A seed treatment suspension concentrate, its preparation method and application

Abstract

The present application relates to the field of pesticides, more particularly, the present application relates to a kind of seed treatment suspending agent and its preparation method and application.The preparation raw material of the suspending agent includes 5-15% active ingredient, 0.01-20% auxiliary agent and the rest water by weight percentage.The present application provides a kind of seed treatment suspending agent, by using the thiamethoxam, the diafenthiuron and the active ingredient of triadimefon and triadimefon three kinds of active ingredient compound, the suspending agent prepared has good internal absorption, is applied to crop seed and can be quickly absorbed by root or just germinated seedling, is conducive to the prevention and treatment of a variety of pests and diseases, and promote the growth of crops, especially for the control of peanut grub and white thread disease, aphid and wheat sharp eyesight disease has remarkable effect.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of pesticides, and more particularly, to a seed treatment suspension concentrate and a preparation method and application thereof. BACKGROUND

[0002] Peanut and wheat are important economic crops and play an important role in the world agricultural production. However, the growth of peanut and wheat is harmed by various pests and pathogens, such as peanut grub and white mould, aphids and wheat sharp eyespot, which seriously affect the yield and quality of peanut and wheat. At present, the prevention and treatment of these pests and diseases is widely used in peanut production by treating seeds with pesticides during sowing due to the advantages of time-saving, labor-saving, easy operation and effective control of pests. However, there are various pesticides for seed dressing on the market, and improper selection or dosage of pesticides will cause physiological harm to seeds, resulting in reduced emergence rate and inhibited seedling growth. In addition, the climate and ecological conditions are quite different in different peanut planting areas, which affects the safety of pesticide treatment. Therefore, it is necessary to develop a seed treatment suspension concentrate which can effectively prevent and treat pests and diseases of crops such as peanut and wheat. SUMMARY

[0003] To solve the above problems, the present application provides a seed treatment suspension concentrate, and the preparation raw materials of the suspension concentrate comprise, by weight percentage, 5-15% active ingredient, 0.01-20% auxiliary agent and the balance water.

[0004] As a preferred technical solution of the present application, the active ingredient is selected from one or more of guanidinoalkyl pyridine, guanidinoalkyl pyridine, imidacloprid, myclobutanil, validamycin, pymetrozine, deltamethrin, chlorpyrifos, buprozin, dichlorvos, thiodicarb, difenoconazole, clothianidin, thiamethoxam, fludioxonil, pyraclostrobin, fipronil, captan, pyracarbolid, carpropamid, flutriafol, thiabendazole, oxadixyl, cypermethrin, metalaxyl, thiodicarb, mefenoxam, thiram, quintozene, captan, phorate, fenobucarb.

[0005] As a preferred technical solution of the present application, the active ingredient comprises clothianidin and carpropamid, and the weight ratio of clothianidin to carpropamid is 1:(0.1-0.2).

[0006] As a preferred technical solution of the present application, the active ingredient further comprises difenoconazole, and the weight ratio of clothianidin to difenoconazole is 1:(0.04-0.06).

[0007] As a preferred technical solution of the present application, the auxiliary agent comprises a film-forming agent, a dispersing agent, a thickening agent, an antifreezing agent, an antifoaming agent and a warning color.

[0008] As a preferred technical solution of the present application, the film forming agent is selected from one or more of attapulgite, acrylic resin modified casein film forming agent, chitosan, acrylic resin polyurethane copolymer resin, acrylate modified butadiene resin, polyurethane modified nitric fiber, polyvinyl alcohol, polyethylene glycol, and polyvinyl acetate.

[0009] The second aspect of the present application provides a preparation method of the seed treatment suspension agent as described above, comprising the following steps:

[0010] After mixing, sand grinding the active ingredient, dispersant, defoaming agent and water, the remaining preparation raw materials are added and mixed to obtain the seed treatment suspension agent.

[0011] The third aspect of the present application provides the use of the seed treatment suspension agent as described above, which is applied to prevent and control diseases and / or insect pests of crops.

[0012] As a preferred technical solution of the present application, the crop is selected from one or more of rice, corn, peanut, wheat, cotton, oilseed rape, potato, radish, cabbage, sorghum, and soybean.

[0013] As a preferred technical solution of the present application, the disease is selected from one or more of sheath blight, white rot, bacterial wilt, root knot nematode disease, scab, stem rust, leaf rust, stripe rust, downy mildew, anthracnose, goss's bacterial wilt, smut, root rot, yellow dwarf, bunchy top, black leaf sheath disease, bacterial leaf spot, cotton leaf curl virus disease, and cyst nematode disease; the insect pest is selected from one or more of grub, leaf beetle, wireworm, cutworm, aphid, planthopper, whitefly, leafhopper, and cotton bollworm.

[0014] Compared with the prior art, the present application has the following beneficial effects: the present application provides a seed treatment suspension agent, which is prepared by compounding thiamethoxam, difenoconazole and carboxin as three active ingredients, and has good systemicity, can be quickly absorbed by the root or seedling of the crop after being applied to the seed of the crop, is conducive to preventing and controlling various insect pests and diseases, and promotes the growth of the crop, especially has significant effects on preventing and controlling the grub and white rot of peanut, the aphid and sheath blight of wheat; in addition, the applicant selects appropriate adjuvants, which is conducive to promoting the dispersion of the active ingredient, increasing the heat storage stability and room temperature storage stability of the suspension agent, and the suspension agent prepared has good adsorption performance and film forming uniformity when used for seed treatment, and is conducive to the absorption of the active ingredient by the seed. DETAILED DESCRIPTION

[0015] The present application can be more easily understood and further advantages and benefits will become more apparent upon consideration of the following detailed description and the accompanying drawings, in which:

[0016] The term "comprising" as used herein is synonymous with "including", "containing", "characterized by" or "characterized in that", and is inclusive or open-ended and does not exclude additional, unrecited elements or method steps. The term "comprising" as used herein is also synonymous with "by means of" or "comprised of". The term "consisting of" is a closed term that excludes any element, step, or ingredient not specified. If used in a claim, this phrase will make the claim closed, meaning that it excludes any material not specified, except for normal impurities that are associated with the specified materials. When the phrase "consisting of is placed after the preamble of a claim, it limits the claim to the elements described in that clause; other elements are not excluded from the claim as a whole.

[0017] The term "consisting of is a closed term that excludes any element, step, or ingredient not specified. If used in a claim, this phrase will make the claim closed, meaning that it excludes any material not specified, except for normal impurities that are associated with the specified materials. When the phrase "consisting of is placed after the preamble of a claim, it limits the claim to the elements described in that clause; other elements are not excluded from the claim as a whole.

[0018] When equivalent, concentration, or other values or parameters are expressed in ranges, preferred ranges, or a series of upper preferred values and lower preferred values, it is to be understood that all ranges formed by any pair of any upper range limit or preferred value and any lower range limit or preferred value, even if the range is not explicitly disclosed, are to be specifically disclosed. For example, where a range of "1 to 5" is disclosed, the described range is to be interpreted to include ranges of "1 to 4," "1 to 3," "1 to 2," "1 to 2 and 4 to 5," "1 to 3 and 5," etc. When numerical ranges are disclosed, unless otherwise stated, the range is intended to include both the upper and lower values and all intervening values, including integers and fractions, unless the context clearly indicates otherwise.

[0019] The singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. "Optional" or "any of" means that the subsequently described event or circumstance can or can not occur, and that the description includes instances where the event occurs and instances where it does not.

[0020] Approximating language in the specification and claims can be applied as "substantially", "approximately", and / or "about" plus or minus a reasonable range of error for the numbers recited therein (e.g., 10% of the recited value) unless otherwise indicated. Ranges of values and / or amounts are provided as approximations, and the end points of the ranges of values and / or amounts are included. Accordingly, the application is not intended to be limited to the values presented in the claim or specification, but rather the definition is meant to be flexible to accommodate reasonable equivalents. Various embodiments of the application are described herein. These and other embodiments of the application can each optionally include one or more of the following features.

[0021] In addition, the indefinite articles "a" and "an" preceding the elements and components of the application are intended to be construed to be inclusive (i.e., the phrases "a" and "an" should be interpreted to mean "at least one" or "one or more") unless otherwise indicated as used in connection with the description herein. As used herein, the notation "a" or "an" should be construed to mean "at least one" or "one or more" unless otherwise indicated.

[0022] The application is hereinafter described by way of specific embodiments, but is not limited to the specific embodiments given herein.

[0023] The first aspect of the application provides a seed treatment suspension concentrate, the raw materials for preparing the suspension concentrate comprising, by weight percentage, 5-15% active ingredient, 0.01-20% adjuvant and the balance water.

[0024] In a preferred embodiment, the raw materials for preparing the suspension concentrate of the application comprise, by weight percentage, 12% active ingredient, 10.6% adjuvant and the balance water.

[0025]

Active ingredient

[0026] In an embodiment, the active ingredient of the application is selected from one or more of guanido, guanido, imidacloprid, carbendazim, validamycin, pymetrozine, deltamethrin, chlorpyrifos, buprofezin, dichlorvos, thiodicarb, difenoconazole, clothianidin, thiamethoxam, fludioxonil, pyraclostrobin, fipronil, anilofos, pyrimethanil, carboxin, fluazinam, chlorothalonil, metalaxyl, thiodicarb, mefenoxam, thiram, quintozene, captan, phorate, fenobucarb.

[0027] Preferably, the active ingredient of the application comprises clothianidin and carboxin in a weight ratio of 1:(0.1-0.2).

[0028] More preferably, the active ingredient of the application comprises clothianidin and carboxin in a weight ratio of 1:0.15.

[0029] clothianidin

[0030] Thiamethoxam, chemical name (E)-1-(2-chloro-1, 3-thiazole-5-ylmethyl)-3-methyl-2-2-nitroguanidine, is a new insecticide in neonicotinoids, which is a new type of insecticide with high safety and high selectivity, and its action is similar to that of nicotine acetylcholine receptor, with contact, stomach poison and systemic activity. It is mainly used for rice, vegetables, fruit trees and other crops to prevent and control aphids, leafhoppers, thrips, planthoppers and other hemiptera, coleoptera, diptera and some lepidoptera pests. It has the advantages of high efficiency, broad spectrum, low dosage, low toxicity, long effective period, no drug damage to crops, safety in use, no cross resistance with conventional pesticides, excellent systemic and penetration, and is another variety to replace highly toxic organophosphorus pesticides. Its structure is novel and special, and its performance is more excellent than that of traditional nicotine insecticides, and it may become a world-class insecticide.

[0031] In a preferred embodiment, the thiamethoxam of the present application is purchased from Zhongnong Lihua Biotechnology Co., Ltd.

[0032] carboxin

[0033] Carboxin, Chinese alias 5, 6-dihydro-2-methyl-N-phenyl-1, 4-oxathiepin-3-carboxamide, is a heterocyclic fungicide with systemic action. The pure product is white needle-like crystal. It is difficult to dissolve in water, but can be dissolved in organic solvents such as methanol, acetone, benzene and the like. It can be used to prevent and control sorghum head smut and other cereal head smut, and can also be used to prevent and control wheat rust, cotton disease, millet white hair disease and the like.

[0034] In a preferred embodiment, the carboxin of the present application is purchased from Zhongnong Lihua Biotechnology Co., Ltd.

[0035] In an embodiment, the active ingredient of the present application further comprises difenoconazole, and the weight ratio of thiamethoxam to difenoconazole is 1: (0.04-0.06).

[0036] Preferably, the weight ratio of thiamethoxam to difenoconazole in the present application is 1:0.05.

[0037] difenoconazole

[0038] Difenoconazole, chemical name: cis, trans-3-chloro-4-[4-methyl-2-1H-1, 2, 4-triazole-1-ylmethyl)-1, 3-dioxan-2-yl) phenyl 4-chlorophenyl ether, is a systemic fungicide with protective and curative effects. Difenoconazole is a triazole fungicide with relatively high safety, which is widely used in crops such as fruits and vegetables, and effectively prevents and controls black star disease, black pustule disease, white rot disease, spot and leaf fall disease, powdery mildew, brown spot disease, rust disease, stripe rust disease, and so on. The prevention and control objects have persistent protective and curative activities on Ascomycotina, Basidiomycotina, and semi-known fungi including Alternaria, Sphaerulina, Cercospora, Podosphaera, Guignardia, Phoma, Mycosphaerella, Septoria, Venturia, Erysipheae, Uredinales, and some species of pathogenic bacteria, and have good curative effects on sugar beet brown spot disease, wheat leaf blight, leaf blight, rust disease, and mildew caused by several pathogenic bacteria, apple black star disease, powdery mildew, grape powdery mildew, potato early blight, peanut leaf spot disease, net spot disease, and so on.

[0039] In a preferred embodiment, the difenoconazole of the present application is purchased from Zhongnong Lihua Biotechnology Co., Ltd.

[0040] The applicant finds that when using a pesticide product containing a single component such as a suspension concentrate, there are often defects in the prevention and control of crop diseases and insect pests, such as the development of drug resistance after continuous use, a narrow insecticidal spectrum, the inability to provide comprehensive protection for crops, and high drug costs. Through the combination of two or more active ingredients, the above-mentioned defects can be overcome to some extent. The applicant finds that when thiamethoxam, difenoconazole, and carboxin are used as active ingredients and the weight ratio is controlled, a synergistic effect can be achieved, the prevention and control effect can be improved, the amount of effective components used can be reduced, costs can be saved, the development of resistance to insect pests and diseases can be slowed down, the prevention and control spectrum can be expanded, and the growth of crops can be promoted. The combination can be used for the prevention and control of diseases and insect pests of various crops, especially the prevention and control of aphids and sharp eyespot of wheat, and the prevention and control of white rot and white leaf spot of peanuts. The applicant finds that when the weight ratio of thiamethoxam, difenoconazole, and carboxin is not 1:(0.04-0.06):(0.1-0.2), the prevention and control effect of diseases and insect pests is weakened.

[0041]

Adjuvant

[0042] Due to the different structures of the active ingredients thiamethoxam, difenoconazole, and carboxin, the water solubility is also different, so it is necessary to select appropriate adjuvants such as dispersants, thickeners, film formers, and the like, so that the prepared suspension concentrate has good stability and high adsorbability and film uniformity with seeds. In addition, in order to meet the requirements of the suspension concentrate during use or transportation, antifreeze, defoaming agent, and warning color can also be added.

[0043] In one embodiment, the adjuvant of the present application comprises a film-forming agent, a dispersing agent, a thickening agent, an anti-freezing agent, an antifoaming agent and a warning color.

[0044] Preferably, the adjuvant of the present application comprises 0.1-2 parts of a film-forming agent, 1-10 parts of a dispersing agent, 0.1-2 parts of a thickening agent, 0.01-4 parts of an anti-freezing agent, 0.01-1 part of an antifoaming agent and 0.1-2 parts of a warning color by weight.

[0045] More preferably, the adjuvant of the present application comprises 0.1-1 part of a film-forming agent, 6-9 parts of a dispersing agent, 0.1-1 part of a thickening agent, 0.01-4 parts of an anti-freezing agent, 0.01-1 part of an antifoaming agent and 0.1-2 parts of a warning color by weight.

[0046] Preferably, the adjuvant of the present application comprises 1 part of a film-forming agent, 6 parts of a dispersing agent, 0.5 part of a thickening agent, 2 parts of an anti-freezing agent, 0.1 part of an antifoaming agent and 1 part of a warning color by weight.

[0047] film-forming agent

[0048] The film-forming agent refers to a substance capable of forming a continuous film, which mainly plays a role of protecting seeds in the seed treatment suspension, and its decomposition rate determines the degree of nutrient absorption by plants in the seed coating agent. When used for seed treatment, the active ingredient can be adhered to the surface of the seed and form a continuous drug film.

[0049] In one embodiment, the film-forming agent of the present application is selected from one or more of attapulgite, acrylic resin modified casein film-forming agent, chitosan, acrylic resin polyurethane copolymer resin, acrylate modified butadiene resin, polyurethane modified nitric acid fiber, polyvinyl alcohol, polyethylene glycol and polyvinyl acetate.

[0050] Preferably, the film-forming agent of the present application is chitosan; further, the film-forming agent of the present application is modified chitosan.

[0051] More preferably, the raw materials for preparing the modified chitosan of the present application comprise sodium N-isostearyl methyl taurate, nano titanium dioxide and chitosan, and the weight ratio is (0.1-0.2):1:(40-60); further, the weight ratio of the sodium N-isostearyl methyl taurate, nano titanium dioxide and chitosan of the present application is 0.15:1:50.

[0052] The modified chitosan of the present application can be purchased or self-made. When self-made, it can be prepared by blending, which is a preparation method well known in the art. It should be noted that when the modified chitosan is used as a film-forming agent for the seed treatment suspension, the weight percentage of the modified chitosan in the seed treatment suspension is the weight percentage of the chitosan in the modified chitosan in the seed treatment suspension.

[0053] Further preferably, the preparation method of the modified chitosan according to the present application comprises the following steps:

[0054] The nano-titanium dioxide is added into water, and the pH is adjusted to 5-6, N-isostearyl methyl sodium taurate is added, and the reaction is carried out at 35-40℃ for 0.5-1h, and then dried to obtain the modified nano-titanium dioxide.

[0055] The modified nano-titanium dioxide is added into a glycerol and acetic acid solution, and chitosan is added, and then degassed by ultrasonic to obtain the modified chitosan.

[0056] The acetic acid solution according to the present application is an acetic acid solution with a volume fraction of 0.6%.

[0057] Further preferably, the nano-titanium dioxide according to the present application is purchased from Shanghai Superwe Nanometer Technology Co., Ltd.

[0058] The applicant found that, by using the modified chitosan as a film-forming agent, the suspension agent prepared is used for seed treatment, especially for wheat and peanut seed treatment, which is beneficial to improve the adsorption to the seeds, and can promote the absorption of the active ingredients by the seeds, which may be because, by using the modified nano-titanium dioxide to act on the chitosan, especially the N-isostearyl methyl sodium taurate modified nano-titanium dioxide and the chitosan, due to the strong force of the taurate in the N-isostearyl methyl sodium taurate and the hydroxyl groups on the surface of the nano-titanium dioxide and the chitosan, it is beneficial to improve the adsorption to the seeds, and due to the multiple hydroxyl groups of the modified chitosan, it is beneficial to form a strong three-dimensional cross-linked network to coat the active ingredients, prevent the active ingredients from falling off during the seed treatment and transportation process, further improve the adsorption, and due to the nano structure of the titanium dioxide and the branched long alkyl chain on the surface of the titanium dioxide, it is beneficial to adsorb and entangle the active ingredients into the seeds, promote the active ingredients to prevent the occurrence of pests and diseases.

[0059] However, the applicant found that, when the modified chitosan according to the present application is used, the adsorption capacity to the seeds is improved, but the film-forming uniformity is easily reduced, which may be because the large structure of the chitosan hinders the uniform distribution of the active ingredients, so that the film-forming uniformity is reduced.

[0060] dispersing agent

[0061] The dispersant is an interfacial active agent with both lipophilicity and hydrophilicity in the molecule. It can uniformly disperse inorganic, organic pigments, solid and liquid particles which are difficult to be dissolved in liquid, and can also prevent the particles from settling and agglomerating to form a stable suspension.

[0062] In one embodiment, the dispersant of the present application is selected from one or more of fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, hydroxyl polyethylene oxide block polymer, polycarboxylic acid ester, polyacrylic acid copolymer, alkyl phenol polyoxyethylene ether, alkyl phenyl ether sulfonate, polyoxyethylene ether phosphate, lignin sulfonate, sodium alkyl naphthalene sulfonate, methyl naphthalene sulfonic acid formaldehyde condensate sulfate, naphthalene sulfonic acid formaldehyde condensate, sodium methylene naphthalene sulfonate, formaldehyde condensate of dibutyl naphthalene sulfonic acid, sodium N-methyl fatty acyl taurate, alkyl phenol polyoxyethylene ether formaldehyde condensate sulfate, sodium polymeric carboxylic acid, alkyl phenol polyoxyethylene ether sulfate, tea dust, saponin, sulfurous acid paper pulp waste liquid, fatty alcohol sulfate, sodium dodecyl sulfonate, fatty amide-N-methyl taurate sodium salt, fatty alcohol polyoxyethylene ether sodium sulfate, block polyether, alkyl phenyl ether sulfonate, polyether phosphate, naphthalene sulfonate condensate, polycarboxylate, polystyrene phenyl ether phosphate, and fatty alcohol polyoxyethylene ether.

[0063] Preferably, the dispersant of the present application comprises polycarboxylate; further, the raw material for preparing the polycarboxylate of the present application comprises acrylic acid, acrylate, and acrylamide, in a molar ratio of (1-3):(0.5-1.5):(1-3); further, the molar ratio of the acrylic acid, acrylate, and acrylamide of the present application is 2:1:2.

[0064] More preferably, the acrylate of the present application is selected from one or more of ethyl acrylate, o-phenylphenoxyethyl acrylate (CAS No. 91442-24-9), 2-phenoxyethyl acrylate (CAS No. 48145-04-6); further, the acrylate of the present application is 2-phenoxyethyl acrylate.

[0065] Further preferably, the acrylamide of the present application is selected from one or more of sodium acrylamidodimethyl taurate, N-(3-dimethylamino)propyl-2-methyl-2-propenamide (CAS No. 5205-93-6), N-methyl(meth)acrylamide, N-ethyl(meth)acrylamide, N-propyl(meth)acrylamide, N-(butyl)(meth)acrylamide, N-tert-butyl(meth)acrylamide, N-pentyl(meth)acrylamide, N-hexyl(meth)acrylamide, N-heptyl(meth)acrylamide, N,N-dimethyl(meth)acrylamide, N,N-diethyl(meth)acrylamide, piperidinyl(meth)acrylamide, morpholinyl(meth)acrylamide, N-(N-butoxymethyl)acrylamide.

[0066] Further preferably, the acrylamide of the present application comprises sodium acryloyldimethyl taurate and N-(3-dimethylamino)propyl-2-methyl-2-propenamide in a weight ratio of (2-3):(2-3); further, the weight ratio of the sodium acryloyldimethyl taurate and N-(3-dimethylamino)propyl-2-methyl-2-propenamide of the present application is 1:1.

[0067] In a preferred embodiment, the preparation method of the polycarboxylate of the present application comprises the following steps:

[0068] The water and the initiator are mixed and heated to 60-70°C, and the acrylic acid, the acrylate and the acrylamide are added dropwise, after the dropwise addition is completed, the reaction is kept at constant temperature for 2-3h, cooled, the pH is adjusted to 7-8, dried to obtain the polycarboxylate.

[0069] The initiator of the present application is well known to those skilled in the art, and is not specifically limited, in an embodiment, the initiator of the present application is ammonium persulfate, and the ammonium persulfate accounts for 0.1-0.5wt% of the acrylic acid.

[0070] The applicant found that by adding the polycarboxylate of the present application, the dispersion of clothianidin, difenoconazole and carboxin is facilitated, and the aggregation among the three is prevented, and the normal temperature stability is improved, which may be because the polycarboxylate prepared by the reaction of acrylic acid, acrylate and acrylamide is an acrylic acid-acrylate and acrylamide copolymer, and the carboxylate ion of the acrylic acid is beneficial to form a strong interaction with the surface of the active ingredient, and when 2-phenoxyethyl acrylate is used as the acrylate, because its side chain contains a benzene ring structure, it is easy to interact with the conjugated electrons of the active ingredients such as difenoconazole and carboxin, thereby increasing the dispersibility of the poorly water-soluble difenoconazole and carboxin, forming a protective layer on the surface of the active ingredient, and the polycarboxylate has a negative charge, so that the active ingredients have electrostatic repulsion, preventing the aggregation of the active ingredients; and by using acrylamide, especially sodium acryloyldimethyl taurate and N-(3-dimethylamino)propyl-2-methyl-2-propenamide, the polycarboxylate prepared contains dimethyl taurine sodium and N-(3-dimethylamino)propyl-2-methyl as the hydrophilic segment of the polyacrylamide side group, when the active ingredient and the polyacrylic acid and polyacrylate segment of the polycarboxylate interact, the hydrophilic polyacrylamide segment tends to stretch in water, and the dimethyl taurine sodium side group can promote the water solubility of the active ingredient, while the long structure of the N-(3-dimethylamino)propyl-2-methyl side group is also beneficial to provide steric hindrance, thereby further promoting the dispersion of the active ingredient and improving the normal temperature storage stability.

[0071] In addition, the applicant surprisingly found that the polycarboxylate salt of the present application can improve the adsorption capacity of the seed and the film uniformity, and promote the absorption of the active ingredient by the seed, which can be due to the interaction between the polycarboxylate salt and the active ingredient, so that the active ingredient surface contains a protective layer formed by the polycarboxylate salt, wherein the protective layer includes polyacrylic acid and polyacrylate segments in contact with the surface of the active ingredient, and the outer polyamide hydrophilic segment, which can promote the adsorption of the seed and facilitate the adsorption of the active ingredient on the surface of the seed, and the amide bond in the polyamide can form a hydrogen bond with chitosan, participate in the film structure formed by chitosan and the seed, the strong polarity of the taurate in the dimethyl taurate sodium in the polyamide is easy to interact with the surface of the nano titanium dioxide, and the side chain of N-(3-dimethylamino) propyl-2-methyl is easy to entangle with the surface of N-isostearyl methyl taurate sodium, which can promote the absorption of the active ingredient by the seed, and also facilitate the dispersion of the active ingredient in the film structure, thereby promoting the dispersion uniformity.

[0072] However, the applicant found that although the addition of 2-phenoxyethyl acrylate as an acrylate can facilitate the dispersion of the active ingredient, the stability of the polycarboxylate salt prepared thereby can decrease when the temperature is relatively high, which can be due to the conjugated electron interaction between the benzene ring of 2-phenoxyethyl acrylate and the active ingredient, which can facilitate the formation of a protective layer between the polycarboxylate salt and the molecule, but the benzene ring in the polycarboxylate salt tends to be adsorbed on the surface of the active ingredient in a flat state, thereby making the protective layer formed thereby thinner, when the temperature is relatively high, the molecular motion increases, the probability of collision and aggregation of the active ingredient increases, thereby making the heat storage stability decrease.

[0073] In a more preferred embodiment, the dispersant of the present application further comprises a polyoxyethylene ether phosphate; further, the weight ratio of the polycarboxylate salt and the polyoxyethylene ether phosphate of the present application is 1:(0.2-0.4); further, the weight ratio of the polycarboxylate salt and the polyoxyethylene ether phosphate of the present application is 1:0.3.

[0074] In a further preferred embodiment, the polyoxyethylene ether phosphate of the present application is aryl polyoxyethylene ether phosphate and / or alkyl polyoxyethylene ether phosphate; further, the polyoxyethylene ether phosphate of the present application is aryl polyoxyethylene ether phosphate and alkyl polyoxyethylene ether phosphate, and the weight ratio is 1:(2-3); further, the weight ratio of the aryl polyoxyethylene ether phosphate and the alkyl polyoxyethylene ether phosphate of the present application is 1:2.

[0075] As examples of aryl polyoxyethylene ether phosphate, including but not limited to, nonylphenol polyoxyethylene ether phosphate, styryl phenol polyoxyethylene ether phosphate.

[0076] As examples of the alkyl polyoxyethylene ether phosphate, there are included, but not limited to, castor oil polyoxyethylene ether phosphate, isooctanol polyoxyethylene ether phosphate, oleyl alcohol polyoxyethylene ether phosphate, cetyl alcohol polyoxyethylene ether phosphate.

[0077] In a further preferred embodiment, the aryl polyoxyethylene ether phosphate of the present application is nonylphenol polyoxyethylene ether phosphate; further, the nonylphenol polyoxyethylene ether phosphate of the present application is purchased from Nantong Chenrun Chemical Co., Ltd.

[0078] In a further preferred embodiment, the alkyl polyoxyethylene ether phosphate of the present application is isooctanol polyoxyethylene ether phosphate; further, the isooctanol polyoxyethylene ether phosphate of the present application is purchased from Nantong Chenrun Chemical Co., Ltd.

[0079] The applicant found that by adding phosphate ester as a dispersant, and polycarboxylate together, the seed treatment suspension prepared has good heat storage stability, and can further improve the adsorption capacity and film uniformity of the seed, which may be because by adding phosphate ester, and controlling the weight ratio of polycarboxylate, the phosphate ester enters the protective layer formed by polycarboxylate, and interacts with the active molecules, thereby forming a denser protective layer, increasing the space resistance, reducing the aggregation of active molecules at high temperature, increasing the heat storage stability, and the applicant found that when nonylphenol polyoxyethylene ether phosphate and isooctanol polyoxyethylene ether phosphate are used together, the hydrophobic ends of the aryl-containing nonylphenol and the long-chain isooctanol are wound around the surface of the active ingredient, which is conducive to the formation of a protective layer with moderate density, when only isooctanol polyoxyethylene ether phosphate and polycarboxylate are used as dispersants, the protective layer is too dense and is easy to break, and when only nonylphenol polyoxyethylene ether phosphate and polycarboxylate are used as dispersants, the protective layer is still relatively thin, and the heat storage stability is less improved; in addition, the applicant found that by using phosphate ester as a dispersant, due to the presence of flexible oxyethylene ether long chain and hydroxyl of phosphate ester, it can participate in the hydrogen bond network of chitosan and be wound around the chitosan molecule, further improving the adsorption capacity and film uniformity of the seed.

[0080] In addition, the applicant found that when the weight ratio of phosphate ester and polycarboxylate is too small, the phosphate ester cannot enter the inside of the polycarboxylate protective layer, but is attached to the surface of the polycarboxylate, which is easy to cause flocculation, reducing the high temperature and room temperature stability of the suspension prepared.

[0081] thickening agent

[0082] The thickening agent is a substance that can increase the viscosity of a liquid, and can increase the viscosity of a system, maintain a uniform and stable suspension state or emulsion state, or form a gel. The thickening agent is not specifically limited in the present application, and examples include starch, gum arabic, pectin, agar, gelatin, algin, carrageenan, dextrin, carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, starch sodium phosphate, sodium carboxymethyl cellulose, sodium alginate, casein, and polyvinylpyrrolidone.

[0083] antifreezing agent

[0084] The antifreeze agent is an auxiliary agent that can stably store the suspension agent in a low-temperature environment, and is not specifically limited in the present application, and examples include isopropyl alcohol, ethylene glycol, propylene glycol, propylene glycol butyl ether, ethylene glycol butyl ether acetate, formamide, calcium chloride, sodium acetate, and urea.

[0085] antifoaming agent

[0086] The antifoaming agent is a substance that can reduce the surface tension of water, a solution, a suspension, and the like, prevent the formation of foam, or reduce or eliminate existing foam. The antifoaming agent is not specifically limited in the present application, and examples include one or more of polyglycerol, a fatty acid, a polyoxypropylene glycerol ether, and a silicone oil or silicone.

[0087] aposematic coloration

[0088] The warning color is not specifically limited in the present application, and examples include water-based magenta, acid magenta, permanent red, and water-fast violet.

[0089] The second aspect of the present application provides a method for preparing the seed treatment suspension agent as described above, comprising the following steps:

[0090] After the active ingredient, the dispersing agent, the antifoaming agent, and water are mixed and sand-milled, the remaining raw materials for preparation are added, mixed, and the seed treatment suspension agent is obtained.

[0091] The third aspect of the present application provides the use of the seed treatment suspension agent as described above, which is used for preventing and treating diseases and / or insect pests of crops.

[0092] In a preferred embodiment, the crop of the present application is selected from one or more of rice, corn, peanut, wheat, cotton, rapeseed, potato, radish, cabbage, sorghum, and soybean.

[0093] In a preferred embodiment, the disease is one or more of sheath blight, white rot, bacterial wilt, root knot nematode, scab, stem rust, leaf rust, stripe rust, downy mildew, anthracnose, gummy stem blight, smut, yellow dwarf, bunchy top, black chaff, bacterial leaf spot, clover proliferation, and cyst nematode; and the insect pest is one or more of grub, leaf beetle, wireworm, cutworm, aphid, planthopper, whitefly, leafhopper, and cotton bollworm.

[0094] The applicant has found that by using the seed treatment suspension provided by the present application for seed treatment, especially for wheat seed and peanut seed treatment, through the combined action of the three active ingredients of clothianidin, difenoconazole and carboxin, the insect pests and diseases of crops can be significantly controlled, especially for controlling aphids and sheath blight of wheat, and grubs and white rot of peanuts, which has a significant effect. When the seed treatment suspension provided by the present application is used for controlling aphids and sheath blight of wheat, 1000-2000 mL of the suspension is used for treating per 100 kg of wheat seeds, and when it is used for controlling grubs and white rot of peanuts, 1200-2400 mL of the suspension is used for treating per 100 kg of peanut seeds.

[0095] Examples

[0096] The present application will be described in detail by the following examples. It is necessary to point out here that the following examples are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Some non-essential improvements and adjustments made by the skilled in the art based on the content of the present application still belong to the scope of protection of the present application.

[0097] In addition, if not otherwise specified, the raw materials used are commercially available and purchased from National Pharmaceutical Chemical Reagents.

[0098] example 1

[0099] Embodiment 1 of the present application provides a seed treatment suspension concentrate, raw materials of the suspension concentrate include, by weight percentage, 12% active ingredient, 1% film forming agent, 6% dispersing agent, 0.5% thickening agent, 2% antifreezing agent, 0.1% defoaming agent and 1% warning color and the balance of water; the active ingredient includes clothianidin and carboxin, the weight ratio is 1:0.15; the film forming agent is modified chitosan, raw materials of the modified chitosan include N-isostearyl methyl sodium taurate, nano titanium dioxide and chitosan, the weight ratio is 0.15:1:50; the dispersing agent includes polycarboxylate and polyoxyethylene ether phosphate, the weight ratio is 1:0.3, raw materials of the polycarboxylate include acrylic acid, 2-phenoxyethyl acrylate, acryloyl dimethyl sodium taurate and N-(3-dimethylamino) propyl-2-methyl-2-acrylamide, the weight ratio is 2:1:1:1, the polyoxyethylene ether phosphate includes nonylphenol polyoxyethylene ether phosphate and isooctanol polyoxyethylene ether phosphate, the weight ratio is 1:2; the thickening agent is gum arabic, the antifreezing agent is propylene glycol, the defoaming agent is silicone oil, and the warning color is water-soluble purple.

[0100] The clothianidin, carboxin and difenoconazole are all purchased from China Nonglihua Biotechnology Co., Ltd.

[0101] The preparation method of the modified chitosan includes the following steps:

[0102] The nano titanium dioxide is added into water, and the pH is adjusted to 6, N-isostearyl methyl sodium taurate is added, and the reaction is carried out at 40℃ for 0.5h, and then the modified nano titanium dioxide is obtained by drying;

[0103] The modified nano titanium dioxide is added into a glycerol and 0.6% acetic acid solution, and chitosan is added, and the modified chitosan is obtained by ultrasonic degassing; the nano titanium dioxide is purchased from Shanghai Superwe Nanometer Technology Co., Ltd.

[0104] The preparation method of the polycarboxylate includes the following steps:

[0105] Water and ammonium persulfate are mixed, and heated to 65℃, and then acrylic acid, 2-phenoxyethyl acrylate, acryloyl dimethyl sodium taurate and N-(3-dimethylamino) propyl-2-methyl-2-acrylamide are added dropwise, and after the dropwise addition is completed, the reaction is carried out at constant temperature for 2.5h, and then the polycarboxylate is obtained by cooling, adjusting the pH to 7 and drying; the ammonium persulfate accounts for 0.4wt% of the acrylic acid.

[0106] The nonylphenol polyoxyethylene ether phosphate and isooctanol polyoxyethylene ether phosphate are purchased from Nantong Chenrun Chemical Co., Ltd.

[0107] The example also provides a preparation method of the seed treatment suspension agent as described above, which comprises the following steps: mixing the active ingredient, the dispersing agent, the defoaming agent and water, sand grinding, then adding the remaining raw materials for preparation, mixing to obtain the seed treatment suspension agent.

[0108] example 2

[0109] Embodiment 2 of the present application provides a seed treatment suspension agent, the specific embodiment of which is the same as that of Embodiment 1, except that the active ingredient comprises clothianidin, difenoconazole and carboxin, with a weight ratio of 1:0.06:0.2.

[0110] The example also provides a preparation method of the seed treatment suspension agent as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0111] example 3

[0112] Embodiment 3 of the present application provides a seed treatment suspension agent, the specific embodiment of which is the same as that of Embodiment 1, except that the active ingredient comprises clothianidin, difenoconazole and carboxin, with a weight ratio of 1:0.04:0.1.

[0113] The example also provides a preparation method of the seed treatment suspension agent as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0114] example 4

[0115] Embodiment 4 of the present application provides a seed treatment suspension agent, the specific embodiment of which is the same as that of Embodiment 1, except that the active ingredient comprises clothianidin, difenoconazole and carboxin, with a weight ratio of 1:0.05:0.15.

[0116] The example also provides a preparation method of the seed treatment suspension agent as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0117] example 5

[0118] Embodiment 5 of the present application provides a seed treatment suspension agent, the specific embodiment of which is the same as that of Embodiment 1, except that the active ingredient comprises clothianidin and difenoconazole, with a weight ratio of 1:0.05.

[0119] The example also provides a preparation method of the seed treatment suspension agent as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0120] example 6

[0121] Embodiment 6 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of embodiment 1, except that the active ingredients include clothianidin, difenoconazole and carboxin, with a weight ratio of 1:0.2:0.15.

[0122] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of embodiment 1.

[0123] example 7

[0124] Embodiment 7 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of embodiment 1, except that the active ingredients include clothianidin, difenoconazole and carboxin, with a weight ratio of 1:0.05:0.5.

[0125] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of embodiment 1.

[0126] example 8

[0127] Embodiment 8 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of embodiment 4, except that the dispersing agent is a polycarboxylate with a brand name of M150, which is purchased from Nanjing Qicheng New Material Co., Ltd.

[0128] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of embodiment 1.

[0129] example 9

[0130] Embodiment 9 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of embodiment 8, except that the N-isostearyl methyl sodium taurate is replaced by sodium dodecyl sulfonate.

[0131] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of embodiment 1.

[0132] example 10

[0133] Embodiment 10 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of embodiment 8, except that the raw materials for preparing the modified chitosan include N-isostearyl methyl sodium taurate, nano titanium dioxide and chitosan, with a weight ratio of 0.15:10:50.

[0134] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of embodiment 1.

[0135] example 11

[0136] Embodiment 11 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 8, except that the raw materials for preparing the modified chitosan include N-isostearyl methyl sodium taurine, nano titanium dioxide and chitosan, with a weight ratio of 0.4:1:50.

[0137] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0138] example 12

[0139] Embodiment 12 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 8, except that the dispersant is a polycarboxylic acid salt, and the raw materials for preparing the polycarboxylic acid salt include acrylic acid, 2-phenoxyethyl acrylate, sodium acryloyldimethyl taurate and N-(3-dimethylamino) propyl-2-methyl-2-propenamide, with a weight ratio of 2:1:1:1.

[0140] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0141] example 13

[0142] Embodiment 13 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the 2-phenoxyethyl acrylate is replaced by ethyl acrylate.

[0143] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0144] example 14

[0145] Embodiment 14 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the 2-phenoxyethyl acrylate is replaced by o-phenylphenoxyethyl acrylate.

[0146] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0147] example 15

[0148] Embodiment 15 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the raw materials for preparing the polycarboxylate include acrylic acid, 2-phenoxyethyl acrylate, sodium acryloyldimethyltaurate and N-(3-dimethylamino)propyl-2-methyl-2-propenamide, with a weight ratio of 2:2:1:1.

[0149] This example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0150] example 16

[0151] Embodiment 16 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the raw materials for preparing the polycarboxylate include acrylic acid, 2-phenoxyethyl acrylate and sodium acryloyldimethyltaurate, with a weight ratio of 2:1:2.

[0152] This example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0153] example 17

[0154] Embodiment 17 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the raw materials for preparing the polycarboxylate include acrylic acid, 2-phenoxyethyl acrylate and N-(3-dimethylamino)propyl-2-methyl-2-propenamide, with a weight ratio of 2:1:2.

[0155] This example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0156] example 18

[0157] Embodiment 18 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 12, except that the N-(3-dimethylamino)propyl-2-methyl-2-propenamide is replaced by N-(N-butoxymethyl)acrylamide.

[0158] This example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0159] example 19

[0160] Embodiment 19 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 4, except that the nonylphenol polyoxyethylene ether phosphate is replaced by nonylphenol polyoxyethylene ether, which is purchased from Nantong Chenrun Chemical Co., Ltd.

[0161] The present example also provides a preparation method of the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0162] example 20

[0163] Embodiment 20 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 4, except that the isooctanol polyoxyethylene ether phosphate is replaced by isooctanol polyoxyethylene ether, which is purchased from Nantong Chenrun Chemical Co., Ltd.

[0164] The present example also provides a preparation method of the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0165] example 21

[0166] Embodiment 21 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 4, except that the isooctanol polyoxyethylene ether phosphate is replaced by oleyl polyoxyethylene ether phosphate, which is purchased from Nantong Chenrun Chemical Co., Ltd.

[0167] The present example also provides a preparation method of the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0168] example 22

[0169] Embodiment 22 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 4, except that the polyoxyethylene ether phosphate is nonylphenol polyoxyethylene ether phosphate.

[0170] The present example also provides a preparation method of the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0171] example 23

[0172] Embodiment 23 of the present application provides a seed treatment suspension concentrate, the specific implementation of which is the same as that of Embodiment 4, except that the polyoxyethylene ether phosphate is isooctanol polyoxyethylene ether phosphate.

[0173] The present example also provides a preparation method of the seed treatment suspension concentrate as described above, the specific implementation of which is the same as that of Embodiment 1.

[0174] example 24

[0175] Embodiment 24 of the present application provides a seed treatment suspension concentrate, the specific embodiment of which is the same as that of Embodiment 4, except that the dispersing agent comprises polycarboxylate and polyoxyethylene ether phosphate in a weight ratio of 1:0.05.

[0176] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0177] example 25

[0178] Embodiment 25 of the present application provides a seed treatment suspension concentrate, the specific embodiment of which is the same as that of Embodiment 4, except that the dispersing agent comprises polycarboxylate and polyoxyethylene ether phosphate in a weight ratio of 1:0.6.

[0179] The present example also provides a method for preparing the seed treatment suspension concentrate as described above, the specific embodiment of which is the same as that of Embodiment 1.

[0180] Performance evaluation

[0181] 1. Field test: the seed treatment suspension concentrate provided by Embodiment 4 was subjected to field test for aphid and sheath blight, respectively.

[0182] (1) Field efficacy test of 12% seed treatment suspension concentrate against wheat sheath blight in Hebei Province

[0183] The Institute of Plant Protection of Hebei Agricultural University was commissioned to conduct field efficacy test in the wheat planting base of Zhangzhuang, Qingyuan District, Baoding City, Hebei Province, with 3% difenoconazole seed treatment suspension concentrate produced by Henan Haodi Agricultural Co., Ltd. and 10% carboxin seed treatment suspension concentrate provided by Henan Xifeng Biological Technology Co., Ltd. as control, wherein the active ingredient dosage and control results are shown in Table 1 and Table 2, respectively.

[0184] Table 1 Dosage and number of test substances of 12% clothianidin·difenoconazole·carboxin seed treatment suspension concentrate against wheat sheath blight

[0185]

[0186]

[0187] Table 2 Test results of 12% clothianidin·difenoconazole·carboxin seed treatment suspension concentrate against wheat sheath blight

[0188]

[0189] (2) Field efficacy test of 12% seed treatment suspension concentrate against wheat aphid in Hebei Province

[0190] The Hebei Agricultural University of Plant Protection was commissioned to conduct field efficacy trials in Niuzhuang Village, Beidian Town, Qingyuan District, Baoding City, Hebei Province, with 8% clothianidin seed treatment suspension concentrate produced by Henan Nongwang Industrial Co., Ltd. as the control. The active ingredient dosage and control results are shown in Table 3.

[0191] Table 3 Field efficacy test of 12% seed treatment suspension concentrate against aphids in Hebei wheat

[0192]

[0193]

[0194] (1) Field efficacy test of 12% seed treatment suspension concentrate against wheat sharp eyespot in Shanghai

[0195] The Shanghai Senwei Agricultural Science and Technology Center was commissioned to conduct field efficacy trials in Jiatian Village Road, Xinhuan Town, Songjiang District, Shanghai, with 3% difenoconazole suspension seed coating produced by Henan Haodi Agricultural Co., Ltd. and 10% carboxin seed treatment suspension concentrate provided by Henan Xifeng Biological Technology Co., Ltd. as control. The active ingredient dosage and control results are shown in Table 4.

[0196] Table 4 Field efficacy test of 12% seed treatment suspension concentrate against wheat sharp eyespot in Shanghai

[0197]

[0198] (4) Field efficacy test of 12% seed treatment suspension concentrate against aphids in Shanghai

[0199] The Shanghai Senwei Agricultural Science and Technology Center was commissioned to conduct field efficacy trials in Jiatian Village Road, Xinhuan Town, Songjiang District, Shanghai, with 8% clothianidin seed treatment suspension concentrate produced by Henan Nongwang Industrial Co., Ltd. as the control. The active ingredient dosage and control results are shown in Table 5.

[0200] Table 5 Field efficacy test of 12% seed treatment suspension concentrate against aphids in Shanghai

[0201]

[0202]

[0203] (5) Field efficacy test of 12% seed treatment suspension concentrate against wheat sharp eyespot in Sichuan

[0204] The field efficacy test was conducted by Sichuan Weibentong Technology Co., Ltd. in Xinguang Village, Heilong Town, Qingshen County, Sichuan Province, with 3% difenoconazole SC produced by Henan Haodi Agricultural Co., Ltd. and 10% carboxin seed treatment SC provided by Henan Xifeng Biological Technology Co., Ltd. as control, the active ingredient dosage is shown in Table 6, and the control results in 2019 and 2020 are shown in Tables 7 and 8, respectively.

[0205] Table 6 Dosage and number of 12% clothianidin·difenoconazole·carboxin seed treatment SC for controlling wheat sharp eyespot

[0206]

[0207] Table 7 Test results of 12% clothianidin·difenoconazole·carboxin seed treatment SC for controlling wheat sharp eyespot (Qingshen, Sichuan, 2019)

[0208]

[0209]

[0210] Table 8 Average control effect of 12% clothianidin·difenoconazole·carboxin seed treatment SC for controlling wheat sharp eyespot (Qingshen, Sichuan, 2020)

[0211]

[0212] (6) Field efficacy test of 12% seed treatment SC for controlling wheat aphids in Sichuan

[0213] The field efficacy test was conducted by Sichuan Weibentong Technology Co., Ltd. in Xinguang Village, Heilong Town, Qingshen County, Sichuan Province, with 3% difenoconazole SC produced by Henan Haodi Agricultural Co., Ltd. and 10% carboxin seed treatment SC provided by Henan Xifeng Biological Technology Co., Ltd. as control, the active ingredient dosage is shown in Table 6, and the control results in 2019 and 2020 are shown in Tables 7 and 8, respectively.

[0214] Table 9 Field efficacy test of 12% seed treatment SC for controlling wheat aphids in Sichuan

[0215]

[0216] 2. Toxicity test: The 12% difenoconazole·clothianidin·carboxin seed treatment SC provided in Example 4 was entrusted to Guizhou Jianand Technology Co., Ltd. for toxicity test:

[0217] (1) Acute oral toxicity test of 12% difenoconazole·clothianidin·carboxin seed treatment SC in rats

[0218] This test is based on the "Pesticide Registration Toxicology Test Method" "Acute Oral Toxicity Test - Sequential Method" (GB15670.3-2017) as the criterion, in accordance with the provisions of the test plan and related SOP, in the laboratory selected healthy adult female SD rats 3, 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent rat acute oral toxicity limit test.

[0219] According to the results of the previous pre-test of the agency and related toxicity data, this test through oral gavage 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent (5000 mg / kg·BW dose) to SD rats acute oral toxicity test, mainly observe the SD rats after a one-time oral gavage 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent produced by the toxic reaction, death and gross anatomy results, and calculate the median lethal dose (LD50).

[0220] Under the conditions of this test, 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent after oral gavage observation period, animals after exposure to general clinical observation was normal, no animal death at the end of the test, no abnormalities were found in gross anatomy. The test results show that: 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent rat acute oral LD50 is greater than 5000 mg / kg·BW. According to the "Annex 14: Pesticide Product Toxicity Classification Standard" of the "Pesticide Registration Data Requirements" of the Ministry of Agriculture of the People's Republic of China No. 2569, 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent rat acute oral toxicity belongs to the microtoxicity level.

[0221] (2) 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent rat acute dermal toxicity test

[0222] This test is based on the "Pesticide Registration Toxicology Test Method" "Acute Dermal Toxicity Test" (GB15670.5-2017) as the criterion, in accordance with the provisions of the test plan and related SOP, in the laboratory selected healthy adult SD rats 10, half male and female, 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent rat acute dermal toxicity limit test.

[0223] According to the relevant toxicity data, this test through 24h continuous dermal application of 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent (2000 mg / kg·BW dose, half male and female) to SD rats acute dermal toxicity test, mainly observe the SD rats after a one-time dermal application of 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent produced by the toxic reaction, death and gross anatomy results, to determine the toxicity of 12% phenyl ether. thiamethoxam. carboxim seed treatment suspension agent classification.

[0224] Under the experimental conditions, the body weight of rats increased normally during the observation period after the 12% phoxim·clothianidin·carboxin seed treatment suspension agent was applied to the skin, no obvious toxic symptoms were observed, and no animal deaths were observed at the end of the test. No abnormalities were observed during the gross autopsy.

[0225] The test results show that the acute percutaneous LD50 values of 12% phoxim·clothianidin·carboxin seed treatment suspension agent in male and female rats are greater than 2000 mg / kg·BW. According to the pesticide registration data requirements (Annex 14 of the Announcement No. 2569 of the Ministry of Agriculture of the People's Republic of China) on the toxicity classification standards of pesticide products, the acute percutaneous toxicity of 12% phoxim·clothianidin·carboxin seed treatment suspension agent in rats belongs to the low toxicity level.

[0226] (3) Acute skin irritation / corrosion test of 12% phoxim·clothianidin·carboxin seed treatment suspension agent This test was conducted according to the guidelines of "Pesticide Registration Toxicology Test Methods" "Part 7: Skin Irritation / Corrosion Test" (GB / T 15670.7-2017), and 3 healthy adult New Zealand rabbits (♂) with normal skin were selected in the laboratory according to the provisions of the test plan and relevant SOPs to conduct the acute skin irritation / corrosion test of 12% phoxim·clothianidin·carboxin seed treatment suspension agent.

[0227] The skin of 3 New Zealand rabbits was prepared about 6 cm2 on both sides of the spine 24 hours before the test, and the skin was examined to confirm that the skin was intact and undamaged. The contralateral skin was used as a control, and 0.5 mL of 12% phoxim·clothianidin·carboxin seed treatment suspension agent was applied to the prepared skin on the test side. A layer of plastic wrap and two layers of gauze were used to cover it, and then non-irritating adhesive tape was used to seal and fix it. After 4 hours (allowable error ±10 minutes) of sealing and application, the remaining test substance was removed with warm water, and the skin irritation response was observed; the other side was used as a self-control.

[0228] Under the experimental conditions, the test site skin was observed 1 hour (allowable error ±10 minutes), 24 hours (allowable error ±30 minutes), 48 hours (allowable error ±30 minutes), and 72 hours (allowable error ±30 minutes) after the test substance was removed. The average irritation score of the test side skin of the 3 animals was 0.0, and no skin irritation response such as erythema and edema occurred in the test skin of all animals within 72 hours.

[0229] According to Table 2 "Skin Irritation Intensity Classification" in "Pesticide Registration Toxicology Test Methods" "Part 7: Skin Irritation / Corrosion Test" (GB / T 15670.7-2017), the skin irritation response intensity was determined. Under the experimental conditions, the average skin irritation score of 12% phoxim·clothianidin·carboxin seed treatment suspension agent was 0 at the 24h, 48h and 72h observation time points of the acute skin irritation / corrosion test, i.e. the skin irritation intensity was non-irritating.

[0230] (4) Acute eye irritation / corrosion test of 12% phoxim · clothianidin · carboxin seed treatment suspension

[0231] This test is based on the "Pesticide Registration Toxicology Test Method" "Part 8: Acute Eye Irritation / Corrosion Test" (GB / T 15670.8-2017) as the guideline, according to the test plan and the relevant SOP of this institution, 3 healthy adult New Zealand rabbits (♂) without abnormality in both eyes were selected in the laboratory to conduct the acute eye irritation / corrosion test of 12% phoxim · clothianidin · carboxin seed treatment suspension.

[0232] Before the test, the eyes of New Zealand rabbits were examined, and after confirming normality, 0.1 mL of 12% phoxim · clothianidin · carboxin seed treatment suspension was dropped into the conjunctival sac of one side of the test animal, the upper and lower eyelids were passively closed for 1 s, and the eyes were not washed within 24 h after exposure. The other side of the eye was used as a control, and the animal eye irritation reaction was observed once at 1 h (allowable error ± 10 min), 24 h (allowable error ± 30 min), 48 h (allowable error ± 30 min), and 72 h (allowable error ± 30 min) after exposure. The damage degree of cornea, iris, conjunctiva and other parts of the animal eye was observed.

[0233] Under the conditions of this test, 1 of the 3 animals showed eye conjunctival hyperemia irritation reaction, with a maximum score of 1, and the other 2 did not show eye irritation reaction. The eye conjunctival irritation reaction of the animals completely recovered within 24 h.

[0234] According to Table 2 "Eye irritation reaction classification" in "Pesticide Registration Toxicology Test Method" "Part 8: Acute Eye Irritation / Corrosion Test" (GB / T 15670.8-2017), the eye irritation reaction classification was determined. Under the conditions of this test, 1 of the 3 animals showed eye conjunctival irritation reaction, with a maximum score of 1, and the other 2 did not show eye irritation reaction. The eye conjunctival irritation reaction of the animals completely recovered within 24 h. The acute eye irritation reaction of 12% phoxim · clothianidin · carboxin seed treatment suspension was classified as mild irritation.

[0235] (5) Skin allergy (sensitization) test of 12% phoxim · clothianidin · carboxin seed treatment suspension

[0236] This test is based on the "Pesticide Registration Toxicology Test Method" "Part 9 Skin Allergy (Sensitization) Test" (GB / T 15670.9-2017) as the guideline, according to the test plan and the relevant SOP of this institution, 30 healthy adult Hartley guinea pigs, half male and half female, were selected in the laboratory to conduct the skin allergy (sensitization) test of 12% phoxim · clothianidin · carboxin seed treatment suspension.

[0237] According to the relevant toxicity data, the skin allergy (sensitization) test was carried out by local occlusion patch test (Buehler Test, BT). The test was divided into blank control group (induction contact 0.2 mL of deionized water, challenge contact 0.2 mL of 12% diafenthiuron·thiamethoxam·carboxin seed treatment suspension concentrate) and test group (induction contact and challenge contact 0.2 mL of 12% diafenthiuron·thiamethoxam·carboxin seed treatment suspension concentrate). The animals were observed for skin reaction 24 h (allowable error ± 30 min) and 48 h (allowable error ± 30 min) after challenge contact.

[0238] Under the test conditions, the sensitization rate of the animals in the blank control group (24 h and 48 h) was 0, and the sensitization rate of the animals in the test group (24 h and 48 h) was 0. The sensitization rate of the animals in the positive control group of the sensitization test in the institution was 60%, and the sensitization rate of the positive control group was greater than 15%, so the sensitization method was reliable.

[0239] According to Table 2 "Sensitization intensity" in GB / T15670.9-2017 "Registered toxicology test method" "Skin allergy (sensitization) test", the sensitization intensity of 12% diafenthiuron·thiamethoxam·carboxin seed treatment suspension concentrate was judged. The sensitization rate (24 h and 48 h) of the test substance 12% diafenthiuron·thiamethoxam·carboxin seed treatment suspension concentrate was 0, which was no skin allergy.

[0240] 3. Heat storage stability test: The seed treatment suspension concentrates provided in Examples 4 and 8-25 were stored in a constant temperature oven at (54±2)℃ for 14 days, the appearance change of the suspension concentrate was observed for rating, and was divided into 1-5 levels, wherein 5 levels was no water separation and stratification, 4 levels was a small amount of water separation, 3 levels was a small amount of water separation, 2 levels was water separation and a small amount of stratification, and 1 level was serious stratification. The results are shown in Table 10.

[0241] 4. Seed adsorption test: The wheat seeds were treated with the seed treatment suspension concentrates provided in Examples 4 and 8-25, and each group of treated wheat seeds was divided into two parts, one part was control and the other part was test. The test group was loaded into a circular guide slot, the guide slot door was opened, and the seeds were allowed to fall freely onto a sieve at the same height. The pesticide detached from the seeds was leaked out of the sieve, and the process was repeated 5 times. The contents of thiamethoxam, diafenthiuron and carboxin on the seeds of the control and test groups were tested, and the adhesion was tested as the ratio of the contents of thiamethoxam, diafenthiuron and carboxin on the seeds of the test group to the control group. The results are shown in Table 10.

[0242] 5. Film uniformity test: the seed treatment suspensions provided by Example 4 and Examples 8-25 were respectively used for seed treatment, the film uniformity of the seed after film formation was observed, and was evaluated as 1-5 levels, wherein 5 level was that the film formed on the seed surface was uniform in color and smooth, 4 level was that the film formed on the seed surface had slightly raised points, 3 level was that the film formed on the seed surface was slightly rough and had a small amount of color unevenness, 2 level was that the film formed on the seed surface was relatively rough and had color unevenness in patches, and 1 level was that the film formed on the seed surface was rough and had obvious color unevenness, and the results are shown in Table 10.

[0243] Table 10 Performance characterization test

[0244]

[0245]

[0246] From the test results in Tables 1-10, it can be seen that the seed treatment suspensions provided by the application can be used for preventing and treating insect pests and diseases of crops, and in particular, when used for treating wheat and peanut seeds, can be significantly used for preventing and treating aphids and sharp eyesight of wheat, peanut grubs and white thread disease, and promoting crop growth; and the seed treatment suspensions provided by the application have good normal temperature storage stability, heat storage stability, and the seed has good adhesion and film uniformity.

[0247] The foregoing examples are illustrative only and are not meant to limit the scope of the methods described in the application. The appended claims are intended to claim as broad a range as possible given the nature of the claims and the prior art. The examples presented herein are merely illustrative of selected embodiments according to all possible combinations of the elements and are not intended to be limiting. Accordingly, Applicant intends to rely on the appended claims as determining the scope of the application and, therefore, makes no undertaking to draft the claims to insure fair scope of the application unless it is expressly stated otherwise in the following claims. Some numerical ranges are included in the claims to indicate that every number and range falling within the pretaxable limits of the range claimed is intended to be a separate and independent claim.

Claims

1. A seed treatment suspension characterized in that, The preparation raw materials of the suspension agent include 5-15% active ingredient, 0.01-20% auxiliary agent and the rest water by weight percentage; The active ingredient includes clothianidin and carboxin, and the weight ratio is 1:0.15; The active ingredient further includes difenoconazole, and the weight ratio of the clothianidin and difenoconazole is 1:0.05; The auxiliary agent includes film forming agent, dispersant, thickening agent, anti-freezing agent, defoaming agent and warning color; The film forming agent is modified chitosan, and the preparation raw materials of the modified chitosan include N-isostearyl methyl sodium taurine, nano titanium dioxide and chitosan, and the weight ratio is (0.1-0.2):1:(40-60); The dispersant includes polycarboxylate and polyoxyethylene ether phosphate, and the weight ratio is 1:(0.2-0.4); the preparation raw materials of the polycarboxylate include acrylic acid, acrylate and acrylamide, and the molar ratio is (1-3):(0.5-1.5):(1-3); the acrylate is 2-phenoxyethyl acrylate; the acrylamide includes sodium acryloyldimethyl taurate and N-(3-dimethylamino) propyl-2-methyl-2-acrylamide, and the weight ratio is (2-3):(2-3); The polyoxyethylene ether phosphate includes nonylphenol polyoxyethylene ether phosphate and isooctanol polyoxyethylene ether phosphate, and the weight ratio is 1:

2.

2. A method of preparing a seed treatment suspension concentrate according to claim 1, characterized in that, The method comprises the following steps: After the active ingredient, dispersant, defoaming agent and water are mixed and sand ground, the remaining preparation raw materials are added and mixed to obtain the seed treatment suspension agent.

3. Use of a seed treatment suspension concentrate according to claim 1, characterized in that The application is applied to the prevention and treatment of diseases and / or insect pests of crops.

4. The use of a seed treatment suspension concentrate according to claim 3, characterized in that The crops are selected from one or more of rice, corn, peanut, wheat, cotton, rapeseed, potato, radish, cabbage, sorghum and soybean.

5. The use of a seed treatment suspension concentrate according to claim 4, characterized in that The diseases are selected from one or more of sheath blight, bacterial wilt, root knot nematode disease, stem rust, leaf rust, stripe rust, anthracnose, gummy stem blight, smut, root rot, bunchy top disease and cyst nematode disease; the insect pests are caused by one or more of pests selected from grub, leaf beetle, wireworm, cutworm, aphid, planthopper, whitefly and leafhopper.

Images