature stability is qualified, and (54 ± 2 ℃, 14d) resolution ratio is 2.7% to heat storage stability.
Field application implementation example:
Following with the control of the ethiprole emulsion in water among the embodiment one to five paddy rice white-backed planthopper preventive effect:
*Annotate: 100 grams per liter second worm nitrile suspending agents, Bayer crop science company produces, and market is bought.
Show that through test under unit are effective ingredient consumption identical (being 3 gram/mus in the test) situation, the 3rd day preventive effect of embodiment of the invention ethiprole emulsion in water control paddy rice white-backed planthopper of participating in the experiment is all more than 88%, preventive effect was all more than 92% in the 7th day; 1st, 3,7 days preventive effects all quite or be superior to contrasting medicament 100 grams per liter second worm nitrile suspending agents.

Claims (3)

1. ethiprole emulsion in water is characterized in that its component and weight percentage thereof are:
Second worm nitrile 1~30%, solvent 5~15%, cosolvent 5~15%, emulsifier 3~15%, antifreezing agent 3~5%, antifoaming agent 0.1~1%, thickener 0.01~0.5%, water supplies 100%;
Said solvent is one or more in xylol, trimethylbenzene, solvent naphtha S-200, the methylated vegetable oil;
Said cosolvent is one or more in cyclohexanone, phosphate, the above alcohol of C4, the pyrrolidones;
Said emulsifier is one or more a composition 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;
Said antifreezing agent is a kind of in ethylene glycol, propane diols, urea, the glycerine;
Said antifoaming agent is one or more in tributyl phosphate, octanol, polyoxypropylene oxygen Ethylene Glycol ether, the silicone defoaming agent;
Said thickener is one or more in gelatin, sodium carboxymethylcellulose, sodium alginate, carragheen, gum Arabic, xanthans, sodium carboxymethyl starch, starch phosphate sodium, the hydroxypropul starch ether.
2. the preparation method of ethiprole emulsion in water as claimed in claim 1 is characterized in that comprising the steps: to take by weighing the former medicine of second worm nitrile of aequum, is dissolved to clear solution with solvent, cosolvent, adds 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, oil phase is slowly added aqueous phase and form emulsion liquid, add thickener again and stir and process said aqueous emulsion.
3. aqueous emulsion as claimed in claim 1 is characterized in that, said aqueous emulsion can be used for cultural control rice hoppers insect.
CN2009101644946A 2009-08-01 2009-08-01 Ethiprole emulsion in water and preparation method thereof Active CN101700017B (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102318630A (en) * 2011-07-19 2012-01-18 陕西美邦农药有限公司 Insecticidal composition containing novaluron and ethiprole
CN104365591B (en) * 2014-10-23 2016-04-06 深圳市科玺化工有限公司 A kind of pesticide synergistic agent, preparation method and application thereof
MX2019001266A (en) * 2016-07-29 2019-07-08 Basf Se A method for controlling insects where an alkoxylated glycerol is applied to soil.
CN106614550A (en) * 2016-12-28 2017-05-10 江苏钟山化工有限公司 Additive used for producing pesticide emulsion in water and preparation and application thereof
CN107372523A (en) * 2017-08-11 2017-11-24 江西天祥通用航空股份有限公司 A kind of ethiprole thermal fog and its preparation method and application

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CN101480185A (en) * 2009-01-05 2009-07-15 深圳诺普信农化股份有限公司 Pesticide composition with synergistic insecticidal action and use thereof

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CN101480185A (en) * 2009-01-05 2009-07-15 深圳诺普信农化股份有限公司 Pesticide composition with synergistic insecticidal action and use thereof

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