CN116035017A - Prochloraz-flumioxazin microcapsule suspending agent and preparation method thereof - Google Patents

Prochloraz-flumioxazin microcapsule suspending agent and preparation method thereof Download PDF

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Publication number
CN116035017A
CN116035017A CN202211223112.4A CN202211223112A CN116035017A CN 116035017 A CN116035017 A CN 116035017A CN 202211223112 A CN202211223112 A CN 202211223112A CN 116035017 A CN116035017 A CN 116035017A
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flumioxazin
metolachlor
soluble capsule
polyoxyethylene ether
oil
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王利
许映蓉
任新峰
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Nantong Jiangshan Agrochemical & Chemicals Co ltd
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Nantong Jiangshan Agrochemical & Chemicals 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/84Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms six-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,4
    • 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
    • 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
    • A01N25/26Biocides, 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 in coated particulate form
    • A01N25/28Microcapsules or nanocapsules
    • 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
    • A01N37/00Biocides, 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
    • A01N37/18Biocides, 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
    • A01N37/22Biocides, 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 the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P13/00Herbicides; Algicides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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

Abstract

The invention relates to the field of A01N43, in particular to a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, wherein the preparation raw materials at least comprise the following components in percentage by mass: 1-45% of metolachlor, 1-5% of flumioxazin, 1-5% of solvent, 1-20% of oily dispersion medium, 1-5% of oil-soluble capsule material A, 0.01-5% of water-soluble capsule material A, 1-5% of oil-soluble capsule material B, 0.01-5% of water-soluble capsule material B, 1-5% of emulsifying dispersant, 1-10% of dispersant, 0.05-3% of thickener, 1-5% of antifreezing agent, 0.1-0.5% of preservative, 0.1-0.5% of defoaming agent, and water to 100% of complement, and has high system stability and good efficacy, and is effectively applied to prevention and treatment of annual gramineous weeds and partial broadleaf weeds in soybean fields, peanut fields and sugarcane fields.

Description

Prochloraz-flumioxazin microcapsule suspending agent and preparation method thereof
Technical Field
The invention relates to the field of A01N43, in particular to a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof.
Background
The chemical name of the metolachlor is (S) -2-chloro-6-ethyl-N- (2-methoxy-1-methylethyl) acetyl o-toluidine, and the metolachlor mainly plays a role in killing weeds through bud sheath and bud absorption of sprouted weeds. Is suitable for soil treatment after sowing and before seedling or transplanting of dry land crops, and can prevent and remove annual gramineous weeds, partial dicotyledonous weeds, annual sedge weeds and the like. The metolachlor is suitable for wide crop spectrum and is the main herbicide for corn and sorghum as important crop in the world. The flumioxazin is an N-phenyl peptide imide selective contact herbicide and is also an important product in other PPO inhibitor herbicides. Can be used for preventing and killing broadleaf weeds in various crops in dry farmland. The water-soluble and quick degradable water-soluble paint has low application amount, ensures the safety to the environment and has no pollution to the underground water.
The single use of the metolachlor has certain limitation, for example, chinese patent application (publication No. CN 104222074A) discloses a metolachlor water emulsion and a preparation method thereof, and particularly the metolachlor is taken as an effective active ingredient, and the water emulsion prepared by the method is practically applied, and has certain prevention effect on annual gramineous weeds and certain broadleaf weeds, but has insufficient weed killing effectiveness and universality, and limits the application range. Chinese patent application (publication No. CN 107593725A) discloses a pesticide composition containing metolachlor and flumioxazin as active ingredients, and the herbicide spectrum is expanded to a certain extent, but the system stability of the prepared composition with different dosage forms affects the exertion of the pesticide effect and the dosage of the pesticide, and the environmental and economic effects are certain.
Disclosure of Invention
In order to solve the problems, the invention provides the fine metolachlor-flumioxazin microcapsule suspending agent and the preparation method thereof, wherein the fine metolachlor and flumioxazin are separately encapsulated and then are compounded to obtain the microcapsule suspending agent with good suspension effect, so that the herbicide controlling spectrum can be expanded by combining different action mechanisms of the fine metolachlor and the flumioxazin microcapsule suspending agent, and meanwhile, the grass controlling period is prolonged, the application times and the application dosage are reduced, and the environmental pollution and the resource waste are reduced through the special slow-release and controlled-release functions of the microcapsule suspending agent.
The invention provides a metolachlor-flumioxazin microcapsule suspending agent, which is prepared from the following raw materials in percentage by mass: 1-45% of metolachlor, 1-5% of flumioxazin, 1-5% of solvent, 1-20% of oily dispersion medium, 1-5% of oil-soluble capsule wall material A, 0.01-5% of water-soluble capsule wall material A, 1-5% of oil-soluble capsule wall material B, 0.01-5% of water-soluble capsule wall material B, 1-5% of emulsifying dispersant, 1-10% of dispersant, 0.05-3% of thickener, 1-5% of antifreezing agent, 0.1-0.5% of preservative, 0.1-0.5% of defoaming agent and the balance of water to 100%.
As a preferable technical scheme, the mass ratio of the metolachlor to the flumioxazin is (3-40): 1, a step of; preferably, the mass ratio of the metolachlor to the flumioxazin is (28-40): 1.
based on the system of the invention, by adopting the metolachlor and the flumioxazin as effective active ingredients, the weeding effect of the mixed combination of the metolachlor and the flumioxazin with different proportions is found, especially when the mass ratio of the metolachlor to the flumioxazin is (28-40): 1, the weeding effect of barnyard grass, nutgrass and glossoside is synergistic, the two medicaments produce synergistic effect through different weeding mechanisms, and the dosage is reduced.
As a preferable technical scheme, the oily dispersion medium is at least one of dimethylbenzene, cyclohexanone, solvent oil and methyl oleate; preferably, the oily dispersion medium is methyl oleate.
As a preferable technical scheme, the solvent is at least one of solvent oil 150#, solvent oil 200#, xylene, toluene, soybean oil, corn oil, rapeseed oil, cottonseed oil and turpentine; preferably, the solvent is solvent oil 150#.
As a preferable technical scheme, the oil-soluble capsule wall material a and the oil-soluble capsule wall material B are respectively selected from at least one of toluene diisocyanate, 4-diphenylmethane diisocyanate, hexamethylene-1, 6-diisocyanate, isophorone diisocyanate trimer and polymethylene polyphenyl polyisocyanate; preferably, the oil-soluble capsule wall material A is hexamethylene-1, 6-diisocyanate; the oil-soluble capsule wall material B is isophorone diisocyanate trimer. The brand of isophorone diisocyanate trimer is Bayer, and is derived from Xuzhou bright Huiyang New materials Co.
As a preferable technical scheme, the water-soluble capsule material A and the water-soluble capsule material B are respectively selected from at least one of triethanolamine, urea resin prepolymer and melamine resin prepolymer; preferably, the water-soluble capsule material A is triethanolamine, and the water-soluble capsule material B is melamine resin prepolymer. The melamine resin prepolymer is of the type Plastopal BTW and is derived from Basoff.
Based on the system, the metolachlor and the flumioxazin are taken as active ingredients, and the metolachlor and the flumioxazin are independently encapsulated and then compounded, so that the controlled release and the sustained release functions of the active ingredients are effectively ensured. The inventor finds that, in the research process, a specific oil-soluble capsule material B is isophorone diisocyanate trimer and a water-soluble capsule material B is melamine resin prepolymer, and the active ingredient flumioxazin is wrapped by an interfacial polymerization method, so that the provided microcapsule suspending agent has high encapsulation efficiency, excellent wall material crosslinking degree and porosity, uniform particle size distribution and stable storage, and simultaneously the action time of the active ingredient is prolonged, so that the provided product is effectively applied to the prevention and treatment of annual gramineous weeds and part of broadleaf weeds in soybean fields, peanut fields and sugarcane fields.
As a preferable technical scheme, the emulsifying dispersant is one or more of benzyl phenol polyoxyethylene ether phosphate, castor oil polyoxyethylene ether, phenethyl phenol polyoxyethylene ether and nonylphenol polyoxyethylene ether. Preferably, the emulsifying dispersant is a combination of castor oil polyoxyethylene ether and phenethyl phenol polyoxyethylene ether; the mass ratio of the castor oil polyoxyethylene ether to the phenethyl phenol polyoxyethylene ether is 1: (0.2-1); the model of the castor oil polyoxyethylene ether is CL-40, and is derived from Nantong Tay chemical industry Co. The model of the phenethyl phenol polyoxyethylene ether is 603# and is from Nantong Tay chemical industry Co.
As a preferable technical scheme, the dispersing agent is at least one of sodium lignin sulfonate, calcium lignin sulfonate and calcium dodecyl benzene sulfonate; preferably, the dispersing agent is a combination of calcium lignosulfonate and calcium dodecylbenzene sulfonate; the mass ratio of the calcium lignin sulfonate to the calcium dodecyl benzene sulfonate is 1: (0.5-2).
Based on the system of the invention, the provided microcapsule suspending agent has long-term stable performance by adopting specific emulsifying dispersant and dispersing agent, is convenient for dispensing, has good in water diffusivity, has good drug effect maintenance under the condition of higher or lower temperature, reduces the application times and dosage, and reduces environmental pollution and resource waste.
As a preferable technical scheme, the thickener is one or more of organic bentonite, magnesium aluminum silicate, xanthan gum, polyvinyl alcohol and sodium alginate; preferably, the thickener is an organobentonite, which is available from Zhejiang Feng Hong New Material Co., ltd. Based on the system, the organic bentonite is introduced as a thickening agent, so that the organic bentonite can be dispersed into a net structure in methyl oleate, the sinking of active ingredients is effectively prevented, and the suspension effect of the microcapsule suspending agent is ensured.
As a preferable technical scheme, the antifreezing agent is at least one of ethylene glycol, 1, 2-propylene glycol and glycerol; preferably, the antifreezing agent is glycerol.
As a preferable technical scheme, the preservative is potassium sorbate.
As a preferable technical scheme, the defoaming agent is an organosilicon defoaming agent, and the organosilicon defoaming agent is derived from a medium-federal defoaming agent factory.
The invention also provides a preparation method of the metolachlor-flumioxazin microcapsule suspending agent, which at least comprises the following preparation steps:
(1) Preparing a metolachlor microcapsule suspending agent;
(2) Preparing flumioxazin microcapsule suspending agent;
(3) And mixing the metolachlor microcapsule suspending agent with the flumioxazin microcapsule suspending agent.
The beneficial effects are that:
1. the invention provides a fine metolachlor and flumioxazin microcapsule suspending agent and a preparation method thereof, wherein the fine metolachlor and flumioxazin are separately encapsulated and then compounded to obtain the microcapsule suspending agent with good suspension effect, so that the weed control spectrum can be expanded by combining different action mechanisms of the fine metolachlor and flumioxazin microcapsule suspending agent, and meanwhile, the grass control period is prolonged, the application times and the application dosage are reduced, and the environmental pollution and the resource waste are reduced by the special slow release and controlled release functions of the microcapsule suspending agent.
2. Based on the system of the invention, by adopting the metolachlor and the flumioxazin as effective active ingredients, the weeding effect of the mixed combination of the metolachlor and the flumioxazin with different proportions is found, especially when the mass ratio of the metolachlor to the flumioxazin is (28-40): 1, the weeding effect of barnyard grass, nutgrass and glossoside is synergistic, the two medicaments produce synergistic effect through different weeding mechanisms, and the dosage is reduced.
3. Based on the system of the invention, the specific oil-soluble capsule material B is isophorone diisocyanate trimer and the water-soluble capsule material B is melamine resin prepolymer, and the active ingredient flumioxazin is wrapped by an interfacial polymerization method, so that the provided microcapsule suspending agent has high encapsulation rate, excellent wall material crosslinking degree and porosity, uniform particle size distribution and stable storage, and simultaneously the action time of the active ingredient is prolonged, and the provided product is effectively applied to the prevention and treatment of annual gramineous weeds and part of broadleaf weeds in soybean fields, peanut fields and sugarcane fields.
4. Based on the system, the metolachlor and the flumioxazin are taken as active ingredients, and the metolachlor and the flumioxazin are independently encapsulated and then compounded, so that the controlled release and the sustained release functions of the active ingredients are effectively ensured.
Detailed Description
Example 1
In one aspect, the embodiment 1 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent, which is prepared from the following raw materials in percentage by mass: 40% of metolachlor, 1% of flumioxazin, 3% of solvent, 10% of oily dispersion medium, 3% of oil-soluble capsule material A, 2% of water-soluble capsule material A, 2% of oil-soluble capsule material B, 1% of water-soluble capsule material B, 3% of emulsifying dispersant, 5% of dispersant, 1% of thickener, 2% of antifreezing agent, 0.2% of preservative, 0.3% of defoaming agent and 100% of water.
The oily dispersion medium is methyl oleate.
The solvent is solvent oil 150#.
The oil-soluble capsule wall material A is hexamethylene-1, 6-diisocyanate; the oil-soluble capsule wall material B is isophorone diisocyanate trimer. The brand of isophorone diisocyanate trimer is Bayer, and is derived from Xuzhou bright Huiyang New materials Co.
The water-soluble capsule material A is triethanolamine, and the water-soluble capsule material B is melamine resin prepolymer. The melamine resin prepolymer is of the type Plastopal BTW and is derived from Basoff.
The emulsifying dispersant is a combination of castor oil polyoxyethylene ether and phenethyl phenol polyoxyethylene ether; the mass ratio of the castor oil polyoxyethylene ether to the phenethyl phenol polyoxyethylene ether is 1:0.5.
the dispersing agent is a combination of calcium lignosulfonate and calcium dodecyl benzene sulfonate; the mass ratio of the calcium lignin sulfonate to the calcium dodecyl benzene sulfonate is 1:1.
the thickener is organic bentonite and is sourced from Zhejiang Feng Hong New Material Co.Ltd.
The antifreezing agent is glycerol.
The preservative is potassium sorbate.
The defoaming agent is an organosilicon defoaming agent, and the organosilicon defoaming agent is derived from a medium federal defoaming agent factory.
The embodiment 1 of the invention provides a preparation method of a fine metolachlor-flumioxazin microcapsule suspending agent, which comprises the following preparation steps:
(1) Preparing a metolachlor microcapsule suspending agent;
(2) Preparing flumioxazin microcapsule suspending agent;
(3) And mixing the metolachlor microcapsule suspending agent with the flumioxazin microcapsule suspending agent.
The preparation method of the metolachlor microcapsule suspending agent specifically comprises the following steps: mixing the metolachlor, the oil-soluble capsule wall material A and a solvent to form a homogeneous phase A; mixing one half of the weight of defoamer and emulsifying dispersant and one third of the weight of water into a homogeneous phase B; mixing the water-soluble capsule wall material A with the other third of water by weight to form a homogeneous phase C; mixing one half of the dispersant, the thickener, the antifreezing agent and the preservative into a homogeneous phase D; and shearing the homogeneous phase B under a high-speed shearing machine, adding the homogeneous phase A into the homogeneous phase B, stirring and mixing, adding the homogeneous phase C, adding the homogeneous phase D after the dripping of the homogeneous phase C is finished, and stirring and mixing to obtain the metolachlor microcapsule suspending agent.
The preparation method of the flumioxazin microcapsule suspending agent specifically comprises the following steps: grinding flumioxazin, the balance of the emulsifying dispersant, the balance of the dispersant and the oily dispersion medium into a homogeneous phase E; mixing the homogeneous phase E with the oil-soluble capsule wall material B to obtain a homogeneous phase F; mixing the water-soluble capsule material B with the balance of water to form a homogeneous phase G; mixing the rest of dispersing agent, thickening agent, antifreezing agent and preservative into homogeneous phase H; and adding the homogeneous phase G into the homogeneous phase F, stirring and mixing, adding the homogeneous phase H after the dropwise addition of the homogeneous phase G is finished, and stirring and mixing to obtain the flumioxazin microcapsule suspending agent.
Example 2
The embodiment 2 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode of the suspending agent is the same as the embodiment 1, wherein the suspending agent comprises the following preparation raw materials in percentage by mass: 28.6% of metolachlor, 1% of flumioxazin, 3% of solvent, 10% of oily dispersion medium, 3% of oil-soluble capsule wall material A, 2% of water-soluble capsule wall material A, 2% of oil-soluble capsule wall material B, 1% of water-soluble capsule wall material B, 3% of emulsifying dispersant, 5% of dispersant, 1% of thickener, 2% of antifreezing agent, 0.2% of preservative, 0.3% of defoaming agent and the balance of water to 100%.
Example 3
The embodiment 3 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode of the suspending agent is the same as the embodiment 1, wherein the suspending agent comprises the following preparation raw materials in percentage by mass: 20% of metolachlor, 1% of flumioxazin, 3% of solvent, 10% of oily dispersion medium, 3% of oil-soluble capsule material A, 2% of water-soluble capsule material A, 2% of oil-soluble capsule material B, 1% of water-soluble capsule material B, 3% of emulsifying dispersant, 5% of dispersant, 1% of thickener, 2% of antifreezing agent, 0.2% of preservative, 0.3% of defoaming agent and 100% of water.
Example 4
The embodiment 4 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode of the suspending agent is the same as the embodiment 1, wherein the suspending agent comprises the following preparation raw materials in percentage by mass: 20% of metolachlor, 3% of flumioxazin, 3% of solvent, 10% of oily dispersion medium, 3% of oil-soluble capsule wall material A, 2% of water-soluble capsule wall material A, 2% of oil-soluble capsule wall material B, 1% of water-soluble capsule wall material B, 3% of emulsifying dispersant, 5% of dispersant, 1% of thickener, 2% of antifreezing agent, 0.2% of preservative, 0.3% of defoaming agent and 100% of water.
Example 5
The embodiment 5 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode of the suspending agent is the same as the embodiment 1, wherein the suspending agent comprises the following preparation raw materials in percentage by mass: 20% of metolachlor, 6% of flumioxazin, 3% of solvent, 10% of oily dispersion medium, 3% of oil-soluble capsule wall material A, 2% of water-soluble capsule wall material A, 2% of oil-soluble capsule wall material B, 1% of water-soluble capsule wall material B, 3% of emulsifying dispersant, 5% of dispersant, 1% of thickener, 2% of antifreezing agent, 0.2% of preservative, 0.3% of defoaming agent and 100% of water.
Comparative example 1
The comparative example 1 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode is the same as the example 1, wherein the oil-soluble capsule wall material A and the oil-soluble capsule wall material B are toluene diisocyanate; the water-soluble capsule material A and the water-soluble capsule material B are ethylenediamine.
Comparative example 2
The comparative example 2 of the invention provides a fine metolachlor-flumioxazin microcapsule suspending agent and a preparation method thereof, and the specific implementation mode is the same as the example 1, wherein the emulsifying dispersant is phenethyl phenol polyoxyethylene ether; the dispersing agent is calcium dodecyl benzene sulfonate.
Performance test method
1. Thermal storage stability: the fine metolachlor-flumioxazin microcapsule suspension prepared in the examples and the comparative examples is placed in a 50mL glass bottle to be sealed, stored in an incubator at 54+/-2 ℃ for 14 days, taken out, observed and recorded for the appearance of the product, and the results are shown in Table 1.
TABLE 1,
Figure BDA0003878730010000071
Figure BDA0003878730010000081
2. And (5) measuring the weeding effects of the metolachlor and the flumioxazin with different proportions.
The specific test method comprises the following steps:
potting soil spraying (NY/T1155.3-2006) was used: the method comprises the steps of filling quantitative soil in a porcelain pot with the height of 6cm and the diameter of 9cm, sowing 15-20 seeds of weeds to be tested in the porcelain pot, covering fine soil with the thickness of 0.5-1 cm, watering, placing in a greenhouse for cultivation for standby, carrying out soil spraying treatment after 24 hours, spraying 1mL of liquid medicine into each pot, repeating the treatment for 4 times, and setting the treatment without the medicament as a control. Culturing the treated test material in a greenhouse, periodically observing the growth condition of target weeds, visually observing the damage symptoms and growth inhibition condition of the target after 21d, weighing the fresh weight or the fresh weight of the overground part, and evaluating the virulence effect of the agent on the target weeds according to the target growth inhibition rate or the fresh weight inhibition rate.
Investigation method
After 21d of test treatment, the target victim symptom and the growth inhibition condition were visually examined, and the fresh weight of the aerial part was weighed, and the fresh weight inhibition rate (%) was calculated.
Figure BDA0003878730010000082
Combined action evaluation method
The mode of action of the herbicide combination was evaluated according to the Gowing method (NY/T1155.7-2006) and the formula is as follows:
E 0 =X+Y-XY/100
wherein X is the fresh weight inhibition rate of flumioxazin to target weeds when a certain dosage is used singly;
y is the fresh weight inhibition rate of the metolachlor on target weeds when a certain dosage is used singly;
e is an actual measurement value of the fresh weight inhibition rate of the target weeds when the flumioxazin and the metolachlor are mixed;
E 0 is a theoretical value of the fresh weight inhibition rate of the two medicaments of flumioxazin and metolachlor on target weeds when the two medicaments are mixed.
Evaluation criteria: the synergy is shown when E0-E is more than or equal to 10%, the summation is shown when E0-E is less than 10% and the antagonism is shown when E0-E is less than or equal to 10%.
Table 2 herbicidal effects of flumioxazin, metolachlor and their blends.
Figure BDA0003878730010000083
Figure BDA0003878730010000091
Test results show that in the mixed combination of the flumioxazin and the metolachlor, the proportion is (A: B=40:1 and A: B=28.6:1) that the flumioxazin and the metolachlor have synergistic effects on weeding effects of barnyard grass, nutgrass flatsedge and glossoma anatipestifer, and the proportion is (A: B=20:1, A: B=20:3 and A: B=20:6) that the fluminella, the sedge and the glossoma anatipestifer have additive effects on weeding effects of barnyard grass, glossoma anatipestifer.

Claims (10)

1. The metolachlor-flumioxazin microcapsule suspending agent is characterized by comprising the following preparation raw materials in percentage by mass: 1-45% of metolachlor, 1-5% of flumioxazin, 1-5% of solvent, 1-20% of oily dispersion medium, 1-5% of oil-soluble capsule wall material A, 0.01-5% of water-soluble capsule wall material A, 1-5% of oil-soluble capsule wall material B, 0.01-5% of water-soluble capsule wall material B, 1-5% of emulsifying dispersant and 1-10% of dispersant, and the balance of water to 100%.
2. The metolachlor-flumioxazin microcapsule suspension agent according to claim 1, which is characterized by further comprising the following preparation raw materials in percentage by mass: 0.05-3% of thickening agent, 1-5% of antifreezing agent, 0.1-0.5% of preservative and 0.1-0.5% of defoaming agent.
3. The fine metolachlor-flumioxazin microcapsule suspension according to claim 1 or 2, wherein the oil-soluble capsule wall material A and the oil-soluble capsule wall material B are respectively selected from at least one of toluene diisocyanate, 4-diphenylmethane diisocyanate, 1, 6-hexamethylene diisocyanate, isophorone diisocyanate trimer and polymethylene polyphenyl polyisocyanate.
4. The fine metolachlor-flumioxazin microcapsule suspension according to claim 3, wherein the emulsifier is one or more of castor oil polyoxyethylene ether, phenethyl phenol polyoxyethylene ether, calcium dodecyl benzene sulfonate, polysorbate, sorbitan fatty acid ester, phenethyl phenol polyoxypropylene ether, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene ether carboxylate, polyoxyethylene ether vinyl ether, alkylphenol polyoxyethylene ether sulfosuccinate and castor oil ethylene oxide adduct.
5. The fine metolachlor-flumioxazin microcapsule suspension agent according to claim 4, wherein the water-soluble capsule material A and the water-soluble capsule material B are respectively selected from at least one of triethanolamine, urea resin prepolymer and melamine resin prepolymer.
6. The fine metolachlor-flumioxazin microcapsule suspension agent according to claim 5, wherein the emulsifying dispersant is one or more of benzyl phenol polyoxyethylene ether phosphate, castor oil polyoxyethylene ether, phenethyl phenol polyoxyethylene ether and nonylphenol polyoxyethylene ether.
7. The fine metolachlor-flumioxazin microcapsule suspension agent according to claim 6, wherein the dispersing agent is at least one of sodium lignin sulfonate, calcium lignin sulfonate and calcium dodecyl benzene sulfonate.
8. The metolachlor-flumioxazin microcapsule suspension agent according to claim 7, wherein the thickener is one or more of organic bentonite, magnesium aluminum silicate, xanthan gum, polyvinyl alcohol and sodium alginate.
9. The metolachlor-flumioxazin microcapsule suspension agent according to claim 8, wherein the solvent is at least one of xylene, cyclohexanone, solvent oil and methyl oleate.
10. A process for the preparation of a fine metolachlor-flumioxazin microcapsule suspension according to any one of claims 1-9, characterized in that it comprises at least the following preparation steps:
(1) Preparing a metolachlor microcapsule suspending agent;
(2) Preparing flumioxazin microcapsule suspending agent;
(3) And mixing the metolachlor microcapsule suspending agent with the flumioxazin microcapsule suspending agent.
CN202211223112.4A 2022-10-08 2022-10-08 Prochloraz-flumioxazin microcapsule suspending agent and preparation method thereof Pending CN116035017A (en)

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CN103651550A (en) * 2012-09-19 2014-03-26 青岛星牌作物科学有限公司 Microcapsule suspending agent prepared from carbosulfan, chlorpyrifos and abamectin by compounding
CN106900723A (en) * 2017-03-03 2017-06-30 江苏莱科化学有限公司 A kind of soybean Herbicidal combinations
CN107535505A (en) * 2016-06-28 2018-01-05 佛山市盈辉作物科学有限公司 Herbicidal combinations containing S-metolachlor and flumioxazin
CN107593725A (en) * 2017-08-30 2018-01-19 北京明德立达农业科技有限公司 A kind of composition pesticide and its application
CN108432751A (en) * 2018-03-27 2018-08-24 江苏邦盛生物科技有限责任公司 A kind of pesticide microcapsule suspending agent and its preparation method and application
CN111972429A (en) * 2020-08-21 2020-11-24 重庆中邦药业(集团)有限公司 Preparation method of double-microcapsule longicorn pesticide
CN114766498A (en) * 2022-05-17 2022-07-22 上海明德立达生物科技有限公司 Preparation method and application of microcapsule suspension-suspending agent containing metolachlor and flumioxazin

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103651550A (en) * 2012-09-19 2014-03-26 青岛星牌作物科学有限公司 Microcapsule suspending agent prepared from carbosulfan, chlorpyrifos and abamectin by compounding
CN107535505A (en) * 2016-06-28 2018-01-05 佛山市盈辉作物科学有限公司 Herbicidal combinations containing S-metolachlor and flumioxazin
CN106900723A (en) * 2017-03-03 2017-06-30 江苏莱科化学有限公司 A kind of soybean Herbicidal combinations
CN107593725A (en) * 2017-08-30 2018-01-19 北京明德立达农业科技有限公司 A kind of composition pesticide and its application
CN108432751A (en) * 2018-03-27 2018-08-24 江苏邦盛生物科技有限责任公司 A kind of pesticide microcapsule suspending agent and its preparation method and application
CN111972429A (en) * 2020-08-21 2020-11-24 重庆中邦药业(集团)有限公司 Preparation method of double-microcapsule longicorn pesticide
CN114766498A (en) * 2022-05-17 2022-07-22 上海明德立达生物科技有限公司 Preparation method and application of microcapsule suspension-suspending agent containing metolachlor and flumioxazin

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