CN110622963A - Emulsifiable granules containing propiconazole and cyproconazole as well as preparation method and application of emulsifiable granules - Google Patents

Emulsifiable granules containing propiconazole and cyproconazole as well as preparation method and application of emulsifiable granules Download PDF

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Publication number
CN110622963A
CN110622963A CN201910939836.0A CN201910939836A CN110622963A CN 110622963 A CN110622963 A CN 110622963A CN 201910939836 A CN201910939836 A CN 201910939836A CN 110622963 A CN110622963 A CN 110622963A
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CN
China
Prior art keywords
cyproconazole
emulsifiable granules
propiconazole
emulsifiable
granules containing
Prior art date
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Pending
Application number
CN201910939836.0A
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Chinese (zh)
Inventor
沈建良
凌江涛
钱兰娟
钱海宾
李宝
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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 CN201910939836.0A priority Critical patent/CN110622963A/en
Publication of CN110622963A publication Critical patent/CN110622963A/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

Abstract

The invention relates to an emulsifiable granule containing propiconazole and cyproconazole, which comprises the following components in percentage by mass: 5-30% of propiconazole; 5-30% of cyproconazole; 10-30% of an emulsifier; 1-15% of a dispersant; 1-80% of filler. According to the invention, propiconazole and cyproconazole are prepared into emulsifiable granules, and compared with other formulations such as wettable powder, missible oil, water dispersible granules and suspending agents, 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 granules containing propiconazole and cyproconazole as well as preparation method and application of emulsifiable granules
Technical Field
The invention particularly relates to emulsifiable granules containing propiconazole and cyproconazole and a preparation method and application thereof.
Background
Propiconazole is a systemic triazole fungicide with protection and treatment effects, can be absorbed by roots, stems and leaves, can be quickly conducted upwards in plant bodies to prevent and treat diseases caused by ascomycetes, basidiomycetes and imperfect fungi, and particularly has good prevention and treatment effects on wheat take-all, powdery mildew, rust disease, root rot, rice bakanae disease and sigatoka, and vegetables planted in greenhouses in summer have good vigorous seedling control and seedling pressing effects while the diseases are prevented and treated.
Cyproconazole, which belongs to triazole bactericides. Is a sterol demethylation inhibitor, and has prophylactic and therapeutic effects. It is effective on powdery mildew, rust fungi, spore, coracocephalosporium, septoria, and Venturia fungi of cereal crops, coffee, beet, fruit trees, and grape. When the composition is mixed with other bactericides, the composition can well prevent and treat the eyespot disease, the leaf spot disease and the net spot disease of cereals. The lasting period for preventing and treating the rust disease of wheat and barley is 4-6 weeks, and the lasting period for preventing and treating the powdery mildew is 3-4 weeks. Powdery mildew of cereals, fruit trees and grapes, leaf spot of peanuts and beets, apple scab and white rot of peanuts.
Disclosure of Invention
The invention aims to provide emulsifiable granules containing propiconazole and cyproconazole, which have good drug effect and are safe and environment-friendly for 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 propiconazole and cyproconazole, and the raw material formula 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 propiconazole and cyproconazole, which comprises the following steps:
(1) mixing cyproconazole, propiconazole and an emulsifier according to the formula amount, selectively adding a solvent according to the formula amount, and mixing until the mixture is 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 obtain the emulsifiable granules.
In a third aspect of the invention, the invention provides an application of the emulsifiable granules containing propiconazole and cyproconazole in controlling wheat take-all, powdery mildew, rust disease, root rot, rice bakanae disease, sigatoka, aleuroidea, aleurospora, corallina, septoria and cladosporium on cereal crops, coffee, sugar beet, fruit trees and grapes and controlling flourish seedlings of vegetables planted in summer in greenhouses.
Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the invention, propiconazole and cyproconazole are prepared into emulsifiable granules, and compared with other formulations such as wettable powder, missible oil, water dispersible granules and suspending agents, 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 propiconazole and cyproconazole emulsifiable granules have good effects on preventing and treating wheat take-all, powdery mildew, rust disease, root rot, rice bakanae disease and sigatoka, and vegetables planted in a greenhouse in summer have good vigorous seedling-pressing control effects while preventing and treating diseases. Can also be used for preventing and treating powdery mildew, rust fungi, spore, coracocephalosporium, septoria and Venturia fungi on cereal crops, coffee, beet, fruit trees and grapes.
Example 1:
an emulsifiable granule containing propiconazole and cyproconazole, which comprises the following raw materials in percentage by weight: 8% of cyproconazole, 20% of propiconazole, 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.), 15% of solvent oil, 10% of 2-naphthalene sulfonic acid formaldehyde polymer sodium salt (Shanghai Tetan 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 cyproconazole, propiconazole, an emulsifier and a solvent according to the formula ratio 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 20% propiconazole and 8% cyproconazole emulsifiable granules.
Comparative example 1:
a suspending agent containing cyproconazole comprises the following raw materials in percentage by weight: 40% of cyproconazole, 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 and 0.4% of preservative, and the balance is made 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 the materials are ground in a continuous sand mill, and the qualified product of 40 percent of cyproconazole suspending agent is obtained when the grain diameter of more than 95 percent of the materials is less than 4 mu m.
Comparative example 2:
the cyproconazole-containing missible oil comprises the following raw materials in percentage by weight: 25% of cyproconazole, 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; adding an emulsifier into the filtered solution, and uniformly stirring to obtain a qualified product of 25% cyproconazole emulsifiable solution.
Comparative example 3:
the propiconazole-containing missible oil comprises the following raw materials in percentage by weight: 25% of propiconazole, 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% propiconazole emulsifiable solution product.
Comparative example 4:
the suspending agent containing propiconazole comprises the following raw materials in percentage by weight: 25% of propiconazole, 1% of polycarboxylate (MSD-516 from Meilong Jingmao Co., Ltd., Liaoning), 3% of calcium dodecylbenzenesulfonate (500 # from Nanjing Taihua chemical Co., Ltd.), 6% of styrylphenol polyoxyethylene ether (602 # from Nanjing Taihua chemical Co., Ltd.), 15% of solvent oil 150# of xanthan gum, 1% of white carbon black, 6% of ethylene glycol, 0.3% of defoaming agent and 0.4% of preservative, wherein the water is added to make up to 100%.
The preparation method of the suspoemulsion comprises the following steps: firstly, mixing and dissolving a propiconazole technical material, an emulsifier 500#, a emulsifier 602# and solvent oil 150#, then premixing other materials with water according to a formula, and then carrying out primary mixing by adopting a high-speed shearing machine; then grinding the mixture in a continuous sand mill to ensure that the grain diameter of more than 95 percent of the material is less than 4 mu m, then slowly dripping the propiconazole solution into the sanded material, and shearing for half an hour to obtain a qualified product of 25 percent propiconazole suspoemulsion.
Comparative example 5:
the missible oil containing the propiconazole and the cyproconazole comprises the following raw materials in percentage by weight: propiconazole 20%, cyproconazole 8%, calcium dodecylbenzene sulfonate (500 #) 5%, styryl phenol polyoxyethylene ether 10% (602 #) and solvent oil 150# 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; adding an emulsifier into the filtered solution, and uniformly stirring to obtain a qualified product of 20% propiconazole and 8% cyproconazole emulsifiable solution.
Application example 1: field efficacy test of propiconazole and cyproconazole emulsifiable granules for preventing and treating wheat leaf rust
The experiment is arranged in Wuxi city and Hui mountain areas of Jiangsu province, and reagents are provided by Jiangsu Qizhou green chemical industry Co. The conditions of wheat leaf rust are investigated before the medicine is taken, and 250g/hm are respectively used2The first administration at the beginning of the disease, once every 10 days, for 2 administrations were carried out by diluting 4000 times the three control agents of example 1, comparative examples 1 and 2, and the like. And (5) respectively investigating the disease index of the wheat leaf rust 5 days, 14 days and 30 days after the second application and calculating the control effect. The results of the experiment are shown in table 1.
TABLE 1
As can be seen from the table 1, the emulsifiable granules prepared from propiconazole and cyproconazole can effectively prevent and treat the wheat leaf rust, the prevention and treatment effects are better than those of comparative examples 1-4, the prevention and treatment effects are basically the same as those of comparative example 5, but the use aspect of a solvent is obviously smaller than that of comparative example 5, and the examples are more environment-friendly than comparative example 5. Has no adverse effect on target crops in the using range.
The invention can generate higher synergistic effect by adopting the formula. Compared with other monomer formulations of propiconazole or cyproconazole for preventing and treating crop diseases, the compound preparation enlarges the disease prevention and treatment range and delays the generation of drug 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 propiconazole and cyproconazole, characterized in that: the raw material formula comprises the following components in percentage by mass:
2. emulsifiable granules containing propiconazole and cyproconazole according to claim 1, characterized in that: the raw material formula comprises the following components in percentage by mass:
3. emulsifiable granules containing propiconazole and cyproconazole 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 propiconazole and cyproconazole 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 propiconazole and cyproconazole 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 propiconazole and cyproconazole 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 propiconazole and cyproconazole 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 propiconazole and cyproconazole 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 process for the preparation of emulsifiable granules containing propiconazole and cyproconazole according to any one of claims 1 to 8, wherein: the method comprises the following steps:
(1) mixing cyproconazole, propiconazole and an emulsifier according to the formula amount, selectively adding a solvent according to the formula amount, and mixing until the mixture is 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 obtain the emulsifiable granules.
10. Use of the emulsifiable granules containing propiconazole and cyproconazole according to any one of claims 1 to 8 for controlling take-all, powdery mildew, rust, root rot of wheat, rice cachexia, sigatoka, erysipales, aleuroidea, botrytis, coffea, sugar beet, aleuroidea, septoria, cladosporium on fruit trees and grapes, and for controlling flourish seedlings of vegetables planted in the summer of greenhouses.
CN201910939836.0A 2019-09-30 2019-09-30 Emulsifiable granules containing propiconazole and cyproconazole as well as preparation method and application of emulsifiable granules Pending CN110622963A (en)

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Cited By (2)

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CN111642509A (en) * 2020-06-29 2020-09-11 江苏七洲绿色化工股份有限公司 Pesticide composition and preparation method and application thereof
CN114747571A (en) * 2022-03-30 2022-07-15 京博农化科技有限公司 Ceibotriene glycol emulsifiable powder and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111642509A (en) * 2020-06-29 2020-09-11 江苏七洲绿色化工股份有限公司 Pesticide composition and preparation method and application thereof
CN114747571A (en) * 2022-03-30 2022-07-15 京博农化科技有限公司 Ceibotriene glycol emulsifiable powder and preparation method and application thereof

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