WO2018205966A1

WO2018205966A1 - Pyraclostrobin aqueous dispersion solid composition and preparation method therefor

Info

Publication number: WO2018205966A1
Application number: PCT/CN2018/086270
Authority: WO
Inventors: 吴一凡
Original assignee: 江苏龙灯化学有限公司
Priority date: 2017-05-10
Filing date: 2018-05-10
Publication date: 2018-11-15
Also published as: TWI772416B; TW201900025A; CN108849952B; CN108849952A

Abstract

Provided in the present invention is a pyraclostrobin aqueous dispersion solid composition, which comprises the following components by weight percentage: pyraclostrobin 5-50%, alkyl sulfonate 0.1-15%, a porous carrier 5-80% and a functional additive 1-45%. Further provided in the present invention is a preparation method for the composition, which comprises: first mixing pyraclostrobin and alkyl naphthalene sulfonate according to a ratio; coarsely crushing the obtained mixture at 35°C or lower to obtain a homogeneous mixture; adding a porous carrier and a functional additive into the obtained homogeneous mixture; finely crushing so as to obtain the pyraclostrobin aqueous dispersion solid composition. The pyraclostrobin aqueous dispersion solid composition prepared in the present invention has good stability in storage at high and normal temperatures, does not collect, does not agglomerate, and will not clog a sprayer filter or spray head, thus making said composition easier for a user to use and increasing the efficiency thereof as a pesticide.

Description

Pyraclostrobin aqueous dispersion solid composition and preparation method thereof

This application claims priority to Chinese Patent Application No. 201710324705.2, entitled "A pyraclostrobin aqueous dispersion solid composition and its preparation method", which is filed on May 10, 2017. The entire contents are incorporated herein by reference.

Technical field

The invention relates to the field of agricultural chemistry, in particular to a water-dispersible solid composition and a preparation method thereof, in particular to a pyraclostrobin aqueous dispersion solid composition and a preparation method thereof.

Background technique

Pyraclostrobin is a methoxy acrylate fungicide developed by BASF in Germany in 1993 and is a mitochondrial respiratory inhibitor. It inhibits mitochondrial respiration by preventing electron transfer between cytochrome b and c1, preventing mitochondria from producing and providing the energy (ATP) required for normal cell metabolism, ultimately leading to cell death.

The chemical name of pyraclostrobin is: N-[2-[[1-(4-chlorophenyl)pyrazol-3-yl]oxymethyl]phenyl]-N-methoxycarbamic acid Methyl ester belongs to the broad spectrum fungicide of methoxy acrylate. Pyraclostrobin can be used in wheat, peanut, rice, vegetables, fruit trees, tobacco, tea trees, ornamental plants, lawns and other crops to control leaf blight caused by ascomycetes, basidiomycetes, deuteromycetes and oomycetes. , rust, powdery mildew, downy mildew, blight, anthracnose, scab, brown spot, blight and other diseases. At present, the market mainly uses pyraclostrobin emulsion and water emulsion products. However, these dosage forms all have a common disadvantage that the emulsifiable concentrate contains a large amount of organic solvents, which are extremely harmful to the ecological environment and aquatic organisms. As people's awareness of environmental protection gradually strengthens, such products will be phased out. Nowadays, various agrochemical companies are stepping up research and development efforts towards environmentally-friendly dosage forms of water-based and granulated products, and gradually developing dosage forms such as suspensions, seed coatings and granules of pyraclostrobin to reduce the use of organic solvents. Environmental hazards.

However, in the aqueous dispersion type, the particle size of the solid preparation such as wettable powder (WP) and water-dispersible granule (WDG) has a great influence on the stability and suspension ratio of the preparation. In order to obtain a solid preparation having a particle diameter of 1 to 15 μm, various types of pulverization are necessary. However, since the active compound has a low melting point, especially when the melting point does not exceed 70 ° C, direct pulverization is difficult because the active material is easily melted or softened during the pulverization process, which eventually leads to risk of physical and chemical quality of the product, and heat storage stability. Problems such as unsatisfactory sex and suspension rate.

The pyridoxal ester has a low melting point of only 56 to 64 ° C, so that the prepared pyraclostrobin composition has a problem of easy agglomeration after heat storage. For the long-term storage of the preparation, when the pesticide spray is used, the filter and the nozzle may be clogged due to the agglomeration and agglomeration, which may cause inconvenience to the user and affect the absorption of the pyraclostrobin active substance by the plant. , reducing the efficacy. These technical difficulties make the pyraclostrobin aqueous dispersion preparation not widely used.

CN102469775A discloses a process for preparing an aqueous suspension of pyraclostrobin by dispersing a large amount of pyraclostrobin in an aqueous phase in the form of amorphous droplets, and then adding a small amount of pyraclostrobin monocrystal A suspension of the type of particles induces the rapid crystallization of the pyridoxine amorphous droplets to form a final aqueous dispersion of the granules. This process requires the melting of pyraclostrobin and is carried out at a temperature above the melting point of the pyraclostrobin active over the heated aqueous phase. Therefore, the actual production and processing energy consumption of the method is relatively large, the operability is relatively complicated, and the equipment requirements are also high. Therefore, how to provide a composition which has good heat storage and storage stability, is not easy to aggregate and agglomerate, and is easy to prepare is currently urgently needed.

Summary of the invention

The inventors have unexpectedly discovered that a combination of pyraclostrobin, an alkyl sulfonate, a porous carrier, and a functional auxiliary can provide water of pyraclostrobin having improved heat storage stability and avoiding agglomeration and agglomeration. The solid composition is dispersed.

Based on the above findings, the present invention provides the following technical solutions:

In a first aspect, the present invention provides a pyraclostrobin aqueous dispersion solid composition comprising, by weight percentage, the following components: pyraclostrobin 5-50%, alkyl sulfonate 0.1-15%, The porous carrier is 5 to 80%, and the functional auxiliary is 1 to 45%.

In the present invention, the pyraclostrobin comprises 5 to 50% by weight of the composition, for example, 5%, 8%, 10%, 12%, 15%, 20%, 22%, 25%, 28%. , 30%, 32%, 35%, 40%, 42%, 45% or 50%.

In the present invention, the alkyl sulfonate accounts for 0.1 to 15% by weight of the composition, for example, 0.1%, 0.5%, 1%, 2%, 3%, 3.5%, 4%, 5.2%, 6%. , 7%, 8.5%, 9%, 10%, 11%, 12%, 13%, 14% or 15%.

In the present invention, the porous carrier accounts for 5 to 80% by weight of the composition, for example, 5%, 8%, 10%, 12%, 13%, 15%, 18%, 20%, 22%, 25 %, 30%, 35%, 40%, 48%, 52%, 60%, 65%, 72%, 79% or 80%.

In the present invention, the functional auxiliary agent accounts for 1 to 45% by weight of the composition, for example, 1%, 2%, 3%, 5%, 8%, 10%, 15%, 20%, 22%, 25%, 30%, 35%, 40%, 42%, 43% or 45%.

The invention selects the content of pyraclostrobin, the alkali sulfonate, the porous carrier and the functional auxiliary, and the prepared pyraclostrobin aqueous dispersion solid composition has heat storage and normal storage stability. Good sex, no aggregation, no caking, no clogging sprayer filter or spray head phenomenon.

The pyraclostrobin aqueous dispersion solid composition may contain other active ingredients, such as tebuconazole, dinotefuran or fluoxazole, in addition to the active ingredient of pyraclostrobin. One or more of them are contained, and the present invention is not particularly limited.

Preferably, the pyraclostrobin aqueous dispersion solid composition consists of the following components by weight:

Pyraclostrobin 6 to 30%, alkyl sulfonate 2 to 5%, porous carrier 10 to 70%, and the balance is a functional auxiliary.

Preferably, the alkyl sulfonate is selected from the group consisting of alkylnaphthalene sulfonates, alkylnaphthalene sulfonate formaldehyde polycondensates, alkylbenzene sulfonates, alkyl ethyl sulfonates or secondary alkyl sulfonates. Any one or a mixture of at least two, wherein a typical but non-limiting mixture is: a mixture of an alkylnaphthalenesulfonate and an alkylnaphthalenesulfonate formaldehyde polycondensate, an alkylnaphthalenesulfonate and an alkyl group a mixture of besylate, a mixture of alkyl ethyl sulfonate and alkylnaphthalene sulfonate formaldehyde polycondensate, a mixture of a secondary alkyl sulfonate and an alkyl benzene sulfonate; preferably an alkylnaphthalene sulfonate Formaldehyde polycondensate.

Preferably, the porous carrier is selected from the group consisting of kaolin, montmorillonite, attapulgite, synthetic silicon, plant fiber, mineral fiber or magnesium aluminum silicate, or a mixture of at least two thereof, of which typical but not The limiting mixture is: a mixture of kaolin and montmorillonite clay, a mixture of montmorillonite and attapulgite, a mixture of synthetic silicon and kaolin, a mixture of plant fibers, mineral fibers and synthetic silicon, magnesium aluminum silicate and montmorillonite. a mixture of clays.

Preferably, the kaolin is selected from any one or a mixture of at least two of kaolinite, dickite, pearlite, silica-rich kaolinite, halloysite or multi-water halloysite, of which typical But a non-limiting mixture is: a mixture of kaolinite and dickite, a mixture of pearlite and silicon-rich kaolinite, a mixture of watery halloysite and pearlite; the montmorillonite is selected from the group consisting of beidellite and lithium. Any one or a mixture of at least two of smectite, saponite or bentonite, wherein a typical but non-limiting mixture is: a mixture of beidellite and hectorite, a mixture of saponite and bentonite, a mixture of hectorite and saponite; the attapulgite is selected from the group consisting of bleaching earth and/or sepiolite; and the synthetic silicon is selected from the group consisting of white carbon black and/or fumed silica.

Preferably, the functional auxiliary agent is selected from the group consisting of a dispersing agent, a wetting agent, an antifoaming agent or an inert carrier, or a mixture of at least two, that is, the pyraclostrobin aqueous dispersion solid composition, Any one of the functional auxiliaries may be contained, or a mixture of two or more kinds may be used.

Preferably, the dispersing agent is selected from any one or a mixture of at least two of lignosulfonate, polycarboxylate, fatty alcohol polyoxyethylene ether or ethylene oxide propylene oxide block copolymer, Typical but non-limiting mixtures thereof are: a mixture of lignosulfonates and polycarboxylates, a mixture of polycarboxylates and fatty alcohol polyoxyethylene ethers, ethylene oxide propylene oxide block copolymers and wood a mixture of sulfonate salts.

Preferably, the wetting agent is selected from any one or a mixture of at least two of nonylphenol ethoxylates, K12 or polyoxyethylene fatty alcohol ethers, wherein a typical but non-limiting mixture is nonylphenol a mixture of polyoxyethylene ether and K12, a mixture of K12 and polyoxyethylene fatty alcohol ether.

Preferably, the antifoaming agent is selected from the group consisting of silicone antifoaming agents. As for the specific silicone antifoaming agent type, those skilled in the art can make conventional selection according to actual needs, and the invention is not particularly limited.

Preferably, the inert carrier is selected from any one or a mixture of at least two of corn starch, talc, sucrose, potassium sulfate, kaolin or diatomaceous earth, wherein a typical but non-limiting mixture is: corn starch and a mixture of talc, a mixture of sucrose and potassium sulfate, a mixture of kaolin and corn starch.

The pyraclostrobin aqueous dispersion solid composition of the present invention is formulated as a wettable powder or a water-dispersible granule.

Further, the present invention provides a method for preparing the pyraclostrobin aqueous dispersion solid composition, comprising the steps of:

(1) mixing pyraclostrobin and an alkyl sulfonate according to a ratio;

(2) coarsely pulverizing the obtained mixture at 35 ° C or lower to obtain a homogeneous mixture;

(3) A porous carrier and a functional auxiliary agent are added to the obtained homogeneous mixture, and finely pulverized to obtain the pyrazolidin ester aqueous dispersion solid composition.

Unlike the previously disclosed preparation method, the present invention firstly mixes pyraclostrobin and an alkyl sulfonate in step (1) without using all components or together with a dispersing agent and an antifoaming agent and a carrier. Carry out a mixed form.

The invention firstly mixes the pyraclostrobin and the alkyl sulfonate in the step (1), and the first coarse pulverization makes the pyraclostrobin and the alkyl sulfonate more fully mixed, the alkyl sulfonic acid. The salt adheres more effectively to the surface of the pyraclostrobin particles, effectively preventing contact aggregation between the particles and the particles during storage.

The inventors have also unexpectedly discovered that when only pyraclostrobin and the alkyl sulfonate are first mixed, by using coarse pulverization at 35 ° C or lower, the pyraclostrobin can be rendered as a paste having Softening, which further contributes to the problem of agglomeration and agglomeration in the back water-dispersible solid particulate product.

For the mixture obtained by mixing pyraclostrobin and the alkyl sulfonate, the present invention employs pulverization at a low temperature, which is specifically carried out at a low temperature of 35 ° C or lower, for example, a temperature of 0 ° C, 4 °C, 8 ° C, 10 ° C, 12 ° C, 15 ° C, 20 ° C, 22 ° C, 25 ° C, 28 ° C, 30 ° C or 35 ° C, of course, can also be carried out below 0 degrees.

The melting point of pyraclostrobin is 56-64 ° C. If it is directly pulverized under normal conditions, the original drug will soften and affect the pulverization efficiency. However, the pulverization at the low temperature of the present invention can effectively solve the problem of particle collision and softening of the pyraclostrobin original drug during the pulverization process, and at the same time, the alkyl sulfonate is sufficiently uniform and closely adhered to the surface of the pyraclostrobin particle. The effect of subsequent secondary jet pulverization on pyraclostrobin particles was solved.

The invention adopts a homogeneous mixture obtained after coarse pulverization, and further adds a porous carrier and a functional auxiliary agent, such an operation can make the pulverization temperature relatively loose, and can be carried out at a relatively high temperature, at this time, the function The auxiliaries can play a certain protective role, and further play a role in promoting the agglomeration and agglomeration of the finally formed pyraclostrobin aqueous dispersion solid composition.

In the preparation method of the present invention, the operation mode of coarse pulverization combined with fine pulverization at a low temperature is adopted, and by mixing the pulverization into two steps of coarse pulverization and fine pulverization, the mixture of the alkyl sulfonate and the pyraclostrobin is more fully and more. Effective adhesion to the surface of the pyraclostrobin particles further effectively prevents contact agglomeration between the particles and the particles during storage.

In the preparation of different forms of the water-dispersible solid composition of the present invention, for example, when preparing a wettable powder, the wettable powder can be directly obtained after the fine pulverization in the above preparation method in the step (3); and when the water-dispersible granule is prepared When the fine pulverization is carried out in the step (3), the granulation drying step is also required to obtain the water-dispersible granule. For the granulation and drying technology, those skilled in the art should understand that it can adopt various operation modes such as extrusion granulation, spray granulation, rotary granulation, fluidized bed granulation, etc., and the present invention does not specifically limit it. .

In the present invention, the coarse pulverization in the step (2) is carried out by airflow pulverization, and the specific operation is as follows: the mixture is passed through the high-speed airflow at a certain speed, so that a strong collision between the particles and the particles, the particles and the inner wall is achieved, and the damage is achieved. It finally makes the particle size after pulverization D90 ≤ 20 μm.

As for the specific gas flow rate used in the above-mentioned airflow pulverization, those skilled in the art can adjust the particle size according to the actual pulverization, and the present invention is not particularly limited.

The invention adopts jet milling to realize uniform mixing of pyraclostrobin and alkylsulfonate, and improves mixing uniformity and heat dissipation effect.

In the present invention, the fine pulverization in the step (3) is carried out by secondary gas flow pulverization, which can adjust the pulverization pressure and the feed rate so that the pulverized particle diameter reaches 1 to 15 μm.

As for the specific gas flow rate, pulverization pressure and feed rate used in the secondary air flow pulverization, those skilled in the art can also adjust according to the actual pulverized particle size to be achieved.

The pyraclostrobin aqueous dispersion solid composition of the present invention may be a wettable powder or a water-dispersible granule. The pyraclostrobin aqueous dispersion solid composition has the advantages of good heat storage and normal storage stability, no aggregation, no agglomeration, no clogging of the filter or the spray head, thereby facilitating storage and user use, and improving pyrazole. The efficacy of ether oxystrobin.

Compared with the prior art, the present invention has at least the following beneficial effects:

(1) The pyraclostrobin aqueous dispersion solid composition of the invention has the advantages of good heat storage and normal storage stability, no aggregation, no agglomeration, no clogging of a filter or a spray head, and good fluidity;

(2) The method for preparing a pyridoxazole aqueous dispersion solid composition of the present invention is simple in operation, low in economic cost, and achievable.

detailed description

To facilitate an understanding of the invention, the invention is set forth below. It should be understood by those skilled in the art that the present invention is not to be construed as limited. The following "%" refers to the weight percentage.

Example 1: 20% pyraclostrobin wettable powder

Pyraclostrobin 20%

Morwet D425 (alkylnaphthalene sulfonate formaldehyde polycondensate) 8%

Gas phase white carbon black 10%

Soap L (sodium tallowate) 2%

Corn starch 60%

Preparation process: the pyraclostrobin original drug and Morwet D425 (alkylnaphthalenesulfonate formaldehyde polycondensate) are mixed in a weight ratio, and after stirring uniformly, the first coarse pulverization is carried out at a temperature of 30 ° C to obtain homogeneity. Mixture; then gas phase white carbon, Soap L (sodium tallow) and corn starch are added to the above coarsely pulverized mixture in a weight ratio, and subjected to a second fine pulverization until the particle diameter D90 < 10 μm, that is, the final product.

Example 2: 50% pyraclostrobin water dispersible granules

Pyraclostrobin 50%

Morwet EFW (alkylnaphthalene sulfonate) 10%

White carbon black 20%

EO/PO block copolymer 5%

Soap L (sodium tallowate) 2%

Diatomaceous earth 13%

The preparation process: mixing the pyraclostrobin original drug with Morwet EFW (alkylnaphthalene sulfonate) in a weight ratio, stirring uniformly, and performing the first coarse pulverization at a temperature of 25 ° C to obtain a homogeneous mixture; White carbon black, EO/PO block copolymer, Soap L (sodium tallowate) and diatomaceous earth were added to the above coarsely pulverized mixture in a weight ratio, and subjected to a second fine pulverization to obtain a particle diameter of D90 < 10 μm. The mother powder, which is kneaded by adding an appropriate amount of water, is dried by extrusion granulation to obtain a final product.

Example 3: 10% pyraclostrobin wettable powder

Pyraclostrobin 10%

Sodium dodecyl sulfonate 5%

Calcined kaolin 20%

Nonylphenol polyoxyethylene ether phosphate 5%

Soap L (sodium tallowate) 1%

Potassium sulfate 59%

The preparation process: mixing the pyraclostrobin original drug with sodium dodecylsulfonate in a weight ratio, stirring uniformly, and performing the first coarse pulverization at a temperature of 22 ° C to obtain a homogeneous mixture; then calcining the kaolin , nonylphenol polyoxyethylene ether phosphate, Soap L (sodium tallow) and potassium sulfate are added to the above coarsely pulverized mixture in a weight ratio, and subjected to a second fine pulverization until the particle diameter D90 < 10 μm, which is the final product.

Example 4: 5% pyraclostrobin + 10% boscalyl wettable powder

Pyraclostrobin 5%

Boscalid 10%

Alkyl ethyl sulfonate 5%

Plant fiber 10%

Fatty alcohol polyoxyethylene ether 10%

Soap L (sodium tallowate) 2%

Talc 58%

The preparation process: mixing the pyraclostrobin original drug with the alkyl ethyl sulfonate in a weight ratio, stirring uniformly, and performing the first coarse pulverization at a temperature of 35 ° C to obtain a homogeneous mixture; then, the acyl bacterium Amine, plant fiber, fatty alcohol polyoxyethylene ether, Soap L (sodium tallow) and talc are added to the above coarsely pulverized mixture in a weight ratio, and subjected to a second fine pulverization until the particle diameter D90 < 10 μm. Final product.

Example 5: 5% pyraclostrobin + 40% chlorothalonil water-dispersible granules

Pyraclostrobin 5%

Chlorothalonil 40%

Alkylnaphthalene sulfonate formaldehyde polycondensate 5%

Mineral fiber 10%

Polycarboxylate 10%

Sodium succinate 5%

Soap L (sodium tallowate) 2%

Kaolin 23%

The preparation process comprises: mixing the pyraclostrobin original drug with the alkylnaphthalenesulfonate formaldehyde polycondensate in a weight ratio, stirring uniformly, and performing the first coarse pulverization at a temperature of 10 ° C to obtain a homogeneous mixture; Chlorothalonil, mineral fiber, polycarboxylate, sodium succinate sulfonate, Soap L (sodium tallowate) and kaolin are added to the above coarsely pulverized mixture in a weight ratio, and subjected to a second fine pulverization to obtain a particle size D90. <10 μm of the mother powder, which is kneaded by adding an appropriate amount of water, and then dried by extrusion granulation to obtain a final product.

Comparative Example 1: 20% pyraclostrobin WP

Preparation process: the above composition is subjected to jet milling to make the particle size D90 <10 μm, that is, the final product

Comparative Example 2: 50% pyraclostrobin water dispersible granules

Preparation process: The above composition is subjected to jet milling to obtain a mother powder having a particle diameter of D90 < 10 μm. The mother powder is kneaded by adding an appropriate amount of water, and then dried by extrusion granulation to obtain a final product.

Comparative Example 3: 10% pyraclostrobin wettable powder

Comparative Example 4: 10% pyraclostrobin wettable powder

Formulation process: The above composition is subjected to jet milling so that the particle diameter D90 < 10 μm, that is, the final product.

Comparative Example 5: 50% pyraclostrobin water dispersible granules

Comparative Example 6: 5% pyraclostrobin + 10% boscalid wettable powder

Comparative Example 7: 5% pyraclostrobin + 40% chlorothalonil Water-dispersible granules

Comparative example 8:

The same components as in Comparative Example 1 were prepared by a similar method of the present invention.

The preparation process: the pyraclostrobin and the polycarboxylate sodium salt are mixed in a weight ratio, and after being uniformly stirred, the first coarse pulverization is carried out at a temperature of 30 ° C, and then the gas phase white carbon black, Soap L (sodium borate) And the corn starch is added to the above coarse powder mixture in a weight ratio, and the second fine pulverization is carried out until the particle diameter D90 < 10 μm, that is, the final product is obtained.

Comparative example 9:

The same components as in Comparative Example 4 were prepared by the formulation method of the present invention.

The preparation process comprises: mixing pyraclostrobin and sodium dodecylsulfonate in a weight ratio, stirring uniformly, performing the first coarse pulverization at a temperature of 30 ° C, and then adding nonylphenol ethoxylate phosphate, Soap L (sodium tallowate) and potassium sulfate are added to the above coarse powder mixture in a weight ratio, and subjected to a second fine pulverization until the particle diameter D90 < 10 μm, that is, the final product is obtained.

Comparative example 10:

The same components as in Comparative Example 5. The preparation is carried out using the formulation method of the present invention.

The preparation process: the pyraclostrobin and Morwet EFW (alkylnaphthalene sulfonate) are mixed in a weight ratio, and after being uniformly stirred, the first coarse pulverization is carried out at a temperature of 30 ° C, and then the EO/PO block copolymer is used. Soap L (sodium tallow) and sodium sulfate are added to the above coarse powder mixture in a weight ratio, and subjected to a second fine pulverization to obtain a mother powder having a particle diameter of D90 < 10 μm, and the mother powder is kneaded by adding an appropriate amount of water. The final product is obtained by extrusion granulation and drying.

The physical and chemical stability of the samples prepared in the above Examples 1 to 5 and Comparative Examples 1 to 10, including room temperature stability and heat storage stability, were tested.

Normal temperature stability test at room temperature sample traits and levitation rate indicators (CIPAC MT184 method).

The heat storage stability test was carried out in an oven at 54 °C. After heat storage in an oven at 54 ° C, the samples were removed from the oven. After cooling to room temperature, each test sample was poured out to observe the fluidity of the sample. The wettable powder sample was then passed directly through a 325 mesh screen; the water dispersed granule sample was diluted with water and passed through a 325 mesh screen.

The results of the test are shown in Table 1.

Table 1

The test results in Table 1 show that the pyraclostrobin aqueous dispersion solid composition prepared according to the present invention has good fluidity at room temperature, uniform sample, no agglomeration, no sticking phenomenon, especially with the comparative phase. Compared with a higher suspension rate, it basically reaches a suspension rate of more than 85%, which is far from being comparable. In the heat storage stability test, the pyraclostrobin aqueous dispersion solid composition of the present invention has more outstanding heat storage stability performance, good fluidity, no agglomeration, no clogging screen, and therefore has more It is convenient for users to use and improve the outstanding advantages of pyraclostrobin.

The Applicant declares that the present invention illustrates the detailed process equipment and process flow of the present invention by the above embodiments, but the present invention is not limited to the above detailed technical solutions, that is, it does not mean that the present invention must rely on the above detailed technical solutions to implement. . It should be apparent to those skilled in the art that any modifications of the present invention, equivalent substitution of the various materials of the products of the present invention, addition of auxiliary components, selection of specific means, and the like, are all within the scope of the present invention.

Claims

A liquid dispersion solid composition of pyraclostrobin characterized by comprising the following components in a weight percentage: 5-50% of pyraclostrobin, 0.1-15% of an alkyl sulfonate, and a porous carrier 5~ 80%, functional additives 1 to 45%.
The pyraclostrobin aqueous dispersion solid composition according to claim 1, which is composed of the following components in a weight percentage: 6 to 30% of pyraclostrobin and 2 to 5% of an alkyl sulfonate. The porous carrier is 10 to 70%, and the balance is a functional auxiliary.
The pyraclostrobin aqueous dispersion solid composition according to claim 1 or 2, wherein the alkyl sulfonate is selected from the group consisting of alkyl naphthalene sulfonates, alkyl naphthalene sulfonate formaldehyde polycondensates, Any one or a mixture of at least two alkylbenzene sulfonates, alkyl ethyl sulfonates or secondary alkyl sulfonates, preferably alkylnaphthalene sulfonate formaldehyde polycondensates;

Preferably, the porous carrier is selected from the group consisting of kaolin, montmorillonite, attapulgite, synthetic silicon, plant fiber, mineral fiber or magnesium aluminum silicate, or a mixture of at least two;

Preferably, the kaolin is selected from any one or a mixture of at least two of kaolinite, dickite, pearlite, silicon-rich kaolinite, halloysite or multi-water halloysite; The montmorillonite clay is selected from any one or a mixture of at least two of beidellite, hectorite, saponite or bentonite; the attapulgite is selected from the group consisting of bleaching earth and/or sepiolite; Said synthetic silicon is selected from the group consisting of white carbon black and/or fumed silica;

Preferably, the functional adjuvant is selected from any one or a mixture of at least two of a dispersing agent, a wetting agent, an antifoaming agent or an inert carrier.
The pyraclostrobin aqueous dispersion solid composition according to claim 3, wherein the dispersing agent is selected from the group consisting of lignosulfonates, polycarboxylates, fatty alcohol polyoxyethylene ethers or ethylene oxide. Any one or a mixture of at least two of propylene oxide block copolymers;

Preferably, the wetting agent is selected from any one or a mixture of at least two of nonylphenol ethoxylate, K12 or polyoxyethylene fatty alcohol ether;

Preferably, the antifoaming agent is selected from the group consisting of silicone antifoaming agents;

Preferably, the inert carrier is selected from any one or a mixture of at least two of corn starch, talc, sucrose, potassium sulfate, kaolin or diatomaceous earth.
The pyraclostrobin aqueous dispersion solid composition according to any one of claims 1 to 4, wherein the composition preparation is a wettable powder or a water-dispersible granule.
The method for preparing a pyraclostrobin aqueous dispersion solid composition according to any one of claims 1 to 5, which comprises the steps of:

(1) mixing pyraclostrobin and an alkyl sulfonate according to a ratio;

(2) coarsely pulverizing the obtained mixture at 35 ° C or lower to obtain a homogeneous mixture;

(3) A porous carrier and a functional auxiliary agent are added to the obtained homogeneous mixture, and finely pulverized to obtain the pyrazolidin ester aqueous dispersion solid composition.
The method according to claim 6, wherein after the fine pulverization in the step (3), granulation and drying are carried out to obtain pyraclostrobin aqueous dispersion granules.
The method according to claim 6 or 7, wherein the coarse pulverization in step (2) is carried out by air flow pulverization, and the particle size after pulverization is D90 ≤ 20 μm;

Preferably, the fine pulverization in the step (3) is carried out by secondary air flow pulverization, and the particle diameter after pulverization is 1 to 15 μm.
The pyraclostrobin aqueous dispersion solid composition prepared by the method of any one of claims 6-8.