CN111587879B - Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof - Google Patents
Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof Download PDFInfo
- Publication number
- CN111587879B CN111587879B CN202010620632.3A CN202010620632A CN111587879B CN 111587879 B CN111587879 B CN 111587879B CN 202010620632 A CN202010620632 A CN 202010620632A CN 111587879 B CN111587879 B CN 111587879B
- Authority
- CN
- China
- Prior art keywords
- water dispersible
- flutolanil
- metrafenone
- agent
- dispersible granule
- 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.)
- Active
Links
- 239000005810 Metrafenone Substances 0.000 title claims abstract description 78
- 239000004562 water dispersible granule Substances 0.000 title claims abstract description 73
- AMSPWOYQQAWRRM-UHFFFAOYSA-N metrafenone Chemical compound COC1=CC=C(Br)C(C)=C1C(=O)C1=C(C)C=C(OC)C(OC)=C1OC AMSPWOYQQAWRRM-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000005786 Flutolanil Substances 0.000 title claims abstract description 70
- PTCGDEVVHUXTMP-UHFFFAOYSA-N flutolanil Chemical compound CC(C)OC1=CC=CC(NC(=O)C=2C(=CC=CC=2)C(F)(F)F)=C1 PTCGDEVVHUXTMP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title abstract description 31
- 239000004480 active ingredient Substances 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 239000000080 wetting agent Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 25
- 239000002738 chelating agent Substances 0.000 claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 201000010099 disease Diseases 0.000 claims abstract description 18
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims abstract description 18
- 235000013311 vegetables Nutrition 0.000 claims abstract description 7
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 6
- -1 alkyl naphthalene sulphonate formaldehyde Chemical compound 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 14
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 14
- 235000011152 sodium sulphate Nutrition 0.000 claims description 14
- 239000006229 carbon black Substances 0.000 claims description 13
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 13
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 10
- 239000007884 disintegrant Substances 0.000 claims description 10
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 9
- 229920005646 polycarboxylate Polymers 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000004898 kneading Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229940095686 granule product Drugs 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 229920002261 Corn starch Polymers 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000008120 corn starch Substances 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
- 235000011180 diphosphates Nutrition 0.000 claims description 2
- 229940009662 edetate Drugs 0.000 claims description 2
- 235000013305 food Nutrition 0.000 claims description 2
- 229940050410 gluconate Drugs 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 229940048084 pyrophosphate Drugs 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 25
- 230000000694 effects Effects 0.000 abstract description 20
- 241000221785 Erysiphales Species 0.000 abstract description 17
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 15
- 229940079593 drug Drugs 0.000 abstract description 8
- 239000000575 pesticide Substances 0.000 abstract description 6
- 238000001228 spectrum Methods 0.000 abstract description 6
- 206010059866 Drug resistance Diseases 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 230000001934 delay Effects 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 17
- 241000209140 Triticum Species 0.000 description 12
- 235000021307 Triticum Nutrition 0.000 description 12
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 11
- 239000012752 auxiliary agent Substances 0.000 description 9
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 8
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 8
- 230000002195 synergetic effect Effects 0.000 description 8
- 240000008067 Cucumis sativus Species 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000003899 bactericide agent Substances 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- FRHYNIAICJRSQH-UHFFFAOYSA-N dodecanoic acid;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC(O)=O FRHYNIAICJRSQH-UHFFFAOYSA-N 0.000 description 5
- 238000009472 formulation Methods 0.000 description 5
- 230000003902 lesion Effects 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 4
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 4
- 206010027145 Melanocytic naevus Diseases 0.000 description 4
- 208000007256 Nevus Diseases 0.000 description 4
- 239000001110 calcium chloride Substances 0.000 description 4
- 229910001628 calcium chloride Inorganic materials 0.000 description 4
- 235000011148 calcium chloride Nutrition 0.000 description 4
- 229920005551 calcium lignosulfonate Polymers 0.000 description 4
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 4
- 235000002639 sodium chloride Nutrition 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 229920005682 EO-PO block copolymer Polymers 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 3
- 235000011130 ammonium sulphate Nutrition 0.000 description 3
- 244000052616 bacterial pathogen Species 0.000 description 3
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229940044652 phenolsulfonate Drugs 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 3
- 229940048086 sodium pyrophosphate Drugs 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 239000000375 suspending agent Substances 0.000 description 3
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 239000004563 wettable powder Substances 0.000 description 3
- XEGMDUOAESTQCC-UHFFFAOYSA-N 1-(naphthalen-1-ylmethyl)naphthalene;sodium Chemical compound [Na].C1=CC=C2C(CC=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 XEGMDUOAESTQCC-UHFFFAOYSA-N 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 235000009849 Cucumis sativus Nutrition 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 244000061456 Solanum tuberosum Species 0.000 description 2
- 235000002595 Solanum tuberosum Nutrition 0.000 description 2
- 241000219094 Vitaceae Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- QKZIVVMOMKTVIK-UHFFFAOYSA-M anilinomethanesulfonate Chemical compound [O-]S(=O)(=O)CNC1=CC=CC=C1 QKZIVVMOMKTVIK-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- HAFJKKYURCIBBG-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid;sodium Chemical compound [Na].O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 HAFJKKYURCIBBG-UHFFFAOYSA-N 0.000 description 2
- 235000021021 grapes Nutrition 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000176 sodium gluconate Substances 0.000 description 2
- 235000012207 sodium gluconate Nutrition 0.000 description 2
- 229940005574 sodium gluconate Drugs 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- PYODKQIVQIVELM-UHFFFAOYSA-M sodium;2,3-bis(2-methylpropyl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(CC(C)C)C(CC(C)C)=CC2=C1 PYODKQIVQIVELM-UHFFFAOYSA-M 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 229940035936 ubiquinone Drugs 0.000 description 2
- 230000001018 virulence Effects 0.000 description 2
- 239000004711 α-olefin Substances 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 241000221198 Basidiomycota Species 0.000 description 1
- ACTIUHUUMQJHFO-UHFFFAOYSA-N Coenzym Q10 Natural products COC1=C(OC)C(=O)C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UHFFFAOYSA-N 0.000 description 1
- 208000035240 Disease Resistance Diseases 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000221787 Erysiphe Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 208000025309 Hair disease Diseases 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 208000030852 Parasitic disease Diseases 0.000 description 1
- 241000579741 Sphaerotheca <fungi> Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- TTWYZDPBDWHJOR-IDIVVRGQSA-L adenosine triphosphate disodium Chemical compound [Na+].[Na+].C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OP(O)(=O)OP([O-])([O-])=O)[C@@H](O)[C@H]1O TTWYZDPBDWHJOR-IDIVVRGQSA-L 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- ZVSKZLHKADLHSD-UHFFFAOYSA-N benzanilide Chemical compound C=1C=CC=CC=1C(=O)NC1=CC=CC=C1 ZVSKZLHKADLHSD-UHFFFAOYSA-N 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- ACTIUHUUMQJHFO-UPTCCGCDSA-N coenzyme Q10 Chemical compound COC1=C(OC)C(=O)C(C\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CC\C=C(/C)CCC=C(C)C)=C(C)C1=O ACTIUHUUMQJHFO-UPTCCGCDSA-N 0.000 description 1
- 235000017471 coenzyme Q10 Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012136 culture method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 208000034653 disorder of pilosebaceous unit Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 230000002888 effect on disease Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 239000012628 flowing agent Substances 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 244000053095 fungal pathogen Species 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000008811 mitochondrial respiratory chain Effects 0.000 description 1
- LCRMGUFGEDUSOG-UHFFFAOYSA-N naphthalen-1-ylsulfonyloxymethyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(OCOS(=O)(=O)C=3C4=CC=CC=C4C=CC=3)=O)=CC=CC2=C1 LCRMGUFGEDUSOG-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 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
- NPCOQXAVBJJZBQ-UHFFFAOYSA-N reduced coenzyme Q9 Natural products COC1=C(O)C(C)=C(CC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C)C(O)=C1OC NPCOQXAVBJJZBQ-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- HLPHHOLZSKWDAK-UHFFFAOYSA-M sodium;formaldehyde;naphthalene-1-sulfonate Chemical compound [Na+].O=C.C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 HLPHHOLZSKWDAK-UHFFFAOYSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 1
- 231100000820 toxicity test Toxicity 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
-
- 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
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/04—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aldehyde or keto groups, or thio analogues thereof, directly attached to an aromatic ring system, e.g. acetophenone; Derivatives thereof, e.g. acetals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
- A01N37/24—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides containing at least one oxygen or sulfur atom being directly attached to the same aromatic ring system
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of pesticides, and discloses a metrafenone and flutolanil-containing water dispersible granule and application thereof, wherein the preparation comprises the following components in percentage by weight: 30-75% of pharmaceutical active ingredients, 3-10% of dispersing agent, 2-6% of wetting agent, 1-8% of disintegrating agent, 1-4% of chelating agent and the balance of filler, wherein the pharmaceutical active ingredients are flutolanil and metrafenone with the mass ratio of less than 10: 1. The preparation of the invention expands the bactericidal spectrum, improves the drug duration, delays the generation of drug resistance and has good effect on preventing and treating powdery mildew and other diseases in grain crops, vegetables and fruit trees. The invention also discloses a preparation method of the water dispersible granule, which has the advantages of simplicity, convenient operation, low energy consumption, environmental protection, easy continuous production and excellent product quality. In addition, the flutolanil and the metrafenone are compounded and prepared into the water dispersible granules suitable for different water qualities, and the application is facilitated.
Description
Technical Field
The invention belongs to the technical field of pesticides, and relates to a pesticide water dispersible granule, in particular to a water dispersible granule containing metrafenone and flutolanil, and a preparation method and application thereof.
Background
Metrafenone (Metrafenone), chemical name: the 3 ' -bromo-2, 3,4,6 ' -tetramethoxy-2 ', 6-dimethyl benzophenone belongs to benzophenone bactericides, is mainly used for preventing and treating diseases such as powdery mildew and the like of crops such as cereals, grapes, cucumbers and the like, and has certain protection and treatment effects; and, its common formulation is a suspension.
However, fungicide varieties containing a single active ingredient often have various degrees of defects in agricultural disease control, such as: the bactericidal spectrum is narrow, the germs are easy to generate drug resistance after continuous use, and the environmental pollution is aggravated when the use frequency is high; in addition, certain types of formulations are inconvenient to store and transport.
Disclosure of Invention
In view of the above, the invention provides a metrafenone and flutolanil-containing water dispersible granule, and a preparation method and application thereof.
The invention aims to provide a water dispersible granule containing metrafenone and flutolanil and a preparation method thereof. The water dispersible granule has better disintegration and suspension rate under different water quality conditions, lower foamability, environmental friendliness and convenient storage and transportation.
The invention also provides a preparation method of the water dispersible granule, and the preparation method of the water dispersible granule is simple, easy to operate, environment-friendly and safe in preparation process, free of pollution problem, low in cost and easy for industrial production.
The invention also provides the application of the water dispersible granule in preventing and treating diseases of grain crops, vegetables or fruit trees, and the water dispersible granule has the advantages of wide bactericidal spectrum, good bactericidal effect and better use experience compared with a single medicament active ingredient preparation.
Through research and a large number of indoor and field tests, the inventor finds that the combination of flutolanil and metrafenone can generate good synergistic effect. The invention is realized by the following measures:
a water dispersible granule containing metrafenone and flutolanil consists of the following components in percentage by weight: 30-75% of active ingredients of the medicine, 3-10% of dispersing agent, 2-6% of wetting agent, 1-8% of disintegrating agent, 1-4% of chelating agent and the balance of filler.
In the water dispersible granule, the active ingredients of the drug are flutolanil and metrafenone in a mass ratio of less than 10:1, preferably 1-8:1, the effect is better when the mass ratio of flutolanil to metrafenone is 1-5:1, and the effect is optimal when the mass ratio of flutolanil to metrafenone is 3: 1.
Wherein, the chemical name of Metrafenone is as follows: the 3 ' -bromo-2, 3,4,6 ' -tetramethoxy-2 ', 6-dimethyl benzophenone belongs to benzophenone bactericides, is mainly used for preventing and treating diseases such as powdery mildew and the like of crops such as cereals, grapes, cucumbers and the like, and has certain protection and treatment effects.
Flutolanil belongs to a new benzoyl aniline bactericide, and mainly inhibits the activity of mitochondrial respiratory chain complex enzyme II (succinic acid-ubiquinone oxidoreductase) in pathogenic fungi, so that electrons cannot be transferred from succinic acid to ubiquinone, ATP (adenosine triphosphate) of bacteria cannot be normally synthesized, and bacteria die due to energy deficiency. The flutolanil has protection and treatment activity, is mainly used for preventing and treating the harm of pathogenic bacteria of basidiomycetes, and can prevent and treat diseases such as rice sheath blight, potato black nevus, vegetable seedling blight, cereal snow rot, rust disease and the like. The flutolanil and the metrafenone have different action mechanisms, and the combination of the flutolanil and the metrafenone generates a good synergistic effect by verification, so that the bactericidal spectrum is expanded, the generation of drug resistance is slowed down, the bactericidal effect is improved, and the sustainable development of the environment is facilitated.
Furthermore, the water dispersible granule also comprises an auxiliary agent acceptable in the agricultural pharmacy besides the active pharmaceutical ingredient; the content of the active ingredients in the water dispersible granules is 30-75 wt%, preferably 50-75 wt%.
Water dispersible granules are also called dry flowing agents and water-suspendable granules; automatically disintegrating after entering water, and dispersing into suspension. It is a new formulation developed on the basis of wettable powder and suspending agent, and has the characteristics of good dispersibility, high suspension rate, good stability, convenient use and the like. Compared with wettable powder and missible oil, the water dispersible granule does not contain organic solvent, is more environment-friendly than missible oil, is more environment-friendly than wettable powder, and is easier to package, store and transport.
The embodiment of the invention aims at the characteristics of active ingredients of the medicine: the flutolanil raw pesticide is a colorless crystal, and the water distribution coefficient of n-octanol/water is as follows: logP ═ 4.81(pH 4.0, 25 ℃), metrafenone as a white crystalline solid, coefficient of n-octanol/water partition: logP ═ 4.3(pH 4.0, 25 ℃), both active ingredients being strong lipophilic bulk drugs. The inventor researches and screens the assistant of the water dispersible granule, and obtains a preferable water dispersible granule formulation and an assistant system by selecting and matching a wetting agent and a dispersing agent.
Further, the water dispersible granule preferably comprises the following components in percentage by weight: 30-75% of active pharmaceutical ingredients (preferably 50-75%), 4-6% of dispersing agent, 3-5% of wetting agent, 3-5% of disintegrating agent, 2-3% of chelating agent and the balance of filler.
For typical water dispersible granules, the dispersant may be one or more of calcium lignosulfonate, polycarboxylate, sodium alkyl phenol sulfonate, dodecylpolyoxyethylene phosphate, sodium methylene dinaphthalene sulfonate, sodium alkyl naphthalene sulfonate formaldehyde polycondensate and ethylene oxide-propylene oxide block copolymer. In the embodiment of the invention, the dispersing agent is preferably one or more of polycarboxylate and alkyl naphthalene sulfonate formaldehyde polycondensate, more preferably a mixture of polycarboxylate and alkyl naphthalene sulfonate sodium salt formaldehyde polycondensate in a mass ratio of 3: 1-2, and most preferably a mass ratio of 3: 1. In the embodiment of the invention, the polycarboxylate is further selected from T-2700 of Hensmei company, the formaldehyde polycondensate of the sodium salt of the alkyl naphthalene sulfonate is further selected from D-425 of Acksu company, and the dispersing agent is matched in combination to realize the performance of the optimal effect of the dispersion suspension rate of the preparation product in water.
For typical water dispersible granules, the wetting agent may be one or more of nekal BX, sodium lauryl sulfate, alkyl naphthalene sulfonate, lauric acid sulfate, alkyl sulfate, sodium naphthalene sulfonate formaldehyde condensate and sodium alpha-olefin sulfonate. In the embodiment of the invention, the wetting agent is preferably one or more of alkyl naphthalene sulfonate and alkyl sulfate, more preferably a mixture of alkyl naphthalene sulfonate and alkyl sulfate in a mass ratio of 1: 1-3, and most preferably a mixture of alkyl naphthalene sulfonate and alkyl sulfate in a mass ratio of 1: 2. In the embodiment of the invention, the alkyl naphthalene sulfonate is further selected as Morwet EFW of Acksonobel, and the alkyl sulfate is further selected as REAX WL of Meidwinhiweigwick, so that the compounding effect is optimal.
For general water dispersible granules, the disintegrant may be one or more of urea, sodium sulfate, ammonium sulfate, calcium chloride, potassium dihydrogen phosphate and sodium chloride. In the embodiment of the invention, the disintegrating agent is preferably a mixture of potassium dihydrogen phosphate and sodium sulfate, more preferably a mixture of potassium dihydrogen phosphate and sodium sulfate in a mass ratio of 1: 1-3, and most preferably a mass ratio of 1: 1.5.
In the water dispersible granule of the invention, the chelating agent can be edetate, pyrophosphate, gluconate, tripolyphosphate, such as one or more of disodium edetate, sodium pyrophosphate, sodium gluconate, and sodium tripolyphosphate, preferably disodium edetate.
In the water dispersible granule, the filler is crushed by airflow in the processing process until the requirement of the particle size is met, and no special requirement is provided for the raw material of the filler. The filler can be one or more of corn starch, talcum powder, diatomite, white carbon black and kaolin, and white carbon black is preferred.
In some preferred embodiments of the present application, the water dispersible granule formulation wherein the dispersant is a mixture of a polycarboxylate and an alkyl naphthalene sulfonic acid sodium salt formaldehyde polycondensate in a mass ratio of 3: 1; the wetting agent is a mixture of alkyl naphthalene sulfonate and alkyl sulfate in a mass ratio of 1: 2; the disintegrating agent is a mixture of monopotassium phosphate and sodium sulfate in a mass ratio of 1: 1.5; the chelating agent is disodium ethylene diamine tetraacetate; the filler is white carbon black.
The embodiment of the invention also provides a preparation method of the water dispersible granule, which comprises the following steps: uniformly mixing flutolanil, metrafenone, a dispersing agent, a wetting agent, a disintegrating agent, a chelating agent and a filler, carrying out ultramicro airflow pulverization to preferably obtain 800-mesh fine powder with the particle size of 680, mixing the obtained fine powder with water, kneading the fine powder, wherein the water addition amount can be 15-30% of the total mass of the materials, carrying out extrusion granulation after kneading, and drying (preferably drying the obtained particles at the temperature of 30-65 ℃) to obtain the flutolanil-metrafenone water dispersible granule product.
The water dispersible granule is mainly used for preventing and treating diseases in grain crops, vegetables or fruit trees, wherein the diseases can be powdery mildew, southern blight, black nevus and the like. In some embodiments of the invention, the disease-controlling crop is peanut, potato, wheat, or the like; in other embodiments, the powdery mildew of plants such as cucumber and apple is pointed out. Wherein, the cucumber powdery mildew is commonly called as 'white hair disease', and at the initial stage of disease occurrence, white small powdery specks are generated on leaves, and gradually expand into large powdery areas and are fully distributed on the leaves; the pathogenic bacteria are fungi belonging to the genus Sphaerotheca of the family Erysiphe of the order Erysipheles of the class Ascomycotina, are obligate parasitic diseases, and can parasitize on host plants throughout the year, becoming a primary source of infection.
In addition, the mode of application of the agent is not particularly limited, as long as it is applied by spraying or the like, which is well known to those skilled in the art.
The beneficial effects of the invention include:
1. the active ingredients of the drug, namely flutolanil and metrafenone, belong to two bactericides with different action mechanisms, and the two bactericides are mutually mixed without conflict, so that the bactericidal spectrum is expanded, and the bactericidal efficiency is improved.
2. The active ingredients of the medicine have good synergistic effect in a certain mass ratio range, the control effect is higher than that of a single agent, the dosage is small, the generation of disease resistance is delayed, and the sustainable development of the environment is facilitated.
3. The water dispersible granule has special effect on diseases such as powdery mildew, southern blight, black nevus and the like of grain crops, vegetables and fruit trees, and has good application prospect.
4. The invention optimizes the types and the contents of the auxiliary agents, prepares flutolanil and metrafenone into the water dispersible granules, improves the sterilization effect of the water dispersible granules, improves the adaptability of the medicament to different water qualities, and has wider application area.
5. The water dispersible granule of the embodiment of the invention has higher control effect than a single agent, has small dosage, reduces the residue of the drug in soil and is more beneficial to the sustainable development of the environment.
Detailed Description
The following specific examples are given to illustrate the technical aspects of the present invention in detail, but the present invention is not limited to these examples. Unless otherwise specified, the following components are contained in weight percent.
The embodiment of the invention adopts a method combining indoor toxicity measurement and field test; firstly, 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, and then field efficacy test is carried out on the basis.
Example 1: indoor toxicity determination of flutolanil and metrafenone compound on cucumber powdery mildew
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 'indoor pesticide bioassay test standard bactericide', and the medicament and the EC after mixed use are determined by a pot culture method50The co-toxicity coefficient was calculated by the method proposed by Sun Yunpei et al (1960).
The calculation formula is as follows (taking metrafenone as a standard medicament and the virulence index thereof is 100):
theoretical virulence index (TTI) of M flutolanil TI XPFluoramides+ metrafenone TI XPMetrafenone (BPM)；
In the formula: m is a mixture of flutolanil and metrafenone in different proportions;
PfluoramidesIs the proportion of the flutolanil in the compound composition;
Pmetrafenone (BPM)Is the proportion of metrafenone in the compound composition.
The test results are shown in table 1:
TABLE 1 toxicity test results of flutolanil and metrafenone in different ratios for cucumber powdery mildew
As can be seen from Table 1, EC of flutolanil and metrafenone on powdery mildew of cucumber505.68mg/L and 2.31mg/L respectively. The co-toxicity coefficients of the flutolanil and the metrafenone are respectively 134.59, 154.16, 137.62 and 131.40 which are respectively greater than 120, the mass ratios of the flutolanil to the metrafenone are 1:1, 3:1, 5:1 and 8:1, the co-toxicity coefficients are synergistic, and the co-toxicity coefficients are no synergistic effect when the mass ratios of the flutolanil to the metrafenone are 10:1 or more, so that the mass ratio of the flutolanil to the metrafenone is preferably 1-8:1, more preferably 1-5:1, and most preferably 3: 1.
After determining the mass ratio of the active ingredients, the active ingredients are prepared into water dispersible granules by adopting proper auxiliary agents, and the following specific list is a few representative examples of suspending agents, which are not exhaustive.
The water dispersible granule containing flutolanil and metrafenone and the bulk drugs or the auxiliary agents used in the preparation method thereof can be purchased from the market. Among them, polycarboxylate T-2700 was obtained from Hensmei, alkyl naphthalene sulfonic acid sodium salt formaldehyde polycondensate D-425 was obtained from Acksu, alkyl naphthalene sulfonate Morwet EFW was obtained from Acksuobel, alkyl sulfate REAX WL was obtained from Maidwei Viagrick, and white carbon black was obtained from Shandong Haishi GmbH.
Example 2: 30% flutolanil/metrafenone water dispersible granule
The formula is as follows: 15% of flutolanil serving as a medicinal active ingredient, 15% of metrafenone, 15% of dispersing agent T27003%, D-4251%, wetting agent Morwet EFW 1%, REAX WL 2%, disintegrating agent monopotassium phosphate 1.2%, sodium sulfate 1.8%, chelating agent disodium ethylene diamine tetraacetate 2%, and filler white carbon black added to 100%.
The preparation method comprises the following steps: uniformly mixing flutolanil, metrafenone, a dispersing agent, a wetting agent, a disintegrating agent, a chelating agent and a filler, carrying out ultramicro airflow crushing to obtain particles with the particle size of 680-800 meshes, adding the obtained fine powder, kneading, wherein the water addition amount is 15-30% of the total mass of the materials, carrying out extrusion granulation after kneading, and drying the obtained particles at the temperature of 30-65 ℃ to obtain the flutolanil-metrafenone water dispersible granule product.
Example 3: 50% flutolanil/metrafenone water dispersible granule
The formula is as follows: 35% of flutolanil serving as a medicinal active ingredient, 15% of metrafenone, T-27004.5% of dispersant, D-4251.5% of wetting agent Morwet EFW 1%, REAX WL 2%, 1.2% of disintegrant potassium dihydrogen phosphate, 1.8% of sodium sulfate, 2.5% of chelating agent disodium ethylene diamine tetraacetate and 100% of filler white carbon black.
The preparation method is the same as example 2.
Example 4: 40% flutolanil/metrafenone water dispersible granule
The formula is as follows: 30% of flutolanil serving as a medicinal active ingredient, 10% of metrafenone, T-27003.75% of dispersant, D-4251.25% of dispersant, 1.33% of wetting agent Morwet EFW, 2.67% of REAX WL, 1.6% of potassium dihydrogen phosphate serving as a disintegrating agent, 2.4% of sodium sulfate, 3% of chelating agent disodium ethylene diamine tetraacetate and 100% of filler white carbon black.
The preparation method is the same as example 2.
Example 5: 48% flutolanil/metrafenone water dispersible granule
The formula is as follows: 40% of flutolanil serving as a medicinal active ingredient, 8% of metrafenone, T-27003%, D-4251%, 1.67% of wetting agent Morwet EFW, 3.33% of REAX WL, 2% of potassium dihydrogen phosphate serving as a disintegrant, 3% of sodium sulfate, 2.4% of disodium ethylene diamine tetraacetate serving as a chelating agent and 100% of white carbon black serving as a filler.
The preparation method is the same as example 2.
Example 6: 72% flutolanil/metrafenone water dispersible granule
The formula is as follows: 64 percent of flutolanil serving as a medicinal active ingredient, 8 percent of metrafenone, T-27003 percent of dispersant, D-4251 percent of wetting agent Morwet EFW 1.67 percent, REAX WL 3.33 percent, 2 percent of potassium dihydrogen phosphate serving as a disintegrant, 3 percent of sodium sulfate, 3 percent of disodium ethylene diamine tetraacetate serving as a chelating agent and 100 percent of white carbon black serving as a filler.
The preparation method is the same as example 2.
Example 7: 75% flutolanil/metrafenone water dispersible granule
The formula is as follows: 50% of flutolanil serving as a medicinal active ingredient, 25% of metrafenone, 25% of dispersing agent T-27004.5%, D-4251.5%, 1.67% of wetting agent Morwet EFW, 3.33% of REAX WL, 1.2% of disintegrant potassium dihydrogen phosphate, 1.8% of sodium sulfate, 2.5% of chelating agent disodium ethylene diamine tetraacetate and 100% of filler white carbon black.
The preparation method is the same as example 2.
Example 8: 40% flutolanil/metrafenone water dispersible granule
The formula is as follows: 20 percent of flutolanil, 20 percent of metrafenone, 2 percent of dispersant calcium lignosulfonate, 1 percent of methylene dinaphthalene sodium sulfonate, 2 percent of wetting agent nekal BX, 2 percent of alpha-olefin sodium sulfonate, 0.7 percent of disintegrant urea, 0.3 percent of sodium chloride, 1 percent of chelating agent sodium pyrophosphate and 100 percent of filler corn starch.
The preparation method is the same as example 2.
Example 9: 45% flutolanil/metrafenone water dispersible granule
The formula is as follows: 30% of flutolanil serving as a medicinal active ingredient, 15% of metrafenone, 4% of polycarboxylate serving as a dispersing agent, 3% of sodium alkyl phenol sulfonate, 1% of sodium dodecyl sulfate serving as a wetting agent, 1% of sodium naphthalene sulfonic acid formaldehyde condensate, 3% of ammonium sulfate serving as a disintegrating agent, 5% of sodium chloride, 1.5% of sodium gluconate serving as a chelating agent and 100% of talcum powder serving as a filler.
The preparation method is the same as example 2.
Example 10: 64% flutolanil/metrafenone water dispersible granule
The formula is as follows: 48 percent of flutolanil, 16 percent of metrafenone, 7 percent of dispersant ethylene oxide-propylene oxide block copolymer, 3 percent of sodium alkyl phenol sulfonate, 3 percent of wetting agent lauric acid sulfate, 1 percent of sodium naphthalene sulfonic acid formaldehyde condensate, 3 percent of disintegrant ammonium sulfate, 3 percent of calcium chloride, 4 percent of chelating agent sodium tripolyphosphate and 100 percent of filler diatomite.
The preparation method is the same as example 2.
Example 11: 42% flutolanil/metrafenone water dispersible granule
The formula is as follows: 35 percent of flutolanil, 7 percent of metrafenone, 4 percent of dispersant ethylene oxide-propylene oxide block copolymer, 3 percent of calcium lignosulfonate, 4 percent of wetting agent lauric acid sulfate, 2 percent of lauryl sodium sulfate, 5 percent of disintegrant monopotassium phosphate, 2 percent of calcium chloride, 4 percent of chelating agent ethylene diamine tetraacetic acid disodium salt and 100 percent of filler kaolin.
The preparation method is the same as example 2.
Example 12: 54% flutolanil/metrafenone water dispersible granule
The formula is as follows: 48 percent of flutolanil, 6 percent of metrafenone, 5 percent of dispersant dodecyl polyoxyethylene phosphate, 2 percent of calcium lignosulphonate, 2 percent of wetting agent lauric acid sulfate, 2 percent of Morwet EFW, 2 percent of disintegrant sodium sulfate, 1 percent of calcium chloride, 3 percent of chelating agent disodium ethylene diamine tetraacetate and 100 percent of filler white carbon black.
The preparation method is the same as example 2.
Example 13: 50% flutolanil/metrafenone water dispersible granule
The formula is as follows: 32 percent of flutolanil serving as a medicinal active ingredient, 18 percent of metrafenone, 3 percent of dispersing agent D-4256 percent of methylene dinaphthalene sodium sulfonate, 3 percent of wetting agent lauric acid sulfate, 2 percent of alkyl sulfate, 2 percent of disintegrating agent sodium sulfate, 3 percent of urea, 3.5 percent of chelating agent sodium pyrophosphate and 100 percent of filler white carbon black.
The preparation method is the same as example 2.
Example 14: 40% flutolanil/metrafenone water dispersible granule
The formula is as follows: 30% of flutolanil serving as a medicinal active ingredient, 10% of metrafenone, 3% of a dispersant polyaryl polyoxyethylene ether phosphate alkyl amine salt, 3% of aryl phenol polyoxyethylene ether, 2% of a wetting agent dialkyl succinate sulfonic acid sodium salt, 3% of a fatty acid sulfate, 2% of a disintegrating agent diammonium hydrogen phosphate, 1% of potassium chloride, 2% of chelating agent ethylene diamine tetraacetic acid tetrasodium salt and 100% of filler light calcium carbonate.
The preparation method is the same as example 2.
Example 15: water dispersible granule product detection
The properties of the products obtained in the above examples were measured and the results are shown in Table 2 below. Wherein, the suspension rate of different water qualities (C water: hardness is 500mg/L, pH is 7.0-8.0; 3WHO water: hardness is 1026mg/L, pH is 6.0-7.0) is detected according to CIPAC MT184, the screening (wet screening test) is detected according to CIPAC MT185, and the heat storage stability is determined according to the requirements of solid preparations in GB/T19136.
The disintegration is expressed by measuring the disintegration time, generally specified to be qualified after less than 3min, and the measuring method is as follows: at 25 ℃, adding 0.5g of sample particles into a 100mL stoppered measuring cylinder (the cylinder height is 22.5cm, the inner diameter is 28mm) containing 90mL of distilled water, clamping the middle part of the measuring cylinder, rotating at a constant speed along the center at a speed of 8r/min until the sample is completely disintegrated in the water, and recording the time, namely the disintegration time.
TABLE 2 quality change of water dispersible granule prepared by compounding flutolanil and metrafenone
As can be seen from Table 2, the products of example 14 had poor quality before and after hot storage, the products of examples 8 to 13 had poor quality after hot storage, and the products of examples 2 to 7 using the preferred auxiliaries had good quality both before and after hot storage, from which it can be seen that the preferred auxiliaries play a critical role in product quality.
Furthermore, as can be seen from examples 2-7, in the case of selecting the preferred adjuvant, the performance of the resulting water dispersible granule was similar when the content of the pharmaceutically active ingredient was varied within the range of 30-75%, which indicates that the effect of the drug content on the dosage form performance was less with the preferred adjuvant ingredients and contents. As can be seen from examples 8-13, in the case of using the common auxiliary agent, the performance of the obtained water dispersible granule is relatively poor, and the replacement auxiliary agent has no obvious effect improvement, which shows that the components and content of the preferred auxiliary agent have obvious effect on improving the performance of the flutolanil-metrafenone water dispersible granule, and the common auxiliary agent does not.
Example 16: drug effect test of flutolanil and metrafenone compound preparation for preventing and treating wheat powdery mildew in field
The experiment is carried out in a cold pavilion area of the Weifang city in Shandong province, the soil fertility of the wheat field is medium, and the pH value is 7.2. The initial stage of wheat powdery mildew is positive when the medicine is applied. And selecting 16 wheat planting areas for testing, wherein one wheat planting area is selected as a blank control area, the control area is clear water spray without spraying a medicament, and the other test areas are medicament treatment areas and are sprayed with different water dispersible granules. The application method comprises the following steps: spraying for 2 times by a worker-farm-16 knapsack manual sprayer, mixing the suspending agent with 450kg of water per hectare to prepare liquid medicine, and uniformly spraying according to the amount of the liquid medicine in a cell, wherein the water for preparing the liquid medicine in the test process is 3WH0 water prepared in a laboratory. The first application is carried out in 2018, 4 and 10 months, the second application is carried out at intervals of 7 days, the weather is good during the test period, and the daily average temperature is 15-25.0 ℃.
The disease base is investigated before application, the control effect is investigated 14 days after the application of the 2 nd time, the control effect is calculated, and the safety of the test medicament to crops is observed.
The investigation method comprises the following steps: sampling is carried out at 5 points on the diagonal of each cell, 50 plants are investigated at each point, the disease condition of flag leaves and the 1 st leaf below the flag leaves of each plant is investigated, and the disease condition is recorded leaf by leaf according to the following 9-grade grading standard:
level 0: no disease;
level 1: the lesion area accounts for less than 5% of the whole leaf area;
and 3, level: the lesion area accounts for 6-15% of the whole leaf area;
and 5, stage: the lesion area accounts for 16-25% of the whole leaf area;
and 7, stage: the lesion area accounts for 26-50% of the whole leaf area;
and 9, stage: the lesion area accounts for more than 51% of the whole leaf area.
The drug effect calculation method comprises the following steps:
disease index ═ Σ (number of diseased leaves at each level × corresponding level value)/total number of investigation × 9 × 100;
the control results of wheat powdery mildew are shown in the following table 3:
TABLE 3 field test results of the efficacy of each treatment agent in preventing and treating wheat powdery mildew
As can be seen from the test results in the above table 3, after the flutolanil and the metrafenone are compounded, the wheat powdery mildew can be effectively prevented and treated, the prevention and treatment effect on the wheat powdery mildew 14 days after the last application is obviously better than that of 2 control agents, and the synergistic effect is shown. The control effect of the examples 2 to 7 using the preferred auxiliary agents and the preferred proportion is obviously better than that of other examples. According to the observation of the whole field test process, the wheat grows well within the test dose range, and the pesticide damage phenomenon does not occur in each treatment agent, which indicates that the wheat is safe.
The water dispersible granules containing metrafenone and flutolanil provided by the invention have good synergistic effect, the bactericidal spectrum is expanded, the drug duration is improved, the generation of drug resistance is delayed, and the water dispersible granules have good effect on preventing and treating powdery mildew, southern blight, black nevus and other diseases in food crops, vegetables and fruit trees. In addition, the preparation process of the water dispersible granule product in the embodiment of the invention is environment-friendly, the product quality is excellent, and the application is facilitated.
Claims (10)
1. The water dispersible granule containing metrafenone and flutolanil is characterized by comprising the following components in percentage by weight: 30-75% of a pharmaceutical active ingredient, 3-10% of a dispersing agent, 2-6% of a wetting agent, 1-8% of a disintegrating agent, 1-4% of a chelating agent and the balance of a filler, wherein the pharmaceutical active ingredient is flutolanil and metrafenone in a mass ratio of 1-8: 1.
2. Water dispersible granules according to claim 1, wherein the dispersant is one or more of a polycarboxylate and an alkyl naphthalene sulphonate formaldehyde polycondensate; the wetting agent is one or more of alkyl naphthalene sulfonate and alkyl sulfate; the disintegrating agent is a mixture of potassium dihydrogen phosphate and sodium sulfate.
3. The water dispersible granule according to claim 2, wherein the dispersant is a mixture of polycarboxylate and alkyl naphthalene sulfonate formaldehyde polycondensate in a mass ratio of 3: 1-2; the wetting agent is a mixture of alkyl naphthalene sulfonate and alkyl sulfate in a mass ratio of 1: 1-3; the disintegrating agent is a mixture of monopotassium phosphate and sodium sulfate in a mass ratio of 1: 1-3.
4. Water dispersible granules according to any of claims 1 to 3, wherein the chelating agent is one or more of edetate, pyrophosphate, gluconate and tripolyphosphate; the filler is one or more of corn starch, talcum powder, diatomite, white carbon black and kaolin.
5. The water dispersible granule according to any one of claims 1 to 3, wherein the mass ratio of flutolanil to metrafenone in the pharmaceutically active ingredient is 1-5: 1.
6. The water dispersible granule according to claim 5, wherein the mass ratio of flutolanil to metrafenone in the pharmaceutically active ingredient is 3: 1.
7. Water dispersible granules according to any of claims 1 to 3, wherein the content of the pharmaceutically active ingredient in the water dispersible granules is between 50 and 75%.
8. The water dispersible granule according to claim 7, wherein the dispersant content is 4-6%, the wetting agent content is 3-5%, the disintegrant content is 3-5%, and the chelating agent content is 2-3%.
9. The method for preparing the metrafenone and flutolanil containing water dispersible granule according to any one of claims 1 to 8, comprising the steps of:
mixing flutolanil, metrafenone, a dispersing agent, a wetting agent, a disintegrating agent, a chelating agent and a filler, carrying out ultramicro airflow pulverization to obtain fine powder with the particle size of 680-mesh and 800-mesh, mixing the obtained fine powder with water, kneading, carrying out extrusion granulation after kneading, and drying to obtain the flutolanil-metrafenone water dispersible granule product.
10. The use of the metrafenone and flutolanil-containing water dispersible granule according to any one of claims 1 to 8 for controlling diseases of food crops, vegetables or fruit trees.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010620632.3A CN111587879B (en) | 2020-06-30 | 2020-06-30 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010620632.3A CN111587879B (en) | 2020-06-30 | 2020-06-30 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111587879A CN111587879A (en) | 2020-08-28 |
| CN111587879B true CN111587879B (en) | 2021-09-21 |
Family
ID=72179803
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010620632.3A Active CN111587879B (en) | 2020-06-30 | 2020-06-30 | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111587879B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101945577A (en) * | 2008-02-22 | 2011-01-12 | 巴斯夫欧洲公司 | Fungicidal compositions comprising 3'-bromine-2,3,4,6'-tetramethoxy-2',6-dimethylbenzophenone |
| CN103168780A (en) * | 2013-03-19 | 2013-06-26 | 海利尔药业集团股份有限公司 | Bactericidal composition containing fluopicolide and metrafenone |
| CN105454245A (en) * | 2016-01-19 | 2016-04-06 | 陕西上格之路生物科学有限公司 | Sterilization composition containing metrafenone and fluxapyroxad |
| CN105831122A (en) * | 2016-05-26 | 2016-08-10 | 南京华洲药业有限公司 | Sterilization composition containing fluoride ether bacteria amide and metrafenone and application thereof |
| CN106857510A (en) * | 2017-04-17 | 2017-06-20 | 北京科发伟业农药技术中心 | Fungicidal composition containing metrafenone |
-
2020
- 2020-06-30 CN CN202010620632.3A patent/CN111587879B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101945577A (en) * | 2008-02-22 | 2011-01-12 | 巴斯夫欧洲公司 | Fungicidal compositions comprising 3'-bromine-2,3,4,6'-tetramethoxy-2',6-dimethylbenzophenone |
| CN103168780A (en) * | 2013-03-19 | 2013-06-26 | 海利尔药业集团股份有限公司 | Bactericidal composition containing fluopicolide and metrafenone |
| CN105454245A (en) * | 2016-01-19 | 2016-04-06 | 陕西上格之路生物科学有限公司 | Sterilization composition containing metrafenone and fluxapyroxad |
| CN105831122A (en) * | 2016-05-26 | 2016-08-10 | 南京华洲药业有限公司 | Sterilization composition containing fluoride ether bacteria amide and metrafenone and application thereof |
| CN106857510A (en) * | 2017-04-17 | 2017-06-20 | 北京科发伟业农药技术中心 | Fungicidal composition containing metrafenone |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111587879A (en) | 2020-08-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105191946B (en) | Bactericidal composition and its application | |
| CN109452292A (en) | Bactericidal composition and its application | |
| CN105211075B (en) | Bactericidal composition and its application | |
| CN101828575A (en) | Pyrimidine nucleoside antibiotic and propiconazole compound bactericide | |
| CN111685117B (en) | Bactericidal composition containing metrafenone and flutolanil and application thereof | |
| CN102047889A (en) | Antibacterial composition containing azoxystrobin and cyproconazole and application thereof | |
| CN111587879B (en) | Water dispersible granule containing metrafenone and flutolanil and preparation method and application thereof | |
| CN101194620B (en) | Bactericide agent composition containing tebuconazole | |
| CN101637170A (en) | Difenoconazole-thiram water dispersible granules | |
| CN104351254A (en) | Nikkomycin and azoxystrobin-containing fungicidal composition | |
| CN108782577A (en) | A kind of bactericidal composition and application thereof containing folpet and ZEN 90160 | |
| CN105052995B (en) | A kind of complex composition and preparation containing toxic fluoride phosphate and oxazole series bactericidal agent | |
| CN104542695B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of toxic fluoride phosphate and preparation | |
| CN107047563A (en) | A kind of bactericidal composition for preventing and treating Zizyphus maurtiana powdery mildew | |
| CN105123746B (en) | A kind of complex composition and bactericide containing toxic fluoride phosphate and bromothalonil | |
| CN112772651A (en) | Oligogalacturonic acid and kasugamycin combined bactericide and application thereof | |
| CN111183998A (en) | 8-hydroxyquinoline calcium-containing bactericidal composition for preventing and treating downy mildew and late blight | |
| CN104886122A (en) | Compound composition containing dufulin and pyrazole amide bactericide and bactericide | |
| CN107467025A (en) | A kind of bactericidal composition containing Metalaxyl-M and phosethyl-Al | |
| CN114391545B (en) | Pesticide composition containing bixafen and copper quinolinate and application thereof | |
| CN111820233B (en) | Jiangchuan mycin and ningnanmycin compounded pesticide composition and preparation method and application thereof | |
| CN114766483B (en) | Sterilization composition containing bronopol and application thereof | |
| JPH04257502A (en) | Fungicidal composition for agricultural and horticultural use | |
| CN112021325B (en) | Weeding composition containing metazosulfuron and indanthrone | |
| CN102084865B (en) | Bactericidal composition containing flutriafol and propineb |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A water dispersible granule containing benzophenone and fluoroamide and its preparation method and application Effective date of registration: 20231229 Granted publication date: 20210921 Pledgee: Qingdao Rural Commercial Bank Co.,Ltd. Pingdu Xinhe Branch Pledgor: QINGDAO RUNNONG CHEMICAL CO.,LTD. Registration number: Y2023980075508 |