CN114831128A - Pesticide preparation containing difenoconazole and azoxystrobin - Google Patents

Pesticide preparation containing difenoconazole and azoxystrobin Download PDF

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Publication number
CN114831128A
CN114831128A CN202210356027.9A CN202210356027A CN114831128A CN 114831128 A CN114831128 A CN 114831128A CN 202210356027 A CN202210356027 A CN 202210356027A CN 114831128 A CN114831128 A CN 114831128A
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China
Prior art keywords
azoxystrobin
difenoconazole
starch
phospholipid
agent
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN202210356027.9A
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Chinese (zh)
Inventor
王小明
姚李
朱仁发
乔琳
丁爱琴
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Anhui Huachen Testing Technology Research Institute Co ltd
Hefei University
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Anhui Huachen Testing Technology Research Institute Co ltd
Hefei University
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Priority to CN202210356027.9A priority Critical patent/CN114831128A/en
Publication of CN114831128A publication Critical patent/CN114831128A/en
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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
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647Triazoles; Hydrogenated triazoles
    • A01N43/6531,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • 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
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • 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
    • A01N43/541,3-Diazines; Hydrogenated 1,3-diazines
    • 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

Abstract

The invention discloses a pesticide preparation containing difenoconazole and azoxystrobin, which is a water dispersible granule and comprises the following components in percentage by mass: 10-20% of difenoconazole, 15-30% of azoxystrobin, 8-12% of dispersing agent, 3-6% of wetting agent, 3-5% of disintegrating agent, 10-15% of starch-phospholipid compound and the balance of kaolin. The pesticide preparation provided by the invention has the advantages of high content of active ingredients, good pesticide effect, high heat-resistant stability, excellent disintegration and dispersion performances in water, convenience in use, easiness in storage and no dust pollution in the production and use processes.

Description

Pesticide preparation containing difenoconazole and azoxystrobin
Technical Field
The invention relates to the technical field of pesticide preparations, and in particular relates to a pesticide preparation containing difenoconazole and azoxystrobin.
Background
The azoxystrobin belongs to strobilurin bactericides, can inhibit spore germination and hypha growth, has the characteristics of high efficiency and broad spectrum, and has good activity on crop fungal diseases such as powdery mildew, rust disease, glume blight, net blotch, downy mildew, rice blast and the like. Difenoconazole is a sterol demethylation inhibitor, can inhibit the synthesis of sterol of cell walls and prevent the growth of fungi, and is commonly used for preventing and treating scab, anthracnose, white rot, alternaria leaf spot, powdery mildew, brown spot, rust disease, stripe rust, gibberellic disease and the like of crops. A plurality of researches show that the combination of azoxystrobin and difenoconazole has a synergistic interaction effect, and can play a very significant effect particularly in preventing and treating two important diseases of rice, namely rice blast and sheath blight.
The water dispersible granule is a granular preparation which can be quickly disintegrated and dispersed in water to form a highly suspended solid-liquid dispersion system, and has the advantages of no dust pollution, easy storage, convenient use and good drug effect. However, the water dispersible granule is easy to have the problems of agglomeration, crystallization, reduced disintegration performance and the like in the preparation process; meanwhile, poor thermal stability is also a common problem in water dispersible granule formulations, and the disintegration performance and the suspension property are usually obviously reduced after the water dispersible granule formulations are stored for a period of time. At present, the water dispersible granules taking azoxystrobin and difenoconazole as main effective components are less researched, and have larger market development potential.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a pesticide preparation containing difenoconazole and azoxystrobin.
The invention provides a pesticide preparation containing difenoconazole and azoxystrobin, which is a water dispersible granule and comprises the following components in percentage by mass: 10-20% of difenoconazole, 15-30% of azoxystrobin, 8-12% of dispersing agent, 3-6% of wetting agent, 3-5% of disintegrating agent, 10-15% of starch-phospholipid compound and the balance of kaolin.
Preferably, the preparation method of the starch-phospholipid complex comprises the following steps: adding starch and phospholipid into water, heating and stirring for reaction, cooling, freeze-drying and crushing to obtain the starch phospholipid liposome, wherein the mass ratio of the starch to the phospholipid is 1: (0.05-0.15).
Preferably, the temperature for heating and stirring reaction is 60-80 ℃ and the time is 1-2 h.
Preferably, the starch is corn starch; the phospholipid is soybean phospholipid.
The disintegrating agent is an auxiliary material for accelerating disintegration and diffusion of the water dispersible granule. The invention adopts urea and polyethylene glycol 6000 according to the mass ratio of 1: (0.5-1) to form a disintegrating agent. The urea has excellent disintegration property and high disintegration speed, but has poor thermal stability, and the viscosity of the material is easily increased in the preparation process of the water dispersible granule or in the environment with higher temperature, so that the disintegration property and the suspension property are reduced; the polyethylene glycol 6000 has certain surface activity, can increase the penetration and wetting property of the granules, and enables water to quickly penetrate into the granules, so that the disintegration of the granules is accelerated, the anti-sticking and lubricating effects can be achieved, and the flowability of the granules is increased. According to the invention, the urea and the polyethylene glycol 6000 are combined according to a certain proportion, so that the thermal stability and the disintegration speed of the granules can be considered, and the granules can be rapidly disintegrated.
The dispersant can be adsorbed on the surface of the particles to prevent the particles from agglomerating, so that the drug particles have good suspension property. The dispersing agent of the present invention is not particularly limited, and preferably, the dispersing agent is at least one of EO/PO block copolymer, maleic acid-acrylic acid copolymer sodium salt, alkyl naphthalene sulfonate; preferably, the dispersing agent is prepared by mixing maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: (0.2-0.5).
The wetting agent can reduce the surface tension of water, improve the wettability of a solid-liquid interface and accelerate the disintegration speed. The wetting agent is not particularly limited in the present invention, and preferably, the wetting agent is at least one of sodium laureth sulfate, dioctyl sodium sulfosuccinate, sodium dodecyl sulfate, and sodium dodecyl benzene sulfonate; preferably, the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: (0.5-1).
A preparation method of the pesticide preparation containing difenoconazole and azoxystrobin comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out air flow crushing to obtain mother powder, mixing the mother powder with a proper amount of water, and carrying out granulation, drying and screening to obtain the difenoconazole.
Preferably, in the preparation method, the mass ratio of the mother powder to the water is 1: (0.08-0.15).
The invention has the following beneficial effects:
according to the invention, the starch-phospholipid compound and kaolin are compounded to serve as a filler, phospholipid has good emulsibility and lubricity, and is complexed on a molecular chain of starch, so that the functions of emulsifying dispersion and viscosity reduction of a medicine fused crystal can be achieved at high temperature, steric hindrance can be generated, and the dispersibility of medicine particles is improved, thereby weakening the aggregation and agglomeration of medicines, and improving the disintegration, suspension and heat storage stability of water dispersible granules; the urea and the polyethylene glycol 6000 are compounded to be used as a disintegrating agent, and the rapid disintegration of the urea, the high penetration wettability, the anti-sticking property, the lubrication property and the fluidity of the polyethylene glycol 6000 are utilized, so that the processing, the heat storage stability and the disintegration speed of the granules can be considered, and the granules can be rapidly disintegrated. The invention provides a water dispersible granule formula with azoxystrobin and difenoconazole as main active ingredients, which has the advantages of high content of active ingredients, good drug effect, high heat-resistant stability, excellent disintegration and dispersion performances in water, convenience in use, easiness in storage and no dust pollution in the production and use processes, and is a novel pesticide preparation with good application prospect.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A pesticide preparation containing difenoconazole and azoxystrobin is a water dispersible granule and comprises the following components in percentage by mass: 10% of difenoconazole, 15% of azoxystrobin, 8% of dispersing agent, 3% of wetting agent, 3% of disintegrating agent, 10% of starch-phospholipid compound and the balance of kaolin;
the preparation method of the starch-phospholipid compound comprises the following steps: adding corn starch and soybean lecithin into water, heating and stirring at 60 ℃ for reaction for 1h, cooling, freeze-drying and crushing to obtain the soybean lecithin-containing corn starch, soybean lecithin-containing corn starch mixture, wherein the mass ratio of corn starch to soybean lecithin is 1: 0.05; the dispersing agent is prepared from maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: 0.2; the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: 0.5; the disintegrating agent is prepared from urea and polyethylene glycol 6000 according to the mass ratio of 1: 0.5.
The preparation method comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out jet milling to obtain mother powder, mixing the mother powder with water accounting for 8% of the mass of the mother powder, and carrying out granulation, drying and screening to obtain the compound difenoconazole.
Example 2
A pesticide preparation containing difenoconazole and azoxystrobin is a water dispersible granule and comprises the following components in percentage by mass: 20% of difenoconazole, 30% of azoxystrobin, 12% of dispersing agent, 6% of wetting agent, 5% of disintegrating agent, 15% of starch-phospholipid compound and the balance of kaolin;
the preparation method of the starch-phospholipid compound comprises the following steps: adding corn starch and soybean lecithin into water, heating and stirring at 80 ℃ for reaction for 2 hours, cooling, freeze-drying and crushing to obtain the soybean lecithin-containing corn starch, soybean lecithin-containing corn starch composite powder, wherein the mass ratio of corn starch to soybean lecithin is 1: 0.15; the dispersing agent is prepared from maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: 0.5; the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: 1, preparing a composition; the disintegrating agent is prepared from urea and polyethylene glycol 6000 according to the mass ratio of 1: 1.
The preparation method comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out jet milling to obtain mother powder, mixing the mother powder with water accounting for 15% of the mass of the mother powder, and carrying out granulation, drying and screening to obtain the difenoconazole.
Example 3
The pesticide preparation containing difenoconazole and azoxystrobin is a water dispersible granule and comprises the following components in percentage by mass: 12.5% of difenoconazole, 20% of azoxystrobin, 10% of dispersing agent, 5% of wetting agent, 1.5% of disintegrating agent, 12.5% of starch-phospholipid compound and the balance of kaolin;
the preparation method of the starch-phospholipid compound comprises the following steps: adding corn starch and soybean lecithin into water, heating and stirring at 75 ℃ for reaction for 1.5 hours, cooling, freeze-drying and crushing to obtain the soybean lecithin-containing corn starch, soybean lecithin-containing soybean lecithin, wherein the mass ratio of corn starch to soybean lecithin is 1: 0.1; the dispersing agent is prepared from maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: 0.25; the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: 0.8; the disintegrating agent is prepared from urea and polyethylene glycol 6000 according to the mass ratio of 1: 0.6.
The preparation method comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out jet milling to obtain mother powder, mixing the mother powder with water accounting for 10% of the mass of the mother powder, and carrying out granulation, drying and screening to obtain the difenoconazole.
Comparative example 1
The pesticide preparation containing difenoconazole and azoxystrobin is a water dispersible granule and comprises the following components in percentage by mass: 12.5% of difenoconazole, 20% of azoxystrobin, 10% of dispersing agent, 5% of wetting agent, 4.5% of disintegrating agent, 12.5% of corn starch and the balance of kaolin;
wherein the dispersant is prepared from maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: 0.25; the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: 0.8; the disintegrating agent is prepared from urea and polyethylene glycol 6000 according to the mass ratio of 1: 0.6.
The preparation method comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, corn starch and kaolin, carrying out jet milling to obtain mother powder, mixing the mother powder with water accounting for 10% of the mass of the mother powder, and carrying out granulation, drying and screening to obtain the difenoconazole-azoxystrobin powder.
Comparative example 2
A pesticide preparation containing difenoconazole and azoxystrobin is a water dispersible granule and comprises the following components in percentage by mass: 12.5% of difenoconazole, 20% of azoxystrobin, 10% of dispersing agent, 5% of wetting agent, 1.5% of disintegrating agent, 12.5% of starch-phospholipid compound and the balance of kaolin;
The preparation method of the starch-phospholipid compound comprises the following steps: adding corn starch and soybean lecithin into water, heating and stirring at 75 ℃ for reaction for 1.5 hours, cooling, freeze-drying and crushing to obtain the soybean lecithin-containing corn starch, soybean lecithin-containing soybean lecithin, wherein the mass ratio of corn starch to soybean lecithin is 1: 0.1; the dispersing agent is prepared from maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: 0.25; the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: 0.8; the disintegrating agent is urea.
The preparation method comprises the following steps: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out jet milling to obtain mother powder, mixing the mother powder with water accounting for 10% of the mass of the mother powder, and carrying out granulation, drying and screening to obtain the difenoconazole.
Test examples
The water dispersible granules prepared in example 3 and comparative examples 1-2 were tested for dispersibility and thermal stability, respectively, wherein the thermal stability was tested by reference to GB-T19136-2003. The test results are shown in table 1:
TABLE 1 Performance index of Water dispersible granules
Figure BDA0003582851090000061
Therefore, the water dispersible granule prepared by optimizing the formula has good dispersibility, can be quickly disintegrated in water, has a suspension rate of over 90 percent after hot storage, and has excellent hot storage stability.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (7)

1. A pesticide preparation containing difenoconazole and azoxystrobin is characterized in that the pesticide preparation is a water dispersible granule, and comprises the following components in percentage by mass: 10-20% of difenoconazole, 15-30% of azoxystrobin, 8-12% of dispersing agent, 3-6% of wetting agent, 3-5% of disintegrating agent, 10-15% of starch-phospholipid compound and the balance of kaolin;
the disintegrating agent is prepared from urea and polyethylene glycol 6000 in a mass ratio of 1: (0.5-1).
2. The pesticide preparation containing difenoconazole and azoxystrobin according to claim 1, characterized in that the preparation method of the starch-phospholipid complex is as follows: adding starch and phospholipid into water, heating and stirring for reaction, cooling, freeze-drying and crushing to obtain the starch phospholipid liposome, wherein the mass ratio of the starch to the phospholipid is 1: (0.05-0.15).
3. The pesticide preparation containing difenoconazole and azoxystrobin according to claim 2, wherein the heating and stirring reaction is carried out at 60-80 ℃ for 1-2 h.
4. A pesticidal formulation containing difenoconazole and azoxystrobin according to claim 2, characterized in that the starch is corn starch; the phospholipid is soybean phospholipid.
5. A pesticide formulation containing difenoconazole and azoxystrobin according to claim 1, characterized in that the dispersant is at least one of EO/PO block copolymer, maleic acid-acrylic acid copolymer sodium salt, alkyl naphthalene sulfonate; preferably, the dispersing agent is prepared by mixing maleic acid-acrylic acid copolymer sodium salt and EO/PO block copolymer according to the mass ratio of 1: (0.2-0.5).
6. The pesticide preparation containing difenoconazole and azoxystrobin according to claim 1, wherein the wetting agent is at least one of sodium laureth sulfate, dioctyl sodium sulfosuccinate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; preferably, the wetting agent is prepared from sodium laureth sulfate and sodium dodecyl sulfate in a mass ratio of 1: (0.5-1).
7. A method for preparing a pesticide formulation containing difenoconazole and azoxystrobin according to any one of claims 1 to 6, which comprises: uniformly mixing difenoconazole, azoxystrobin, a dispersing agent, a wetting agent, a disintegrating agent, a starch-phospholipid compound and kaolin, carrying out air flow crushing to obtain mother powder, mixing the mother powder with a proper amount of water, and carrying out granulation, drying and screening to obtain the compound difenoconazole.
CN202210356027.9A 2022-04-06 2022-04-06 Pesticide preparation containing difenoconazole and azoxystrobin Pending CN114831128A (en)

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