CN111418603A

CN111418603A - Water suspending agent containing bifenthrin and fluopyram, and preparation method and application thereof

Info

Publication number: CN111418603A
Application number: CN202010386311.1A
Authority: CN
Inventors: 李志清; 刘振民; 王建伟; 赵保臣; 张小兵
Original assignee: Shandong Weifang Rainbow Chemical Co Ltd
Current assignee: Shandong Weifang Rainbow Chemical Co Ltd
Priority date: 2020-05-09
Filing date: 2020-05-09
Publication date: 2020-07-17

Abstract

The invention discloses a water suspending agent containing bifenthrin and fluopicolide, a preparation method and application thereof, wherein the water suspending agent comprises the following components in percentage by weight: 20-60% of bifenthrin, 5-25% of fluopicolide, 2-10% of a dispersing agent, 1-10% of a wetting agent, 0.1-1% of a defoaming agent, 3-8% of an antifreezing agent, 0.1-1% of a preservative, 0.1-1% of a thickening agent and the balance of water to 100%. The bifenthrin and the flufen-ethyl are compounded and prepared into the water suspending agent, the water suspending agent has the advantages of remarkable pesticide effect, high suspension rate, safety, low toxicity and the like, has good control effects on grubs, cotton bollworms, cotton red spiders, thrips, wireworms, flea beetles, leaf beetles and other pests, and on various diseases of crops such as potato black nevus, wheat sharp eyespot, rice sheath blight, sclerotinia rot of colza, wheat loose smut, wheat stinking smut, small leaf spot of corn, maize head smut and the like, and has obviously improved insecticidal and disease prevention effects compared with a single agent of bifenthrin and flufen-ethyl.

Description

Water suspending agent containing bifenthrin and fluopyram, and preparation method and application thereof

Technical Field

The invention relates to an aqueous suspension, in particular to an aqueous suspension containing bifenthrin and fluopicolide, a preparation method and application thereof, and belongs to the technical field of chemical pesticides.

Background

Bifenthrin, english name: bifenthrin, chemical name: methyl biphenyl-3-yl methyl (Z) (1RS,3RS)3- (2-chloro-3, 3, 3-trifluoro propyl-1-alkenyl) -2, 2-dimethyl cyclopropane carboxylic ester, which belongs to pyrethroid insecticides and acaricides. Bifenthrin has the characteristics of strong knock-down effect, broad spectrum, high efficiency, rapidness, long residual effect and the like, mainly has the contact killing effect and the stomach toxicity effect, has no systemic effect, is suitable for various crops such as cotton, fruit trees, vegetables, tea leaves and the like, can be used for preventing and controlling cotton bollworms, red bollworms, tea geometrid, tea caterpillars, red spiders of apples or hawthorns, peach fruit borers, cabbage aphids, cabbage caterpillars, diamondback moths, citrus leaf miners and the like, has quick effect, does not move in soil, is safe to environment and has long residual effect period.

Fluopicolide, english name: fluxapyroxad, chemical name: 3- (difluoromethyl) -1-methyl-N- (3 ', 4 ', 5 ' -trifluoro [1, 1-biphenyl ] -2-yl)) -1H-pyrazole-4-formamide is a broad-spectrum pyrazole formamide bactericide and has protection and treatment effects. The treated seeds can absorb fluopicolide in the germination process and are conducted to other parts of plants through xylem, so that the effect of protecting crops is achieved. Fluopyram has good treatment and protection effects on other fungal infection diseases such as blight and the like, has high biological activity on oomycete pathogenic bacteria, has strong permeability, can protect leaves from being infected by plant pathogenic bacteria after treatment of sprouts, can provide comprehensive and durable protection for new leaves, stems and young fruits, and has good prevention, control and treatment effects on diseases such as potato black nevus, wheat sharp eyespot, rice sheath blight, sclerotinia rot of colza, wheat loose smut, wheat stinking smut, corn small leaf spot, corn head smut and the like caused by rhizoctonia solani, smut and the like.

In agricultural production, various pathogens, such as: the pathogens in the soil, the pathogens propagated by air in the seedling stage, the insect pests in all stages of plant growth and the like often cause crop yield reduction, serious even no grain income exists, the main limiting factor of agricultural production is formed, and the bactericide is used for killing the pathogens in time in the early stage of disease attack and insect pest so as to have great improvement effect on yield increase. The water suspension agent has the advantages of high active ingredient content of the effective ingredients, small volume and material saving, can ensure that the effective ingredients of the pesticide can be intensively acted on the roots of seeds and plants when in use, are slowly released and have no toxic action on the germination and growth of crops, has the characteristics of high efficiency, economy, safety, long residual period, multifunction and the like, can promote the yield increase of agricultural production, reduce the production cost, and realize the standardization of improved varieties of crops and the accurate quantification of seeding. At present, no report related to bifenthrin and fluopicolide suspension concentrates is found.

Disclosure of Invention

In order to meet the actual requirements of agricultural production, the invention provides the aqueous suspension containing bifenthrin and fluopicolide, the aqueous suspension takes the compounded bifenthrin and fluopicolide as effective components, the double killing of diseases and pests can be realized, in addition, the stability and compatibility of the effective components are improved through the selection of auxiliary agents, and the performance and the stability of the preparation are ensured.

The bifenthrin has a melting point of 68-70.6 ℃, and an oil-water distribution coefficient logP of 6.66, and belongs to active ingredients with low melting points and high lipophilicity; the flufenapyr has the melting point of 156.8 ℃, the oil-water distribution coefficient logP 3.08, and the two active medicines have stronger lipophilicity, particularly bifenthrin, are not easy to disperse and suspend in water, and because the melting point of the bifenthrin is lower, the problems of creaming or crystallization caused by over-temperature sanding easily occur in the processing process, the heat storage stability is poor, serious abnormity such as crystallization and caking easily occur, and the problems are more prominent when the content of the active ingredients is higher. Aiming at the problems, the inventor carries out a large amount of screening work on an auxiliary agent system (auxiliary agent type, auxiliary agent components and auxiliary agent content) through research and a large amount of experiments, and finally obtains the auxiliary agent system with good matching degree, stable performance and good insecticidal and bactericidal effects. Through the selection of the auxiliary agents, particularly the screening and combination of 2 auxiliary agents, namely the dispersing agent and the wetting agent, the stability of the suspending agent is improved, the processing difficulty of the preparation form is greatly reduced, the bifenthrin and the fluopicolide can not only realize lower content but also realize high content of more than 50 percent when being prepared into the suspending agent, and the finally obtained suspending agent has the advantages of high suspension rate, good uniformity, good heat storage stability and the like.

The specific technical scheme of the invention is as follows:

the water suspending agent containing bifenthrin and fluopicolide comprises the following components in percentage by weight: 20-60% of bifenthrin, 5-25% of fluopicolide, 2-10% of a dispersing agent, 1-10% of a wetting agent, 0.1-1% of a defoaming agent, 3-8% of an antifreezing agent, 0.1-1% of a preservative, 0.1-1% of a thickening agent and the balance of water to 100%.

Further, the aqueous suspension agent comprises the following components in percentage by weight: 25-55% of bifenthrin, 10-20% of fluopicolide, 4-8% of dispersing agent, 2-8% of wetting agent, 0.1-0.2% of defoaming agent, 4-8% of antifreezing agent, 0.1-0.2% of preservative, 0.1-0.2% of thickening agent and the balance of water to 100%.

Further, in the above aqueous suspension, the total content of bifenthrin and fluoxafen in the aqueous suspension is 30 to 75wt%, preferably 45 to 75wt%, more preferably 55 to 75wt%, and still more preferably 60 to 75 wt%.

Furthermore, in the aqueous suspension, the mass ratio of bifenthrin to fluoxafen is 2-6:1, preferably 3: 1.

Preferably, in the aqueous suspension, the content of bifenthrin in the aqueous suspension is 45wt%, and the content of fluopicolide in the aqueous suspension is 15 wt%.

Preferably, in the aqueous suspension, the weight percentage of each component is as follows: 45% of bifenthrin, 15% of fluopyram, 6% of a dispersing agent, 4% of a wetting agent, 0.1% of a defoaming agent, 5% of an antifreezing agent, 0.1% of a preservative, 0.1% of a thickening agent and the balance of water to 100%.

Further, in the aqueous suspension, the dispersant is one or more of sodium lignosulfonate, styrylphenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, styrylphenol polyoxyethylene ether sulfonate, polyoxyethylene-polyoxypropylene block copolymer, polycarboxylate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, naphthalene sulfonic acid formaldehyde condensation product sodium salt and ethylene oxide-propylene oxide block copolymer. The dispersing agent is used for uniformly dispersing the active ingredients and preventing agglomeration, and is the key of stable preparation and successful preparation. Experiments show that when the dispersing agent is in a mass ratio of 1: 1-2, the water suspending agent has the best dispersion performance, the effective components of the medicines and other auxiliary agents do not have agglomeration and precipitation phenomena, the dispersibility is good, the suspension rate is high, and the contact between the effective components and seeds is more facilitated. The polycarboxylate used in the present invention may be styrene maleic anhydride acrylate polymer ammonium salt, styrene maleic anhydride polymer sodium salt, styrene and acrylic acid and methacrylic acid copolymer sodium salt, etc., each polycarboxylate acting similarly when used as a dispersant.

Furthermore, in the aqueous suspension, the wetting agent is one or more of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium a-olefin sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, nekal BX, fatty acid sulfate and fatty acid ester sulfate. The fatty acid ester sulfate may be fatty acid methyl ester sulfate, fatty acid ethyl ester sulfate, etc. The wetting agent has the functions of improving the surface hydrophilicity of the active ingredient particles, improving the affinity with water and reducing the surface tension of the solution, and is the key for the preparation to exert the stability and the drug effect fully. When the wetting agent is a mixture of sodium dodecyl sulfate and sodium alkylphenol polyoxyethylene ether sulfate in a mass ratio of 1:1-3, the water suspension agent has the best wetting performance, the effective components of the medicaments are wetted quickly, the suspension rate is high, the surface tension of the liquid medicine is reduced, the liquid medicine is more easily compatible on the surface of a blade and does not drip, and the purposes of killing insects and sterilizing can be better achieved.

In addition, in the aqueous suspension, the defoaming agent is one or more of glycerol polyoxypropylene ether, a higher alcohol fatty acid ester compound, organic silicone, C8-C10 fatty alcohol, C10-C20 saturated aliphatic carboxylic acid and C10-C20 saturated aliphatic carboxylic acid ester. The defoaming agent has the functions of eliminating foam generated in the product and when the product is mixed with water and shaken, so that the product is more stable, the production and the use of the product are more convenient, the spreading capacity of the leaf surfaces of the product can be improved, liquid drops are easier to disperse on the leaf surfaces, and the insecticidal and bactericidal activity of the preparation is further optimized. When the defoaming agent is glycerol polyoxyethylene ether, the defoaming effect and the use experience are better.

Furthermore, in the aqueous suspension, the antifreezing agent is one or more of ethylene glycol, propylene glycol and glycerol, and the antifreezing agent has the functions of reducing the melting point of the product, keeping the product in fluidity in a lower temperature range, ensuring the normal use of the product at a lower temperature and widening the temperature range of the preparation. When the antifreezing agent is propylene glycol, the product has low melting point and high moisturizing effect.

Further, in the above aqueous suspension, the preservative is one or more of paraformaldehyde, sodium nitrite, sodium benzoate, potassium sorbate and dehydroacetic acid. The preservative has the effects of delaying the putrefaction caused by the growth of microorganisms or chemical changes, enabling the product to have a longer shelf life, improving the stability of the product, and having a better putrefaction prevention effect and a longer shelf life when the preservative is paraformaldehyde.

Furthermore, in the aqueous suspension, the thickening agent is one or more of xanthan gum, bentonite, kaolin, magnesium aluminum silicate type SM gel and white carbon black, and when the thickening agent is the xanthan gum, the aqueous suspension has better overall fluidity and higher stability, is not layered or bottomed after being stored for a long time, and can better achieve the aims of disinsection and sterilization.

The aqueous suspension agent is simple to prepare and easy to implement, has the advantages of high suspension rate, good dispersion in water, good uniformity, good stability and the like through selection of various auxiliary agents, and can obtain the high-content aqueous suspension agent with high stability and the content of active ingredients of the medicine preferably more than 45%, more preferably more than 55%. The invention also provides a preparation method of the water suspending agent, which comprises the following steps: mixing bifenthrin, fluopicolide, a dispersing agent, a wetting agent, a defoaming agent, an antifreezing agent, a preservative, a thickening agent and water, uniformly stirring, and then crushing the uniformly mixed materials by a wet method to obtain the water suspending agent containing bifenthrin and fluopicolide.

Furthermore, in the preparation method, the temperature is controlled to be 20-30 ℃ when the materials are ground by a wet method. By controlling the low temperature and selecting the auxiliary agent, the effective components can be more stable in the preparation process.

Furthermore, the water suspending agent has good control effect on grub, cotton bollworm, cotton red spider, thrips, wireworm, flea beetle, leaf beetle and other pests, and on various diseases such as potato black rot, wheat sharp eyespot, rice sheath blight, rape sclerotinia rot, wheat loose smut, wheat stinking smut, corn small leaf spot, corn head smut and the like of crops, and can be widely applied to the crops such as wheat, corn, peanut, potato, rape and the like, but not only to the listed crops, but also to other crops.

Furthermore, the invention also provides the application of the water suspending agent in the seed treatment or leaf treatment of crops, such as wheat, peanut, corn, rape, potato and the like, but the water suspending agent is not only applicable to the above listed crops, but also applicable to other crops. The water suspending agent can be used for seed dressing treatment before seeding of crop seeds or seed blocks, can also be used for treatment of crop leaves, and is convenient to use. After the aqueous suspension agent is used, the effects of killing insects and bacteria can be achieved, the occurrence rate of crop diseases and insect pests is reduced, and the crop yield can be improved to a certain extent.

Furthermore, the leaf treatment by the aqueous suspension agent generally refers to leaf spraying treatment, and the method for the leaf spraying treatment comprises the following steps: adding a proper amount of water into the aqueous suspension agent to dilute and uniformly stir the aqueous suspension agent into liquid medicine, and uniformly spraying the liquid medicine onto the leaves of the crops by adopting a spraying device. When the seed dressing treatment is carried out on the water suspending agent, the method comprises the following steps: diluting the aqueous suspension with appropriate amount of water, and mixing with seed or seed block under stirring.

The invention has the following beneficial effects:

1. the bifenthrin and the fluopicolide are compounded and prepared into the water suspending agent, the compatibility and the stability of the bifenthrin and the fluopicolide are improved through the selection of an auxiliary agent system, particularly the selection of a dispersing agent and a wetting agent, and the water suspending agent has the advantages of high suspension rate, good dispersibility in water, high uniformity, good drug effect, good heat storage stability, low-temperature storage resistance, safety, low toxicity and the like, and particularly still has good suspension rate and stability when the drug content is high.

2. In the water suspending agent, the bifenthrin and the flufenitrofen are compounded to have good synergistic effect, the compatibility of the bifenthrin and the flufenitrofen is good, the bifenthrin and the flufenitrofen are mutually mixed and can not generate conflict, the double killing of diseases and pests can be realized, the water suspending agent can be widely used for crops such as wheat, corn, peanut, potato, rape and the like, and the water suspending agent can be used for controlling pests such as grubs, cotton bollworms, cotton red spiders, thrips, wireworms, flea beetles, leaf beetles and the like of the crops and various diseases such as potato black nevus, wheat sharp eyespot, rice sheath blight, sclerotinia sclerotiorum, wheat loose smut, wheat stinking smut, corn small spot, corn head smut and the like of the crops, and compared with a single agent of the bifenthrin and.

3. The water suspension agent provides good growing environment for crops after disinsection and sterilization, and has positive significance for improving the crop yield.

4. The aqueous suspension agent has high suspension rate, good uniformity and good stability, can still keep better stability when the content of the medicament is high, and has simple preparation method process, easy operation, no strict requirement on preparation packaging materials and low cost.

Detailed Description

The technical solution of the present invention is further illustrated below with reference to specific examples, but the essence of the present invention is not limited to the following examples, which should not be construed as limiting the scope of the present invention. Unless otherwise specified, the following components are contained in weight percentage.

Example 130% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 20% of bifenthrin and 10% of fluopyram; 2% of dispersant styrene maleic anhydride polymer sodium salt and 2% of polyoxyethylene-polyoxypropylene block copolymer; 1% of sodium dodecyl sulfate and 1% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1 percent of defoaming agent glycerol polyoxyethylene ether; 4% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water makes up to 100%.

The preparation method comprises the following steps: putting bifenthrin, fluopyram, a dispersing agent, a wetting agent, a defoaming agent, an antifreezing agent, a preservative, a thickening agent and water into a stirring tank, stirring for 30 minutes to uniformly mix the materials, then crushing the materials at 20-35 ℃ by a wet method, sieving the crushed materials by a 100-mesh sieve, and subpackaging to obtain the finished product of the water suspending agent.

Example 240% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 30% of bifenthrin and 10% of fluopyram; 2% of dispersant styrene maleic anhydride acrylate polymer ammonium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer; 1% of sodium dodecyl sulfate and 2% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1 percent of defoaming agent high alcohol fatty acid ester compound; 4% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent bentonite; water makes up to 100%. The preparation method is the same as example 1.

Example 350% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 35% of bifenthrin and 15% of fluopyram; 3% of dispersing agent styrene, acrylic acid and methacrylic acid copolymer sodium salt and 3% of polyoxyethylene-polyoxypropylene block copolymer; 2% of sodium dodecyl sulfate and 2% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1 percent of defoaming agent glycerol polyoxyethylene ether; 4% of antifreeze glycol; 0.1% of preservative sodium benzoate; 0.1 percent of thickening agent magnesium aluminum silicate type SM gel; water makes up to 100%. The preparation method is the same as example 1.

Example 440% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 20% of bifenthrin and 20% of fluopyram; 2% of dispersant styrene maleic anhydride acrylate polymer ammonium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer; 1% of sodium dodecyl sulfate and 3% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1% of defoaming agent organic silicone; 4% of antifreeze propylene glycol; 0.1% of preservative potassium sorbate; 0.1% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

Example 550% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 30% of bifenthrin and 20% of fluopyram; 3% of dispersant styrene maleic anhydride acrylate polymer ammonium salt and 5% of polyoxyethylene-polyoxypropylene block copolymer; 3% of sodium dodecyl sulfate and 5% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1 percent of defoaming agent glycerol polyoxyethylene ether; 6% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

Example 660% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 45% of bifenthrin and 15% of fluopyram; 3% of dispersant styrene maleic anhydride acrylate polymer ammonium salt and 3% of polyoxyethylene-polyoxypropylene block copolymer; 2% of sodium dodecyl sulfate and 2% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1 percent of defoaming agent glycerol polyoxyethylene ether; 5% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

Example 770% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 50% of bifenthrin and 20% of fluopyram; 3% of dispersant styrene maleic anhydride acrylate polymer ammonium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer; 3% of sodium dodecyl sulfate and 4% of sodium alkylphenol polyoxyethylene ether sulfate serving as wetting agents; 0.1% of defoamer C10-C20 saturated aliphatic carboxylic ester; 7% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

Example 875% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 55% of bifenthrin and 20% of fluopyram; 4% of dispersing agent styrene maleic anhydride polymer sodium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer; 4% of sodium dodecyl sulfate and 4% of sodium alkylphenol polyoxyethylene ether sulfate as wetting agents; 0.1% of defoaming agent C8-C10 fatty alcohol; 8% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent kaolin; water makes up to 100%. The preparation method is the same as example 1.

Example 925% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 20% of bifenthrin and 5% of fluopyram; 2% of dispersant polyoxyethylene-polyoxypropylene block copolymer; wetting agent a-sulfo fatty acid methyl ester 1%; 0.1 percent of defoaming agent high alcohol fatty acid ester compound; 3% of antifreeze glycerol; 0.1% of preservative dehydroacetic acid; 1% of thickening agent white carbon black; water makes up to 100%. The preparation method is the same as example 1.

Example 1085% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 60% of bifenthrin and 25% of fluopyram; 5% of dispersant sodium lignosulfonate and 5% of naphthalene sulfonic acid formaldehyde condensate sodium salt; wetting agent sodium dodecyl benzene sulfonate 3%, fatty acid ester sodium sulfate 3%, nekal BX 4%; 0.2% of defoaming agent organic silicone; 8% of antifreeze glycol; 1% of preservative sodium benzoate; 1% of thickening agent magnesium aluminum silicate type SM gel; water makes up to 100%. The preparation method is the same as example 1.

Example 1160% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 45% of bifenthrin and 15% of fluopyram; dispersing agent tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt 6.5%, styrylphenol polyoxyethylene ether phosphate 3.5%; wetting agent fatty acid sodium sulfate 1%, sodium dodecyl sulfate 1%; 1% of defoamer C10-C20 saturated aliphatic carboxylic ester; 5% of antifreeze glycerol; 1% of preservative sodium nitrite; 0.16% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

Example 1275% Biphenthrin Fluopyram aqueous suspension

The formula is as follows: 50% of bifenthrin and 20% of fluopyram; 5% of dispersant ethylene oxide-propylene oxide block copolymer and 5% of alkylphenol polyoxyethylene phosphate; wetting agent fatty acid sulfate 5%, alpha-olefin sodium sulfonate 5%; 1% of defoaming agent organic silicone; 8% of antifreeze glycerol; 0.1% of preservative potassium sorbate; 1% of thickening agent bentonite; water makes up to 100%. The preparation method is the same as example 1.

Comparative example

The formula is as follows: 45% of bifenthrin and 15% of fluopyram; 6 percent of dispersant dioctyl sodium sulfosuccinate; wetting agent sodium lauryl ether sulfate 4%; 0.1 percent of defoaming agent glycerol polyoxyethylene ether; 5% of antifreeze propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water makes up to 100%. The preparation method is the same as example 1.

The finished products prepared in the above examples and comparative examples are tested for suspension rate, uniformity and stability, the suspension rate is tested by GB/T14825-2006, and the stability is tested by GB/T19136-2003.

The uniformity detection method comprises the steps of subpackaging samples with 10cm high sample bottles, standing uniformly, then respectively sampling the bottom and the upper parts of the samples with a micro-sampler, and respectively sampling the bottom and the upper parts of the samples to detect the content of active ingredients, wherein uniformity is not= (upper content/bottom content) × 100%.

The results of the measurements are shown in Table 1 below.

From the data in the table, the suspension rate and the uniformity of the products in each example are all over 83%, the products are all qualified, and the products have the characteristics of high suspension rate, high uniformity, good stability, no crystallization after thermal storage and the like, wherein the products in examples 1 to 8 have better performance and good thermal storage stability, and the product in example 6 has the best performance. The product of the comparative example has poor heat storage stability and low suspension rate, and a large amount of crystals are separated out by microscopic examination, which is not qualified.

From examples 1-8, with the preferred dispersing and wetting agents selected, the performance of the resulting aqueous suspension products varied from 30-75% of the active pharmaceutical ingredient, indicating that the drug content had some effect on the dosage form performance. It can be seen from examples 9 to 12 that in the case of conventional dispersants and wetting agents, the resulting aqueous suspensions show a relatively reduced performance, and that there is no significant improvement in the replacement of the dispersants and wetting agents, indicating that the dispersants and wetting agents are preferred to provide a significant improvement in the performance of the aqueous suspensions, and that conventional adjuvants are absent.

Field efficacy test determination of bifenthrin-fluopyram water suspending agent

1. Test material

The corn variety to be tested is chat jade 22. The application period is adult plant period, and the maize head smut and thrips are artificially inoculated.

The test agents were bifenthrin-fenfluramine aqueous suspensions obtained in examples 1-12 and comparative examples.

2. Experimental methods

2.1 design of the experiment

The test was carried out in 2018 in a corn field in a coastal economic development area of the Weifang city in Shandong province. Dividing the corn field into zones, and arranging in random block groups for 4 times, wherein the area of each zone is 66.7m². The corn field is provided with 4 treatments which are respectively as follows: treatment 1: no drug application treatment is carried out, and the blank control is used; and (3) treatment 2: carrying out foliar spray treatment using the bifenthrin-fluoxafen aqueous suspension agents obtained in examples 1-12 and comparative example respectively; and (3) treatment: carrying out foliar spray treatment by using 40wt% of bifenthrin water suspending agent (self-made, the formula comprises 40% of bifenthrin as an active pesticide ingredient, 2% of styrene maleic anhydride acrylate polymer ammonium salt and 4% of polyoxyethylene-polyoxypropylene block copolymer, 2% of lauryl sodium sulfate and 2% of alkylphenol polyoxyethylene ether sodium sulfate as wetting agents, 0.1% of glycerol polyoxyethylene ether as a defoaming agent, 5% of propylene glycol as an antifreeze agent, 0.1% of paraformaldehyde as an antiseptic, 0.1% of xanthan gum as a thickening agent and the balance of water being 100%); and (4) treatment: carrying out leaf surface spraying treatment by using 15% fluopyram aqueous suspending agent (self-made formula: 15% of pesticide active ingredient fluopyram, 2% of styrene maleic anhydride acrylate polymer ammonium salt and 4% of polyoxyethylene-polyoxypropylene segmented copolymer, 2% of lauryl sodium sulfate and 2% of alkylphenol polyoxyethylene ether sodium sulfate as wetting agent, 0.1% of defoaming agent glycerol polyoxyethylene ether, and antifreezing agent5% of propylene glycol; 0.1% of preservative paraformaldehyde; 0.1% of thickening agent xanthan gum; water to make up 100%).

And in the adult stage of the corn, counting the number of plants in each cell, and processing the corn plants in an artificial inoculation mode to ensure that each corn plant has the maize head smut and the thrips. After 6 days, the corn plants were subjected to a drug application treatment. And (3) spraying different medicinal preparations to the corn fields treated 2-4, and spraying the same amount of clear water to the corn fields treated 1 as a control. When the pesticide is sprayed, the pharmaceutical preparations are diluted by water and stirred uniformly to form liquid medicine, and then the liquid medicine is uniformly sprayed on the surface of the leaf surface. The weather is good during the test period, and the daily average temperature is 20-26.0 ℃. No rain is produced on the day of application, and no rain is produced 15 days after application. Counting the number of diseased plants and the number of insect plants except for the inoculation point of the plants 30 days after the pesticide application, and counting the number of survival plants of the plants.

2.2 survey items

And (4) investigating the plant survival rate, the corn head smut and the diseased plant rate and the insect plant rate caused by the corn thrips.

Corn head smut and thrips investigation method: after 30 days of application, the number of strains with the maize head smut and thrips except the inoculation point in each plot was investigated, and the disease strain rate, the insect strain rate and the control effect were calculated.

Disease strain rate/insect strain rate (%) = number of diseased strains (number of insect pests strains)/total number of strains in cell × 100%

The control effect =100% -the disease strain rate/insect strain rate.

Plant survival rate (%) = plant survival number/cell stock number × 100% 30 days after drug administration

3. Test results and analysis

As can be seen from Table 2, the product of the invention has the performance of treating both pests and diseases, which is not possessed by bifenthrin aqueous suspending agent or fluopicolide aqueous suspending agent. As can be seen from the data in Table 2, the two effective components have a synergistic effect with each other, and the selection of the auxiliary agent of the invention has a good effect of improving the drug effect by comparing the comparative example with the example, and the example 6 has the best synergistic effect in disinsection and sterilization.

The above is a detailed description of the technical solutions of the present invention, and it should be understood that the above-described specific embodiments are only for explaining the present invention, and are not intended to limit the present invention. Obvious variations or modifications which are within the spirit of the invention are possible within the scope of the invention.

Claims

1. The aqueous suspension containing bifenthrin and fluopicolide is characterized by comprising the following components in percentage by weight: 20-60% of bifenthrin, 5-25% of fluopicolide, 2-10% of a dispersing agent, 1-10% of a wetting agent, 0.1-1% of a defoaming agent, 3-8% of an antifreezing agent, 0.1-1% of a preservative, 0.1-1% of a thickening agent and the balance of water to 100%.

2. The aqueous suspension concentrate of claim 1, which is prepared from the following components in percentage by weight: 25-55% of bifenthrin, 10-20% of fluopicolide, 4-8% of dispersing agent, 2-8% of wetting agent, 0.1-0.2% of defoaming agent, 4-8% of antifreezing agent, 0.1-0.2% of preservative, 0.1-0.2% of thickening agent and the balance of water to 100%.

3. An aqueous suspension according to claim 1 or 2, characterized in that: the total content of bifenthrin and fluopicolide in the aqueous suspension is 30-75wt%, preferably 45-75 wt%, more preferably 55-75 wt%, and more preferably 60-75 wt%.

4. An aqueous suspension according to claim 1, 2 or 3 wherein: the mass ratio of bifenthrin to fluopicolide is 2-6:1, and preferably 3: 1.

5. An aqueous suspension according to claim 1 or 2, characterized in that: the content of bifenthrin in the aqueous suspension is 45wt%, and the content of fluopicolide in the aqueous suspension is 15 wt%.

6. The aqueous suspension concentrate of claim 1, which is prepared from the following components in percentage by weight: 45% of bifenthrin, 15% of fluopyram, 6% of a dispersing agent, 4% of a wetting agent, 0.1% of a defoaming agent, 5% of an antifreezing agent, 0.1% of a preservative, 0.1% of a thickening agent and the balance of water to 100%.

7. An aqueous suspension according to any one of claims 1 to 6 wherein: the dispersing agent is one or more of sodium lignosulfonate, styryl phenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether phosphate, styryl phenol polyoxyethylene ether sulfonate, polyoxyethylene-polyoxypropylene block copolymer, polycarboxylate, tristyryl phenol polyoxyethylene ether phosphate triethanolamine salt, naphthalene sulfonic acid formaldehyde condensate sodium salt and ethylene oxide-propylene oxide block copolymer; the wetting agent is one or more of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, a-olefin sodium sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, nekal BX, fatty acid sulfate and fatty acid ester sulfate; the defoaming agent is one or more of glycerol polyoxypropylene ether, a high-carbon alcohol fatty acid ester compound, organic silicone, C8-C10 fatty alcohol, C10-C20 saturated aliphatic carboxylic acid and C10-C20 saturated aliphatic carboxylic ester; the antifreezing agent is one or more of ethylene glycol, propylene glycol and glycerol; the preservative is one or more of paraformaldehyde, sodium nitrite, sodium benzoate, potassium sorbate and dehydroacetic acid; the thickener is one or more of xanthan gum, bentonite, kaolin, magnesium aluminum silicate type SM gel and white carbon black.

8. The aqueous suspension according to claim 7, characterized in that: the dispersing agent is prepared from the following components in a mass ratio of 1: 1-2 and a mixture of a polycarboxylate and a polyoxyethylene-polyoxypropylene block copolymer; the wetting agent is a mixture of sodium dodecyl sulfate and sodium alkylphenol polyoxyethylene ether sulfate in a mass ratio of 1: 1-3; the defoaming agent is glycerol polyoxyethylene ether; the antifreezing agent is propylene glycol; the preservative is paraformaldehyde; the thickening agent is xanthan gum.

9. A process for the preparation of an aqueous suspension concentrate containing bifenthrin and fluoxafen as claimed in any one of claims 1 to 8, characterized by comprising the steps of: mixing bifenthrin, fluopicolide, a dispersing agent, a wetting agent, a defoaming agent, an antifreezing agent, a preservative, a thickening agent and water, uniformly stirring, and then crushing the uniformly mixed materials by a wet method to obtain a water suspending agent containing bifenthrin and fluopicolide; preferably, the temperature during pulverization is controlled to 20 to 30 ℃.

10. Use of a bifenthrin and fenfluramine-containing aqueous suspension formulation as claimed in any one of claims 1 to 8 in seed treatment or foliar treatment of crops; preferably, the seed treatment refers to seed dressing treatment before the bifenthrin and fluopicolide-containing water suspension is used for sowing of crop seeds or seed blocks; preferably, the crop comprises wheat, peanut, corn, canola or potato.