CN111134113B - Ethiprole-dicyclopropanate oil suspending agent and preparation method and application thereof - Google Patents

Ethiprole-dicyclopropanate oil suspending agent and preparation method and application thereof Download PDF

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CN111134113B
CN111134113B CN201911392640.0A CN201911392640A CN111134113B CN 111134113 B CN111134113 B CN 111134113B CN 201911392640 A CN201911392640 A CN 201911392640A CN 111134113 B CN111134113 B CN 111134113B
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ethiprole
suspending agent
oil
oil suspending
dicyclopropyl
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CN111134113A (en
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马斌武
王永生
吴亚清
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Jiangsu Zhongshan new material Co.,Ltd.
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N31/00Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/08Oxygen or sulfur directly attached to an aromatic ring system
    • A01N31/16Oxygen or sulfur directly attached to an aromatic ring system with two or more oxygen or sulfur atoms directly attached to the same aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N53/00Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention provides an ethiprole-dicyclopropanate oil suspending agent and a preparation method and application thereof, and relates to the technical field of pesticides. The dicyclopropanetin oil suspending agent consists of the following components in percentage by weight: 5-20% of ethiprole, 2-20% of dicyclopropyl, 1-3% of tert-butylhydroquinone, 5-25% of surfactant, 0.1-10% of thickener and solvent for complementing the weight to 100%. The preparation method of the oil suspending agent comprises the following steps: the ethiprole and the dicyclopropanesefat original drug, the tert-butyl hydroquinone, the surfactant, the thickening agent and the solvent are mixed, and the ethiprole and the dicyclopropanesefat oil suspending agent are obtained after sanding and filtering. The oil suspending agent has the advantages of overcoming the technical problem that ethiprole and dicyclopropanate are easy to decompose due to ingenious formula, obviously enhancing the stability, avoiding the defect of excessive medicine loss during medicine application and reducing the medicine application times.

Description

Ethiprole-dicyclopropanate oil suspending agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to an ethiprole-dicyclopropionate oil suspending agent as well as a preparation method and application thereof.
Background
The ethiprole is an aryl pyrazole pesticide, can prevent and control sweet potato whiteflies and scale insects, and has the characteristics of high efficiency, small dosage, long lasting period, safety to crops, low toxicity to fishes and small influence on ecological environment. Can be used for preventing and treating homoptera, thysanoptera, diptera and lepidoptera pests. Its inhibitory effect on insects is manifested by affecting the molting and reproduction of insects. For sanitary pests of mosquitoes and flies, the later 4 th instar larvae can be killed in the pupation stage by using the low-dose product, and the formation of adults is inhibited. It also has systemic transfer activity, and can affect larva hidden on the back of leaf.
The dicyclopropyl caterpillar is found in a biological fermentation product, is a propylene (pyropenes) compound, is a brand-new pesticide for preventing and treating piercing-sucking mouthpart pests, and has the characteristics of quick response, high efficiency, broad spectrum and the like. The dicyclopropyl cinquel can quickly inhibit the feeding of insects, and effectively reduce virus diseases and bacterial diseases transmitted by insect vectors; has excellent insecticidal (aphid, whitefly and the like) effect; the lasting period is long; effective against a variety of insect states of pests (ineffective against eggs); the leaf penetration capability is excellent; it has unique dosage form and is rain wash resistant. The amitraz disturbs the function of the chord organ of the insect, so that the insect loses the induction on gravity, balance, sound, position, motion and the like, and the insect is deaf, loses coordination and direction feeling, cannot eat, loses water and finally dies due to hunger.
The oil suspending agent is one or more than one effective pesticide ingredients (at least one of which is a solid original drug) and forms a high-dispersion stable suspension system in a non-aqueous dispersion medium, and the development of the oil suspending agent is rapidly developed from the later 70 s to 80 s in the 20 th century. Compared with water suspending agent, wettable powder, water dispersible granule and other formulations, the water dispersible granule has the advantages of good permeability, strong adhesion and the like, and greatly improves the biological activity of the preparation. However, the prior art lacks the oil suspending agent of ethiprole and dicyclopropyl.
Disclosure of Invention
The invention aims to provide the ethiprole-dicyclopropionate oil suspending agent, and the suspending agent overcomes the technical problem that the ethiprole and the dicyclopropionate are easy to decompose due to ingenious formula, obviously enhances the stability, avoids the defect of excessive medicine loss during medicine application, and reduces the medicine application times.
The purpose of the invention is realized by adopting the following technical scheme.
The ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight: 5-20% of ethiprole, 2-20% of dicyclopropyl, 1-3% of tert-butylhydroquinone, 5-25% of surfactant, 0.1-10% of thickener and solvent for complementing the weight to 100%.
In a preferred technical scheme, the solvent is one or a mixture of more than two of corn oil, soybean oil, methyl oleate and cottonseed oil.
In a preferred technical scheme, the thickening agent is one or a mixture of more than two of magnesium aluminum silicate, organic bentonite and white carbon black.
In a preferred technical scheme, the surfactant is one or a mixture of more than two of alkylphenol ethoxylates, oleic acid polyoxyethylene ether and castor oil polyoxyethylene ether.
The invention also provides a preparation method of the ethiprole-dicyclopropionate oil suspending agent, which comprises the following steps: the ethiprole and the dicyclopropanesefat original drug, the tert-butyl hydroquinone, the surfactant, the thickening agent and the solvent are mixed, and the ethiprole and the dicyclopropanesefat oil suspending agent is obtained after sanding and filtering.
In a preferred technical scheme, the solvent is selected from one or more than two of corn oil, soybean oil, methyl oleate and cottonseed oil.
In a preferred technical scheme, the thickening agent is one or a mixture of more than two of magnesium aluminum silicate, organic bentonite and white carbon black.
The invention also provides application of the ethiprole-dicyclopropyl cycloate oil suspending agent in prevention and treatment of aphids and whiteflies.
The ethiprole-dicyclopropanetate oil suspending agent is convenient to use, can be diluted by water or oil when in use, and can adopt various application modes according to requirements: 1. diluting with oil or water by 1-10 times, and spraying with ultra-low volume technology; 2. diluting with water by 10-100 times, and spraying with low dosage; 3. diluting with water by 1000 times and then adopting conventional spraying.
The ethiprole and dicyclopropanate oil suspending agent overcomes the technical problem that the ethiprole and the dicyclopropanate are easy to decompose, and has the following beneficial effects due to ingenious formula: the pesticide has stable physical and chemical properties, is not easy to decompose and deteriorate, has less oil precipitation after long-term storage, does not bottom, increases the adsorption and permeability of the pesticide to a target, improves the effective utilization rate of the pesticide, can greatly improve the control effect on target pests, avoids the defect of excessive pesticide loss during pesticide application, and reduces the pesticide application times. In addition, high-content ethiprole is easy to generate austenite curing in water to cause agglomeration, and the oil suspending agent has the advantages that the formula is ingenious, the concentrations of the ethiprole and the dicyclopropanate in the oil suspending agent can reach 20 percent, and the concentration is obviously higher than that of the prior art, so the use and production cost is obviously reduced. The ethiprole-dicyclopropyl esterase oil suspending agent can be used for preventing and controlling sucking mouthparts pests such as aphids, whiteflies and the like, and has long lasting period; is effective to various insect states of pests, and especially improves the killing effect to eggs. The control experiment on trialeurodes vaporariorum shows that the control effect can reach more than 90 percent in 1 to 15 days after the pesticide is applied, and is far higher than that of the existing ethiprole and dicyclopropyl pesticide preparation.
Detailed Description
Example A10% Ethoxynitrile-Dicyclobuterol oil suspension
The 10% ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight;
Figure BDA0002345411660000031
adding ethiprole, crude drug of diproprionate, tert-butyl hydroquinone, surfactant, thickener and solvent into a reaction kettle according to a formula proportion, mixing for 20min under high shear, grinding by a sand mill until the particle size D95 is less than 3 microns, and filtering to obtain the oil suspending agent.
Example two 18% Ethoxynitrile-Dicyclobuterol oil suspension
The 18% ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight:
Figure BDA0002345411660000032
Figure BDA0002345411660000041
an 18% oil suspension of ethiprole and dicyclopropionate was prepared as in example 1.
EXAMPLE three 24% Ethonitrile-Dicyclobuterol oil suspension
The 24% ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight:
Figure BDA0002345411660000042
a24% oil suspension of ethiprole and dicyclopropionate was prepared as in example 1.
Example four 30% Ethonitrile-Dicyclobuterol oil suspension
The 30% ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight:
Figure BDA0002345411660000043
a30% oil suspension of ethiprole and dicyclopropionate was prepared as in example 1.
Example five 40% Ethanenitrile, Dipropylenectasin oil suspension
The 40% ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight:
Figure BDA0002345411660000051
a40% oil suspension of ethiprole and dicyclopropionate was prepared as in example 1.
Example 6 stability and efficacy of ethiprole-dicyclopropionate oil suspending agent
(1) Contrast ethiprole-dicyclopropyl tetramat oil suspending agent
The contrast ethiprole-dicyclopropyl caterpillar ester oil suspending agent comprises the following components in percentage by weight:
Figure BDA0002345411660000052
(2) stability of ethiprole-dicyclopropyl caterpillar ester oil suspending agent
And (3) test treatment: the 18% ethiprole and diproprionate oil suspending agent and the control ethiprole and diproprionate oil suspending agent in the embodiment 2 are respectively stored for 30 days at normal temperature, 14 days at 54 ℃ and 14 days at 0 ℃, and the oil bleeding condition, the discoloration condition, the bottom formation condition and the decomposition rate of active ingredients (diproprionate and ethiprole) are examined.
TABLE 1 stability of the respective suspending agents
Figure BDA0002345411660000053
Figure BDA0002345411660000061
As can be seen from Table 1, the stability of the suspending agent in the second embodiment of the invention is significantly better than that of the control ethiprole-dicyclopropionate oil suspending agent no matter the suspending agent is stored for 30 days at normal temperature, stored for 14 days at 54 ℃ or stored for 14 days at 0 ℃. In particular, in the process of thermal storage, compared with the ethiprole and dicyclopropionate oil suspending agent, the bottom is harder, the discoloration is severe, the decomposition rate of the dicyclopropionate is 8.2 percent, the decomposition rate of the ethiprole is 4.3 percent, and the decomposition is severe. Therefore, the suspending agent of the second embodiment of the present invention has very good stability.
(2) Field control of each suspending agent
Spraying the second oil suspending agent and a control ethiprole-dicyclopropionate oil suspending agent according to a set dilution multiple, and uniformly spraying 30 kilograms of diluted agent to eggplant plants per mu. The death rate of the eggplant whitefly is investigated 1 day, 7 days and 15 days after the pesticide application. And respectively investigating the base number of the whitefly before the pesticide and the number of live insects after the pesticide treated by each liquid medicine, and calculating to obtain the dead insect rate.
TABLE 2 field control of Agents against Aleggplants whitefly
Figure BDA0002345411660000062
Note: the 2000-fold liquid in the table 2 refers to the medicament obtained by diluting the oil suspending agent by 2000-fold water, and the rest is analogized.
In addition, the second oil suspending agent of the embodiment of the invention and the control ethiprole-dicyclopropionate oil suspending agent are sprayed according to the set dilution times, and the diluted agent is sprayed to pepper plants uniformly by using 30 kilograms of diluted agent per mu. Pepper aphid mortality was investigated 1, 7 and 15 days after dosing. And respectively investigating the base number of aphids before the pesticide and the number of live insects after the pesticide in each treatment, and calculating to obtain the dead insect rate.
TABLE 3 field control of Pepper aphids
Figure BDA0002345411660000071
Note: in table 3, the 2000-fold liquid refers to the agent obtained by diluting the oil suspending agent by 2000-fold water, and the rest is analogized.
As can be seen from tables 2 and 3, the control ethiprole-dicyclopropyl oil suspending agent and the second oil suspending agent of the embodiment show consistent trend of field control effect on the trialeurodes vaporariorum and the pepper aphid one day after the application, namely, no obvious difference exists; however, the control effect difference is very obvious after 15 days of application, and the control effect of the second oil suspending agent in the embodiment is far superior to that of a control ethiprole and dicyclopropanate oil suspending agent, because the stability of the oil suspending agent is obviously superior to that of the control ethiprole and dicyclopropanate oil suspending agent in a field environment, and the sustained exertion of active ingredients of the oil suspending agent is facilitated, so that the application times in the field can be obviously reduced.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (5)

1. The ethiprole-dicyclopropyl caterpillar ester oil suspending agent is characterized by comprising the following components in percentage by weight: 5-20% of ethiprole, 2-20% of dicyclopropyl, 1-3% of tert-butyl hydroquinone, 5-25% of surfactant, 0.1-10% of thickening agent and solvent for complementing the weight to 100%; the solvent is one or a mixture of more than two of corn oil, soybean oil, methyl oleate and cottonseed oil; the thickening agent is one or a mixture of more than two of magnesium aluminum silicate, organic bentonite and white carbon black; the surfactant is selected from one or a mixture of more than two of alkylphenol polyoxyethylene, oleic acid polyoxyethylene and castor oil polyoxyethylene.
2. The method for preparing the ethiprole-dicyclopropyl carbamate oil suspending agent as claimed in claim 1, which is characterized by comprising the following steps: the ethiprole and the dicyclopropanesefat original drug, the tert-butyl hydroquinone, the surfactant, the thickening agent and the solvent are mixed, and the ethiprole and the dicyclopropanesefat oil suspending agent is obtained after sanding and filtering.
3. The method according to claim 2, wherein the solvent is one or more selected from the group consisting of corn oil, soybean oil, methyl oleate and cotton seed oil.
4. The method according to claim 3, wherein the thickener is one or more selected from the group consisting of magnesium aluminum silicate, organobentonite, and silica.
5. The use of the ethiprole-dicyclopropyl amitraz oil suspending agent of claim 1 for preventing and controlling aphids and whiteflies.
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