CN113661989A - Trifloxystrobin and tebuconazole compounded nano bactericide and preparation method thereof - Google Patents
Trifloxystrobin and tebuconazole compounded nano bactericide and preparation method thereof Download PDFInfo
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- CN113661989A CN113661989A CN202111014620.7A CN202111014620A CN113661989A CN 113661989 A CN113661989 A CN 113661989A CN 202111014620 A CN202111014620 A CN 202111014620A CN 113661989 A CN113661989 A CN 113661989A
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- trifloxystrobin
- tebuconazole
- bactericide
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- compounded
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- 239000005857 Trifloxystrobin Substances 0.000 title claims abstract description 51
- 239000005839 Tebuconazole Substances 0.000 title claims abstract description 47
- ONCZDRURRATYFI-TVJDWZFNSA-N trifloxystrobin Chemical compound CO\N=C(\C(=O)OC)C1=CC=CC=C1CO\N=C(/C)C1=CC=CC(C(F)(F)F)=C1 ONCZDRURRATYFI-TVJDWZFNSA-N 0.000 title claims abstract description 47
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 45
- 239000003899 bactericide agent Substances 0.000 title claims abstract description 42
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 12
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000000080 wetting agent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 12
- 238000010008 shearing Methods 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- -1 trifloxystrobin tebuconazole compound Chemical class 0.000 claims description 6
- CDOUZKKFHVEKRI-UHFFFAOYSA-N 3-bromo-n-[(prop-2-enoylamino)methyl]propanamide Chemical group BrCCC(=O)NCNC(=O)C=C CDOUZKKFHVEKRI-UHFFFAOYSA-N 0.000 claims description 3
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 claims description 3
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- 239000000230 xanthan gum Substances 0.000 claims description 3
- 229940082509 xanthan gum Drugs 0.000 claims description 3
- 235000010493 xanthan gum Nutrition 0.000 claims description 3
- 229920000142 Sodium polycarboxylate Polymers 0.000 claims description 2
- 239000003082 abrasive agent Substances 0.000 claims description 2
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical group [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 230000000361 pesticidal effect Effects 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 10
- 201000010099 disease Diseases 0.000 description 8
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 239000004563 wettable powder Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 241000221785 Erysiphales Species 0.000 description 4
- 241000233679 Peronosporaceae Species 0.000 description 4
- 230000000857 drug effect Effects 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000000417 fungicide Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 241001474928 Ustilaginoidea virens Species 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000192542 Anabaena Species 0.000 description 1
- 241000235349 Ascomycota Species 0.000 description 1
- 241000221198 Basidiomycota Species 0.000 description 1
- 240000002791 Brassica napus Species 0.000 description 1
- 235000006008 Brassica napus var napus Nutrition 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- 241000233654 Oomycetes Species 0.000 description 1
- 241000736122 Parastagonospora nodorum Species 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 241000918585 Pythium aphanidermatum Species 0.000 description 1
- 241000221662 Sclerotinia Species 0.000 description 1
- 229930182692 Strobilurin Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940054066 benzamide antipsychotics Drugs 0.000 description 1
- 150000003936 benzamides Chemical class 0.000 description 1
- 150000001556 benzimidazoles Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002888 effect on disease Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 159000000000 sodium salts Chemical group 0.000 description 1
- 229940074404 sodium succinate Drugs 0.000 description 1
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- A01N37/50—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 the nitrogen atom being doubly bound to the carbon skeleton
-
- 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
-
- 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
Abstract
The invention discloses a trifloxystrobin and tebuconazole compounded nano bactericide and a preparation method thereof, wherein the preparation method of the bactericide comprises the following steps: s1, weighing 10-20% of trifloxystrobin, 10-40% of tebuconazole, 4-8% of emulsifying dispersant, 2-6% of dispersing wetting agent, 1-5% of viscosity reducer, 10-15% of synergist, 0.1-0.5% of binder, 1-3% of pH regulator, 0.1-2% of defoaming agent and the balance of water according to mass percentage; s2, mixing part of water with all the emulsifying dispersant, and then mixing with trifloxystrobin and tebuconazole to obtain a first solid-liquid mixture; s3, uniformly mixing the first solid-liquid mixture with the other raw materials except the synergist to obtain a second solid-liquid mixture; s4, grinding the second solid-liquid mixture to a particle size of less than or equal to 5 microns to obtain a coarse ground mixture; s5, grinding the coarse ground mixture to a particle size of less than or equal to 600nm to obtain a fine ground mixture; s6, adding a synergist into the finely ground mixture and uniformly mixing to obtain the trifloxystrobin and tebuconazole compounded nano bactericide. The trifloxystrobin and tebuconazole compounded nano bactericide disclosed by the invention has the advantages of good dispersibility, strong permeability, obvious pesticide effect and the like.
Description
Technical Field
The invention relates to the technical field related to crop fungicides, in particular to a trifloxystrobin and tebuconazole compounded nano fungicide and a preparation method thereof.
Background
The trifloxystrobin is a novel fluorine-containing bactericide developed by taking natural product Strobilurins as a bactericide lead compound. The trifloxystrobin has the characteristics of high efficiency, broad spectrum, protection, treatment, eradication, permeation, systemic activity, rain wash resistance, long duration and the like, is effective on strains which generate resistance to 1, 4-demethylase inhibitors, benzamides, dicarboxamides and benzimidazoles, and has no cross resistance with the existing bactericides. Has good activity on almost all fungal diseases (ascomycetes, basidiomycetes, oomycetes and fungi imperfecti) such as powdery mildew, rust disease, septoria nodorum, net blotch, downy mildew, rice blast and the like. Besides the special effect on powdery mildew and leaf spot, the bactericidal composition has good activity on rust disease, downy mildew, damping off, apple anabaena and sclerotinia rot of colza. Is safe to crops, and is safe to the environment because the fertilizer can be quickly degraded in soil and water. Therefore, the trifloxystrobin has very wide application prospect.
At present, one of the common utilization modes of trifloxystrobin is to compound trifloxystrobin with tebuconazole to prepare a compound bactericide. The trifloxystrobin and tebuconazole compound bactericide has excellent bactericidal effect, long duration and wide bactericidal range, and is an excellent product aiming at diseases such as powdery mildew, rust disease, anthracnose, leaf spot, downy mildew, gummy stem blight, gibberellic disease, rice blast and the like in the market at present. However, the dosage forms of the existing trifloxystrobin and tebuconazole compound bactericide are mainly low-content wettable powder and spraying solid granules.
The wettable powder is prepared by crushing materials at normal temperature by a common crusher, the fineness of the wettable powder basically passes through a 45-micron wet sieve, the particle spectrum is wide, and the wettable powder has large dust during processing and is very easy to cause the problem of cross contamination of products; in addition, the wettable powder has a relatively low suspension rate index due to a relatively large particle size, and the pesticide damage is easily caused by the excessively large particle size; meanwhile, the melting points of the trifloxystrobin and the tebuconazole are both lower, the dispersion capacity and the drug effect are reduced due to material melting caused by poor temperature control in the production process, the materials are agglomerated after being placed for a period of time and cannot be dispersed, and the using effect is greatly reduced.
The preparation method of the spray solid granules is a spray granulation method, the granules produced by the granulation method are finer, the suspension rate is higher, but the production energy consumption is high, the cost of the used auxiliary agent is high during production, and the drug effect durability is also very short; also, as mentioned above, the melting points of trifloxystrobin and tebuconazole are relatively low, while the drying temperature of spray granulation is high, the drying temperature is difficult to control, and it is usually required to be above 110 ℃ to obtain a dried product, which causes the same problems as wettable powder: the dispersion ability is poor, the agglomeration is easy, the drug effect is poor, the drug effect durability of the product is poor due to fine and uneven particles, the dilution times are required to be reduced or the use times are required to be increased during application, and the use cost is increased.
Disclosure of Invention
Therefore, the invention provides the trifloxystrobin and tebuconazole compounded nano bactericide and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
in a first aspect, the embodiment of the invention provides a trifloxystrobin tebuconazole compound nano bactericide which is prepared from the following components in percentage by mass:
10-20% of trifloxystrobin, 10-40% of tebuconazole, 4-8% of emulsifying dispersant, 2-6% of dispersing wetting agent, 1-5% of viscosity reducer, 10-15% of synergist, 0.1-0.5% of binder, 1-3% of pH regulator, 0.1-2% of defoaming agent and the balance of water.
Preferably, the emulsifying dispersant is polyoxyethylene polyoxypropylene ether.
Preferably, the dispersing wetting agent is sodium sulfosuccinate.
Preferably, the viscosity reducing agent is a sodium salt of a polycarboxylic acid.
Preferably, the synergist is dioctyl sodium sulfosuccinate.
Preferably, the binder is xanthan gum.
Preferably, the pH adjusting agent is citric acid
Preferably, the anti-foaming agent is silicone.
In a second aspect, an embodiment of the present invention provides a preparation method of the above fungicide, including the following steps:
s1, weighing the following raw materials in percentage by mass:
10-20% of trifloxystrobin, 10-40% of tebuconazole, 4-8% of emulsifying dispersant, 2-6% of dispersing wetting agent, 1-5% of viscosity reducer, 10-15% of synergist, 0.1-0.5% of binder, 1-3% of pH regulator, 0.1-2% of defoaming agent and the balance of water;
s2, mixing part of water with all the emulsifying dispersant according to the mass ratio of 38: 8, mixing the mixture with trifloxystrobin and tebuconazole to obtain a first solid-liquid mixture;
s3, circularly shearing and mixing the first mixture, a dispersing wetting agent, a viscosity reducer, a binder, a pH regulator, a defoaming agent and the rest water at the temperature of 30 ℃ at the rotating speed of 2800r/min for 15min to obtain a second solid-liquid mixture;
s4, grinding the second solid-liquid mixture to a particle size of less than or equal to 5 microns to obtain a coarse ground mixture;
s5, grinding the coarse ground mixture at 25 ℃ until the grain diameter is less than or equal to 600nm to obtain a fine ground mixture;
s6, adding a synergist into the finely ground mixture, and circularly shearing and mixing for 3min at the rotating speed of 2400r/min to obtain the trifloxystrobin and tebuconazole compounded nano bactericide.
Preferably, the abrasives used in grinding in S4 and S5 are 95 zirconium beads, wherein the particle size of the 95 zirconium beads used in S4 is 0.8-1.0mm, and the particle size of the 95 zirconium beads used in S5 is 0.3-0.4 mm.
Compared with the prior art, the embodiment of the invention at least has the following beneficial effects:
(1) according to the trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment of the invention, a first shearing and mixing process can break large particles into small particles, so that the particle size of the material is effectively reduced, the emulsification dispersant is more sufficiently and uniformly adsorbed with trifloxystrobin and tebuconazole, and the dispersibility, uniformity, suspension rate and stability of the emulsification dispersant can be improved; the second shearing and mixing process has the mixing function to improve the uniformity of the bactericide, and can further refine the granularity to prepare for grinding; the grain diameter of the bactericide reaches the nanometer level through coarse grinding and fine grinding, so that agglomeration of bactericide particles is effectively avoided, the bactericide is not easy to layer even if stored for a long time, long-time transportation is very convenient, meanwhile, the permeability and wettability of the bactericide are improved, the pesticide effect is obviously improved, and the improvement effect on the comprehensive performance of the bactericide is obvious; and no dust exists during production and processing, and the safety to the environment and the human body can be effectively ensured.
(2) The trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment of the invention is a suspending agent in dosage form, is environment-friendly, does not use an organic solvent in the formula, and has high use safety and small environmental pollution.
(3) The trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment of the invention has the preparation temperature below 30 ℃ all the time, and effectively prevents bactericide agglomeration, dispersion reduction, pesticide effect weakness and the like caused by high-temperature melting of trifloxystrobin and tebuconazole.
(4) The trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment of the invention has the advantages that the yield, the product quality and the quality uniformity of the bactericide are greatly improved through specific grinding time, grinding temperature and zirconium bead particle size.
(5) The trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment of the invention has obvious control effects on diseases such as powdery mildew, rust disease, anthracnose, leaf spot, downy mildew, gummy stem blight, gibberellic disease, rice blast and the like.
Detailed description of the invention
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In the description of the present invention, "a plurality" means two or more unless otherwise specified. The terms first, second and the like in the description and in the claims, are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order.
Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements specifically listed, but may include other steps or elements not expressly listed that are inherent to such process, method, article, or apparatus or that are added to such process, method, article, or apparatus based on the optimization concepts of the present invention.
The details of examples 1 to 3 are shown in tables 1 and 2.
TABLE 1-proportions by mass of the components of examples 1 to 3
The preparation of example 1 is as follows:
s1, weighing the following raw materials in percentage by mass:
12% of trifloxystrobin, 24% of tebuconazole, 5% of emulsifying dispersant polyoxyethylene polyoxypropylene ether, 3% of dispersing wetting agent sodium succinate, 2% of viscosity-reducing agent sodium polycarboxylate, 15% of synergist dioctyl sodium sulfosuccinate, 0.25% of binder xanthan gum, 1.5% of pH regulator citric acid, 0.55% of defoaming agent organosilicon and 36.7% of water;
s2, mixing part of water with all the emulsifying dispersant according to the mass ratio of 36.7: 5, mixing the mixture with trifloxystrobin and tebuconazole to obtain a first solid-liquid mixture;
s3, carrying out high-speed dead-corner-free circular shearing and mixing on the first solid-liquid mixture, a dispersing wetting agent, a viscosity reducer, a binder, a pH regulator, a defoaming agent and the rest water for 15min under the conditions that the temperature is reduced by using jacket circular chilled water to ensure that the mixing temperature is constant at 30 ℃ and the rotating speed of a dead-corner-free high-speed shearing machine is 2800r/min to obtain a second solid-liquid mixture;
s4, grinding the second solid-liquid mixture to a particle size of below 5 mu m by taking 95 zirconium beads with the particle size of 0.8-1.0mm as grinding materials to obtain a coarse grinding mixture;
s5, taking 95 zirconium beads with the particle size of 0.3-0.4mm as an abrasive, cooling by using jacket circulating chilled water to enable the grinding temperature to be below 25 ℃, and grinding the coarse ground mixture to the average particle size within 600nm to obtain a fine ground mixture;
s6, adding a synergist into the finely ground mixture, and circularly shearing the finely ground mixture at a high speed without dead angles for 3min by using a high-speed dead angle-free shearing machine at a rotating speed of 2400r/min to obtain the trifloxystrobin tebuconazole compounded nano bactericide.
Examples 2-3 were prepared in the same manner as in example 1.
Next, performance tests were performed on the above examples 1 to 3 to illustrate the advantageous effects of the present invention.
Test 1
The performance parameters of the trifloxystrobin tebuconazole compound nano bactericide provided by the embodiments 1-3 of the invention are measured. The measurement results are shown in table 2 below.
TABLE 2-examples 1 to 3 Performance parameters
| Test item and superior standard | Example 1 | Example 2 | Example 3 |
| Trifloxystrobin mass fraction% | 12.04 | 10.01 | 15.04 |
| The mass fraction of tebuconazole% | 24.03 | 30.02 | 25.04 |
| PH range (6-9) | 6.8 | 6.4 | 6.5 |
| Trifloxystrobin suspension percentage% (≧ 75) | 100 | 99.7 | 99.2 |
| Tebuconazole suspension percent (more than or equal to 75) | 100 | 100 | 100 |
| Particle size (nm) D50 | 470 | 560 | 540 |
| The residue after pouring is less than or equal to 5 percent | 1.2 | 3.4 | 4.6 |
| The residue after washing is less than or equal to 0.5 percent | 0.07 | 0.22 | 0.25 |
| Lasting foam (after 1 min) is less than or equal to 60ml | 12 | 8 | 15 |
| Wet sieve test (passing 75 μm test sieve)% | 100 | 100 | 100 |
| Stability at Low temperature | Qualified | Qualified | Qualified |
| Heat storage stability (54 ℃ +/-2 ℃) for 14 days | Qualified | Qualified | Qualified |
Test 2
The trifloxystrobin and tebuconazole compounded nano bactericide provided by the embodiment 1 of the invention is selected to test the prevention and treatment effect on the false smut of rice, and the test is divided into 1-5 treatment groups, wherein the treatment groups 1-3 are experimental groups, and the treatment groups 4-5 are control groups; details of each treatment group are shown in table 3.
The first pesticide application is carried out at the last stage of rice booting, and the second pesticide application is carried out at the full heading stage of rice; the control of groups 1-5 was statistically treated 10 days after the second application, and the results are shown in Table 4.
TABLE 3 details of treatment groups 1-5
TABLE 4-treatment groups 1-5 control
| Process group numbering | Disease index of pre-drug crops | Average control effect% (repeat average) |
| 1 | 0.95 | 82.48％ |
| 2 | 0.8 | 85.66％ |
| 3 | 0.71 | 88.78％ |
| 4 | 0.80 | 79.21％ |
| 5 | 0.83 | 76.20％ |
The results show that the comprehensive performance of the trifloxystrobin tebuconazole compound nano bactericide provided by the embodiments 1-3 of the invention is obviously superior to that of a control group, and tests show that the embodiments 1-3 have very good prevention and treatment effects on false smut of rice, are safe to rice and have no obvious adverse effect on other non-target organisms in the field.
All the technical features of the above embodiments can be combined arbitrarily, and for simplicity of description, all possible combinations of the technical features of the above embodiments are not described; these examples, which are not explicitly described, should be considered to be within the scope of the present description.
The present invention has been described in considerable detail by the general description and the specific examples given above. It should be noted that it is obvious that several variations and modifications can be made to these specific embodiments without departing from the inventive concept, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The trifloxystrobin and tebuconazole compounded nano bactericide is characterized by being prepared from the following components in percentage by mass:
10-20% of trifloxystrobin, 10-40% of tebuconazole, 4-8% of emulsifying dispersant, 2-6% of dispersing wetting agent, 1-5% of viscosity reducer, 10-15% of synergist, 0.1-0.5% of binder, 1-3% of pH regulator, 0.1-2% of defoaming agent and the balance of water.
2. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the emulsifying dispersant is polyoxyethylene polyoxypropylene ether.
3. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the dispersing and wetting agent is sodium sulfosuccinate.
4. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the viscosity reducer is a sodium polycarboxylate.
5. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the synergist is dioctyl sodium sulfosuccinate.
6. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the binder is xanthan gum.
7. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the pH regulator is citric acid.
8. The trifloxystrobin and tebuconazole compounded nano bactericide as claimed in claim 1, wherein the defoaming agent is organic silicon.
9. The preparation method of the trifloxystrobin and tebuconazole compounded nano bactericide of claim 1 is characterized by comprising the following steps of:
s1, weighing the following raw materials in percentage by mass:
10-20% of trifloxystrobin, 10-40% of tebuconazole, 4-8% of emulsifying dispersant, 2-6% of dispersing wetting agent, 1-5% of viscosity reducer, 10-15% of synergist, 0.1-0.5% of binder, 1-3% of pH regulator, 0.1-2% of defoaming agent and the balance of water;
s2, mixing part of the water weighed in the S1 and all the emulsifying dispersant according to the mass ratio of 38: 8, mixing the mixture with the trifloxystrobin and the tebuconazole to obtain a first solid-liquid mixture;
s3, circularly shearing and mixing the first solid-liquid mixture, the dispersing and wetting agent, the viscosity reducer, the binder, the pH regulator, the defoaming agent and the rest of water at the temperature of 30 ℃ at the rotating speed of 2800r/min for 15min to obtain a second solid-liquid mixture;
s4, grinding the second solid-liquid mixture to a particle size of less than or equal to 5 microns to obtain a coarse ground mixture;
s5, grinding the coarse ground mixture at 25 ℃ until the particle size is less than or equal to 600nm to obtain a fine ground mixture;
s6, adding the synergist into the finely ground mixture, and circularly shearing and mixing for 3min at the rotating speed of 2400r/min to obtain the trifloxystrobin tebuconazole compound nano bactericide.
10. The method according to claim 9, wherein the abrasives used in the grinding in S4 and S5 are 95 zirconium beads, wherein the 95 zirconium beads used in S4 have a particle size of 0.8 to 1.0mm, and the 95 zirconium beads used in S5 have a particle size of 0.3 to 0.4 mm.
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