CN113598166A - Bactericidal granules and preparation method and application thereof - Google Patents

Bactericidal granules and preparation method and application thereof Download PDF

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Publication number
CN113598166A
CN113598166A CN202110932499.XA CN202110932499A CN113598166A CN 113598166 A CN113598166 A CN 113598166A CN 202110932499 A CN202110932499 A CN 202110932499A CN 113598166 A CN113598166 A CN 113598166A
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agent
wetting agent
optionally
dispersant
metalaxyl
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王杰
罗湘仁
王欢
郭一兵
刘寿
叶开
单亮
胡泽鹏
刘斌
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Shijiazhuang Nongxin Biotechnology Group Co ltd
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Shijiazhuang Nongxin Biotechnology Group Co ltd
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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
    • 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
    • A01N25/12—Powders or granules
    • 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
    • A01N25/12—Powders or granules
    • A01N25/14—Powders or granules wettable
    • 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
    • A01N37/44—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 at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/46—N-acyl derivatives
    • 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
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings

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

Abstract

The embodiment of the invention relates to a sterilization granule and a preparation method and application thereof, relating to the field of pesticides, and the sterilization granule comprises the following raw materials in parts by mass based on the total weight of the granule: 0.1-5% of pesticide active ingredient, 1-10% of wetting agent, 2-8% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of monopotassium phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%; wherein the pesticide active ingredients comprise the following components in a mass ratio of 1: fludioxonil and metalaxyl-M of (1-10). The invention utilizes silicon dioxide to adsorb metalaxyl-M, thereby preparing granules with good storage stability, the two components have complementary toxic effects, the drug effect can be improved, and the lasting period can be prolonged; no dust flying during application and no environmental pollution; convenient to use, it is efficient.

Description

Bactericidal granules and preparation method and application thereof
Technical Field
The invention relates to the field of pesticides, and particularly relates to a bactericidal granule as well as a preparation method and application thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Fludioxonil is a non-systemic phenylpyrrole fungicide, has the name of fludioxonil in English and the chemical name of 4- (2, 2-difluoro-1, 3-benzodioxyl-4-yl) pyrrole-3-nitrile in molecular formula C12H6F2N2O2Relative molecular weight 248.18, CAS No.: 131341-86-1, the structural formula is as formula (I), inhibits hypha growth by inhibiting the transshipment related to glucose phosphorylation, finally leads to germ death, has good control effect on crop diseases caused by various ascomycetes, basidiomycetes and adelomycetes, and is widely applied to disease control in storage of various crops and fruits and vegetables.
Figure BDA0003211631710000011
metalaxyl-M is a ribosome RNAI synthesis inhibitor with systemic property, and is named as YingwenMetaxalyl-M, chemical name N- (2, 6-xylyl) -N- (methoxyacetyl) -D-alanine methyl ester, molecular formula C15H20O4N, relative molecular weight 279.33, CAS No.: 70630-17-0, the structural formula is shown in formula (II), can be absorbed by root, stem and leaf of plant, and transmitted to each organ of plant, has bidirectional transmission performance, and has high efficiency on plant diseases caused by downy mildew, phytophthora, and pythium.
Figure BDA0003211631710000012
At present, fludioxonil and metalaxyl-M are mainly suspending agents, and the suspending agent has the problems of slow effect, short duration and need of multiple application. The pure metalaxyl-M is viscous liquid and is difficult to process into a stable solid dosage form.
Disclosure of Invention
Object of the Invention
The invention aims to provide a bactericidal granule which has quick response and long duration and can reduce the application times, a preparation method and application thereof.
Solution scheme
In order to achieve the purpose of the present invention, an embodiment of the present invention provides a bactericidal granule, which comprises the following raw materials, by weight: 0.1-5% of pesticide active ingredient, 1-10% of wetting agent, 2-8% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of monopotassium phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%;
wherein the pesticide active ingredients comprise the following components in a mass ratio of 1: fludioxonil and metalaxyl-M of (1-10).
Further, the material comprises the following raw materials in percentage by mass: 0.1-2.5% of pesticide active ingredient, 2-5% of wetting agent, 3-7% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of potassium dihydrogen phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%; optionally, 0.1-1% of pesticide active ingredient, 2-5% of wetting agent, 3-7% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of potassium dihydrogen phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%; optionally, 0.1-0.6% of pesticide active ingredient, 3% of wetting agent, 5% of dispersing agent, 0.3% of defoaming agent, 15% of corn starch, 2% of glucose, 15% of monopotassium phosphate and 1% of silicon dioxide, and the balance of kaolin to 100%.
Further, the weight ratio of fludioxonil to metalaxyl-M is 1: (2-5), optionally 1: 3.
further, the wetting agent is at least one selected from sodium dodecyl sulfate, wetting agent SA, nekal BX, wetting agent BT8F, wetting agent SR-05 and wetting agent GY-W04; optionally, the wetting agent is wetting agent SA.
Further, the dispersant is selected from at least one of NNO, dispersant 1628, dispersant Ufoxane3A, dispersant SD816, dispersant GY-D800 and sodium lignosulfonate LX; optionally, the dispersant is dispersant 1628.
Further, the defoaming agent is defoaming agent Soap-L.
On the other hand, the preparation method of the bactericidal granule is provided, and the bactericidal granule is obtained by uniformly mixing the raw materials, crushing, granulating and drying.
Further, the raw material mixing method comprises the following steps: mixing metalaxyl-M and silicon dioxide in proportion, stirring until no blocky matter exists, and then uniformly mixing fludioxonil, a wetting agent, a dispersing agent, a defoaming agent, corn starch, glucose, monopotassium phosphate, silicon dioxide and kaolin in proportion to obtain a mixed material.
Further, the crushing method comprises the following steps: and crushing the mixed material into primary particle materials with D90 being less than or equal to 75 mu m.
Further, the granulation method comprises the following steps: adding water into the primary particle material, uniformly mixing, and then performing granulation treatment; optionally, water is added in an amount of 5-30% by weight of the primary particulate material; optionally, the grain size of the material obtained by the granulation treatment is 12-80 meshes.
Further, the drying conditions were: 70-90 ℃ for 0.5-2 h.
Proper technological parameters can improve the passenger flow and the fineness, improve the particle size distribution and the particle size, further improve the storage stability of the micro-granules and improve the drug effect of the granules. Preferably, the specific steps may be: the raw materials are mixed in a double-helix conical mixer, the stirring speed is 12-30r/min, and the time duration is 0.5-1 h. The pulverization is carried out under the condition of jet milling, and the air pressure is 0.7-0.9 Mpa; the speed of the grading wheel is 2500-; obtaining particles with D90 being less than or equal to 75 mu m to obtain primary particle materials; then adding the primary particle material and water into a tank type mixer for kneading, wherein the kneading time is 5-30min, and then granulating in a rotary granulator, and the motor frequency is 5-30 Hz. The granulation time is 2-10min, and the proportion of the target particles of 12-80 meshes is 70-85%. And drying in a vibration fluidized bed at 70-70 deg.C for 0.5-2 h. And screening the dried material by a 12-80 mesh vibrating screen, and obtaining granules obtained by screening, namely the target finished product granules.
On the other hand, the application of the bactericidal granules in preventing and treating plant diseases is provided.
Further, the plant diseases include blight, downy mildew, phytophthora, and pythium.
In another aspect, the present invention provides a method for controlling plant diseases by using the bactericidal granule, wherein the granule is sprayed or applied by broadcasting.
Advantageous effects
(1) The invention utilizes silicon dioxide to adsorb metalaxyl-M, thereby preparing granules with good storage stability, the two components have complementary toxic effects, the drug effect can be improved, and the lasting period can be prolonged; no dust flying during application and no environmental pollution; convenient to use, it is efficient.
(2) The granules provided by the invention are effective for economic crops mainly comprising at least one of cucumbers, tomatoes, hot peppers and lettuce, and have high efficiency for crop diseases such as vegetables, fruit trees, tobaccos, oil plants, cottons, potatoes and grains, and the main diseases and insect pests are blight, downy mildew, phytophthora, pythium, botrytis cinerea, rhizopus and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. 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. Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, elements, methods, means, and the like that are well known to those skilled in the art are not described in detail in order to not unnecessarily obscure the present invention.
Example 1
The raw materials of the 0.2 percent fludioxonil metalaxyl-M granule comprise:
fludioxonil 0.1 wt%, metalaxyl-M0.1 wt%, SA3 wt%, 16285 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, kaolin to make up 100 wt%.
Example 2
The raw materials of the 0.2 percent fludioxonil metalaxyl-M granule comprise:
fludioxonil 0.1 wt%, metalaxyl-M0.1 wt%, sodium lauryl sulfate 3 wt%, dispersant NNO5 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 3
The raw material composition of the 0.3 percent fludioxonil metalaxyl-M granule is as follows:
fludioxonil 0.1 wt%, metalaxyl-M0.2 wt%, wetting agent SA3 wt%, dispersing agent 16285 wt%, defoaming agent Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 4
The raw material composition of the 0.3 percent fludioxonil metalaxyl-M granule is as follows:
fludioxonil 0.1 wt%, metalaxyl-M0.2 wt%, nekal BX 3 wt%, dispersant SD-8365 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, monopotassium phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 5
The raw materials of the 0.4 percent fludioxonil metalaxyl-M granule comprise the following components:
fludioxonil 0.1 wt%, metalaxyl-M0.3 wt%, wetting agent SA3 wt%, dispersing agent 16285 wt%, defoaming agent Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 6
The raw materials of the 0.4 percent fludioxonil metalaxyl-M granule comprise the following components:
fludioxonil 0.1 wt%, metalaxyl-M0.3 wt%, wetting agent SR-053 wt%, dispersant GY-D8005 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, monopotassium phosphate 15 wt%, silicon dioxide 1 wt%, kaolin to 100 wt%.
Example 7
The raw materials of the 0.5 percent fludioxonil metalaxyl-M granule comprise the following components:
fludioxonil 0.1 wt%, metalaxyl-M0.4 wt%, wetting agent SA3 wt%, dispersing agent 16285 wt%, defoaming agent Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 8
The raw materials of the 0.5 percent fludioxonil metalaxyl-M granule comprise the following components:
fludioxonil 0.1 wt%, metalaxyl-M0.4 wt%, wetting agent BT8F 3 wt%, sodium lignosulfonate LX 5 wt%, defoaming agent Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin 100 wt%.
Example 9
The raw materials of the 0.6 percent fludioxonil metalaxyl-M granule comprise:
fludioxonil 0.1 wt%, metalaxyl-M0.5 wt%, wetting agent SA3 wt%, dispersing agent 16285 wt%, defoaming agent Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, and kaolin to make up 100 wt%.
Example 10
The raw materials of the 0.6 percent fludioxonil metalaxyl-M granule comprise:
fludioxonil 0.1 wt%, metalaxyl-M0.5 wt%, wetting agent GY-W043 wt%, dispersant Ufoxane3A5 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, silicon dioxide 1 wt%, kaolin to make up 100 wt%.
Method embodiment
The preparation method of the granules comprises the following steps:
a. mixing metalaxyl-M and silicon dioxide, and stirring until no block exists to obtain a first material;
b. fludioxonil, a first material, a wetting agent, a dispersing agent, a defoaming agent, corn starch, glucose, monopotassium phosphate and kaolin are uniformly mixed, the rotating speed is 30r/min, and the mixture is mixed for 30min to obtain a second material;
c. crushing the second material into particles with D90 being less than or equal to 75 microns, wherein the pressure of jet milling is 0.8Mpa, and the rotating speed of a classifying wheel is 2600 r/min; obtaining a third material;
d. adding water into the third material and uniformly mixing to obtain a fourth material; the water addition amount is 15 wt% of the weight of the third material;
e. extruding and granulating the fourth material, wherein the motor frequency is 25 Hz; obtaining particles with 12-80 meshes as a fifth material;
f. drying the fifth material at 80 deg.C to obtain granule.
Comparative example 1
35g/L fludioxonil and metalaxyl-M suspending agent, wherein the weight ratio of the fludioxonil and the metalaxyl-M suspending agent is 1: 2.5.
Comparative example 2
Fludioxonil granules 0.1%
The difference from example 1 is that metalaxyl-M is not added. The preparation method refers to the method examples.
Comparative example 3
0.3% metalaxyl-M granule
The difference from example 5 is that fludioxonil was not added. The preparation method refers to the method examples.
Comparative example 4
Fludioxonil thifluzamide 0.4% granule
Fludioxonil 0.1 wt%, thifluzamide 0.3 wt%, SA3 wt%, dispersant 1628: 5 wt%, defoamer soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
Comparative example 5
0.4% fluopicolide-metalaxyl-M granule
Fluopicolide 0.1 wt%, metalaxyl-M0.3 wt%, silicon dioxide 1 wt%, SA3 wt%, dispersant 1628: 5 wt%, defoamer soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
Comparative example 6
0.4% fludioxonil mefenoxam granules (wetting agent not added)
Fludioxonil 0.1 wt%, metalaxyl-m 0.3 wt%, silica 1 wt%, dispersant 1628: 5 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
Comparative example 7
0.4% fludioxonil mefenoxam granules (no dispersant added)
Fludioxonil 0.1 wt%, metalaxyl-M0.3 wt%, silicon dioxide 1 wt%, SA3 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
Comparative example 8
0.4% fludioxonil mefenoxam granules (without corn starch and glucose)
Fludioxonil 0.1 wt%, metalaxyl-M0.3 wt%, silicon dioxide 1 wt%, SA3 wt%, dispersant 16285 wt%, defoamer Soap-L0.4 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
Comparative example 9
0.4% fludioxonil mefenoxam granules (without silica)
Fludioxonil 0.1 wt%, metalaxyl-M0.3 wt%, SA3 wt%, dispersant 16285 wt%, defoamer Soap-L0.3 wt%, corn starch 15 wt%, glucose 2 wt%, potassium dihydrogen phosphate 15 wt%, and kaolin to make up 100 wt%.
The preparation method refers to the method examples.
In the above examples and comparative examples, the raw pesticide and the auxiliary agent are commercially available products, wherein the wetting agent BT8F is purchased from seiran high-tech limited (the specific trade name of the wetting agent BT8F is called wettable powder high-efficiency wetting dispersant, and the main component is modified fatty alcohol phosphate), the wetting agent SR-05 (belonging to carboxylate wetting agent) is purchased from shanghai large polymer material limited, the wetting agent GY-W04 is purchased from beijing guangyuan agrichemical limited company (the wetting agent GY-W04 is modified anionic wetting agent), and the wetting agent SA is purchased from shengshi synbiotic technology limited in zhen city. NNO and Dispersant 1628 were purchased from taixing yun chess science and technology ltd (NNO is sodium methylenedinaphthalene sulfonate as a main component, Dispersant 1628 is Dispersant 1628 as a specific trade name, which belongs to naphthalene sulfonate), Dispersant Ufoxane3A is purchased from south beijing jiemn science and technology ltd (Dispersant Ufoxane3A belongs to high-purity modified lignin sodium salt), Dispersant SD816 is purchased from shanghai is a large polymer material ltd (Dispersant SD816 belongs to ionic polycarboxylate surfactant), Dispersant GY-D800 is purchased from beijing guangyaoyuan agronomy chemical ltd (Dispersant GY-D800 is carboxylate Dispersant, which is anionic high-molecular surfactant having a comb-type structure copolymerized from unsaturated monomer), and lignin sodium salt LX is purchased from shanghai tesk chemical ltd (lignin sodium salt LX is a specific trade name, which belongs to tensofix LX specific, which is anionic surfactant). Defoamer Soap-L was purchased from Basff (a specific trade name for defoamer Soap-L is AGNIQUE)
Figure BDA0003211631710000082
L, belonging to the Defoamer antifoam).
Test example 1
This test example was conducted to test the heat storage stability test, the low temperature stability test and the normal temperature storage stability of the granules obtained in examples 1 to 10 and the bactericides obtained in comparative examples 1 to 9, and the results are shown in Table 1.
Testing the heat storage stability: the granules obtained in examples 1 to 10 and the fungicides obtained in comparative examples 1 to 9 were sealed, placed in a constant temperature oven at (54 ± 2) ° c, left to stand for 14 days, and then taken out, and the stability was measured according to the GB/T14825-2006 standard.
And (3) low-temperature stability test: the granules obtained in examples 1 to 10 and the fungicides obtained in comparative examples 1 to 9 were sealed, placed at a constant temperature of (0. + -. 2). degree.C. for 7 days, then taken out, left to stand at room temperature for recovery, and then the stability was measured according to GB/T14825-2006.
And (3) measuring the normal-temperature storage stability: the granules obtained in examples 1 to 10 and the fungicides obtained in comparative examples 1 to 9 were sealed and then left at a constant temperature of (25. + -. 2). degree.C.for 12 months, and then their stability was measured according to GB/T14825-2006.
Table 1 stability testing of each fungicide
Figure BDA0003211631710000081
Figure BDA0003211631710000091
Figure BDA0003211631710000101
As can be seen from table 1, the granules of the present invention have good storage stability compared to the common suspension agents on the market, and the various additives added in the preparation method of the present invention greatly improve the storage stability in different aspects.
Test example 2
This test compares the granules prepared in examples 1 to 10 with the fungicides obtained in comparative examples 1 to 9, and tests the control effect. The granules obtained in examples 1 to 10 were uniformly applied at a rate of 10 kg/mu, and the fungicides in comparative examples 1 to 9 were diluted to the same ratio and sprayed or applied by applying a spreading method. And a blank control 10 was added, and the blank control was compared using an equal amount of clear water.
Test site: shandong province chat about Shenmei Zhongzhangtuncun, the test field is a planting base for many years of cucumbers, and the test field has flat vigor and moderate fertility. And (4) managing the cucumbers in each treatment area after the application according to the conventional production.
The specific steps comprise that the uniform spreading granules of the examples 1-10 are sprayed or spread by adopting a spraying mode when the spraying amount (calculated by active ingredients) is 10 kg/mu, and the uniform spreading granules of the comparative examples 1-10 are diluted to the same dilution times. Comparative example 10 is a blank control group, cucumber plants in the planting area were sprayed with equal amounts of clear water. The area of the test cell is 20 square meters, and the conditions of soil, cultivation, water and fertilizer management and the like of each test cell are consistent. The investigation statistical method of cucumber diseases is as follows:
the quick-acting effect of cucumber fusarium wilt prevention and control is investigated after 12h, 24h, 36h and 48h after application of the pesticide respectively, and the lasting period effect of cucumber fusarium wilt prevention and control is investigated after 3 days, 7 days and 15 days, wherein the specific method comprises the following steps:
sampling is carried out at random 5 points in each treatment area, 30 plants are investigated in each treatment area, the plant disease rate and the disease index of the diseases in the seedling stage of each treatment area are investigated, and the control effect is calculated according to the formula (1) and the formula (2).
The statistics of the cucumber fusarium wilt refer to the pesticide field efficacy test criteria.
Figure BDA0003211631710000111
Figure BDA0003211631710000112
The quick-acting effect of controlling cucumber fusarium wilt is shown in table 2.
The effect of the cucumber fusarium wilt prevention and treatment lasting period is shown in table 3.
TABLE 2 quick-acting effect on controlling cucumber fusarium wilt
Figure BDA0003211631710000113
Figure BDA0003211631710000121
Figure BDA0003211631710000131
TABLE 3 persistent effect of cucumber fusarium wilt prevention and treatment
Figure BDA0003211631710000132
Figure BDA0003211631710000141
As can be seen from Table 2, the fludioxonil-metalaxyl-M granules prepared by the preparation method provided by the invention under the conditions of optimized process flow and reasonable control parameters can achieve the bactericidal effect faster than that of the suspending agent in the market under the condition of adding the wetting agent, and the effect is better than that of the suspending agent when the suspending agent plays a role.
As can be seen from Table 3, the fludioxonil-metalaxyl-M granules prepared by the preparation method provided by the invention under the conditions of optimized process flow and reasonable control parameters have longer lasting period compared with the suspending agent in the market under the condition of adding the dispersing agent, and the effect is better than that of the suspending agent in the lasting period.
As can be seen from tables 2 and 3, when the wetting agent is selected as SA and the dispersing agent is selected as 1628, the weight ratio of fludioxonil to metalaxyl-m is 1: (1-5), the quick-acting property and the lasting effect are better than those of other auxiliary agents and the selection of the weight ratio range.
In conclusion, compared with other formulations of fludioxonil and metalaxyl-M, the fludioxonil and metalaxyl-M granule has the characteristics of quick response and long duration of drug effect, so that the drug taking times and the drug dosage can be reduced, the cost is saved, and the pollution to the environment can be reduced. The active ingredients and the auxiliary agents in the granules have good synergistic effect.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present 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 solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The bactericidal granule is characterized by comprising the following raw materials in percentage by mass based on the total weight of the granule:
0.1-5% of pesticide active ingredient, 1-10% of wetting agent, 2-8% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of monopotassium phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%;
wherein the pesticide active ingredients comprise the following components in a mass ratio of 1: fludioxonil and metalaxyl-M of (1-10).
2. The bactericidal granule according to claim 1, which comprises the following raw materials in percentage by mass:
0.1-2.5% of pesticide active ingredient, 2-5% of wetting agent, 3-7% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of potassium dihydrogen phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%;
optionally, 0.1-1% of pesticide active ingredient, 2-5% of wetting agent, 3-7% of dispersing agent, 0.1-0.5% of defoaming agent, 10-20% of corn starch, 1-5% of glucose, 10-20% of potassium dihydrogen phosphate and 0.5-2% of silicon dioxide, and the balance of kaolin to 100%;
optionally, 0.1-0.6% of pesticide active ingredient, 3% of wetting agent, 5% of dispersing agent, 0.3% of defoaming agent, 15% of corn starch, 2% of glucose, 15% of monopotassium phosphate and 1% of silicon dioxide, and the balance of kaolin to 100%.
3. The bactericidal granule according to claim 1 or 2, wherein the weight ratio of fludioxonil to metalaxyl-M is 1: (2-5), optionally 1: 3.
4. the bactericidal granule according to any one of claims 1 to 3, wherein the wetting agent is at least one selected from sodium dodecyl sulfate, wetting agent SA, nekal BX, wetting agent BT8F, wetting agent SR-05, wetting agent GY-W04; optionally, the wetting agent is wetting agent SA;
optionally, the dispersant is selected from at least one of NNO, dispersant 1628, dispersant Ufoxane3A, dispersant SD816, dispersant GY-D800, sodium lignosulfonate LX; optionally, the dispersant is dispersant 1628;
optionally, the antifoaming agent is antifoaming agent, Soap-L.
5. A method for preparing the bactericidal granule according to any one of claims 1 to 4, wherein the bactericidal granule is obtained by uniformly mixing the raw materials, pulverizing, granulating and drying.
6. The method according to claim 5, wherein the raw material mixing method comprises: mixing metalaxyl-M and silicon dioxide in proportion, stirring until no blocky matter exists, and then uniformly mixing fludioxonil, a wetting agent, a dispersing agent, a defoaming agent, corn starch, glucose, monopotassium phosphate, silicon dioxide and kaolin in proportion to obtain a mixed material;
optionally, the crushing method comprises: and crushing the mixed material into primary particle materials with D90 being less than or equal to 75 mu m.
7. The method according to claim 6, wherein the granulation method comprises: adding water into the primary particle material, uniformly mixing, and then performing granulation treatment; optionally, water is added in an amount of 5-30% by weight of the primary particulate material; optionally, the average particle size of the material obtained by the granulation treatment is 12-80 meshes;
optionally, the drying conditions are: 70-90 ℃ for 0.5-2 h.
8. Use of the fungicidal granules according to any one of claims 1 to 7 for controlling plant diseases.
9. The use according to claim 8, wherein the plant diseases include blight, downy mildew, phytophthora, pythium.
10. A method for controlling plant diseases by the fungicidal granules according to any one of claims 1 to 7, wherein the granules are sprayed or applied by broadcasting.
CN202110932499.XA 2021-08-13 2021-08-13 Bactericidal granules and preparation method and application thereof Pending CN113598166A (en)

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Application publication date: 20211105