CN114208822B - Suspending agent containing prothioconazole and meperflutonazol and preparation method thereof - Google Patents

Suspending agent containing prothioconazole and meperflutonazol and preparation method thereof Download PDF

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CN114208822B
CN114208822B CN202111645143.4A CN202111645143A CN114208822B CN 114208822 B CN114208822 B CN 114208822B CN 202111645143 A CN202111645143 A CN 202111645143A CN 114208822 B CN114208822 B CN 114208822B
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agent
prothioconazole
meperflutonazol
sodium
suspension concentrate
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CN114208822A (en
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余思策
李蕾
刘润峰
陈坤
张瑜
叶小妹
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Jiangsu Mingde Lida Crop Technology 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
    • 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
    • A01N25/02Biocides, 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 containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N25/30Biocides, 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 characterised by the surfactants
    • 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

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

Abstract

The invention discloses a suspending agent containing prothioconazole and meperflutonazol and a preparation method thereof. The suspension containing prothioconazole and meperflutonazol comprises the following components in percentage by weight: 1-50% of prothioconazole raw drug, 1-50% of chlorofluoromethane raw drug, 1-15% of dispersing agent, 1-10% of wetting agent, 1-10% of antifreezing agent, 0.1-5% of thickening agent, 0.1-1% of preservative, 0.1-1% of defoaming agent and deionized water which are added to 100%. The preparation method of the suspension containing prothioconazole and meperflutonazol is simple, the prepared suspension has stable storage particle size and high suspension rate of each component, and the problem of low suspension rate caused by easy particle size growth of a compound preparation of prothioconazole and meperflutonazol in the process of thermal storage is solved. The suspending agent prepared by the invention has high suspension rate and excellent and stable product performance, and is beneficial to long-term storage and use.

Description

Suspending agent containing prothioconazole and meperflutonazol and preparation method thereof
Technical Field
The invention relates to the field of preparation of pesticide preparations, in particular to a prothioconazole and meperflutonazol compound suspending agent and a preparation method thereof.
Background
Prothioconazole is a novel broad-spectrum triazolethione fungicide, and the mechanism of action is to inhibit the demethylation of the sterol precursor in fungi, lanosterol or 24-methylene dihydrolanosterol in the l4 position, i.e. demethylation inhibitors (DMIs). Not only has good systemic activity, excellent protection, treatment and eradication activity, but also has long lasting period.
Chlorofloxacin (mefentrifluconazole) is the 1 st novel isopropanol triazole bactericide developed and marketed in 2016 by Pasteur corporation, is a C14-demethylation inhibitor in sterol biosynthesis, has broad spectrum, high efficiency and systemic property, and has eradicating and protecting effects. In a resistance test, the chlorofluoroether azole has a good control effect on septoria, and different from other triazole bactericides, an isopropanol structure contained in a molecule of the chlorofluoroether azole is beneficial to reducing germ mutation and delaying generation and development of resistance of the bactericides, and the chlorofluoroether azole has good biological activity on a plurality of intractable fungal diseases and is expected to become an important tool for efficiently controlling the diseases.
Suspending agents (SC), also called aqueous suspending agents, colloidal suspending agents and concentrated suspending agents, are used for dispersing raw medicines which are insoluble or difficultly soluble in water into water under the action of surfactants and other auxiliary agents to form a uniform and stable suspending system. Because the dispersion medium is water, the suspending agent has the characteristics of low cost, safe production, storage, transportation and use and the like, is easy to mix with water, and is convenient to use. Compared with pesticide formulations using organic solvents as media, the pesticide formulation has the advantages of small environmental impact, light phytotoxicity and the like.
The suspending agent is a highly dispersed heterogeneous complex system. The composition of the emulsion contains active ingredients and a dispersing medium, and also contains a plurality of auxiliary agents. Thus, the stability of the formulation is affected by the physical form, melting point, volatility, solubility and chemical properties of the pesticide active ingredient itself, including hydrolytic and photochemical stability, thermal stability, redox properties, and interactions of the compound with the dispersion medium, surfactants and other ingredients in the formulation. Also, since it is always present in the form of a suspension, chemical instability during storage, especially long term storage, may occur, while physical stability is more often encountered. To maintain physical stability of the pesticide suspension reservoirs, suspension build-up, settling and crystal growth must be controlled by formulation and processing techniques. It is necessary to ensure that the suspending agent does not coalesce during storage and that the particle size of the dispersed particles and their distribution remain unchanged. The dispersed phase particles need to be stably suspended in the dispersion medium without settling.
The frequent use of the bactericide containing a single active component causes the drug resistance of most germs, and the control effect is not ideal. The prothioconazole and meperflutonazole compound suspending agent has the effect of compounding and synergism, but the problems that the increase of the heat storage particle size is difficult to control, the suspension rate is low and the qualified suspending agent cannot be prepared are often caused.
Therefore, a formula and a preparation process of the prothioconazole and chlorofluoromethoate compound suspending agent are urgently needed, the physical stability of the prothioconazole and chlorofluoromethoate compound suspending agent is improved, and the economic loss is reduced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a prothioconazole and chlorofluoromethane compounded suspending agent and a preparation method thereof, so that the problems that the increase of the heat storage particle size after the prothioconazole and chlorofluoromethane are compounded is difficult to control, the suspension rate is low, and the qualified suspending agent cannot be prepared are solved, and the finally prepared prothioconazole and chlorofluoromethane compounded suspending agent has high suspension rate and stable performance, and is beneficial to long-term storage.
In order to realize the purpose of the invention, the technical scheme provided by the invention is as follows:
the invention relates to a suspending agent containing prothioconazole and meperflutonazol, which comprises 1-50% of prothioconazole, 1-50% of meperflutonazol, 1-15% of dispersing agent, 1-10% of wetting agent, 1-10% of antifreezing agent, 0.1-5% of thickening agent, 0.1-1% of preservative, 0.1-1% of defoaming agent and deionized water which are supplemented to 100%.
Furthermore, the suspending agent containing prothioconazole and meperflutonazole comprises 5-30% of prothioconazole raw material, 5-30% of meperflutonazole raw material, 3-12% of dispersing agent, 1-5% of wetting agent, 3-6% of antifreezing agent, 0.1-2% of thickening agent, 0.1-0.5% of preservative, 0.1-1% of defoaming agent and deionized water which are added to 100%.
The suspending agent containing prothioconazole and meperflutonazol is characterized in that the dispersant is; one or more of alkyl naphthalene sulfonate, bis (alkyl) naphthalene sulfonate formaldehyde condensate, aryl phenol polyoxyethylene succinate sulfonate, octyl phenol polyoxyethylene ether sulfate, polycarboxylate, lignin sulfonic acid sodium salt, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylbenzene sulfonic acid calcium salt, naphthalene sulfonic acid formaldehyde condensate sodium salt, alkylphenol polyoxyethylene, polyoxyethylene-polyoxypropylene block copolymer, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ester and ester polyoxyethylene ether.
Furthermore, the suspending agent containing prothioconazole and meperflutonazol is characterized in that the dispersing agent is one or more of polycarboxylate, naphthalene sulfonic acid formaldehyde condensate sodium salt or polyoxyethylene-polyoxypropylene block copolymer.
Further preferably, the suspending agent containing prothioconazole and meperflutonazole provided by the invention has 5-8% of dispersing agent.
Preferably, the dispersant is a combination of a polycarboxylate, a sodium salt of a naphthalene sulfonic acid formaldehyde condensate and a polyoxyethylene-polyoxypropylene block copolymer, and the weight ratio of the polycarboxylate, the sodium salt of a naphthalene sulfonic acid formaldehyde condensate and the polyoxyethylene-polyoxypropylene block copolymer is (1-5): (1-5): (1-5); further preferably (1.5 to 3): (2-2.5): (1.5-2.5).
The suspending agent containing prothioconazole and meperfluorfen-sodium is characterized in that the wetting agent is one or more of sodium dodecyl sulfate, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate and sodium lauryl sulfate.
Further, the suspending agent containing prothioconazole and meperfluorfen-sodium according to the present invention preferably comprises a mixture of sodium dodecyl sulfate and sodium alkyl naphthalene sulfonate, and optionally, the weight ratio of the sodium dodecyl sulfate to the sodium alkyl naphthalene sulfonate is (0.5-1.2): (0.5-1.2).
The suspending agent containing prothioconazole and meperflutonazole is characterized by also comprising an antifreezing agent, a thickening agent, a preservative and an antifoaming agent. The antifreezing agent is one or more of ethylene glycol, 1, 2-propylene glycol, glycerol and urea; ethylene glycol is preferred.
The thickening agent is one or more of magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose and phenolic resin; preferably a mixture of magnesium aluminum silicate and xanthan gum.
The defoaming agent is one or more of C8-10 fatty alcohol, C10-20 saturated fatty acid (such as capric acid) and amide, glycerol polyoxyethylene ether and organic silicon defoaming agent.
The preservative is one or more of sodium nitrite, sodium benzoate, sodium sorbate and Kathon.
The preparation method of the suspending agent containing prothioconazole and meperflutonazole disclosed by the invention comprises the following steps of:
the method comprises the following steps: uniformly mixing the dispersing agent, the wetting agent, the defoaming agent, the antifreezing agent, the preservative and the deionized water, carrying out high-speed shearing, and obtaining a feed liquid A after the high-speed shearing is finished;
step two: putting the prothioconazole and the meperflutonazole in the feed liquid A, uniformly dispersing, controlling the temperature of the material at 0-30 ℃, sanding, and obtaining feed liquid B after sanding;
step three: and (3) putting the thickening agent into the material liquid B according to a proportion, and uniformly dispersing to obtain the suspending agent.
The preparation method of the suspending agent containing prothioconazole and meperfluorfen-ethyl is characterized in that in the second step of sanding, zirconia beads with the particle size of 0.8-1mm are added into a sanding machine for sanding, and the detected particle size D90 is smaller than 5 microns.
Advantageous effects
(1) The prothioconazole and chlorofluoromethane compound suspending agent has the effect of compounding and synergism, and reduces the frequent use of bactericides.
(2) The addition of a suitable dispersing agent, which adsorbs on the particles of the base drug, generally prevents irreversible flocculation.
(3) Proper pesticide auxiliaries such as a dispersing agent, a wetting agent, a thickening agent, a defoaming agent, an antifreezing agent, a preservative and the like are selected, so that the raw pesticide can be dispersed in water to form a stable dispersion system.
(4) The selection of the original drug and the auxiliary agent solves the problems that the increase of the heat storage particle size is difficult to control after the prothioconazole and the meperflutonazol are compounded, the suspension rate is low, and the qualified suspending agent cannot be prepared easily.
(5) The prothioconazole and meperflutonazol compound suspending agent prepared by the invention has high suspension rate and stable performance, is beneficial to long-term storage, and still has good fluidity and suspension rate when being prepared into suspending agent with higher content.
(6) In the preparation method, zirconia balls with the diameter of 0.8-1mm are selected, the size is small, the wear resistance is strong, and the particle size D90 of the prepared prothioconazole and chlorofluoroether conazole compound suspending agent is less than 5 microns.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention. Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, elements, methods, means, and the like that are well known to those skilled in the art are not described in detail in order to not unnecessarily obscure the present invention.
Example 1
The embodiment provides a 10% prothioconazole-5% Chlorofluoroether (CFR) azole suspending agent, which comprises the following components in percentage by mass: 10% of prothioconazole and 5% of fluroxypyr; dispersing agent: 1.5% of polycarboxylate, 2% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 1.5% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 0.5%, alkyl naphthalene sulfonic acid sodium 0.5%; thickening agent: 0.2% of xanthan gum and 1% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method comprises the following steps:
will dispersant, wetting agent, antifreeze, defoaming agent, antiseptic and deionized water misce bene carry out the high-speed shearing, add prothioconazole and chlorine fluoride ether bacteria oxazole original medicine after the high-speed shearing finishes, after the dispersion is even, control material temperature at 0 ~ 30 ℃ sand, adopt 0.8-1 mm's zirconia pearl sand, sand to particle diameter D90 and reach below 5um, add at last the thickener obtains 10% prothioconazole 5% chlorine fluoride ether bacteria oxazole suspending agent after the dispersion is even.
Example 2
The embodiment provides a 10% prothioconazole-10% Chlorofluoroether (CFR) azole suspending agent, which comprises the following components in percentage by mass: 10% of prothioconazole and 10% of fluroxypyr; dispersing agent: 2% of polycarboxylate, 2% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 2% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 0.5%, alkyl naphthalene sulfonic acid sodium 1%; thickening agent: 0.2% of xanthan gum and 1% of magnesium aluminum silicate; antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Example 3
The embodiment provides a 20% prothioconazole-10% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: 20% of prothioconazole and 10% of fluroxypyr; dispersing agent: 3% of polycarboxylate, 2% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 2% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 1%, alkyl naphthalene sulfonate 1%; thickening agent: 0.16% of xanthan gum and 0.7% of magnesium aluminum silicate; antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Example 4
The embodiment provides a 25% prothioconazole-15% meperflutonazol suspension concentrate, which comprises the following components in percentage by mass: 25% of prothioconazole and 15% of meperflutonazol; dispersing agent: 3% of polycarboxylate, 2.5% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 2% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 1.2%, alkyl naphthalene sulfonic acid sodium 1.2%; thickening agent: 0.14% of xanthan gum and 0.5% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Example 5
The embodiment provides a 30% prothioconazole-15% meperflutonazol suspension concentrate which comprises the following components in percentage by mass: 30% of prothioconazole and 15% of meperflutonazol; dispersing agent: 3% of polycarboxylate, 2.5% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 2.5% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 0.5%, alkyl naphthalene sulfonic acid sodium 1.2%; thickening agent: 0.1% of xanthan gum and 0.5% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Example 6
The embodiment provides a 10% prothioconazole-5% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: 10% of prothioconazole and 5% of fluroxypyr; dispersing agent: 1% of polycarboxylate, 1% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 1% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 1.2%, alkyl naphthalene sulfonic acid sodium 0.5%; thickening agent: 0.2% of xanthan gum and 1% of magnesium aluminum silicate; antifreezing agent: 4% of glycerol; defoaming agent: 0.3 percent of glycerol polyoxyethylene ether; preservative: 0.2% of Kathon; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Example 7
The embodiment provides a 30% prothioconazole-15% meperflutonazol suspension concentrate which comprises the following components in percentage by mass: 30% of prothioconazole and 15% of fluroxypyr; dispersing agent: 4% of polycarboxylate, 4% of naphthalene sulfonic acid formaldehyde condensate sodium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: sodium dodecyl sulfate 1.5%, alkyl naphthalene sulfonic acid sodium 1.5%; thickening agent: 0.1% of xanthan gum and 0.5% of magnesium aluminum silicate; antifreezing agent: 4% of glycerol; defoaming agent: 0.3 percent of glycerol polyoxyethylene ether; preservative: 0.2 percent of Kathon; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 1
The comparative example provides a 15% prothioconazole-15% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: prothioconazole 15%, fluroxypyr 15%; dispersing agent: 3.5% of octyl phenol polyoxyethylene ether sulfate and 3.5% of sodium lignosulfonate; wetting agent: 2% of sodium lauryl sulfate; thickening agent: 0.16% of xanthan gum and 0.7% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 2
The comparative example provides a 20% prothioconazole-15% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: 20% of prothioconazole and 15% of fluroxypyr; dispersing agent: 3.5% of octyl phenol polyoxyethylene ether sulfate and 3.5% of polycarboxylate; wetting agent: 2% of sodium lauryl sulfate; thickening agent: 0.14% of xanthan gum and 0.7% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 3
The comparative example provides a 25% prothioconazole.15% Chlorofluoroether (CFR) azole suspending agent, which consists of the following components in percentage by mass: 25% of prothioconazole and 15% of fluroxypyr; dispersing agent: 3.5 percent of sodium lignosulphonate and 3.5 percent of calcium alkyl benzene sulfonate; wetting agent: 2% of sodium lauryl sulfate; thickening agent: 0.14% of xanthan gum and 0.5% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 4
The comparative example provides a 15% prothioconazole.15% Chlorofluoroether (CFR) azole suspending agent, which consists of the following components in percentage by mass: prothioconazole 15%, fluroxypyr 15%; dispersing agent: 7% of polycarboxylate; wetting agent: 2% of sodium lauryl sulfate; thickening agent: 0.16% of xanthan gum and 0.7% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 5
The comparative example provides a 15% prothioconazole-15% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: prothioconazole 15%, fluroxypyr 15%; dispersing agent: naphthalene sulfonic acid formaldehyde condensate sodium salt 7%; wetting agent: sodium lauryl sulfate 2%; thickening agent: 0.16% of xanthan gum and 0.7% of magnesium aluminum silicate; an antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Comparative example 6
The comparative example provides a 15% prothioconazole-15% chlorofluoroether bacteria azole suspending agent, which comprises the following components in percentage by mass: prothioconazole 15%, fluroxypyr 15%; dispersing agent: 7% of polyoxyethylene-polyoxypropylene block copolymer; wetting agent: 2% of sodium lauryl sulfate; thickening agent: 0.16% of xanthan gum and 0.7% of magnesium aluminum silicate; antifreezing agent: 4% of ethylene glycol; defoaming agent: 0.3 percent of organic silicon defoamer; preservative: 0.2 percent of sodium benzoate; the deionized water is added to make up to 100 percent.
The preparation method is the same as example 1.
Test examples:
the particle size and suspension percentage of the finished products obtained in the above examples and comparative examples were measured before and after 54 ℃ heat storage. The results of the measurements are shown in Table 1 below. The suspension rate is measured by GB/T14825-2006, and the particle size is measured by an Euramerican LS-POP (9) laser particle sizer.
TABLE 1
Figure BDA0003443342720000071
Figure BDA0003443342720000081
As can be seen from the data in the table above, the suspension rate of the product of each example is more than 90%, the product is qualified, and the product has the characteristics of high suspension rate, small particle size increase after heat storage, good stability and the like. The product of the comparative example has larger grain size increase, low suspension rate and poor stability after heat storage, and does not meet the requirements. From examples 1-7, the properties of the resulting suspension products were slightly different when the content of the pharmaceutically active ingredient was varied from 15 to 45% with the selection of the preferred dispersing and wetting agents, indicating that the content of the drug has some effect on the dosage form properties. From the data of the examples and comparative examples, it is preferred that the dispersing and wetting agents provide a significant improvement in the performance of the suspending agents, whereas conventional adjuvants do not.
By selecting the raw pesticide and the auxiliary agent, the invention solves the problems that the increase of the heat storage particle size is difficult to control after the prothioconazole and the meperflutonazol are compounded, the suspension rate is low, and the qualified suspending agent cannot be prepared easily.
The prothioconazole and chlorofluoromethane compound suspending agent prepared by the invention has high suspension rate and stable performance, is beneficial to long-term storage, and still has good fluidity and suspension rate when preparing suspending agent with higher content.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (12)

1. A suspension containing prothioconazole and meperflutonazol, which is characterized in that: the suspending agent comprises 5-30% of prothioconazole raw drug, 5-30% of chlorofluoromethane raw drug, 3-12% of dispersing agent, 1-5% of wetting agent, 3-6% of antifreezing agent, 0.1-2% of thickening agent, 0.1-0.5% of preservative, 0.1-1% of defoaming agent and deionized water for supplementing to 100%;
the dispersing agent is a composition of polycarboxylate, naphthalene sulfonic acid formaldehyde condensate sodium salt and polyoxyethylene-polyoxypropylene block copolymer, and the weight ratio of the polycarboxylate, the naphthalene sulfonic acid formaldehyde condensate sodium salt to the polyoxyethylene-polyoxypropylene block copolymer is (1-5): (1 to 5): (1 to 5);
the wetting agent is a mixture of sodium dodecyl sulfate and sodium alkyl naphthalene sulfonate, and the weight ratio of the sodium dodecyl sulfate to the sodium alkyl naphthalene sulfonate is (0.5-1.2): (0.5 to 1.2).
2. The prothioconazole and meperflutonazole-containing suspension concentrate according to claim 1, characterized in that: in the dispersant, the weight ratio of the polycarboxylate to the sodium salt of the naphthalene sulfonic acid formaldehyde condensate to the polyoxyethylene-polyoxypropylene block copolymer is (1.5 to 3): (2 to 2.5): (1.5 to 2.5).
3. The prothioconazole and meperflutonazole-containing suspension concentrate according to claim 1, wherein the dispersant is added in an amount of 5-8%.
4. The prothioconazole and meperflutonazole-containing suspension concentrate of claim 1, wherein the anti-freezing agent is one or more of ethylene glycol, 1, 2-propylene glycol, glycerol and urea.
5. The prothioconazole and meperflutonazol-containing suspension concentrate of claim 1, wherein the cryoprotectant is ethylene glycol.
6. The prothioconazole and meperflutonazol-containing suspension concentrate of claim 1, wherein the thickener is one or more of magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, and phenolic resin.
7. The prothioconazole and meperflutonazol-containing suspension concentrate of claim 1, wherein the thickening agent is a mixture of magnesium aluminum silicate and xanthan gum.
8. The suspension concentrate containing prothioconazole and meperflutonazole of claim 1, wherein the antifoaming agent is one or more of C8-10 fatty alcohols, C10-20 saturated fatty acids and amides, glycerol polyoxyethylene ethers and silicone antifoaming agents.
9. The prothioconazole and meperflutonazole-containing suspension concentrate of claim 8, wherein the C10-20 saturated fatty acid is decanoic acid.
10. The prothioconazole and meperflutonazol-containing suspension concentrate of claim 1, wherein the preservative is one or more of sodium nitrite, sodium benzoate, sodium sorbate, and kathon.
11. A process for the preparation of a suspension containing prothioconazole and meperflutonazole according to any one of claims 1 to 10,
the method comprises the following steps:
the method comprises the following steps: uniformly mixing the dispersing agent, the wetting agent, the defoaming agent, the antifreezing agent, the preservative and the deionized water, and carrying out high-speed shearing to obtain a feed liquid A after the high-speed shearing is finished;
step two: putting the prothioconazole and the meperflutonazole in the feed liquid A, uniformly dispersing, controlling the temperature of the material at 0-30 ℃, sanding, and obtaining feed liquid B after sanding;
step three: and (3) putting the thickening agent into the material liquid B according to a proportion, and uniformly dispersing to obtain the suspending agent.
12. The method for preparing a prothioconazole and meperflutonazol-containing suspension concentrate as claimed in claim 11, wherein the sand grinding in the second step is performed by adding zirconia beads with a particle size of 0.8-1mm into a sand grinder and grinding until the particle size D90 is less than 5 microns.
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Citations (3)

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CN103314964A (en) * 2012-03-20 2013-09-25 陕西韦尔奇作物保护有限公司 Pesticide composition containing fenhexamid and triazole
CN111559984A (en) * 2019-02-14 2020-08-21 刘力 Broad-spectrum sterilization low-toxicity low-residue growth promoting prothioconazole manganese zinc compound and composition thereof

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN102258049A (en) * 2011-08-26 2011-11-30 陕西美邦农药有限公司 Pesticidal composition containing prothioconazole and triazole
CN103314964A (en) * 2012-03-20 2013-09-25 陕西韦尔奇作物保护有限公司 Pesticide composition containing fenhexamid and triazole
CN111559984A (en) * 2019-02-14 2020-08-21 刘力 Broad-spectrum sterilization low-toxicity low-residue growth promoting prothioconazole manganese zinc compound and composition thereof

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