CN114097809A - Suspending agent containing diafenthiuron and etoxazole and preparation method thereof - Google Patents
Suspending agent containing diafenthiuron and etoxazole and preparation method thereof Download PDFInfo
- Publication number
- CN114097809A CN114097809A CN202111517649.7A CN202111517649A CN114097809A CN 114097809 A CN114097809 A CN 114097809A CN 202111517649 A CN202111517649 A CN 202111517649A CN 114097809 A CN114097809 A CN 114097809A
- Authority
- CN
- China
- Prior art keywords
- etoxazole
- agent
- diafenthiuron
- percent
- polyoxyethylene ether
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000005897 Etoxazole Substances 0.000 title claims abstract description 72
- IXSZQYVWNJNRAL-UHFFFAOYSA-N etoxazole Chemical compound CCOC1=CC(C(C)(C)C)=CC=C1C1N=C(C=2C(=CC=CC=2F)F)OC1 IXSZQYVWNJNRAL-UHFFFAOYSA-N 0.000 title claims abstract description 71
- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000375 suspending agent Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002562 thickening agent Substances 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 17
- 239000003755 preservative agent Substances 0.000 claims abstract description 16
- 230000002335 preservative effect Effects 0.000 claims abstract description 16
- 239000000080 wetting agent Substances 0.000 claims abstract description 16
- 239000004480 active ingredient Substances 0.000 claims abstract description 14
- 230000002528 anti-freeze Effects 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 17
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 claims description 11
- TVFWYUWNQVRQRG-UHFFFAOYSA-N 2,3,4-tris(2-phenylethenyl)phenol Chemical compound C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 TVFWYUWNQVRQRG-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims description 9
- 238000010008 shearing Methods 0.000 claims description 9
- 159000000000 sodium salts Chemical class 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 8
- 229920001732 Lignosulfonate Polymers 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- -1 alkyl naphthalene sulfonate formaldehyde Chemical compound 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229920002545 silicone oil Polymers 0.000 claims description 5
- 239000000230 xanthan gum Substances 0.000 claims description 5
- 229920001285 xanthan gum Polymers 0.000 claims description 5
- 229940082509 xanthan gum Drugs 0.000 claims description 5
- 235000010493 xanthan gum Nutrition 0.000 claims description 5
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 239000004546 suspension concentrate Substances 0.000 claims description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical group COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 2
- 239000004299 sodium benzoate Substances 0.000 claims description 2
- 235000010234 sodium benzoate Nutrition 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- PZZYQPZGQPZBDN-UHFFFAOYSA-N aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 claims 1
- 229910000323 aluminium silicate Inorganic materials 0.000 claims 1
- 235000012211 aluminium silicate Nutrition 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910021653 sulphate ion Inorganic materials 0.000 claims 1
- 239000000575 pesticide Substances 0.000 abstract description 16
- 239000000725 suspension Substances 0.000 abstract description 14
- 230000000749 insecticidal effect Effects 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 5
- 230000009471 action Effects 0.000 abstract description 3
- 239000002917 insecticide Substances 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 17
- 239000000203 mixture Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 238000011282 treatment Methods 0.000 description 11
- 241000238876 Acari Species 0.000 description 8
- 241000607479 Yersinia pestis Species 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 6
- 241000219146 Gossypium Species 0.000 description 6
- 241000488583 Panonychus ulmi Species 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 230000001988 toxicity Effects 0.000 description 4
- 231100000419 toxicity Toxicity 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- BOLQUPOXTWHXIX-UHFFFAOYSA-N OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 Chemical compound OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 BOLQUPOXTWHXIX-UHFFFAOYSA-N 0.000 description 3
- 241001454293 Tetranychus urticae Species 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- OARRHUQTFTUEOS-UHFFFAOYSA-N safranin Chemical compound [Cl-].C=12C=C(N)C(C)=CC2=NC2=CC(C)=C(N)C=C2[N+]=1C1=CC=CC=C1 OARRHUQTFTUEOS-UHFFFAOYSA-N 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 206010059866 Drug resistance Diseases 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 241001454295 Tetranychidae Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 150000001718 carbodiimides Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 235000013601 eggs Nutrition 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005338 heat storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- DTQJMAHDNUWGFH-UHFFFAOYSA-N 2,4-diphenyl-4,5-dihydro-1,3-oxazole Chemical class C1OC(C=2C=CC=CC=2)=NC1C1=CC=CC=C1 DTQJMAHDNUWGFH-UHFFFAOYSA-N 0.000 description 1
- 240000002234 Allium sativum Species 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 241001414720 Cicadellidae Species 0.000 description 1
- 239000005898 Fenoxycarb Substances 0.000 description 1
- 241000258937 Hemiptera Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 244000141359 Malus pumila Species 0.000 description 1
- 241000256259 Noctuidae Species 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 241000344246 Tetranychus cinnabarinus Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 235000021016 apples Nutrition 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000003958 fumigation Methods 0.000 description 1
- 235000004611 garlic Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 231100000518 lethal Toxicity 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003151 ovacidal effect Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000002723 toxicity assay Methods 0.000 description 1
- 231100000820 toxicity test Toxicity 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 230000001018 virulence Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/30—Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
Abstract
The invention provides a suspending agent containing diafenthiuron and etoxazole, which comprises the following components in percentage by mass: 20 to 60 percent of active component; 2 to 10 percent of dispersant; 1 to 6 percent of wetting agent; 0.05 to 1 percent of thickening agent; 0.1 to 1 percent of defoaming agent; 0.01-0.2% of preservative; 2 to 8 percent of antifreeze; the balance of water; the active ingredients comprise diafenthiuron and etoxazole; the mass ratio of the diafenthiuron to the etoxazole is (1-40): 1. the active ingredients of the pesticide disclosed by the invention, namely the diafenthiuron and the etoxazole, belong to two insecticides with different action mechanisms, and the diafenthiuron and the etoxazole are mixed with each other without conflict, so that the insecticidal spectrum is expanded, and the insecticidal efficiency is improved. The stability of the product is improved through the compatibility of the auxiliary agents, and the product can tolerate the temperature range from-15 ℃ to 65 ℃. The suspending agent prepared by the invention has the advantages of excellent performance, low foamability, high suspension rate, little residue after pouring and good cold/hot storage stability.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a suspending agent containing diafenthiuron and etoxazole and a preparation method thereof.
Background
Diafenthiuron belongs to a novel thiourea high-efficiency insecticide and acaricide, has the effects of contact poisoning, stomach poisoning, systemic absorption and fumigation, and has a certain ovicidal effect. Under the irradiation of ultraviolet rays, the multifunctional oxidase in the insect body decomposes into carbodiimide, influences the respiration and energy conversion of the carbodiimide, and causes the pests to suffocate. Can be used for preventing and treating aphid, whitefly, leafhopper, noctuidae pests and mites on various crops and ornamental plants.
Etoxazole belongs to a diphenyl oxazoline derivative, inhibits the embryo formation of mite eggs and the molting process from young mites to adult mites, is effective to eggs and young mites, is ineffective to adult mites, and has a good sterile effect on female adult mites. Mainly used for preventing and treating red spiders of apples and oranges, and also has prevention effect on mites such as tetranychid mites, panonychus ulmi koch, tetranychus urticae koch, tetranychus cinnabarinus and the like of crops such as cotton, flowers, vegetables and the like.
Pesticide varieties containing a single active ingredient often have different degrees of defects in agricultural pest control, such as: the insecticidal spectrum is narrow, resistance is easy to generate after continuous use, and environmental pollution is aggravated by more use times. The above disadvantages can be effectively overcome by compounding active ingredients with different mechanisms of action. Meanwhile, the synergistic effect generated by mixing the two active components can improve the control effect, expand the insecticidal spectrum, delay the generation of the drug resistance of pests and reduce the environmental pollution, thereby being an important means for comprehensively controlling the pests.
At present, the combined use of diafenthiuron and etoxazole has been reported to kill pests, for example, patent CN 102210321A. The composition of diafenthiuron and etoxazole has been proved to have the effects of synergy, expansion of insecticidal spectrum and delay of pest drug resistance. However, the products in the current market are easily influenced by environmental changes in the marine transportation process, are easy to have the phenomena of caking, creaming, large particle size, water precipitation and the like at high temperature, have the crystallization risk at low temperature and seriously influence the drug effect. In the using process, the suspension rate under 3WHO water is lower than 90 percent, which is not beneficial to the use and popularization of the product.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a suspension containing diafenthiuron and etoxazole, wherein the stability of the product is improved by selecting an auxiliary agent.
A suspending agent containing diafenthiuron and etoxazole comprises the following components in percentage by mass:
20 to 60 percent of active component;
2 to 10 percent of dispersant;
1 to 6 percent of wetting agent;
0.05 to 1 percent of thickening agent;
0.1 to 1 percent of defoaming agent;
0.01-0.2% of preservative;
2 to 8 percent of antifreeze;
the balance of water;
the active ingredients comprise diafenthiuron and etoxazole; the mass ratio of the diafenthiuron to the etoxazole is (1-40): 1.
the pure etoxazole is white crystal powder, the melting point is 101-102 ℃, and the relative density is 1.24(20 ℃). The partition coefficient log P is 5.59(25 ℃). Solubility in water at 20 ℃ was 75.4. mu.g/L, and solubility in other solutions (g/L, 20 ℃): methanol 90, ethanol 90, acetone 300, cyclohexanone 500, ethyl acetate 250, xylene 250, n-heptane 13, acetonitrile 80, tetrahydrofuran 750, stable under alkaline conditions, slightly unstable to light, and unstable to acids.
Diafenthiuron is a white crystal, melting point: 149.6 ℃. Solubility at 20 ℃: 600g/L of dichloromethane, 380g/L of cyclohexanone, 320g/L of toluene, 280g/L of acetone, 210g/L of xylene, 8g/L of hexane and 0.05mg/L of water, wherein the distribution coefficient log P is 5.76.
Wherein, diafenthiuron and etoxazole are both strong and highly lipophilic, and etoxazole is unstable to acid, and the two are difficult to be prepared into stable-quality aqueous suspension agents by mixing. The inventor creatively obtains a system with the best matching degree among the components, greatly reduces the processing difficulty of the preparation formulation, improves the stability of the preparation formulation, has the advantages of high suspension rate, tolerance to different water qualities and small foamability, and effectively solves the problems of influence of environmental change on the product quality in the transportation process and the like.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 20-60% of active ingredients in percentage by mass; preferably 30 to 50 percent; more preferably from 30% to 45%.
The active ingredients comprise diafenthiuron and etoxazole; the mass ratio of the diafenthiuron to the etoxazole is (1-40): 1; preferably (1-30): 1; more preferably (1-25): 1; most preferably, the pesticide comprises 38.5% of diafenthiuron and 1.93% of etoxazole.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 2-10% of dispersant by mass percentage; preferably 3% -8%; more preferably 3 to 6 percent; most preferably 4%.
The dispersant is preferably one or more of triphenylethylene phenol polyoxyethylene ether phosphate triethanolamine, styrene maleic anhydride copolymer sodium salt, acrylic acid-maleic anhydride copolymer, triphenylethylene phenol polyoxyethylene ether sulfate ammonium salt, alkyl naphthalene sulfonate formaldehyde condensate and lignosulfonate;
more preferably, the dispersant is one of a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and an acrylic acid-maleic anhydride copolymer, a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and a styrene maleic anhydride copolymer sodium salt, a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and an alkylnaphthalene sulfonate formaldehyde condensate, a combination of a styrene maleic anhydride copolymer sodium salt and tristyrylphenol polyoxyethylene ether phosphate triethanolamine, a combination of a styrene maleic anhydride copolymer sodium salt and a lignin sulfonate, or a combination of an alkylnaphthalene sulfonate formaldehyde condensate and a lignin sulfonate. Most preferably, the dispersing agent is prepared by mixing styrene maleic anhydride copolymer sodium salt and triphenylethylene phenol polyoxyethylene ether phosphate triethanolamine according to the weight ratio of 1: 1-3; specifically, the ratio of 1:1, 2: 3. 1: 3.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 1-6% of wetting agent by mass percentage; preferably 2% -4%; specifically, the content can be 2%, 3% or 4%; or a point between any of the foregoing, most preferably 2%.
The wetting agent is preferably one or more of fatty alcohol polyoxyethylene polyoxypropylene ether, methyl cocoalcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether sulfate and ethylene oxide-propylene oxide block polyether, and most preferably ethylene oxide-propylene oxide block polyether.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 0.05-1% of thickening agent by mass percent; more preferably 0.1 to 0.5 percent of thickening agent; most preferably 0.1 to 0.3 percent of thickening agent; particularly preferably 0.1%.
The thickening agent is preferably one or more of polyvinyl alcohol, magnesium aluminum silicate or xanthan gum; more preferably, the thickener is one or more of magnesium aluminum silicate or xanthan gum; most preferably, the thickener is xanthan gum.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 0.1-1% of defoaming agent by mass percentage; preferably comprises 0.2 to 0.8 percent of defoaming agent; most preferably 0.2% defoamer is included.
The defoaming agent is preferably silicone oil or C10-20Saturated fatty acids or C8-10One or more of fatty alcohol compounds; more preferably silicone oil or C10-20One or more of saturated fatty acid compounds; most preferred is silicone oil.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 0.01-0.2% of preservative by mass percent; preferably 0.1 to 0.2 percent; most preferably 0.1%.
The preservative is preferably any one of paraformaldehyde, cason or sodium benzoate; more preferably, cason or paraformaldehyde; most preferably, cason.
The suspending agent containing diafenthiuron and etoxazole provided by the invention comprises 2-8% of an antifreezing agent by mass percent; preferably 3% -8%; more preferably from 5% to 8%; most preferably 5%.
The antifreezing agent is preferably one or more of ethylene glycol, propylene glycol or glycerol; more preferably ethylene glycol or glycerol; most preferably ethylene glycol.
In a part of preferred embodiments of the present invention, the suspension concentrate containing diafenthiuron and etoxazole comprises, by mass:
30-50% of active ingredients of the medicine, 3-6% of dispersing agent, 2-4% of wetting agent, 0.1-0.5% of thickening agent, 0.2-0.8% of defoaming agent, 0.1-0.2% of preservative, 5-8% of antifreezing agent and the balance of water.
In a part of preferred embodiments of the present invention, the suspension containing diafenthiuron and etoxazole comprises, by mass:
30-50% of active ingredients of the medicine, 3-6% of dispersing agent, 2-4% of wetting agent, 0.1% of thickening agent, 0.2% of defoaming agent, 0.1% of preservative, 5% of antifreezing agent and the balance of water.
In a part of preferred embodiments of the present invention, the suspension containing diafenthiuron and etoxazole comprises, by mass:
38.5% of diafenthiuron, 1.93% of etoxazole, 4% of dispersant, 2% of wetting agent, 0.1% of thickening agent, 0.2% of defoaming agent, 0.1% of preservative, 5% of antifreezing agent and the balance of water.
The inventor improves the stability of the product by screening a large amount of auxiliary agents, can tolerate the high and low temperature range of-15 ℃ to 65 ℃, effectively solves the influence of environmental change on the product quality in the transportation process, and avoids the product quality problems of creaming, caking, water precipitation and the like. Meanwhile, the invention can resist different water qualities such as C water, D water, 3WHO water and the like, has small foamability, meets the use requirements of different countries and regions, and is beneficial to large-scale popularization and application.
The invention provides a preparation method of the suspending agent containing diafenthiuron and etoxazole, which comprises the following steps:
the suspending agent containing the diafenthiuron and the etoxazole is obtained by shearing and mixing the wetting agent, the dispersing agent, the defoaming agent, the preservative and water at a high speed, adding the diafenthiuron and the etoxazole, grinding, adding the antifreezing agent and the thickening agent and shearing.
The components and the proportion of the components are clearly described in the invention, and the description is omitted.
Firstly, shearing and mixing a wetting agent, a dispersing agent, a defoaming agent, a preservative and water at a high speed; preferably, the mixture is uniformly mixed in a reaction kettle.
Adding the active ingredients diafenthiuron and etoxazole into the mixture, sanding by using a sand mill, and detecting by using a laser particle size distribution instrument until the particle size of the product is below 3 mu m after grinding;
adding an antifreezing agent and a thickening agent, and shearing to obtain the suspending agent containing diafenthiuron and etoxazole.
Preferably, the thickening agent is added into the antifreezing agent and uniformly mixed, then the thickening agent and the antifreezing agent are added into the liquid mixture after the sanding in the above steps, and the high-speed shearing and uniform mixing are carried out to obtain the suspending agent containing the diafenthiuron and the etoxazole.
Compared with the prior art, the invention provides a suspending agent containing diafenthiuron and etoxazole, which comprises the following components in percentage by mass: 20 to 60 percent of active component; 2 to 10 percent of dispersant; 1 to 6 percent of wetting agent; 0.05 to 1 percent of thickening agent; 0.1 to 1 percent of defoaming agent; 0.01-0.2% of preservative; 2 to 8 percent of antifreeze; the balance of water; the active ingredients comprise diafenthiuron and etoxazole; the mass ratio of the diafenthiuron to the etoxazole is (1-40): 1. the active ingredients of the pesticide disclosed by the invention, namely the diafenthiuron and the etoxazole, belong to two insecticides with different action mechanisms, and the diafenthiuron and the etoxazole are mixed with each other without conflict, so that the insecticidal spectrum is expanded, and the insecticidal efficiency is improved. The product stability is improved through the compatibility of the auxiliary agents, the high-temperature and low-temperature range of-15 ℃ to 65 ℃ can be tolerated, and the influence of environmental change on the product quality in the transportation process is effectively solved. The invention prepares the diafenthiuron and the etoxazole into the suspending agent, and the obtained suspending agent has excellent performance, low foamability, high suspension rate, little residue after pouring, good cold/hot storage stability and different water qualities.
Detailed Description
In order to further illustrate the present invention, the suspension containing diafenthiuron and etoxazole and the preparation method thereof provided by the present invention are described in detail below with reference to examples.
Examples 1 to 8
The suspending agents were prepared according to the formulation of table 1, the preparation method being as follows:
shearing water, a dispersing agent, a wetting agent, a defoaming agent and a preservative at a high speed, and uniformly mixing; adding the active pharmaceutical ingredients diafenthiuron and etoxazole into the mixture, sanding by using a sand mill, and detecting by using a laser particle size distribution instrument until the particle size of the product is below 3 mu m after grinding; and adding the thickening agent into the antifreezing agent, uniformly mixing, adding the thickening agent into the liquid mixture after sanding, and performing high-speed shearing and uniform mixing to obtain the suspending agent containing the diafenthiuron and the etoxazole.
Comparative example 1
The suspending agents were prepared according to the ratios in table 1, the preparation method being as above:
TABLE 1 summary of the raw materials and their amounts for the inventive and comparative examples
The performance of the aqueous suspensions prepared in the above examples and comparative examples was measured, and the results are shown in Table 2 below. Wherein, the suspension percentage is detected according to a GB/T14825-2006 pesticide suspension percentage measuring method, the pourability is detected according to a GB/T31737-2015 pesticide pourability measuring method, the spontaneous dispersibility in water is detected according to a CIPAC MT160 method, and the foamability is detected according to a GB/T28137-2011 persistent foamability method.
As can be seen from Table 2, the comparative examples had poor quality before and after thermal storage, the samples did not tolerate high and low temperatures ranging from-15 ℃ to 65 ℃, the samples were stored at-15 ℃ for 2 days, the samples had no fluidity after being stored at room temperature, the samples were stored at 65 ℃ for 3 days, and the samples had crystallization and poor fluidity after being stored at room temperature. Examples 1, 3, 7, 8, slightly deteriorated in quality after heat storage, while examples 2, 4, 5, 6, both good in quality before and after heat storage, with the preferred range of adjuvants and proportions playing a critical role in product quality.
TABLE 2 Properties of suspensions made by compounding diafenthiuron and etoxazole
Field test
The test arrangement test is arranged in east China village of Wu town in Wu county of Wu county, Shandong province, seedling culture in middle ten days of 4 months, transplanting in middle ten days of 5 months, planting distance 35cm, row distance 90cm, and planting 2118 plants per mu; the first crop is garlic. Spider mites occur more heavily throughout the year, generally on the 2-4 scale, and moderate to moderate. And other cultivation management conditions of the test field are consistent. The amount of the pesticide is 450kg/ha, and a manual sprayer is adopted for uniformly spraying, so that the front and back sides of cotton leaves in each cell are required to be uniformly sprayed with the pesticide. A blank control is additionally arranged, five points of diagonal lines in a test cell are sampled, 2 plants are fixed at each point, 3 leaves are fixed at the upper part, the middle part and the lower part of each plant, and the number of live red spiders on 30 leaves of 10 plants is investigated.
The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: diafenthiuron etoxazole suspensions obtained in examples 3, 4, 9 and comparative example 1; and (3) treatment: 50% diafenthiuron suspension; and (4) treatment: 20% etoxazole suspension.
Among them, diafenthiuron etoxazole obtained in examples 3, 4 and 7 and comparative example was subjected to stem and leaf spray treatment at an effective ingredient usage of 60 g/hectare, treatment 3 was subjected to stem and leaf spray treatment at an effective ingredient usage of 120 g/hectare, and treatment 4 was subjected to stem and leaf spray treatment at an effective ingredient usage of 30 g/hectare.
The drug effect calculation method comprises the following steps:
the control results of cotton spider mites are shown in the following table:
test results of field pesticide effect of surface treatment medicament for preventing and treating cotton red spider
The test results in the table show that the compound of diafenthiuron and etoxazole can effectively prevent and treat cotton red spiders, the control effect on the cotton red spiders 2 days, 7 days and 14 days after the pesticide application is obviously better than that of 2 control pesticides, and the synergistic effect is shown. As can be seen from the comparison of the drug effects of the examples and the comparative examples, the selection of the auxiliary agent has important influence on the exertion of the effective components, and improper selection of the auxiliary agent can influence the compounding effect of the diafenthiuron and the etoxazole. According to the observation of the whole field test process, the cotton grows well within the test dose range, and the pesticide damage phenomenon does not occur in each treatment agent, which indicates that the cotton is safe to the cotton.
Indoor toxicity assay
The embodiment of the invention adopts an indoor toxicity determination method. Indoor toxicity measurement is carried out according to the Sun Yunpei method, the cotoxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion is determined, the CTC is less than 80 and is antagonistic, the CTC is more than or equal to 80 and is less than or equal to 120 and is additive, and the CTC is more than 120 and is synergistic.
The test agents were provided by Shandong Weifang Runfeng Feng chemical company Limited.
And (3) experimental design: after the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated with a series of concentrations according to the content of effective components, and clear water is used for comparison. The method is carried out according to the standard pesticide for indoor bioassay of pesticides, the lethal medium concentration of the pesticide and the mixed pesticide is measured by adopting a glass sheet immersion method, and the cotoxicity coefficient is obtained by a method for calculating the combined toxicity provided by Sun Yunpei et al (1960).
The calculation formula is as follows (using diafenthiuron as a standard medicament and the toxicity index is 100)
Theoretical virulence index (TTI) of M-diafenthiuron TI XPDiafenthiuron+ etoxazole TI is multiplied by PEtoxazole
In the formula: m is a mixture of diafenthiuron and etoxazole in different proportions;
PdiafenthiuronIs the proportion of diafenthiuron in the compound composition;
PfenoxycarbIs the proportion of etoxazole in the compound composition.
The test results are shown in table 1:
TABLE 1 toxicity test results of diafenthiuron and etoxazole in different ratios to Tetranychus urticae
As can be seen from Table 1, LC of diafenthiuron and etoxazole against Tetranychus urticae Koch5088.61mg/L and 39.56mg/L, respectively. The mass ratio of the diafenthiuron to the etoxazole is 1:1, 10:1, 20:1, 30:1, 40:1,The co-toxicity coefficient of 50:1 is 134.96, 135.71, 148.80, 136.41, 136.80 and 128.94 which are all larger than 120, and the synergistic effect is shown.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A suspending agent containing diafenthiuron and etoxazole comprises the following components in percentage by mass:
20 to 60 percent of active component;
2 to 10 percent of dispersant;
1 to 6 percent of wetting agent;
0.05 to 1 percent of thickening agent;
0.1 to 1 percent of defoaming agent;
0.01-0.2% of preservative;
2 to 8 percent of antifreeze;
the balance of water;
the active ingredients comprise diafenthiuron and etoxazole; the mass ratio of the diafenthiuron to the etoxazole is (1-40): 1.
2. the suspending agent containing diafenthiuron and etoxazole according to claim 1, which is characterized by comprising the following components in percentage by mass:
30-50% of active ingredients of the medicine, 3-6% of dispersing agent, 2-4% of wetting agent, 0.1-0.5% of thickening agent, 0.2-0.8% of defoaming agent, 0.1-0.2% of preservative, 5-8% of antifreezing agent and the balance of water.
3. The suspension concentrate containing diafenthiuron and etoxazole as claimed in claim 1, wherein the dispersant is one or more of tristyrylphenol polyoxyethylene ether phosphate triethanolamine, styrene maleic anhydride copolymer sodium salt, acrylic acid-maleic anhydride copolymer, tristyrylphenol polyoxyethylene ether sulfate ammonium salt, alkyl naphthalene sulfonate formaldehyde condensate and lignosulfonate.
4. The suspending agent containing diafenthiuron and etoxazole as claimed in claim 3, wherein the dispersing agent is one of a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and an acrylic acid-maleic anhydride copolymer, a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and a styrene maleic anhydride copolymer sodium salt, a combination of tristyrylphenol polyoxyethylene ether phosphate triethanolamine and an alkylnaphthalenesulfonate formaldehyde condensate, a combination of styrene maleic anhydride copolymer sodium salt and tristyrylphenol polyoxyethylene ether phosphate triethanolamine, a combination of styrene maleic anhydride copolymer sodium salt and a lignosulfonate, or a combination of an alkylnaphthalenesulfonate formaldehyde condensate and a lignosulfonate.
5. The suspension concentrate containing diafenthiuron and etoxazole as claimed in claim 1, wherein the wetting agent is one or more of fatty alcohol polyoxyethylene polyoxypropylene ether, methyl cocoalcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether sulphate and ethylene oxide-propylene oxide block polyether.
6. The suspending agent containing diafenthiuron and etoxazole as claimed in claim 1, wherein the thickening agent is one or more of polyvinyl alcohol, magnesium aluminium silicate or xanthan gum;
the defoaming agent is silicone oil or C10-20Saturated fatty acids or C8-10One or more of fatty alcohol compounds;
the antifreezing agent is one or more of ethylene glycol, propylene glycol or glycerol;
the preservative is one or more of paraformaldehyde, cason or sodium benzoate.
7. The suspending agent containing diafenthiuron and etoxazole as claimed in claim 1, wherein the wetting agent is an ethylene oxide-propylene oxide block polyether;
the thickening agent is xanthan gum;
the antifreezing agent is ethylene glycol;
the defoaming agent is silicone oil;
the preservative is cason.
8. The preparation method of the suspending agent containing diafenthiuron and etoxazole as claimed in any one of claims 1 to 7, which comprises the following steps:
the suspending agent containing the diafenthiuron and the etoxazole is obtained by shearing and mixing the wetting agent, the dispersing agent, the defoaming agent, the preservative and water at a high speed, adding the diafenthiuron and the etoxazole, grinding, adding the antifreezing agent and the thickening agent and shearing.
9. The production method according to claim 8, wherein the grinding is carried out until a particle diameter is 3 μm or less.
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| CN115363040A (en) * | 2022-08-31 | 2022-11-22 | 山东润博生物科技有限公司 | Suspending agent containing topramezone and amicarbazone and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102210321A (en) * | 2011-05-04 | 2011-10-12 | 陕西韦尔奇作物保护有限公司 | Pesticide composite containing etoxazole |
| CN104351228A (en) * | 2014-12-08 | 2015-02-18 | 佛山市盈辉作物科学有限公司 | Diafenthiuron and etoxazole mixed suspending agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102210321A (en) * | 2011-05-04 | 2011-10-12 | 陕西韦尔奇作物保护有限公司 | Pesticide composite containing etoxazole |
| CN104351228A (en) * | 2014-12-08 | 2015-02-18 | 佛山市盈辉作物科学有限公司 | Diafenthiuron and etoxazole mixed suspending agent |
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| CN115363040A (en) * | 2022-08-31 | 2022-11-22 | 山东润博生物科技有限公司 | Suspending agent containing topramezone and amicarbazone and preparation method thereof |
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