CN110583640A - Emulsifiable granule containing pyraclostrobin and difenoconazole and preparation method and application thereof - Google Patents

Emulsifiable granule containing pyraclostrobin and difenoconazole and preparation method and application thereof Download PDF

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Publication number
CN110583640A
CN110583640A CN201910939467.5A CN201910939467A CN110583640A CN 110583640 A CN110583640 A CN 110583640A CN 201910939467 A CN201910939467 A CN 201910939467A CN 110583640 A CN110583640 A CN 110583640A
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CN
China
Prior art keywords
difenoconazole
pyraclostrobin
emulsifiable granules
emulsifiable
containing pyraclostrobin
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Pending
Application number
CN201910939467.5A
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Chinese (zh)
Inventor
沈建良
凌江涛
钱海宾
钱兰娟
张晓腾
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Jiangsu Sevencontinent Green Chemical Co Ltd
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Jiangsu Sevencontinent Green Chemical Co Ltd
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Priority to CN201910939467.5A priority Critical patent/CN110583640A/en
Publication of CN110583640A publication Critical patent/CN110583640A/en
Pending legal-status Critical Current

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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
    • 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
    • A01N43/64Biocides, 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
    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof

Abstract

The invention relates to emulsifiable granules containing pyraclostrobin and difenoconazole, which comprises the following components in percentage by mass: 5-30% of pyraclostrobin; 5-30% of difenoconazole; 0-30% of an emulsifier; 1-15% of a dispersant; 1-80% of filler. Compared with other formulations such as wettable powder, missible oil, water dispersible granules, suspending agents and the like, the emulsifiable granules are safer for users than wettable powder in the aspect of no dust; the solvent is less in amount, so that the emulsion is more environment-friendly than missible oil; is more convenient to transport than a suspending agent; the particle size is smaller than that of the water dispersible granules, so that the drug effect of the emulsifiable granules is better. The preparation formulation of the invention is emulsifiable granules, is an environment-friendly preparation formulation and accords with the development direction of national industrial policies.

Description

Emulsifiable granule containing pyraclostrobin and difenoconazole and preparation method and application thereof
Technical Field
The invention particularly relates to emulsifiable granules containing pyraclostrobin and difenoconazole and a preparation method and application thereof.
Background
Pyraclostrobin has a very wide sterilization range, has a very obvious sterilization effect due to a unique action mechanism, is relatively high in environmental protection, is used according to a scientific and reasonable method when being used, is a mitochondrial respiration inhibitor, namely has the functions of protection, treatment and leaf permeation and conduction by preventing electron transfer in cytochrome synthesis.
The difenoconazole belongs to triazole bactericides, is a systemic bactericide, has a wide bactericidal spectrum, and has lasting protection and treatment effects on ascomycetes, basidiomycetes and some species-borne diseases including alternaria, ascomycetes and some species-borne diseases. Is safe to crops, is used for seed coating, has no adverse effect on seedlings, and is different from triazolone and other medicaments, and the emergence of seedlings is fast and uniform. Seed treatment and foliar spray can both improve crop yield and ensure quality.
Disclosure of Invention
The invention aims to provide emulsifiable granules containing pyraclostrobin and difenoconazole, which have good drug effect and are safe and environment-friendly to users, and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
one aspect of the invention provides emulsifiable granules containing pyraclostrobin and difenoconazole, which comprises the following components in percentage by mass:
preferably, the raw material formula comprises the following components in percentage by mass:
preferably, the emulsifier is calcium dodecyl benzene sulfonate and styryl phenol polyoxyethylene ether in a weight ratio of 1: 1-5.
Further preferably, the emulsifier is calcium dodecylbenzene sulfonate and styrylphenol polyoxyethylene ether in a weight ratio of 1: 1-3.
Preferably, the dispersant is 2-naphthalene sulfonic acid formaldehyde polymer sodium salt.
Preferably, the filler is one or more of inorganic salt, diatomite, bentonite, white carbon black and silica gel.
Preferably, the raw materials of the emulsifiable granules further comprise 5-25% of a solvent, and the solvent is solvent oil.
More preferably, the content of the solvent is 10-20%.
According to a specific and preferred embodiment, the raw material formula comprises the following components in percentage by mass:
preferably, the raw materials of the emulsifiable granules further comprise 1-5% of a binder.
The second aspect of the invention provides a preparation method of the emulsifiable granules containing pyraclostrobin and difenoconazole, which comprises the following steps:
(1) mixing difenoconazole, pyraclostrobin and an emulsifier according to the formula amount, selectively adding a solvent according to the formula amount, and mixing to a homogeneous phase;
(2) uniformly mixing the filler and the dispersant according to the formula amount, and then carrying out jet milling;
(3) spraying the raw materials treated in the step (1) into the raw materials treated in the step (2), and uniformly mixing by shearing and stirring;
(4) and (4) extruding and granulating the uniformly mixed materials in the step (3) to obtain the emulsifiable granules.
The third aspect of the invention provides application of the emulsifiable granules containing pyraclostrobin and difenoconazole in preventing and treating powdery mildew, downy mildew, scab, leaf spot, sclerotinia, anthracnose, white rot, alternaria leaf spot, brown spot, rust disease, stripe rust disease and gibberellic disease of crops such as wheat, rice, cucumber, banana and the like.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
compared with other formulations such as wettable powder, missible oil, water dispersible granules, suspending agents and the like, the emulsifiable granules are safer for users than wettable powder in the aspect of no dust; the solvent is less in amount, so that the emulsion is more environment-friendly than missible oil; is more convenient to transport than a suspending agent; the particle size is smaller than that of the water dispersible granules, so that the drug effect of the emulsifiable granules is better. The preparation formulation of the invention is emulsifiable granules, is an environment-friendly preparation formulation and accords with the development direction of national industrial policies.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that these embodiments are provided to illustrate the basic principles, essential features and advantages of the present invention, and the present invention is not limited by the following embodiments. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments. The contents are all mass contents.
The effective components of the pesticide are prepared into different pesticide preparations, which are researched and developed aiming at different control effects and control objects thereof. The different pesticide preparations mainly embody: the processing mode, environmental protection, safety and drug effect, and the advantages of the pesticide preparation can be known only through a large number of tests.
Through a large number of screening tests, the inventor finds that the pyraclostrobin and difenoconazole emulsifiable granules are applied to control of powdery mildew, downy mildew, scab, leaf spot, sclerotinia, anthracnose, white rot, alternaria leaf spot, brown spot, rust disease, stripe rust and gibberellic disease of crops such as wheat, rice, cucumber, banana and the like. .
Example 1:
an emulsifiable granule containing pyraclostrobin and difenoconazole comprises the following raw materials in percentage by weight: 15% of difenoconazole, 15% of pyraclostrobin, 5% of calcium dodecyl benzene sulfonate (500 # of Nanjing Taihua chemical Co., Ltd.), 10% of styrylphenol polyoxyethylene ether (602 # of Nanjing Taihua chemical Co., Ltd.), 15% of solvent oil, 10% of 2-naphthalene sulfonic acid formaldehyde polymer sodium salt (Shanghai Temple auxiliary Co., Ltd.), 20% of white carbon black and the balance of diatomite to 100%.
The preparation method of the emulsifiable granules comprises the following steps:
(1) mixing and dissolving the difenoconazole, the pyraclostrobin, the emulsifier and the solvent according to the formula amount to be homogeneous;
(2) uniformly mixing the filler and the dispersant according to the formula amount, and then carrying out jet milling;
(3) spraying the raw materials treated in the step (1) into the raw materials treated in the step (2), and uniformly mixing by shearing and stirring;
(4) and (4) extruding and granulating the uniformly mixed materials in the step (3) to prepare the 15% pyraclostrobin + 15% difenoconazole emulsifiable granules.
Comparative example 1:
the suspending agent containing difenoconazole comprises the following raw materials in percentage by weight: 40% of difenoconazole, 1% of polycarboxylate (MSD-516 from Liaoning Meilong Jingmao Co., Ltd.), 6% of phosphate (TXP-10 from Jiangsu province Haian petrochemical plant TXP), 0.2% of xanthan gum, 1% of white carbon black, 6% of ethylene glycol, 0.3% of defoaming agent, 0.4% of preservative and water, and the balance is up to 100%.
The preparation method of the suspending agent comprises the following steps: premixing the materials with water according to a formula, and then carrying out primary mixing by adopting a high-speed shearing machine; then grinding the materials in a continuous sand mill to ensure that the grain diameter of more than 95 percent of the materials is less than 4 mu m to obtain a qualified product of the 40 percent difenoconazole suspending agent.
Comparative example 2:
the suspending agent containing pyraclostrobin comprises the following raw materials in percentage by weight: 25% of pyraclostrobin, 1% of polycarboxylate (MSD-516 from Liaoning Meilong Jingmao Co., Ltd.), 6% of phosphate (TXP-10 from Haian petrochemical plant of Jiangsu province), 0.2% of xanthan gum, 1% of white carbon black, 6% of ethylene glycol, 0.3% of defoaming agent, 0.4% of preservative and water, and the balance is up to 100%.
The preparation method of the suspending agent comprises the following steps: premixing the materials with water according to a formula, and then carrying out primary mixing by adopting a high-speed shearing machine; and then grinding the materials in a continuous sand mill to ensure that the particle size of more than 95 percent of the materials is less than 4 mu m to obtain a qualified product of the 25 percent pyraclostrobin suspending agent.
Comparative example 3:
missible oil containing difenoconazole comprises the following raw materials in percentage by weight: 25% of difenoconazole, 5% of calcium dodecyl benzene sulfonate (500 # of Nanjing Taihua chemical Co., Ltd.), 10% of styryl phenol polyoxyethylene ether (602 # of Nanjing Taihua chemical Co., Ltd.), and 150# of solvent oil to make up to 100%.
The preparation method of the missible oil comprises the following steps: mixing and dissolving the original medicine and the solvent according to the formula; filtering the dissolved solution; and adding an emulsifier into the filtered solution, and uniformly stirring to obtain a qualified 25% difenoconazole emulsifiable concentrate product.
Comparative example 4:
the pyraclostrobin-containing missible oil comprises the following raw materials in percentage by weight: 25% of pyraclostrobin, 5% of calcium dodecyl benzene sulfonate (500 # of Nanjing Taihua chemical Co., Ltd.), 10% of styrylphenol polyoxyethylene ether (602 # of Nanjing Taihua chemical Co., Ltd.), and the balance of solvent oil 150# to 100%.
The preparation method of the missible oil comprises the following steps: mixing and dissolving the original medicine and the solvent according to the formula; filtering the dissolved solution; and adding an emulsifier into the filtered solution, and uniformly stirring to obtain a 25% pyraclostrobin missible oil qualified product.
Comparative example 5:
a wettable powder containing pyraclostrobin and difenoconazole comprises the following raw materials in percentage by weight: 20% of difenoconazole, 20% of pyraclostrobin, 5% of polycarboxylate (SD-816, Shanghai, Dagholen Co., Ltd.), sulfonate (SD-661, Shanghai, Dagholen Co., Ltd.), 10% of 2-naphthalene sulfonic acid formaldehyde polymer sodium salt (Skantan auxiliary Co., Ltd., Shanghai), 20% of white carbon black and clay, wherein the balance is up to 100%.
The preparation method of the wettable powder comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the formula, then carrying out air flow crushing, crushing until 98 percent of the mixture passes through a 325-mesh wet sieve, and obtaining the qualified 20 percent difenoconazole and 20 percent pyraclostrobin wettable powder
Example 2: field pesticide effect test of pyraclostrobin and difenoconazole emulsifiable granules for preventing and treating watermelon anthracnose
The test was carried out in the Dongtai protected area of Jiangsu province (the watermelon variety is Dongtai watermelon). The reagent is provided by the green chemical industry of Qizhou Jiangsu. Investigating the state of watermelon anthracnose before administration, 250g/hm2The example 1 and comparative example agents were diluted 4000 times and administered for the first time in the early stage of the disease, once every 10 days, for 2 times. And (5) 5 days, 14 days and 30 days after the second pesticide application, respectively investigating the disease index of the watermelon anthracnose and calculating the control effect. The results of the experiment are shown in table 1:
TABLE 1 field test of efficacy of the bactericidal composition of the present invention in controlling watermelon anthracnose
As can be seen from the table 1, the emulsified granules prepared from the pyraclostrobin and the difenoconazole can effectively prevent and treat the watermelon anthracnose, the prevention and treatment effects are all superior to those of comparative examples 1-5, and no adverse effect is caused to target crops in the use range.
The invention can generate higher synergistic effect by adopting the formula. Compared with single dose or compound dose of pyraclostrobin and difenoconazole for preventing and treating crop diseases, the pesticide composition enlarges the disease prevention and treatment range and delays the generation of pesticide resistance. Obviously improves the pesticide effect, reduces the pesticide dosage and the pesticide application frequency used per mu, lightens the burden of farmers, promotes the yield and income increase of the farmers, better ensures the safe production of agriculture and protects the ecological environment. The method is applied to the field of agricultural plant chemical protection, and has excellent and efficient protection and treatment effects on the harm of germs such as fruit trees, vegetables, wheat, rice and the like.
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and implement the invention, and not to limit the scope of the invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.

Claims (10)

1. An emulsifiable granule containing pyraclostrobin and difenoconazole, which is characterized in that: the raw material formula comprises the following components in percentage by mass:
2. emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1, characterized in that: the raw material formula comprises the following components in percentage by mass:
3. emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1 or 2, characterized in that: the emulsifier is calcium dodecyl benzene sulfonate and styryl phenol polyoxyethylene ether in a weight ratio of 1: 1-5.
4. Emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 3, characterized in that: the emulsifier is calcium dodecyl benzene sulfonate and styryl phenol polyoxyethylene ether in a weight ratio of 1: 1-3.
5. Emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1 or 2, characterized in that: the dispersing agent is 2-naphthalene sulfonic acid formaldehyde polymer sodium salt.
6. Emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1 or 2, characterized in that: the filler is one or more of inorganic salt, diatomite, bentonite, white carbon black and silica gel.
7. Emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1 or 2, characterized in that: the raw materials of the emulsifiable granules also comprise 5-25% of solvent, and the solvent is solvent oil.
8. Emulsifiable granules containing pyraclostrobin and difenoconazole according to claim 1 or 2, characterized in that: the raw materials of the emulsifiable granules also comprise 1-5% of a binder.
9. A method of preparing emulsifiable granules containing pyraclostrobin and difenoconazole according to any one of claims 1 to 8, characterized in that: the method comprises the following steps:
(1) mixing difenoconazole, pyraclostrobin and an emulsifier according to the formula amount, selectively adding a solvent according to the formula amount, and mixing to a homogeneous phase;
(2) uniformly mixing the filler and the dispersant according to the formula amount, and then carrying out jet milling;
(3) spraying the raw materials treated in the step (1) into the raw materials treated in the step (2), and uniformly mixing by shearing and stirring;
(4) and (4) extruding and granulating the uniformly mixed materials in the step (3) to obtain the emulsifiable granules.
10. Use of an emulsifiable granule formulation containing pyraclostrobin and difenoconazole according to any one of claims 1 to 8 for the control of powdery mildew, downy mildew, scab, leaf spot, sclerotinia, anthracnose, white rot, alternaria leaf spot, brown spot, rust, stripe rust, gibberellic disease.
CN201910939467.5A 2019-09-30 2019-09-30 Emulsifiable granule containing pyraclostrobin and difenoconazole and preparation method and application thereof Pending CN110583640A (en)

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Application publication date: 20191220

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