CN114342927A - Preparation method and application of chlorothalonil nano pesticide preparation - Google Patents
Preparation method and application of chlorothalonil nano pesticide preparation Download PDFInfo
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- CRQQGFGUEAVUIL-UHFFFAOYSA-N chlorothalonil Chemical compound ClC1=C(Cl)C(C#N)=C(Cl)C(C#N)=C1Cl CRQQGFGUEAVUIL-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000005747 Chlorothalonil Substances 0.000 title claims abstract description 80
- 239000000575 pesticide Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 124
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000006185 dispersion Substances 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 19
- 239000002562 thickening agent Substances 0.000 claims abstract description 19
- 239000000080 wetting agent Substances 0.000 claims abstract description 19
- 229920001690 polydopamine Polymers 0.000 claims abstract description 14
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000004480 active ingredient Substances 0.000 claims abstract description 8
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 49
- 239000007788 liquid Substances 0.000 claims description 41
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 21
- 239000012528 membrane Substances 0.000 claims description 20
- 239000003090 pesticide formulation Substances 0.000 claims description 20
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 18
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 18
- 239000007983 Tris buffer Substances 0.000 claims description 18
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 18
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 235000007466 Corylus avellana Nutrition 0.000 claims description 16
- 241000221785 Erysiphales Species 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 229920001285 xanthan gum Polymers 0.000 claims description 13
- 239000000230 xanthan gum Substances 0.000 claims description 13
- 229940082509 xanthan gum Drugs 0.000 claims description 13
- 235000010493 xanthan gum Nutrition 0.000 claims description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 229920002472 Starch Polymers 0.000 claims description 12
- 239000008107 starch Substances 0.000 claims description 12
- 235000019698 starch Nutrition 0.000 claims description 12
- 241000723382 Corylus Species 0.000 claims description 11
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- -1 alkyl naphthalene sulfonate formaldehyde Chemical compound 0.000 claims description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000005995 Aluminium silicate Substances 0.000 claims description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims description 8
- 229920001400 block copolymer Polymers 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 7
- 230000002528 anti-freeze Effects 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229920005646 polycarboxylate Polymers 0.000 claims description 6
- 239000002671 adjuvant Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 229920002261 Corn starch Polymers 0.000 claims description 4
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 4
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000440 bentonite Substances 0.000 claims description 4
- 229910000278 bentonite Inorganic materials 0.000 claims description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 4
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000008120 corn starch Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 229920013747 hydroxypolyethylene Polymers 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 229940074404 sodium succinate Drugs 0.000 claims description 3
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 13
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000013268 sustained release Methods 0.000 abstract description 3
- 239000012730 sustained-release form Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000013459 approach Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 34
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 17
- 238000011068 loading method Methods 0.000 description 14
- 238000001514 detection method Methods 0.000 description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 230000003902 lesion Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 8
- 201000010099 disease Diseases 0.000 description 8
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 8
- 230000001804 emulsifying effect Effects 0.000 description 8
- 235000001543 Corylus americana Nutrition 0.000 description 7
- 230000010355 oscillation Effects 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 240000007582 Corylus avellana Species 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 241000607479 Yersinia pestis Species 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000002538 fungal effect Effects 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 230000002459 sustained effect Effects 0.000 description 2
- OWEFQTXQEHYDEJ-UHFFFAOYSA-N 2,3-dihydroxypropanal diphosphono hydrogen phosphate Chemical compound OCC(O)C=O.OP(O)(=O)OP(O)(=O)OP(O)(O)=O OWEFQTXQEHYDEJ-UHFFFAOYSA-N 0.000 description 1
- 241000688227 Curculio nucum Species 0.000 description 1
- 101710088194 Dehydrogenase Proteins 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007798 antifreeze agent Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 229920006391 phthalonitrile polymer Polymers 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
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- 108090000623 proteins and genes Proteins 0.000 description 1
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- 239000007921 spray Substances 0.000 description 1
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- 239000004562 water dispersible granule Substances 0.000 description 1
- 239000004563 wettable powder Substances 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present disclosure relates to a preparation method and an application of a chlorothalonil nano pesticide preparation, wherein the pesticide preparation comprises an active ingredient, graphene flakes, polydopamine and an auxiliary agent, wherein the active ingredient comprises chlorothalonil, and the auxiliary agent comprises a dispersion wetting agent, a thickening agent, a defoaming agent, an antifreezing agent, water and a solid carrier; wherein, based on the total weight of the nano pesticide preparation, the content of chlorothalonil is 1-75%, the content of graphene flakes is 0.5-50%, and the content of polydopamine is 0.2-20%. The nano pesticide preparation provided by the disclosure has obvious sustained-release effect and low usage amount, and is one of approaches for solving environmental pollution and material waste caused by the large-scale use of pesticides.
Description
Technical Field
The disclosure relates to the technical field of pesticides, and particularly relates to a preparation method and application of a chlorothalonil nano pesticide preparation.
Background
The hazelnut tree has shorter cultivation period and lighter pest and disease damage than other fruit trees. The diseases mainly comprise powdery mildew and fruit stalk blight, and the pests mainly comprise hazelnut weevils, some leaf-eating pests and the like. Powdery mildew mainly damages leaves, yellow spots are generated on the leaves, then the yellow spots are expanded and developed into circular or oval disease spots, and white powdery mildew layers are generated on the surfaces of the leaves. The mildew stains are independently dispersed in the early stage and then combined into a large mildew spot, even the large mildew spot can cover the whole leaves, the photosynthesis is seriously influenced, the normal metabolism is interfered, the premature senility is caused, and the yield is lost.
In the process of treating powdery mildew, environmental pollution and material waste caused by the use of a large amount of pesticides are always the problems of great concern in the pesticide use process, most of the pesticides applied to the farmland run off to the environment along with leaching, evaporation, drifting and decomposition, only a small part of the pesticides reach an action target, and the environmental pollution and the threat to human health are caused. The research and development of novel pesticide preparations are important ways for solving the problems, and the development of novel organic polymers, biogenic materials and inorganic materials provides a theoretical basis for the research and development of nano pesticides. The nano pesticide can improve the utilization rate of the pesticide, reduce the dosage of the pesticide and reduce agricultural non-point source pollution caused by the pesticide, and has important significance for modern ecological agriculture.
The chlorothalonil is a broad-spectrum protective bactericide, and the action mechanism is that the chlorothalonil can act with glyceraldehyde triphosphate dehydrogenase in fungal cells and is combined with protein containing cysteine in the enzyme, so that the enzyme activity is damaged, and the metabolism of the fungal cells is damaged to lose the vitality. The chlorothalonil has no internal absorption and conduction effects, so that the prolongation of the efficacy duration of the chlorothalonil by a preparation technology has important significance.
Disclosure of Invention
The invention provides a preparation method and application of a chlorothalonil nano pesticide preparation, which can improve the contact area of chlorothalonil and plant leaves, improve the pesticide utilization rate, reduce the pesticide use amount and prolong the pesticide duration.
In order to achieve the above object, the present disclosure provides a chlorothalonil nano pesticide formulation comprising an active ingredient, graphene flakes, polydopamine and an adjuvant, wherein the active ingredient comprises chlorothalonil and the adjuvant comprises a dispersion wetting agent, a thickening agent, a defoaming agent, an antifreezing agent, water and a solid carrier; wherein, based on the total weight of the nano pesticide preparation, the content of chlorothalonil is 1-75%, the content of graphene flakes is 0.5-50%, and the content of polydopamine is 0.2-20%.
In another aspect, the present disclosure provides a method for preparing chlorothalonil nano pesticide formulation, the method comprising:
s1, adding the graphene raw material into N-methyl pyrrolidone to obtain a graphene raw material dispersion liquid;
s2, shearing the graphene raw material dispersion liquid, centrifuging to obtain a supernatant, performing suction filtration on the supernatant by using a polyvinylidene fluoride membrane filter membrane to obtain filter residues, and drying the filter residues to obtain graphene sheets;
s3, mixing chlorothalonil technical, the graphene sheet and a solvent, and then oscillating for 12-48h at the temperature of 20-40 ℃ and the rotating speed of 100-200rpm to obtain a first dispersion liquid;
s4, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 7.0-9.0;
s5, mixing the second dispersion liquid with dopamine hydrochloride, stirring and reacting for 4-10h at the rotation speed of 800rpm of 500-;
s6, uniformly mixing the first material and the auxiliary agent; the adjuvant is selected from at least one of a dispersing wetting agent, a thickener, a defoamer, an antifreeze, water and a solid carrier.
On the other hand, the disclosure also provides application of the chlorothalonil nano pesticide preparation in preventing and treating powdery mildew of hazelnuts.
By the technical scheme, the nano pesticide preparation provided by the disclosure has an obvious sustained-effect and sustained-release effect; meanwhile, the nanometer pesticide preparation reduces leaching, evaporation, drifting and decomposition loss of pesticide components to the environment, has low usage amount, and is an effective way for solving environmental pollution and material waste caused by large-scale use of pesticides.
Additional features and advantages of the disclosure will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present disclosure. It should be understood that the detailed description and specific examples, while indicating the present disclosure, are given by way of illustration and explanation only, not limitation.
The first aspect of the present disclosure provides a chlorothalonil nano pesticide formulation, which is characterized in that the pesticide formulation contains an active ingredient, graphene flakes, polydopamine and an auxiliary agent, wherein the active ingredient comprises chlorothalonil, and the auxiliary agent comprises a dispersion wetting agent, a thickening agent, an antifoaming agent, an antifreezing agent, water and a solid carrier;
according to the first aspect of the present disclosure, optionally, based on the total weight of the nano pesticide preparation, the chlorothalonil content is 1 to 75%, the graphene flakes content is 0.5 to 50%, and the polydopamine content is 0.2 to 20%.
Chlorothalonil is a trade name of tetrachloroisophthalonitrile (2, 4, 5, 6-tetrachloro-1, 3-phthalonitrile), and has a molecular formula: c8N2Cl4Relative molecular weight: 265.91, english name: chlorothalonil, CAS No.: 1897-45-6, the structural formula is shown in formula (1):
graphene is a two-dimensional carbon material in which a single layer of graphene consists of one layer of carbon atoms, typically only 0.35nm thick. England physicists Andelim Gem and Constantine Novoschloff successfully isolated graphene from graphite in 2004 and confirmed that it could exist alone. 3 of 4 valence electrons of carbon atoms in the graphene form a planar regular hexagonal linked honeycomb structure with three nearest carbon atoms in an sp2 hybridized form, and the other one is sigma perpendicular to the plane of the carbon atomszOrbital electrons form large pi bonds on both sides of the lattice plane, as do benzene rings, which are highly roving. The binary electron valence bond structure enables the graphene to have a large pi electron system and a large specific surface area, and the characteristics make the graphene suitable for each kind of grapheneThe adsorption of organic compounds and metals has many articles reporting that graphene is used for drug loading and treatment of pesticide pollution in water, and the mechanism of the graphene loaded drug can be pi-pi action, intermolecular action, hydrophobic action and the like. The graphene prepared by the ultrasonic stripping method is used for researching pesticide loading, and has important significance for research and development of nano pesticides.
According to the first aspect of the present disclosure, the particle size of the nano pesticide preparation can be varied in a wide range, the thickness of the graphene sheet is 1.0-5.0nm, and the length and width are 200-500 nm.
According to the first aspect of the present disclosure, preferably, the content of chlorothalonil is 1-40%, the content of graphene flakes is 0.2-20%, and the content of polydopamine is 0.1-10%, based on the total weight of the nano pesticide preparation.
According to the first aspect of the present disclosure, optionally, based on the total weight of the nano pesticide formulation, the content of the dispersion wetting agent is 1 to 30%, the content of the thickener is 0 to 10%, the content of the defoamer is 0 to 1%, the content of the antifreeze agent is 0 to 10%, the content of the water is 0 to 95%, and the content of the solid carrier is 0 to 95%.
Preferably, based on the total weight of the nano pesticide preparation, the content of the dispersing wetting agent is 1-10%, the content of the thickening agent is 0-5%, the content of the defoaming agent is 0-0.5%, the content of the antifreezing agent is 0-5%, the content of the water is 0-80%, and the content of the solid carrier is 0-80%.
The dispersing wetting agent is at least one selected from fatty alcohol-polyoxyethylene ether, polyoxyethylene polyoxypropylene ether block copolymer, alkyl naphthalene sulfonate formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, phosphate, sodium succinate, sodium dodecyl sulfate and hydroxy polyethylene oxide block copolymer.
The thickener is at least one selected from magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black.
The defoaming agent is selected from silicone oil, organic silicone compound, ester-ether compound, and C8-C12Fatty alcohol compounds of (1) and (C)10-C20At least one of the fatty acid compounds of (1).
The water is selected from at least one of deionized water, distilled water and tap water.
The solid carrier is at least one selected from kaolin, calcined kaolin, white carbon black, diatomite, argil, corn starch and soluble starch.
The second aspect of the present disclosure provides a preparation method of chlorothalonil nano pesticide preparation, which comprises:
s1, adding the graphene raw material into N-methyl pyrrolidone to obtain graphene raw material dispersion liquid,
s2, shearing the graphene raw material dispersion liquid, centrifuging to obtain a supernatant, performing suction filtration on the supernatant by using a polyvinylidene fluoride membrane filter membrane to obtain filter residues, and drying the filter residues to obtain graphene sheets;
s3, mixing chlorothalonil technical, the graphene sheet and a solvent, and then oscillating for 12-48h at the temperature of 20-40 ℃ and the rotating speed of 100-200rpm to obtain a first dispersion liquid;
s4, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 7.0-9.0;
s5, mixing the second dispersion liquid with dopamine hydrochloride, stirring and reacting for 4-10h at the rotation speed of 800rpm of 500-;
s6, uniformly mixing the first material and the auxiliary agent; the adjuvant is selected from at least one of a dispersing wetting agent, a thickener, a defoamer, an antifreeze, water and a solid carrier.
According to the second aspect of the present disclosure, optionally, based on the total weight of the nano pesticide preparation, the content of chlorothalonil is 1 to 75%, the content of graphene flakes is 0.2 to 50%, and the content of polydopamine is 0.2 to 20%.
According to the second aspect of the present disclosure, preferably, the content of chlorothalonil is 1-40%, the content of graphene flakes is 0.5-20%, and the content of polydopamine is 0.2-10%, based on the total weight of the nano pesticide preparation.
According to the second aspect of the present disclosure, the graphene sheet has a thickness of 1.0-5.0nm and a length and width of 200-500 nm.
According to the second aspect of the present disclosure, based on the total weight of the nano pesticide formulation, the content of the dispersion wetting agent is 1 to 30%, the content of the thickener is 0 to 10%, the content of the defoamer is 0 to 1%, the content of the antifreeze is 0 to 10%, the content of the water is 0 to 95%, and the content of the solid carrier is 0 to 95%; preferably, based on the total weight of the nano pesticide preparation, the content of the dispersion wetting agent is 1-10%, the content of the thickening agent is 0-5%, the content of the defoaming agent is 0-0.5%, the content of the antifreezing agent is 0-5%, the content of the water is 0-80%, and the content of the solid carrier is 0-80%;
according to the second aspect of the present disclosure, the dispersion wetting agent is selected from at least one of fatty alcohol-polyoxyethylene ether, polyoxyethylene polyoxypropylene ether block copolymer, alkyl naphthalene sulfonate formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, phosphate ester, sodium sulfosuccinate, sodium lauryl sulfate and hydroxy polyethylene oxide block copolymer;
according to a second aspect of the present disclosure, the thickener is selected from at least one of magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite, and white carbon black;
according to a second aspect of the present disclosure, the antifoaming agent is selected from silicone oils, silicone-based compounds, ester-ether-type compounds, C8-C12Fatty alcohol compounds of (1) and (C)10-C20At least one of the fatty acid compounds of (a);
according to a second aspect of the present disclosure, the water is selected from at least one of deionized water, distilled water, and tap water;
according to a second aspect of the present disclosure, the solid support is selected from at least one of kaolin, calcined kaolin, white carbon, diatomaceous earth, china clay, corn starch, and soluble starch.
In a third aspect of the present disclosure, an application of chlorothalonil nano pesticide preparation in controlling powdery mildew of hazelnut is provided, wherein the nano pesticide preparation is the nano pesticide preparation described in the first aspect of the present disclosure or the nano pesticide preparation prepared by the method described in the second aspect of the present disclosure.
The present disclosure is further illustrated by the following examples, but is not to be construed as being limited thereby.
The raw materials, reagents, instruments and equipment involved in the examples of the present disclosure may be commercially available, unless otherwise specified.
Example 1
S1, adding a graphene raw material into N-methyl pyrrolidone to obtain a graphene raw material dispersion liquid, dispersing at room temperature for 15 hours at the rotation speed of 18000rpm by using a high shear emulsifying machine, centrifuging for 60 minutes at the rotation speed of 1000rpm after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane to obtain filter residues, and performing vacuum drying on the filter residues to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 100.
s2, dispersing original chlorothalonil and graphene sheets in acetone, and oscillating for 24 hours at the rotating speed of 200rpm in a constant-temperature oscillation incubator at the temperature of 30 ℃ to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to the acetone is 1: 0.5: 50.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 8.0, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 0.02.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm for reaction for 6 hours, centrifuging at 1500rpm for 30 minutes, removing the supernatant, and drying the remainder to obtain a first material, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.2.
s5, adding sodium lignosulfonate, xanthan gum, ethylene glycol and deionized water into the first material, and uniformly mixing, wherein the weight ratio of the first material to the sodium lignosulfonate, the xanthan gum, the ethylene glycol and the deionized water is 1: 0.1: 0.01: 0.1: 1, obtaining the chlorothalonil nano pesticide preparation.
Through detection, the thickness of the graphene sheet layer is 2.0-3.0nm, the length and width are 200-480nm, and the pesticide loading rate is 84.62%.
Example 2
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: the weight ratio of the graphene to the N-methylpyrrolidone is 1: 400.
through detection, the thickness of the sheet layer of the graphene sheet is 1.0-2.0nm, the length and width are 200-480nm, and the pesticide loading rate is 84.53%.
Example 3
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: the weight ratio of chlorothalonil to graphene flakes to acetone is 1: 0.5: 200.
through detection, the thickness of the graphene sheet layer is 1.5-3.0nm, the length and width are 210-480nm, and the pesticide loading rate is 83.50%.
Example 4
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: the weight ratio of the first dispersion to the Tris buffer was 1: 0.05.
through detection, the thickness of the graphene sheet layer system sheet layer is 2.5-4.0nm, the length and width are 210-480nm, and the pesticide loading rate is 83.04%.
Example 5
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.01.
through detection, the thickness of the graphene sheet layer is 2.5-4.0nm, the length and width are 210-480nm, and the pesticide loading rate is 83.12%.
Example 6
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: the weight ratio of the chlorothalonil-graphene sheet layer system to sodium lignin sulfonate, xanthan gum, glycol and deionized water is 1: 0.15: 0.015: 0.1: 1.
through detection, the thickness of the graphene sheet layer system sheet layer is 2.0-3.0nm, the length and width are 200-480nm, and the pesticide loading rate is 84.54%.
Example 7
S1, adding a graphene raw material into N-methyl pyrrolidone to obtain a graphene dispersion liquid, dispersing at room temperature for 15 hours at a rotation speed of 20000rpm by using a high shear emulsifying machine, centrifuging for 60 minutes at a rotation speed of 1000rpm after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 200.
s2, dispersing original chlorothalonil and graphene sheets in acetone, and oscillating for 24 hours in a constant-temperature oscillation incubator at 25 ℃ at the rotating speed of 200rpm to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to a solvent is 1: 1: 98.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 8.5, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 0.05.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring and reacting for 6h at 800rpm, centrifuging for 30min at the rotating speed of 2000rpm, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.05.
s5, adding sodium lignosulfonate, xanthan gum, ethylene glycol and deionized water into the chlorothalonil-graphene sheet system, and uniformly mixing. The weight ratio of the chlorothalonil-graphene sheet layer system to sodium lignin sulfonate, xanthan gum, glycol and deionized water is 1: 0.05: 0.01: 0.2: 2.
through detection, the thickness of the graphene sheet layer system sheet layer is 1.5-3.0nm, the length and width are 150nm-450nm, and the pesticide loading rate is 80.33%.
Example 8
S1, adding a graphene raw material into N-methyl pyrrolidone to obtain a graphene dispersion solution, dispersing at room temperature for 16 hours at 10000rpm by using a high shear emulsifying machine, centrifuging for 60 minutes at 1000rpm after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 800.
s2, dispersing original chlorothalonil and graphene sheets in N, N-dimethylformamide, and oscillating for 12 hours at a constant temperature of 35 ℃ in an oscillation incubator at a speed of 180rpm to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to the N, N-dimethylformamide is 1: 2: 20.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 7.8, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 2.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm for reaction for 8 hours, centrifuging at 2000rpm for 30 minutes, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.5.
s5, adding sodium lignosulfonate and soluble starch into the chlorothalonil-graphene sheet system, and uniformly mixing to obtain the chlorothalonil nano pesticide preparation, wherein the weight ratio of the chlorothalonil-graphene sheet system to the sodium lignosulfonate to the soluble starch is 1: 0.1: 0.1.
through detection, the thickness of the graphene sheet layer system sheet layer is 1.0-2.0nm, the length and width are 250-480nm, and the pesticide loading rate is 80.05%.
Example 9
S1, adding a graphene raw material into N-methyl pyrrolidone to obtain a graphene dispersion solution, dispersing at 28000rpm for 24 hours at room temperature by using a high shear emulsifying machine, centrifuging at 900rpm for 60 minutes after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 500.
s2, dispersing original chlorothalonil and graphene flakes in aromatic hydrocarbon solvent oil, and oscillating for 36 hours at a constant temperature of 38 ℃ at 200rpm in an oscillation incubator to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene flakes to the aromatic hydrocarbon solvent oil is 1: 0.1: 48.9.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 7.5, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 0.5.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm for reaction for 6 hours, centrifuging for 30 minutes, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.08.
s5, adding sodium lignosulfonate, silicone oil and anhydrous sodium sulphate into the chlorothalonil-graphene sheet layer system, and uniformly mixing to obtain the chlorothalonil nano pesticide preparation, wherein the weight ratio of the chlorothalonil-graphene sheet layer system to the sodium lignosulfonate, the silicone oil and the anhydrous sodium sulphate is 1: 0.05: 1.2.
through detection, the thickness of the graphene sheet layer system sheet layer is 1.0-2.0nm, the length and width are 250-370nm, and the pesticide loading rate is 78.64%.
Example 10
S1, adding graphene into N-methyl pyrrolidone to obtain a graphene dispersion solution, dispersing at the room temperature for 12 hours at the rotation speed of 19000rpm by using a high shear emulsifying machine, centrifuging for 60 minutes at the rotation speed of 900rpm after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 100.
s2, dispersing original chlorothalonil and graphene sheets in aromatic hydrocarbon solvent oil, and oscillating for 24 hours in a constant-temperature oscillation incubator at the temperature of 30 ℃ at the rotating speed of 190rpm to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to the aromatic hydrocarbon solvent oil is 1: 30: 90.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 8.8, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 0.02.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm for reaction for 5 hours, centrifuging for 30 minutes, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.009.
s5, adding sodium lignosulfonate, silicone oil and anhydrous sodium sulphate into the chlorothalonil-graphene sheet system to obtain the chlorothalonil nano pesticide preparation, wherein the weight ratio of the chlorothalonil-graphene sheet system to the sodium lignosulfonate, the silicone oil and the anhydrous sodium sulphate is 1: 0.2: 0.002: 2.
through detection, the thickness of the graphene sheet is 1.7-5.0nm, the length and the width are 180-500 nm, and the pesticide loading rate is 76.20%.
Example 11
S1, adding graphene into N-methyl pyrrolidone to obtain graphene dispersion liquid, dispersing for 12-24 h at room temperature at 12000rpm by using a high shear emulsifying machine, centrifuging for 60min at 900rpm after dispersion to obtain supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 100.
s2, dispersing original chlorothalonil and graphene sheets in N, N-dimethylformamide, and oscillating for 18h at 180rpm in a constant-temperature oscillation incubator at 28 ℃ to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to the N, N-dimethylformamide is 1: 40: 90.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 8.5, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 1.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm, reacting for 6 hours, centrifuging for 30 minutes, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.2.
s5, adding polycarboxylate, lauryl sodium sulfate, xanthan gum, glycerol and deionized water into the chlorothalonil-graphene sheet layer system to obtain the chlorothalonil nano pesticide preparation, wherein the weight ratio of the chlorothalonil-graphene sheet layer system to the polycarboxylate, the lauryl sodium sulfate, the xanthan gum, the glycerol and the deionized water is 1: 0.3: 0.1: 0.01: 0.2: 40.
through detection, the thickness of the graphene sheet layer system sheet layer is 1.0-2.0nm, the length and width are 200-450nm, and the pesticide loading rate is 75.07%.
Example 12
S1, adding graphene into N-methyl pyrrolidone to obtain a graphene dispersion solution, dispersing at a rotation speed of 30000rpm for 12 hours at room temperature by using a high shear emulsifying machine, centrifuging at a rotation speed of 800rpm for 60 minutes after dispersion to obtain a supernatant containing graphene flakes, performing suction filtration by using a polyvinylidene fluoride membrane filter membrane, and performing vacuum drying to obtain the graphene flakes, wherein the weight ratio of graphene to N-methyl pyrrolidone is 1: 80.
s2, dispersing original chlorothalonil and graphene sheets in acetone, and oscillating for 12 hours at a constant temperature of 25 ℃ in an oscillation incubator at 200rpm to obtain a first dispersion liquid, wherein the weight ratio of the chlorothalonil to the graphene sheets to the acetone is 1: 1: 98.
s3, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 8.2, wherein the weight ratio of the first dispersion solution to the Tris buffer solution is 1: 0.3.
s4, adding dopamine hydrochloride into the second dispersion liquid, stirring at 800rpm for reaction for 4 hours, centrifuging at 2000rpm for 30 minutes, and drying to obtain a chlorothalonil-graphene sheet layer system, wherein the mass ratio of the second dispersion liquid to the dopamine hydrochloride is 1: 0.01.
s5, adding sodium lignosulfonate and soluble starch into the chlorothalonil-graphene sheet layer system, and uniformly mixing to obtain the chlorothalonil nano pesticide preparation, wherein the weight ratio of the chlorothalonil-graphene sheet layer system to the sodium lignosulfonate to the soluble starch is 1: 0.5: 23.5.
through detection, the thickness of the graphene sheet layer system sheet layer is 2.0-4.0nm, the length and width are 260nm-470nm, and the pesticide loading rate is 73.45%.
Comparative example 1
Mixing chlorothalonil, sodium lignosulfonate, xanthan gum, glycol and deionized water, wherein the weight ratio of the chlorothalonil to the sodium lignosulfonate, the xanthan gum, the glycol and the deionized water is 1: 0.1: 0.01: 0.1: suspending agents are prepared according to conventional methods in the art.
Comparative example 2
Mixing chlorothalonil, sodium lignosulfonate and soluble starch, wherein the weight ratio of the chlorothalonil to the sodium lignosulfonate to the soluble starch is 1: 0.1: 0.1, preparing wettable powder according to the conventional method in the field.
Comparative example 3
Mixing chlorothalonil, sodium lignosulfonate and soluble starch, wherein the weight ratio of the chlorothalonil to the sodium lignosulfonate to the soluble starch is 1: 0.1: 0.1, preparing the water dispersible granule according to the conventional method in the field.
Comparative example 4
Chlorothalonil nano pesticide formulations were prepared using the method of example 1, except that: and dispersing the graphene dispersion liquid for 24 hours at room temperature at 8000rpm by using a high-shear emulsifying machine.
Through detection, the method cannot prepare the chlorothalonil nano pesticide preparation.
Test example 1
The test example tests the indoor control effect of the chlorothalonil nano pesticide preparations obtained in examples 1-12 and the chlorothalonil preparations obtained in comparative examples 1-3 on powdery mildew of hazelnuts. Before the test, a certain amount of distilled water is added, the mixture is uniformly stirred, and the concentration of the chlorothalonil in the embodiment is adjusted to be 0.1 weight percent for standby.
Selecting potted seedlings with uniform growth height of 70-80cm, spraying the leaves of the above medicinal preparation, adding clear water blank control, and repeating for 3 times. Inoculating the application agent by spore shaking method on the 2 nd day after treatment, and normally managing the inoculated crops in a greenhouse (25 +/-1) DEG C. After 10 days of drug application, 30 leaves are respectively collected for each treatment of each hazel tree. The lesion and the leaf area are measured by Photoshop CC2014, and the percentage of the lesion to the leaf area is calculated.
The hazard degree of powdery mildew is divided into 6 grades, 0 grade: no disease spots; level 1: the ratio of the lesion area to the leaf area is 0 to 10%; and 2, stage: the ratio of the lesion area to the leaf area is 10-25 percent; and 3, level: the ratio of the lesion area to the leaf area is 25-50 percent; 4, level: the ratio of the lesion area to the leaf area is 50-75 percent; and 5, stage: the ratio of the lesion area to the leaf area is greater than 75%. The prevention and treatment effect is calculated according to the disease index.
The control effect of powdery mildew on hazelnuts is shown in table 1.
| Treatment of | Powdery mildew control effect (%) |
| Example 1 | 98.40 |
| Example 2 | 98.32 |
| Example 3 | 98.34 |
| Example 4 | 98.06 |
| Example 5 | 98.12 |
| Example 6 | 98.04 |
| Example 7 | 97.46 |
| Example 8 | 96.55 |
| Example 9 | 96.30 |
| Example 10 | 95.44 |
| Example 11 | 95.20 |
| Example 12 | 95.05 |
| Comparative example 1 | 80.65 |
| Comparative example 2 | 78.45 |
| Comparative example 3 | 76.60 |
| Blank control | — |
The test example tests the field control effect of the chlorothalonil nano pesticide preparations obtained in examples 1-12 and the chlorothalonil preparations obtained in comparative examples 1-3 on powdery mildew of hazelnuts. Before the test, a certain amount of distilled water is added, the mixture is uniformly stirred, and the concentration of the chlorothalonil in the embodiment is adjusted to be 0.1 weight percent for standby.
Test site: chang tu county, Liaoning province. The application time is 2017 in late 4 th of month. The land has flat land and good fertility. And (4) carrying out conventional production management on the hazelnut in each treatment area after the pesticide is applied. The tree age of the selected hazel tree is 8 years, and the average height of the crown is 1.25 m. The disease conditions of the powdery mildew strains of the hazelnut are consistent, and the disease indexes reach 80 percent.
The method comprises the specific steps that a backpack sprayer is used, liquid medicine is uniformly sprayed on hazel tree plants in each planting area, a blank control group uses equal amount of clear water to spray the hazel tree plants in the planting areas, and when the liquid medicine is applied, a plastic film is used for shielding adjacent cells to prevent mutual interference of the liquid medicine. Each agent treatment was repeated 3 times. Control was water, repeated 3 times. The control effect of powdery mildew on hazelnuts was investigated 10 days, 20 days, 30 days and 50 days after the application of the pesticide. Each treatment area adopts random 5-point sampling, each treatment area investigates 25 hazelnuts, old leaves are separated from new leaves, and each treatment area collects 30 new leaves and old leaves respectively. The lesion and the leaf area are measured by Photoshop CC2014, and the percentage of the lesion to the leaf area is calculated.
The method for calculating the grading condition of powdery mildew, disease index and prevention and treatment effect is the same as that in test example 1. The control effect of powdery mildew on hazelnuts in each treatment area is shown in table 2.
TABLE 2
As can be seen from tables 1 and 2, the chlorothalonil nano pesticide preparation provided by the disclosure has a sustained and sustained release effect, is low in usage amount, and improves the pesticide utilization rate.
The preferred embodiments of the present disclosure have been described in detail above, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all fall within the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of various embodiments of the present disclosure may be made, and the same should be considered as the disclosure of the present disclosure, as long as it does not depart from the spirit of the present disclosure.
Claims (10)
1. A chlorothalonil nano pesticide preparation comprises an active ingredient, graphene flakes, polydopamine and auxiliaries, wherein the active ingredient comprises chlorothalonil, and the auxiliaries comprise a dispersion wetting agent, a thickening agent, an antifoaming agent, an antifreezing agent, water and a solid carrier; wherein, based on the total weight of the nano pesticide preparation, the content of chlorothalonil is 1-75%, the content of graphene flakes is 0.5-50%, and the content of polydopamine is 0.2-20%.
2. The pesticide formulation as claimed in claim 1, wherein the chlorothalonil content is 1-40%, the graphene flakes content is 0.5-20%, and the polydopamine content is 0.2-10%, based on the total weight of the nano pesticide formulation.
3. The pesticide formulation as set forth in claim 1 wherein the graphene flakes have a thickness of 1.0 to 5.0nm and a length and width of 200-500 nm.
4. The pesticide formulation as set forth in claim 1 wherein the content of said dispersion wetting agent is 1 to 30%, the content of said thickener is 0 to 10%, the content of said defoamer is 0 to 1%, the content of said antifreeze is 0 to 10%, the content of said water is 0 to 95%, the content of said solid carrier is 0 to 95% based on the total weight of said nano pesticide formulation; preferably, based on the total weight of the nano pesticide preparation, the content of the dispersion wetting agent is 1-10%, the content of the thickening agent is 0-5%, the content of the defoaming agent is 0-0.5%, the content of the antifreezing agent is 0-5%, the content of the water is 0-80%, and the content of the solid carrier is 0-80%;
the dispersing wetting agent is selected from at least one of fatty alcohol-polyoxyethylene ether, polyoxyethylene polyoxypropylene ether block copolymer, alkyl naphthalene sulfonate formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, phosphate, sodium succinate, lauryl sodium sulfate and hydroxy polyethylene oxide block copolymer;
the thickening agent is selected from at least one of magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black;
the defoaming agent is selected from silicone oil, organic silicone compound, ester-ether compound, and C8-C12Fatty alcohol compounds of (1) and (C)10-C20At least one of the fatty acid compounds of (a);
the water is selected from at least one of deionized water, distilled water and tap water;
the solid carrier is at least one selected from kaolin, calcined kaolin, white carbon black, diatomite, argil, corn starch and soluble starch.
5. A preparation method of chlorothalonil nano pesticide preparation comprises the following steps:
s1, adding the graphene raw material into N-methyl pyrrolidone to obtain a graphene raw material dispersion liquid;
s2, shearing the graphene raw material dispersion liquid, centrifuging to obtain a supernatant, performing suction filtration on the supernatant by using a polyvinylidene fluoride membrane filter membrane to obtain filter residues, and drying the filter residues to obtain graphene sheets;
s3, mixing chlorothalonil technical, the graphene sheet and a solvent, and then oscillating for 12-48h at the temperature of 20-40 ℃ and the rotating speed of 100-200rpm to obtain a first dispersion liquid;
s4, adding a Tris buffer solution into the first dispersion solution to obtain a second dispersion solution with the pH value of 7.0-9.0;
s5, mixing the second dispersion liquid with dopamine hydrochloride, stirring and reacting for 4-10h at the rotation speed of 800rpm of 500-;
s6, uniformly mixing the first material and the auxiliary agent; the adjuvant is selected from at least one of a dispersing wetting agent, a thickener, a defoamer, an antifreeze, water and a solid carrier.
6. The preparation method according to claim 5, wherein the chlorothalonil is in an amount of 1-75%, the graphene flakes are in an amount of 0.5-50%, and the polydopamine is in an amount of 0.2-20%, based on the total weight of the nano pesticide preparation.
7. The preparation method according to claim 5, wherein the chlorothalonil content is 1-40%, the graphene flakes content is 0.5-20%, and the polydopamine content is 0.2-10%, based on the total weight of the nano pesticide preparation.
8. The method as claimed in claim 5, wherein the graphene sheet has a thickness of 1.0-5.0nm and a length and width of 200-500 nm.
9. The preparation method according to claim 5, wherein the content of the dispersion wetting agent is 1-30%, the content of the thickener is 0-10%, the content of the defoamer is 0-1%, the content of the antifreeze is 0-10%, the content of the water is 0-95%, and the content of the solid carrier is 0-95% based on the total weight of the nano pesticide formulation; preferably, based on the total weight of the nano pesticide preparation, the content of the dispersion wetting agent is 1-10%, the content of the thickening agent is 0-5%, the content of the defoaming agent is 0-0.5%, the content of the antifreezing agent is 0-5%, the content of the water is 0-80%, and the content of the solid carrier is 0-80%;
the dispersing wetting agent is selected from at least one of fatty alcohol-polyoxyethylene ether, polyoxyethylene polyoxypropylene ether block copolymer, alkyl naphthalene sulfonate formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate, phosphate, sodium succinate, lauryl sodium sulfate and hydroxy polyethylene oxide block copolymer;
the thickening agent is selected from at least one of magnesium aluminum silicate, xanthan gum, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, bentonite and white carbon black;
the defoaming agent is selected from silicone oil, organic silicone compound, ester-ether compound, and C8-C12Fatty alcohol compounds of (1) and (C)10-C20At least one of the fatty acid compounds of (a);
the water is selected from at least one of deionized water, distilled water and tap water;
the solid carrier is at least one selected from kaolin, calcined kaolin, white carbon black, diatomite, argil, corn starch and soluble starch.
10. Use of the chlorothalonil nano pesticide formulation according to any one of claims 1 to 4 or prepared by the preparation method of the chlorothalonil nano pesticide formulation according to any one of claims 5 to 9 for preventing and treating powdery mildew of hazelnuts.
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