CN115500353B - Fluazinam and benziothiazolinone granules and preparation method thereof - Google Patents

Fluazinam and benziothiazolinone granules and preparation method thereof Download PDF

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CN115500353B
CN115500353B CN202211355929.7A CN202211355929A CN115500353B CN 115500353 B CN115500353 B CN 115500353B CN 202211355929 A CN202211355929 A CN 202211355929A CN 115500353 B CN115500353 B CN 115500353B
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coating agent
fluazinam
benziothiazolinone
film coating
water
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CN115500353A (en
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张磊
刘润峰
曾学彬
叶小妹
尹玉娟
李桂兰
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Yunfa Biotechnology Shanghai Co ltd
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Yunfa Biotechnology Shanghai Co ltd
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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
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • 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
    • A01N25/26Biocides, 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 in coated particulate form
    • 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
    • A01N43/80Biocides, 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 five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00Disinfectants; Antimicrobial compounds or mixtures thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P3/00Fungicides
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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

Abstract

The invention discloses fluazinam and benziothiazolinone granules and a preparation method thereof. The granule comprises fluazinam, benziothiazolinone, a polymer film coating agent and auxiliary materials. The preparation method of the invention comprises the following steps: (1) Mixing fluazinam, benziothiazolinone and auxiliary materials, and performing jet milling to form granule mother powder; (2) Uniformly mixing a water-soluble film coating agent and a non-water-soluble film coating agent to form a film coating agent mixed solution; (3) And adding the prepared film coating agent mixed solution into the granule master powder for adsorption and kneading, granulating, drying and screening to obtain fluazinam and benziothiazolinone granules. The invention has the advantages of easily obtained granule materials and simple process, and particularly creatively uses the polymer film coating agent to replace water for kneading and granulating, so that the prepared product has obvious controlled release effect on the basis of not improving the complexity of the granulating process, achieves the purpose of long-acting disease control, and particularly effectively relieves the problem that the benziothiazolinone and fluazinam are easy to degrade and lose efficacy in soil on the basis of not influencing the control effect, has fewer times and less dosage, improves the pesticide utilization rate, simultaneously is safe to crops, saves the cost and reduces the pollution to the environment.

Description

Fluazinam and benziothiazolinone granules and preparation method thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to fluazinam and benziothiazolinone granules and a preparation method thereof.
Background
In the 21 st century, the planting area of Chinese potatoes is the second place in the world, but the potatoes in China are affected by diseases such as late blight, black shank, scab and the like all the year round, and the prevention and treatment of the diseases such as the late blight, the black shank, the scab and the like of the potatoes by fluazinam and benziothiazolinone are conventional choices, and the effect is excellent.
Fluazinam (fluazinam) is an organic compound belonging to the class of pyridine amine derivatives, dinitroaniline bactericides. Has no therapeutic effect and systemic activity, and is a broad-spectrum efficient protective bactericide. Is very effective against alternaria, phytophthora, uniaxial mould, sclerotinia and black fungus. Fluazinam acts on a plurality of specific sites of ATP synthase to release the association of oxidation and phosphorylation at the tail end of respiratory chain, so as to consume the electrochemical potential energy accumulated by electron transfer to the maximum extent and block the formation of germ energy (ATP), thereby leading germ to die. The fluazinam is stable under acidic conditions, is easy to hydrolyze under neutral and alkaline conditions, and is more favorable for degrading the fluazinam in soil under alkaline and higher organic matter content.
Benziothiazolinone is a novel broad-spectrum bactericide and is mainly used for preventing and treating various bacterial and fungal diseases of cruciferous crops, vegetables, fruits and the like. The sterilization mechanism mainly comprises two aspects of destroying the nuclear structure of germ cells, leading the germ cells to lose heart parts and failure death and interfering metabolism of germ cells, leading the germ cells to be physiological disorder and finally leading the germ cells to death. The plant can be effectively protected from being infected by the pathogen when the plant is used in the early stage of disease occurrence, and the spreading of germs can be obviously controlled by increasing the dosage after the disease occurrence, so that the double functions of protection and eradication are achieved. The solubility in water (20 ℃) was 4g/L.
The main potato producing areas in China are in Gansu, inner Mongolia and northeast three provinces, most of the places are northern, the rainfall is small, acidic substances in soil are small, the soil is alkaline, the soil is fat, the organic matter content is high, the stability of soil treatment agent pesticides for preventing and treating potato diseases such as fluazinam is influenced, the degradation in the soil is easy, the lasting time is short, and multiple application is needed.
At present, the common preparation used for preventing and treating potato related diseases is granules, because the granules are produced by mixing active ingredients with auxiliary materials, carrying out jet milling, adding a proper amount of water, carrying out kneading granulation by a granule kneader, drying and screening; in application, the granular product has the advantages of good sedimentation, small drift, light environmental pollution, convenient application, labor and time saving, and can be released as a concentrated area of the soil treatment agent, but the pesticide active ingredient fluazinam and the like are easily lost or degraded due to the rain wash leaching effect and/or the soil pH influence and the microorganism effect, the duration is shorter, and further the application times and the application amount are required to be increased, so that the application cost is increased and the environmental pollution is caused. Therefore, there is an urgent need to develop a stable and long-acting granule preparation method with controlled release to change the condition.
Furthermore, the information disclosed in this background section is only for the purpose of increasing the understanding of the general background of the invention and should not be taken as an acknowledgment or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Disclosure of Invention
The invention aims to solve the problems that the fluazinam and the benziothiazolinone containing granules prepared in the prior art are easy to cause loss or degradation of the effective components of pesticides due to the rain wash leaching effect and/or the soil pH influence and the microbial effect, and further the application times and the application dosage are required to be increased, so that the application cost is increased and the environment is polluted.
The granule containing fluazinam and benziothiazolinone comprises fluazinam, benziothiazolinone, a polymer film coating agent and auxiliary materials, wherein the polymer film coating agent comprises 4-20% of water-soluble film coating agent and 80-96% of water-insoluble film coating agent.
The invention also provides a fluazinam and benziothiazolinone granule and a preparation method thereof, comprising the following steps of
(1) Mixing fluazinam, benziothiazolinone and auxiliary materials, and performing jet milling to form granule mother powder;
(2) Uniformly mixing a water-soluble film coating agent and a non-water-soluble film coating agent to form a film coating agent mixed solution;
(3) And adding the prepared film coating agent mixed solution into the granule master powder for adsorption and kneading, granulating, drying and screening to obtain fluazinam and benziothiazolinone granules.
The invention also discloses application of the fluazinam and benziothiazolinone-containing granules in preventing and treating potato late blight, black shank and scab.
The beneficial effects of the invention are that
The high molecular water-soluble and water-insoluble film coating agent is adsorbed on the surface of the master powder of the fluazinam and benziothiazolinone-containing granules to form a layer-by-layer film coating. Wherein, a small amount of water-soluble film coating agent in the coating film can be dissolved in the water in the soil, and the agent is released to achieve the prevention effect; wherein, a large amount of water-insoluble film coating agents in the coating film can prevent most surfaces of the granules from contacting with water in soil to form a water-impermeable film, and prevent a large amount of agents from being released into the soil rapidly. Therefore, the granule provided by the invention can obviously control the release effect after being applied to soil, prolong the duration of the medicament, reduce the application times and frequency, and simultaneously can well control the occurrence of diseases in the whole growth period of potatoes.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated component or section without excluding other components or sections. In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention.
The invention provides a fluazinam and benziothiazolinone-containing granule, which comprises fluazinam, benziothiazolinone, a high polymer film coating agent and auxiliary materials, wherein the high polymer film coating agent comprises 4-20% of a water-soluble film coating agent and 80-96% of a water-insoluble film coating agent. The granule with excellent performance can be obtained by selecting proper dosage of the water-soluble film coating agent and the water-insoluble film coating agent. The water-soluble film coating agent can achieve the effect of releasing pesticides, and the water-insoluble film coating agent can prevent the influence of soil environment on the pesticides, so that the release time and degradation speed of the pesticides can be prolonged.
In some embodiments, the fluazinam and the benziothiazolinone granules have a weight percentage of 5-40% and the benziothiazolinone has a weight percentage of 1-10%; preferably, the fluazinam is 15-37.5% by weight and the benziothiazolinone is 2-5% by weight.
Further, in some embodiments, the weight ratio of the fluazinam to the benziothiazolinone and the fluazinam in the granule is 1: (1-10); preferably, the weight ratio of the benziothiazolinone to the fluazinam is 1: (5-10). The combination of the two pesticide components in the above ratio range has better synergistic effect.
In some embodiments, the weight percentage of the polymer film coating agent contained in the fluazinam and benziothiazolinone granules is 10-20%; preferably, the weight percentage of the polymer film coating agent is 12-16%. The polymer film coating agent comprises 4-20% of water-soluble film coating agent and 80-96% of water-insoluble film coating agent, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1: (4-24); optionally, the polymer film coating agent comprises 8-12% of water-soluble film coating agent and 88-92% of water-insoluble film coating agent, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1: (7.3-11.5). The water-soluble film coating agent is selected from one or two of polyethylene glycol, gelatin, gum arabic, sodium carboxymethyl cellulose and polyvinylpyrrolidone; the water-insoluble film coating agent is one or two of cellulose acetate phthalate emulsion, polyvinyl acetate emulsion, vinyl acetate-ethylene copolymer emulsion and acrylic acid copolymer emulsion. The applicant has found that, in particular, the use of a combination of a water-soluble film-forming agent and a water-insoluble film-forming agent, both of which are preferably used, provides more excellent effects such as sustained release performance, release duration, etc. of the granules produced in a certain ratio range.
Furthermore, the fluazinam and benziothiazolinone granules contain auxiliary materials, wherein the auxiliary materials comprise humic acid fertilizer, dispersing agent, wetting agent, solid carrier and warning color. Wherein the auxiliary material contains humic acid fertilizer, wherein the humic acid fertilizer comprises humic acid, nitro humic acid, humic acid water-soluble salt and nitro humic acid water-soluble salt, and the water-soluble salt comprises sodium salt, potassium salt, calcium salt, zinc salt, manganese salt and ammonium salt. The humic acid fertilizer can promote the growth of plants and improve the yield of the plants.
The invention also provides a preparation method of the fluazinam and benziothiazolinone granule, which comprises the following steps:
(1) Mixing fluazinam, benziothiazolinone and auxiliary materials, and performing jet milling to form granule mother powder;
(2) Uniformly mixing a water-soluble film coating agent and a non-water-soluble film coating agent to form a film coating agent mixed solution;
(3) And adding the prepared film coating agent mixed solution into the granule master powder for adsorption and kneading, granulating, drying and screening to obtain the fluazinam and benziothiazolinone granule.
The preparation method is simple, easy for industrial production and stable in product quality.
The invention also discloses application of the fluazinam and benziothiazolinone granules in preventing and treating potato late blight, black shank and scab. The fluazinam and benziothiazolinone granule prepared by the invention has good effect in application in preventing and treating potato late blight, black shank and scab, has long lasting period, and can play a good role in preventing and treating potato in the whole growth period.
It will be appreciated by those skilled in the art that in some embodiments, materials, methods, means, etc. well known to those skilled in the art have not been described in detail in order to facilitate the salient features of the present invention. The raw materials in the following examples are all commercially available.
1. Preparation examples
Example 1
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 3g of benziothiazolinone, 22.5g of fluazinam with 10g of ammonium humate, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 1.4g of polyethylene glycol and 12.6g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 14%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:9.
example 2
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 3g of benziothiazolinone, 22.5g of fluazinam with 10g of ammonium humate, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 1.69g of polyethylene glycol and 12.31g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 14%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:7.3.
example 3
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 3g of benziothiazolinone, 22.5g of fluazinam with 10g of nitro humic acid, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 1.45g of polyethylene glycol and 10.55g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 12 percent, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:7.3.
example 4
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 2g of benziothiazolinone, 15g of fluazinam with 10g of nitro humic acid, 3g of methylene dinaphthyl sodium sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 1.12g of polyvinylpyrrolidone and 12.88g of cellulose acetate phthalate emulsion to form a coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 14%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:11.5.
example 5
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 2g of benziothiazolinone, 15g of fluazinam with 10g of sodium humate, 3g of polycarboxylate, 3g of alkyl naphthalene formaldehyde condensate sulfonate, 30g of kaolin and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 1.28g of polyvinylpyrrolidone and 14.72g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 16%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:11.5.
example 6
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 5g of benziothiazolinone, 37.5g of fluazinam with 10g of sodium humate, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of white carbon black and 0.5g of Prussian blue, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 2g of gum arabic and 8g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 10%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:4.
example 7
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 5g of benziothiazolinone, 37.5g of fluazinam with 10g of potassium humate, 3g of calcium lignosulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of metal phthalocyanine, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 4g of sodium carboxymethyl cellulose, 16g of vinyl acetate-ethylene copolymer emulsion and acrylic acid copolymer emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 20%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:4.
example 8
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 1g of benziothiazolinone, 7.5g of fluazinam with 10g of potassium humate, 3g of sodium lignin sulfonate, 3g of nekal, 30g of bentonite and 0.5g of triphenylmethane dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 0.4g of polyethylene glycol and 9.6g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 10%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:24.
example 9
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 1g of benziothiazolinone, 7.5g of fluazinam with 10g of calcium humate, 3g of sodium lignin sulfonate, 3g of nekal, 30g of talcum powder and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 0.8g of polyethylene glycol, 19.2g of vinyl acetate-ethylene copolymer emulsion and acrylic acid copolymer emulsion to form a laminating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 20%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:24.
example 10
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 1g of benziothiazolinone, 5g of fluazinam with 10g of magnesium humate, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 2g of polyethylene glycol and 8g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:5, a step of; the weight percentage of the prepared polymer film coating agent is 10%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:4.
example 11
A preparation method of fluazinam and benziothiazolinone granules, which comprises the following steps:
(1) Mixing 4g of benziothiazolinone, 40g of fluazinam with 10g of zinc humate, 3g of sodium lignin sulfonate, 3g of sodium dodecyl benzene sulfonate, 30g of kieselguhr and 0.5g of azo dye, and performing jet milling to form granule mother powder;
(2) Uniformly mixing 4g of polyethylene glycol and 16g of polyvinyl acetate emulsion to form a film coating agent mixed solution;
(3) And (3) dripping the film coating agent mixture obtained in the step (2) into the granule master batch obtained in the step (1), carrying out adsorption kneading, granulating, drying and screening to obtain fluazinam benziothiazolinone granules.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:10; the weight percentage of the prepared polymer film coating agent is 20%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:24.
comparative example 1
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
the coating agent mixture obtained in the step (2) is replaced by equal amount of water.
Comparative example 2
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
the coating agent mixed solution in the step (2) is replaced by the same amount of polyethylene glycol.
Comparative example 3
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
the coating agent mixed solution in the step (2) is replaced by an equivalent amount of polyvinyl acetate emulsion.
Comparative example 4
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
in the step (2), 3.5g of polyethylene glycol and 10.5g of polyvinyl acetate emulsion are selected and uniformly mixed to form a film coating agent mixed solution.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 14%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:3.
comparative example 5
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
in the step (2), 0.54g of polyethylene glycol and 13.46g of polyvinyl acetate emulsion are selected and uniformly mixed to form a film coating agent mixed solution.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 14%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:25.
comparative example 6
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
the diatomite in the step (1) is used for 30g;
in the step (2), 2.1g of polyethylene glycol and 18.9g of polyvinyl acetate emulsion are selected and uniformly mixed to form a film coating agent mixed solution.
The method can not prepare fluazinam and benziothiazolinone granules because the materials are in gel paste form after the film covering agent mixed solution is added, and can not be granulated, and the weight ratio of the benziothiazolinone to the benziothiazolinone in the method is 1:7.5; the weight percentage of the prepared polymer film coating agent is 21%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:9.
comparative example 7
A preparation method of fluazinam and benziothiazolinone granules, which is similar to example 1 in that:
the diatomite in the step (1) is used for 30g;
in the step (2), 0.9g of polyethylene glycol and 8.1g of polyvinyl acetate emulsion are selected and uniformly mixed to form a film coating agent mixed solution.
In the fluazinam and benziothiazolinone granules prepared by the method, the weight ratio of the benziothiazolinone to the fluazinam is 1:7.5; the weight percentage of the prepared polymer film coating agent is 9%, wherein the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1:9.
2. application examples
Test example 1
Indoor determination of release rate of fluazinam and benziothiazolinone granules in soil
Test preparation: taking soil of a northeast potato planting area in China, wherein no other pesticide components are applied to the soil for nearly 2 years, taking cultivated soil with the depth of 10cm from the surface of the soil, crushing uniformly, sieving with a 40-mesh sieve, adjusting the humidity to 75-85%, and putting the ground soil into a flowerpot (with the diameter of 20 cm) with a bottom without holes, wherein the thickness of 15cm for later use; placing the sieved soil in a high-temperature box at 600 ℃ for baking for 8 hours to enable organic substances in the soil to be fully burnt into inorganic substances, taking out, cooling, adjusting the humidity to 75-85%, and placing the soil into a flowerpot (diameter is 20 cm) with a bottom without holes, wherein the thickness is 15cm for standby;
2g of each flowerpot is placed into a treatment agent, the fluazinam and benziothiazolinone granules of examples 1, 3, 5, 7, 9 and 11 and comparative examples 1-5 and comparative example 7 are placed into a mesh cloth bag with holes of 200 meshes, the agent can be paved in the mesh cloth bag, a binding opening is placed into the flowerpot, 10cm of soil which is not subjected to high-temperature baking treatment is covered, 500mL of water is dripped in the center, and then a plastic film is covered on the flowerpot opening for moisturizing. Each dose was repeated 12 times for a total of 12 experimental groups. In addition, fluazinam and benziothiazolinone granules in the embodiment 1 and the comparative example 1 are filled into a mesh bag with pores of 200 meshes, so that the medicine can be paved in the mesh bag, a binding opening is put into the flowerpot, the flowerpot is covered with 10cm of soil subjected to high-temperature baking treatment, 500mL of water is dripped in the center, and a plastic film is covered on the flowerpot opening for moisturizing. Each dose was repeated 12 times for a total of 2 experimental groups.
And (3) result detection: and (3) randomly selecting 3 pots each time after standing for 14 days, 30 days, 45 days and 60 days at the temperature of 25 ℃, taking out a powder charge agent net cloth bag, detecting the content and the weight of fluazinam and benziothiazolinone in soil by using a high performance liquid chromatography, calculating to obtain the release speed of fluazinam and benziothiazolinone granules in the soil, taking the average value of the data obtained by 3 groups of samples, and obtaining the results shown in the table 1 below.
The statistical method comprises the following steps: release rate of granule effective component in soil = (measured weight of effective component in soil/initial theoretical weight of effective component) ×100%
TABLE 1
As can be seen from table 1, in the soil experiment after the high-temperature baking treatment, fluazinam and benziothiazolinone granules obtained by the preparation method provided by the invention in embodiment 1 are slowly released in the soil along with time, the release dosage is relatively uniform, the release time can reach 60 days, and the purpose of controlled release is achieved; the release speed of fluazinam and benziothiazolinone granules prepared in the conventional method in comparative example 1 in soil is high, and the granules can be completely released on day 14.
Meanwhile, the experiment groups of the soil used in the embodiment 1 and the comparison 1 after being baked at high temperature are found that the release content of fluazinam and benziothiazolinone is obviously higher than that of the experiment groups of the soil used in the embodiment 1 and the comparison 1 without being baked at high temperature after the same days of treatment, and as a result, in the same bottom non-porous flowerpot, organic matters in the experiment soil obviously promote the degradation of fluazinam and benziothiazolinone, and in the table 1, the degradation rate of fluazinam and benziothiazolinone can reach more than 25% after the granules prepared by directly adding water into the mother powder are applied to the soil without being baked for 60 days according to the conventional method; after the fluazinam and the benziothiazolinone granules obtained by the preparation method provided by the invention are applied for the same application time, the granules can be slowly released in soil, so that a large amount of active ingredients of the granules are prevented from contacting with organic substances in the soil, the degradation problem of the fluazinam and the benziothiazolinone is obviously relieved, the degradation rate of the fluazinam and the benziothiazolinone can be reduced to be within 15% after the fluazinam and the benziothiazolinone are applied in the soil for 60 days, and the degradation problem of the active ingredients in the granules is obviously improved.
Test example 2
Test the control effect duration of fluazinam and benziothiazolinone granules on potato late blight
The test area is a potato farm in northeast, and is affected by potato late blight in the past year and severely lost.
The efficacy of the fluazinam and benziothiazolinone granules of examples 1, 2, 4, 6, 8, 10 and comparative examples 1-5 and comparative example 7 on the prevention and treatment effect of potato late blight is tested at Tian Nafen, and the planting area of each sample is tested to be 1 mu, and the specific steps comprise: in the bud emergence and flowering stage of the potatoes, 20g of various granular agents are accurately weighed according to the area of a test plot, the granules and fine sand are uniformly stirred, the granules are spread in the periphery of 5-15cm of the root of the potatoes (the application amount of the active ingredients of the granules is that of each mu of land), and other materials in the embodiment 1 after the active ingredients of fluazinam and benziothiazolinone are removed are used for replacing the granules to serve as blank treatment.
After the application of the agents according to the above protocol, the late blight spore suspensions were inoculated at a concentration of 1×105 spores/ml for 7 days, 14 days, 30 days, 45 days and 60 days, respectively. And (3) maintaining normal water and fertilizer management after inoculation, and when the blank control is fully ill, investigating the ill condition, and calculating the disease index and the prevention and treatment effect, wherein the result is shown in the following table 2.
The calculating method of the disease index and the prevention and treatment effect comprises the following steps:
TABLE 2
As can be seen from the treatment results in Table 2, the fluazinam and benziothiazolinone granules obtained by the preparation method provided by the invention can effectively control the occurrence of potato late blight after being applied in the bud bloom stage of potatoes, and the incidence rate of medicament treatment is obviously reduced. The test result shows that the prevention and treatment effect of the granules on diseases reaches a peak 14 days after the administration. After 45 days, the control effect of fluazinam and benziothiazolinone granules obtained by the preparation method provided by the invention on potato late blight is slightly reduced, but is far higher than that of a comparative example, the control effect can be kept for 60 days at more than 82%, the control effect is obvious, and the duration is longer; particularly, in comparative example 1, the granules prepared by the conventional method have high release speed in soil, part of active ingredients are easy to degrade in soil over time, and the active ingredients in the medicament are easy to be lost in a large amount along with rain leaching, so that the environment is seriously polluted while the duration is short. The comparison result shows that the fluazinam and the benziothiazolinone granules obtained by the preparation method provided by the invention have excellent long-acting controlled release effects, especially effectively relieve the problem that the benziothiazolinone and the fluazinam are easy to degrade and lose efficacy in soil, have fewer times and less dosage, save cost and reduce environmental pollution.
In conclusion, the fluazinam and the benziothiazolinone granules obtained by the preparation method provided by the invention have excellent control effect on potato late blight, have longer lasting period without affecting the control effect, can basically meet the whole growth period of the potato after the bud bloom stage, and most importantly, effectively relieve the problem that the benziothiazolinone and the fluazinam are easy to degrade and lose efficacy in soil, save cost and reduce environmental pollution, and have wide application prospect and market popularization value.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A fluazinam and benziothiazolinone containing granule is characterized in that: the granule comprises fluazinam, benziothiazolinone, a polymer film coating agent and auxiliary materials, wherein the polymer film coating agent comprises 4-20% of water-soluble film coating agent and 80-96% of water-insoluble film coating agent; the fluazinam accounts for 5-40% by weight, and the benziothiazolinone accounts for 1-10% by weight; the weight ratio of the benziothiazolinone to the fluazinam is 1: (1-10); the weight percentage of the polymer film coating agent is 10-20%; the water-soluble film coating agent is selected from one or two of polyethylene glycol, gelatin, gum arabic, sodium carboxymethyl cellulose and polyvinylpyrrolidone; the water-insoluble film coating agent is one or two of cellulose acetate phthalate emulsion, polyvinyl acetate emulsion, vinyl acetate-ethylene copolymer emulsion and acrylic acid copolymer emulsion; the weight ratio of the water-soluble film coating agent to the water-insoluble film coating agent is 1: (4-24).
2. The granule of claim 1, wherein the weight percentage of fluazinam is 15-37.5%, the weight percentage of benziothiazolinone is 2-5%, and the weight ratio of benziothiazolinone to fluazinam is 1: (5-10).
3. The granule as claimed in claim 2, wherein the polymer coating agent is 12-16% by weight.
4. The granule as claimed in claim 3, wherein the polymer film-forming agent comprises 8-12% of water-soluble film-forming agent and 88-92% of water-insoluble film-forming agent, and the weight ratio of the water-soluble film-forming agent to the water-insoluble film-forming agent is 1: (7.3-11.5).
5. The granule as claimed in any one of claims 1 to 4, wherein: the auxiliary materials comprise humic acid fertilizer, dispersing agent, wetting agent, solid carrier and warning color.
6. The granule of claim 5, wherein the humic acid fertilizer comprises humic acid, nitro humic acid, water soluble salts of humic acid and water soluble salts of nitro humic acid, and the water soluble salts comprise sodium salt, potassium salt, calcium salt, zinc salt, manganese salt and ammonium salt.
7. A process for preparing the granules according to any of claims 1 to 6, comprising the steps of:
(1) Mixing fluazinam, benziothiazolinone and auxiliary materials, and performing jet milling to form granule mother powder;
(2) Uniformly mixing a water-soluble film coating agent and a non-water-soluble film coating agent to form a film coating agent mixed solution;
(3) And adding the prepared film coating agent mixed solution into the granule master powder for adsorption and kneading, granulating, drying and screening to obtain fluazinam and benziothiazolinone granules.
8. Use of the granule according to any one of claims 1 to 6 for controlling potato late blight, black shank, scab.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103314968A (en) * 2013-06-09 2013-09-25 江苏辉丰农化股份有限公司 Bactericidal composition with synergistic effect
CN107258776A (en) * 2017-06-29 2017-10-20 山东大农药业有限公司 A kind of sustained releasing pesticide granule and preparation method thereof
CN107361080A (en) * 2017-08-31 2017-11-21 广西沙田仙人滩农业投资有限公司 A kind of black scurf of potato bactericide containing tolelofos-methyl
CN112616842A (en) * 2021-01-11 2021-04-09 中国烟草总公司郑州烟草研究院 Bactericidal composition for preventing and treating bacterial wilt, bactericide and application

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103314968A (en) * 2013-06-09 2013-09-25 江苏辉丰农化股份有限公司 Bactericidal composition with synergistic effect
CN107258776A (en) * 2017-06-29 2017-10-20 山东大农药业有限公司 A kind of sustained releasing pesticide granule and preparation method thereof
CN107361080A (en) * 2017-08-31 2017-11-21 广西沙田仙人滩农业投资有限公司 A kind of black scurf of potato bactericide containing tolelofos-methyl
CN112616842A (en) * 2021-01-11 2021-04-09 中国烟草总公司郑州烟草研究院 Bactericidal composition for preventing and treating bacterial wilt, bactericide and application

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