CN115119837B - Flonicamid-spirotetramat mixed preparation and application thereof - Google Patents
Flonicamid-spirotetramat mixed preparation and application thereof Download PDFInfo
- Publication number
- CN115119837B CN115119837B CN202210893969.0A CN202210893969A CN115119837B CN 115119837 B CN115119837 B CN 115119837B CN 202210893969 A CN202210893969 A CN 202210893969A CN 115119837 B CN115119837 B CN 115119837B
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- CN
- China
- Prior art keywords
- acid
- spirotetramat
- flonicamid
- weight
- formulation
- Prior art date
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- 239000005931 Spirotetramat Substances 0.000 title claims abstract description 137
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- CLSVJBIHYWPGQY-GGYDESQDSA-N spirotetramat Chemical compound CCOC(=O)OC1=C(C=2C(=CC=C(C)C=2)C)C(=O)N[C@@]11CC[C@H](OC)CC1 CLSVJBIHYWPGQY-GGYDESQDSA-N 0.000 claims abstract description 104
- 239000005900 Flonicamid Substances 0.000 claims abstract description 83
- RLQJEEJISHYWON-UHFFFAOYSA-N flonicamid Chemical compound FC(F)(F)C1=CC=NC=C1C(=O)NCC#N RLQJEEJISHYWON-UHFFFAOYSA-N 0.000 claims abstract description 83
- 239000000375 suspending agent Substances 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000009472 formulation Methods 0.000 claims abstract description 37
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 239000002253 acid Substances 0.000 claims abstract description 31
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 44
- -1 methacrylic acid-methacrylate-polyethylene Chemical group 0.000 claims description 32
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 24
- 229920000570 polyether Polymers 0.000 claims description 24
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 18
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 16
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 16
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 claims description 16
- 239000000230 xanthan gum Substances 0.000 claims description 16
- 229920001285 xanthan gum Polymers 0.000 claims description 16
- 229940082509 xanthan gum Drugs 0.000 claims description 16
- 235000010493 xanthan gum Nutrition 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 229920001897 terpolymer Polymers 0.000 claims description 14
- 239000013530 defoamer Substances 0.000 claims description 10
- 241000607479 Yersinia pestis Species 0.000 claims description 9
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 229960004838 phosphoric acid Drugs 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical group O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 229940083037 simethicone Drugs 0.000 claims description 6
- 229960004106 citric acid Drugs 0.000 claims description 5
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- XOAAWQZATWQOTB-UHFFFAOYSA-N taurine Chemical compound NCCS(O)(=O)=O XOAAWQZATWQOTB-UHFFFAOYSA-N 0.000 claims description 4
- 239000003086 colorant Substances 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000005711 Benzoic acid Substances 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
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 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
- 229960000583 acetic acid Drugs 0.000 claims description 2
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- 239000000987 azo dye Substances 0.000 claims description 2
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- 235000010233 benzoic acid Nutrition 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
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 2
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- 239000000975 dye Substances 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 claims description 2
- 229960004949 glycyrrhizic acid Drugs 0.000 claims description 2
- 239000001685 glycyrrhizic acid Substances 0.000 claims description 2
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 claims description 2
- 235000019410 glycyrrhizin Nutrition 0.000 claims description 2
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 claims description 2
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- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical compound CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- HUSXNIFVQFHSEA-UHFFFAOYSA-N 2-hydroxypropanoic acid;hydrochloride Chemical compound Cl.CC(O)C(O)=O HUSXNIFVQFHSEA-UHFFFAOYSA-N 0.000 description 1
- IMOYOUMVYICGCA-UHFFFAOYSA-N 2-tert-butyl-4-hydroxyanisole Chemical compound COC1=CC=C(O)C=C1C(C)(C)C IMOYOUMVYICGCA-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 241001124076 Aphididae Species 0.000 description 1
- 241001465977 Coccoidea Species 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 241001466030 Psylloidea Species 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 241001414989 Thysanoptera Species 0.000 description 1
- 229930003537 Vitamin B3 Natural products 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 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
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- DFPAKSUCGFBDDF-UHFFFAOYSA-N nicotinic acid amide Natural products NC(=O)C1=CC=CN=C1 DFPAKSUCGFBDDF-UHFFFAOYSA-N 0.000 description 1
- YTXCAJNHPVBVDJ-UHFFFAOYSA-N octadecyl propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CC YTXCAJNHPVBVDJ-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- IBBMAWULFFBRKK-UHFFFAOYSA-N picolinamide Chemical compound NC(=O)C1=CC=CC=N1 IBBMAWULFFBRKK-UHFFFAOYSA-N 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 235000019160 vitamin B3 Nutrition 0.000 description 1
- 239000011708 vitamin B3 Substances 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 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
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
-
- 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
-
- 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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
-
- 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
- A01N47/02—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 no bond to a nitrogen atom
- A01N47/06—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 no bond to a nitrogen atom containing —O—CO—O— groups; Thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
-
- 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
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Insects & Arthropods (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a flonicamid-spirotetramat mixed preparation and application thereof, which belong to the filed of pesticides, and comprise the following raw materials in parts by weight: 1-50% of flonicamid, 1-50% of spirotetramat, a stabilizer and formulation auxiliary materials; the preparation is an aqueous suspension agent; the stabilizer comprises acid and carboxylic acid dispersing agent, wherein the acid accounts for 0.1-20% of the total mass of the preparation, and the carboxylic acid dispersing agent accounts for 0.1-20% of the total mass of the preparation. According to the flonicamid-spirotetramat mixed water suspending agent, the stabilizer (acid and carboxylic acid dispersing agent are matched) is introduced, so that the reduction of the spirotetramat content of the suspending liquid after storage can be effectively inhibited.
Description
The invention relates to a Chinese application division application with the application name of 'flonicamid and spirotetramat mixed preparation and application', wherein the application date is 2021, 08 and 10, and the application number is 202110912586.9.
Technical Field
The invention relates to the field of pesticides, in particular to a flonicamid-spirotetramat mixed preparation and application thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
The novel low-toxicity pyridine amide insect growth regulator pesticide developed by Nippon rock original industries, inc. has unique action mechanism, extremely high biological activity, is particularly effective on piercing-sucking mouthpart pests, has high safety and is effective on other pests with resistance to pesticides. Molecular formula C9H6F3N3O; molecular weight: 229, melting point: 157.5 ℃, vapor pressure: 2.55X10-6 Pa, solubility in water: 5.2g/L.
The spirotetramat has unique action characteristics and is one of modern pesticides with double inward suction conductivity. It can be used for preventing and treating various piercing-sucking mouthparts pests such as aphid, thrips, psyllid, mealybugs, whiteflies, scale insects, etc.
The pesticide water suspending agent (Suspension Concentrate, SC) refers to a multiphase dispersion system formed by dispersing solid raw pesticide insoluble in water with a particle size of about 0-5 microns after being processed by a certain mechanical means (sand milling or ball milling). The aqueous suspension concentrate is suitable for being processed into an original drug of an aqueous suspension concentrate, generally requires stable content in water, water solubility of less than 100mg/L and melting point of more than 60 ℃.
The dispersible oil suspending agent (oil-based suspension concentrate, OD) is a high-efficiency and environment-friendly green preparation which is pushed out by the United nations grain and agriculture organization (FAO) in recent years, and is a liquid preparation which takes environment-friendly oil as a medium and stably suspends active ingredients in the oil; common carriers of the dispersible oil suspending agent are methyl oleate, soybean oil methyl ester, 150# solvent oil and 200# solvent oil, and common emulsifying agents are calcium dodecyl benzene sulfonate, fatty alcohol polyoxyethylene ether and the like. The pesticidal active ingredients suitable for processing into dispersible oil suspensions generally have at least two characteristics: firstly, the melting point of the raw medicine is high (preferably more than 60 ℃), and secondly, the raw medicine is basically insoluble in an oil medium; otherwise, the production and processing difficulties are very high; the processing technology is grinding, namely grinding materials into particles with certain fineness by a grinding medium in a sand mill, and uniformly dispersing the particles in an oil medium by the dispersion action of a surfactant.
The soluble agent is a clear uniform liquid formed by mixing and dissolving pesticide, solvent and emulsifier, and can be infinitely mixed with water when in use.
The storage stability of the effective components of the pesticide (14 days for 54 DEG, 7 days for 0 DEG and 2 years for normal temperature storage) is a necessary condition for registering, selling and using pesticide products, and the unstable products after storage, especially pesticide products with the content decomposition rate of more than 5% after storage, cannot pass the registration permission of the pesticide inspection department in the rural area and cannot be circulated and sold on the market.
The flonicamid and spirotetramat developed and mixed water suspending agent (SC) can reduce the content of spirotetramat by 8-30% after long-time heat storage, besides the problems of particle growth and precipitation crystallization (see figure 1 and figure 2). The flonicamid and the spirotetramat are developed and mixed into a Solution (SL) and a dispersible oil suspension (OD), and the problem that the content of the spirotetramat is obviously reduced after storage is also caused.
Disclosure of Invention
Object of the Invention
The invention aims to provide a flonicamid-spirotetramat mixed preparation and application thereof, and solves the problem of reduced spirotetramat content after long-time storage.
Solution scheme
In order to achieve the aim of the invention, the embodiment of the invention provides a flonicamid-spirotetramat mixed preparation, which comprises the following raw materials in parts by weight:
1-50% of flonicamid, 1-50% of spirotetramat, a stabilizer and formulation auxiliary materials;
the preparation is an aqueous suspending agent, a soluble agent or a dispersible oil suspending agent; wherein:
when the preparation is an aqueous suspension agent, the stabilizer comprises acid and carboxylic acid dispersing agents, wherein the acid accounts for 0.1-20% of the total mass of the preparation, and the carboxylic acid dispersing agents account for 0.1-20% of the total mass of the preparation;
when the preparation is a soluble agent, the stabilizer is one or more selected from rosin, tea polyphenol, octadecyl propionate, epoxidized soybean oil, 2, 6-di-tert-butyl-p-cresol, epichlorohydrin, tert-butyl-4-hydroxyanisole, isoamyl alcohol, benzyl alcohol, phenethyl alcohol and phenoxyethanol; the stabilizer accounts for 1 to 20 percent of the total weight of the preparation;
when the preparation is a dispersible oil suspending agent, the stabilizer is one or more selected from diisooctyl succinate sodium sulfonate, 2, 6-di-tert-butyl-p-cresol, epoxidized soybean oil, triglyceryl oleate, triglyceryl linoleate, vitamin E, vitamin B3, benzyl alcohol, phenoxyethanol and hexadecanol; the stabilizer accounts for 3-60% of the total weight of the preparation.
Alternatively, when the formulation is a soluble or dispersible oil suspension, the stabilizer is benzyl alcohol and/or phenoxyethanol.
Further, when the formulation is an aqueous suspension, the aqueous suspension comprises the following ingredients in weight fraction: 1-40% of flonicamid, 1-40% of spirotetramat, 0.3-5% of acid and 1-15% of carboxylic acid dispersing agent;
optionally, the aqueous suspension comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 0.5-2% of acid and 3-8% of carboxylic acid dispersing agent.
Further, the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 0.5-2% of acid and 5% of carboxylic acid dispersing agent.
Further, the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 4-6% of carboxylic acid dispersing agent.
Further, the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of organic acid and 5% of carboxylic acid dispersing agent.
Further, the acid is one or more of dodecylbenzene sulfonic acid, dilute hydrochloric acid, dilute sulfuric acid, phosphoric acid, lactic acid, taurine, succinic acid, glycyrrhizic acid, methylsulfonic acid, chloroacetic acid, glacial acetic acid, benzoic acid, salicylic acid, citric acid, malic acid, tartaric acid and ascorbic acid;
optionally, the acid is selected from one or more of dilute hydrochloric acid, phosphoric acid, lactic acid, methanesulfonic acid and citric acid.
Optionally, the carboxylic acid dispersant is methacrylic acid-methacrylate-polyethylene glycol terpolymer and ATLOX TM 4913 One or more of (CRODA), agrilan 755 (Nouryon), tersperse 2500 (Indoroma), and EMULSON AG/TRN 14105; optionally, the carboxylic acid dispersant is methacrylic acid-methacrylate-polyethylene glycol terpolymer.
Further, the water suspending agent comprises the following raw materials in parts by weight: 15-20% of flonicamid, 10-20% of spirotetramat, 1-2% of acid and 5% of carboxylic acid dispersing agent, wherein the acid is selected from one of phosphoric acid, dilute lactic acid hydrochloride and methylsulfonic acid, and the carboxylic acid dispersing agent is methacrylic acid-methacrylate-polyethylene glycol terpolymer.
Further, the preparation also contains the following auxiliary materials in parts by weight: 0.1 to 1 percent of xanthan gum, 0.5 to 2 percent of magnesium aluminum silicate, 0.01 to 0.5 percent of isothiazolinone, 2 to 8 percent of glycol and 0.1 to 0.5 percent of defoamer.
Further, the preparation also contains the following auxiliary materials in parts by weight: 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol and 0.2% of defoamer; optionally, the defoamer is simethicone polyether.
Preferably: the water suspending agent comprises the following raw materials in parts by weight: 15-20% of flonicamid, 10-20% of spirotetramat, 1-2% of acid, 5% of carboxylic acid dispersing agent, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol and 0.2% of simethicone polyether; optionally, the acid is selected from one of phosphoric acid, dilute hydrochloric acid, lactic acid and methanesulfonic acid, preferably, the acid is an organic acid, the organic acid can be lactic acid or methanesulfonic acid, and the carboxylic acid dispersant is methacrylic acid-methacrylate-polyethylene glycol terpolymer.
Further, when the formulation is a soluble formulation, the soluble formulation comprises the following raw materials in weight fraction: 1-40% of flonicamid, 1-40% of spirotetramat, 1-20% of stabilizer and 10-80% of solvent;
optionally, the soluble agent comprises the following raw materials in parts by weight: 10-20% of flonicamid, 8-20% of spirotetramat, 1-20% of stabilizer and 10-80% of solvent.
Further, the solvent is selected from one or more of propylene glycol methyl ether, propylene glycol ethyl ether, N-methylpyrrolidone, N-ethylpyrrolidone, N-butylpyrrolidone, N-octylpyrrolidone, N-dimethylformamide, N-dimethylacetamide, N-dimethyldecanoamide, gamma-butyrolactone and 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate; optionally, the solvent is selected from one or more of propylene glycol diethyl ether, N-methylpyrrolidone, N-ethylpyrrolidone, N-butylpyrrolidone, N-octylpyrrolidone, N-dimethylformamide, N-dimethylacetamide and N, N-dimethyldecanoamide; optionally, the solvent is selected from one or more of propylene glycol diethyl ether, N-methyl pyrrolidone, N-ethyl pyrrolidone, N-octyl pyrrolidone and N, N-dimethyl decyl amide.
Optionally, the soluble agent comprises the following raw materials in parts by weight: 12-15% of flonicamid, 8-12% of spirotetramat, 10-15% of stabilizer and 20-30% of solvent; optionally, the soluble agent comprises the following raw materials in parts by weight: 12-15% of flonicamid, 8-12% of spirotetramat, 15% of stabilizer and 20% of solvent; optionally, the solvent is selected from one or more of propylene glycol diethyl ether, N-octyl pyrrolidone and N, N-dimethyl decyl amide; optionally, the stabilizer is one or more of benzyl alcohol, phenethyl alcohol and phenoxyethanol.
Further, the preparation also comprises the following emulsifying agent and filling medium in parts by weight: 1-8% of propylene glycol block polyether, 3-8% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate; optionally propylene glycol block polyether 3%, fatty alcohol polyoxyethylene ether 5%, propylene glycol methyl ether acetate 100%;
optionally, the preparation further comprises the following emulsifying agent and filling medium in parts by weight: 1-8% of butanol block polyether, 3-8% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate; optionally 5% of butanol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Preferably, the soluble agent comprises the following raw materials in parts by weight: 12-15% of flonicamid, 8-12% of spirotetramat, 15% of stabilizer, 20% of solvent, 3% of propylene glycol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate; optionally, the solvent is selected from one or more of propylene glycol diethyl ether, N-octyl pyrrolidone and N, N-dimethyl decyl amide; optionally, the stabilizer is one or more of benzyl alcohol, phenethyl alcohol and phenoxyethanol.
Preferably, the soluble agent comprises the following raw materials in parts by weight: 12-15% of flonicamid, 8-12% of spirotetramat, 15% of stabilizer, 20% of solvent, 5% of butanol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate; optionally, the solvent is selected from one or more of propylene glycol diethyl ether, N-octyl pyrrolidone and N, N-dimethyl decyl amide; optionally, the stabilizer is one or more of benzyl alcohol, phenethyl alcohol and phenoxyethanol.
Further, when the formulation is a dispersible oil suspension agent, the dispersible oil suspension agent comprises the following raw materials in parts by weight: 1-30% of flonicamid, 1-30% of spirotetramat, 3-60% of stabilizer, 10-30% of emulsifier and 10-60% of medium oil;
optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 3-40% of stabilizer, 10-30% of emulsifier and 10-59% of medium oil (medium oil is preferably 19-59%);
optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 3-40% of stabilizer, 16-23% of emulsifier and 10-51% of medium oil (medium oil is preferably 19-51%);
optionally, the stabilizer is one or more selected from sodium diisooctyl succinate, 2, 6-di-tert-butyl-p-cresol, epoxidized soybean oil, triglyceryl oleate, triglyceryl linoleate, benzyl alcohol, phenoxyethanol and hexadecanol.
Optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 20-40% of stabilizer, 23% of emulsifier and 10-31% of medium oil (medium oil is preferably 19-31%); optionally, the stabilizer is one or more of oleic acid triglyceride, linoleic acid triglyceride, cetyl alcohol, benzyl alcohol and epoxidized soybean oil.
Optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 20% of stabilizer, 23% of emulsifier and 19-31% of medium oil; optionally, the stabilizer is one or more of oleic acid triglyceride, linoleic acid triglyceride, cetyl alcohol, benzyl alcohol and epoxidized soybean oil; further optionally, the stabilizer is benzyl alcohol and/or epoxidized soybean oil; further alternatively, when the stabilizer is a triglyceride linoleate, the medium oil comprises methyl linolenate, the methyl linolenate comprising at least 20% of the formulation.
Optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 40% of stabilizer, 23% of emulsifier and 10-19% of medium oil; optionally, the stabilizer is a triglyceride of linoleic acid.
Optionally, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 3-7% of stabilizer, 23% of emulsifier and 36-54% of medium oil; the stabilizer is selected from diisooctyl sodium sulfosuccinate and/or 2, 6-di-tert-butyl-p-cresol.
Alternatively, the medium oil is a medium oil in a common sense, including methyl oleate, methyl linoleate, methyl stearate, solvent oil, pine ester oil, mineral oil and the like which are common carrier medium oils in the industry; optionally, the medium oil is selected from one or two of methyl oleate, methyl linoleate, methyl stearate, corn oil and soybean oil;
optionally, the emulsifier is one or more selected from calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, tristyrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene ether oleoyl ricinoleate and sorbitan monooleate polyoxyethylene ether. Wherein, the fatty alcohol polyoxyethylene ether, polyoxyethylene ether oleoyl ricinoleate and sorbitan monooleate polyoxyethylene ether belong to vegetable oil emulsifier.
Optionally, the preparation also contains the following auxiliary materials in parts by weight: 1% of organic bentonite and 1% of gas-phase white carbon black.
Preferably, the dispersible oil suspending agent comprises the following raw materials in parts by weight: 10-16% of flonicamid, 8-16% of spirotetramat, 20-40% of stabilizer, 23% of emulsifier and 19-31% of medium oil, and optionally, one or more of linoleic acid triglyceride, benzyl alcohol and epoxidized soybean oil. The emulsifier is at least two selected from calcium dodecyl benzene sulfonate, polyoxyethylene ether oleoyl ricinoleate, fatty alcohol polyoxyethylene ether and polyoxyethylene ether oleoyl ricinoleate.
The emulsifier comprises the following raw materials in total weight of the preparation: 8% of calcium dodecyl benzene sulfonate, 5% of polyoxyethylene ether oleoyl ricinoleate and 8% of fatty alcohol polyoxyethylene ether.
Alternatively, the emulsifier comprises the following materials in total weight of the formulation: 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether and 5% of castor oil polyoxyethylene ether.
Alternatively, the emulsifier comprises the following materials in total weight of the formulation: 8-8% of calcium dodecyl benzene sulfonate and 15% of polyoxyethylene ether oleoyl ricinoleate.
Further, the water suspending agent, the soluble agent or the dispersible oil suspending agent preparation also contains a coloring agent; such as azo dyes or triphenylmethane dyes.
On the other hand, the preparation method of the flonicamid-spirotetramat mixed preparation is characterized in that,
when the preparation is an aqueous suspension, the preparation method comprises the following steps: firstly, mixing the flonicamid raw material, the spirotetramat raw material, the auxiliary material and water in proportion, shearing and sanding until the particle size is smaller than 5 microns to obtain a suspending agent with uniform appearance and dispersibility in water;
when the preparation is a soluble agent, the preparation method comprises the following steps: firstly, mixing the flonicamid raw material, the spirotetramat raw material, the auxiliary material and the solvent in proportion, heating and stirring for 10-20 minutes at 30-40 ℃ until the mixture is clear and transparent;
when the preparation is a dispersible oil suspending agent, the preparation method comprises the following steps: the preparation method comprises the steps of mixing the flonicamid raw material, the spirotetramat raw material, the emulsifying agent and the auxiliary materials in proportion, and grinding the mixture by a sand mill to obtain the dispersible oil suspending agent.
In still another aspect, the application of the flonicamid-spirotetramat mixed preparation in controlling plant insect pests is provided.
Further, the plant diseases and insect pests are piercing-sucking mouthparts pests.
The equipment of the processing technology of the preparation of the invention is publicly known.
Advantageous effects
According to the flonicamid-spirotetramat mixed water suspending agent, the stabilizer (acid and carboxylic acid dispersing agent are matched) is introduced, so that the reduction of the spirotetramat content of the suspending liquid after storage can be effectively inhibited. The flonicamid and spirotetramat are mixed into a soluble solution, and a stabilizer is introduced to further screen a solvent, so that the content reduction of spirotetramat can be effectively inhibited. The flonicamid and spirotetramat are mixed with the dispersible oil suspending agent, and the corresponding emulsifying agent is screened by screening the stabilizer and the medium oil type, so that the content reduction of spirotetramat can be effectively inhibited.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings. The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
FIG. 1 is a content chromatogram of spirotetramat after 14 days of storage at normal temperature in the prior art;
FIG. 2 is a chromatogram of the content of the spirotetramat after 14 days of heat storage at 54 ℃.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are 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. Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising", etc. will be understood to include the stated element or component without excluding other elements or components.
In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, elements, methods, means, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention. The percentages in all the formulas of the invention are weight ratios.
The flonicamid and spirotetramat of the invention can be obtained in a commercial mode.
1. Preparation of a Water-dispersible suspension agent:
preparation of a Water-dispersible suspension agent: firstly, the flonicamid, the spirotetramat raw medicine, the auxiliary agent and water are weighed and mixed, sheared for a certain time, and sanded until the particle size is smaller than 5 microns, so as to obtain the suspending agent which has uniform appearance and can be dispersed in water. Specific formulation examples are as follows:
example 1 (no stabilizer):
15% of flonicamid, 10% of spirotetramat, 5% of tritolyl polyether phosphate triethanolamine salt, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoamer and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 2:
15% of flonicamid, 10% of spirotetramat, 0.5% of methylsulfonic acid, 5% of trisstyrol polyether phosphate triethanolammonium salt, 2% of EO-PO block polyether dispersant, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of glycol, 0.2% of defoamer and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 3:
15% of flonicamid, 10% of spirotetramat, 1.5% of methylsulfonic acid, 5% of trisstyrol polyether phosphate triethanolammonium salt, 2% of EO-PO block polyether dispersant, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of glycol, 0.2% of defoamer and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 4:
15% of flonicamid, 10% of spirotetramat, 1.5% of methylsulfonic acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoamer and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 5:
15% of flonicamid, 10% of spirotetramat, 2% of phosphoric acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 6:
10% of flonicamid, 8% of spirotetramat, 2% of dilute hydrochloric acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension agent.
Example 7:
18% of flonicamid, 12% of spirotetramat, 1.5% of lactic acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension.
Example 8:
8% of flonicamid, 15% of spirotetramat, 1% of citric acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension agent.
Example 9:
20% of flonicamid, 20% of spirotetramat, 1% of methylsulfonic acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension agent.
Example 10:
20% of flonicamid, 20% of spirotetramat, 2% of methylsulfonic acid, 5% of methacrylic acid-methacrylate-polyethylene glycol terpolymer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol, 0.2% of defoaming agent and the balance of water, and grinding the materials by a sand mill to prepare the water suspension agent.
The defoamer of the above embodiment is simethicone polyether.
The contents of flonicamid and spirotetramat after 14 days of storage at 54℃in each of the above examples of the aqueous suspension are shown in the following table. In table 1, example 2..the term "example 10" refers to example 1, example 2..the term "example 10".
TABLE 1 Water suspending agent content and decomposition Rate after heat storage
As can be seen from Table 1, the dissolution rate of spirotetramat is as high as 32% after 14 days of heat storage at 54 ℃ without using the stabilizer of the invention in example 1; in the examples 2 and 3, the organic acid stabilizer provided by the invention is only used, and after 14 days of heat storage at 54 ℃, the decomposition rate of the spirotetramat is respectively 21% and 14%, and compared with the example 1, the decomposition rate is obviously improved, but the decomposition rate is still higher; the combination scheme of the invention is adopted in examples 4-10, and the decomposition rate of spirotetramat after 14 days of heat storage at 54 ℃ can be controlled below 5%, which accords with the content quality standard requirement of the pesticide preparation product after heat storage.
2. Preparation of the soluble agent:
preparation of the soluble agent: firstly, the flonicamid and the spirotetramat are used as raw materials, the auxiliary agent and the solvent are weighed and mixed, and then the mixture is heated and stirred for 10 to 20 minutes at the temperature of between 30 and 40 ℃ until the mixture is clear and transparent. Specific formulation examples are as follows:
example 1:
15% of flonicamid, 10% of spirotetramat, 20% of N-octyl pyrrolidone, 3% of propylene glycol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 2:
15% of flonicamid, 10% of spirotetramat, 30% of N-octyl pyrrolidone, 3% of propylene glycol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 3:
15% of flonicamid, 10% of spirotetramat, 20% of N-octyl pyrrolidone, 10% of benzyl alcohol, 3% of propylene glycol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 4:
15% of flonicamid, 10% of spirotetramat, 20% of N-octyl pyrrolidone, 15% of benzyl alcohol, 3% of propylene glycol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 5:
15% of flonicamid, 10% of spirotetramat, 20% of N, N-dimethyl capramide, 15% of phenoxyethanol, 5% of butanol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 6:
14% of flonicamid, 12% of spirotetramat, 20% of N-octyl pyrrolidone, 15% of phenethyl alcohol, 5% of butanol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
Example 7:
12% of flonicamid, 8% of spirotetramat, 20% of propylene glycol diethyl ether, 15% of phenethyl alcohol, 5% of butanol block polyether, 5% of fatty alcohol polyoxyethylene ether and 100% of propylene glycol methyl ether acetate.
After 14 days of storage of the samples of the above examples at 54℃the flonicamid and spirotetramat contents are as shown in the following table. In table 2, example 1, example 2..example 7 refers to example 1, example 2..example 7.
TABLE 2 Table of the contents and decomposition rates of the solutions after heat storage
From Table 2, examples 1 to 2, in which the stabilizer of the present invention was not used, showed that the decomposition rate of spirotetramat was as high as 12 to 18% after 14 days of heat storage at 54℃and the solvent did not exert an obvious stabilizing effect; examples 3-7 use the stabilizer scheme of the invention, the decomposition rate of spirotetramat is obviously reduced after 14 days of heat storage at 54 ℃, and except example 3, the decomposition rate can be controlled below 5%, and the requirements of the quality standard of the content of the heat storage pesticide preparation products are met.
3. Dispersible oil suspension agent
Preparation of dispersible oil suspending agent: the flonicamid, spirotetramat technical, emulsifying agent, dispersing agent, thickening agent, methyl ester oil and the like are weighed and mixed, and then the mixture is ground by a sand mill to prepare the dispersible oil suspending agent. Specific formulation examples are as follows:
example 1:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 2:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 1% of organic bentonite, 1% of gas-phase white carbon black, 20% of methyl palmitate and 100% of methyl oleate.
Example 3:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 1% of organic bentonite, 1% of gas-phase white carbon black, 20% of methyl stearate and 100% of methyl oleate.
Example 4:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 1% of organic bentonite, 1% of gas-phase white carbon black, 20% of methyl linolenate and 100% of methyl oleate.
Example 5:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 20% of linoleic acid triglyceride, 1% of organic bentonite, 1% of gas-phase white carbon black, 20% of linolenic acid methyl ester and 100% of oleic acid methyl ester.
Example 6:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of polyoxyethylene ether oleoyl ricinoleate, 20% of linoleic acid triglyceride, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of oleic acid methyl ester.
Example 7:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 5% of polyoxyethylene ether oleoyl ricinoleate, 8% of fatty alcohol polyoxyethylene ether, 20% of oleic acid triglyceride, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 8:
10% of flonicamid, 8% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 5% of polyoxyethylene ether oleoyl ricinoleate, 8% of fatty alcohol polyoxyethylene ether, 40% of linoleic acid triglyceride, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of methyl oleate.
Example 9:
16% of flonicamid, 10% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of castor oil polyoxyethylene ether, 20% of benzyl alcohol, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 10:
16% of flonicamid, 10% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 20% of cetyl alcohol, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 11:
16% of flonicamid, 10% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of diisooctyl succinate sodium sulfonate, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 12:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 7% of sodium diisooctyl succinate, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 13:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 3% of 2, 6-di-tert-butyl-p-cresol, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of methyl oleate.
Example 14:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 5% of 2, 6-di-tert-butyl-p-cresol, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of methyl oleate.
Example 15:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 8% of fatty alcohol polyoxyethylene ether, 20% of epoxidized soybean oil, 1% of organic bentonite, 1% of gas-phase white carbon black and 100% of methyl oleate.
Example 16:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 15% of polyoxyethylene ether oleoyl ricinoleate, 20% of epoxidized soybean oil, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of soybean oil.
Example 17:
16% of flonicamid, 16% of spirotetramat, 8% of calcium dodecyl benzene sulfonate, 15% of polyoxyethylene ether oleoyl ricinoleate, 20% of epoxidized soybean oil, 1% of organic bentonite, 1% of gas phase white carbon black and 100% of corn oil.
After 14 days of storage of the samples of the above examples at 54℃the flonicamid and spirotetramat contents are as shown in the following table. In table 3, example 1, example 2..example 17 refers to example 1, example 2..example 17.
TABLE 3 Table 3 content and decomposition Rate of dispersible oil suspending agent after heat storage
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As can be seen from Table 3, in example 1, the decomposition rate of spirotetramat was as high as 18% after heat-storing at 54℃for 14 days without using the stabilizer of the present invention, while in examples 2 to 4, the decomposition rate of spirotetramat was varied to a different extent after heat-storing at 54℃for 14 days while increasing or changing the kind of medium oil, but still a relatively high decomposition rate was present; except for example 6 and example 12 (the content of the spirotetramat is obviously improved in comparison with example 1), the decomposition rate of spirotetramat can be controlled below 5% after the spirotetramat is thermally stored for 14 days at 54 ℃ by using the stabilizer scheme of the invention in examples 5-17, and the requirements of the quality standard of the content of the pesticide preparation products after the heat storage are met. The inventors of the present invention have also found an interesting phenomenon: the stabilizers used in examples 5, 6 and 8 are all linoleic acid triglyceride, but the decomposition rate of example 6 is obviously higher than that of examples 8 and 5, and the medium oil methyl linolenate in example 5 probably plays a certain role in stabilizing, but the decomposition rate of spirotetramat can be obviously reduced when methyl linolenate is replaced by linoleic acid triglyceride (namely example 8).
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (23)
1. The flonicamid-spirotetramat mixed preparation is characterized by comprising the following raw materials in parts by weight:
the preparation is an aqueous suspending agent, and the aqueous suspending agent comprises the following raw materials in parts by weight: 1-40% of flonicamid, 1-40% of spirotetramat, 0.3-5% of acid, 1-15% of carboxylic acid dispersing agent and formulation auxiliary materials;
the carboxylic acid dispersing agent is methacrylic acid-methacrylate-polyethylene glycol terpolymer and ATLOX TM 4913. One or more of Agrilan 755, tersperse 2500 and EMULSON AG/TRN 14105;
the acid is one or more of dodecylbenzene sulfonic acid, dilute hydrochloric acid, dilute sulfuric acid, phosphoric acid, lactic acid, taurine, succinic acid, glycyrrhizic acid, methanesulfonic acid, chloroacetic acid, glacial acetic acid, benzoic acid, salicylic acid, citric acid, malic acid, tartaric acid and ascorbic acid.
2. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 0.5-2% of acid and 3-8% of carboxylic acid dispersing agent.
3. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 3-8% of carboxylic acid dispersing agent.
4. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 5-8% of carboxylic acid dispersing agent.
5. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 0.5-2% of acid and 5% of carboxylic acid dispersing agent.
6. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 4-6% of carboxylic acid dispersing agent.
7. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 5-6% of carboxylic acid dispersing agent.
8. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 8-20% of flonicamid, 8-20% of spirotetramat, 1-2% of acid and 5% of carboxylic acid dispersing agent.
9. The flonicamid-spirotetramat mixed formulation of claim 1, wherein the water suspending agent comprises the following raw materials in parts by weight: 15-20% of flonicamid, 10-20% of spirotetramat, 1-2% of acid and 5% of carboxylic acid dispersing agent.
10. The flonicamid-spirotetramat formulation of claim 1, wherein the carboxylic acid dispersant is a methacrylic acid-methacrylate-polyethylene glycol terpolymer.
11. The flonicamid-spirotetramat mixed formulation according to any one of claims 1 to 10, wherein the acid is one or more selected from the group consisting of dilute hydrochloric acid, phosphoric acid, lactic acid, methylsulfonic acid and citric acid.
12. The flonicamid-spirotetramat mixed formulation according to any one of claims 1 to 10, further comprising the following auxiliary materials in parts by weight: 0.1 to 1 percent of xanthan gum, 0.5 to 2 percent of magnesium aluminum silicate, 0.01 to 0.5 percent of isothiazolinone, 2 to 8 percent of glycol and 0.1 to 0.5 percent of defoamer.
13. The flonicamid-spirotetramat formulation of claim 12, wherein the defoamer is simethicone polyether.
14. The flonicamid-spirotetramat mixed formulation according to any one of claims 1 to 10, further comprising the following auxiliary materials in parts by weight: xanthan gum 0.2%, magnesium aluminum silicate 1%, isothiazolinone 0.1%, ethylene glycol 4% and simethicone polyether 0.2%.
15. The flonicamid-spirotetramat mixed formulation according to any one of claims 1 to 10, wherein the aqueous suspension comprises the following raw materials in parts by weight: 15-20% of flonicamid, 10-20% of spirotetramat, 1-2% of acid, 5% of carboxylic acid dispersing agent, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.1% of isothiazolinone, 4% of ethylene glycol and 0.2% of simethicone polyether.
16. The flonicamid-spirotetramat formulation of claim 15, wherein the acid is selected from one of phosphoric acid, dilute hydrochloric acid, lactic acid and methylsulfonic acid.
17. The flonicamid-spirotetramat formulation of claim 15, wherein the acid is an organic acid.
18. The flonicamid-spirotetramat formulation of claim 17, wherein the organic acid is lactic acid or methylsulfonic acid and the carboxylic acid dispersant is methacrylic acid-methacrylate-polyethylene glycol terpolymer.
19. The flonicamid-spirotetramat mixed formulation according to any one of claims 1 to 10, further comprising a coloring agent.
20. The flonicamid-spirotetramat formulation of claim 19, wherein the coloring agent is an azo dye or a triphenylmethane dye.
21. A process for preparing the flonicamid-spirotetramat compound formulation of any one of claims 1 to 20, characterized in that:
when the preparation is an aqueous suspension, the preparation method comprises the following steps: the flonicamid raw material, the spirotetramat raw material, the auxiliary material and water are mixed according to a proportion, sheared and sanded until the particle size is smaller than 5 microns, and the suspending agent with uniform appearance and dispersibility in water is obtained.
22. Use of the flonicamid-spirotetramat compound formulation of any one of claims 1 to 20 or the flonicamid-spirotetramat compound formulation prepared by the preparation method of claim 21 for controlling plant pests.
23. The use of claim 22, wherein the plant pest is a piercing-sucking mouth gag pest.
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CN102696582A (en) * | 2012-04-23 | 2012-10-03 | 广东中迅农科股份有限公司 | Flonicamid suspension concentrate and method for preparing same |
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CN106417330A (en) * | 2016-09-19 | 2017-02-22 | 佛山市盈辉作物科学有限公司 | Insecticidal composition containing cyclaniliprole and spirotetramat |
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CN111328819A (en) * | 2020-04-20 | 2020-06-26 | 六夫丁作物保护有限公司 | Low-temperature-resistant suspending agent containing spirotetramat and preparation method thereof |
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CN102578121A (en) * | 2011-12-19 | 2012-07-18 | 河南金田地农化有限责任公司 | Pesticide insecticidal and acaricidal composition containing spiroteramat |
CN102696582A (en) * | 2012-04-23 | 2012-10-03 | 广东中迅农科股份有限公司 | Flonicamid suspension concentrate and method for preparing same |
CN103858899A (en) * | 2012-12-12 | 2014-06-18 | 王丽君 | Pesticide composition containing spirotetramat and amide insecticide |
CN106417330A (en) * | 2016-09-19 | 2017-02-22 | 佛山市盈辉作物科学有限公司 | Insecticidal composition containing cyclaniliprole and spirotetramat |
CN109452267A (en) * | 2018-11-22 | 2019-03-12 | 深圳诺普信农化股份有限公司 | The preparation method and aqueous pesticide formulations of aqueous pesticide formulations |
CN111328819A (en) * | 2020-04-20 | 2020-06-26 | 六夫丁作物保护有限公司 | Low-temperature-resistant suspending agent containing spirotetramat and preparation method thereof |
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