CN108552183B - Pyrazolyl cloquintocet-mexyl suspension seed coating agent and application thereof - Google Patents
Pyrazolyl cloquintocet-mexyl suspension seed coating agent and application thereof Download PDFInfo
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- CN108552183B CN108552183B CN201810241669.8A CN201810241669A CN108552183B CN 108552183 B CN108552183 B CN 108552183B CN 201810241669 A CN201810241669 A CN 201810241669A CN 108552183 B CN108552183 B CN 108552183B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C1/00—Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
- A01C1/06—Coating or dressing seed
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
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Abstract
The invention relates to a mefenpyr-diethyl suspension seed coating agent and application thereof. The mefenpyr-diethyl suspension seed coating agent comprises the following components in parts by weight: 5-80 parts of mefenpyr-diethyl, 0.1-10 parts of wetting agent, 0.1-10 parts of dispersing agent, 0.1-5 parts of thickening agent, 1-5 parts of film forming agent, 0.1-10 parts of antifreezing agent, 0.1-5 parts of defoaming agent, 0.1-5 parts of warning agent, 0.1-5 parts of preservative and the balance of deionized water. The mefenpyr-diethyl suspension seed coating agent provided by the invention meets the quality standard of the suspension seed coating agent, the mefenpyr-diethyl suspension seed coating agent provided by the invention is adopted for seed treatment, and is matched with herbicide spraying, compared with the existing mixed spraying technology of mefenpyr-diethyl and herbicide, the mefenpyr-diethyl suspension seed coating agent can obviously improve the drug resistance of crops to the herbicide, improve the weed control effect of the herbicide and reduce the dosage of the herbicide.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a mefenpyr-diethyl suspension seed coating agent and application thereof.
Background
According to the report, the area of wheat field weeds in China accounts for more than 55% of the planting area, the area of serious damage accounts for 28%, the average yield loss reaches 15%, wherein the wheat field grassy weeds such as the Jiejiemai have the problem that the area is rapidly enlarged in recent years, so that the wheat is seriously reduced in yield and even never harvested. Meanwhile, with the continuous improvement of labor cost in China, the weed harm control in wheat fields by using the herbicide becomes a necessary measure for wheat production. However, the gramineous weeds in wheat fields such as the jiejie are close to the relativity of wheat, so that the herbicide is difficult to obtain high selectivity between the wheat and the gramineous weeds, and the herbicide for preventing and controlling the gramineous weeds in the wheat fields is seriously deficient. At present, the herbicide for effectively preventing and controlling the jiezhimao in China only contains mesosulfuron-methyl, but the mesosulfuron-methyl has higher risk of phytotoxicity to wheat and is easy to generate phytotoxicity, so that a safener pyraclofen-ethyl is usually added into a mesosulfuron-methyl preparation, and the two are sprayed in a mixed manner to protect the wheat and improve the drug resistance of the wheat to the mesosulfuron-methyl without influencing weeds such as wild oats.
However, the applicant finds through research that the pyracloquintocet-mexyl serving as a safener and a herbicide are mixed for spraying and used, and the following problems exist: (1) although the mefenpyr-diethyl has no influence on weeds such as wild oat, the mefenpyr-diethyl has a protection effect on weeds such as arthroncus sylvestris and the like, and can improve the drug resistance of the mefenpyr-diethyl to herbicides, so that the control effect of the herbicides on the weeds such as the arthroncus sylvestris is reduced, and finally the dosage of the herbicides is greatly increased. (2) The compound has strong specificity on the parts which can be absorbed by plants and the conduction direction in plants, for example, ethirimol and analogues thereof can effectively prevent apple powdery mildew by spraying stem leaves, but is ineffective when being applied from roots. At present, the mefenpyr-diethyl is added into a herbicide preparation in a using mode, and the mefenpyr-diethyl can be sprayed by stems and leaves to play a role through the absorption of the stems and leaves, but the report on whether the mefenpyr-diethyl has activity and the effect when being used for other application parts of crops is not found. (3) The melting point of the mefenpyr-diethyl raw pesticide is 50-52 ℃, and the mefenpyr-diethyl raw pesticide belongs to a low-melting raw pesticide. The problems of layering, solidification and suspension rate reduction are easy to occur after the low-melting-point raw medicine is prepared into the suspending agent.
Disclosure of Invention
In order to solve the technical problems, the invention provides the mefenpyr-diethyl suspended seed coating agent which not only improves the drug resistance of wheat to herbicides, but also can improve the control effect of the herbicides on weeds such as jiejia and the like and reduce the dosage of the herbicides. In addition, the suspension seed coating agent also has the characteristic of good stability.
The invention is realized by adopting the following technical scheme.
The mefenpyr-diethyl suspension seed coating agent comprises the following components in parts by weight:
5-80 parts of mefenpyr-diethyl,
0.1 to 10 parts of a wetting agent,
0.1 to 10 parts of a dispersant,
0.1 to 5 parts of a thickening agent,
1-5 parts of a film-forming agent,
0.1 to 10 parts of an antifreezing agent,
0.1 to 5 parts of a defoaming agent,
0.1 to 5 parts of a warning agent,
0.1 to 5 parts of a preservative,
the balance of deionized water.
Preferably, the mefenpyr-diethyl suspension seed coating agent comprises the following components in parts by weight:
10-50 parts of mefenpyr-diethyl,
1-7 parts of a wetting agent,
1-7 parts of a dispersing agent,
0.1 to 3 parts of a thickening agent,
1-3 parts of a film-forming agent,
1-5 parts of an anti-freezing agent,
0.5 to 3 parts of a defoaming agent,
0.1 to 2 parts of a warning agent,
0.5 to 3 parts of a preservative,
the balance of deionized water.
More preferably, the mefenpyr-diethyl suspension seed coating agent consists of the following components in percentage by weight: 30% of mefenpyr-diethyl, 4% of wetting agent, 5% of dispersing agent, 1.1% of thickening agent, 2% of film forming agent, 2% of antifreezing agent, 1.5% of defoaming agent, 0.5% of warning agent, 1% of preservative and the balance of deionized water.
In the mefenpyr-diethyl suspension seed coating agent, the wetting agent can be one or more of styrylphenol polyoxyethylene polyoxypropylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, benzyl dimethyl phenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, 9-octadecylamine, castor oil polyoxyethylene ether, nekal (diisobutyl naphthalene sodium sulfonate), sodium dodecyl benzene sulfonate, sodium lauryl sulfate, dioctyl sodium succinate sulfonate, sodium diisopropyl naphthalene sulfonate and tridecanol polyoxyethylene ether; preferably, the wetting agent can be one or more of alkylphenol formaldehyde resin polyoxyethylene ether, nonylphenol polyoxyethylene ether and castor oil polyoxyethylene ether; more preferably, the wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether.
The dispersant may be one or more of sodium lignosulfonate, calcium lignosulfonate, ammonium lignosulfonate, NNO (sodium naphthalenesulfonate formaldehyde condensate), NO (sodium dibutylnaphthalenesulfonate formaldehyde condensate), a dispersing agent MF (sodium methylnaphthalenesulfonate formaldehyde condensate), nekal (sodium diisobutylnaphthalenesulfonate), a fatty alcohol ethylene oxide adduct phosphate, an alkylphenol polyoxyethylene ether phosphate, SOPA (alkylphenol polyoxyethylene ether formaldehyde condensate sulfate), a polyoxyethylene polyoxypropylene ether block copolymer, alkylphenol polyoxyethylene phosphate, gum arabic, lecithin, carboxymethylcellulose, polyvinyl alcohol, polyvinylpyrrolidone, and polyethylene glycol; preferably, the dispersant may be: one or more of sodium lignosulfonate, NNO, polyoxyethylene polyoxypropylene ether block copolymer, alkylphenol polyoxyethylene phosphate and polyvinylpyrrolidone; more preferably, the dispersant is NNO and/or a polyoxyethylene polyoxypropylene ether block copolymer.
The thickener can be one or more of gypsum, clay, magnesium aluminum silicate, water glass, sodium carboxymethyl starch, soluble starch, sodium carboxymethyl cellulose, sodium alginate, agar, xanthan gum, hydroxyethyl cellulose and bentonite; preferably, the thickener can be one or more of magnesium aluminum silicate, xanthan gum, sodium alginate and hydroxyethyl cellulose; more preferably, the thickener is magnesium aluminium silicate and/or xanthan gum.
The film forming agent can be one or more of sodium alginate, agar, polyvinyl alcohol, polyethylene glycol, polyvinyl acetate, polyacrylamide, polyvinyl acetate, polyvinylpyrrolidone, poly (methyl) acrylic acid derivatives, polyalcohol polymers, ethyl cellulose, light propyl cellulose, polyvinyl acetate lactone and polyacrylamide; preferably, the film forming agent can be one or more of polyvinyl alcohol, polyethylene glycol and polyacrylamide; more preferably, the film-forming agent is polyethylene glycol.
The antifreezing agent can be one or more of ethylene glycol, propylene glycol, glycerol, urea, glycerol-diethyl ether diglycol and methyl propylene diglycol; preferably, the antifreeze can be one or more of ethylene glycol, glycerol and urea; more preferably, the antifreeze agent is urea.
The defoaming agent can be one or more of isooctyl alcohol, isoamyl alcohol, stearic acid and lauric acid; preferably, the antifoaming agent is isooctanol.
The warning agent can be one or more of acid scarlet, alkaline rose essence and Rudaming 2B; preferably, the warning agent is rhodamine.
The preservative can be one or more of formaldehyde, sodium salicylate, sodium benzoate, 1, 2-benzothiazolin-3-one, 2-hydroxybiphenyl, sorbic acid, benzoic acid, benzaldehyde, p-hydroxybenzaldehyde, p-hydroxybenzyl ester and isothiazolinone (carbazone); preferably, the preservative is an isothiazolinone.
The various starting materials and reagents used in the present invention are commercially available and readily available. For example, the mefenpyr ester original drug can be purchased from Jiangsu Tianfu group GmbH, alkylphenol formaldehyde resin polyoxyethylene ether (Nongru No. 700) is purchased from Hebei Yancheng chemical auxiliary agent GmbH, NNO is purchased from Guangzhou city, Chuang chemical engineering technology GmbH, and polyoxyethylene polyoxypropylene ether block copolymer (polyether F-68) is purchased from Santana chemical engineering (Nantong) GmbH.
The mefenpyr-diethyl suspension seed coating agent can be prepared by adopting a conventional suspension seed coating agent preparation method in the field.
In the invention, the preparation method of the mefenpyr-diethyl suspension seed coating agent comprises the following steps:
sieving the above materials (such as 320 mesh), mixing with deionized water at a certain proportion, high-speed stirring for pre-dispersing for 30min, controlling system at below 45 deg.C, and removing impurities. Preferably, a sand mill is adopted for sanding, the sanding medium is zirconium beads, the coefficient of the medium is 1, the sanding time is 2.5 hours, and the sanding temperature is controlled below 45 ℃.
The invention also provides application of the mefenpyr-diethyl suspension seed coating agent in preventing and controlling weeds in wheat fields. The method specifically comprises the following steps: and coating the wheat seeds by using the mefenpyr-diethyl suspension seed coating agent.
The wheat field weeds mainly comprise gramineous weeds, broadleaf weeds and cyperaceae weeds. Preferably, the weeds in the wheat field are selected from one or more of jiejie, brome, canary grass, alopecurus, bluegrass, beckmark beck, stiff grass, club grass, lolium multiflorum, poison wheat, candlelia, aegilops tauschii, aegilops cylindrica, descurainia, shepherd's purse, alopecurus, hordei, goosegrass, goosefoot, beefwood, sedge and the like. More preferably, the weeds in the wheat field are the jointed wheat and/or the descurainia sophia.
In specific application, the dosage of the active ingredient of the mefenpyr-diethyl suspension seed coating agent is 1-2000g/100kg of seeds. Preferably, the usage amount of the mefenpyr-diethyl suspension seed coating agent is 10-1000g/100kg of seeds. More preferably, the usage amount of the mefenpyr-diethyl suspension seed coating agent is 20-500g/100kg of seeds.
In specific application, the dosage of the mefenpyr-diethyl suspension seed coating agent is 1.875-3750g/hm2(ii) a Preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 18.75-1875g/hm2(ii) a Further preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 37.5-937.5g/hm2(ii) a More preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 45-375g/hm2。
When the mefenpyr-diethyl suspending seed coating agent is specifically applied, the mefenpyr-diethyl suspending seed coating agent is matched with the mesosulfuron for use, and if the mefenpyr-diethyl suspending seed coating agent is firstly used for coating seeds and then the mesosulfuron is sprayed, a better effect can be obtained; preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 1.875-3750g/hm2(ii) a Further preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 18.75-1875g/hm2(ii) a Still more preferably, the usage amount of the mefenpyr-diethyl suspension seed coating agent is 37.5-937.5g/hm2(ii) a More preferably, the dosage of the mefenpyr-diethyl suspension seed coating agent is 45-375g/hm2(ii) a The amount of mesosulfuron is 8-20ghm2It is preferable.
The invention has the following positive and beneficial effects:
1. the mefenpyr-diethyl suspension seed coating agent disclosed by the invention is matched with a herbicide to be used for preventing and controlling weeds in a wheat field, and through coating treatment on wheat seeds, the mefenpyr-diethyl is prevented from protecting the weeds such as the jointed wheat, the prevention and control effect of the herbicide on the weeds such as the jointed wheat can be obviously improved, and the dosage of the herbicide is reduced.
2. According to the invention, through a large number of screening and research, the mefenpyr-diethyl suspension seed coating agent with qualified quality is prepared, and the problems that the formulation of the mefenpyr-diethyl suspension seed coating agent is easy to delaminate, solidify and reduce the suspension rate are solved;
3. the mefenpyr-diethyl suspension seed coating agent disclosed by the invention is matched with a herbicide to prevent and control weeds in a wheat field, so that the drug resistance of wheat to the herbicide can be obviously improved, and the phytotoxicity of the herbicide is reduced;
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications.
The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Unless otherwise specified, all percentages in all examples and experimental examples of the present invention are by weight.
Example 130% mefenpyr-diethyl suspension seed coating
The formula comprises the following components in percentage by mass:
30% of mefenpyr-diethyl, 4% of alkylphenol formaldehyde resin polyoxyethylene ether, 2% of NNO, 3% of polyoxyethylene polyoxypropylene ether block copolymer, 1% of magnesium aluminum silicate, 0.1% of xanthan gum, 2% of polyethylene glycol, 2% of urea, 1.5% of isooctanol, 0.5% of rose essence, 1% of isothiazolinone and the balance of deionized water.
Example 210% mefenpyr-diethyl suspension seed coating
The formula comprises the following components in percentage by mass:
10% of mefenpyr-diethyl, 2% of nonylphenol polyoxyethylene ether, 1% of NNO, 1% of alkylphenol polyoxyethylene phosphate, 0.5% of magnesium aluminum silicate, 0.1% of hydroxyethyl cellulose, 3% of polyvinyl alcohol, 5% of ethylene glycol, 1% of isoamyl alcohol, 1% of acid scarlet, 1.5% of sorbic acid and the balance of deionized water.
Example 340% mefenpyr-diethyl suspension seed coating
The formula comprises the following components in percentage by mass:
40% of mefenpyr-diethyl, 8% of castor oil polyoxyethylene ether, 4% of sodium lignosulfonate, 5% of alkylphenol polyoxyethylene phosphate, 2% of sodium alginate, 3% of polyacrylamide, 3% of glycerol, 2% of lauric acid, 2B 2% of damine, 2% of benzoic acid and the balance of deionized water.
Effect test 1:
the invention also provides a series of auxiliary agent comparison tests for verifying the remarkable effect of specific selection of each auxiliary agent in the mefenpyr-diethyl suspension seed coating agent in the embodiment 1 of the invention.
1. Wetting agent, dispersant comparative test
(1) Wetting agent and dispersant prescreening
And (4) adopting a flow point method to carry out primary screening on the wetting agent and the dispersing agent. Dissolving a wetting agent or a dispersing agent in water, fixing the volume of the solution to prepare an aqueous solution with the mass fraction of 5%, accurately weighing 2.0000g of pre-crushed mefenpyr-diethyl technical material in a 20mL test tube, and weighing the mass of the test tube; 5% of wetting agent or dispersant aqueous solution is dripped drop by drop, a few drops of wetting agent or dispersant aqueous solution are added for mixing by ultrasonic wave, when the dope can just slide down along the wall of the test tube, the mass of the dope is called, the mass difference (m) between the front and the back is the mass of the dripped wetting agent or dispersant solution, the flow point of the wetting and dispersant to the mefenpyr-diethyl can be expressed by dividing m by the mass of the original drug, and the smaller the flow point is, the better the wetting and dispersing effects are. The same wetting agent and dispersant were tested 3 times separately and the average was taken.
TABLE 1 Pre-screening results for mefenpyr-diethyl suspension seed coating wetting agent and dispersant (pour-point method)
The results of the primary screening of the wetting agent and dispersant are shown in Table 1. The wetting agents with small flow point (less than 1.00), namely castor oil polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, dispersant NNO, polyoxyethylene polyoxypropylene ether block copolymer, polyvinylpyrrolidone, sodium lignosulfonate and alkylphenol polyoxyethylene phosphate are selected for further test.
(2) Screening of wetting agent and dispersant
And (4) further screening the primarily screened wetting agent and dispersing agent by adopting a trial method to determine the specific types. Combining the wetting agent and the dispersing agent which are primarily screened out in different modes, mixing the wetting agent and the dispersing agent with 30g of mefenpyr-diethyl (fennel-butyl), adding water to 100g, taking zirconium beads as a medium, controlling the medium coefficient to be 1, sanding for 2.5h, and controlling the sanding temperature to be below 45 ℃ to prepare 30% mefenpyr-diethyl suspension. The types of the wetting agent and the dispersing agent are determined by taking the suspension percentage, the viscosity and the dispersibility as indexes.
The dispersibility is measured by adopting a visual grading method: a100 mL measuring cylinder is filled with 99.5mL standard hard water, 0.5mL suspension sample to be measured is taken by a pipette, and the suspension sample is dropped into water from a position 5cm away from the water surface of the measuring cylinder, and the dispersion state of the suspension sample is observed. The dispersion was classified into 8 grades according to the quality of the dispersion.
Level 1: can not be automatically dispersed in water, quickly sinks to the bottom in a block shape, and has no turbid liquid;
and 2, stage: the sample can not be automatically dispersed in water and sinks in a lump shape, the sinking speed is slightly reduced, turbid liquid appears, and finally all samples sink to the bottom;
and 3, level: the sample can not be automatically dispersed in water, obvious turbid liquid appears, and part of the sample sinks to the bottom in a bulk shape;
4, level: the sample can be automatically dispersed in water, the particles fall slowly in the form of clusters, 1/3 turbid liquid appears in the measuring cylinder, and part of the sample sinks to the bottom;
and 5, stage: automatically dispersing in water, slowly descending in a cloud cluster, allowing 1/2 turbid liquid to appear in the measuring cylinder, and allowing part of sample to sink to the bottom;
and 6, level: automatically dispersing in water, slowly descending in a cloud cluster, allowing 3/4 turbid liquid to appear in the measuring cylinder, and allowing a small part of sample to sink to the bottom;
and 7, stage: the water automatically disperses in a cloud form in water, no obvious particle groups slowly fall, and the turbid liquid quickly diffuses;
and 8, stage: the water is automatically dispersed in the form of mist, and the turbid liquid is quickly formed.
TABLE 2 screening results (trial and error method) for the type of the suspending agent wetting agent and the dispersant of mefenpyr-diethyl suspension seed coating agent
The screening results of the wetting agent and the dispersant types show that: the wetting agent is nonylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether and castor oil polyoxyethylene ether, and the dispersing agent is NNO, polyoxyethylene polyoxypropylene ether block copolymer and alkylphenol polyoxyethylene phosphate, so that the suspension has high suspension rate (90.4-92.8%), good dispersibility (7-8), moderate viscosity (303-377 mPs & s), and good quality. The suspension obtained when the wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether and the dispersing agent is NNO and polyoxyethylene polyoxypropylene ether block copolymer has the best quality, the dispersibility is 8 grade, the viscosity is moderate (332mPs & s), the suspension rate is 92.4 percent, and the method is preferable in the invention, so that the alkylphenol formaldehyde resin polyoxyethylene ether is used as the wetting agent, and the NNO and polyoxyethylene polyoxypropylene ether block copolymer is used as the dispersing agent for the next test.
(3) Screening of dispersant ratio
The selected dispersant is further screened by trial and error to determine the use ratio. NNO and polyoxyethylene polyoxypropylene ether block copolymer are mixed according to different proportions, 4g of wetting agent alkylphenol formaldehyde resin polyoxyethylene ether and 30g of mefenpyr-diethyl (fennel) are mixed, water is added until the weight is 100g, zirconium beads are used as a medium, the medium coefficient is 1, sanding is carried out for 2.5h, the sanding temperature is controlled below 45 ℃, and then 30% mefenpyr-diethyl suspension is prepared. The optimal proportion of the dispersing agent is determined by taking the suspension percentage, the viscosity and the dispersibility as indexes.
TABLE 3 screening results (trial and error) for pyraclostrobin suspension seed coating dispersant ratio
The screening result of the proportion of the dispersant shows that: when the proportion of the NNO and the polyoxyethylene polyoxypropylene ether block copolymer is 1:2, 1:3, 2:4, 2:5 and 2:6, the suspension rate is high (90.3-93.4%), the dispersibility is good (7-8 grades), the viscosity is moderate (251-362 mPs & s), and the obtained suspension has good quality. Among them, the suspension obtained when the proportion of the NNO and the polyoxyethylene polyoxypropylene ether block copolymer is 2:3 has the best quality, the dispersibility is 8 grade, the viscosity is moderate (340mPs & s), and the suspension rate is 93.4 percent, which is a preferable scheme of the invention, therefore, the weight ratio of the NNO: the next experiment was carried out using a polyoxyethylene polyoxypropylene block copolymer 2:3 as the dispersant.
2. Thickener control test
Screening thickening agents by an empirical method. Mixing different thickeners with 4g of alkylphenol formaldehyde resin polyoxyethylene ether serving as a wetting agent, 2g of NNO serving as a dispersant, 3g of polyoxyethylene polyoxypropylene ether block copolymer and 30g of mefenpyr-diethyl, adding water to 100g, taking zirconium beads as a medium, setting the medium coefficient to 1, sanding for 2.5 hours, and controlling the sanding temperature to be below 45 ℃ to prepare 30% mefenpyr-diethyl suspension. The type of the thickener is determined by taking the viscosity, the suspension percentage and the heat storage stability as indexes.
TABLE 4 screening results of mefenpyr-diethyl suspended seed coating thickener
The screening result of the thickening agent shows that: when the thickening agent is magnesium aluminum silicate, sodium alginate, xanthan gum and hydroxyethyl cellulose, the suspension rate is high (89.5-97.8%), the viscosity is moderate (242-506 mPs & s), the heat storage stability is good, and the quality of the obtained suspension is good (Table 4). The suspension obtained when the ratio of the magnesium aluminum silicate to the xanthan gum is 1:0.1 has the best quality, the suspension rate is 97.3%, the viscosity is moderate (325mPs & s), and the heat storage stability is the preferable scheme of the invention, so the next test is carried out by taking the magnesium aluminum silicate and the xanthan gum (the mass ratio is 1:0.1) as the thickening agent.
3. Comparative tests of the amounts of wetting agent, dispersant and thickener
The interaction among the wetting agent, the dispersing agent and the thickening agent is determined through orthogonal tests, and the final dosage is determined. Respectively mixing a wetting agent (alkylphenol formaldehyde resin polyoxyethylene ether), a dispersing agent (NNO: polyoxyethylene polyoxypropylene ether block copolymer 2:3) and a thickening agent (magnesium aluminum silicate: xanthan gum 1:0.1) with 30g (folded hundred) of mefenpyr-diethyl, adding water to 100g, using zirconium beads as a medium, with the medium coefficient of 1, sanding for 2.5h, and controlling the sanding temperature to be below 45 ℃ to prepare a 30% mefenpyr-diethyl suspension. The dosage of the wetting agent, the dispersant and the thickener is determined by taking the suspension percentage as an index.
TABLE 5 screening results of usage amounts of wetting agent, dispersant and thickener of mefenpyr-diethyl suspension seed coating agent
Note: the wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether, and the dispersant is NNO: polyoxyethylene polyoxypropylene ether block copolymer 2:3, thickening agent magnesium aluminum silicate: xanthan gum is 1: 0.1.
The screening results of the dosage of the wetting agent, the dispersing agent and the thickening agent show that: the suspension percentage was high (90.0% to 98.3%) when the wetting agent, dispersant and thickener were used in amounts of 4% + 5% + 1.1%, 5% + 5% + 0.1%, 3% + 5% + 0.5%, 5% + 4% + 1.1%, 3% + 4% + 0.1%, 4% + 4% + 0.5% and 5% + 6% + 0.5%, and the resulting suspension was good in quality (Table 5). Among them, the next test was carried out using 4% of a wetting agent (alkylphenol formaldehyde resin polyoxyethylene ether), 5% of a dispersant (NNO: polyoxyethylene polyoxypropylene ether block copolymer ═ 2:3), and 1.1% of a thickener (magnesium aluminum silicate: xanthan gum ═ 1:0.1), and the suspension obtained was the best in quality, and the suspension percentage was 98.3%, which is a preferable embodiment of the present invention, and therefore, using 4% of alkylphenol formaldehyde resin polyoxyethylene ether as the wetting agent, NNO 2% + polyoxyethylene polyoxypropylene ether block copolymer 3% as the dispersant, and magnesium aluminum silicate 1% + xanthan gum 0.1% as the thickener.
4. Comparison test of type and dosage of film forming agent
And screening the type and the dosage of the film forming agent by an empirical method. Mixing different film forming agents with 4g of alkylphenol formaldehyde resin polyoxyethylene ether serving as a wetting agent, 2g of NNO serving as a dispersant, 3g of polyoxyethylene polyoxypropylene ether block copolymer, 1g of magnesium aluminum silicate serving as a thickening agent, 0.1g of xanthan gum and 30g (folding to one hundred) of mefenpyr-diethyl, adding water to 100g of the mixture, taking zirconium beads as a medium, setting the medium coefficient to be 1, sanding for 2.5 hours, and controlling the sanding temperature to be below 45 ℃ to prepare 30% mefenpyr-diethyl suspension. And (3) sucking 1mL of the prepared suspension by using a pipette gun, adding 50g of wheat seeds into the culture dish, uniformly shaking the culture dish for 5min by adding a cover, opening the cover, flatly spreading the coated seeds to form a film, observing the surface of the seeds, recording the film forming time (the time required by all seed coatings on the surface of the seeds to be solidified into the film) and measuring the coating uniformity and the shedding rate.
TABLE 6 screening results of the types and amounts of film-forming agents for mefenpyr-diethyl suspension seed coating agent
| Numbering | Film forming agent | Mass fraction/% | Film formation time/min | Degree of uniformity/%) | Rate of fall/%) |
| 1 | Polyvinyl alcohol | 1 | 6 | 86.5 | 9.6 |
| 2 | Polyvinyl alcohol | 2 | 6 | 87.0 | 8.4 |
| 3 | Polyvinyl alcohol | 3 | 6 | 92.9 | 4.8 |
| 4 | Polyvinyl alcohol | 4 | 4 | 92.0 | 1.4 |
| 5 | Polyvinyl alcohol | 5 | 3 | 92.0 | 0.8 |
| 6 | Polyethylene glycol | 1 | 6 | 86.4 | 6.6 |
| 7 | Polyethylene glycol | 2 | 5 | 95.7 | 3.4 |
| 8 | Polyethylene glycol | 3 | 5 | 92.8 | 1.3 |
| 9 | Polyethylene glycol | 4 | 5 | 90.6 | 0.6 |
| 10 | Polyethylene glycol | 5 | 3 | 89.5 | 0.2 |
| 11 | Polyacrylamide | 1 | 6 | 86.9 | 6.6 |
| 12 | Polyacrylamide | 2 | 5 | 86.6 | 6.4 |
| 13 | Polyacrylamide | 3 | 5 | 93.5 | 5.8 |
| 14 | Polyacrylamide | 4 | 4 | 94.6 | 3.2 |
| 15 | Polyacrylamide | 5 | 4 | 86.8 | 2.8 |
The screening results of the types and the dosages of the film forming agents show that: when the dosage of polyvinyl alcohol is 3-5%, the dosage of polyethylene glycol is 2-4% and the dosage of polyacrylamide is 3-4%, the coating uniformity is high (90.6-95.7%), the shedding rate is low (0.2-6.6%), the film forming time is short (3-6 min), and the film forming effect is good (Table 6). Wherein, the uniformity is 95.7 percent when the dosage of the polyethylene glycol is 2 percent, the shedding rate is 3.4 percent, the film forming time is 5min, the dosage is less, the cost is low, and the preferable scheme of the invention is provided, therefore, the next test is carried out by taking 2 percent of the polyethylene glycol as the film forming agent.
5. Comparative test of type and amount of antifreeze
And screening the types and the dosage of the antifreeze by adopting an empirical method. Mixing 4g of alkylphenol formaldehyde resin polyoxyethylene ether serving as a wetting agent and different antifreezing agents, 2g of NNO serving as a dispersant, 3g of polyoxyethylene polyoxypropylene ether block copolymer, 1g of magnesium aluminum silicate serving as a thickening agent, 0.1g of xanthan gum, 2g of polyethylene glycol serving as a film forming agent and 30g (folded) of mefenpyr-diethyl, adding water to 100g, taking zirconium beads as a medium, sanding for 2.5 hours at the medium coefficient of 1, and controlling the sanding temperature to be below 45 ℃ to prepare 30% mefenpyr-diethyl suspension. And (3) placing the prepared suspension at 0 +/-1 ℃ for 7 days, recovering to room temperature after 7 days, and measuring viscosity, suspension rate and screening.
TABLE 7 screening results of the types and amounts of the mefenpyr-diethyl suspended seed coating antifreeze
| Numbering | Antifreezing agent | Mass fraction/% | viscosity/mPs · s | Suspension rate/% | Analysis by sieving/%) |
| 1 | Ethylene glycol | 1 | 322 | 80.0 | 97.7 |
| 2 | Ethylene glycol | 2 | 383 | 91.2 | 98.4 |
| 3 | Ethylene glycol | 3 | 330 | 93.1 | 98.9 |
| 4 | Ethylene glycol | 4 | 299 | 93.3 | 99.6 |
| 5 | Ethylene glycol | 5 | 278 | 93.4 | 99.0 |
| 6 | Glycerol | 1 | 324 | 86.7 | 97.6 |
| 7 | Glycerol | 2 | 424 | 88.6 | 99.4 |
| 8 | Glycerol | 3 | 363 | 89.5 | 99.1 |
| 9 | Glycerol | 4 | 325 | 94.3 | 99.2 |
| 10 | Glycerol | 5 | 419 | 96.4 | 99.9 |
| 11 | Urea | 1 | 347 | 88.7 | 97.6 |
| 12 | Urea | 2 | 373 | 94.9 | 99.7 |
| 13 | Urea | 3 | 262 | 94.8 | 99.0 |
| 14 | Urea | 4 | 403 | 93.8 | 99.7 |
| 15 | Urea | 5 | 397 | 95.4 | 99.1 |
The results of screening the types and the dosages of the antifreezing agents show that: 4 to 5 percent of glycol, 4 to 5 percent of glycerol and 2 to 5 percent of urea, the suspension rate is high (91.2 to 96.4 percent), the sieve analysis is high (99.0 to 99.9 percent) and the viscosity is moderate (Table 7) after cold storage test. Wherein, when the dosage of the urea is 2%, the viscosity is moderate (373mPs & s) after low-temperature storage, the suspension percentage is 94.9%, the sieve analysis is 99.7%, the dosage is small, the cost is low, and the method is the preferable scheme of the invention, therefore, the next test is carried out by taking the urea 2% as the antifreezing agent.
6. Comparative test of the type and amount of the defoaming agent
And screening the type and the dosage of the defoaming agent by an empirical method. Mixing different defoaming agents and wetting agents of 4g of alkylphenol formaldehyde resin polyoxyethylene ether, 2g of dispersing agent NNO, 3g of polyoxyethylene polyoxypropylene ether block copolymer, 1g of thickener magnesium aluminum silicate, 0.1g of xanthan gum, 2g of film-forming agent polyethylene glycol, 2g of antifreezing agent urea and 30g (folded hundred) of mefenpyr-diethyl, adding water to 100g, taking zirconium beads as a medium, controlling the medium coefficient to be 1, sanding for 2.5h, controlling the sanding temperature to be below 45 ℃, preparing 30% of mefenpyr-diethyl suspension, and observing the preparation process and the number of bubbles in the product.
TABLE 8 screening results of the types and amounts of the antifoaming agents for the mefenpyr-diethyl suspension seed coating agent
The screening results of the types and the dosages of the defoaming agents show that: when the amount of isooctanol is 1.0-2.5%, there are fewer bubbles in the preparation process and the product (Table 8). Wherein, when the dosage of the isooctanol is 1.5 percent, no obvious bubbles exist in the preparation process and the product, the dosage is less, the cost is low, and the method is the preferable scheme of the invention, therefore, the isooctanol 1.5 percent is taken as the defoaming agent for the next test.
Example 430% preparation method of mefenpyr-diethyl suspension seed coating agent
The 30% mefenpyr-diethyl suspension seed coating agent described in example 1 was prepared as follows:
sieving various solid components with a 320-mesh sieve, adding pyrazolate benazolin ester original drug, alkylphenol formaldehyde resin polyoxyethylene ether, NNO, polyoxyethylene polyoxypropylene ether block copolymer, magnesium aluminum silicate, xanthan gum, polyethylene glycol, urea, isooctanol, rose essence, isothiazolinone and deionized water into a sand mill in proportion, stirring at a high speed for pre-dispersion for 30min, adding zirconium beads (the medium coefficient is 1) as a sanding medium, sanding for 2.5h, controlling the sanding temperature below 45 ℃, and filtering to remove the sanding medium and impurities.
Effect verification quality detection of 230% mefenpyr-diethyl suspension seed coating agent
5 batches of samples were prepared according to the 30% mefenpyr-diethyl suspension seed coating formulation described in example 1.
The quality index of the 30% mefenpyr-diethyl suspension seed coating agent refers to NY 621-2002, and specifically comprises the following steps:
1. appearance: the suspension is a flowable uniform suspension, can be slightly precipitated or layered after being stored for a long time, but can be restored to the original state by being placed at room temperature by hand shaking and is free from caking;
2. the content of the effective components is more than or equal to the marked content;
3. pH value: 5.0 to 7.0;
4. the suspension rate is more than or equal to 90 percent;
5. the sieve analysis (passing a 44-micron test sieve) is more than or equal to 99 percent;
6. viscosity range (25 ℃): 100 to 600 mPas;
7. film forming property: qualified;
8. the coating uniformity is more than or equal to 90 percent;
9. the coating falling rate is less than or equal to 8 percent;
10. low-temperature stability: qualified;
11. heat storage stability: and (4) passing.
The content of effective components is determined by high performance liquid chromatography, Hypersil C18 chromatographic column, and injection volume is 5.0 μ L; the column temperature is 35 ℃; mobile phase: v (acetonitrile): v (water) ═ 25:75, flow rate 1.0 mL/min; filtering with filter membrane with pore diameter of 0.45 μm, and degassing in ultrasonic bath for 15 min; the detection wavelength is 273 nm; the retention time was about 7.24 min. The pH determination was carried out in accordance with GB/T1601-1993. The sieve analysis was performed according to GB/T16150-1995. The suspension, viscosity range, film-forming properties, coating uniformity, coating release rate, low temperature stability, and heat storage stability were determined according to NY 621-2002.
The quality detection results of the 30% mefenpyr-diethyl suspension seed coating agent show that all the quality detection results of 5 batches of samples are qualified, and the formula and the preparation method are feasible (table 9).
Table 930% mefenpyr-diethyl suspension seed coating agent quality detection result
Effect verification 330% determination of safety of mefenpyr-diethyl suspension seed coating agent to seeds
The dosage of the mefenpyr-diethyl is 47.1g/hm2I.e. with very good results, therefore, at 47.1g/hm2For normal dosage, the seeds are treated according to 1,2, 4, 6, 8 and 10 times of the normal dosage in the test respectively, so as to clarify the safety of the seeds. Diluting the prepared 30% mefenpyr-diethyl suspension seed coating agent in proportion according to the dosage of 47.1, 94.2, 188.4, 282.6, 376.8 and 471.0g/hm2Wheat seeds (variety: Jimai 22) were coated at a drug-to-seed ratio (seed coating agent liquid mass: seed mass) of 1:50, respectively, with clear water treatment as a control.
The influence of the 30% mefenpyr-diethyl suspension seed coating agent on the indoor germination potential and the indoor germination rate of the seeds is determined by an indoor test: arranging seeds on the wetted filter paper at equal intervals, culturing in a constant-temperature incubator at 20 ℃, observing the germination condition every day, supplementing water in time, counting and calculating the indoor germination vigor at the 4 th day, and measuring the indoor germination rate at the 12 th day. There were 4 replicates, 50 per replicate.
The influence of the 30% mefenpyr-diethyl suspension seed coating agent on the field germination rate of the seeds is determined through a field test: and (5) after land preparation in the field, manually ditching and sowing, respectively checking the number of seedlings 7d and 15d after sowing, and calculating the rate of emergence. There were 4 replicates of 200 per replicate.
Safety of table 1030% mefenpyr-diethyl suspension seed coating agent on wheat seeds
The result of the safety measurement of the 30% pyraclofen-ethyl suspension seed coating agent on seeds shows that the treatment with the normal dosage of 10 times has certain phytotoxicity on wheat, and the germination vigor and the germination rate of the wheat can be reduced; the normal dosage is 1-8 times, and the wheat is safe. The 30% mefenpyr-diethyl suspension seed coating prepared by the invention is safe for seeds (table 10).
Effect experiment 4 indoor bioassay example
The indoor bioassay example of the present invention was based on "indoor bioassay of pesticides test criteria herbicides part 4: activity determination test carried out by stem and leaf spray method (NY/T1155.4-2006), and the application effect of the 30% mefenpyr-diethyl suspension seed coating agent is determined through indoor bioassay. The test method is as follows:
2.5263g of 95% mesosulfuron technical material is accurately weighed and dissolved in 25mL of N, N-dimethylformamide to prepare 96g/L mesosulfuron mother liquor. 2.0942g of raw mefenpyr-diethyl with concentration of 95.5 percent is accurately weighed and dissolved in 25mL of acetone to prepare the mefenpyr-diethyl mother liquor with concentration of 80 g/L. During the test, a proper amount of mesosulfuron-methyl mother liquor and carfentrazone-ethyl mother liquor are respectively taken and diluted by a proper amount of 0.1% Tween 80 aqueous solution to prepare the spraying liquid medicine for the test.
The test targets of the pot experiment method are winter wheat (variety: Jimai 22), Jijijimai, wild oat and descurainia sophia. In a sunlight greenhouse, selecting plastic pots with diameter of 12cm and height of 11cm for seedling, and fixing seedlings before pesticide application, wherein each pot is reserved10 uniform plants. Spraying herbicide methyldisulfuron or mixture of methyldisulfuron and mefenpyr-diethyl at 2-3 leaf stage of wheat and weed to be tested, repeating the treatment for 4 times, wherein the liquid medicine amount is 450L/hm2. And (2) coating the seeds, namely diluting 30% of mefenpyr-diethyl suspended seed coating agent in proportion before sowing, coating the wheat seeds according to the medicine seed ratio (seed coating agent liquid medicine mass: seed mass) of 1:50, and then sowing. And 14d after the application, weighing the fresh weight of each pot of plants, and calculating the control effect of each treatment on weeds or the phytotoxicity rate E on wheat:
in the formula: e-controlling efficacy against weeds or phytotoxicity against wheat
T-fresh weight of the overground part of the wheat or the weed in the medicament treatment group;
c-the fresh weight of the overground part of the wheat or the weed in the blank control group.
The results of the bioassay are shown in Table 11. The results show that: the dosage of the mesosulfuron-methyl is 15.7g/hm2When the mefenpyr-diethyl is not used, the phytotoxicity rate to wheat is 27.84 percent, and the mefenpyr-diethyl is 47.1g/hm2After the seed treatment, the phytotoxicity rate to the wheat is-0.20 percent; the dosage of the mesosulfuron-methyl is 11.2g/hm2When the mefenpyr-diethyl is not used, the phytotoxicity rate to wheat is 19.35 percent, and the mefenpyr-diethyl is 47.1g/hm2After the seed treatment, the phytotoxicity rate to wheat is-0.15%, which shows that the mefenpyr-diethyl has the seed treatment activity under indoor conditions.
The dosage of the mesosulfuron-methyl is 15.7g/hm2After being coated by 30 percent of pyraclofen-ethyl suspension seed coating agent, the control effect on the wheat-burclover is 99.59 percent, the control effect on the descurainia sophia is 85.36 percent, the phytotoxicity rate on the wheat is-0.20 percent, and the control effect on the wild oat is 94.08 percent; the existing mixed spraying technology of pyraclofen-ethyl and mesosulfuron has the control effect on arthroncus of 90.48 percent, the control effect on descurainia sophia of 76.66 percent, the phytotoxicity rate on wheat of 6.81 percent and the control effect on wild oat of 93.15 percent. Shows that the 30 percent mefenpyr-diethyl suspension seed coating agent provided by the invention can be used for seed treatmentObviously improves the control effect of the mesosulfuron on the jiejie and the descurainia sophia, obviously reduces the phytotoxicity on wheat and has no influence on the control effect of wild oat.
In addition, when the mefenpyr-diethyl is not used, the control effect on the wheat-burclover is 98.05 percent, the control effect on the descurainia sophia is 85.43 percent, the phytotoxicity rate on the wheat is 27.84 percent, and the control effect on the wild oat is 92.92 percent, which indicates that the mesosulfuron-methyl must be used together with the mefenpyr-diethyl for ensuring the safety of crops, but the mixed spraying of the mefenpyr-diethyl and the mesosulfuron-methyl in the prior art can obviously reduce the control effect of the herbicide on weeds, and the pesticide effect of the herbicide is not influenced when the 30 percent mefenpyr-diethyl suspension seed coating agent provided by the invention is used for seed treatment.
The dosage of the mesosulfuron-methyl is 11.2g/hm2After being coated by 30% of pyraclofen-ethyl suspension seed coating agent, the control effect on the wheat-burclover is 95.07%, the control effect on the descurainia sophia is 85.39%, the phytotoxicity rate on the wheat is-0.15%, and the control effect on the wild oat is 83.25%; the existing mixed spraying technology of mefenpyr-diethyl and mesosulfuron has the control effect of 80.86 percent on Jiegeng wheat, 56.67 percent on descurainia sophia, 5.16 percent on the phytotoxicity rate of wheat and 81.74 percent on wild oat. The 30% pyracloquintocet-mefenpyr suspended seed coating agent provided by the invention is used for seed treatment, so that the control effect of mesosulfuron-methyl on the jiegeng wheat and the descurainia sophia can be obviously improved, the phytotoxicity on the wheat is obviously reduced, and the control effect on wild oat is not influenced. In addition, when the mefenpyr-diethyl is not used, the control effect on the wheat straw and stalk is 93.47%, the control effect on the descurainia sophia is 84.30%, the phytotoxicity rate on the wheat is 19.35%, and the control effect on the wild oat is 81.43%, which indicates that the mesosulfuron-methyl must be used together with the mefenpyr-diethyl for ensuring the safety of crops, but the mixed spraying of the mefenpyr-diethyl and the mesosulfuron-methyl in the prior art can obviously reduce the control effect of the herbicide on weeds, and the pesticide effect of the herbicide is not influenced when the 30% mefenpyr-diethyl suspension seed coating agent provided by the invention is used for seed treatment.
After the 30 percent pyracloquintocet-mefenpyr suspension seed coating agent provided by the invention is adopted for seed treatment, the mesosulfuron-methyl is sprayed, and the dosage is 11.2g/hm2The control effect of the paradise wheat is 95.07 percent, and the paradise wheat is broadcastThe control effect of the descurainia sophia is 85.39%; the dosage of the mesosulfuron-methyl in the prior art is 15.7g/hm2The control effect on the wheat-burclover is 90.48 percent, and the control effect on the descurainia sophia is 76.66 percent; the results show that the 30% mefenpyr-diethyl suspension seed coating agent provided by the invention is used for seed treatment and then is sprayed with mesosulfuron-methyl, so that the dosage of the herbicide can be obviously reduced, and the weed control effect of the herbicide is improved.
After the 30 percent pyracloquintocet-mefenpyr suspension seed coating agent provided by the invention is adopted for seed treatment, the mesosulfuron-methyl is sprayed, and the dosage is 15.7g/hm2The phytotoxicity rate to wheat is-0.20%; the dosage of the mesosulfuron-methyl in the prior art is 11.2g/hm2The damage rate to wheat is 5.16%; the result shows that the safety of the herbicide to crops can be obviously improved by using the 30 percent mefenpyr-diethyl suspension seed coating agent for seed treatment.
Table 1130% mefenpyr-diethyl suspension seed coating agent seed treatment effect on herbicide efficacy and phytotoxicity biological test results
Note: the treatment dosage of the mefenpyr-diethyl seed is 47.1g/hm2The seeding rate is 187.5kg/hm2The conversion is 25.12g/100kg of seeds, namely a g/hm2Amounting to (a/187.5X 100) g/100kg of seeds.
Effect verification 5 field efficacy test example
The field efficacy test embodiment of the invention is carried out according to the pesticide field efficacy test criterion (I) that the herbicide prevents and treats weeds in wheat crop fields (GB/T17980.41-2000), and the indoor bioassay test result is verified through field plot tests. The test method is as follows:
spraying the stems and leaves of weeds at the 2-3 leaf stage, wherein the liquid medicine amount is 450L/hm2Each treatment was repeated 4 times, and the cell area was 25m2Random block permutation. Investigation 30 days after drug administration, randomly sampling 4 samples at 1m per cell2Separately investigating the fresh weight of wheat and each weed, and calculating the control effect of each treatment on the weeds or the phytotoxicity rate E on the wheat:
in the formula: e-controlling efficacy against weeds or phytotoxicity against wheat
PT-fresh weight of wheat or weeds in the medicament treatment area;
CK-fresh weight of wheat or weed in blank control area.
The test was carried out in temple village of Handan city, Lianshan county, Lianzhou, Hebei province, with the targets of winter wheat (variety: Jimai 22), Jijimai, wild oat, Tanshao, etc., and the treatment method, the control effect of each treatment on weeds and the phytotoxicity rate on wheat are shown in Table 12.
The field efficacy test result shows that: the dosage of the mesosulfuron-methyl is 15.7g/hm2When the mefenpyr-diethyl is not used, the phytotoxicity rate to the wheat is 20.09 percent, and the mefenpyr-diethyl is 47.1g/hm2After the seed treatment, the phytotoxicity rate to the wheat is 0.88 percent; the dosage of the mesosulfuron-methyl is 11.2g/hm2When the mefenpyr-diethyl is not used, the phytotoxicity rate to wheat is 18.28 percent, and the mefenpyr-diethyl is 47.1g/hm2After the seed treatment, the phytotoxicity rate to wheat is 0.24%, which indicates that the mefenpyr-diethyl has the seed treatment activity under the field condition.
The dosage of the mesosulfuron-methyl is 15.7g/hm2After being coated by 30 percent of pyracloquintocet-mexyl suspension seed coating agent, the control effect on the wheat-burclover is 96.49 percent, the control effect on the descurainia sophia is 81.75 percent, the phytotoxicity rate on the wheat is 0.88 percent, and the control effect on the wild oat is 91.86 percent; the existing mixed spraying technology of mefenpyr-diethyl and mesosulfuron has the control effect of 87.55% on Arthron, 71.21% on descurainia sophia, 7.75% on wheat and 91.21% on wild oat. The 30% pyracloquintocet-mefenpyr suspended seed coating agent provided by the invention is used for seed treatment, so that the control effect of mesosulfuron-methyl on the jiegeng wheat and the descurainia sophia can be obviously improved, the phytotoxicity on the wheat is obviously reduced, and the control effect on wild oat is not influenced. In addition, when the mefenpyr-diethyl is not used, the control effect on the Jiegeng wheat is 96.62 percent, the control effect on the descurainia sophia is 79.99 percent, the phytotoxicity rate on the wheat is 20.09 percent, and the pesticide effect on the Yeyan is not only effective for the Jiegao wheat but also effective for the Jiegao wheatThe control effect of the wheat is 91.99%, which indicates that the mesosulfuron-methyl must be used together with the mefenpyr-diethyl for ensuring the safety of crops, but the mixed spraying of the mefenpyr-diethyl and the mesosulfuron-methyl in the prior art can obviously reduce the control effect of the herbicide on weeds, and the pesticide effect of the herbicide is not influenced when the 30% mefenpyr-diethyl suspension seed coating agent provided by the invention is adopted for seed treatment.
The dosage of the mesosulfuron-methyl is 11.2g/hm2After being coated by 30% of pyraclofen-ethyl suspension seed coating agent, the control effect on the wheat-burclover is 91.82%, the control effect on the descurainia sophia is 80.93%, the phytotoxicity rate on the wheat is 0.24%, and the control effect on the wild oat is 82.20%; the existing mixed spraying technology of pyraclofen-ethyl and mesosulfuron has the control effect on the festival wheat of 72.88 percent, the control effect on the descurainia sophia of 50.38 percent, the phytotoxicity rate on the wheat of 6.56 percent and the control effect on the wild oat of 80.38 percent. The 30% pyracloquintocet-mefenpyr suspended seed coating agent provided by the invention is used for seed treatment, so that the control effect of mesosulfuron-methyl on the jiegeng wheat and the descurainia sophia can be obviously improved, the phytotoxicity on the wheat is obviously reduced, and the control effect on wild oat is not influenced. In addition, when the mefenpyr-diethyl is not used, the control effect on the wheat straw and stalk is 91.75%, the control effect on the descurainia sophia is 79.26%, the phytotoxicity rate on the wheat is 18.28%, and the control effect on the wild oat is 81.26%, which indicates that the mesosulfuron-methyl must be used together with the mefenpyr-diethyl for ensuring the safety of crops, but the mixed spraying of the mefenpyr-diethyl and the mesosulfuron-methyl in the prior art can obviously reduce the control effect of the herbicide on weeds, and the pesticide effect of the herbicide is not influenced when the 30% mefenpyr-diethyl suspension seed coating agent provided by the invention is used for seed treatment.
After the 30 percent pyracloquintocet-mefenpyr suspension seed coating agent provided by the invention is adopted for seed treatment, the mesosulfuron-methyl is sprayed, and the dosage is 11.2g/hm2The control effect on the wheat festival is 91.82 percent, and the control effect on the descurainia sophia is 80.93 percent; the dosage of the mesosulfuron-methyl in the prior art is 15.7g/hm2The control effect on the wheat-burclover is 87.55 percent, and the control effect on the descurainia sophia is 71.21 percent; shows that the 30 percent pyracloquintocet-mefenpyr suspended seed coating agent provided by the invention is used for carrying out seed treatment and then spraying mesosulfuron-methyl, can obviously reduce the dosage of the herbicide and improve the effect of the herbicide on weedsPreventing and treating effect.
After the 30 percent pyracloquintocet-mefenpyr suspension seed coating agent provided by the invention is adopted for seed treatment, the mesosulfuron-methyl is sprayed, and the dosage is 15.7g/hm2The phytotoxicity rate to wheat is 0.88%; the dosage of the mesosulfuron-methyl in the prior art is 11.2g/hm2The damage rate to wheat is 6.56%; the result shows that the safety of the herbicide to crops can be obviously improved by using the 30 percent mefenpyr-diethyl suspension seed coating agent for seed treatment.
Table 1230% effect of mefenpyr-diethyl suspended seed coating seed treatment on herbicide efficacy and phytotoxicity field test results
Note: the treatment dosage of the mefenpyr-diethyl seed is 47.1g/hm2The seeding rate is 187.5kg/hm2The conversion is 25.12g/100kg of seeds, namely a g/hm2Amounting to (a/187.5X 100) g/100kg of seeds.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (18)
1. The mefenpyr-diethyl suspension seed coating agent is characterized by comprising the following components in parts by weight:
10-50 parts of mefenpyr-diethyl,
1-7 parts of a wetting agent,
1-7 parts of a dispersing agent,
0.1 to 3 parts of a thickening agent,
1-3 parts of a film-forming agent,
1-5 parts of an anti-freezing agent,
0.5 to 3 parts of a defoaming agent,
0.1 to 2 parts of a warning agent,
0.5 to 3 parts of a preservative,
the balance of deionized water;
the wetting agent is selected from one or more of alkylphenol formaldehyde resin polyoxyethylene ether, nonylphenol polyoxyethylene ether and castor oil polyoxyethylene ether;
the dispersing agent is selected from one or more of sodium lignosulfonate, NNO, polyoxyethylene polyoxypropylene ether block copolymer, alkylphenol polyoxyethylene phosphate and polyvinylpyrrolidone;
the thickening agent is selected from one or more of magnesium aluminum silicate, xanthan gum, sodium alginate and hydroxyethyl cellulose;
the film forming agent is selected from one or more of polyvinyl alcohol, polyethylene glycol and polyacrylamide;
the antifreezing agent is selected from one or more of ethylene glycol, glycerol and urea;
the defoaming agent is selected from one or more of isooctyl alcohol, isoamyl alcohol, stearic acid and lauric acid;
the warning agent is selected from one or more of acid scarlet, alkaline rose essence and Rudaming 2B;
the preservative is selected from one or more of formaldehyde, sodium salicylate, sodium benzoate, 1, 2-benzothiazolinone-3-one, 2-hydroxybiphenyl, sorbic acid, benzoic acid, benzaldehyde, p-hydroxybenzaldehyde, p-hydroxybenzyl ester and isothiazolinone.
2. The mefenpyr diethyl suspension seed coating agent of claim 1, which is characterized by comprising the following components by weight: 30% of mefenpyr-diethyl, 4% of wetting agent, 5% of dispersing agent, 1.1% of thickening agent, 2% of film forming agent, 2% of antifreezing agent, 1.5% of defoaming agent, 0.5% of warning agent, 1% of preservative and the balance of deionized water.
3. The mefenpyr diethyl suspension seed coating of claim 2, wherein the wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether;
the dispersant is NNO and/or polyoxyethylene polyoxypropylene ether block copolymer;
the thickening agent is magnesium aluminum silicate and/or xanthan gum;
the film forming agent is polyethylene glycol;
the antifreeze is urea;
the antifoaming agent is isooctanol;
the warning agent is alkaline rose essence;
the preservative is isothiazolinone.
4. Use of the mefenpyr-diethyl suspension seed coating agent as claimed in any one of claims 1 to 3 for controlling weeds in wheat fields.
5. The application according to claim 4, wherein the application is: and coating the wheat seeds by using the mefenpyr-diethyl suspension seed coating agent.
6. The use according to claim 4, wherein the weeds in wheat fields are grasses, broadleaf weeds, sedge weeds.
7. The use of claim 6, wherein the weeds in the wheat field are selected from one or more of jiejie, brome, aloesbill, alopecurus, beckia, beckmelon beck, beckmelon, club grass, lolium multiflorum, poison wheat, conyza sativa, aegilops tauschii, descurainia, shepherd's purse, male mallow, hordeum vulgare, chenopodium quinoa, calystegia chinensis, and sedge.
8. The use of claim 7, wherein the weeds in the wheat field are Arthrobacter and/or Aleurites sophia.
9. The use as claimed in claim 4, wherein the mefenpyr-diethyl suspension seed coating agent is used in an amount of 1-2000g of active ingredient per 100kg of seeds.
10. The use as claimed in claim 9, characterized in that the amount of active principle of the mefenpyr-diethyl suspension seed coating agent is 10-1000g per 100kg of seeds.
11. The use as claimed in claim 10, characterized in that the amount of active principle of the mefenpyr-diethyl suspension seed coating agent is 20-500g per 100kg of seeds.
12. The application as claimed in claim 4, wherein the amount of the mefenpyr-diethyl suspension seed coating agent is 1.875-3750g/hm2。
13. The use of claim 12, wherein the mefenpyr-diethyl suspension seed coating agent is used in an amount of 18.75-1875g/hm2。
14. The use as claimed in claim 13, wherein the mefenpyr-diethyl suspension seed coating agent is used in an amount of 37.5-937.5g/hm2。
15. The use as claimed in claim 4, wherein, in a specific application, the mefenpyr-diethyl suspension seed coating agent is used in combination with mesosulfuron-methyl: coating seeds with the mefenpyr-diethyl suspension seed coating agent, and spraying mesosulfuron-methyl.
16. The use as claimed in claim 15, wherein the mefenpyr-diethyl suspension seed coating agent is used in an amount of 1.875 to 3750g/hm2。
17. The use of claim 16, wherein the mefenpyr-diethyl suspension seed coating agent is used in an amount of 18.75-1875g/hm2。
18. Use according to claim 17The method is characterized in that the dosage of the mefenpyr-diethyl suspension seed coating agent is 37.5-937.5g/hm2(ii) a The dosage of the mesosulfuron-methyl is 8-20g/hm2It is preferable.
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