CN110859187A - Sterilization composition containing ametoctradin and flumorph and preparation method thereof - Google Patents

Sterilization composition containing ametoctradin and flumorph and preparation method thereof Download PDF

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Publication number
CN110859187A
CN110859187A CN201911032264.4A CN201911032264A CN110859187A CN 110859187 A CN110859187 A CN 110859187A CN 201911032264 A CN201911032264 A CN 201911032264A CN 110859187 A CN110859187 A CN 110859187A
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Prior art keywords
flumorph
ametoctradin
agent
wetting agent
mixed solution
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CN201911032264.4A
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Inventor
石伟贤
莫俊锐
刘爱杰
王爱臣
廖联安
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Huizhou Yinnong Technology Co Ltd
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Huizhou Yinnong Technology Co Ltd
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Priority to CN201911032264.4A priority Critical patent/CN110859187A/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
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • 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
    • A01N37/36Biocides, 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 at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38Biocides, 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 at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, 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

Abstract

The embodiment of the invention discloses a sterilization composition containing ametoctradin and flumorph and a preparation method thereof, wherein the sterilization composition comprises 10-30% of ametoctradin and 10-30% of flumorph in mass percentage as effective components, 1-10% of a wetting agent, 1-10% of a dispersing agent, 0.5-2% of a pH value regulator, 0.1-0.3% of a defoaming agent and 18-77% of a filling agent. The method for preparing the bactericidal composition comprises the step of dissolving the dispersing agent, the wetting agent, the pH value regulator, the defoaming agent and the filling agent in water according to the proportion to form a mixed solution. According to the embodiment of the invention, the pesticide effective components ametoctradin and flumorph are subjected to wet grinding by a sand mill under the action of a dispersing agent and a wetting agent to form fine particles with the particle size of less than 4 microns, the fine particles are atomized into small droplets by a high-pressure spraying device, and the small droplets are contacted with hot air in a drying tower to be instantly evaporated to form spherical particles with hollow interiors.

Description

Sterilization composition containing ametoctradin and flumorph and preparation method thereof
Technical Field
The embodiment of the invention relates to the technical field of pesticides, and particularly relates to a bactericidal composition containing ametoctradin and flumorph and a preparation method thereof.
Background
At present, conventional fungicides for controlling diseases caused by peronospora and phytophthora fungi are mainly amides, such as: metalaxyl, benalaxyl and oxadixyl, but the two diseases obviously generate drug resistance to amide compounds, so the control effect is poor; another class is aliphatic fungicides, such as: the bactericide is a mixture of cymoxanil and mancozeb, and the problems of drug resistance of the bactericide in different degrees also occur in most areas of China. In addition, organic phosphorus such as fosetyl-aluminum and thiocarbamates such as mancozeb and thiram also have a certain prevention effect on diseases caused by peronospora and phytophthora, fosetyl-aluminum is not ideal at present due to resistance problems, mancozeb is a protective agent, and no treatment effect is realized after the diseases occur.
In conclusion, in the prior art, when the adopted bactericide is used for preventing and treating diseases, the bactericide has the problem of poor pesticide effect.
Disclosure of Invention
Therefore, the embodiment of the invention provides a sterilization composition and a preparation method thereof, and aims to solve the problems of poor effect and high dosage of a sterilization agent in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
the sterilizing composition containing ametoctradin and flumorph comprises 10-30% of ametoctradin and 10-30% of flumorph in mass percentage as effective components.
Preferably, the bactericidal composition further comprises the following raw materials in percentage by mass: 1 to 10% of wetting agent, 1 to 10% of dispersing agent, 0.5 to 2% of pH value regulator, 0.1 to 0.3% of defoaming agent and 18 to 77% of filling agent.
Preferably, the dispersant is one or more of polycarboxylate dispersant Ultrasperse, polycarboxylate dispersant Geropon T/36, polycarboxylate dispersant Tersperse 2700, sulfonate dispersant YUS-207K and phenolsulfonic acid condensate sodium salt Tamol DN.
Preferably, the wetting agent is one or more of alkyl naphthalene sulfonate wetting agent YUS-SXC, anion wetting agent Terwet1004 and naphthalene sulfonate wetting agent L-WET/P.
Preferably, the pH regulator is ammonium sulfate or citric acid.
Preferably, the filler is one or more of sodium lignosulfonate dispersants REAX910, D863, LX SPECIAL, calcined kaolin and white carbon black.
The embodiment of the invention also provides a method for preparing the ametoctradin and flumorph-containing bactericidal composition, which comprises the steps of adding the ametoctradin and the flumorph into a solution according to the mass percentage, homogenizing and dispersing to form a mixed solution, grinding materials in the mixed solution until the particle size D98 is not more than 4 mu m, and then carrying out spray drying to obtain the bactericidal composition.
Preferably, the temperature of the mixed solution is controlled to be not higher than 35 ℃ during the grinding process.
Preferably, the spray drying results in spherical particles having a diameter of 0.1mm to 0.2 mm.
Preferably, the preparation of the mixed solution further comprises the step of adding the dispersing agent, the wetting agent, the pH value regulator, the defoaming agent and the filler into water according to the proportion and uniformly mixing.
Preferably, the homogenizing and dispersing process is to homogenize and disperse the mixed solution for 30min by a homogenizer, and the rotating speed is 1470 r/min.
In the examples of the present invention, Ametoctradin (Ametoctradin) CAS accession number: 865318-97-4, is a triazolopyrimidine bactericide, belongs to mitochondrial respiration inhibitor, has control effect on downy mildew and phytophthora oomycetes fungi, has strong residual activity and rain resistance, and can effectively prevent fungi from generating resistance by adding flumorph in the formula.
In the embodiment of the invention, flumorph, common name: flumorph, trade name: mike, test code: SYP-L190, has prophylactic and therapeutic effects and good systemic conductivity. A large number of indoor and field use results show that flumorph has good treatment and protection effects on various diseases caused by oomycete fungi, such as cucumber downy mildew, grape downy mildew, litchi downy/mildew and the like.
The embodiment of the invention has the following advantages:
according to the embodiment of the invention, the pesticide active ingredients ametoctradin and flumorph are subjected to wet grinding by a sand mill under the action of a dispersing agent and a wetting agent to form fine particles with the particle size of less than 4 microns, the fine particles are atomized into small droplets by a high-pressure spraying device and are contacted with hot air in a drying tower, moisture is evaporated instantly to form hollow spherical particles, and the hollow spherical particles have certain structural strength and good flow, can bear external force of packaging and transportation and cannot be crushed to form dust, and are immediately reduced into the state of the active ingredients before spray drying by water when in use, so that the advantages of small particle size, high suspension percentage and safety, convenience and no dust in use of water dispersible granules are achieved.
Compared with the conventional medicament for preventing and treating the similar diseases, the bactericidal composition provided by the embodiment of the invention has the advantages of outstanding efficacy, low dosage, high activity and longer application interval period, and particularly has more obvious reflection on test results in regions with serious drug resistance.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples 1 to 5
Table 1 shows a fungicidal composition containing ametoctradin and flumorph according to embodiments 1 to 5 of the present invention.
TABLE 1
Figure BDA0002250504580000041
Table 2 shows the germicidal compositions of comparative examples 1 to 4 in the prior art.
TABLE 2
Figure BDA0002250504580000042
In the embodiment of the invention, the dispersing agent Ultrasperse and Geropon T/36 are selected from Solvay (Zhenjiang) chemical Co., Ltd, the dispersing agent Tamol DN is selected from Pasv (China) Co., Ltd, the dispersing agent YUS-207K is selected from Jersey chemical Co., Ltd, the dispersing agent Terspese 2700 is selected from Henski functional products, the wetting agent L-WET/P is selected from Solvay (Zhenjiang) chemical Co., Ltd, the wetting agent Terwet1004 is selected from Henski functional products, the wetting agent YUS-SXC is selected from Jersey chemical Co., Ltd, the antifoaming agent 1501 is selected from Guangzhou chemical Co., Ltd, the filling agent REAX910 is selected from Maidwey Virgig (China) investment Co., Ltd, the filling agent D863 is selected from Shenzhen Zhongsheng biological science Co., Ltd, and the filling agent LX SPECIAL is selected from Shanghai Tesski chemical Co..
Table 3 shows the properties of the fungicidal compositions containing ametoctradin and flumorph of examples 1 to 5 of the present invention
TABLE 3
Figure BDA0002250504580000051
Table 4 shows the properties of the fungicidal compositions of comparative examples 1 to 4 of the present invention
TABLE 4
Figure BDA0002250504580000061
As shown in tables 3 and 4, the fungicidal compositions containing ametoctradin and flumorph according to the examples of the present invention have the optimum values in various properties.
Example 6
The preparation method of the pyrimethanil-containing and flumorph-containing bactericidal composition provided by the embodiment 1, the embodiment 2, the embodiment 3, the embodiment 4 or the embodiment 5 of the invention comprises the following steps:
1. adding a dispersing agent, a wetting agent, a pH value regulator and a filling agent into water according to a proportion to dissolve to form a mixed solution;
2. adding ametoctradin and flumorph into the mixed solution, and homogenizing and dispersing for 30min by using a homogenizer at the rotating speed of 1470 r/min;
3. grinding the uniformly dispersed mixed material by using a colloid mill, and then grinding by using a sand mill, wherein the temperature of the mixed material is controlled to be not higher than 35 ℃ in the grinding process, and the particle size D98 of the material is not more than 4 mu m; after grinding, the viscosity of the mixed material is not higher than 300mpa & s, the viscosity is too high, the slurry fluidity is poor, and a nozzle is easily blocked during spray drying, so that the spray efficiency is influenced;
4. transferring the ground mixed material to a high-temperature high-pressure spray tower for spray drying to obtain spherical particles, wherein the diameter of the spherical particles is 0.1-0.2 mm, and the water content is less than or equal to 3%; when spraying at high temperature and high pressure, the temperature and pressure are controlled to be proper, so that water is evaporated instantly when the slurry is atomized, and the bactericidal composition of the embodiment of the invention is obtained.
In the embodiment of the invention, certain defoaming agents are respectively added in the steps 1, 2 and 3 in the manufacturing process for defoaming.
Comparative example 1
The comparative example differs from inventive example 4 in that the dispersant and filler are different, the dispersant of the comparative example is 6kg Morwet D425, the filler is clay supplemented to 100%, and the preparation method is the same as example 4.
Comparative example 2
The comparative example differs from example 4 according to the invention in that the dispersant and wetting agent used are different, the dispersant of the comparative example being 8kg Suagil NSR and the wetting agent 4kg Cresplus 1209, and the preparation method being identical to example 4.
Comparative example 3
The difference between the comparative example and the inventive example is that the wetting agent and the filler are different, the wetting agent of the comparative example is 6kg Tersperse 4894, the filler is titanium dioxide to 100%, and the preparation method is the same as that of example 4.
Comparative example 4
The difference between the comparative example and the embodiment of the invention is that the used dispersing agent, wetting agent and filling agent are different, the dispersing agent of the comparative example is 5kg Agrilan700, the wetting agent is 4kg MORFET-IP, the filling agent is white carbon black to supplement 100 percent, and the preparation method is consistent with the embodiment 4.
Test examples
1. And (3) test treatment: the test subjects are treated according to the grouping shown in the table 5, the ametoctradin and flumorph-containing sterilization composition of the examples 1-5 is used as a test medicament, the sterilization composition of the comparative examples 1-4 and a commercial product are used as a control medicament, and a clear water blank is used as a control to perform a control effect test.
TABLE 5
Figure BDA0002250504580000081
2 method of application
2.1 application time and times: the medicine application is started at the early stage of the potato late blight, and the medicine application is continuously carried out for 2 times at intervals of 7 days. The specific time is as follows: 22 days 5 and 29 months 2019 and 5 and 29 months 2019.
2.2 instruments used and application method: the liquid medicine is prepared by adopting a secondary dilution method, and the main preparation tools comprise: graduated cylinders, pipettes, glass rods, and the like. The PB-16 type sprayer sprays, the spraying pressure is 0.2-0.4Mpa, the diameter of a spray hole is 1mm, and the average water consumption of each district is about 1.35 liters.
2.3 soil data: sandy soil, pH value 5.6, organic matter content 24.8 g/kg.
2.4 prevention and treatment of non-target biological conditions: no other agents were administered during the trial.
3 investigation and results
3.1 investigation method: sampling was done at 5 points on the diagonal of each cell, 2 plants were investigated at each point, and all leaves were examined. Classification method (in units of leaves): level 0: no disease spots; level 1: the lesion area accounts for less than 5% of the whole leaf area; and 3, level: the lesion area accounts for 6-10% of the whole leaf area; and 5, stage: the lesion area accounts for 11-20% of the whole leaf area; and 7, stage: the lesion area accounts for 21-50% of the whole leaf area; and 9, stage: the lesion area accounts for more than 50% of the whole leaf area.
3.2 survey time and number: the survey was conducted 2 times 7 and 14 days after 2 times of administration, respectively, 1 time. The specific time is as follows: 6 and 5 days in 2019 and 6 and 12 days in 2019.
3.3 the test complies with the quality management standard of pesticide registration test, the standard of pesticide field efficacy test GB/T17980.34-2000, SOP-TM-003a potato late blight test, and the calculation formula is as follows
Figure BDA0002250504580000091
Figure BDA0002250504580000092
3.4 Effect on other organisms: no significant effect of the test agent on other organisms was observed during the test.
3.5 test results
3.5.1 evaluation of control Effect: the average control results for potato late blight are shown in table 6.
TABLE 6
Figure BDA0002250504580000093
Figure BDA0002250504580000101
The data in the table are mean values of 4 replicates and the analysis of variance was processed by DPS (v7.05 version).
3.5.2 safety: during the test period, the potatoes grow normally, and no phytotoxicity symptoms are observed.
3.5.3 results: through the comparison of pesticide effects, the control effect of the bactericidal composition containing the ametoctradin and the flumorph in the embodiment of the invention is obviously better than that of a comparative example, which shows that the bactericidal composition in the embodiment of the invention has more reasonable collocation and stronger compounding effect.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. The sterilizing composition containing ametoctradin and flumorph is characterized by comprising 10-30% of ametoctradin and 10-30% of flumorph in mass percentage as effective components.
2. The ametoctradin-containing bactericidal composition according to claim 1,
the bactericidal composition also comprises the following raw materials in percentage by mass: 1 to 10% of wetting agent, 1 to 10% of dispersing agent, 0.5 to 2% of pH value regulator, 0.1 to 0.3% of defoaming agent and 18 to 77% of filling agent.
3. The ametoctradin-and flumorph-containing fungicidal composition according to claim 2,
the dispersant is one or more of polycarboxylate dispersant Ultrasperse, polycarboxylate dispersant Geropon T/36, polycarboxylate dispersant Terspese 2700, sulfonate dispersant YUS-207K and phenolsulfonate dispersant Tamol DN.
4. The ametoctradin-and flumorph-containing fungicidal composition according to claim 2,
the wetting agent is one or more of alkyl naphthalene sulfonate wetting agent YUS-SXC, anion wetting agent Terwet1004 and naphthalene sulfonate wetting agent L-WET/P.
5. The ametoctradin-and flumorph-containing fungicidal composition according to claim 2,
the pH value regulator is ammonium sulfate or citric acid.
6. The ametoctradin-and flumorph-containing fungicidal composition according to claim 2,
the filler is one or more of sodium lignosulfonate dispersants REAX910, D863 and LX SPECIAL and calcined kaolin and white carbon black.
7. The preparation method of the ametoctradin-flumorph-containing bactericidal composition according to claim 1 is characterized by comprising the steps of adding ametoctradin and flumorph into a solution according to mass percentage, carrying out homogeneous dispersion to form a mixed solution, grinding materials in the mixed solution until the particle size D98 is not more than 4 μm, and carrying out spray drying to obtain the bactericidal composition.
8. The method of claim 7,
and controlling the temperature of the mixed solution to be not higher than 35 ℃ in the grinding process.
9. The method of claim 7,
and carrying out spray drying to obtain spherical particles, wherein the diameter of the spherical particles is 0.1-0.2 mm.
10. The method of claim 7,
the preparation of the mixed solution also comprises the steps of adding the dispersing agent, the wetting agent, the pH value regulator, the defoaming agent and the filler into water according to the proportion, uniformly mixing, and carrying out uniform dispersion on the mixed solution for 30min by a homogenizer at the rotating speed of 1470 r/min.
CN201911032264.4A 2019-10-28 2019-10-28 Sterilization composition containing ametoctradin and flumorph and preparation method thereof Pending CN110859187A (en)

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Application publication date: 20200306