CN104115854B - A kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester - Google Patents
A kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester Download PDFInfo
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- CN104115854B CN104115854B CN201310146253.5A CN201310146253A CN104115854B CN 104115854 B CN104115854 B CN 104115854B CN 201310146253 A CN201310146253 A CN 201310146253A CN 104115854 B CN104115854 B CN 104115854B
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- Prior art keywords
- bacterium ester
- chlorine nalidixic
- nalidixic bacterium
- disease
- bactericidal composition
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- 241000894006 Bacteria Species 0.000 title claims abstract description 83
- 150000002148 esters Chemical class 0.000 title claims abstract description 80
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000460 chlorine Substances 0.000 title claims abstract description 78
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 78
- MHWLWQUZZRMNGJ-UHFFFAOYSA-N nalidixic acid Chemical compound C1=C(C)N=C2N(CC)C=C(C(O)=O)C(=O)C2=C1 MHWLWQUZZRMNGJ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000000203 mixture Substances 0.000 title claims abstract description 44
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 38
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 18
- 201000010099 disease Diseases 0.000 claims abstract description 56
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims abstract description 56
- 230000000694 effects Effects 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000004480 active ingredient Substances 0.000 claims abstract description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 17
- 241000233679 Peronosporaceae Species 0.000 claims description 17
- 235000009566 rice Nutrition 0.000 claims description 17
- 239000000375 suspending agent Substances 0.000 claims description 17
- 239000003094 microcapsule Substances 0.000 claims description 14
- 241000221785 Erysiphales Species 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 12
- 239000004563 wettable powder Substances 0.000 claims description 9
- 206010039509 Scab Diseases 0.000 claims description 8
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 241001530056 Athelia rolfsii Species 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000004562 water dispersible granule Substances 0.000 claims description 7
- 239000004530 micro-emulsion Substances 0.000 claims description 6
- 240000007594 Oryza sativa Species 0.000 claims 1
- OIPMQULDKWSNGX-UHFFFAOYSA-N bis[[ethoxy(oxo)phosphaniumyl]oxy]alumanyloxy-ethoxy-oxophosphanium Chemical compound [Al+3].CCO[P+]([O-])=O.CCO[P+]([O-])=O.CCO[P+]([O-])=O OIPMQULDKWSNGX-UHFFFAOYSA-N 0.000 abstract description 15
- LDVVMCZRFWMZSG-OLQVQODUSA-N (3ar,7as)-2-(trichloromethylsulfanyl)-3a,4,7,7a-tetrahydroisoindole-1,3-dione Chemical compound C1C=CC[C@H]2C(=O)N(SC(Cl)(Cl)Cl)C(=O)[C@H]21 LDVVMCZRFWMZSG-OLQVQODUSA-N 0.000 abstract description 14
- 239000005745 Captan Substances 0.000 abstract description 14
- 229940117949 captan Drugs 0.000 abstract description 14
- 239000005764 Dithianon Substances 0.000 abstract description 13
- PYZSVQVRHDXQSL-UHFFFAOYSA-N dithianon Chemical compound S1C(C#N)=C(C#N)SC2=C1C(=O)C1=CC=CC=C1C2=O PYZSVQVRHDXQSL-UHFFFAOYSA-N 0.000 abstract description 13
- 230000000855 fungicidal effect Effects 0.000 abstract description 4
- 238000001228 spectrum Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 238000013329 compounding Methods 0.000 description 25
- 238000012360 testing method Methods 0.000 description 19
- 230000003449 preventive effect Effects 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 241000209094 Oryza Species 0.000 description 16
- 239000003814 drug Substances 0.000 description 14
- 239000002270 dispersing agent Substances 0.000 description 13
- 239000012071 phase Substances 0.000 description 13
- 239000013530 defoamer Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 239000000575 pesticide Substances 0.000 description 12
- 235000002566 Capsicum Nutrition 0.000 description 11
- 239000006002 Pepper Substances 0.000 description 10
- 241000722363 Piper Species 0.000 description 10
- 235000016761 Piper aduncum Nutrition 0.000 description 10
- 235000017804 Piper guineense Nutrition 0.000 description 10
- 235000008184 Piper nigrum Nutrition 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 239000003995 emulsifying agent Substances 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 240000008067 Cucumis sativus Species 0.000 description 8
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 8
- 230000002528 anti-freeze Effects 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 8
- 239000002562 thickening agent Substances 0.000 description 8
- 231100000820 toxicity test Toxicity 0.000 description 8
- 239000000080 wetting agent Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 6
- 240000003768 Solanum lycopersicum Species 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 206010067482 No adverse event Diseases 0.000 description 5
- 239000008346 aqueous phase Substances 0.000 description 5
- 229940079593 drug Drugs 0.000 description 5
- PCCSBWNGDMYFCW-UHFFFAOYSA-N 5-methyl-5-(4-phenoxyphenyl)-3-(phenylamino)-1,3-oxazolidine-2,4-dione Chemical compound O=C1C(C)(C=2C=CC(OC=3C=CC=CC=3)=CC=2)OC(=O)N1NC1=CC=CC=C1 PCCSBWNGDMYFCW-UHFFFAOYSA-N 0.000 description 4
- 206010011732 Cyst Diseases 0.000 description 4
- 239000005772 Famoxadone Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 208000031513 cyst Diseases 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 238000013401 experimental design Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 229920002521 macromolecule Polymers 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000001629 suppression Effects 0.000 description 4
- 230000001018 virulence Effects 0.000 description 4
- 230000008485 antagonism Effects 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003002 pH adjusting agent Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 235000009754 Vitis X bourquina Nutrition 0.000 description 2
- 235000012333 Vitis X labruscana Nutrition 0.000 description 2
- 240000006365 Vitis vinifera Species 0.000 description 2
- 235000014787 Vitis vinifera Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- ASDRZZPTJLDISZ-UHFFFAOYSA-N chlorine;pyridine Chemical compound [Cl].C1=CC=NC=C1 ASDRZZPTJLDISZ-UHFFFAOYSA-N 0.000 description 2
- 239000007884 disintegrant Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000000417 fungicide Substances 0.000 description 2
- 230000009036 growth inhibition Effects 0.000 description 2
- GTCAXTIRRLKXRU-UHFFFAOYSA-N methyl carbamate Chemical compound COC(N)=O GTCAXTIRRLKXRU-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000085543 Acourtia wrightii Species 0.000 description 1
- 240000008574 Capsicum frutescens Species 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- 241000219112 Cucumis Species 0.000 description 1
- 235000015510 Cucumis melo subsp melo Nutrition 0.000 description 1
- YPHMISFOHDHNIV-FSZOTQKASA-N Cycloheximide Natural products C1[C@@H](C)C[C@H](C)C(=O)[C@@H]1[C@H](O)CC1CC(=O)NC(=O)C1 YPHMISFOHDHNIV-FSZOTQKASA-N 0.000 description 1
- -1 Cycloheximide triazole Chemical class 0.000 description 1
- 102100025287 Cytochrome b Human genes 0.000 description 1
- 102100030497 Cytochrome c Human genes 0.000 description 1
- 108010075028 Cytochromes b Proteins 0.000 description 1
- 108010075031 Cytochromes c Proteins 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000510928 Erysiphe necator Species 0.000 description 1
- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 description 1
- 241000233614 Phytophthora Species 0.000 description 1
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- IHYVOJBVNJQSAY-UHFFFAOYSA-N anthracene-9,10-dione oxalonitrile Chemical compound C1=CC=CC=2C(C3=CC=CC=C3C(C12)=O)=O.N#CC#N IHYVOJBVNJQSAY-UHFFFAOYSA-N 0.000 description 1
- 230000010165 autogamy Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000001390 capsicum minimum Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 208000010801 foot rot Diseases 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 210000003470 mitochondria Anatomy 0.000 description 1
- 230000002438 mitochondrial effect Effects 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- RXJKFRMDXUJTEX-UHFFFAOYSA-N triethylphosphine Chemical compound CCP(CC)CC RXJKFRMDXUJTEX-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester, active ingredient is active components A and active component B, and active components A is selected from chlorine nalidixic bacterium ester, and active component B is selected from any one following compound：Phosethyl-Al, captan, dithianon, famoxadones, and active components A and active component B weight ratio are 1:80~60:1.The present composition has greater activity to the multiple diseases in various crop, and has obvious synergistic effect, expands fungicidal spectrum.And with the characteristics of dosage is small, resistance of rainwater washing against, and synergy is obvious.
Description
Technical field
The invention belongs to technical field of pesticide, is related to a kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester in crop disease
Application.
Technical background
Chlorine nalidixic bacterium ester：Molecular formula is C15H13Cl3N2O4, chemical name is N- methoxyl groups-N- [2- [[(3,5,6- trichlorine pyrroles
Pyridine -2- bases) oxygen] methyl] phenyl] methyl carbamate, belong to carbamate fungicide, outward appearance is pale solid, with
The mechanism of action of other methoxy acrylic bactericides is the same, and chlorine nalidixic bacterium ester is also mitochondrial respiratory inhibitor, that is,
Cause to imitate by suppressing the breathing of electronics transfer Mitochondria between cytochrome b and c.
Phosethyl-Al, captan, dithianon are widely used in crops He famoxadone belongs to common fungicide
Disease on, wherein phosethyl-Al also known as Yimeiling, aliette, mould spirit, gram bacterium spirit, downy mildew spirit, phytophthora be net or phosphoric acid second
Ester aluminium.
In the real process of agricultural production, controlling disease is easiest to generate the problem that the drug-fast generation of germ.No
Compounded with kind composition, be to prevent and treat the very common method of resistance germ.Heterogeneity is compounded, and is imitated according to practical application
Fruit, to judge that certain compounding is synergy plus and or antagonism.In most cases, the compounding effect of agricultural chemicals is all to add
And effect, really have that the compounding of synergistic effect is seldom, especially synergistic effect clearly, the very high compounding of synergy ratio just more
It is few.Studied by inventor, find mutually to compound chlorine nalidixic bacterium ester and effective active composition B, had within the specific limits very well
Synergistic effect, and about chlorine nalidixic bacterium ester and phosethyl-Al, captan, dithianon, famoxadones related compounding, at present
At home and abroad there is not yet relevant report.
The content of the invention
The purpose of the present invention is to propose to it is a kind of with synergistic function, use cost is low, preventive effect is good contains chlorine nalidixic bacterium ester
Synergistic bactericidal composition.
A kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester, active ingredient are active components A and active component B, activity into
It is 1 to divide A and active component B weight ratio:80~60:1, described active components A is selected from chlorine nalidixic bacterium ester, and active component B is selected from three
One kind in fosetyl-aluminium, captan, dithianon, famoxadones, active components A and active component B preferred weight ratio are
1:60~40:1；More preferably：The weight of chlorine nalidixic bacterium ester and phosethyl-Al ratio is 1:35~5:1, chlorine nalidixic bacterium ester and captan
Weight ratio be 1:30~10:1, the weight ratio of chlorine nalidixic bacterium ester and dithianon is 1:25~15:1, chlorine nalidixic bacterium ester Yu oxazole bacterium
The weight ratio of ketone is 1:20~20:1；Most preferably：The weight of chlorine nalidixic bacterium ester and phosethyl-Al ratio is 1:24~1:4, chlorine pyridine
The weight of bacterium ester and captan ratio is 1:19~1:1, the weight ratio of chlorine nalidixic bacterium ester and dithianon is 1:14~4:1, chlorine pyridine bacterium
The weight ratio of Zhi Yu famoxadones is 1:9~9:1.
The described Synergistic bactericidal composition containing chlorine nalidixic bacterium ester, is made wettable powder, water dispersible granules, suspending agent, water
Emulsion, microemulsion, microcapsule suspending agent or microcapsule suspension-suspendinagent agent.
The described Synergistic bactericidal composition containing chlorine nalidixic bacterium ester is used for the disease for preventing and treating crops, and described crops include
Cereal crops, legume crop, oil crops, fibre crops, sugar crop, melon crop, fruits crop, dry fruit crop,
Have a liking for crop, root crop, flower crop, medicinal crop, crop and green manure pasture crop.
Described disease include sclerotiniose, powdery mildew, false smut, rice blast, banded sclerotial blight, downy mildew, gray mold, epidemic disease,
Leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease, rust, glume blight or net blotch.
The amount of application when content of active component depends on being used alone in the bactericidal composition of the present invention, also depends on one
The mixed ratio and synergistic effect degree of kind compound and another compound, at the same it is also relevant with target disease.Usual group
The weight percentage of active component is the 1%~90% of gross weight, preferably 5%~80% in compound.According to different preparations
Type, active component content scope are different.Generally, liquid preparation contains by weight 1%~60% active material, compared with
It is 5%~50% goodly；Solid pharmaceutical preparation contains by weight 5%~80% active material, preferably 10%~80%.
The present invention bactericidal composition at least contain a kind of surfactant, in favor of administration when active component in water
It is scattered.Surface-active contents are the 2%~30% of total formulation weight, and surplus is solid or liquid diluent.
Surfactant selected by the bactericidal composition of the present invention is known in those skilled in the art, by user
Through dilution or directly using its preparation before use, it can be prepared, will lived by processing method known in those skilled in the art
After property composition mixes with liquid flux or solid carrier, surfactant such as dispersant, stabilizer, wetting agent, bonding are added
One or more in agent, defoamer etc..
Composition includes following component and content when wettable powder is made：Active components A 0.5%~60%, active component
B0.5%~80%, dispersant 1%~12%, wetting agent 1%~8%, filler surplus.
Composition includes following component and content when water dispersible granules are made：Active components A 0.5%~60%, active component
B0.5%~80%, dispersant 1%~12%, wetting agent 1%~8%, disintegrant 1%~10%, binding agent 0~8%, filler surplus.
Composition includes following component and content when suspending agent is made：Active components A 0.5%~50%, active component
B0.5%~50%, dispersant 1%~10%, wetting agent 1%~10%, defoamer 0.01%~2%, thickener 0~2%, antifreeze 0~
8%th, deionized water adds to 100%.
Composition includes following component and content when suspension emulsion is made：Active components A 0.5%~50%, active component
B0.5%~50%, emulsifying agent 1%~10%, dispersant 1%~10%, solvent 0~20%, defoamer 0.01%~2%, thickener 0~
2%th, antifreeze 0~8%, stabilizer 0~3%, deionized water add to 100%.
Composition includes following component and content when aqueous emulsion is made：Active components A 0.5%~50%, active component
B0.5%~50%, solvent 1%~20%, emulsifying agent 1%~12%, antifreeze 0~8%, defoamer 0.01%~2%, thickener 0~2%,
Deionized water adds to 100%.
Composition includes following component and content when microemulsion is made：Active components A 0.5%~50%, active component
B0.5%~50%, emulsifying agent 3%~25%, solvent 1%~10%, antifreeze 0~8%, stabilizer 0~3%, defoamer 0.01%~2%,
Deionized water adds to 100%.
Composition includes following component and content when microcapsule suspending agent is made：Active components A 0.5%~50%, active component
B0.5%~50%, macromolecule cyst material 1%~10%, dispersant 2%~10%, solvent 1%~10%, emulsifying agent 1%~7%, pH are adjusted
Section agent 0.01%~5%, defoamer 0.01%~2%, deionized water add to 100%.
Composition includes following component and content when microcapsule suspension-suspendinagent agent is made：Active components A 0.5%~50%, live
Property composition B0.5%~50%, macromolecule cyst material 1%~12%, dispersant 1%-12%, wetting agent 1%-8%, solvent 1%~15%,
Emulsifying agent 1%~8%, defoamer 0.01%~2%, thickener 0~2%, pH adjusting agent 0.01%~5%, deionized water add to 100%.
The wettable powder the key technical indexes of the present invention：
The water dispersible granules the key technical indexes of the present invention：
The suspending agent the key technical indexes of the present invention：
The suspension emulsion the key technical indexes of the present invention：
The aqueous emulsion the key technical indexes of the present invention：
The microemulsion the key technical indexes of the present invention：
The microcapsule suspending agent the key technical indexes of the present invention：
The microcapsule suspension-suspendinagent agent the key technical indexes of the present invention：
The advantage of the invention is that：（1）The present composition has good synergy and lasting effect within the specific limits, prevents
Effect is higher than single dose；（2）Pesticide usage amount is reduced, and is reduced residual quantity of the agricultural chemicals on crop, is mitigated environmental pollution；（3）Expand
Fungicidal spectrum, to multiple diseases such as sclerotiniose, powdery mildew, false smut, rice blast, banded sclerotial blight, downy mildew, gray mold, epidemic disease, leaf mold
The disease such as disease, resin disease, anthracnose, scab, ring spot, base rot disease, rust, glume blight or net blotch has special efficacy.
Embodiment
With reference to embodiment to further instruction of the present invention, the percentage in embodiment is weight percentage, but
The invention is not limited in this.
Application Example one
The wettable powder of embodiment 1~13
Chlorine nalidixic bacterium ester, active ingredient B, dispersant, wetting agent, filler are mixed, are well mixed in mixed cylinder, through air-flow
Pulverizer remixes uniformly after crushing, you can wettable powder product of the present invention is made.Specifically it is shown in Table 1.
The each component of 1 embodiment of table 1~13 and content
The water dispersible granules of embodiment 14~26
By chlorine nalidixic bacterium ester, active component B, dispersant, wetting agent, binding agent（Can add to be not added with）, disintegrant, filler together
The particle diameter needed through air-flow crushing, obtain materials of pelletizing.Item is quantified and is sent into fluidized bed granulating dryer by system
After grain and drying, water dispersible granules product of the present invention is made.Specifically it is shown in Table 2.
The each component of 2 embodiment of table 14~26 and content
The suspending agent of embodiment 27~39
By dispersant, wetting agent, defoamer, thickener（Can add to be not added with）, antifreeze（Can add to be not added with）By at a high speed
Shear-mixed is uniform, adds chlorine nalidixic bacterium ester, active component B, and surplus is supplied with deionized water, and ball milling 2~3 is small in ball mill
When, make diameter of particle all below 5 μm, suspending agent product of the present invention is made.Specifically it is shown in Table 3.
The each component of 3 embodiment of table 27~39 and content
The suspension emulsion of embodiment 40~44
By dispersant, defoamer, thickener in above-mentioned formulation material（Can add to be not added with）, antifreeze（Can add to be not added with）, warp
It is uniform to cross high speed shear-mixed, add chlorine nalidixic bacterium ester, ball milling 2~3 hours in ball mill, make diameter of particle all 5 μm with
Under, chlorine nalidixic bacterium ester suspending agent is made, it is then that active component B, solvent, emulsifying agent and various auxiliary agents is directly newborn with high speed agitator
Change into suspending agent, suspension emulsion product of the present invention is made.Specifically it is shown in Table 4.
The each component of 4 embodiment of table 40~44 and content
The aqueous emulsion of embodiment 45~49
Chlorine nalidixic bacterium ester, solvent, emulsifying agent are added together, make to be dissolved into homogeneous oil phase；Active component B, by deionized water,
Antifreeze（Can add to be not added with）, thickener（Can add to be not added with）, defoamer mix, into homogeneous aqueous phase.In high-speed stirred
Under, aqueous phase is added into oil phase, aqueous emulsion product of the present invention is made.Specifically it is shown in Table 5.
The each component of 5 embodiment of table 45~49 and content
The microemulsion of embodiment 50~54
By chlorine nalidixic bacterium ester, active component B, solvent, emulsifying agent, antifreeze（Can add to be not added with）, defoamer is sufficiently mixed into
The oil phase of homogeneous transparent, deionized water is slowly added under agitation, form WO emulsion, then agitated heating, be allowed to
Rapid phase inversion is cooled to room temperature and makes up to balance, filtered, surplus is supplied with deionized water into oil-in-water type；It can be prepared by this
The described microemulsion product of invention, is specifically shown in Table 6.
The each component of 6 embodiment of table 50~54 and parts by weight
Active component B phosethyl-Als, captan, dithianon, famoxadones in table 1~6 are exchanged, brand-new can be made
Agent.
Embodiment 55,56 microcapsule suspending agents
Chlorine nalidixic bacterium ester, active component B, macromolecule cyst material, solvent are mixed, makes to be dissolved into homogeneous oil phase, is shearing
Under the conditions of, by oil phase be added to containing emulsifying agent, pH adjusting agent, dispersant aqueous phase solution in, surplus is supplied with deionized water,
Two kinds of materials react in oil-water interfaces, form high score ascus wall, the well dispersed microcapsule suspension of the present composition is made
Agent product.Specifically it is shown in Table 7.
The embodiment 55 of table 7,56 each components and parts by weight
Embodiment 57,58 microcapsule suspension-suspendinagent agents
Active component B, macromolecule cyst material, solvent are mixed, make to be dissolved into homogeneous oil phase, by oil phase in shearing condition
Under be added to containing emulsifying agent, pH adjusting agent aqueous phase solution in, well dispersed microcapsule suspending agent is made.By dispersant, wet
Moisten agent, defoamer, thickener（Can add to be not added with）It is well mixed by high speed shear, adds chlorine nalidixic bacterium ester, the ball in ball mill
Mill 2~3 hours, makes diameter of particle all below 5 μm, and suspending agent is made, suspending agent then is added into micro-capsule suspension
Aqueous phase solution in, deionized water supplies surplus, and the well dispersed microcapsule suspension-suspendinagent agent product of the present composition is made,
Specifically it is shown in Table 8.
The embodiment 57 of table 8,58 each components and parts by weight
The embodiment of the present invention is the method being combined using Toxicity Determination and field test.First pass through indoor virulence survey
Calmly, the synergy ratio after clear and definite two kinds of medicaments compound by a certain percentage（SR）, SR ＜ 0.5 are antagonism, 0.5≤SR≤1.5
For summation action, SR ＞ 1.5 are synergistic effect, on this basis, then carry out field test.
Test method:After prerun determines the effective inhibition concentration scope of each medicament, medicament sets 5 respectively by active constituent content
Individual dosage processing, if clear water compares.Reference《Farm-chemical indoor determination test rule bactericide》Carry out, using mycelial growth speed
Rate method determines virulence of the medicament to crop germ.Colony diameter is measured with crossing method after 72h, calculates the net growth of each processing
Amount, mycelial growth inhibition rate.
Net growth（mm）=measurement colony diameter -5
Mycelial growth inhibition rate is converted into probit value（y）, liquor strength（μg/mL）It is converted into logarithm value（x）, with minimum
Square law tries to achieve virulence regression equation（y=a+bx）, and thus calculate the EC of every kind of medicament50Value.Simultaneously according to Wadley method meters
Calculate two medicament different ratio synergy ratios（SR）, SR ＜ 0.5 are antagonism, and 0.5≤SR≤1.5 are summation action, SR
＞ 1.5 is synergistic effect.Calculation formula is as follows:
Wherein:A, b is respectively active components A and active component B ratio shared in combination；
A is chlorine nalidixic bacterium ester；
B is selected from one of phosethyl-Al, captan, dithianon, famoxadones kind.
Virulence experiment part：Test medicine provides by Shaanxi Meibang Pesticide Co., Ltd..
Application Example two：
For trying disease：Rice blast；
Experimental design：Effective suppression of chlorine nalidixic bacterium ester and both phosethyl-Als different ratio mixture is determined by pilot study
Concentration range processed.
Toxicity test result
The chlorine nalidixic bacterium ester of table 9 compounds the toxicity test analysis of results table to rice blast with phosethyl-Al
As shown in Table 9, chlorine nalidixic bacterium ester prevents and treats the proportioning of rice blast 1 with phosethyl-Al compounding:80~60:When 1,
Synergy ratio SR is all higher than 1.5, illustrates both 1:80~60:Mixture shows synergistic effect in the range of 1, chlorine nalidixic bacterium ester with
The proportioning of phosethyl-Al is 1:35~5: 1, synergistic effect is more prominent, and synergy ratio is all higher than 2.30, chlorine nalidixic bacterium ester and three
Fosetyl-aluminium weight ratio is 1:Synergy ratio is maximum when 14, and synergistic effect is the most obvious.Test and find through applicant, chlorine nalidixic bacterium ester
Proportioning with phosethyl-Al is 5 ︰ 1,4 ︰ 1,3 ︰ 1,2 ︰ 1,1 ︰ 1,1 ︰ 2,1 ︰ 3,1 ︰ 4,1 ︰ 5,1 ︰ 6,1 ︰ 7,1 ︰ 8,1 ︰ 9,1 ︰
10th, 1 ︰ 11,1 ︰ 12,1 ︰ 13,1 ︰ 14,1 ︰ 15,1 ︰ 16,1 ︰ 17,1 ︰ 18,1 ︰ 19,1 ︰ 20,1 ︰ 21,1 ︰ 22,1 ︰ 23,1 ︰ 24,1 ︰
25th, it is bent to sclerotiniose, powdery mildew, rice when 1 ︰ 26,1 ︰ 27,1 ︰ 28,1 ︰ 29,1 ︰ 30,1 ︰ 31,1 ︰ 32,1 ︰ 33,1 ︰ 34,1 ︰ 35
Disease, rice blast, banded sclerotial blight, downy mildew, gray mold, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, brown foot rot
The preventing and treating of disease, rust, glume blight or net blotch has obvious synergistic effect, and synergy ratio is more than 1.5.
Application Example three：
For trying disease：Pepper anthracnose；
Experimental design：Determine that the effectively suppression of chlorine nalidixic bacterium ester and both captans different ratio mixture is dense by pilot study
Spend scope.
Toxicity test result
The chlorine nalidixic bacterium ester of table 10 compounds the toxicity test analysis of results table to pepper anthracnose with captan
As shown in Table 10, chlorine nalidixic bacterium ester prevents and treats the proportioning of pepper anthracnose 1 with captan compounding:80~60:When 1, increase
Effect ratio SR is all higher than 1.5, illustrates both 1:80~60:Mixture shows synergistic effect in the range of 1, chlorine nalidixic bacterium ester with gram
The red proportioning of bacterium is 1:30~10: 1, synergistic effect is more prominent, and synergy ratio is all higher than 2.30, chlorine nalidixic bacterium ester and captan weight
Amount is than being 1:Synergy ratio is maximum when 7, and synergistic effect is the most obvious.Test and find through applicant, chlorine nalidixic bacterium ester and captan
Match for 10 ︰ 1,9 ︰ 1,8 ︰ 1,7 ︰ 1,6 ︰ 1,5 ︰ 1,4 ︰ 1,3 ︰ 1,2 ︰ 1,1 ︰ 1,1 ︰ 2,1 ︰ 3,1 ︰ 4,1 ︰ 5,1 ︰ 6,1 ︰ 7,1 ︰ 8,
1 ︰ 9,1 ︰ 10,1 ︰ 11,1 ︰ 12,1 ︰ 13,1 ︰ 14,1 ︰ 15,1 ︰ 16,1 ︰ 17,1 ︰ 18,1 ︰ 19,1 ︰ 20,1 ︰ 21,1 ︰ 22,1 ︰ 23,1 ︰
24th, to sclerotiniose, powdery mildew, false smut, rice blast, banded sclerotial blight, downy mildew when 1 ︰ 25,1 ︰ 26,1 ︰ 27,1 ︰ 28,1 ︰ 29,1 ︰ 30
Disease, gray mold, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease, rust, glume blight or filigree
The preventing and treating of disease has obvious synergistic effect, and synergy ratio is more than 1.5.
Application Example four：
For trying disease：Pepper anthracnose；
Experimental design：Effective suppression of chlorine nalidixic bacterium ester and both dithianons different ratio mixture is determined by pilot study
Concentration range.
Toxicity test result
The chlorine nalidixic bacterium ester of table 11 compounds the toxicity test analysis of results table to pepper anthracnose with dithianon
As shown in Table 11, chlorine nalidixic bacterium ester prevents and treats the proportioning of pepper anthracnose 1 with dithianon compounding:80~60:When 1,
Synergy ratio SR is all higher than 1.5, illustrates both 1:80~60:Mixture shows synergistic effect in the range of 1, chlorine nalidixic bacterium ester with
The proportioning of dithianon is 1:25~15: 1, synergistic effect is more prominent, and synergy ratio is all higher than 2.35, chlorine nalidixic bacterium ester and two
Cyanogen anthraquinone weight ratio is 1:Synergy ratio is maximum when 5, and synergistic effect is the most obvious.Through applicant test find, chlorine nalidixic bacterium ester with
The proportioning of dithianon is 15 ︰ 1,14 ︰ 1,13 ︰ 1,12 ︰ 1,11 ︰ 1,10 ︰ 1,9 ︰ 1,8 ︰ 1,7 ︰ 1,6 ︰ 1,5 ︰ 1,4 ︰ 1,3 ︰ 1,2
︰ 1,1 ︰ 1,1 ︰ 2,1 ︰ 3,1 ︰ 4,1 ︰ 5,1 ︰ 6,1 ︰ 7,1 ︰ 8,1 ︰ 9,1 ︰ 10,1 ︰ 11,1 ︰ 12,1 ︰ 13,1 ︰ 14,1 ︰ 15,1 ︰ 16,1 ︰
17th, to sclerotiniose, powdery mildew, false smut, rice blast, line when 1 ︰ 18,1 ︰ 19,1 ︰ 20,1 ︰ 21,1 ︰ 22,1 ︰ 23,1 ︰ 24,1 ︰ 25
Rot, downy mildew, gray mold, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease, rust, grain husk are withered
The preventing and treating of disease or net blotch has obvious synergistic effect, and synergy ratio is more than 1.5.
Application Example five：
For trying disease：Cucumber downy mildew；
Experimental design：Effective suppression of both chlorine nalidixic bacterium ester Yu famoxadones different ratio mixture is determined by pilot study
Concentration range.
Toxicity test result
The chlorine nalidixic bacterium ester Yu famoxadones of table 12 compound the toxicity test analysis of results table to cucumber downy mildew
As shown in Table 12, the proportioning of chlorine nalidixic bacterium ester Yu famoxadones compounding preventing and treating cucumber downy mildew is 1:80~60:When 1,
Synergy ratio SR is all higher than 1.5, illustrates both 1:80~60:Mixture shows synergistic effect in the range of 1, chlorine nalidixic bacterium ester with
The proportioning of famoxadone is 1:20~20: 1, synergistic effect is more prominent, and synergy ratio is all higher than 2.30, chlorine nalidixic bacterium ester Yu Evil
Cycloheximide triazole weight ratio is 2:Synergy ratio is maximum when 3, and synergistic effect is the most obvious.Through applicant test find, chlorine nalidixic bacterium ester with
The proportioning of famoxadone is 20 ︰ 1,19 ︰ 1,18 ︰ 1,17 ︰ 1,16 ︰ 1,15 ︰ 1,14 ︰ 1,13 ︰ 1,12 ︰ 1,11 ︰ 1,10 ︰ 1,9 ︰ 1,8
︰ 1,7 ︰ 1,6 ︰ 1,5 ︰ 1,4 ︰ 1,3 ︰ 1,2 ︰ 1,1 ︰ 1,2 ︰ 3,1 ︰ 2,1 ︰ 3,1 ︰ 4,1 ︰ 5,1 ︰ 6,1 ︰ 7,1 ︰ 8,1 ︰ 9,1 ︰ 10,1 ︰
11st, to sclerotiniose, powdery mildew, false smut, rice blast when 1 ︰ 12,1 ︰ 13,1 ︰ 14,1 ︰ 15,1 ︰ 16,1 ︰ 17,1 ︰ 18,1 ︰ 19,1 ︰ 20
Disease, banded sclerotial blight, downy mildew, gray mold, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease, rust
The preventing and treating of disease, glume blight or net blotch has obvious synergistic effect, and synergy ratio is more than 1.5.Effect experiment part：Examination
Test medicament to research and develop, provide by Shaanxi Meibang Pesticide Co., Ltd., compare 15% chlorine nalidixic bacterium ester missible oil（Autogamy）, 40% triethylphosphine acid
Aluminium wettable powder（It is purchased in market）, 50% captan wettable powder（It is purchased in market）, 75% dithianon wettable powder（It is purchased in market）、
6.25% famoxadone water dispersible granules（It is purchased in market).The state of an illness is investigated before medicine, in state of an illness first time at initial stage dispenser, altogether dispenser 1 time.
Application Example six：
Chlorine nalidixic bacterium ester and active component B and its compounding preventing and treating powdery mildew of cucumber test of pesticide effectiveness, this experimental arrangement is in Shaanxi Province
Xi'an suburban area, 2 days after dispenser, disease index is investigated respectively and calculates preventive effect within 10 days, 30 days.Experimental result is as follows：
The chlorine nalidixic bacterium ester of table 13 and active component B and its compounding preventing and treating powdery mildew of cucumber test of pesticide effectiveness
As can be seen from Table 13, chlorine nalidixic bacterium ester is prevented and treated with can effectively prevent and treat powdery mildew of cucumber after active component B and its compounding
Effect more than 97%, better than the preventive effect of single dose, and grow, and can prevent and treat cucumber downy mildew and cucumber anthracnose by preventive effect phase,
Target crop is had no adverse effects in experiment scope of medication.
Application Example seven：
Chlorine nalidixic bacterium ester and active component B and its compounding preventing and treating rice blast test of pesticide effectiveness, this experimental arrangement is in Shaanxi Province
Hanzhong City, 2 days after dispenser, disease index is investigated respectively and calculates preventive effect within 10 days, 30 days.Experimental result is as follows：
The chlorine nalidixic bacterium ester of table 14 and active component B and its compounding preventing and treating rice blast test of pesticide effectiveness
As can be seen from Table 14, chlorine nalidixic bacterium ester is prevented and treated with can effectively prevent and treat rice blast after active component B and its compounding
Effect more than 97%, better than the preventive effect of single dose, and grow, and can prevent and treat rice green smut and rice sheath blight disease by preventive effect phase,
Target crop is had no adverse effects in experiment scope of medication.
Application Example eight：
Chlorine nalidixic bacterium ester and active component B and its compounding preventing and treating pepper anthracnose test of pesticide effectiveness, this experimental arrangement is in Shaanxi Province
Xi'an, 2 days after dispenser, disease index is investigated respectively and calculates preventive effect within 10 days, 30 days.Experimental result is as follows：
The chlorine nalidixic bacterium ester of table 15 and active component B and its compounding preventing and treating pepper anthracnose test of pesticide effectiveness
As can be seen from Table 15, chlorine nalidixic bacterium ester is prevented and treated with can effectively prevent and treat pepper anthracnose after active component B and its compounding
Effect more than 97%, better than the preventive effect of single dose, and grow, and can prevent and treat pepper powdery mildew and capsicum epidemic disease by preventive effect phase,
Target crop is had no adverse effects in experiment scope of medication.
Application Example nine：
Chlorine nalidixic bacterium ester and active component B and its compounding preventing and treating downy mildew of garpe test of pesticide effectiveness, this experimental arrangement is in Shaanxi Province
Weinan City Dali County, 2 days after dispenser, disease index is investigated respectively and calculates preventive effect within 10 days, 30 days.Experimental result is as follows：
The chlorine nalidixic bacterium ester of table 16 and active component B and its compounding preventing and treating downy mildew of garpe test of pesticide effectiveness
As can be seen from Table 16, chlorine nalidixic bacterium ester is prevented and treated with can effectively prevent and treat downy mildew of garpe after active component B and its compounding
Effect is more than 97%, and better than the preventive effect of single dose, and preventive effect phase is grown, and can prevent and treat uncinula necator, grape grey mould and
Grape epidemic disease, target crop is had no adverse effects in experiment scope of medication.
Application Example ten：
Chlorine nalidixic bacterium ester and active component B and its compounding preventing and treating tomato blight test of pesticide effectiveness, this experimental arrangement is in Shaanxi Province Weihe
Nanshi Dali County, 2 days after dispenser, disease index is investigated respectively and calculates preventive effect within 10 days, 30 days.Experimental result is as follows：
The chlorine nalidixic bacterium ester of table 17 and active component B and its compounding preventing and treating tomato blight test of pesticide effectiveness
As can be seen from Table 17, chlorine nalidixic bacterium ester is with can effectively prevent and treat tomato blight, preventing and treating effect after active component B and its compounding
Fruit more than 97%, better than the preventive effect of single dose, and grow, and can be with tomato downy mildew, graw mold of tomato and tomato leaf by preventive effect phase
Mildew, target crop is had no adverse effects in experiment scope of medication.
The experiment by different places throughout the country is drawn afterwards, chlorine nalidixic bacterium ester and phosethyl-Al, captan, dicyan anthracene
To the sclerotiniose in various crop, powdery mildew, false smut, rice blast, banded sclerotial blight, downy mildew, grey mold after Kun, famoxadones compounding
Disease, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease, rust, glume blight or net blotch etc. are common
The preventive effect of disease is obvious better than single dose preventive effect, synergistic effect more than 97%.
Claims (6)
1. a kind of Synergistic bactericidal composition containing chlorine nalidixic bacterium ester, active ingredient is active components A and active component B, and its feature exists
In：Active components A and active component B weight ratio are 1:80~60:1, described active components A is selected from chlorine nalidixic bacterium ester, activity into
Divide B Wei famoxadones.
2. the Synergistic bactericidal composition according to claim 1 containing chlorine nalidixic bacterium ester, it is characterised in that：Active components A and work
Property composition B weight ratio be 1:60~40:1.
3. the Synergistic bactericidal composition according to claim 2 containing chlorine nalidixic bacterium ester, it is characterised in that：
The weight ratio of chlorine nalidixic bacterium ester Yu famoxadones is 1:20~20:1.
4. the Synergistic bactericidal composition according to any one of claim 1 to 3 containing chlorine nalidixic bacterium ester, it is characterised in that：Group
Compound is made wettable powder, water dispersible granules, suspending agent, suspension emulsion, aqueous emulsion, microemulsion, microcapsule suspending agent or micro-capsule and hanged
Floating-suspending agent.
5. the Synergistic bactericidal composition according to claim 4 containing chlorine nalidixic bacterium ester is used for the use for preventing and treating disease on crops
On the way.
6. purposes according to claim 5, it is characterised in that：Described disease include sclerotiniose, powdery mildew, false smut,
Rice blast, banded sclerotial blight, downy mildew, gray mold, epidemic disease, leaf mold, resin disease, anthracnose, scab, ring spot, base rot disease,
Rust, glume blight or net blotch.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101822251A (en) * | 2010-01-27 | 2010-09-08 | 深圳诺普信农化股份有限公司 | Sterilization compound containing ZJ0712 |
| CN102239866A (en) * | 2011-04-19 | 2011-11-16 | 山东省烟台市农业科学研究院 | Composite bactericide containing dithianon and pyraclostrobin and application thereof |
| CN102626098A (en) * | 2012-03-28 | 2012-08-08 | 陕西上格之路生物科学有限公司 | Bactericidal composition containing pyraclostrobin |
| CN102696646A (en) * | 2012-06-29 | 2012-10-03 | 陕西上格之路生物科学有限公司 | Sterilizing composite containing captan |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101822251A (en) * | 2010-01-27 | 2010-09-08 | 深圳诺普信农化股份有限公司 | Sterilization compound containing ZJ0712 |
| CN102239866A (en) * | 2011-04-19 | 2011-11-16 | 山东省烟台市农业科学研究院 | Composite bactericide containing dithianon and pyraclostrobin and application thereof |
| CN102626098A (en) * | 2012-03-28 | 2012-08-08 | 陕西上格之路生物科学有限公司 | Bactericidal composition containing pyraclostrobin |
| CN102696646A (en) * | 2012-06-29 | 2012-10-03 | 陕西上格之路生物科学有限公司 | Sterilizing composite containing captan |
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Address after: 715500 Pucheng high tech Industrial Development Zone, Weinan, Shaanxi Patentee after: SHAANXI MEIBANG PHARMACEUTICAL GROUP Co.,Ltd. Address before: 715500 Shaanxi Pucheng Weinan County agricultural base industrial park Patentee before: Shaanxi Meibang pesticide Co.,Ltd. |
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