CN104412980A - Efficient haloxyfop-methyl and clethodim compound emulsion in water and preparation method and use thereof - Google Patents
Efficient haloxyfop-methyl and clethodim compound emulsion in water and preparation method and use thereof Download PDFInfo
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- CN104412980A CN104412980A CN201310403366.9A CN201310403366A CN104412980A CN 104412980 A CN104412980 A CN 104412980A CN 201310403366 A CN201310403366 A CN 201310403366A CN 104412980 A CN104412980 A CN 104412980A
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Abstract
The invention discloses an efficient haloxyfop-methyl and clethodim compound emulsion in water. The emulsion in water comprises the following raw materials by weight percent: 1%-50% of an efficient haloxyfop-methyl active compound, 1%-70% of a clethodim active compound, 5%-15% of a solvent, 1%-10% of a surfactant, 1%-15% of a stabilizing agent, and the balance of water, wherein the content of the efficient haloxyfop-methyl in the efficient haloxyfop-methyl active compound is 97%, and the content of the clethodim in the clethodim active compound is 93%. The invention further discloses a preparation method and use of the efficient haloxyfop-methyl and clethodim compound emulsion in water. The emulsion in water has the advantages that the herbicide controlling spectrum is enlarged, the obvious gain effect is provided, and the weed controlling effect is obviously improved; the pesticide residue is reduced, and the occurrence and the development of the weed drug resistance are prolonged; the compound emulsion in water is low toxic to human, animal and beneficial organisms, and capable of reducing the phytotoxicity on the crops, and is a low-carbon environment-friendly and safe novel pesticide.
Description
Technical field
The present invention relates to pesticide field, particularly haloxyfop-r-methyl and the composite aqueous emulsion of clethodim and preparation method thereof.
Background technology
Clethodim, has another name called and receives happy leading to.Chemical name: (±)-2-(E)-3-chloroallyloxyamino imino group] and propyl group-5-[2-(ethylmercapto group) propyl group]-3-hydroxy cyclohexylphenyl-2-ketenes, belong to cyclohexenone analog weed killer herbicide.This weed killer herbicide is inner sucting conduction type branches and leaves inorganic agents, has excellent selectivity, has very strong lethal effect to grassy weed, to dicotyledonous crops safety.Absorb rapidly through leaf after cauline leaf process, be transmitted to meristematic tissue, in sensitive plant, suppress the biosynthesis of branched chain fatty acid and flavonoids and work, its cell division is destroyed, suppress the merismatic activity of plant, plant strain growth is delayed, after dispenser, in 1-3 week, plant chlorisis is downright bad, burn with posterior lobe withered and dead, to most of annual and perennial grassy weed is effective.Can decompose rapidly in resistant plant, form polarity, and rapid loss of activity, the very little or non-activity to dicotyledon, nutgrass flatsedge activity.But it is invalid to broad leaved weed.
Clethodim preparation mainly single dose missible oil and the missible oil bactericide compounded with other of current domestic registration.
Haloxyfop-r-methyl, chemical name: 2-[4-(the chloro-pyridine of 5-trifluoromethyl-3--2-oxygen base) phenoxy group] methyl propionate, can be absorbed by the blade of grassy weed very soon after efficient haloxyfop-r-methyl dispenser, and conduct to whole plant, suppress the growth of plant meristematic tissue, thus kill weeds.Lasting period is long, after emerging, all have good preventive effect to the annual of initial stage of tillering, ear and perennial grassy weed.To various broad leaf crop high safety under normal service condition.Excellent herbicidal effect still can be shown under low temperature, drought condition.
Composite missible oil, the suspending agent of the haloxyfop-r-methyl preparation of current domestic registration mainly single dose missible oil, microemulsion, suspending agent and other agricultural chemicals.
The single-dose product of above-mentioned two kinds of agricultural chemicals in use develops immunity to drugs at present, and drug effect declines much than before, and cost accounting also obviously increases; And the agricultural chemicals of organic solvent type in use, because its sprinkling droplet is smaller, drift is far away, very easily pollutes non-sprinkling region, large to the toxicity of warm blooded animal, also stronger to the toxicity of plant; And wetting powder can leave vestiges after spraying, also cause residue of pesticide.
Summary of the invention
In order to solve the problem, the invention provides a kind of haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.The technical problem to be solved in the present invention is: overcome and use that single dose agricultural chemicals easily develops immunity to drugs, usage amount is large, and the existing formulations of pesticide such as missible oil, wetting powder exist easily pollute, toxicity is large, safety is low defect; And provide a kind of good drug efficacy, pesticide resistance little, delay pesticide resistance and produce and be conducive to protection of the environment, the haloxyfop-r-methyl of use safety and the composite aqueous emulsion of clethodim.Aqueous emulsion is the effective ways with water to replace organic solvent, in use, because its sprinkling droplet is larger than missible oil, drift alleviates, the phenomenons such as the vestiges after not having wetting powder to spray, reduce greatly to the toxicity of warm blooded animal, to the toxicity of plant also than missible oil safety.In order to reach above-mentioned technical purpose, technical scheme of the present invention is: haloxyfop-r-methyl and the composite aqueous emulsion of clethodim, it is characterized in that, by weight percentage, be made up of the former medicine 1% ~ 50% of haloxyfop-r-methyl, clethodim technical pesticide 1% ~ 70%, solvent 5% ~ 15%, surfactant 1% ~ 10%, stabilizing agent 1% ~ 15%, water surplus, described each constituent content percentage sum is 100%; In the former medicine of described haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in described clethodim technical pesticide, the content of clethodim is 93%.
In such scheme, the content of the former medicine of described haloxyfop-r-methyl is 3.75% ~ 7.5%, and the content of clethodim technical pesticide is 7.5% ~ 15%.Under this proportioning, the drug effect of controlling weeds of the present invention is best.
In such scheme, the content of described solvent is 12% ~ 15%, and described solvent is any one or multiple mixture in aliphatic alcohols, benzene class, fat hydrocarbon.
Described solvent is ethanol, propyl alcohol, butanols, isobutanol, amylalcohol, hexanol, enanthol, octanol, isooctanol, cyclohexanone, pentane, hexane, cyclohexane, heptane, octane, isooctane, benzinum, 1-METHYLPYRROLIDONE, NOP, the two pyrrolidines-2 of two C12 thiazolinyl, 5-diketone ethane, the two pyrrolidines-2 of two C12 thiazolinyl, 5-diketone hexane, No. 70 solvent naphthas, No. 90 solvent naphthas, No. 120 solvent naphthas, No. 180 solvent naphthas, No. 190 solvent naphthas, No. 200 solvent naphthas, alkyl chain length carbon number is a kind of or several mixture in the alkyl methyl of 6-18.
In such scheme, the content of described surfactant is 5% ~ 8%, and described surfactant is any one or multiple mixture in benzene alkenyl polyether class, castor oil polyethers, Sulfonates.
Described surfactant is polyoxyethylene polyoxypropylene block copolymer, fatty alcohol-polyoxyethylene ether, rope uncle SOPA, phenethyl phenol polyethenoxy formaldehyde condensation products, castor oil polyoxyethylene ether, alkyl polyoxyethylene formaldehyde condensation products, neopelex, dodecyl sodium sulfate, lauryl sodium sulfate, lauryl alcohol polyethylene glycol oxide sodium sulphate, sorbitan fatty acid ester, sodium lignin sulfonate, soil temperature 20, soil temperature 60, soil temperature 65, POLYSORBATE 80, soil temperature 85, span 20, span 40, sorbester p18, a kind of or several mixture in sorbester p17 and alkylphenol polyoxyethylene.
In such scheme, the content of described stabilizing agent is 5% ~ 10%, and described stabilizing agent is any one in ethylene glycol, propane diols, urea, glycerine.
The invention also discloses the preparation method of haloxyfop-r-methyl and the composite aqueous emulsion of clethodim, comprise the following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 1000 ~ 200000 revs/min, and stirring the time of shearing is 1 ~ 30 minute, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
In such scheme, it is 8000 ~ 10000 revs/min that rotating speed is sheared in described stirring, and stirring shear time is 20 ~ 30 minutes.
The invention also discloses the purposes of haloxyfop-r-methyl and the composite aqueous emulsion of clethodim, the weeds of control are annual standing grain herbaceous weed or perennial weed.
In such scheme, the weeds of control comprise: annual bluegrass, caput grass, amur foxtail.
The invention provides advantage of the present invention and beneficial effect is: expand herbicide spectrum, have obvious gain effect, weed control efficacy significantly improves; Reduce residue of pesticide, the generation delaying herbicide resistance and development; To people, animal, beneficial organism low toxicity, the poisoning of medicine to crop can be reduced; The formulations of pesticide of low-carbon environment-friendly, safety.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 3.75% of haloxyfop-r-methyl, clethodim technical pesticide 15%, solvent 12%, surfactant 5%, stabilizing agent 7%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is ethanol, and surfactant is Tween 80, and stabilizing agent is propane diols.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 8000 revs/min, and stirring the time of shearing is 30 minutes, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 2
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 7.5% of haloxyfop-r-methyl, clethodim technical pesticide 7.5%, solvent 15%, surfactant 7%, stabilizing agent 5%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is No. 120 solvent naphthas, and surfactant is castor oil polyoxyethylene ether, and stabilizing agent is ethylene glycol.The product that castor oil polyoxyethylene ether selects Jiangsu Hai'an Petrochemical Plant to produce.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 10000 revs/min, and stirring the time of shearing is 20 minutes, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 3
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 5% of haloxyfop-r-methyl, clethodim technical pesticide 10%, solvent 12%, surfactant 8%, stabilizing agent 9%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is hexane, and surfactant is neopelex, and stabilizing agent is urea.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 9000 revs/min, and stirring the time of shearing is 25 minutes, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 4
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 50% of haloxyfop-r-methyl, clethodim technical pesticide 1%, solvent 15%, surfactant 1%, stabilizing agent 1%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is benzinum, and surfactant is lauryl alcohol polyethylene glycol oxide sodium sulphate, and stabilizing agent is propane diols.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 1000 revs/min, and stirring the time of shearing is 30 minutes, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 5
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 1% of haloxyfop-r-methyl, clethodim technical pesticide 70%, solvent 15%, surfactant 2%, stabilizing agent 3%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is No. 90 solvent naphthas, and surfactant is Tween 80, and stabilizing agent is ethylene glycol.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 200000 revs/min, and stirring the time of shearing is 1 minute, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 6
Haloxyfop-r-methyl and the composite aqueous emulsion of clethodim formulated by the component of following percentage by weight: the former medicine 20% of haloxyfop-r-methyl, clethodim technical pesticide 20%, solvent 5%, surfactant 10%, stabilizing agent 15%, water add to 100%; Wherein, in the former medicine of haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in clethodim technical pesticide, the content of clethodim is 93%; Solvent is 1-METHYLPYRROLIDONE, and surfactant is sodium lignin sulfonate, and stabilizing agent is glycerine.
Above-mentioned formula is prepared according to following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 20000 revs/min, and stirring the time of shearing is 10 minutes, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
Embodiment 7
For examination weeds: annual bluegrass, caput grass and amur foxtail.
Implementation method: adopt indoor biometrics method, every for the seed of each weeds 30 are planted in flowerpot as a process, after weeds are broadcast before seedling or carry out cauline leaf spraying process about growing to for 3.0 ~ 3.5 leaf phases after emerging, observe the victimization state of weeds, and add up test of pesticide effectiveness result.
Experimental result refers to following table:
Experiment shows: haloxyfop-r-methyl can significantly improve preventive effect with clethodim is mixed compared with single dose preventive effect, and to crop safety.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. haloxyfop-r-methyl and the composite aqueous emulsion of clethodim, it is characterized in that, by weight percentage, be made up of the former medicine 1% ~ 50% of haloxyfop-r-methyl, clethodim technical pesticide 1% ~ 70%, solvent 5% ~ 15%, surfactant 1% ~ 10%, stabilizing agent 1% ~ 15%, water surplus, described each constituent content percentage sum is 100%; In the former medicine of described haloxyfop-r-methyl, the content of haloxyfop-r-methyl is 97%, and in described clethodim technical pesticide, the content of clethodim is 93%.
2. haloxyfop-r-methyl according to claim 1 and the composite aqueous emulsion of clethodim, is characterized in that, the content of the former medicine of described haloxyfop-r-methyl is 3.75% ~ 7.5%, and the content of clethodim technical pesticide is 7.5% ~ 15%.
3. haloxyfop-r-methyl according to claim 1 and the composite aqueous emulsion of clethodim, is characterized in that, the content of described solvent is 12% ~ 15%, and described solvent is any one or multiple mixture in aliphatic alcohols, benzene class, fat hydrocarbon.
4. haloxyfop-r-methyl according to claim 1 and the composite aqueous emulsion of clethodim, it is characterized in that, the content of described surfactant is 5% ~ 8%, and described surfactant is any one or multiple mixture in benzene alkenyl polyether class, castor oil polyethers, Sulfonates.
5. haloxyfop-r-methyl according to claim 1 and the composite aqueous emulsion of clethodim, is characterized in that, the content of described stabilizing agent is 5% ~ 10%, and described stabilizing agent is any one in ethylene glycol, propane diols, urea, glycerine.
6. the preparation method of haloxyfop-r-methyl according to claim 1 and the composite aqueous emulsion of clethodim, is characterized in that, comprise the following steps:
1) prepare oil phase: by former for haloxyfop-r-methyl medicine, clethodim technical pesticide and solvent, make the former medicine of haloxyfop-r-methyl, clethodim technical pesticide is dissolved in solvent, obtain uniform oil phase;
2) aqueous phase is prepared: surfactant, stabilizing agent and water are mixed, obtain uniform aqueous phase;
3) aqueous emulsion is prepared: under high-speed stirred is sheared, by step 2) aqueous phase that obtains joins in the oil phase that step 1) obtains, stirring and shearing rotating speed is 1000 ~ 200000 revs/min, and stirring the time of shearing is 1 ~ 30 minute, obtains haloxyfop-r-methyl and the composite aqueous emulsion of clethodim.
7. the preparation method of haloxyfop-r-methyl according to claim 6 and the composite aqueous emulsion of clethodim, is characterized in that, it is 8000 ~ 10000 revs/min that rotating speed is sheared in described stirring, and stirring shear time is 20 ~ 30 minutes.
8. the purposes of haloxyfop-r-methyl and the composite aqueous emulsion of clethodim, is characterized in that, the weeds of control are annual standing grain herbaceous weed or perennial weed.
9. the purposes of haloxyfop-r-methyl according to claim 8 and the composite aqueous emulsion of clethodim, is characterized in that, the weeds of control comprise: annual bluegrass, caput grass, amur foxtail.
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Cited By (1)
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Application publication date: 20150318 |