CN117918344A - High-efficiency cyhalothrin soluble solid nano-preparation and preparation method thereof - Google Patents
High-efficiency cyhalothrin soluble solid nano-preparation and preparation method thereof Download PDFInfo
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- CN117918344A CN117918344A CN202311492639.1A CN202311492639A CN117918344A CN 117918344 A CN117918344 A CN 117918344A CN 202311492639 A CN202311492639 A CN 202311492639A CN 117918344 A CN117918344 A CN 117918344A
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- cyhalothrin
- soluble solid
- solid nano
- preparation
- sulfonate
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- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 title claims abstract description 52
- 239000007787 solid Substances 0.000 title claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002270 dispersing agent Substances 0.000 claims abstract description 29
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 239000000080 wetting agent Substances 0.000 claims abstract description 9
- 239000003755 preservative agent Substances 0.000 claims abstract description 7
- 230000002335 preservative effect Effects 0.000 claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 25
- -1 alkyl glycosides Chemical class 0.000 claims description 24
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 16
- 238000009472 formulation Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- 230000001804 emulsifying effect Effects 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 11
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 11
- 239000003945 anionic surfactant Substances 0.000 claims description 10
- 238000010008 shearing Methods 0.000 claims description 10
- 229910019142 PO4 Inorganic materials 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 9
- 239000010452 phosphate Substances 0.000 claims description 9
- ZXQYGBMAQZUVMI-RDDWSQKMSA-N (1S)-cis-(alphaR)-cyhalothrin Chemical compound CC1(C)[C@H](\C=C(/Cl)C(F)(F)F)[C@@H]1C(=O)O[C@@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-RDDWSQKMSA-N 0.000 claims description 8
- 125000000129 anionic group Chemical group 0.000 claims description 8
- 239000005910 lambda-Cyhalothrin Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 239000012876 carrier material Substances 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 5
- 239000000194 fatty acid Substances 0.000 claims description 5
- 229930195729 fatty acid Natural products 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- 229930195725 Mannitol Natural products 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 3
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 3
- 239000000594 mannitol Substances 0.000 claims description 3
- 235000010355 mannitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 235000010356 sorbitol Nutrition 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 239000000811 xylitol Substances 0.000 claims description 3
- 235000010447 xylitol Nutrition 0.000 claims description 3
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 3
- 229960002675 xylitol Drugs 0.000 claims description 3
- SQAINHDHICKHLX-UHFFFAOYSA-N 1-naphthaldehyde Chemical compound C1=CC=C2C(C=O)=CC=CC2=C1 SQAINHDHICKHLX-UHFFFAOYSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 2
- WQZGKKKJIJFFOK-PHYPRBDBSA-N alpha-D-galactose Chemical compound OC[C@H]1O[C@H](O)[C@H](O)[C@@H](O)[C@H]1O WQZGKKKJIJFFOK-PHYPRBDBSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 150000002193 fatty amides Chemical class 0.000 claims description 2
- 229930182830 galactose Natural products 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229930182470 glycoside Natural products 0.000 claims description 2
- 239000001863 hydroxypropyl cellulose Substances 0.000 claims description 2
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- 229940069328 povidone Drugs 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 229940104261 taurate Drugs 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 26
- 239000002245 particle Substances 0.000 abstract description 22
- 229940079593 drug Drugs 0.000 abstract description 17
- 239000000575 pesticide Substances 0.000 abstract description 15
- 239000007788 liquid Substances 0.000 abstract description 12
- 241000607479 Yersinia pestis Species 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000009736 wetting Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract description 2
- 238000003892 spreading Methods 0.000 abstract description 2
- 230000007480 spreading Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000725 suspension Substances 0.000 description 8
- 238000012512 characterization method Methods 0.000 description 6
- 241001124076 Aphididae Species 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000002552 dosage form Substances 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 241000238631 Hexapoda Species 0.000 description 3
- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004563 wettable powder Substances 0.000 description 3
- 244000061456 Solanum tuberosum Species 0.000 description 2
- 235000002595 Solanum tuberosum Nutrition 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000004495 emulsifiable concentrate Substances 0.000 description 2
- 239000008233 hard water Substances 0.000 description 2
- 230000000749 insecticidal effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000239290 Araneae Species 0.000 description 1
- 241001674044 Blattodea Species 0.000 description 1
- 230000005653 Brownian motion process Effects 0.000 description 1
- 241000254173 Coleoptera Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 241000738498 Epitrix pubescens Species 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 241000255967 Helicoverpa zea Species 0.000 description 1
- 241000346285 Ostrinia furnacalis Species 0.000 description 1
- 241000255969 Pieris brassicae Species 0.000 description 1
- 241000500437 Plutella xylostella Species 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 241000985245 Spodoptera litura Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of nano pesticides, and discloses a high-efficiency cyhalothrin soluble solid nano preparation and a preparation method thereof; the nanometer preparation comprises 1-30 high-efficiency cyhalothrin, 0.1-15 wetting agent, 0.1-15 dispersing agent, 0.1-3 preservative and 0.1-37 water; compared with the prior art, the high-efficiency cyhalothrin soluble solid nano preparation overcomes the defects of poor water dispersibility and slow dissolution rate of insoluble pesticides, the particle size of the drug particles is smaller than 300nm, the specific surface area is obviously increased, the dispersion performance of the drug particles is improved, the spreading and wetting performance of the drug liquid on the surfaces of the blades are enhanced, and the control effect of the drug liquid on target pests in the blades in unit area is further improved. In addition, the preparation method is simple and feasible, and the prepared high-efficiency cyhalothrin soluble solid nano preparation has stable physical and chemical properties, is convenient to store and transport, does not contain an organic solvent, has high drug loading capacity and safety, and can be produced in a large scale.
Description
Technical Field
The invention relates to the technical field of nano pesticides, in particular to a high-efficiency cyhalothrin soluble solid nano preparation and a preparation method thereof.
Background
The high-efficiency cyhalothrin is a synthetic pyrethroid insecticide, has the effects of contact killing and stomach poisoning, and has the advantages of wide insecticidal spectrum, quick knockdown and long lasting period. Can be used for preventing and treating cotton bollworm, corn borer, cotton spider mite, vegetable yellow stripe flea beetle, plutella xylostella, cabbage caterpillar, prodenia litura, potato long tube aphid, potato beetle, etc., and also has effect on mosquito, fly, cockroach, etc. The conventional dosage forms of the conventional high-efficiency cyhalothrin mainly comprise emulsifiable concentrate, aqueous emulsion, suspending agent, wettable powder and the like with low concentration content. The emulsifiable concentrate contains a large amount of organic solvents, the aqueous emulsion contains chemical solvents, and the residual pollution is serious. Dust drift can occur in the production and use of wettable powder, and the effective utilization rate of actual pesticides is not high. The dispersion degree of the drug particles in the suspending agent is large, so that the stability problems such as sedimentation and precipitation are easy to occur, and the storage and transportation are inconvenient.
At present, with the rapid development of the nano technology in the agricultural field, the processing of a new pesticide preparation by a nano material and a nano preparation technology becomes a hot spot for the current dosage form processing. The soluble solid nanometer preparation is a novel pesticide preparation prepared by efficiently combining the raw materials, the carrier and the auxiliary agent through a nanometer technology or method.
Disclosure of Invention
The invention provides a high-efficiency cyhalothrin soluble solid nano preparation which can solve the problems of poor water dispersibility and low dissolution rate of the high-efficiency cyhalothrin, overcomes the defects of the traditional dosage form and improves the effective utilization rate of the cyhalothrin soluble solid nano preparation.
The invention provides a high-efficiency cyhalothrin soluble solid nano preparation, which comprises the following components in percentage by weight:
1-30 high-efficiency cyhalothrin, 0.1-15 wetting agent, 0.1-15 dispersing agent, 0.1-3 preservative and 0.1-37 water.
Further, the wetting agent is one or more of nonionic surfactant, sulfonate anionic surfactant, phosphate anionic surfactant, carboxylate anionic surfactant and oligomeric surfactant;
Further, the nonionic surfactant is one or more of alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty amine ethoxylates, alkyl glycosides, polyarylphenol ethoxylates, castor oil ethoxylates, polyoxyethylene fatty acid esters, ethylene oxide/propylene oxide block copolymers, sorbitol esters and polyglycerol fatty acid esters;
The sulfonate anionic surfactant is selected from one or more of alkylbenzene sulfonate, alpha-alkenyl sodium sulfonate, polyoxyethylene ether sulfate, polycyclic aromatic hydrocarbon formaldehyde condensate sulfonate or alkyl aromatic hydrocarbon sulfonate, sodium alkyl succinic sulfonate, polyoxyethylene ether monosuccinate sulfonate, fatty alcohol sulfate and fatty amide N-methyl taurate sodium salt;
The phosphate anionic surfactant is one or more of polyoxyethylene ether phosphate, alkyl alcohol phosphate and alcohol ether carboxylate.
Further, the dispersing agent is one or more of anionic dispersing agent, nonionic dispersing agent, anionic nonionic dispersing agent, high molecular dispersing agent and cationic dispersing agent.
Further, the anionic dispersing agent is one or more of naphthalene formaldehyde condensate sulfonate, alkyl naphthalene formaldehyde condensate sulfonate and lignin sulfonate;
And/or the anionic non-ionic dispersant is one or more of phosphate dispersant, sulfate dispersant and succinate sulfonate;
and/or the nonionic dispersant is one or more of fatty alcohol polyoxypropylene polyoxyethylene ether and polyoxyethylene polypropylene ether block copolymers.
Further, the preparation method of the high-efficiency cyhalothrin soluble solid nano preparation is characterized by comprising the following steps:
(1) Dispersing the high-efficiency cyhalothrin in water, heating, and obtaining a molten phase in a molten state;
(2) Dissolving a wetting agent, a dispersing agent and a preservative in water, and stirring to a transparent state to obtain a dispersed phase;
(3) Mixing the disperse phase with the melt phase at high temperature, and emulsifying the mixture by high-shear dispersion until the emulsion is uniform to obtain emulsion;
(4) And adding a water-soluble carrier material into the emulsion, stirring to obtain a uniform emulsion mixture, and drying to obtain the high-efficiency cyhalothrin soluble solid nano preparation.
Further, in the step (1), the high-efficiency cyhalothrin is dispersed in water and heated to 80 ℃;
and/or, in the step (3), the high temperature is 80 ℃;
And/or in the step (4), the water-soluble carrier material is one or more of polyethylene glycol, povidone, tartaric acid, succinic acid, chitosan, glucose, galactose, sucrose, lactose, mannitol, sorbitol, xylitol, hydroxypropyl cellulose and hydroxypropyl methylcellulose.
Further, in the step (3), the shear rate of the high shear dispersion emulsification is 1000 to 30000rpm/min; the shearing time of the high shearing dispersion emulsifying machine is 0.05-1h;
and/or, in the step (3), the stirring speed is 100-1000rpm/min;
and/or, in the step (4), the drying is drying or freeze drying.
Further, the temperature of the drying is 40 ℃, and the drying time is 2-8 hours;
The pre-freezing temperature of the freeze drying is-80 ℃, the pre-freezing time is 1-6h, and the freeze drying is 12-72h.
The invention also provides a preparation method of any one of the high-efficiency cyhalothrin soluble solid nano-preparation, which comprises the following steps:
(1) Dispersing the high-efficiency cyhalothrin in water, heating, and obtaining a molten phase in a molten state;
(2) Dissolving a wetting agent, a dispersing agent and a preservative in water, and stirring to a transparent state to obtain a dispersed phase;
(3) Mixing the disperse phase with the melt phase at high temperature, and emulsifying the mixture by high-shear dispersion until the emulsion is uniform to obtain emulsion;
(4) And adding a water-soluble carrier material into the emulsion, stirring to obtain a uniform emulsion mixture, and drying to obtain the high-efficiency cyhalothrin soluble solid nano preparation.
Compared with the prior art, the beneficial effects of the method are as follows:
The invention provides a preparation method of a high-efficiency cyhalothrin soluble solid nano preparation, which solves the problem of poor water solubility and dispersibility of the high-efficiency cyhalothrin, obviously enhances the spreading and wetting effects of liquid medicine on the surfaces of blades, further enhances the control effect of the liquid medicine on target pests, and obviously improves the effective utilization rate of pesticides.
The medicine particles prepared by the invention have uniform size distribution, the average particle size is about 10-300nm, the specific surface area of the medicine particles is obviously improved, the contact area between the pesticide active component and the plant diseases and insect pests is enhanced, the control effect of the plant diseases and insect pests is enhanced, the using amount of the pesticide is reduced, and the environmental pollution is further reduced.
The high-efficiency cyhalothrin soluble solid nano preparation has the advantages of small dosage of surfactant, no organic solvent, greatly reduced toxicity and increased non-target biological safety, and can be used as an environment-friendly dosage form.
The high-efficiency cyhalothrin soluble solid nano-preparation has high content of pesticide compound, high drug loading, simple preparation process and capability of being used for amplifying production process.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The primary object and other advantages of the invention may be realized and attained by means of the instrumentalities and particularly pointed out in the specification.
Drawings
FIG. 1 is a process flow diagram of a high-efficiency cyhalothrin soluble solid nano-preparation prepared by the invention;
FIG. 2 is a scanning electron microscope characterization of the 10% lambda-cyhalothrin soluble solid nano-formulation of the present invention of example 1;
FIG. 3 is a scanning electron microscope characterization of a 15% lambda-cyhalothrin soluble solid nano-formulation of the present invention as described in example 2;
FIG. 4 is a scanning electron microscope characterization of the 20% lambda-cyhalothrin soluble solid nano-formulation of the present invention of example 3.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
FIG. 1 is a process flow diagram of a high-efficiency cyhalothrin soluble solid nano-formulation prepared by the invention.
Example 1
The 10% high-efficiency cyhalothrin soluble solid nano preparation comprises the following steps:
(1) Weighing 5g of high-efficiency cyhalothrin raw material, dispersing in water, heating to 80 ℃ in a water bath kettle, and obtaining a molten phase in a molten state;
(2) 1.0g of polyoxyethylene sorbitan fatty acid ester and 0.5g of castor oil polyoxyethylene ether are weighed and dissolved in deionized water, and are fully stirred to a transparent state to obtain a disperse phase;
(3) Dripping the dispersed phase into the molten phase at 80 ℃, dispersing and emulsifying for a period of time by a high-shear dispersing and emulsifying machine until the emulsion is uniform, wherein the shearing rate is 8000rpm, and the shearing time is 5min;
(4) And taking out the emulsion after emulsification and dispersion, adding 43.5g of sucrose, continuously stirring to obtain uniform emulsion, stirring at 300rpm, and freeze-drying to obtain the 10% high-efficiency cyhalothrin soluble solid nano preparation.
The invention prepares the high-efficiency cyhalothrin soluble solid nano preparation with the concentration of 10 percent, and the nano preparation is mixed with water to form uniform and stable solution, the particle size is about 90nm, and the characterization result of a scanning electron microscope is shown in figure 2.
Example 2
15% High-efficiency cyhalothrin soluble solid nano-preparation comprises the following steps:
(1) 10g of high-efficiency cyhalothrin raw medicine is weighed and dispersed in water, and is placed in a water bath kettle to be heated to 80 ℃, and the whole is in a molten state to obtain a molten phase;
(2) 1.5g of fatty alcohol polyoxyethylene ether and 1.0g of polyethylene glycol are weighed and dissolved in deionized water, and are fully stirred to a transparent state to obtain a disperse phase;
(3) Dripping the dispersed phase into the molten phase at 80 ℃, dispersing and emulsifying for a period of time by a high-shear dispersing and emulsifying machine until the emulsion is uniform, wherein the shearing rate is 10000rpm, and the shearing time is 10min;
(4) And taking out the emulsion after emulsification and dispersion, adding 34.2g of sucrose and 20g of mannitol, continuously stirring to obtain uniform emulsion, stirring at 300rpm, and freeze-drying to obtain the 15% high-efficiency cyhalothrin soluble solid nano preparation.
The invention prepares the high-efficiency cyhalothrin soluble solid nano preparation with the concentration of 15 percent, and the nano preparation is mixed with water to form uniform and stable solution, the particle size is about 150nm, and the characterization result of a scanning electron microscope is shown in figure 3.
Example 3
The 20% high-efficiency cyhalothrin soluble solid nano preparation comprises the following steps:
(1) 10g of high-efficiency cyhalothrin raw medicine is weighed and dispersed in water, and is placed in a water bath kettle to be heated to 80 ℃, and the whole is in a molten state to obtain a molten phase;
(2) 2g of fatty alcohol polyoxyethylene ether, 2g of ethylene oxide/propylene oxide segmented copolymer and 0.5g of sodium dodecyl sulfate are weighed and dissolved in deionized water, and the mixture is fully stirred to a transparent state to obtain a disperse phase;
(3) Dripping the dispersed phase into the molten phase at 80 ℃, dispersing and emulsifying for a period of time by a high-shear dispersing and emulsifying machine until the emulsion is uniform, wherein the shearing rate is 12000rpm, and the shearing time is 10min;
(4) And taking out the emulsion after emulsification and dispersion, adding 35.5g of xylitol, continuously stirring to obtain uniform emulsion, and obtaining the 20% high-efficiency cyhalothrin soluble solid nano-preparation through freeze drying at the stirring speed of 300 rpm.
The invention prepares the high-efficiency cyhalothrin soluble solid nano preparation with the concentration of 20 percent, and the nano preparation is mixed with water to form uniform and stable solution, the particle size is about 240nm, and the characterization result of a scanning electron microscope is shown in figure 4.
Comparative example
The control group of the comparative example is high-efficiency cyhalothrin wettable powder with the concentration content of the commercial drug of 5 percent.
The suspension rate analysis experiment is used for examining the dispersion performance of the active components of the pesticide preparation after being mixed with water for dispersion, and is one of the important means for evaluating the dispersion performance of the pesticide preparation.
Firstly, accurately measuring 5.0mL of pesticide preparation, transferring the pesticide preparation into a 200mL beaker containing 50mL of standard hard water, performing circular motion on the beaker by hand for 2min (120 times/min), placing the beaker in a water bath condition of 30+/-1 ℃ for 13min, transferring the beaker into a 250mL measuring cylinder by using the standard hard water, dripping the measuring cylinder into a scale mark, and then, plugging a plug and reversing the beaker upside down for 30 times (1 min). The plug is opened, and the mixture is kept stand for 30min in a constant temperature water bath kettle with the temperature of 30+/-1 ℃. Finally, the upper 225mL suspension was removed, ensuring that the time was controlled within 10-15s, ensuring that the sediment at the bottom of the cylinder was not stirred, and ensuring that the solution was sucked up a few millimeters below the liquid level. Finally, the initial active ingredient content m 0 of the initial suspension and the active ingredient content m 1 of 225mL of the suspension were measured by a liquid chromatograph, and the suspension ratio (Suspensibility, S) was calculated according to the following formula:
TABLE 1 suspension Rate of pesticide formulations
As shown in Table 1, the suspension rate of the high-efficiency cyhalothrin soluble solid nano preparation with different concentrations is obviously superior to that of a control group, namely, the active ingredients of the medicine can be uniformly suspended and dispersed in the liquid medicine after the preparation is diluted by adding water. After the drug particles are nanocrystallized, the particle size of the particles is obviously reduced, the drug particles are dispersed faster in unit time, and meanwhile, the Brownian motion of the particles becomes more severe along with the reduction of the particle size, so that the dispersion of the particles is quickened. The higher the suspension rate is, the better the dispersion performance of the drug particles is, the particles of the active ingredients can be uniformly suspended in the drug liquid for a long time, the drug liquid ensures the concentration of the drug liquid to be consistent in the spraying use process and is uniformly deposited on a target, and the control effect of the drug liquid on target pests is further improved.
Indoor biological Activity test
According to the standard of the "biological assay in pesticide Chamber" test guidelines (NY/T1154.10-2008). Firstly, the high-efficiency cyhalothrin soluble solid nano-preparation and an experimental control group are diluted into 5 series of concentrations in equal proportion, each concentration is repeated for 4 times, and deionized water with the same volume is used as a control. Aphids are used as target pests and are fed in a constant temperature incubator, and finally, the death number of the aphids in each concentration gradient culture dish is counted, and the semi-lethal concentration (LC 50) and a 95% confidence interval thereof are calculated.
TABLE 2 determination of indoor biological Activity of lambda-cyhalothrin formulations against aphids
As shown in Table 2, the toxicity effect of the high-efficiency cyhalothrin soluble solid nano-preparation with different concentrations is obviously higher than that of the control group, and the high-efficiency cyhalothrin soluble solid nano-preparation has better insecticidal effect. After the efficient cyhalothrin drug particles are subjected to nanocrystallization, the smaller the particle size is, the larger the specific surface area is, the adhesion of the drug particles on leaf surfaces is increased, the contact area with the surfaces of crop pests is further increased, and the active components are easier to act on biological targets. Meanwhile, the dispersion performance and the wetting performance of the high-efficiency cyhalothrin soluble solid nano preparation are obviously enhanced, and the liquid medicine can be uniformly dispersed on the leaf surfaces of crops, so that the effectiveness of the preparation and the control effect on plant diseases and insect pests are improved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The high-efficiency cyhalothrin soluble solid nano preparation is characterized by comprising the following components in percentage by weight:
1-30 high-efficiency cyhalothrin, 0.1-15 wetting agent, 0.1-15 dispersing agent, 0.1-3 preservative and 0.1-37 water.
2. The lambda-cyhalothrin-soluble solid nano-formulation of claim 1, wherein the wetting agent is one or more of a non-ionic surfactant, a sulfonate-type anionic surfactant, a phosphate-type anionic surfactant, a carboxylate-type anionic surfactant, and an oligomeric surfactant.
3. The lambda-cyhalothrin soluble solid nano-formulation of claim 2, wherein the non-ionic surfactant is one or more of alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty amine ethoxylates, alkyl glycosides, polyarylphenol ethoxylates, castor oil ethoxylates, polyoxyethylene fatty acid esters, ethylene oxide/propylene oxide block copolymers, sorbitol ethers and polyglycerin fatty acid esters;
The sulfonate anionic surfactant is selected from one or more of alkylbenzene sulfonate, alpha-alkenyl sodium sulfonate, polyoxyethylene ether sulfate, polycyclic aromatic hydrocarbon formaldehyde condensate sulfonate or alkyl aromatic hydrocarbon sulfonate, sodium alkyl succinic sulfonate, polyoxyethylene ether monosuccinate sulfonate, fatty alcohol sulfate and fatty amide N-methyl taurate sodium salt;
the phosphate anionic surfactant is one or more of polyoxyethylene ether phosphate, alkyl alcohol phosphate and alcohol ether carboxylate.
4. The lambda-cyhalothrin-soluble solid nano-formulation of claim 2, wherein the dispersant is one or more of an anionic dispersant, a nonionic dispersant, an anionic nonionic dispersant, a polymeric dispersant, and a cationic dispersant.
5. The lambda-cyhalothrin soluble solid nano-formulation of claim 4, wherein the anionic dispersant is one or more of naphthalene formaldehyde condensate sulfonate, alkyl naphthalene formaldehyde condensate sulfonate and lignin sulfonate;
And/or the anionic non-ionic dispersant is one or more of phosphate dispersant, sulfate dispersant and succinate sulfonate;
and/or the nonionic dispersant is one or more of fatty alcohol polyoxypropylene polyoxyethylene ether and polyoxyethylene polypropylene ether block copolymers.
6. The efficient cyhalothrin-soluble solid nano-formulation of any one of claims 1-5, wherein the method of preparing the efficient cyhalothrin-soluble solid nano-formulation is:
(1) Dispersing the high-efficiency cyhalothrin in water, heating, and obtaining a molten phase in a molten state;
(2) Dissolving a wetting agent, a dispersing agent and a preservative in water, and stirring to a transparent state to obtain a dispersed phase;
(3) Mixing the disperse phase with the melt phase at high temperature, and emulsifying the mixture by high-shear dispersion until the emulsion is uniform to obtain emulsion;
(4) And adding a water-soluble carrier material into the emulsion, stirring to obtain a uniform emulsion mixture, and drying to obtain the high-efficiency cyhalothrin soluble solid nano preparation.
7. The lambda-cyhalothrin-soluble solid nano-formulation of claim 6, wherein in step (1), the lambda-cyhalothrin is dispersed in water and heated to 80 ℃;
and/or, in the step (3), the high temperature is 80 ℃;
And/or in the step (4), the water-soluble carrier material is one or more of polyethylene glycol, povidone, tartaric acid, succinic acid, chitosan, glucose, galactose, sucrose, lactose, mannitol, sorbitol, xylitol, hydroxypropyl cellulose and hydroxypropyl methylcellulose.
8. The lambda-cyhalothrin-soluble solid nano-formulation according to claim 7, wherein in step (3), the shear rate of the high shear dispersion emulsification is 1000-30000rpm/min; the shearing time of the high shearing dispersion emulsifying machine is 0.05-1h;
and/or, in the step (3), the stirring speed is 100-1000rpm/min;
and/or, in the step (4), the drying is drying or freeze drying.
9. The lambda-cyhalothrin soluble solid nano-formulation of claim 8, wherein the temperature of the drying is 40 ℃ and the time of the drying is 2-8 hours;
The pre-freezing temperature of the freeze drying is-80 ℃, the pre-freezing time is 1-6h, and the freeze drying is 12-72h.
10. A method of preparing the lambda-cyhalothrin-soluble solid nano-formulation as claimed in any one of claims 1-9, comprising:
(1) Dispersing the high-efficiency cyhalothrin in water, heating, and obtaining a molten phase in a molten state;
(2) Dissolving a wetting agent, a dispersing agent and a preservative in water, and stirring to a transparent state to obtain a dispersed phase;
(3) Mixing the disperse phase with the melt phase at high temperature, and emulsifying the mixture by high-shear dispersion until the emulsion is uniform to obtain emulsion;
(4) And adding a water-soluble carrier material into the emulsion, stirring to obtain a uniform emulsion mixture, and drying to obtain the high-efficiency cyhalothrin soluble solid nano preparation.
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