CN113170794B - tebuconazole-metalaxyl-M seed treatment suspending agent and preparation method and application thereof - Google Patents
tebuconazole-metalaxyl-M seed treatment suspending agent and preparation method and application thereof Download PDFInfo
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- CN113170794B CN113170794B CN202110469359.3A CN202110469359A CN113170794B CN 113170794 B CN113170794 B CN 113170794B CN 202110469359 A CN202110469359 A CN 202110469359A CN 113170794 B CN113170794 B CN 113170794B
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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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/46—N-acyl derivatives
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Abstract
The invention provides a tebuconazole-metalaxyl-M seed treatment suspending agent as well as a preparation method and application thereof, belonging to the technical field of pesticide bactericides, wherein the tebuconazole-M seed treatment suspending agent comprises the following components in parts by weight: 0.8-1.2 parts of metalaxyl-M, 1.8-2.2 parts of tebuconazole, 4-6 parts of tristyrylphenol polyoxyethylene ether, 0.8-1.2 parts of docusate sodium, 0.18-0.22 part of xanthan gum, 0.8-1.2 parts of magnesium aluminum silicate, 4-6 parts of propylene glycol, 4-6 parts of warning color BBC dye, 2.8-3.2 parts of acrylic emulsion, 0.18-0.22 part of organic silicon and 76-77 parts of water. The tebuconazole-metalaxyl-M seed treatment suspending agent provided by the invention has high safety and good stability.
Description
Technical Field
The invention belongs to the technical field of pesticide bactericides, and particularly relates to a tebuconazole-metalaxyl-M seed treatment suspending agent as well as a preparation method and application thereof.
Background
metalaxyl-M has molecular formula C15H20O4N; it was light brown, viscous, and clear liquid. Melting point: 38.7 ℃ (pure), vapor pressure: 3.3X 10-3Pa (25 ℃, pure product); metalaxyl-M is miscible with acetone, ethyl acetate, methanol, dichloromethane, toluene and n-octanol. metalaxyl-M has high-efficiency control effect on diseases of vegetables, fruit trees, tobaccos, oil plants, cottons, grains and other crops caused by peronospora parasitica, phytophthora parasitica and pythium bacteria.
Tebuconazole is an organic compound with the molecular formula C16H22ClN3O is a triazole bactericidal pesticide with high efficiency, broad spectrum and systemic property, has three functions of protection, treatment and eradication, and has wide bactericidal spectrum and long lasting period. Tebuconazole is capable of inhibiting the biosynthesis of fungal ergosterol.
At present, no tebuconazole-metalaxyl-M seed treatment suspending agent with high control effect and small dosage exists in the prior art.
Disclosure of Invention
In view of the above, the invention aims to provide a tebuconazole-metalaxyl-M seed treatment suspending agent which has high safety, good stability, good control effect on crops, small dosage, convenient application and reduced later application times, and a preparation method and application thereof.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a tebuconazole-metalaxyl-M seed treatment suspending agent which comprises the following components in parts by weight: 0.8-1.2 parts of metalaxyl-M, 1.8-2.2 parts of tebuconazole, 4-6 parts of tristyrylphenol polyoxyethylene ether, 0.8-1.2 parts of docusate sodium, 0.18-0.22 part of xanthan gum, 0.8-1.2 parts of magnesium aluminum silicate, 4-6 parts of propylene glycol, 4-6 parts of warning color BBC dye, 2.8-3.2 parts of acrylic emulsion, 0.18-0.22 part of organic silicon and 76-77 parts of water.
Preferably, the composition comprises the following components in parts by weight: 0.9-1.1 parts of metalaxyl-M, 1.9-2.1 parts of tebuconazole, 4.5-5.5 parts of tristyrylphenol polyoxyethylene ether, 0.9-1.1 parts of docusate sodium, 0.19-0.21 part of xanthan gum, 0.9-1.1 parts of magnesium aluminum silicate, 4.5-5.5 parts of propylene glycol, 4.5-5.5 parts of warning color BBC dye, 2.9-3.1 parts of acrylic emulsion, 0.19-0.21 part of organic silicon and 76.4-76.8 parts of water.
Preferably, the warning color BBC dye is C18H11N2O6SCICa。
Preferably, the pH value of the tebuconazole-metalaxyl-M seed treatment suspending agent is 5.0-8.0.
Preferably, the weight part of the xanthan gum is calculated as a pure product, the xanthan gum is used in the form of a xanthan gum swelling solution when in use, and the mass percentage of the xanthan gum in the xanthan gum swelling solution is 0.1-0.3%.
The invention provides a preparation method of tebuconazole-metalaxyl-M seed treatment suspending agent, which comprises the following steps:
1) premixing water, tristyrylphenol polyoxyethylene ether, docusate sodium, propylene glycol and organic silicon which are 60-70% of the total volume of the water to obtain premixed liquid;
2) mixing the premixed liquid, metalaxyl-M, tebuconazole, aluminum magnesium silicate and a warning color BBC dye, and shearing to obtain a shearing liquid;
3) sanding the shearing liquid to obtain sanding liquid;
4) and mixing and homogenizing the balance of water, the sanding liquid, the xanthan gum and the acrylic emulsion to obtain the seed treatment suspending agent.
Preferably, the sand mill in step 3) comprises: sequentially carrying out first sanding, second sanding and third sanding; the fineness of the first sand mill is 16.5-17.5 mu m; the fineness of the second sand mill is 6.5-7.5 mu m; the fineness of the third sand grinding is 3.3-3.7 mu m.
Preferably, the shearing time in the step 2) is 15-30 min.
Preferably, the homogenizing time in the step 4) is 30-50 min.
The invention also provides application of the tebuconazole-metalaxyl-M seed treatment suspending agent in seed coating.
The invention has the beneficial effects that: the tebuconazole-metalaxyl-M seed treatment suspending agent provided by the invention comprises metalaxyl-M, tebuconazole, tristyrylphenol polyoxyethylene ether, docusate sodium, xanthan gum, magnesium aluminum silicate, propylene glycol, warning color BBC dye, acrylic emulsion, organic silicon and water; the tebuconazole-metalaxyl-M seed treatment suspending agent provided by the invention is a red suspending liquid, and has no special pungent smell; wherein the mass fraction of the metalaxyl-M is 0.96 +/-0.14 percent, and the mass concentration is 10.0 +/-1.5 g/L; the mass fraction of the tebuconazole is 1.92 +/-0.28 percent, and the mass concentration is 20.0 +/-3.0 g/L. The tebuconazole-metalaxyl-M seed treatment suspending agent provided by the invention has the adhesion property of more than or equal to 90 percent, and the adhesion property of tebuconazole is more than or equal to 90 percent; the suspension rate of metalaxyl-M is more than or equal to 90 percent, and the suspension rate of tebuconazole is more than or equal to 90 percent; the low-temperature stability and the thermal stability are good, and the low-temperature stability is as follows: 0 ℃. + -. 1 ℃, good 7d, heat storage stability: 54 ℃ 2 ℃ C. +, 14d was good.
In the embodiment of the invention, the dosage (drug species ratio) of the 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent in the preparation is 1: 666. 1.5: 666. 2: 666. 2.5: 666 (namely 1 time dosage, 1.5 time dosage, 2 times dosage and 2.5 times dosage) has no obvious influence on the wheat emergence rate, the plant height, the plant morphology and the leaf color of the three varieties. The result shows that the 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent is safe to wheat emergence and seedling growth under the treatment dosage.
The toxicity test result of the suspending agent for treating tebuconazole-metalaxyl-M seeds in the embodiment of the invention is as follows: 1. acute oral toxicity of birds: LD50(7d)>500mg a.i./kg body weight, low toxicity; 2. acute toxicity of earthworm: LC (liquid Crystal)50(14d)>10mg a.i./kg dry soil, low toxicity.
In the embodiment of the invention, the 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent is acceptable to the risks of bird acute diseases, short-term diseases of birds, bees, silkworms, underground water, non-target arthropods and soil organisms.
Drawings
FIG. 1 is a structural formula of metalaxyl-M;
FIG. 2 is a structural formula of tebuconazole;
FIG. 3 is a schematic structural diagram of an adhesion detection device.
Detailed Description
The invention provides a tebuconazole-metalaxyl-M seed treatment suspending agent which comprises the following components in parts by weight: 0.8-1.2 parts of metalaxyl-M, 1.8-2.2 parts of tebuconazole, 4-6 parts of tristyrylphenol polyoxyethylene ether, 0.8-1.2 parts of docusate sodium, 0.18-0.22 part of xanthan gum, 0.8-1.2 parts of magnesium aluminum silicate, 4-6 parts of propylene glycol, 4-6 parts of warning color BBC dye, 2.8-3.2 parts of acrylic emulsion, 0.18-0.22 part of organic silicon and 76-77 parts of water.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 0.8-1.2 parts of metalaxyl-M as an effective component, preferably 0.9-1.1 parts, and more preferably 1 part; the CAS number of the metalaxyl-M is 70630-17-0, the chemical name is (N- (2, 6-xylyl) -N- (methoxyacetyl) -D-alanine methyl ester, and the chemical formula of the metalaxyl-M is C15H21NO4The relative molecular mass is 279.3, and the structural formula is shown in figure 1.
In the invention, the specific gravity of the metalaxyl-M is 1.125g/cm3(20 ℃, pure product); the pure metalaxyl-M is thermally decomposed at the temperature of about 270 ℃; melting point is-38.7 deg.C (pure product); vapor pressure of 3.3X 10-3Pa(25℃Pure product); the solubility of metalaxyl-M in water is 26g/l (25 ℃, pure product), and the solubility in an organic solvent is 59g/l (25 ℃, normal hexane); the metalaxyl-M is mutually soluble with acetone, ethyl acetate, methanol, dichloromethane, toluene and n-octanol. The metalaxyl-M of the invention is not hydrolyzed basically under acidic and neutral conditions; under alkaline conditions, DT50 was hydrolyzed to 116d (pH9.0, 25 ℃).
In the invention, the metalaxyl-M is used as a bactericide, and the mass percentage of the metalaxyl-M in the tebuconazole-metalaxyl-M seed treatment suspending agent is preferably 0.8-1.2%, more preferably 0.9-1.1%, and most preferably 1.0%, calculated on the pure product of the metalaxyl-M. In the invention, the metalaxyl-M can penetrate through seed coats, can be systemically transmitted to each part of plants along with the germination and growth of seeds, and can be used for treating the seeds to prevent and control various seed-borne and soil-borne diseases caused by low-grade fungi.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 1.8-2.2 parts of tebuconazole as an effective component, preferably 1.9-2.1 parts, and more preferably 2 parts. In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises tebuconazole as an active ingredient, wherein the CAS (CAS) accession number of the tebuconazole is 107534-96-3, the chemical name of the tebuconazole is (RS) -1-p-chlorophenyl-4, 4-dimethyl-3 (1H-1,2, 4-triazole-1-ylmethyl) pentanol, and the chemical formula of the suspending agent is C16H22ON3Cl, relative molecular mass 307.8, structural formula shown in figure 2. The tebuconazole is colorless crystal, has the melting point of 102.4 ℃, the vapor pressure of 1.3 mu Pa (20 ℃), the Kow ═ 5000, the solubility in water of 32mg/L (20 ℃, the pH ═ 7) and the solubility in dichloromethane>200g/L, 50-100 g/L of solubility in isopropanol and toluene and 50-100 g/L of solubility in normal hexane<0.1g/L (20 ℃), the tebuconazole of the invention is stable to disinfection in the absence of light.
In the invention, the tebuconazole is used as a bactericide, and the mass percentage of the tebuconazole in the tebuconazole-metalaxyl-M seed treatment suspending agent is preferably 1.8-2.2%, more preferably 1.9-2.1%, and most preferably 2.0% in terms of tebuconazole pure product. In the invention, the tebuconazole belongs to triazole agents, and the performance of the tebuconazole is very similar to that of triazolone; the tebuconazole has stronger systemic property and can kill germs attached to the surface layer of the seeds. Tebuconazole can effectively prevent the damage caused by septoria, erysiphe and puccinia by controlling the biosynthesis of ergosterol of pathogenic bacteria.
In the invention, the compounding of metalaxyl-M and tebuconazole can improve the bactericidal activity, and the two effective components can realize advantage complementation; the dosage is reduced, the dosage of the auxiliary agent is reduced, and the environment is protected. Within the dosage range of metalaxyl-M and tebuconazole defined in the invention, the synergistic effect is remarkable, for example, when the ratio of metalaxyl-M to tebuconazole is 1: 2, the co-toxicity coefficient is 151.57, and the synergy is 0.52 times.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 4-6 parts, preferably 5 parts, of tristyrylphenol polyoxyethylene ether, the tristyrylphenol polyoxyethylene ether is used as a dispersing agent, the source of the tristyrylphenol polyoxyethylene ether is not particularly limited, and the tristyrylphenol polyoxyethylene ether can be prepared from products sold in the field.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 0.8-1.2 parts of docusate sodium, preferably 0.9-1.1 parts, and more preferably 1 part; in the invention, the docusate sodium is used as a wetting agent, and the source of the docusate sodium is not particularly limited, and a product which is commercially available in the field can be adopted.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 0.18-0.22 part of xanthan gum, preferably 0.19-0.21 part of xanthan gum, and more preferably 0.2 part of xanthan gum. In the present invention, the xanthan gum is used in the form of a xanthan gum swelling solution when used, in parts by weight calculated as a pure product. In the invention, the mass percentage content of the xanthan gum swelling solution is preferably 1.5-2.5%, and more preferably 2%; in the invention, the xanthan gum swelling solution preferably further comprises a preservative, the preservative is preferably sodium benzoate, and the addition amount of the preservative is preferably 0.1%; the preparation method of the xanthan gum swelling solution is preferably as follows: mixing xanthan gum, preservative and water to prepare xanthan gum swelling solution with the mass percentage of the xanthan gum of 2%.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 0.8-1.2 parts of magnesium aluminum silicate, preferably 0.9-1.1 parts, and more preferably 1 part. In the invention, the magnesium aluminum silicate is used as a thickening agent, the source of the magnesium aluminum silicate is not particularly limited, and a product which is commercially available in the field can be adopted.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 4-6 parts of propylene glycol, more preferably 4.5-5.5 parts, and more preferably 5 parts; the propylene glycol is used as the antifreezing agent, the source of the propylene glycol is not particularly limited, and the propylene glycol can be obtained by adopting a product sold in the field.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 4-6 parts of warning color BBC dye, preferably 4.5-5.5 parts, and more preferably 5 parts; in the present invention, the warning color BBC dye is preferably C18H11N2O6SCICA. The source of the warning color BBC dye is not particularly limited in the invention, and the conventional commercial products in the field can be adopted.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 2.8-3.2 parts of acrylic emulsion, preferably 2.9-3.1 parts, and more preferably 3 parts; in the invention, the acrylic emulsion is used as a film forming agent, and in the invention, the solid content of the acrylic solution is preferably 49-51% (150 ℃,20 min). The source of the acrylic emulsion is not particularly limited in the present invention, and conventional commercial products in the art can be used.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 0.18-0.22 part of organic silicon, preferably 0.19-0.21 part of organic silicon, and more preferably 0.2 part of organic silicon. The organic silicon is used as the defoaming agent in the invention, the source of the organic silicon is not particularly limited in the invention, and the organic silicon defoaming agent which is conventional and commercially available in the field can be adopted.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent comprises 76-77 parts of water, preferably 76.4-76.8 parts, and more preferably 76.6 parts. The source and the type of the water are not particularly limited, and the water can be prepared by using water which is conventional in the field of pesticides.
In the specific implementation process of the invention, the composition of the tebuconazole-metalaxyl-M seed treatment suspending agent is shown in table 1.
The auxiliary materials of tristyrylphenol polyoxyethylene ether, docusate sodium, xanthan gum, magnesium aluminum silicate, propylene glycol, a warning color BBC dye, acrylic emulsion, organic silicon and water are adopted, and the working effect can ensure that the tebuconazole-metalaxyl-M seed treatment suspending agent has good stability, high suspension rate and adhesion rate of effective components, good coating performance and high safety.
The invention also provides a preparation method of the tebuconazole-metalaxyl-M seed treatment suspending agent, which comprises the following steps:
1) premixing water, tristyrylphenol polyoxyethylene ether, docusate sodium, propylene glycol and organic silicon which account for 60-70% of the total volume of the water to obtain premixed liquid;
2) mixing the premixed liquid, metalaxyl-M, tebuconazole, magnesium aluminum silicate and a warning color BBC dye, and shearing to obtain a shearing liquid;
3) sanding the shearing liquid to obtain sanding liquid;
4) and mixing and homogenizing the balance of water, the sanding liquid, the xanthan gum and the acrylic emulsion to obtain the seed treatment suspending agent.
In the invention, water, tristyrylphenol polyoxyethylene ether, docusate sodium, propylene glycol and organic silicon which are 60-70% of the total volume of the water are premixed to obtain a premixed solution. In the present invention, the premixing is performed by stirring, and the rotation speed and time of the stirring are not particularly limited, and the purpose of uniform mixing can be achieved. In the present invention, the premixing is preferably carried out in a stirred tank reactor.
After the premixed liquid is obtained, the premixed liquid, metalaxyl-M, tebuconazole, magnesium aluminum silicate and warning color dye are mixed and sheared to obtain shearing liquid. In the invention, the shearing time is preferably 15-30 min, and more preferably 20-25 min; the rotation speed of the shearing is preferably 1300-1500 rpm, and more preferably 1480 rpm. In the present invention, the shearing is preferably carried out in a high shear stirred tank, and the purpose of the shearing is to fully emulsify the materials.
After the shearing fluid is obtained, sanding is carried out on the shearing fluid to obtain the sanding fluid. In the present invention, the sanding preferably includes first sanding, second sanding, and third sanding performed in this order; the fineness of the first sand grinding material is preferably 16.5-17.5 micrometers, and more preferably 17 micrometers; the fineness of the second sanding is preferably 6.5-7.5 micrometers, and more preferably 7 micrometers; the fineness of the third sand is preferably 3.3-3.7 μm, and more preferably 3.5 μm. In the invention, the sanding is preferably carried out in a horizontal type sanding machine, and the sanding machine preferably operates under the conditions that the current is controlled to be 25A, the air pressure is 0.05Mpa and the discharging temperature is lower than 25 ℃ so as to prevent the situations of high temperature of the liquid medicine, unsmooth discharging and the like.
In the invention, the fineness of the material is preferably detected by a laser particle sizer.
In the practice of the invention, the sanding is preferably performed as follows: opening a primary sand mill for primary sand milling, adjusting the discharge speed of the liquid medicine to 500-600 kg/h, and detecting the fineness of the material after 2-4 min; after the liquid medicine volume in the one-level sand mill explosive tank reaches 70% -80%, the preferred 75% back that reaches, open the second grade sand mill and carry out the second sanding, after the second grade sanding is stable, open tertiary sand mill and carry out the third sanding. In the present invention, the stabilization is preferably determined by measuring the fineness of the material, which is considered to be stable if the fineness of the material is within a defined range and the fluctuation of the fineness of the material is within 5%. In the invention, the feeding and discharging speeds of the three-pass sanding are preferably adjusted, so that the discharging speed is kept consistent, and the sanding efficiency can be ensured. After the three-stage sanding is stable, the fineness of the three-stage sanded material is preferably checked once every 15min, so that the qualified fineness of the finally discharged material is ensured. In the invention, when the fineness of the discharged material meets the requirement, the material can be completely conveyed into the batching kettle.
After the sand grinding liquid is obtained, the balance of water, the sand grinding liquid, xanthan gum and acrylic emulsion are mixed and homogenized to obtain the seed treatment suspending agent. In the present invention, the "balance water" is used in two parts, one part is used for preparing xanthan gum swelling liquid, and the other part is used for washing the residual materials in the dosing tank and the sand mill. In the invention, the preservative sodium benzoate, the xanthan gum and water are preferably mixed to prepare the xanthan gum swelling solution with the mass percentage content of 1.5-2.5% of xanthan gum; after the xanthan gum swelling solution is prepared, the sand grinding solution, the xanthan gum swelling solution, the acrylic emulsion and the rest water are mixed. In the specific implementation process of the invention, the dosing tank and the sand mill are connected, and the residual materials in the dosing tank and the sand mill are preferably washed by the residual water in sequence and then mixed with the sanding liquid, the xanthan gum, the sodium benzoate and the acrylic emulsion. In the present invention, the homogenization is preferably carried out in a stirred tank reactor.
After the obtained seed treatment suspending agent is obtained, preferably detecting, and packaging after the detection is qualified; if the detection is not qualified, homogenizing is preferably carried out again until the detection is qualified, and then packaging is carried out.
In the present invention, the main equipment used in the preparation process of the tebuconazole-metalaxyl-M seed treatment suspending agent is described in Table 3.
The invention also provides application of the tebuconazole-metalaxyl-M seed treatment suspending agent in seed coating. The type of the seeds treated by the tebuconazole-metalaxyl-M seed treatment suspending agent is not particularly limited, and the seeds can be conventional seeds in the field; in the specific implementation process of the invention, wheat seeds are taken as an example. The method for coating the seeds is not limited in the present invention, and conventional seed dressing treatment in the field can be adopted.
In the invention, the tebuconazole-metalaxyl-M seed treatment suspending agent can inhibit loose smut of wheat when used for treating wheat seeds.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Tebuconazole: 97% tebuconazole original drug, low toxicity, PD20141503, provided by Dunhuang chemical Co., Ltd.
Content of tebuconazole: more than or equal to 97.0 percent, less than or equal to 0.5 percent of water and less than or equal to 0.5 percent of acetone insoluble substance.
metalaxyl-M: 92% metalaxyl-M technical material, low toxicity, PD20094902, provided by Zhejiang Hebei science and technology Limited.
Content of metalaxyl-M: more than or equal to 92.0 percent, less than or equal to 0.5 percent of water and less than or equal to 0.5 percent of acetone insoluble substance.
The composition of the product is shown in Table 1 (total amount is 100 kg).
TABLE 130 composition of tebuconazole/liter metalaxyl-M seed treatment suspension
| Name of ingredient | Content (%) | Has main effect in product |
| metalaxyl-M (folding hundred) | 1.0 | Active ingredient |
| Tebuconazole (book Bai) | 2.0 | Active ingredient |
| Tristyrylphenol polyoxyethylene ether | 5.0 | Dispersing agent |
| Sodium docusate | 1.0 | Wetting agent |
| Xanthan gum | 0.2 | Thickening agent |
| Magnesium aluminum silicate | 1.0 | Thickening agent |
| Propylene glycol | 5.0 | Antifreezing agent |
| BBC dye (C18H 11N)2O6SCICa) | 5.0 | Alert color |
| Acrylic emulsion | 3.0 | Film forming agent |
| Silicone | 0.2 | Defoaming agent |
| Water (W) | 76.6 | Dispersion medium |
The amounts and order of addition of the components are shown in Table 2.
TABLE 230 g/l Tebuconazole-metalaxyl-M seed treatment suspending agent raw material addition amount and sequence
The main equipment is shown in table 3.
Main equipment used for preparing tebuconazole-metalaxyl-M seed treatment suspending agent with the weight of 330 g/L
The method comprises the following operation steps:
the preparation method comprises the following steps:
before the materials enter the sand mill, a cold water circulating system is started at least one hour in advance, and the outlet water temperature is strictly controlled to be 10-14 ℃.
Adding a preservative sodium benzoate into xanthan gum to prepare xanthan gum swelling liquid with the mass percentage of 2 percent of xanthan gum, wherein the mass percentage of the sodium benzoate is 0.1 percent; and (5) standby.
Determining that the pre-added water amount of the material feeding pharmacy is 65.27% of the total volume of water and 50% of the total amount of materials; water was added to the high shear stirred tank and the remaining water was reserved to rinse the high shear stirred tank and sand mill.
The experimental steps are as follows:
1) adding tristyrylphenol polyoxyethylene ether, docusate sodium, propylene glycol and organic silicon, premixing to obtain a premixed solution, stirring uniformly, sequentially adding metalaxyl-M, tebuconazole, aluminum magnesium silicate and a warning color BBC dye, mixing, shearing for not less than 15min, fully dispersing and emulsifying, and then feeding into a sand mill.
2) The sand mill is controlled to operate under the conditions of current 25A, air pressure 0.05Mpa and discharging temperature lower than 25 ℃. Opening a first-level sand mill for sanding, wherein the discharging speed of the liquid medicine is 550 kg/h, extracting a sample after 3min, and detecting the fineness by using a laser particle analyzer, wherein the fineness is controlled to be 17 mu m by the first sanding. If more foams are generated in the liquid medicine in the medicine tank after discharging, a small amount of defoaming agent can be properly added for 1-3 kg.
And opening the secondary sand mill when the liquid medicine in the primary medicine tank reaches 75 percent, discharging the liquid medicine at a speed of 550 kg/h, and controlling the fineness to be 7 mu m.
And after the second-stage sand mill is stabilized, opening the third-stage sand mill, discharging the liquid medicine at 550 kg/h, and controlling the fineness to be 3.5 mu m.
After the three sanding operations are stable, the granularity of the three-stage sanding operation is checked once every 15min, the fineness reaches 3.5 mu m, and then the materials can be conveyed into the batching kettle completely.
After the sanding, add remaining water and wash remaining liquid medicine in high shear mixing tank and the sand mill in order to observe the clarity of discharge gate water yield and in order to ensure to wash totally, wash the water of liquid medicine and carry in the batching cauldron in the lump.
3) And finally, adding the 2% xanthan gum swelling solution and the acrylic acid emulsion which are prepared in advance into the material mixing kettle under stirring, and stirring for at least 30min to ensure full and uniform stirring.
And (5) sample sending detection, and packaging production is carried out after the detection meets the standard requirement. If the standard requirement is not met, the packaging production can not be carried out until the previous procedure is carried out and the standard requirement is met.
Identification test
Detecting the mass fractions of metalaxyl-M and tebuconazole by high performance liquid chromatography, wherein the relative difference between the retention time of a certain chromatographic peak in a sample solution and the retention time of chromatographic peaks of metalaxyl-M and tebuconazole in a standard sample solution is within 1.5%.
And (3) detecting physical and chemical properties:
TABLE 430 g/L Tebuconazole-metalaxyl-M seed treatment suspending agent physical and chemical property determination test results
Product quality standard
1. Composition and appearance: a red, flowable, homogeneous suspension is visually observed, which may precipitate or delaminate slightly on prolonged storage, but should recover to its original shape upon shaking by hand and should not cake.
2. Control item indicator
TABLE 530 grams/liter Tebuconazole-mefenoxam seed treatment suspending agent project index
The detection method corresponding to the control item index in table 5 is as follows:
determination of active ingredients
Determination of metalaxyl-M: after the sample is dissolved by the mobile phase, the high performance liquid chromatography separation and the measurement are carried out on the metalaxyl-M in the sample by using n-hexane + isopropanol 75+25(V/V) as the mobile phase and using a Chiralcel OJ-H chiral column and a variable wavelength ultraviolet detector, and the quantification is carried out by adopting an external standard method.
Determination of tebuconazole: after the sample was dissolved in methanol, acetonitrile + water (65 +35 (V/V)) was used as a mobile phase, and C was used18The high performance liquid chromatography separation and determination are carried out on the tebuconazole in the sample by a stainless steel column used as a filler and a variable wavelength ultraviolet detector, and the quantification is carried out by adopting an external standard method.
Determination of 2, 6-dimethylaniline: the sample was dissolved in acetone, and 2, 6-dimethylaniline was separated by gas chromatography using a capillary column packed with n-dodecane and a hydrogen flame ionization detector using DB-1701 as an internal standard, and quantified by the internal standard method. The minimum limit of quantification of 2, 6-dimethylaniline in the method is 0.0025 g/kg.
The mass fraction of the mefenoxam in the tebuconazole/liter and the mass fraction of the tebuconazole in the suspension for treating the mefenoxam seeds is determined to be (0.96 +/-0.14)%, and the mass fraction of the tebuconazole is determined to be (1.92 +/-0.28)% to be qualified.
Determination of the pH value
The pH value is qualified at 5.0-8.0 according to GB/T1601-1993.
Determination of the suspension Rate
The assay was performed according to "method 4.5" of GB/T14825-.
Pourability
According to GB/T31737-. In order to ensure that the product system is stable and has good fluidity, the pourability index is controlled to be less than or equal to 5 percent of residue after pouring and less than or equal to 0.5 percent of residue after washing.
Wet sieve test
According to the "wet sieving method" of GB/T16150-1995, the coating effect is poor if larger particles are present in the coating product. Because the local active ingredients are too much to cause phytotoxicity, the proportion of larger particles in the product is controlled through a wet sieve test. The content of the sieve passing the 75 mu m test is more than or equal to 98 percent, and the sieve is qualified.
Long-lasting foamability
According to GB/T28137-2011, in order to ensure that the product is uniformly sprayed in use and avoid the influence of excessive foam on the spraying quality, the content of effective components in the sprayed liquid medicine is not uniform, so that the pesticide application effect is influenced. The permanent foaming property is not more than 60 mL.
Adhesion Property
Adhesive device and reagent
Glass cylindrical guide groove: the length (410-470) mm, the inner diameter (80-85) mm, the lower end is hermetically connected with a glass funnel (the lower caliber is 15-30 mm, and the length is 15-30 mm).
An upper end glass funnel: the upper caliber (145-175) mm, the lower caliber (15-30) mm and the lower caliber length (15-30) mm.
The lower end is hermetically connected with a glass funnel: the height is 100mm, the inner diameter (80mm-85mm), the lower caliber (15-30) mm and the length of the lower caliber (15-30) mm.
Sliding cover door: is arranged at the bottom of the funnel
A support: ensure the guide groove to be in a vertical state
And (4) testing and screening: the mesh size is smaller than the tested seeds to prevent the tested seeds from passing through the test sieve.
A conical flask: 250mL
Acetonitrile, methanol, n-hexane, isopropanol: pure chromatography
metalaxyl-M standard sample: the known mass fraction is more than or equal to 98.0 percent;
tebuconazole standard sample: the known mass fraction is more than or equal to 98.0 percent;
the adhesive means is shown in fig. 3.
Adhesion test method
The coated seeds fall on the guide groove partition door through the upper end glass funnel, the partition door is opened, the seeds freely fall on the sieve at a fixed height, and the medicament powder falling off from the seeds is separated through the sieve. The above process was repeated 5 times, and the amount of the drug remaining on the seeds was measured and compared with the amount of the drug on the non-tested seeds to calculate the adherence of the drug.
The adhesion is more than or equal to 90 percent, which is qualified.
Adhesion test procedure
Weighing 50g (accurate to 1g) of seeds in a culture dish, sucking 1g of sample by using a syringe, injecting the sample into the culture dish, covering and turning for 5min, opening the cover, flatly spreading the coated seeds, and placing the coated seeds until the liquid medicine is dried for later use.
330g of the seeds treated by the method are stored for at least 24 hours under the environmental conditions of temperature (23 +/-5) DEG C and relative humidity of 40-60 percent.
3 portions of 20g samples are weighed from the prepared seed samples into 3 conical flasks, 100mL of methanol (75 mL +25mL of n-hexane + isopropanol) is added, and the mixture is ultrasonically shaken until the pigment on the surface of the seed is completely dissolved. Taking out, standing for 10min or centrifuging, transferring 50mL of clear liquid into a 100mL volumetric flask, diluting to scale with methanol (n-hexane + isopropanol 75+25), and measuring the mass of metalaxyl-M (tebuconazole) in three samples according to the adhesion method.
The remaining 270g of seeds were divided into 3 portions on average and tested as follows: the 90g sample was slowly poured into the glass cylindrical chute through the upper glass funnel, and when all the seeds reached the bottom of the chute, the door was opened to allow the seeds to fall freely onto the screen, and the door was closed. The experimental device does not need to be cleaned in the falling process of the seeds. The above process was repeated 4 times. A 20g sample was taken for testing of the seed drug dose. The guide channels, screens and apparatus were cleaned of residual powder before the next batch of sample experiments was run. The above experimental procedure was repeated for the remaining 2 samples. After the drop test, 20g samples of 3 samples were taken out into 3 erlenmeyer flasks, 100mL of methanol (n-hexane + isopropanol 75+25) was added, and the mixture was ultrasonically shaken until the pigment on the surface of the seeds was completely dissolved. Taking out, standing for 10min or centrifuging, transferring 50mL of clear liquid into a 100mL volumetric flask, diluting the clear liquid to a scale with methanol (n-hexane + isopropanol-75 +25), and measuring the mass of the metalaxyl-M (tebuconazole) in 3 samples according to the method.
Computing
The adhesion X3 of the sample was calculated according to equation (3):
X3＝m2÷m1×100％..(3)
in the formula:
x3-adhesion of sample, expressed as%;
m 2-number in grams (g) of the mean value of the masses of tebuconazole (metalaxyl-M) in 3 samples after being subjected to a drop test procedure;
m 1-number in grams (g) of the average value of the mass of tebuconazole (metalaxyl-M) in 3 samples not subjected to drop test procedures.
Stability at Low temperature
According to the GB/T19137-2003 low-temperature stability determination method for pesticides, the screening index is tested, and the test result meets the standard requirement and is qualified.
The seed coating product is basically produced in winter and used in spring festival in the market, and if the product is stored unstably under low temperature condition and is layered, the use of the product is directly influenced, so the index should be formulated. The low temperature storage stability test is performed at least once every three months.
Heat storage stability test
According to GB/T19136-2003. And (3) after the mixture is placed at the temperature of 54 +/-2 ℃ for 14d for hot storage, the mass fractions of the metalaxyl-M and the tebuconazole are not less than 95 percent of the average value measured before the hot storage, and the results of the pH value, the pourability, the suspension rate, the wet sieve test and the adhesiveness still meet the standard and are qualified.
The quality of the heat storage stability of the product directly reflects the rationality of the formula of the product and simulates the storage stability of the product within the shelf life, so that the index of the heat storage stability is formulated. The heat storage stability test is performed at least once every three months.
Signs, labels, packaging, storage and transportation, safety and warranty period
The product mark, label and package are in accordance with the relevant regulations of GB 3796-2006 and GB 20813-2006.
The inner package of the product adopts polyester bottles, the net content of each bottle is 500g, the outer package adopts five-layer film-coated corrugated paper boxes, and the net content of each box is 9 kg.
Product quality guarantee period: under the specified storage and transportation conditions, the product quality guarantee period is two years from the date of production.
Drug effect test of 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent
Test conditions
Test target
Wheat loose smut (Ustilago nuda (Jens.) Rosr.) was provided by Shenyang agriculture university plant pathology laboratory.
Instrument for measuring the position of a moving object
Microscope, electronic balance (induction 0.1mg), XZ-1600 biological incubator, beaker, pipette, counter, coverslip, etc.
Design of experiments
Preparation of test material
The wheat leaves infected with the pseudosmus graminis are cut off, the scab pseudosmus layer, namely the conidia, on the leaves is brushed into a beaker by a writing brush, and sterile water is added to prepare spore suspension with proper concentration for later use.
Medicament
95% tebuconazole technical product provided by rill chemical company; 92% metalaxyl-M technical product, available from Zhejiang Hebei science and technology Limited.
Test procedure
Spore suspension preparation
Resuspend spores to 1X 10 Per ml with sterile Water9spore-1X 101Spores were added and 0.5% glucose solution was added.
Pharmaceutical formulation
Dissolving tebuconazole and metalaxyl-M with acetone respectively to prepare high-concentration mother liquor, and mixing the mother liquor according to the ratio of 7: 2. 6: 3. 5: 4. 4: 5 and 3: 6, preparing a mixed solution of 5 groups of tebuconazole and metalaxyl-M. On the basis of the preliminary test, tebuconazole, metalaxyl-M mother liquor and the mixed liquor thereof are diluted into liquor with the mass concentration of 97.2, 32.4, 10.8, 3.6 and 1.2 mu g/L by using 0.1 percent by volume of Tween aqueous solution (see table 6).
Drug treatment
And (3) sequentially sucking 0.5mL of liquid medicine from low concentration to high concentration by using a pipette, respectively adding the liquid medicine into small test tubes, sucking 0.5mL of prepared spore suspension, and uniformly mixing the liquid medicine and the spore suspension in equal amount. The mixed solution is dripped onto a concave glass by a micro-sampler, and then the concave glass is placed into a culture dish with shallow water and is covered in a (20 soil 2) DEG C incubator for moisture preservation culture. Each treatment was repeated 4 times and blanked with a 0.1% aqueous tween solution without the agent.
Investigation
And (5) checking the germination condition of each treated spore 24h after treatment, namely when the germination rate of the blank control spore reaches over 90 percent. The spores were investigated 200 at random for 4 fields per treatment and the number of sprouts recorded. Germinating the spore with the length of the spore germ tube being larger than the short radius of the spore.
Data statistics and analysis
Calculation method
From the survey data, the relative inhibition of spore germination in percent (%) was calculated for each treatment. And (4) calculating according to the formulas (1) and (2), and reserving two digits after the decimal point in the calculation result.
R＝Ng÷Nt×100.....(1)
In the formula: r is the spore germination rate; ng is the spore germination number; nt is the total number of spores investigated.
Re＝RT÷R0×100........(2)
In the formula: re is the treatment correction spore germination rate; rTProcessing spore germination rate; r0Blank control spore germination rate.
Results of the experiment
TABLE 6 Combined virulence for inhibiting wheat loose smut conidiospore germination by tebuconazole and metalaxyl-M compounded
The tebuconazole and the metalaxyl-M have different chemical structures and different action modes, and the combination of the two medicaments is beneficial to overcoming or delaying the development of the drug resistance of the wheat loose smut and improving the control effect. Test results show that the inhibition activities of different proportions of tebuconazole and metalaxyl-M for the germination of wheat loose smut spores all show synergistic effects, wherein the ratio of tebuconazole to metalaxyl-M is 6: 3-4: 5 the ratio has the highest activity and the synergistic effect is obvious (Table 6). The optimal proportion recommended for controlling wheat loose smut by compounding tebuconazole and metalaxyl-M is 6: 3-4: 5.
toxicity test of 30g/l Tebuconazole-M metalaxyl-M seed treatment suspension in example 1
Entrusted Liaoning thousand one test and evaluation science and technology development Limited company to complete the toxicity test, the results are as follows:
1. acute oral toxicity test. Experimental animals: a rat; LD 50: 3690mg/kg, the toxicity grade is low.
2. Acute transdermal toxicity test. Experimental animals: a rat; LD50 female: >2000mg/kg, LD50 male: >2000 mg/kg; the toxicity grade is low toxicity.
3. Acute inhalation toxicity test. Application for exemption. The three items are combined, and the toxicity level is low.
4. Eye irritation test. Experimental animals: a rabbit; stimulus intensity: moderate irritation, recovery time 7 d.
5. Skin irritation test. Experimental animals: a rabbit; stimulus intensity: has no irritation.
6. Skin sensitization test. Experimental animals: guinea pigs; sensitization intensity: weak sensitizers.
7. And (5) a health risk assessment report of the drug administrator. Whether the health risk to the drug administrator is acceptable: it is acceptable.
Indoor safety determination experimental report of 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent
The purpose of the test is as follows: evaluation of safety of 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent to different varieties of wheat
Test targets: wheat (Triticum aestivum L.)
The test method comprises the following steps: seed coating method
The test basis is as follows: reference is made to the evaluation criteria of pesticide on crop safety (NY/T1965.3-2013)
The experiment was committed to the plant protection college of Shandong university of agriculture.
Results of the experiment
TABLE 7 test effect of seed coating treatment on wheat plant growth (variety: Tainong 18)
TABLE 8 test of the effect of seed coating treatment on wheat plant growth (variety: Jimai 22)
TABLE 9 test effect of seed coating treatment on wheat plant growth (variety: Linmai No. 4)
In tables 7 to 9, a represents the level of significance of the difference.
From the test results shown in tables 7-9, the dosage (drug species ratio) of the test drug 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent in the preparation is 1: 666. 1.5: 666. 2: 666. 2.5: 666 (namely 1 time dosage, 1.5 time dosage, 2 times dosage and 2.5 times dosage) has no obvious influence on the wheat emergence rate, the plant height, the plant morphology and the leaf color of the three varieties. The experimental agent is safe to wheat emergence and seedling growth under the treatment dosage.
Pesticide effect test of 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent for preventing and treating wheat loose smut in field plot
The research center of agricultural chemicals biology and research of Shenyang chemical research and development Limited company, the plant protection institute of northwest agriculture and forestry science and technology university, the plant protection research institute of Jiangsu province agricultural science institute and the plant protection research institute of Tianjin city are entrusted to carry out the operations respectively.
The drug delivery reagent is shown in table 10.
TABLE 10 dosing agent
The test method comprises the following steps: seed coating
The results of the experiment are shown in Table 11.
TABLE 11 field plot efficacy test results for wheat head smut control (Shenyang chemical research and development Co., Ltd. pesticide biological test center)
Note: the letters indicate differential significance, with lower case letters indicating a significance level of 0.05 and upper case letters indicating a significance level of 0.01.
The 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent has excellent control effect on wheat loose smut. The medicine seed ratio is 1: 666. 1: 1000. 1: 2000 treatment dosage, the control effect is better than that of the contrast medicament 350 g/L metalaxyl-M seed treatment emulsion in the drug seed ratio of 1: 2000 doses; the medicine seed ratio is 1: 666. 1: 1000 seed treatment doses are superior to the control medicament 60 g/L tebuconazole seed treatment suspending agent in the ratio of 1: 2500, the ratio of drug species is 1: 2000 treatment doses, equivalent to 60 g/l tebuconazole seed treatment suspension concentrate. The medicine seed ratio is 1: 666. 1: 1000. 1: 2000 treatment doses are different from each other in the control effect on the loose smut of wheat.
The suspension agent is used for treating and coating wheat seeds by using 30g/L tebuconazole-refined shell seeds to prevent and control wheat loose smut, and recommended dosage is as follows: the medicine seed ratio is 1: 666-1: 1000. in the test, the suspension concentrate for treating the tebuconazole-spermatozoa seed of 30g/L is observed in a ratio of 1: 666. 1: 1000. 1: under the dosage of 2000, the fertilizer has no adverse effect on wheat seed emergence and environmental organisms.
The results are shown in Table 12.
TABLE 12 field plot pesticide test results for wheat loose smut prevention and treatment (northwest university of agriculture and forestry, science and technology, plant protection academy)
The appropriate application period and dosage are as follows: before wheat seeding, wheat seeds are treated by adopting a seed coating method, and are immediately sown after air drying. The application amount of the effective components is 1.5 g/100 kg of seeds to 4.5 g/100 kg of seeds (the drug-seed ratio is 1: 2000-1: 666). The using method comprises the following steps: the seeds are treated by a method of coating the seeds before sowing. Safety: the test medicament is safe to the growth of wheat within the test dose range, and has no adverse effect.
TABLE 13 field plot pesticide effect test results for wheat head smut prevention and treatment (Jiangsu province plant protection institute of agricultural academy of sciences)
TABLE 14 field plot test results of wheat loose smut prevention and treatment (Tianjin plant protection institute)
TABLE 15 summary of the test results of the efficacy of the field plot against loose smut of wheat
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent has influence on environment
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent is a seed treatment agent, and tebuconazole raw drug and metalaxyl-M raw drug are both low-toxicity, and are used by a seed coating method according to the release and detail table required by pesticide preparation registration data in the pesticide registration data requirement 1. the environmental test in the chemical pesticide preparation data requirement needs to complete the following two tests: 1. acute oral toxicity test of birds, 2. acute toxicity test of earthworm.
The experiment is completed by Guizhou Jianande technology, Inc., and the specific results are as follows:
1. acute oral toxicity of birds: LD5o (7d) >500mg a.i./kg body weight, low toxicity;
2. acute toxicity of earthworm: LC3o (14d) >10mg a.i./kg dry soil, low toxicity.
Environmental risk assessment of 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent
The tebuconazole-metalaxyl-M seed treatment suspending agent with the concentration of 30g/L is used for carrying out risk assessment on birds, bees, silkworms, underground water, non-target arthropods and soil organisms.
The data source is as follows:
environmental toxicology test reports from Guizhou Jian German technology Limited; PPDB (pesticide attribute database), EU (european union committee pesticide database), EFSA (european food safety agency).
Evaluation basis:
section 3 of the pesticide registration environmental risk assessment guidelines: birds (race of birds);
section 4 of the pesticide registration environmental risk assessment guidelines: bees (bee);
section 5 of the pesticide registration environmental risk assessment guidelines: silkworm (Bombyx mori);
section 6 of the pesticide registration environmental risk assessment guidelines: groundwater "(groundwater);
section 7 of the pesticide registration environmental risk assessment guidelines: non-target arthropods ";
section 8 of the pesticide registration environmental risk assessment guidelines: soil organisms (Wt.%).
The evaluation used the China developed China-PEARL model, PECfill SFO _ China (xls) model.
Evaluation results and conclusions:
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent is used for preventing and treating wheat loose smut, and the application method is seed coating.
A water ecosystem: the wheat loose smut prevention and control agent belongs to a dry farmland bactericide, and does not contact an aquatic ecosystem in the using process, so that risk assessment on the aquatic ecosystem is not needed.
Birds: the 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent is acceptable for acute and short-term risks of birds, and the long-term risk is unacceptable.
Honeybee: the 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent has acceptable risk to bees.
Silkworm: the 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent does not cause contact with silkworms and does not cause risks to the silkworms.
Underground water: 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent is acceptable for the risk of underground water.
Non-target arthropods: the tebuconazole-metalaxyl-M seed treatment suspending agent with the concentration of 30g/L does not cause contact with non-target arthropods and does not cause risks to the non-target arthropods.
Soil biology: 30g/l tebuconazole-metalaxyl-M seed treatment suspending agent can accept the risk of soil organisms.
The 30g/L tebuconazole-metalaxyl-M seed treatment suspending agent can be accepted for the risks of bird acute diseases, bird short-term diseases, bees, silkworms, underground water, non-target arthropods and soil organisms. The long-term risk of the birds cannot be accepted, measures need to be taken in the pesticide application process to reduce the risk of the product to the birds, soil is covered in time after wheat fields are sowed, and the product is forbidden to be used in a bird protection area. And the product label is marked with that the product has higher risk to birds, soil is covered in time after wheat fields are sowed, and the birds protection area and the nearby areas are forbidden to use.
From the above examples, it is clear that the tebuconazole-metalaxyl-M seed treatment suspending agent provided by the invention has high safety and good stability.
Comparative example 1
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent
Product composition (500 g):
tebuconazole (purity 92%): 1.0 percent of the percentage content and 5.43g of the material dosage;
metalaxyl-M (purity 98%): 2.0 percent of the percentage content and 10.2g of the material dosage;
xanthan gum: the percentage content is 0.2 percent, and the material dosage is 1 g;
magnesium aluminum silicate: 1.0 percent of the percentage content and 5g of the material dosage;
propylene glycol: 5.0 percent of the percentage content and 25g of the material dosage;
BBC: 2.0 percent of the percentage content and 10g of the material dosage;
acrylic acid: 3.0 percent of the percentage content and 15g of the material dosage;
defoaming agent: the percentage content is 0.2 percent, and the material dosage is 1 g;
sk-92FS 1: 2.0 percent of the percentage content and 10g of the material dosage;
2.0 percent of Sk-551 and 10g of material consumption;
water: the balance to 100 percent and the material dosage is 407.37 g.
The preparation method refers to the preparation method of the conventional seed treatment suspending agent.
After the product is prepared, the phenomena of precipitation and creaming are avoided; the color of the coating is light; precipitation occurred after 14 days of hot storage.
Comparative example 2
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent
Product composition (500 g):
tebuconazole (purity 92%): 1.0 percent of the percentage content and 5.43g of the material dosage;
metalaxyl-M (purity 98%): 2.0 percent of the percentage content and 10.2g of the material dosage;
xanthan gum: the percentage content is 0.2 percent, and the material dosage is 1 g;
magnesium aluminum silicate: 1.0 percent of the percentage content and 5g of the material dosage;
propylene glycol: 5.0 percent of the percentage content and 25g of the material dosage;
BBC: 10.0 percent of the weight percentage and 50g of the material dosage;
acrylic acid: 3.0 percent of the percentage content and 15g of the material dosage;
defoaming agent: the percentage content is 0.2 percent, and the material dosage is 1 g;
sk-92FS 1: 5.0 percent of the percentage content and 25g of the material dosage;
2.0 percent of Sk-551 and 10g of material consumption;
water: the balance to 100 percent and the material dosage is 352.37 g.
The preparation method refers to the preparation method of the conventional seed treatment suspending agent.
After the preparation of the product is finished, no precipitate exists; the color of the coating is dark red; creaming appeared after 14 days of heat storage.
Comparative example 3
30g/L tebuconazole-metalaxyl-M seed treatment suspending agent
Product composition (500 g):
tebuconazole (purity 92%): 1.0 percent of the percentage content and 5.43g of the material dosage;
metalaxyl-M (purity 98%): 2.0 percent of the percentage content and 10.2g of the material dosage;
xanthan gum: the percentage content is 0.2 percent, and the material dosage is 1 g;
magnesium aluminum silicate: 1.0 percent of the percentage content and 5g of the material dosage;
propylene glycol: 5.0 percent of the percentage content and 25g of the material dosage;
BBC: 5.0 percent of the percentage content and 25g of the material dosage;
acrylic acid: 3.0 percent of the percentage content and 15g of the material dosage;
defoaming agent: the percentage content is 0.2 percent, and the material dosage is 1 g;
sk-92FS 1: 5.0 percent of the percentage content and 25g of the material dosage;
2.0 percent of Sk-551 and 10g of material consumption;
water: the balance to 100 percent and the material dosage is 377.37 g.
The preparation method refers to the preparation method of the conventional seed treatment suspending agent.
After the preparation of the product is finished, no precipitate exists; the coating has bright color; the product is stable after being stored for 14 days, and has no precipitation and creaming phenomenon.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The tebuconazole-metalaxyl-M seed treatment suspending agent is characterized by comprising the following components in parts by weight: 0.8-1.2 parts of metalaxyl-M, 1.8-2.2 parts of tebuconazole, 4-6 parts of tristyrylphenol polyoxyethylene ether, 0.8-1.2 parts of docusate sodium, 0.18-0.22 part of xanthan gum, 0.8-1.2 parts of magnesium aluminum silicate, 4-6 parts of propylene glycol, 4-6 parts of warning color BBC dye, 2.8-3.2 parts of acrylic emulsion, 0.18-0.22 part of organic silicon and 76-77 parts of water.
2. The tebuconazole-metalaxyl-M seed treatment suspending agent according to claim 1, which consists of the following components in parts by weight: 0.9-1.1 parts of metalaxyl-M, 1.9-2.1 parts of tebuconazole, 4.5-5.5 parts of tristyrylphenol polyoxyethylene ether, 0.9-1.1 parts of docusate sodium, 0.19-0.21 part of xanthan gum, 0.9-1.1 parts of magnesium aluminum silicate, 4.5-5.5 parts of propylene glycol, 4.5-5.5 parts of warning color BBC dye, 2.9-3.1 parts of acrylic emulsion, 0.19-0.21 part of organic silicon and 76.4-76.8 parts of water.
3. The tebuconazole-metalaxyl-M seed treatment suspension concentrate of claim 1, wherein the warning color BBC dye is C18H11N2O6SCICa。
4. The tebuconazole-metalaxyl-M seed treatment suspending agent according to claim 1, wherein the pH value of the tebuconazole-metalaxyl-M seed treatment suspending agent is 5.0-8.0.
5. tebuconazole-metalaxyl-M seed treatment suspension according to claim 1, characterized in that said xanthan gum is used in the form of a xanthan gum swelling solution when in use; the mass percentage of the xanthan gum in the xanthan gum swelling solution is 0.1-0.3%; the xanthan gum solution also comprises a preservative.
6. The method for preparing tebuconazole-metalaxyl-M seed treatment suspending agent according to any one of claims 1 to 5, comprising the following steps:
1) premixing water, tristyrylphenol polyoxyethylene ether, docusate sodium, propylene glycol and organic silicon which are 60-70% of the total volume of the water to obtain premixed liquid;
2) mixing and shearing the premixed liquid, metalaxyl-M, tebuconazole, aluminum magnesium silicate and a warning color BBC dye to obtain shearing liquid;
3) sanding the shearing liquid to obtain sanding liquid;
4) and mixing and homogenizing the balance of water, the sanding liquid, the xanthan gum and the acrylic emulsion to obtain the seed treatment suspending agent.
7. The method as claimed in claim 6, wherein the sand mill in step 3) comprises: sequentially carrying out first sanding, second sanding and third sanding; the fineness of the first sand mill is 16.5-17.5 mu m; the fineness of the second sand mill is 6.5-7.5 mu m; the fineness of the third sand grinding is 3.3-3.7 mu m.
8. The preparation method according to claim 6, wherein the shearing time in the step 2) is 15-30 min.
9. The method according to claim 6, wherein the time for homogenizing in step 4) is 30 to 50 min.
10. The tebuconazole-metalaxyl-M seed treatment suspending agent of any one of claims 1 to 5 and the tebuconazole-M seed treatment suspending agent prepared by the preparation method of any one of claims 6 to 9 are applied to seed coating.
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