CN111903686A - Pesticide compound mixture microemulsion containing dimehypo and fosthiazate and production method thereof - Google Patents
Pesticide compound mixture microemulsion containing dimehypo and fosthiazate and production method thereof Download PDFInfo
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- CN111903686A CN111903686A CN202010851581.5A CN202010851581A CN111903686A CN 111903686 A CN111903686 A CN 111903686A CN 202010851581 A CN202010851581 A CN 202010851581A CN 111903686 A CN111903686 A CN 111903686A
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- fosthiazate
- dimehypo
- water
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/26—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-nitrogen bonds
- A01N57/32—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-nitrogen bonds containing heterocyclic radicals
Abstract
The invention discloses a pesticide compound mixture microemulsion containing dimehypo and fosthiazate and a production method thereof, wherein the pesticide compound mixture microemulsion comprises the following raw materials in percentage by weight: 5-30% of dimehypo, 5-30% of fosthiazate, 5-30% of solvent, 5-30% of emulsifier, 1-8% of antifreezing agent and 16-32% of water. The production steps are as follows: step 1: dissolving fosthiazate with cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution; step 2: uniformly mixing the bisultap mother liquor, the antifreezing agent and water to obtain a transparent clear solution; and step 3: and (3) dropwise adding the transparent clear solution obtained in the step (2) into the transparent clear solution obtained in the step (1) while stirring, so that the system is gradually converted from a water-in-oil phase to an oil-in-water phase, and thus the microemulsion is prepared. The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate has long lasting period, has a certain synergistic effect, reduces the use amount of the pesticide, reduces the production cost, reduces the economic burden of farmers and has little pollution to the environment.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a pesticide compound mixture microemulsion containing dimehypo and fosthiazate and a production method thereof.
Background
Bisultap, a nereistoxin insecticide, is a nerve poison that appears to be sluggish, slow-moving, incapacitating, halting development, softening, paralyzing, and dying after insects contact and take the insecticide. The bisultap has strong systemic action and can be absorbed and conducted by leaves, roots and the like of crops. It is used for preventing and treating insect pest of vegetables, rice, wheat, fruit trees, etc. The insecticidal double-effect is one of few created pesticides in China, the dosage form of the insecticidal double-effect is mainly 18-30% of water, and brilliant effects are created in pesticide history. However, with the advent of extended active monosultap with higher activity and content, dimehypo has become a byproduct of the monosultap production process, and the market is gradually replaced by monosultap. A large amount of bisultap byproduct becomes a bottleneck problem restricting the development of monosultap manufacturers, and new application of bisultap is urgently found.
The fosthiazate has contact killing and systemic effects, has low toxicity, and has special effects on root-knot nematodes, root-rot (pratylenchus) nematodes, cyst nematodes, stem nematodes and the like. The insecticidal composition is used for controlling many pests of ground Thysanoptera, Lepidoptera, Coleoptera and Diptera, and is also very effective for pests at underground roots; it is also effective on many mites, has good killing activity on various nematodes, and has good systemic killing activity on resistant pests (such as aphids) generated by common insecticides. The fosthiazate is most effective when mixed in soil immediately after being applied, can be directly applied to the soil surface before the crops are planted, and can also be used when the crops are sowed. Worldwide, the economic losses due to nematode damage are as high as $ 1570 billion, with a market opportunity of approximately $ 30 billion. In the united states, 75% of tomato, 70% of cotton, and 60% of grape fields are damaged by nematodes. The annual cost of controlling nematode damage in major crops is estimated to be between $ 10 and $ 800 per hectare, depending on the level of damage and cultivation requirements. Similarly, the annual loss caused by the harm of the nematodes in China is up to 700 million yuan, the market potential is huge, and because the pesticide for preventing and controlling the nematodes is lacked in the market at present, the pesticide is mostly adopted for preventing and controlling, the cost is higher, the economic burden of farmers is increased, and the pollution is serious.
Disclosure of Invention
The invention aims to provide a pesticide compound mixture microemulsion containing dimehypo and fosthiazate and a production method thereof, the pesticide compound mixture microemulsion containing dimehypo and fosthiazate has long lasting period, has certain synergistic effect, reduces the usage amount of pesticide, reduces the production cost, lightens the economic burden of farmers, has little pollution to the environment and solves the problems provided in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 5-30% of dimehypo, 5-30% of fosthiazate, 5-30% of solvent, 5-30% of emulsifier, 1-8% of antifreezing agent and 16-32% of water.
Further, the feed comprises the following raw materials in percentage by weight: 10-25% of dimehypo, 5-20% of fosthiazate, 10-20% of solvent, 15-25% of emulsifier, 1-5% of antifreezing agent and 20-28% of water.
Further, the emulsifier is selected from at least one of alkylphenol formaldehyde resin polyoxyethylene ether, calcium dodecylbenzene sulfonate, phenethyl phenol polyoxyethylene ether, tristyrylphenol polyoxypropylene polyoxyethylene block polymer and castor oil polyoxyethylene ether, and the ternary combination of alkylphenol formaldehyde resin polyoxyethylene ether, calcium dodecylbenzene sulfonate and tristyrylphenol polyoxypropylene polyoxyethylene block polymer is preferred.
Further, the solvent is selected from at least one of cyclohexanone, pyrrolidone, dimethylformamide, S-150 and S-100, and cyclohexanone is preferred.
Further, the antifreezing agent is at least one selected from ethylene glycol, propylene glycol and glycerol, and preferably ethylene glycol.
The invention provides another technical scheme: the production method of the pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following steps:
step 1: dissolving fosthiazate with cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution;
step 2: uniformly mixing the bisultap mother liquor, the antifreezing agent and water to obtain a transparent clear solution;
and step 3: and (3) dropwise adding the transparent clear solution obtained in the step (2) into the transparent clear solution obtained in the step (1) while stirring, so that the system is gradually converted from a water-in-oil phase to an oil-in-water phase, and thus the microemulsion is prepared.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts the bisultap and the fosthiazate to prepare the microemulsion for preventing and controlling the nematodes by dry-land crop root irrigation, can delay the generation of drug resistance of pests to medicaments, has certain synergistic effect, reduces the using amount of the pesticides, has low bisultap price and fosthiazate price, reduces the production cost, lightens the economic burden of farmers and has little pollution to the environment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 20% of dimehypo, 20% of fosthiazate, 10% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 3% of ethylene glycol and 27% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 8: 5: 7.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the 40% pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate.
Example 2
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: the pesticide composition comprises 25% of dimehypo, 20% of fosthiazate, 10% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 3% of ethylene glycol and 22% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 9: 4: 7.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the 45% pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate.
Example 3
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 15% of dimehypo, 15% of fosthiazate, 30% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 3% of ethylene glycol and 17% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 5: 7: 3.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 30% of the dimehypo and the fosthiazate.
Example 4
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 20% of dimehypo, 10% of fosthiazate, 28% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 3% of ethylene glycol and 19% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 9: 4: 7.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 30% of the dimehypo and the fosthiazate.
Example 5
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 10% of dimehypo, 20% of fosthiazate, 27% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 3% of ethylene glycol and 20% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 6: 4: 10.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 30% of the dimehypo and the fosthiazate.
Example 6
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 5% of dimehypo, 30% of fosthiazate, 20% of cyclohexanone, 20% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 1% of ethylene glycol and 24% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 8: 5: 7.
dissolving the fosthiazate in the weight ratio by using pyrrolidone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 35 percent of the dimehypo and the fosthiazate.
Example 7
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 10% of dimehypo, 10% of fosthiazate, 30% of cyclohexanone, 18% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 8% of ethylene glycol and 24% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: phenethylphenol polyoxyethylene ether ═ 8: 5: 5.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the 20% pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate.
Example 8
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 30% of dimehypo, 5% of fosthiazate, 5% of cyclohexanone, 30% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 14% of ethylene glycol and 16% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: phenethylphenol polyoxyethylene ether ═ 9: 5: 6.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 35 percent of the dimehypo and the fosthiazate.
Example 9
The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate comprises the following raw materials in percentage by weight: 18% of dimehypo, 18% of fosthiazate, 18% of cyclohexanone, 18% of (alkylphenol formaldehyde resin polyoxyethylene ether + calcium dodecyl benzene sulfonate + triphenylethylphenol polyoxypropylene polyoxyethylene block polymer), 4% of ethylene glycol and 24% of water.
Wherein, alkylphenol formaldehyde resin polyoxyethylene ether: calcium dodecylbenzenesulfonate: triphenylethylphenol polyoxypropylene polyoxyethylene block polymer ═ 7: 5: 6.
dissolving the fosthiazate in the weight ratio by using cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution (oil phase); uniformly mixing the bisultap mother liquor, ethylene glycol and water to obtain a transparent clear solution (water phase); and dropwise adding the water phase into the oil phase while stirring to gradually convert the water-in-oil phase into the oil-in-water phase, thereby preparing the pesticide compound mixture microemulsion containing 35 percent of the dimehypo and the fosthiazate.
The physical and chemical properties of the microemulsions prepared in examples 1-9 are as follows:
appearance: a light yellow homogeneous transparent liquid.
Transparent temperature region: -5 to 65 ℃.
Stability over time: can be stored for 2 years at normal temperature.
Low-temperature stability: no delamination, no precipitation and no turbidity at the temperature of minus 10 to 0 ℃ for two weeks.
Emulsion stability: qualified (200 times liquid).
Now, indoor mixed agent synergy toxicity measurement is carried out on the pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate prepared in the embodiments 1 to 9 of the invention, and an LC50 value, a toxicity regression equation and a co-toxicity coefficient are calculated. The cotoxicity coefficient is calculated by the Sun Yunpei method.
The co-toxicity coefficient CTC is 100 x actual combined virulence index/theoretical combined virulence index.
When the co-toxicity coefficient is obviously more than 100, the synergistic effect is shown; near 100, indicating additive effect; obviously less than 100, indicating antagonism.
The co-toxicity coefficient pairs of the pesticidal mixture microemulsions containing bisultap and fosthiazate prepared in examples 1 to 9 and the conventional insecticides 1 and 2 are shown in the following table.
As can be seen from the above table, the microemulsion of the pesticide compound mixture containing dimehypo and fosthiazate prepared in examples 1 to 9 has a co-toxicity coefficient significantly greater than 100, and all have synergistic effects, wherein the co-toxicity coefficients of examples 1, 3, 7 and 9 all reach more than 150, and all have significant synergistic effects, especially the co-toxicity coefficient of example 3 is the highest, and the synergistic effects are the most significant, compared with the existing microemulsion of the pesticide compound mixture containing dimehypo and fosthiazate, in which the co-toxicity coefficients of pesticide 1 and pesticide 2 are only close to 100, and only some additive effects are provided, and the effect of preventing and controlling nematodes is significantly weaker than that of the microemulsion of the pesticide compound mixture containing dimehypo and fosthiazate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (6)
1. The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate is characterized by comprising the following raw materials in percentage by weight: 5-30% of dimehypo, 5-30% of fosthiazate, 5-30% of solvent, 5-30% of emulsifier, 1-8% of antifreezing agent and 16-32% of water.
2. The pesticide compound mixture microemulsion containing the dimehypo and the fosthiazate as claimed in claim 1, which is characterized by comprising the following raw materials in percentage by weight: 10-25% of dimehypo, 5-20% of fosthiazate, 10-20% of solvent, 15-25% of emulsifier, 1-5% of antifreezing agent and 20-28% of water.
3. The microemulsion of claim 1 wherein the emulsifier is at least one member selected from the group consisting of alkylphenol formaldehyde polyoxyethylene ether, calcium dodecylbenzene sulfonate, phenethylphenol polyoxyethylene ether, tristyrylphenol polyoxypropylene polyoxyethylene block polymer, and castor oil polyoxyethylene ether, preferably a ternary combination of alkylphenol formaldehyde polyoxyethylene ether, calcium dodecylbenzene sulfonate, tristyrylphenol polyoxypropylene polyoxyethylene block polymer.
4. The microemulsion of claim 1 wherein the solvent is at least one selected from cyclohexanone, pyrrolidone, dimethylformamide, S-150, S-100, preferably cyclohexanone.
5. The microemulsion of claim 1 wherein the anti-freezing agent is at least one of ethylene glycol, propylene glycol and glycerol, preferably ethylene glycol.
6. The method for producing the pesticidal combination mixture microemulsion containing dimehypo and fosthiazate according to claim 1, comprising the steps of:
step 1: dissolving fosthiazate with cyclohexanone, adding an emulsifier, and uniformly mixing to obtain a transparent clear solution;
step 2: uniformly mixing the bisultap mother liquor, the antifreezing agent and water to obtain a transparent clear solution;
and step 3: and (3) dropwise adding the transparent clear solution obtained in the step (2) into the transparent clear solution obtained in the step (1) while stirring, so that the system is gradually converted from a water-in-oil phase to an oil-in-water phase, and thus the microemulsion is prepared.
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| EP3254564A1 (en) * | 2015-02-06 | 2017-12-13 | Ishihara Sangyo Kaisha, Ltd. | Insecticidal composition and insect pest control method |
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2020
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1839695A (en) * | 2005-03-28 | 2006-10-04 | 北京华京五方实用纳米科技开发有限公司 | Aqueous pesticide and preparation method thereof |
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Application publication date: 20201110 |