CN114651823A - Suspending agent of pyraflufen-ethyl and cloransulam-methyl, and preparation method and application thereof - Google Patents

Suspending agent of pyraflufen-ethyl and cloransulam-methyl, and preparation method and application thereof Download PDF

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CN114651823A
CN114651823A CN202011538918.3A CN202011538918A CN114651823A CN 114651823 A CN114651823 A CN 114651823A CN 202011538918 A CN202011538918 A CN 202011538918A CN 114651823 A CN114651823 A CN 114651823A
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agent
cloransulam
suspending agent
ethyl
suspension
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CN114651823B (en
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袁良国
李志清
王建伟
张小兵
赵保臣
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Shandong Weifang Rainbow Chemical Co Ltd
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Shandong Weifang Rainbow Chemical 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
    • A01N43/72Biocides, 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
    • 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

Abstract

The invention relates to the technical field of pesticide preparations, and discloses a suspending agent of pyraflufen-ethyl and cloransulam, a preparation method and application thereof. The suspending agent comprises a herbicidal composition of the topramezone and the cloransulam as active ingredients and a pesticide acceptable auxiliary agent; the mass ratio of cloransulam-methyl to the xaflufen-ethyl is 1: 1-1: 10. The effective active ingredients of the suspending agent comprise the Sulfopyrazole and the cloransulam, the mutual mixing of the Sulfopyram and the cloransulam does not generate conflict, the synergistic interaction is good in a specific range, and the generation of drug resistance of weeds can be delayed; meanwhile, the better physical and chemical properties of the suspending agent can be obtained through optimizing the auxiliary agent, particularly, the suspending agent can keep better suspension rate after hot storage, can be applied to weeds such as crabgrass, cockspur grass, dayflower, piemarker, spiny sedge, endive and the like in soybean fields, and has good application prospect.

Description

Suspending agent of pyraflufen-ethyl and cloransulam, and preparation method and application thereof
Technical Field
The invention relates to the technical field of pesticide preparations, and particularly relates to a suspending agent of pyraflufen-ethyl and cloransulam, and a preparation method and application thereof.
Background
Pyraflufen-ethyl (Pyroxasulfone), chemical name: the 3- [5- (difluoromethoxy) -1-methyl-3- (trifluoromethyl) pyrazol-4-yl methylsulfonyl ] -4, 5-dihydro-5, 5-dimethyl-1, 2-isoxazole belongs to a novel isoxazole herbicide, is widely applied to crops, is mainly used for crops such as corn, cotton, peanut, wheat and sunflower, and can effectively prevent and kill gramineous weeds such as setaria, crabgrass and cockspur grass and broadleaf weeds such as amaranthus, stramonium, solanum and abutilon.
Cloransulam-methyl, chemical name: methyl 3-chloro-2- (5-ethoxy-7-fluoro [1,2,4] triazolo [1,5-c ] pyrimidine-2-yl sulfonyl) aminobenzoate belongs to sulfonamide herbicides and is mainly used for controlling broadleaf weeds by spraying stem leaves of soybean fields.
Herbicide varieties containing a single active component often have different degrees of defects in agricultural pest control, such as: the weeding spectrum is narrow, the weeds are easy to generate drug resistance after continuous use, the environmental pollution is aggravated after the weeds are used for many times, and researches show that the fenpyrazazole can be continuously and singly applied for three years, the hard ryegrass can generate resistance to the fenpyrazazole and even generate interactive resistance to other agents, and after the cloransulam-methyl is applied, the soybean leaves are easy to generate the symptom of chlorotic phytotoxicity and are easy to generate phytotoxicity to succeeding crops.
Disclosure of Invention
In view of the above, the present invention aims to provide a suspension with synergistic effect of pyraflufen-ethyl and cloransulam, so that the pyraflufen-ethyl and cloransulam can synergistically improve the control effect of each other; simultaneously has better physical and chemical properties, such as long-lasting foamability, residue after pouring, suspension rate before and after heat storage and appearance;
the invention also aims to provide the application of the suspending agent in the aspect of crop weeding and the application of preparing related pesticide formulations.
In order to achieve the above purpose, the invention provides the following technical scheme:
a suspending agent of the sulfuryl pyraoxystrobin and the cloransulam, comprises a weeding composition of the sulfuryl pyraoxystrobin and the cloransulam as active ingredients and a pesticide acceptable auxiliary agent; the mass ratio of cloransulam-methyl to the xaflufen-ethyl is 1: 1-1: 10.
The two effective components of the compound composition of the topramezone and the cloransulam-methyl have different mechanisms of action and different chemical structures, the indoor toxicity measurement is carried out on the compound composition of the topramezone and the cloransulam-methyl, piemarker is taken as a test object, and the result shows that after the topramezone and the cloransulam-methyl are compounded, compared with a single agent, the compound composition has an obvious synergistic effect on the prevention effect of the piemarker, and the cotoxicity coefficient is higher than 120 within the range of 1: 1-1: 10. In a specific embodiment of the invention, the mass ratio of cloransulam-methyl to pyriftalid is 1:1, 1:3, 1:5, 1:7 or 1: 10.
Preferably, the herbicidal composition comprises 20% to 60%, preferably 30% to 60% by weight of the total composition. In particular embodiments of the invention, the herbicidal composition comprises 20%, 24%, 30%, 40%, 45%, 48%, 50%, 56% or 60% of the total weight.
Preferably, the auxiliary agent in the water dispersible granule is selected from a dispersing agent, a wetting agent, a thickening agent, an antifoaming agent, an antifreezing agent, a preservative and deionized water. Wherein, the auxiliary agent comprises 2-12% of dispersant, 2-6% of wetting agent, 0.1-1% of thickening agent, 0.05-0.5% of defoaming agent, 2-6% of antifreezing agent, 0.05-0.2% of preservative and the balance of deionized water to 100% by weight.
The embodiment of the invention aims at the characteristics of the active ingredients of the medicine: the raw pesticide of the pyriftalid is white solid, and the water distribution coefficient of n-octanol/water is as follows: logP 2.39 (pH: 8.7, 25 ℃), cloransulam technical as a white solid, solubility (mg/L, 25 ℃): in water 3(pH5 buffer), 184(pH7 buffer), 3430(pH9 buffer), density: 1.538g/cm3N-octanol/water partition coefficient: the logP is 1.12(25 ℃), wherein, cloransulam-methyl has higher solubility and density in water, the two kinds of mixing are difficult to prepare into suspending agents, and the raw drug particles are easy to aggregate and flocculate in a suspension dispersion system. The inventors have studied and screened the adjuvants for their suspending agents by wettingThe selection and matching of the suspending agent and the dispersing agent obtain a preferable suspending agent formulation and an auxiliary agent system, so that the suspending agent has better lasting foamability, residue after pouring, and suspension rate and appearance before and after heat storage.
Further, the suspending agent preferably comprises the following components in percentage by weight: 30-60% of active ingredients of the medicine, 4-8% of dispersing agent, 3-5% of wetting agent, 0.2-0.8% of thickening agent, 0.1-0.5% of defoaming agent, 3-5% of antifreezing agent, 0.1-0.15% of preservative and the balance of deionized water to 100%.
Furthermore, the suspending agent preferably comprises the following components in percentage by weight: 48 percent of active pharmaceutical ingredients, 6 percent of dispersant, 4 percent of wetting agent, 0.5 percent of thickening agent, 0.4 percent of defoaming agent, 5 percent of antifreezing agent, 0.1 percent of preservative, and the balance of deionized water to 100 percent
For the selection of the auxiliary agent of the suspending agent, the dispersing agent is preferably one or more of tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, lignosulfonate, styrene acrylic acid copolymer, alkyl naphthalene sulfonate formaldehyde condensate and tristyrylphenol polyoxyethylene ether sulfate ammonium salt, and more preferably the dispersing agent is formed by mixing tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt and styrene acrylic acid copolymer according to the weight ratio of 1-3: 1. In the specific embodiment of the invention, the tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt is further selected from TRST of Ningbydi, the styrene acrylic copolymer is further selected from Agrilan788 of Acksotrey, and the product performance with the best dispersion suspension rate effect can be realized by matching TRST and Agrilan 788.
Further, in the suspending agent, the wetting agent is one or more of fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether, lauryl fatty alcohol polyoxyethylene ether and propylene oxide-ethylene oxide block polyether; preferably prepared by mixing propylene oxide-ethylene oxide block polyether and fatty alcohol polyoxyethylene polyoxypropylene ether according to the weight ratio of 1: 2-4. In the specific embodiment of the invention, the propylene oxide-ethylene oxide block polyether is further selected from PE6400 of Pasteur, the fatty alcohol polyoxyethylene polyoxypropylene ether is further selected from LBC-2 of Lanbo of Shijiazhuang, and the PE6400 and LBC-2 are matched to realize the best wetting and foaming effects of the solid technical during shearing dispersion and sanding, and the product can be well wetted and spread on the leaf surfaces of crops when being mixed with water for spraying.
Further, in the above suspending agent, the thickener is one or more of methylcellulose, organobentonite, xanthan gum and sodium polyacrylate, and xanthan gum is preferred.
In the suspending agent, the defoaming agent is one or more of silicone oil, saturated fatty acid (preferably C10-20 saturated fatty acid compounds) and fatty alcohol (preferably C8-10 fatty alcohol compounds), and silicone oil is preferred.
In the above suspending agent, the antifreeze is a polyhydric alcohol, preferably one or more of ethylene glycol, propylene glycol and glycerol, and more preferably glycerol. The present invention also unexpectedly discovered the effect of antifreeze on the anti-skinning and water loss of the suspension, which was not previously mentioned in other prior art, during the optimization of antifreeze, which had the lowest water loss and the most desirable performance of anti-skinning with the optimal glycerol antifreeze selection of the present invention.
Further, in the above suspending agent, the preservative is one or more of paraformaldehyde, sodium benzoate and cason, preferably cason.
In some preferred embodiments of the present application, in the suspension formulation, the dispersant is a mixture of tristyrene phenol polyoxyethylene ether phosphate triethanolamine salt and styrene acrylic acid copolymer at a weight ratio of 1-3: 1; the wetting agent is formed by mixing epoxypropane-ethylene oxide block polyether and fatty alcohol polyoxyethylene polyoxypropylene ether according to the weight ratio of 1: 2-4; the thickening agent is xanthan gum; the defoaming agent is silicone oil; the antifreezing agent is glycerol; the preservative is cason.
The embodiment of the invention also provides a preparation method of the suspending agent, which comprises the following steps:
(1) shearing water, a dispersing agent, a wetting agent, a defoaming agent and a preservative at a high speed, and uniformly mixing;
(2) adding the active ingredients of the medicine, namely the sulfurpyraflufen and the cloransulam, into the mixture obtained in the step (1), and sanding the mixture by using a sand mill until the particle size of the product is below 4 mu m;
(3) and (3) adding a thickening agent into an antifreezing agent, uniformly mixing, adding the thickening agent into the liquid mixture after sanding in the step (2), and carrying out high-speed shearing and uniform mixing to obtain the suspending agent containing the active ingredient.
The beneficial effects of the invention include:
1. the active ingredients of the herbicide, namely the sultopyrazole and the cloransulam-methyl, belong to two herbicides with different action mechanisms, and the two herbicides are mutually mixed without conflict, so that the weeding spectrum is expanded, and the weeding efficiency is improved.
2. The active ingredients of the herbicide have good synergistic effect in a certain mass ratio range, the control effect is higher than that of a single agent, the dosage is small, the generation of drug resistance of weeds is delayed, and the environment sustainable development is facilitated.
3. The invention optimizes the types and the contents of the auxiliary agents, and prepares the sultopyrazole and the cloransulam-methyl into the suspending agent, so that the suspending agent has better lasting foamability, residue after pouring, suspension rate and appearance before and after hot storage, and the weeding effect of the suspending agent can be improved.
Detailed Description
The invention discloses a suspending agent of pyraflufen-ethyl and cloransulam, a preparation method and application thereof, and a person skilled in the art can realize the suspending agent by properly improving process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the suspending agents and methods of making and using the same of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the suspending agents and methods of making and using the same described herein may be made and used without departing from the spirit, scope and spirit of the invention.
The suspending agent can be applied to annual and perennial weeds in soybean fields, and the weeds can be large crabgrass, cockspur grass, dayflower, piemarker, glechoma, endive and the like.
The suspension agent of the topramezone and the cloransulam-methyl provided by the invention, the preparation method and the application thereof are further explained below.
Example 1: indoor toxicity assay
The joint action mode of the binary herbicides is evaluated according to a Sun Yunpei co-toxicity coefficient method, the co-toxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion is determined, the CTC is less than 80 and is antagonistic, the CTC is more than or equal to 80 and is less than or equal to 120 and is additive, and the CTC is more than or equal to 120 and is synergistic.
The indoor toxicity assay was as follows:
the test agents were provided by Shandong Weifang Runfeng Feng chemical company Limited.
And (3) experimental design: after the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated with a series of concentrations according to the content of effective components, and clear water is used for comparison. The test material is cultured in a climatic chamber at a temperature of 25-35 ℃. Sowing a certain amount of piemarker seeds into a plastic basin with the diameter of 9cm, covering soil for 1-2 mm, putting the piemarker seeds into an enamel tray filled with water, allowing the water to gradually permeate, spraying the liquid medicine when the piemarker grows to 2-4 leaves, and transferring the liquid medicine into a phytotron for later use after treatment. Weighing the fresh weight of the aerial parts of the treated weeds 30 days after application, and calculating the fresh weight control effect and ED50And the co-toxicity coefficient is obtained by the method for calculating the co-toxicity proposed by Sun Yunpei et al.
The calculation formula is as follows (taking cloransulam-methyl as a standard medicament, the toxicity index is 100);
Figure BDA0002854349880000051
Figure BDA0002854349880000052
theoretical virulence index (TTI) of M-cloransulam-methyl TI XPCloransulam-methyl+ Sulfuron pyrazoxazoleTI×PSulfoxaden
Figure BDA0002854349880000053
In the formula: m is a mixture of cloransulam-methyl and pyraflufen-ethyl in different proportions;
Pcloransulam-methylIs the proportion of cloransulam-methyl in the mixture;
PsulfoxadenIs the proportion of the sultopyrazole in the mixture.
The test results are shown in table 1:
TABLE 1 measurement of the Activity of Sulfoxaden and cloransulam under different formulation ratios to Abutilon
Figure BDA0002854349880000061
As can be seen from the above table, ED of cloransulam-methyl, pyriftalid against abutilon50Are respectively 10.25g a.i/hm2And 22.52g a.i/hm2. The mixture ratio of cloransulam-methyl to the xaflufen-ethyl is 1:15, the cotoxicity coefficient is 92.09, is more than 80 but less than 120, and the cloransulam-methyl and the xaflufen-ethyl are shown to be additive; the co-toxicity coefficients of the mixture ratio of 1:1, 1:3, 1:5, 1:7 and 1:10 are respectively 122.93, 133.25, 141.15, 134.75 and 121.20 which are all larger than 120, and the synergistic effect is shown, wherein the synergistic effect is highest when the mixture ratio of cloransulam-methyl and the topramezone is 1: 5.
Example 2: 24% sulfonylpyraflufen-cloransulam suspension
The formula is as follows: the active ingredients of the medicine are 16 percent of the sulfurpyraflufen, 8 percent of cloransulam, 2 percent of the dispersant TRST, 7882 percent of Agrilan, 64001 percent of the wetting agent PE, LBC-22 percent, 0.8 percent of the thickening agent xanthan gum, 0.1 percent of the defoaming agent silicone oil, 3 percent of the antifreezing agent glycerol, 0.12 percent of the preservative Kathon and 100 percent of deionized water.
The preparation method comprises the following steps: shearing the dispersing agent, the wetting agent, the defoaming agent, the preservative and the water in the formula at a high speed, uniformly mixing, then adding the pyraflufen-ethyl sulfone and the cloransulam, and sanding in a sand mill, wherein the grain size of the material needs to be detected frequently during sanding, and the grain size is 2-4 mu m after sanding; adding the thickening agent into the antifreezing agent, uniformly mixing, then adding the mixture of the thickening agent and the antifreezing agent into the liquid mixture after sanding, and uniformly mixing by high-speed shearing to obtain the 24% sulfuryl pyraflufen-cloransulam suspending agent product.
Example 3: 20% sulfonylpyraflufen-cloransulam suspension
The formula is as follows: 15% of the active pharmaceutical ingredients of the topramezone, 5% of cloransulam, 3% of the dispersant TRST, 7882% of Agrilan, 64001% of the wetting agent PE, LBC-22%, 0.8% of the thickening agent xanthan gum, 0.2% of the defoaming agent silicone oil, 4% of the antifreezing agent glycerol, 0.1% of the preservative Kathon and 100% of deionized water.
The preparation method is the same as example 2.
Example 4: 60% suspension concentrate of pyraflufen-ethyl cloransulam
The formula is as follows: 50% of the active pharmaceutical ingredients of the topramezone, 10% of cloransulam, 6% of a dispersant TRST, 7882% of Agrilan, 64001% of a wetting agent PE, LBC-24%, 0.5% of a thickening agent xanthan gum, 0.4% of a defoaming agent silicone oil, 5% of an antifreezing agent glycerol, 0.1% of a preservative Kathon and 100% of deionized water.
The preparation method is the same as example 2.
Example 5: 48% suspension concentrate of pyraflufen-ethyl cloransulam
The formula is as follows: 42 percent of the active ingredients of the medicine, namely the topramezone, 6 percent of cloransulam, 4 percent of the dispersant TRST, 7883 percent of Agrilan, 64001 percent of the wetting agent PE, 23 percent of LBC, 0.4 percent of the thickening agent xanthan gum, 0.3 percent of the defoaming agent silicone oil, 4 percent of the antifreezing agent glycerol, 0.15 percent of the preservative Kathon and 100 percent of deionized water.
The preparation method is the same as example 2.
Example 6: 50% suspension concentrate of Sulfoxaden-cloransulam-methyl
The formula is as follows: 45% of the active pharmaceutical ingredients of the topramezone, 5% of cloransulam, 4% of a dispersant TRST, 7882% of Agrilan, 64001% of a wetting agent PE, LBC-22%, 0.4% of a thickening agent xanthan gum, 0.5% of a defoaming agent silicone oil, 4% of an antifreezing agent glycerol, 0.1% of a preservative Kathon and 100% of deionized water.
The preparation method is the same as example 2.
Example 7: 30% pyraflufen-ethyl cloransulam suspension
The formula is as follows: the active ingredients of the medicine are 15% of Sulfopyrazole, 15% of cloransulam, 1% of dispersant lignosulfonate, 7881% of Agrilan, 1% of wetting agent fatty alcohol-polyoxyethylene ether, 1% of PE 64001%, 1% of thickening agent methyl cellulose, 0.05% of defoamer C10-20 saturated fatty acid compound, 2% of antifreeze propylene glycol, 0.05% of preservative paraformaldehyde and 100% of deionized water.
The preparation method is the same as example 2.
Example 8: 45% suspension concentrate of pyraflufen-ethyl cloransulam
The formula is as follows: 30% of the active pharmaceutical ingredients of the topramezone, 15% of cloransulam-methyl, 4% of a dispersant alkyl naphthalene sulfonate formaldehyde condensate, 2% of TRST, 1% of a wetting agent lauryl fatty alcohol polyoxyethylene ether, 1% of LBC-22%, 0.8% of a thickening agent organic bentonite, 0.1% of a defoaming agent C8-10 fatty alcohol compound, 4% of an antifreezing agent propylene glycol, 0.05% of a preservative paraformaldehyde and deionized water to make up to 100%.
The preparation method is the same as example 2.
Example 9: 40% pyraflufen-ethyl cloransulam suspension
The formula is as follows: 30% of the active pharmaceutical ingredients of the topramezone, 10% of cloransulam-methyl, 5% of dispersing agent tristyrylphenol polyoxyethylene ether sulfate ammonium salt, 7883% of Agrilan, 1% of wetting agent lauryl fatty alcohol polyoxyethylene ether, 3% of fatty alcohol polyoxyethylene ether, 0.6% of thickening agent sodium polyacrylate, 0.2% of defoaming agent C8-10 fatty alcohol compounds, 6% of antifreezing agent propylene glycol, 0.2% of preservative Kathon and the balance of deionized water to 100%.
The preparation method is the same as example 2.
Example 10: 48% suspension concentrate of pyraflufen-ethyl cloransulam
The formula is as follows: 40% of the active ingredients of the medicine, namely the topramezone, 8% of cloransulam-methyl, 7% of dispersant, namely tristyrylphenol polyoxyethylene ether sulfate ammonium salt, 3% of TRST, 1% of wetting agent, namely lauryl fatty alcohol polyoxyethylene ether, 64003%, 0.1% of thickening agent, namely xanthan gum, 0.5% of defoaming agent silicone oil, 4% of antifreezing agent ethylene glycol, 0.15% of preservative sodium benzoate and 100% of deionized water.
The preparation method is the same as example 2.
Example 11: 56% sulfonylpyraflufen-cloransulam suspension
The formula is as follows: the active ingredients of the medicine are 48 percent of the sulfuryl pyraflufen, 8 percent of cloransulam, 7886 percent of dispersant Agrilan, 3 percent of TRST, 1 percent of wetting agent lauryl fatty alcohol polyoxyethylene ether, 1 percent of LBC-22 percent, 0.1 percent of thickening agent xanthan gum, 0.5 percent of defoaming agent C10-20 saturated fatty acid compound, 4 percent of antifreezing agent glycerol, 0.1 percent of preservative paraformaldehyde and 100 percent of deionized water.
The preparation method is the same as example 2.
Example 12: 60% suspension concentrate of pyraflufen-ethyl cloransulam
The formula is as follows: 54 percent of the active ingredients of the medicine, namely, 54 percent of the topramezone, 6 percent of cloransulam, 8 percent of the dispersant, 4 percent of TRST, 2 percent of wetting agent, namely fatty alcohol-polyoxyethylene ether, PE 64004 percent of the active ingredients, 0.05 percent of thickening agent xanthan gum, 0.3 percent of defoamer C10-20 saturated fatty acid compound, 5 percent of antifreeze propylene glycol, 0.12 percent of preservative paraformaldehyde and 100 percent of deionized water.
The preparation method is the same as example 2.
Example 13: 48% pyraflufen-ethyl cloransulam suspension
The formula is as follows: 40% of the active pharmaceutical ingredients of the topramezone, 8% of cloransulam, 3% of a dispersant alkyl naphthalene sulfonate formaldehyde condensate, 1% of an acrylic acid-maleic anhydride copolymer, 3% of a wetting agent alkylphenol polyoxyethylene ether, 4% of a polyoxyethylene ether phosphate salt, 0.5% of a thickener xanthan gum, 0.3% of a defoamer C10-20 saturated fatty acid compound, 5% of an antifreeze glycol, 0.1% of a preservative paraformaldehyde and 100% of deionized water.
The preparation method is the same as example 2.
Example 14: suspension product testing
The properties of the products obtained in the above examples were measured and the results are shown in Table 2 below. The suspension rate is detected according to a GB/T14825-2006 pesticide suspension rate measuring method, the pourability is detected according to a GB/T31737-2015 pesticide pourability measuring method, and the lasting foamability is written according to HG/T2467.5-2003 pesticide suspension product standard: 4.11 the determination method of the long-lasting foamability test is used for detection, and the heat storage stability is determined according to the determination method of the heat storage stability of the GB/T19136-2003 pesticide.
The suspending agent products prepared in the examples are added with different antifreezing agents (ethylene glycol, propylene glycol and glycerol), culture dishes with the diameter of 9cm are selected, 50g of materials are added into each dish, and the dishes are placed in a constant temperature box (25 ℃) in an open mode for 24 hours to measure the water loss and the skinning conditions of the materials. The results are shown in Table 3.
TABLE 2 quality of suspension product prepared by compounding pyraflufen-ethyl and cloransulam-methyl
Figure BDA0002854349880000091
Figure BDA0002854349880000101
TABLE 3 Sulfoxaden and cloransulam-methyl compounding to make anti-caking situation for suspension agent product
Figure BDA0002854349880000102
Figure BDA0002854349880000111
It can be seen from table 2 that, in example 13, compared with the previous examples, the suspension percentage, the foaming property and the heat storage stability are poor, which shows that the selection of the auxiliary agent has an important influence on the performance of the suspending agent, and the invention improves the performance of the suspending agent through the screening of the auxiliary agent and the content. The suspending agents of examples 7-11 were slightly inferior in quality after heat storage, while the suspending agents of examples 2-6 using the preferred adjuvants were good in quality both before and after heat storage, indicating that the selection of the preferred adjuvants improved the performance of the suspending agents.
As can be seen from Table 3, the material state of the example using the preferred antifreeze, glycerin, is significantly better than that of other antifreeze, and the preferred antifreeze not only has an antifreezing effect but also has a moisturizing and anti-skinning effect.
Furthermore, as can be seen from examples 2-6, in the case of the selection of preferred adjuvants, the performance of the resulting suspension concentrate is similar when the content of the pharmaceutically active ingredient varies within the range of 20-60%, which means that the effect of the drug content on the performance of the dosage form is less with the preferred adjuvant ingredients and contents. From examples 7 to 11, it can be seen that the suspension concentrate obtained has relatively poor performance and no significant improvement in the replacement of the auxiliary agent is observed in the case of the conventional auxiliary agent, which indicates that the components and contents of the preferred auxiliary agent have significant effect on improving the performance of the suspension concentrate containing pyriftalid cloransulam-methyl, which is absent in the conventional auxiliary agent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (12)

1. The suspending agent of the pyraflufen-ethyl and the cloransulam is characterized by comprising a herbicidal composition of the pyraflufen-ethyl and the cloransulam as active ingredients and an auxiliary agent acceptable to pesticides; the mass ratio of cloransulam-methyl to the xaflufen-ethyl is 1: 1-1: 10.
2. The suspension concentrate of claim 1, wherein the herbicidal composition comprises from about 20% to about 60% by weight.
3. The suspension concentrate of claim 1, wherein the adjuvant is selected from the group consisting of dispersants, wetting agents, thickeners, defoamers, antifreeze, preservatives, and deionized water.
4. The suspension concentrate as claimed in claim 3, wherein the weight percentage of the auxiliary agent is 2-12% of dispersing agent, 2-6% of wetting agent, 0.1-1% of thickening agent, 0.05-0.5% of defoaming agent, 2-6% of antifreezing agent, 0.05-0.2% of preservative, and the balance of deionized water to 100%.
5. The suspension according to claim 3 or 4, wherein the dispersant is one or more selected from the group consisting of tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, lignosulfonate, styrene acrylic acid copolymer, alkylnaphthalenesulfonate formaldehyde condensate, tristyrylphenol polyoxyethylene ether sulfate ammonium salt.
6. The suspending agent according to claim 3 or 4, wherein the wetting agent is one or more selected from fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether, lauryl fatty alcohol polyoxyethylene ether and propylene oxide-ethylene oxide block polyether.
7. The suspension concentrate according to claim 3 or 4, wherein the thickener is one or more of methylcellulose, organobentonite, xanthan gum and sodium polyacrylate.
8. The suspension according to claim 3 or 4, wherein the defoaming agent is one or more of silicone oil, saturated fatty acid and fatty alcohol.
9. A suspension concentrate according to claim 3 or 4, characterized in that the anti-freezing agent is a polyol, preferably one or more of ethylene glycol, propylene glycol and glycerol.
10. A suspension concentrate as claimed in claim 3 or 4 wherein the preservative is one or more of paraformaldehyde, sodium benzoate and cason.
11. Use of a suspension according to any of claims 1 to 10 for controlling crop weeds and for the preparation of a pesticide formulation for controlling crop weeds.
12. A process for preparing a suspension formulation as claimed in claim 3, which comprises:
(1) shearing water, a dispersing agent, a wetting agent, a defoaming agent and a preservative at a high speed, and uniformly mixing;
(2) adding the active ingredients of the sulphone pyraoxystrobin and cloransulam to the mixture obtained in the step (1), and sanding;
(3) and (3) adding a thickening agent into an antifreezing agent, uniformly mixing, adding the thickening agent into the liquid mixture after sanding in the step (2), and carrying out high-speed shearing and uniform mixing to obtain the suspending agent.
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CN115363040A (en) * 2022-08-31 2022-11-22 山东润博生物科技有限公司 Suspending agent containing topramezone and amicarbazone and preparation method thereof
CN115777700A (en) * 2022-11-30 2023-03-14 山东润博生物科技有限公司 Suspending agent containing metribuzin and topramezone and preparation method thereof

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CN109526973A (en) * 2018-12-14 2019-03-29 青岛清原化合物有限公司 Ternary weeding composition and its application comprising sulfone pyrrole grass azoles

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN109526973A (en) * 2018-12-14 2019-03-29 青岛清原化合物有限公司 Ternary weeding composition and its application comprising sulfone pyrrole grass azoles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115363040A (en) * 2022-08-31 2022-11-22 山东润博生物科技有限公司 Suspending agent containing topramezone and amicarbazone and preparation method thereof
CN115777700A (en) * 2022-11-30 2023-03-14 山东润博生物科技有限公司 Suspending agent containing metribuzin and topramezone and preparation method thereof

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