CN116746580A - Ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, preparation method and application thereof - Google Patents

Ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, preparation method and application thereof Download PDF

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Publication number
CN116746580A
CN116746580A CN202310740379.9A CN202310740379A CN116746580A CN 116746580 A CN116746580 A CN 116746580A CN 202310740379 A CN202310740379 A CN 202310740379A CN 116746580 A CN116746580 A CN 116746580A
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China
Prior art keywords
terbuthylazine
acetochlor
isooctyl
drop
weeding
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CN202310740379.9A
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Chinese (zh)
Inventor
刘跃怡
崔晶
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Jilin Jinqiu Pesticide Co ltd
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Jilin Jinqiu Pesticide Co ltd
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Priority to CN202310740379.9A priority Critical patent/CN116746580A/en
Publication of CN116746580A publication Critical patent/CN116746580A/en
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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
    • A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
    • A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
    • A01N39/04—Aryloxy-acetic acids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G22/00—Cultivation of specific crops or plants not otherwise provided for
    • A01G22/20—Cereals
    • 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
    • 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
    • A01N25/30—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 characterised by the surfactants
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/26—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
    • 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P13/00—Herbicides; Algicides

Abstract

The invention provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which is characterized by comprising the following preparation components: 2, 4-isooctyl drop, terbuthylazine, acetochlor and dispersing agent; an emulsifying agent; a stabilizer; a dispersion medium; other auxiliary agents; water; wherein the stabilizer comprises vitamin E polyethylene glycol succinate and modified silica. According to the invention, 2, 4-isooctyl drop, terbuthylazine and acetochlor are compounded in a specific proportion, so that the weeding range is enlarged, the weeding effect is improved, and the weeding composition has the advantages of quick weeding, thorough weeding and low toxicity; the particle size obtained in the grinding preparation process of the specific stabilizer is small, and the suspension rate is high; according to the invention, the proper emulsifier is selected, and the characteristics of the raw materials are considered, so that the weeding performance of the product is excellent, and the growth and development of crops are not influenced.

Description

Ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, preparation method and application thereof
Technical Field
The invention relates to the technical field of agriculture, in particular to a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, a preparation method and application thereof.
Background
Corn is an economic crop widely planted in China, and is often planted in spring with a plurality of weed invasion planting areas such as crabgrass, barnyard grass, green bristlegrass and the like, and the corn can occupy more than 90% of the planting area when serious, so that weed control is necessary.
The prior art and the product show a fatigue trend aiming at corn weeds, and the long-term use of a single herbicide leads to serious drug resistance of partial weeds such as crabgrass, abutilon, field bindweed, horsetail, black nightshade and the like in the whole country; it is known that 65 weeds and 233 organisms are resistant to atrazine worldwide. The conventional dosage is difficult to kill weeds, and excessive use of the herbicide can cause phytotoxicity to corns. And enterprises also repeatedly match old products such as atrazine, acetochlor, nicosulfuron, mesotrione and the like, and few new products appear in the market.
The phenoxy carboxylic acid herbicide is a hormone herbicide, has systemic property, can be quickly absorbed by roots and leaves of plants and is transmitted to the whole body of the plants, so that the concentration of hormone in weeds is too high, and further the cell growth and metabolism of the plants are affected.
Chinese patent CN112088887B discloses a weeding suspending emulsion for sedge crops, a preparation method, application and an application method thereof, and by compounding prometryn, metolachlor and flumioxazin according to a specific proportion, the weeding suspending emulsion has high control efficiency on annual weeds which come out of soil, also has high control efficiency on partial weeds which come out of soil during application, and has high safety on cyperus esculentus. However, metabolites migrate to soil, surface water and groundwater after degradation of metolachlor, and at the beginning of 2023, the french food, environmental and occupational health safety agency (Anses) announced on their grids that procedures for canceling the main use of the herbicide active substance metolachlor for crop protection have been initiated with the aim of reducing the environmental pollution of this substance and its metabolites, gradually restoring groundwater quality.
Chinese patent CN110352974A discloses a post-seedling early-stage weeding active composition and herbicide, wherein the component A is quizalofop-p-ethyl or clethodim, the component B is clomazone, the component C is acetochlor or metolachlor, and the composition has the characteristics of high efficiency, safety, broad herbicide controlling spectrum, stable efficacy under low temperature and drought conditions and safety to main aftercrop crops, however, the quizalofop-p-ethyl can achieve better control effect only by increasing the dosage when the grass age is larger, the control effect is extremely poor when the grass age is overlarge or even the heading is started, and the control effect of applying the quizalofop-ethyl is poor when the soybean blooming period is used.
Aiming at the defects of the prior art, the invention provides the suspension emulsion special for weeding in the corn field, which can effectively remove weeds, has high safety, little influence on corn and wide application range.
Disclosure of Invention
The first aspect of the invention provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
2, 4-isooctyl-droplet;
terbuthylazine;
acetochlor;
a dispersing agent;
an emulsifying agent;
a stabilizer;
a dispersion medium;
other auxiliary agents;
water;
wherein the stabilizer comprises vitamin E polyethylene glycol succinate and modified silica.
As an embodiment of the present invention, the emulsifier comprises an amphoteric surfactant and a nonionic surfactant.
As an embodiment of the present invention, the amphoteric surfactant comprises an alkyl betaine or biuret.
As one embodiment of the present invention, the nonionic surfactant includes atlax 4913 and Termu1 1284.
As one embodiment of the present invention, the dispersant includes a polycarboxylate dispersant, a polycarboxylate dispersant.
As one embodiment of the invention, the polycarboxylate dispersant is Ackesu Agrlian-700, and the polycarboxylate dispersant is Metasersee-550S and DuramaxD-518.
As an embodiment of the present invention, the dispersion medium includes one or more of modified castor oil, methyl oleate, soybean oil.
As an embodiment of the present invention, other auxiliary agents include defoamers, antifreeze agents, preservatives, pH adjusters; wherein the defoaming agent is an organosilicon defoaming agent; the antifreezing agent is one or more selected from propylene glycol, ethylene glycol, polyethylene glycol 400 and glycerol;
the preservative is selected from one or more of potassium sorbate, sodium benzoate, isothiazolinone and benzisothiazolinone.
The second aspect of the invention provides an application of a ternary weeding suspension emulsion containing 2, 4-isooctyl, terbuthylazine and acetochlor in preventing and controlling annual weeds in spring corn fields.
The third aspect of the invention provides a method for preparing the ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following steps:
the terbuthylazine suspending agent, the 2, 4-isooctyl drop emulsifiable solution and the acetochlor emulsifiable solution are obtained through stirring, mixing, grinding and/or high-speed shearing; finally, adding the emulsifiable concentrate into a suspending agent, grinding and/or shearing at a high speed to obtain the suspoemulsion.
By adopting the technical scheme, the invention has the following beneficial effects:
1. according to the invention, 2, 4-isooctyl drop, terbuthylazine and acetochlor are compounded in a specific proportion, so that the weeding range is enlarged, the weeding effect is improved, and the weeding composition has the advantages of quick weeding, thorough weeding and low toxicity;
2. the particle size obtained in the grinding preparation process of the specific stabilizer is small, and the suspension rate is high;
3. according to the invention, the proper emulsifier is selected, and the characteristics of the raw materials are considered, so that the weeding performance of the product is excellent, and the growth and development of crops are not influenced.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The first aspect of the invention provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
2, 4-Diisooctyl ester
Terbuthylazine
Acetochlor
A dispersing agent;
an emulsifying agent;
a stabilizer;
a dispersion medium;
other auxiliary agents;
water;
wherein the stabilizer comprises vitamin E polyethylene glycol succinate and modified silica.
As a preferable mode of the invention, the ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor comprises the following preparation components:
dispersing agent: the method mainly wets the surface particles of the solid pesticide, is favorable for grinding the solid pesticide, ensures that the solid active ingredients of the pesticide are better dispersed in a continuous phase (water), and can improve the stability of the water phase and the oil phase in the whole system. In the present invention, the dispersant includes polycarboxylate dispersants and polycarboxylate dispersants; the polycarboxylate dispersant is Ackesu Agrlian-700, the polycarboxylate dispersant is Metasese-550S and Duramaxd-518, and the ratio of Metasese-550S and Duramaxd-518 is 8:1, a step of; and the mass ratio of the polycarboxylate dispersant to the polycarboxylate dispersant is 1:3.
emulsifying agent: the emulsifier can reduce the surface tension between oil and water, so that the emulsion phase can be better dispersed in water, the flocculation phenomenon of the system can be reduced, and the stability of the system can be improved. In the present invention, the emulsifier comprises an amphoteric surfactant and a nonionic surfactant.
In the invention, the amphoteric surfactant is alkyl betaine or biuret; specifically dodecyl betaine.
In the present invention, the nonionic surfactants are atlax 4913 and Termu1 1284.
Stabilizing agent: the stabilizer comprises vitamin E polyethylene glycol succinate and modified silicon dioxide.
The preparation method of the modified silicon dioxide comprises the following steps: mixing silicon dioxide, sodium metabisulfite, sodium acrylate and water according to proportion by ultrasonic, drying the mixture at constant temperature, and carrying out electron beam irradiation treatment on the dried product for 5-10min with energy of 5-10keV and dosage of 10-40 kGy.
Preferably, the weight ratio of the silicon dioxide to the sodium metabisulfite to the sodium acrylate to the water is 50: (1-3): (3-4): (100-300).
Preferably, the silica has a particle size of 0.1-0.15 μm and a specific surface area of 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
Dispersion medium: the dispersion medium comprises one or more of modified castor oil, methyl oleate and soybean oil.
Other auxiliaries: the other auxiliary agents in the invention comprise defoamer, antifreezing agent, preservative and pH value regulator; wherein the defoaming agent is an organic silicon defoaming agent, and specifically BYK-080 of Pick company. The antifreezing agent is one or more selected from propylene glycol, ethylene glycol, polyethylene glycol 400 and glycerol; in particular to ethylene glycol.
The preservative is selected from one or more of potassium sorbate, sodium benzoate, isothiazolinone and benzisothiazolinone; in particular to sodium benzoate.
The pH regulator is sodium hydroxide.
The second aspect of the invention provides an application of a ternary weeding suspension emulsion containing 2, 4-isooctyl, terbuthylazine and acetochlor in preventing and controlling annual weeds in spring corn fields.
The third aspect of the invention provides a method for preparing the ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following steps:
the terbuthylazine suspending agent, the 2, 4-isooctyl drop emulsifiable solution and the acetochlor emulsifiable solution are obtained through stirring, mixing, grinding and/or high-speed shearing; finally, adding the emulsifiable concentrate into a suspending agent, grinding and/or shearing at a high speed to obtain the suspoemulsion.
The invention is further illustrated with reference to specific embodiments.
Example 1
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer comprises the following components in percentage by mass: 1, vitamin E polyethylene glycol succinate and modified silica.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle size of the silicon dioxide is 0.1-0.15 mu m, and the specific surface area is 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
The dispersion medium is methyl oleate. The defoamer is BYK-080 of Pick company; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 2
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer is modified silicon dioxide.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle size of the silicon dioxide is 0.1-0.15 mu m, and the specific surface area is 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
The dispersion medium is methyl oleate. The defoamer is BYK-080 of Pick company; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 3
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer comprises vitamin E polyethylene glycol succinate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 4
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer comprises the following components in percentage by mass: 1, vitamin E polyethylene glycol succinate and modified silica.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle diameter of the silicon dioxide is 20 mu m, and the specific surface area is 4-5m 2 And/g, purchased from Ningbo gold nanotechnology Co., ltd., model number JL-SiO2-W20..
The dispersion medium is methyl oleate. The defoamer is BYK-080 of Pick company; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 5
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifying agent is Atlox4913 and Termu1 1284, and the mass ratio is 1:1.
the stabilizer comprises the following components in percentage by mass: 1, vitamin E polyethylene glycol succinate and modified silica.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle size of the silicon dioxide is 0.1-0.15 mu m, and the specific surface area is 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
The dispersion medium is methyl oleate. The defoamer is BYK-080 of Pick company; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 6
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer comprises the following components in percentage by mass: 1, vitamin E polyethylene glycol succinate and modified silica.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle size of the silicon dioxide is 0.1-0.15 mu m, and the specific surface area is 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
The dispersion medium is methyl oleate. The defoamer is BYK-080 of Pick company; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Example 7
The embodiment provides a ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, which comprises the following preparation components:
the dispersing agent is Metaserse-550S, duramaxd-518 and Ackesu Agrlian-700 with the mass ratio of 8:1:3.
the emulsifier is dodecyl betaine, atlax 4913 and Termu1 1284, and the mass ratio is 2:1:1.
the stabilizer comprises the following components in percentage by mass: 1, vitamin E polyethylene glycol succinate and modified silica.
The preparation method of the modified silicon dioxide comprises the following steps: according to the weight portions, 50 portions of silicon dioxide, 2 portions of sodium metabisulfite, 3 portions of sodium acrylate and 200 portions of water are mixed in proportion by ultrasonic, the mixture is dried at constant temperature, and the dried product is irradiated by an electron beam with energy of 8keV and dosage of 30kGy for 10min.
The particle size of the silicon dioxide is 0.1-0.15 mu m, and the specific surface area is 15-27m 2 /g, model number BK94, purchased from Shandong Boken silicon materials Co.
The dispersion medium is methyl oleate. The defoaming agent is a polyether defoaming agent, and is specifically a GPE type polyether defoaming agent; the antifreezing agent is glycol; the preservative is sodium benzoate.
The second aspect of the invention provides a preparation method of the suspoemulsion, which comprises the following steps:
s01, mixing terbuthylazine, a stabilizer, a nonionic surfactant, metasese-550S, duramaxd-518 of Dow and water by grinding to obtain a terbuthylazine suspension;
wherein the zirconium beads are sand milling media, the sand milling time is 2h, and the rotating speed is 1300rpm;
s02, uniformly stirring 2, 4-isooctyl drop, acetochlor, a dispersing medium and the rest emulsifying agent by grinding to obtain emulsifiable concentrate;
s03, mixing the emulsifiable concentrate and the suspending agent under high shear, then adding the rest preparation raw materials, and finally preparing the suspension emulsion through modulation and mixing;
wherein the shear emulsification time was 30min and the rotational speed was 2500rpm.
Performance testing
1. Suspension ratio: the measurement is carried out by referring to GB/T14825-2006 pesticide suspension rate measurement method; wherein, the lowest suspension rate of the three raw materials is the suspension rate value of the whole system.
2. The measurement of the heat storage stability is carried out by referring to a GB/T19136-2003 pesticide heat storage stability measurement method; the low temperature stability measurement is performed by referring to the GB/T19137-2003 pesticide low temperature stability measurement method.
3. Dispersion stability test: 0.5mL of the suspoemulsion was added dropwise to hard water, and the dispersion of the suspoemulsion in water was observed.
Priority level: automatically dispersing, and no visible particles/oily matters are separated out;
grade (C): can be automatically dispersed, and a small amount of particles/oily matters are separated out;
inferior grade: cannot be automatically dispersed, and obvious particles/oily matters are separated out.
TABLE 1 Performance test results
"-" indicates that the suspension rate does not meet the standard, and the suspension rate is lower.
In the invention, the suspoemulsion is subjected to grinding and modulation processes of a grinder in the preparation process, and meanwhile, due to multiple phases in the system, for example, interphase transfer between an emulsifying agent and a dispersing agent can occur, so that the dosage of the emulsifying agent or the dispersing agent of the other phase is insufficient. According to the invention, vitamin E polyethylene glycol succinate is selected as the stabilizer, so that a finer particle size can be obtained in the grinding process, and the suspension rate of the whole system is higher. However, the particle size is smaller, so that agglomeration is easy to occur, and the suspension rate is reduced; meanwhile, the 2,4-D isooctyl ester in the system has better drug effect under the acidic condition, and terbuthylazine is more stable in neutral, weak acidic and weak alkaline mediums and is easy to hydrolyze in acidic or alkaline mediums; to improve this, the present inventors found that the use of an amphoteric emulsifier can improve the above-mentioned conditions, while the addition of modified silica can improve both the above-mentioned problems. The results show that the vitamin E polyethylene glycol succinate is selected as the stabilizer, the modified silicon dioxide is compounded, the overall stability of the system is high, and the suspension rate is high.
And (3) field test:
efficacy test of 83%2, 4-D-i Xin Zhi T Ding Jin acetochlor suspension emulsion for preventing and killing annual weeds in spring corn field
Test crop: spring corn
Control object: annual weeds
Test time: (2022.05.26-2022.10.10)
Table 2 test agents:
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the application method and the water consumption are as follows: the test agent is sprayed on the soil which is clear and has wind power less than 3 grades after spring corn is sowed and before the seedling emergence, weeds are germinated and do not come out of soil, and 750L of soil is sprayed per hectare.
Test target conditions
Barnyard grass Echinochloria crus-galli (L) Beauv, wild millet Eriochloa villosa (thunder.) Kunth, quinoa (Chenopodium album L), amaranthus retroflexus (Amaranthus retroflexus L), polygonum (Polygonum bungeanum Turcz.), acalypha australis (Acalypha australis L.), commelina communis (Commelina communis L.), saussurea [ Rorippa globosa (Leys) Bess ], humulus scandens (Lour) Merr ], field thistle (Cirsium arvense var. Integrifolium), kochia scoparia (L.) schrad ], ragweed (Ambrosia tricida L.), xanthan (Xanthium sibiricum Patrin), abutilum (Abutilon theophrasti Medi), solanum nigrum L.), herba Pogostemonis (Amethystea caerulea L.) and the like.
Crop: spring corn; variety: gemini 63, 3 days after corn sowing when applied.
Black loam, organic matter content 2.3%, and neutral pH value.
Day of application climate: the medicine is applied in the case of 5.26 a.m. 5-11 a.m. in 2022, in the case of light rain, in the case of application, in the case of 2 North America, in the shade, at 11-14 ℃ and in the weather condition, the medicine effect is exerted.
Table 3 test results:
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conclusion: 83%2, 4-D-i Xin Zhi T Ding Jin acetochlor suspension emulsion is sprayed by adding water and soil after spring corn is sown to the time before emergence, and the proper dosage is as follows: the field with low weed base number in the last year is 1120.5g/hm 2 (amount of active ingredient) field with large weed base can be properly increased to 1369.5g/hm 2 The water-mixed 750L soil spray treatment can effectively prevent and remove weeds such as barnyard grass, crab grass, abutilon, quinoa, black nightshade and the like, has better control effect on other broadleaf weeds (scandent hop, herba Cephalanoploris, polygonum and the like), and is safe to corn.
Investigation method
Artificially prepared 0.25m by absolute value investigation 2 Iron frames were examined at 3 points per cell, at random, and the type and number of weeds in which heart leaves did not die were examined and recorded.
Drug effect calculation method
The plant number or fresh weight control effect of each treatment is calculated according to the formula (1):
wherein:
e-control effect in percentage (%)
PT-the number of residual weed plants or fresh weight in plants or gram (g);
CK-control weed plants or fresh weight in plants or grams (g).
Results were analyzed using biological statistical methods (DMRT method)
Direct impact on crops
Visual inspection of corn leaf color, growth, emasculation, plant height and other biological characters is carried out 1, 5, 10, 20, 30 and 40 days after the medicine, and if the medicine injury is found, the medicine injury character is recorded.
The grading method of the phytotoxicity is specifically as follows:
stage 1: the crops grow normally without any victim symptoms;
2 stages: the crop is slightly phytosanitary, and the phytosanitary is less than 10%;
3 stages: the crop and other phytotoxicity can be recovered later, and the yield is not affected;
4 stages: the crop injury is heavy, and is difficult to recover, so that the yield is reduced.
5 stages: the crop injury is serious, and the crop cannot be recovered, so that the yield is obviously reduced or absolute.
Effect on crop growth
After the application, the influence of each treatment on the indexes such as corn seedling emergence, leaf color, growth, jointing, emasculation, yield and the like is observed and tested.
And taking 1 ridge in the middle of each district after autumn to measure the fresh weight of the seeds, converting the fresh weight into hectare yield, and calculating the yield increase.
The corn yield increase is calculated according to the formula (2):
wherein:
Y-increase in yield in percent (%);
y-target herbicide treatment zone yield in kilograms (kg);
y0-control yield in kilograms (kg).
Results were analyzed using biological statistical methods (DMRT method)
Table 4 investigation of the effect of 83%2, 4-d i Xin Zhi t Ding Jin acetochlor suspoemulsion on crop yield
Preventing and killing effect: statistical analysis of the investigation data was performed using DPS data processing system software, and specific results are shown in tables 5 and 6.
Table 5 effects (%) of 83%2, 4-Di-i Xin Zhi T Ding Jin acetochlor suspoemulsion on weed control in spring corn fields-20. 20 d after application
Note that: 1. other broadleaf weeds including scandent hop, herba Cephalanoploris, polygonum tinctorium, etc.; 2. the difference in the table is 5% of the difference in the statistics of weed plants, as follows.
Table 6 effect (%) of 83%2, 4-Di-i Xin Zhi T Ding Jin acetochlor suspension emulsion on control of annual weeds in spring corn fields-40 d after application
At the same time, other crops were found to be less effective than corn.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (10)

1. A ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor is characterized by comprising the following preparation components:
2, 4-isooctyl-droplet;
terbuthylazine;
acetochlor;
a dispersing agent;
an emulsifying agent;
a stabilizer;
a dispersion medium;
other auxiliary agents;
water;
wherein the stabilizer comprises vitamin E polyethylene glycol succinate and modified silica.
2. A ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor as claimed in claim 1, wherein the emulsifier comprises an amphoteric surfactant and a nonionic surfactant.
3. A ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor as claimed in claim 2, wherein the amphoteric surfactant is an alkyl betaine or biuret.
4. A ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor as claimed in claim 2, wherein the non-ionic surfactant comprises atlax 4913 and Termu1 1284.
5. The ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor according to claim 1, wherein the dispersing agent comprises a polycarboxylate dispersing agent and a polycarboxylate dispersing agent.
6. The ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor according to claim 4, wherein the polycarboxylate dispersant is aclavak Agrlian-700, and the polycarboxylate dispersant is Metasese-550S and Duramaxd-518.
7. A ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor as claimed in claim 1, wherein the dispersion medium comprises one or more of modified castor oil, methyl oleate, soybean oil.
8. The ternary herbicidal suspoemulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor according to claim 1, wherein the other auxiliary agents comprise defoamer, antifreezing agent, preservative and pH regulator; wherein the defoaming agent is an organosilicon defoaming agent; the antifreezing agent is one or more selected from propylene glycol, ethylene glycol, polyethylene glycol 400 and glycerol;
the preservative is selected from one or more of potassium sorbate, sodium benzoate, isothiazolinone and benzisothiazolinone.
9. Use of a ternary herbicidal suspoemulsion comprising 2, 4-isooctyl, terbuthylazine and acetochlor according to any one of claims 1-8 for controlling annual weeds in spring corn fields.
10. A process for preparing a ternary herbicidal suspoemulsion comprising 2, 4-isooctyl drop, terbuthylazine and acetochlor according to any one of claims 1 to 8, characterized in that it comprises:
the terbuthylazine suspending agent, the 2, 4-isooctyl drop emulsifiable solution and the acetochlor emulsifiable solution are obtained through stirring, mixing, grinding and/or high-speed shearing; finally, adding the emulsifiable concentrate into a suspending agent, grinding and/or shearing at a high speed to obtain the suspoemulsion.
CN202310740379.9A 2023-06-21 2023-06-21 Ternary weeding suspension emulsion containing 2, 4-isooctyl drop, terbuthylazine and acetochlor, preparation method and application thereof Pending CN116746580A (en)

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