CN115885984A - Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof - Google Patents
Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof Download PDFInfo
- Publication number
- CN115885984A CN115885984A CN202211584307.1A CN202211584307A CN115885984A CN 115885984 A CN115885984 A CN 115885984A CN 202211584307 A CN202211584307 A CN 202211584307A CN 115885984 A CN115885984 A CN 115885984A
- Authority
- CN
- China
- Prior art keywords
- polyoxyethylene ether
- pyraclostrobin
- epoxiconazole
- block polyether
- microemulsion
- 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.)
- Pending
Links
- 239000005767 Epoxiconazole Substances 0.000 title claims abstract description 86
- ZMYFCFLJBGAQRS-IRXDYDNUSA-N (2R,3S)-epoxiconazole Chemical compound C1=CC(F)=CC=C1[C@@]1(CN2N=CN=C2)[C@H](C=2C(=CC=CC=2)Cl)O1 ZMYFCFLJBGAQRS-IRXDYDNUSA-N 0.000 title claims abstract description 83
- 239000005869 Pyraclostrobin Substances 0.000 title claims abstract description 83
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000000593 microemulsion method Methods 0.000 title description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 131
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 131
- 229920000570 polyether Polymers 0.000 claims abstract description 48
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 24
- 239000006184 cosolvent Substances 0.000 claims abstract description 22
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000013530 defoamer Substances 0.000 claims abstract description 8
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 78
- -1 aryl phenol Chemical compound 0.000 claims description 47
- 150000002191 fatty alcohols Chemical class 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 16
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 12
- BOLQUPOXTWHXIX-UHFFFAOYSA-N OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 Chemical compound OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 BOLQUPOXTWHXIX-UHFFFAOYSA-N 0.000 claims description 10
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 241000209140 Triticum Species 0.000 claims description 6
- 235000021307 Triticum Nutrition 0.000 claims description 6
- 201000010099 disease Diseases 0.000 claims description 5
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 4
- 241000221785 Erysiphales Species 0.000 claims description 3
- PGEBXGLGFFYYFX-UHFFFAOYSA-N 2,3-dibenzylphenol Chemical compound C=1C=CC=CC=1CC=1C(O)=CC=CC=1CC1=CC=CC=C1 PGEBXGLGFFYYFX-UHFFFAOYSA-N 0.000 claims description 2
- DMAXMXPDVWTIRV-UHFFFAOYSA-N 2-(2-phenylethyl)phenol Chemical compound OC1=CC=CC=C1CCC1=CC=CC=C1 DMAXMXPDVWTIRV-UHFFFAOYSA-N 0.000 claims description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical group C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 claims description 2
- BXCCKEJWQJEUMS-UHFFFAOYSA-N formaldehyde;4-nonylphenol Chemical compound O=C.CCCCCCCCCC1=CC=C(O)C=C1 BXCCKEJWQJEUMS-UHFFFAOYSA-N 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- XIPFMBOWZXULIA-UHFFFAOYSA-N pivalamide Chemical compound CC(C)(C)C(N)=O XIPFMBOWZXULIA-UHFFFAOYSA-N 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 239000000575 pesticide Substances 0.000 abstract description 26
- 240000008042 Zea mays Species 0.000 abstract description 10
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 abstract description 10
- 235000002017 Zea mays subsp mays Nutrition 0.000 abstract description 10
- 235000005822 corn Nutrition 0.000 abstract description 10
- 244000052616 bacterial pathogen Species 0.000 abstract description 6
- 206010059866 Drug resistance Diseases 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract description 5
- 230000009471 action Effects 0.000 abstract description 4
- 230000035515 penetration Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 29
- 230000000694 effects Effects 0.000 description 15
- 239000012895 dilution Substances 0.000 description 10
- 238000010790 dilution Methods 0.000 description 10
- MBHINSULENHCMF-UHFFFAOYSA-N n,n-dimethylpropanamide Chemical compound CCC(=O)N(C)C MBHINSULENHCMF-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 9
- 235000019796 monopotassium phosphate Nutrition 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- 239000007859 condensation product Substances 0.000 description 8
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexyloxide Natural products O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 8
- 239000000375 suspending agent Substances 0.000 description 8
- 239000002518 antifoaming agent Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000000693 micelle Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 210000001072 colon Anatomy 0.000 description 5
- 239000012847 fine chemical Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 230000001988 toxicity Effects 0.000 description 5
- 231100000419 toxicity Toxicity 0.000 description 5
- RZVHIXYEVGDQDX-UHFFFAOYSA-N 9,10-anthraquinone Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3C(=O)C2=C1 RZVHIXYEVGDQDX-UHFFFAOYSA-N 0.000 description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 125000002243 cyclohexanonyl group Chemical group *C1(*)C(=O)C(*)(*)C(*)(*)C(*)(*)C1(*)* 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000000857 drug effect Effects 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 4
- 238000005338 heat storage Methods 0.000 description 4
- 230000000361 pesticidal effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 240000005561 Musa balbisiana Species 0.000 description 3
- 235000021015 bananas Nutrition 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 230000002045 lasting effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 239000004563 wettable powder Substances 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 2
- 241000207199 Citrus Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 240000003553 Leptospermum scoparium Species 0.000 description 2
- 235000015459 Lycium barbarum Nutrition 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 235000020971 citrus fruits Nutrition 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 244000053095 fungal pathogen Species 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 230000005923 long-lasting effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 241000235349 Ascomycota Species 0.000 description 1
- 241000221198 Basidiomycota Species 0.000 description 1
- 102000012286 Chitinases Human genes 0.000 description 1
- 108010022172 Chitinases Proteins 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 240000007154 Coffea arabica Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000009849 Cucumis sativus Nutrition 0.000 description 1
- 102000015782 Electron Transport Complex III Human genes 0.000 description 1
- 108010024882 Electron Transport Complex III Proteins 0.000 description 1
- 240000009088 Fragaria x ananassa Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 241000208818 Helianthus Species 0.000 description 1
- 235000003222 Helianthus annuus Nutrition 0.000 description 1
- 241000758791 Juglandaceae Species 0.000 description 1
- 235000011430 Malus pumila Nutrition 0.000 description 1
- 244000070406 Malus silvestris Species 0.000 description 1
- 235000015103 Malus silvestris Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 241000233654 Oomycetes Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 235000016213 coffee Nutrition 0.000 description 1
- 235000013353 coffee beverage Nutrition 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 244000037666 field crops Species 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000006540 mitochondrial respiration Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 235000012015 potatoes Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 235000021012 strawberries Nutrition 0.000 description 1
- 239000004548 suspo-emulsion Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
- 239000004562 water dispersible granule Substances 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of pesticides, in particular to pyraclostrobin and epoxiconazole microemulsion and a preparation method and application thereof, wherein the pyraclostrobin and epoxiconazole microemulsion comprises the following components in percentage by weight: 2-15% of pyraclostrobin, 1-6% of epoxiconazole, 8-30% of polyoxyethylene ether emulsifier, 1-5% of block polyether type nonionic surfactant, 15-45% of solvent, 3-15% of cosolvent, 0.005-0.05% of defoamer and deionized water which are added to 100%. By adopting the pyraclostrobin and the epoxiconazole as effective active ingredients, under the action of a specific polyoxyethylene ether emulsifier, a block polyether type nonionic surfactant, a solvent and a cosolvent, the prepared microemulsion has the functions of protection, treatment and leaf penetration and conduction, can well prevent and treat the corn northern leaf blight, can reduce the dosage and delay and treat the drug resistance of pathogenic bacteria.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to pyraclostrobin and epoxiconazole microemulsion as well as a preparation method and application thereof.
Background
Pyraclostrobin was first developed and successfully developed by basf corporation, germany in 1993, reported in 2000, and registered and marketed in 2001 under the trade name of 250 g/l pyraclostrobin missible oil, and single and mixed preparations of pyraclostrobin registered in China mainly come from basf european corporation and guangdong dely biotechnology limited company and the like. The bactericidal composition is widely used for preventing and treating diseases caused by almost all types of fungal pathogens such as ascomycetes, basidiomycetes, deuteromycetes and oomycetes on cereals, soybeans, tea trees, peanuts, cotton, grapes, vegetables, potatoes, sunflowers, bananas, lemons, coffee, fruit trees, walnuts, tea trees, tobacco, ornamental plants, lawns and other field crops, and can also be used for seed treatment. According to Chinese pesticide information network data, up to 711 registered pyraclostrobin products are obtained in China by 1 month in 2022, wherein the registered pyraclostrobin products comprise 294 single agents and 417 mixed agents. The registered formulations comprise raw pesticide, suspending agent, wettable powder, seed treatment suspending agent, missible oil and the like, and the main registered crops comprise apple trees, cucumbers, bananas, strawberries and the like.
Epoxiconazole is a novel, broad-spectrum, long-lasting fungicide developed by basf corporation in 1985. In early 1993, epoxiconazole first entered the french market under the Opus trade name, and then entered europe, south america and asia. Epoxiconazole was first registered in 2000 by basf gmbh, germany, and subsequently, it was registered in 2005 by yosu cultivation chemical gmbh, yosu flying chemical gmbh, shenyang chemical research institute laboratory, liao ning province, and shanghai sheng nong biochemical products gmbh, and yosu zhongqi chemical gmbh in 2006. According to Chinese pesticide information network data, by 11 months in 2020, 208 registered epoxiconazole products are obtained in China, wherein 109 single agents and 99 mixed agents are adopted, the dosage forms of the epoxiconazole product comprise raw pesticide, water dispersible granules, suspending agents, emulsion and the like, and the main registered crops are bananas, rice, wheat and the like.
In the prior art, the drug resistance of a single drug is avoided and the drug effect is improved at the same time by compounding, for example, chinese patent application (publication No. CN 113575604A) discloses a water suspending agent containing pyraclostrobin and epoxiconazole and a preparation method thereof, the pyraclostrobin and the epoxiconazole are specifically used as main active ingredients, and the water suspending agent is prepared under the condition of the presence of other additives, so that the water suspending agent has the advantages of good dispersibility, good storage stability, high drug effect and long lasting period, but is not beneficial to adhesion and development on crops, polypide and germs, and the pesticide utilization rate is low; chinese patent application (publication No. CN 114651822A) provides a composition, a medicine and application thereof in preventing and treating citrus anthracnose, and particularly adopts epoxiconazole and pyraclostrobin with the mass ratio of (2-16): 1 as effective components, so that the provided product is used for preventing and treating citrus acute anthracnose, but does not relate to the research on the prevention and treatment effects of corn northern leaf blight, wheat powdery mildew and gibberellic disease.
Disclosure of Invention
On the one hand, the pyraclostrobin and epoxiconazole microemulsion comprises the following components in percentage by weight: 2-15% of pyraclostrobin, 1-6% of epoxiconazole, 8-30% of polyoxyethylene ether emulsifier, 1-5% of block polyether type nonionic surfactant, 15-45% of solvent, 3-15% of cosolvent, 0.005-0.05% of defoamer and deionized water which are added to 100%.
As a preferred technical scheme, the mass ratio of the pyraclostrobin to the epoxiconazole is (1-5): 1; preferably, the mass ratio of the pyraclostrobin to the epoxiconazole is (2-3): 1.
the inventor finds that pyraclostrobin and epoxiconazole are used as effective active ingredients to prepare the suspending agent for subsequent application in the actual research and development process, the pyraclostrobin is easy to melt after a sample is stored for 24 hours at normal temperature, crystals are separated out from a formula system, the suspending agent is low in formula cost, the surface tension of liquid medicine after dilution (2000 times of dilution) is too large, the spreading capability on crops is not good enough, the drug effect is insufficient in competitiveness compared with other dosage forms, the existing commercial product has the problems that a wet sieve test is carried out after hot storage, the passing rate is not qualified, a large amount of jelly residues exist on a screen, and the particle size of the product is increased seriously.
Based on the system, the pyraclostrobin and epoxiconazole are used as effective active ingredients, and under the action of a specific polyoxyethylene ether emulsifier, a block polyether type nonionic surfactant, a solvent and a cosolvent, the prepared microemulsion has the functions of protection, treatment and leaf permeation and conduction, can well prevent and treat the corn northern leaf blight, can reduce the dosage and delay and treat the drug resistance of pathogenic bacteria. The reason for the analysis by the inventor is probably that: pyraclostrobin is a quinone external inhibitor, mitochondrial respiration is inhibited by preventing electron transfer of a cytochrome bc1 complex, a sterilization effect is achieved, epoxiconazole can effectively inhibit pathogenic fungi, the activity of chitinase of crops is improved, contraction of fungus haustorium is caused, pathogen invasion is inhibited, protection and treatment effects are achieved, the pyraclostrobin and the epoxiconazole generate obvious synergistic effects in two different action modes, advantage complementation is achieved, and generation of pest drug resistance is relieved. The inventor discovers that the synergistic effect of the pyraclostrobin and the epoxiconazole is most remarkable and the highest co-toxicity coefficient is obtained when the pyraclostrobin and the epoxiconazole are introduced into a system in a mass ratio of (2-3) to 1, the pesticide composition can effectively reduce the use amount of pesticides and agricultural cost, is efficient, low in toxicity and low in residue, and provides a choice for controlling agricultural pests. In addition, the microemulsion is prepared by using low organic solvent, high surfactant and high utilization rate of raw pesticide, reduces environmental pollution, has lower surface tension (2000 times of dilution), has good spreadability, can promote the penetration of the raw pesticide into animal and plant tissues, improves the transfer efficiency, is convenient to produce, has stable state, is homogeneous and stable under use concentration, and is safe to transport and store.
As a preferable technical scheme, the polyoxyethylene ether emulsifier is at least one of aryl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, phenolic resin polyoxyethylene ether, fatty alcohol polyoxypropylene ether, nonylphenol formaldehyde condensate polyoxyethylene ether and diphenylethylphenol formaldehyde condensate polyoxyethylene ether; preferably, the polyoxyethylene ether emulsifier is a combination of aryl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and diphenyl ethyl phenol formaldehyde condensation compound polyoxyethylene ether.
Preferably, the aryl phenol polyoxyethylene ether is at least one of triphenylethylene phenol polyoxyethylene ether, dibenzyl diphenol polyoxyethylene ether, dibenzyl complex phenol polyoxyethylene ether, cumyl phenethyl phenol polyoxyethylene ether and dibenzyl phenol polyoxyethylene ether; most preferably, the aryl phenol polyoxyethylene ether is triphenylethylene phenol polyoxyethylene ether.
Preferably, the fatty alcohol-polyoxyethylene ether is at least one of C16-18 fatty alcohol-polyoxyethylene ether, heterogeneous dodecanol polyoxyethylene ether, heterogeneous tridecanol polyoxyethylene ether and lauryl alcohol polyoxyethylene ether; preferably, the fatty alcohol-polyoxyethylene ether is isomeric tridecanol polyoxyethylene ether.
As a preferred technical scheme, the block polyether type nonionic surfactant is propylene glycol block polyether; preferably, the propylene glycol block polyether is at least one of polyether 2040, L31, L42, L43, L61, L62, L64, L68 and L81; further preferably, the propylene glycol block polyether has an HLB value of 7 to 13; the average molecular weight of the propylene glycol block polyether is 2500-2900; most preferably, the propylene glycol block polyether is a combination of L62, L64; the mass ratio of L62 to L64 is (1-2): (1.5-3). The L62 and the L64 are from Liaoning Colon Fine chemical industries, inc.
In the research process, the inventor finds that the compounding effect and the system stability of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenylethylphenol formaldehyde condensate polyoxyethylene ether and the propylene glycol block polyether introduced into the system are greatly influenced by the propylene glycol block polyether, so that the synergistic effect of the pyraclostrobin and the epoxiconazole cannot be fully exerted. Based on triphenylethylene phenol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether and diphenylethyl phenol formaldehyde condensation compound polyoxyethylene ether in the system, block polyether type nonionic surfactant propylene glycol block polyether is introduced, and particularly, the mass ratio is (1-2): the L62 and the L64 of (1.5-3) are matched for use, mixed micelles are formed in the system, the emulsification effect is improved to the maximum extent, the stability of the system is ensured, and meanwhile, the provided microemulsion has good drug effect and longer lasting period, and the reason analyzed by the inventor is that: introducing a mixture of (1-2): the L62 and the L64 of the (1.5-3) are well matched with the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether and the diphenyl ethyl phenol formaldehyde condensation product polyoxyethylene ether in the system to realize synergism, so that the pyraclostrobin and the epoxiconazole are favorably adhered and spread on crops and pathogenic bacteria, the pesticide application deposition effect and the pesticide utilization efficiency are obviously improved, the provided microemulsion is not easily influenced by the environment humidity and the temperature, and the lasting and effective prevention and treatment are realized. Furthermore, the inventors have surprisingly found that by introducing a mass ratio of (1-2): and (1.5-3) L62 and L64 improve the emulsification effect, and avoid the unqualified milky state of the preparation diluted by 200 times with water due to the overlarge particle size of the emulsified liquid drop in water, so that the prepared preparation diluted by 200 times is transparent in water and has blue fluorescence. The reason for the analysis by the inventor is probably that: in the process of using a preparation sample in water, the difference of dilution and dispersion effects of the preparation is large due to different water-entering states, the concentration of a direct high-dilution-multiple diluted surfactant in water is low and the diluted surfactant is effectively dispersed in a molecular state, while in the process of mixing the preparation sample and water by 1:1, the concentration of the surfactant is far higher than the critical micelle concentration of the diluted surfactant, so that the surfactant molecules are combined into large groups to form micelles, and the mixture cannot be effectively dispersed even after being diluted by water, and is in an unqualified milky state, and the mass ratio is (1-2): the combination of the L62 and L64 propylene glycol block polyethers in the formula (1.5-3) effectively improves the critical micelle concentration of the system, so that the system can be rapidly and effectively dispersed under the high-concentration dilution condition, and the dilution liquid is transparent and has blue fluorescence (in a nano-scale state).
As a preferable technical scheme, the mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenylethyl phenol formaldehyde condensation product polyoxyethylene ether and the propylene glycol block polyether is (6-10): (7-9): (5-10): (2-5).
Most products on the market are good in state under the condition of being diluted by over 1000 times and used independently at low concentration, but pesticides are often mixed with pesticide fertilizers and other pesticides in the actual use process, the pesticides are required to be used under the condition of being diluted by 20-50 times along with the development of the flight control technology, and the water hardness difference of different areas is very large, so that the practical application of the pesticides is used in a high electrolyte system, the electrolyte resistance of a plurality of pesticide preparations is not enough, homogeneous stable dispersion cannot be maintained under the system, and flocculation, delamination, creaming and even agglomeration can occur in the use process to block a nozzle filter screen of an airplane. The inventor finds that triphenylethylene phenol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether are introduced into the system to effectively improve the water-entering emulsification state of the preparation and effectively enhance the surface permeability and systemic property of crops and germs, but finds that the layering demulsification phenomenon of the product occurs in the actual application and research process of carrying out flight control by matching with high-concentration potassium dihydrogen phosphate blending, which directly causes that the product cannot effectively and uniformly act on a receptor, and greatly reduces the utilization rate of pyraclostrobin and epoxiconazole and the disease control effect. The inventor introduces the polyoxyethylene ether of the diphenylethylphenol formaldehyde condensate and the propylene glycol block polyether, so that the finally prepared microemulsion has remarkably improved electrolyte resistance, is mixed with common foliar fertilizer, monopotassium phosphate, wettable powder and the like 1:1 on the market, and still keeps homogeneous phase stability under the condition of 20 times of dilution. The reason the inventor analyzes may be: after triphenylethylene phenol polyoxyethylene ether is contacted with high-concentration potassium dihydrogen phosphate electrolyte, changing the mixed CMC micelle to cause demulsification and layering, introducing diphenyl ethyl phenol formaldehyde condensation product polyoxyethylene ether and propylene glycol block polyether, and simultaneously controlling the mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenyl ethyl phenol formaldehyde condensation product polyoxyethylene ether to the propylene glycol block polyether to be (6-10): (7-9): (5-10): (2-5), on one hand, the derivative can generate synergistic effect with triphenylethylene phenol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether in a system, further improve the stability of the system, improve the protection effect on crops and reduce the irritation; on the other hand, the electrolyte resistance of the microemulsion formula system is obviously improved, layering demulsification failure after contact with high-concentration monopotassium phosphate is avoided, and the application scene of flight control is met.
As a preferable technical scheme, the solvent is at least one of dimethyl propionamide, dimethyl formamide and dimethyl carbonate; preferably, the solvent is a combination of dimethyl carbonate and dimethylpropionamide; the mass ratio of the dimethyl carbonate to the dimethyl propionamide is (0.8-1.2): 1.
as a preferred technical scheme, the cosolvent is cyclohexanone;
the inventor finds out in the practical production and development process that when the preparation is subjected to a low-temperature stability test according to a GB/T19137-2003 pesticide low-temperature stability testing method, the preparation is found to have the problem of crystal precipitation in a 7-day cold storage process under the condition of 0 ℃, and based on the system, the invention adopts the following components in a mass ratio of (0.8-1.2): the dimethyl carbonate and the dimethyl propionamide of 1 are combined to be used as a solvent, and cyclohexanone is introduced to be used as a cosolvent, so that the pyraclostrobin and the epoxiconazole in the system are fully mixed and compatible, the subsequent emulsifying and dispersing effect is ensured, the cold and hot storage stability of the preparation is effectively improved, the improved preparation still keeps homogeneous, clear and transparent after being stored for 30 days at the temperature of-6 ℃, and the crystal precipitation phenomenon does not occur.
The invention also provides a preparation method of the pyraclostrobin and epoxiconazole microemulsion, which comprises the following steps:
(1) Adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, adding the pyraclostrobin and the epoxiconazole, stirring, dissolving and mixing for 30-60min;
(2) Accurately weighing polyoxyethylene ether emulsifier, block polyether type nonionic surfactant and defoamer according to the feeding proportion, sequentially adding into a preparation kettle, and opening a stirrer for mixing for 30-60min;
(3) Adding deionized water into the preparation kettle, and mixing for 30-60 min.
The third aspect of the invention provides an application of pyraclostrobin and epoxiconazole microemulsion: can be used for preventing and treating corn leaf blight, wheat powdery mildew and gibberellic disease.
Advantageous effects
1. The invention provides a pyraclostrobin and epoxiconazole microemulsion, which adopts pyraclostrobin and epoxiconazole as effective active ingredients, and has the functions of protection, treatment and leaf permeation and conduction under the action of a specific polyoxyethylene ether emulsifier, a block polyether type nonionic surfactant, a solvent and a cosolvent, so that the prepared microemulsion has the functions of preventing and treating corn northern leaf blight well, the dosage can be reduced, and the drug resistance of pathogenic bacteria is delayed and treated.
2. Based on the system, the mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenyl ethyl phenol formaldehyde condensation compound polyoxyethylene ether and the propylene glycol block polyether is controlled to be (6-10): (7-9): (5-10): (2-5), the finally prepared microemulsion has remarkably improved electrolyte resistance, is mixed with common foliar fertilizer, monopotassium phosphate, wettable powder and the like 1:1 on the market, still keeps homogeneous phase stability under the condition of 20 times dilution, and meets the application scene of flight control; meanwhile, the protective effect on crops is improved, and the irritation is reduced.
3. Based on the system, the block polyether type nonionic surfactant propylene glycol block polyether is introduced, and particularly, the mass ratio of (1-2): the L62 and the L64 of the (1.5-3) are matched for use, a mixed micelle is formed in the system, the emulsification effect is improved to the maximum extent, the stability of the system is ensured, the provided preparation is diluted by 200 times into water to be transparent and has blue fluorescence, and meanwhile, the provided microemulsion has good efficacy and longer lasting period.
4. Based on the system of the invention, the mass ratio of (0.8-1.2): the dimethyl carbonate and the dimethyl propionamide of 1 are combined to be used as a solvent, and cyclohexanone is introduced to be used as a cosolvent, so that the pyraclostrobin and the epoxiconazole in the system are fully mixed and compatible, the subsequent emulsifying and dispersing effect is ensured, the cold and hot storage stability of the preparation is effectively improved, the improved preparation still keeps homogeneous, clear and transparent after being stored for 30 days at the temperature of-6 ℃, and the crystal precipitation phenomenon does not occur.
Drawings
Fig. 1 is a test result of the physical and chemical properties of the pyraclostrobin and epoxiconazole microemulsions prepared in example 1 of the present invention.
FIG. 2 shows pyraclostrobin, epoxiconazole and 1:1,2:1,3:1,4:1 and 5:1 and testing the toxicity of the mixed strain to the northern leaf blight of corn.
Fig. 3 is a field pesticide effect test report of the pyraclostrobin and epoxiconazole microemulsion prepared in the embodiment 1 of the invention for preventing and treating corn northern leaf blight.
Fig. 4 is a field pesticide effect test report of the pyraclostrobin and epoxiconazole microemulsion prepared in the embodiment 1 of the invention for preventing and treating wheat scab.
FIG. 5 is a graph comparing the surface tension results of example 1 of the present invention and comparative example 1 diluted 2000 times, wherein (a) example 1 and (b) comparative example 1.
FIG. 6 is a graph comparing the results of the low temperature stability tests of example 1 and comparative example 2 of the present invention, wherein (a) comparative example 2 and (b) example 1.
FIG. 7 is a graph comparing the results of the heat storage stability tests of example 1 of the present invention and comparative example 3, wherein (a) comparative example 3 and (b) example 1.
FIG. 8 is a graph comparing the results of a 200-fold dilution in water test conducted for example 1 of the present invention and comparative example 4, wherein (a) is comparative example 4 and (b) is example 1.
FIG. 9 is a graph comparing the results of the test of example 1 and comparative example 5 of the present invention with a 20-fold dilution of potassium dihydrogen phosphate, wherein (a) comparative example 5 and (b) example 1.
Detailed Description
Example 1
In embodiment 1 of the invention, on the one hand, the pyraclostrobin and epoxiconazole microemulsion comprises the following components in percentage by weight: 12.3% of pyraclostrobin, 4.7% of epoxiconazole, 22% of polyoxyethylene ether emulsifier, 3% of block polyether type nonionic surfactant, 20% of solvent, 5% of cosolvent, 0.01% of defoaming agent and the balance of deionized water to 100%.
The polyoxyethylene ether emulsifier is a combination of aryl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and diphenyl ethyl phenol formaldehyde condensation compound polyoxyethylene ether.
The aryl phenol polyoxyethylene ether is triphenylethylene phenol polyoxyethylene ether.
The fatty alcohol-polyoxyethylene ether is isomeric tridecanol polyoxyethylene ether.
The mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenyl ethyl phenol formaldehyde condensation product polyoxyethylene ether and the propylene glycol block polyether is 8:8:7:3.
the propylene glycol block polyether is a combination of L62 and L64; the mass ratio of L62 to L64 is 2:3. the L62 and L64 are from the Liaoning Colon Fine chemical industries, inc.
The solvent is a combination of dimethyl carbonate and dimethyl propionamide; the mass ratio of the dimethyl carbonate to the dimethyl propionamide is 1:1.
the cosolvent is cyclohexanone;
in another aspect, embodiment 1 of the invention provides a preparation method of pyraclostrobin and epoxiconazole microemulsion, which comprises the following steps:
(1) Adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, adding the pyraclostrobin and the epoxiconazole, stirring, dissolving and mixing for 40min;
(2) Accurately weighing polyoxyethylene ether emulsifier, block polyether type nonionic surfactant and defoamer according to the feeding proportion, sequentially adding the weighed materials into a preparation kettle, and opening a stirrer to mix for 40min;
(3) Adding deionized water into the preparation kettle, and mixing for 60 min.
Example 2
Embodiment 2 of the invention provides a pyraclostrobin and epoxiconazole microemulsion, which comprises the following components in percentage by weight: 11.3% of pyraclostrobin, 5.7% of epoxiconazole, 28% of polyoxyethylene ether emulsifier, 3% of block polyether type nonionic surfactant, 20% of solvent, 5% of cosolvent, 0.01% of defoaming agent and the balance of deionized water to 100%.
The polyoxyethylene ether emulsifier is a combination of aryl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and diphenyl ethyl phenol formaldehyde condensation compound polyoxyethylene ether.
The aryl phenol polyoxyethylene ether is triphenylethylene phenol polyoxyethylene ether.
The fatty alcohol-polyoxyethylene ether is isomeric tridecanol polyoxyethylene ether.
The propylene glycol block polyether is a combination of L62 and L64; the mass ratio of L62 to L64 is 2:3. the L62 and L64 are from the Liaoning Colon Fine chemical industries, inc.
The mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenylethyl phenol formaldehyde condensation product polyoxyethylene ether to the propylene glycol block polyether is 8:8:10:3.
the solvent is a combination of dimethyl carbonate and dimethyl propionamide; the mass ratio of the dimethyl carbonate to the dimethyl propionamide is 1:1.
the cosolvent is cyclohexanone;
in another aspect, embodiment 2 of the invention provides a preparation method of pyraclostrobin and epoxiconazole microemulsion, which comprises the following steps:
(1) Adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, adding the pyraclostrobin and the epoxiconazole, stirring, dissolving and mixing for 40min;
(2) Accurately weighing polyoxyethylene ether emulsifier, block polyether nonionic surfactant and defoamer according to the feeding proportion, sequentially adding into a preparation kettle, and opening a stirrer for mixing for 40min;
(3) Adding deionized water into the preparation kettle, and mixing for 60 min.
Example 3
The polyoxyethylene ether emulsifier is a combination of aryl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and diphenyl ethyl phenol formaldehyde condensation compound polyoxyethylene ether.
The aryl phenol polyoxyethylene ether is triphenylethylene phenol polyoxyethylene ether.
The fatty alcohol-polyoxyethylene ether is isomeric tridecanol polyoxyethylene ether.
The propylene glycol block polyether is a combination of L62 and L64; the mass ratio of L62 to L64 is 2:3. the L62 and the L64 are from Liaoning Colon Fine chemical industries, inc.
The mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenylethyl phenol formaldehyde condensation product polyoxyethylene ether to the propylene glycol block polyether is 8:8:10:3.
the solvent is a combination of dimethyl carbonate and dimethyl propionamide; the mass ratio of the dimethyl carbonate to the dimethyl propionamide is 1:1.
the cosolvent is cyclohexanone;
the embodiment 3 of the invention provides a preparation method of the pyraclostrobin and epoxiconazole microemulsion on the other hand, which comprises the following steps:
(1) Adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, adding the pyraclostrobin and the epoxiconazole, stirring, dissolving and mixing for 40min;
(2) Accurately weighing polyoxyethylene ether emulsifier, block polyether nonionic surfactant and defoamer according to the feeding proportion, sequentially adding into a preparation kettle, and opening a stirrer for mixing for 40min;
(3) Adding deionized water into the preparation kettle, and mixing for 60 min.
Comparative example 1
Comparative example 1 of the present invention is a commercial 17% oxazolefetoepoxiconazole suspoemulsion.
Comparative example 2
The invention provides pyraclostrobin and epoxiconazole microemulsion and a preparation method thereof in a comparative example 2, which are the same as example 1 in specific implementation mode and are different in that the microemulsion comprises the following components in percentage by weight: 12.3 percent of pyraclostrobin, 4.7 percent of epoxiconazole, 22 percent of polyoxyethylene ether emulsifier, 3 percent of block polyether type nonionic surfactant, 20 percent of solvent, 0.01 percent of defoaming agent and deionized water which are added to 100 percent.
Comparative example 3
The invention provides pyraclostrobin and epoxiconazole microemulsion and a preparation method thereof in a comparative example 3, wherein the specific implementation mode of the pyraclostrobin and epoxiconazole microemulsion is the same as that of example 1, and the differences are that the pyraclostrobin and epoxiconazole microemulsion comprises the following components in percentage by weight: 12.3% of pyraclostrobin, 4.7% of epoxiconazole, 22% of polyoxyethylene ether emulsifier, 1% of block polyether type nonionic surfactant, 20% of solvent, 5% of cosolvent, 0.01% of defoaming agent and the balance of deionized water to 100%, wherein the mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenyl phenol formaldehyde condensation product polyoxyethylene ether and the propylene glycol block polyether is 10:10:2:1.
comparative example 4
The invention provides a pyraclostrobin and epoxiconazole microemulsion and a preparation method thereof in a comparative example 4, which is the same as that in example 1 in specific implementation mode, and is different in that the type of the propylene glycol block polyether is L31 and is sourced from Liaoning Colon fine chemical industry Co.
Comparative example 5
The invention provides pyraclostrobin and epoxiconazole microemulsion and a preparation method thereof in a comparative example 5, which have the same specific implementation manner as that of example 1, except that the microemulsion comprises the following components in percentage by weight: 12.3% of pyraclostrobin, 4.7% of epoxiconazole, 22% of polyoxyethylene ether emulsifier, 3% of block polyether type nonionic surfactant, 20% of solvent, 5% of cosolvent, 0.01% of defoaming agent and deionized water, wherein the polyoxyethylene ether emulsifier is a combination of aryl phenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether when the total amount is 100%; the mass ratio of the aryl phenol polyoxyethylene ether to the fatty alcohol polyoxyethylene ether to the propylene glycol block polyether is 11.
Performance test method
(1) According to O31/0116000265C039-2020 < 17% Azole Ether-Epoxiconazole microemulsion >, with reference to the standard GB/T1601-93 < determination method of pH value of pesticide >, < GB/T28137-2011 < determination method of persistent foamability of pesticide >, < GB/T1603-2001 < determination method of stability of pesticide emulsion >, < GB/T19137-2003 < determination method of low temperature stability of pesticide >, < GB/T19136-2003 < determination method of stability of thermal storage of pesticide >, < 17% Azole Ether-Epoxiconazole microemulsion > provided by example 1 has appearance, pyraclostrobin mass fraction, epoxiconazole mass fraction, pH value, emulsion stability, persistent foamability, low temperature stability and thermal storage stability, and the test results all meet the requirements of O31/0116000265C039-2020, and are shown in figure 1.
(2) According to the standards of NY/T1156.2-2006 and NY/T1156.6-2006, pyraclostrobin and epoxiconazole and the ratio of 1:1,2:1,3:1,4:1 and 5: the toxicity to the northern leaf blight of corn caused by the mixing of the pyraclostrobin and the epoxiconazole is shown by the proportion of 1, the pyraclostrobin and the epoxiconazole are mixed according to the proportion of 5, the toxicity to the northern leaf blight of corn is shown as a synergistic effect, the EC50 values of the toxicity are respectively 1.38mg/L, 1.44mg/L, 1.56mg/L, 1.80mg/L and 2.08mg/L, and the cotoxicity coefficients are respectively 131.78, 149.02, 151.04, 139.36 and 125.68. The two are mixed according to the proportion of 2:1 and 3:1, the synergistic effect is obvious, and the result is shown in figure 2.
(3) The 17% azoleth and epoxiconazole microemulsion prepared in the example is subjected to a field pesticide effect test for preventing and treating wheat scab, and the method and the result are shown in figure 3.
(4) The 17% azolether-epoxiconazole microemulsion prepared in the example is subjected to a field pesticide effect test for preventing and treating corn northern leaf blight, and the method and the result are shown in figure 4.
(5) The surface tension was measured after diluting example 1 and comparative example 1 with water 2000 times, and the results are shown in fig. 5.
(6) The low-temperature stability of the pyraclostrobin and epoxiconazole microemulsions obtained in example 1 and comparative example 2 of the present invention was determined by reference to GB/T19137-2003, the results of which are shown in FIG. 6. In comparative example 2, the crystal precipitation problem occurred during 7 days cold storage at 0 deg.C (FIG. 6 a), while example 1 remained homogeneous, clear and transparent after 30 days storage at-6 deg.C, and no crystal precipitation phenomenon occurred (FIG. 6 b).
(7) The low-temperature stability of the pyraclostrobin and epoxiconazole microemulsions obtained in example 1 and comparative example 3 of the invention is measured by referring to the GB/T19136-2003 pesticide heat storage stability measuring method, and as a result, referring to FIG. 6, the sample is qualified after the comparative example 3 is subjected to heat storage at 54 ℃ for 14 days (FIG. 7 a), and the sample is not subjected to heat storage at 54 ℃ for 14 days (FIG. 7 b).
(8) The pyraclostrobin and epoxiconazole microemulsions obtained from example 1 and comparative example 4 of the present invention were diluted 200 times with water, and as a result, referring to fig. 8, comparative example 4 was milky white after being diluted 200 times with water (fig. 8 a), whereas example 1 was transparent and showed blue fluorescence after being diluted 200 times with water (fig. 8 b).
(9) The pyraclostrobin and epoxiconazole microemulsions obtained in example 1 and comparative example 5 of the present invention were mixed with the 20-fold diluted solution of potassium dihydrogen phosphate, and as a result, referring to fig. 9, the comparative example 5 mixed with the 20-fold diluted solution of potassium dihydrogen phosphate failed to maintain homogeneous stable dispersion and showed flocculation (fig. 9 a), while the example 1 mixed with the 20-fold diluted solution of potassium dihydrogen phosphate maintained homogeneous stable dispersion and showed no flocculation (fig. 9 b).
Claims (10)
1. The pyraclostrobin and epoxiconazole microemulsion is characterized by comprising the following components in percentage by weight: 2-15% of pyraclostrobin, 1-6% of epoxiconazole, 8-30% of polyoxyethylene ether emulsifier, 1-5% of block polyether type nonionic surfactant, 15-45% of solvent, 3-15% of cosolvent, 0.005-0.05% of defoamer and deionized water which are complemented to 100%.
2. The pyraclostrobin and epoxiconazole microemulsion according to claim 1, wherein the mass ratio of pyraclostrobin to epoxiconazole is (1-5): 1; preferably, the mass ratio of the pyraclostrobin to the epoxiconazole is (2-3): 1.
3. the pyraclostrobin and epoxiconazole microemulsion according to claim 1 or 2, wherein the polyoxyethylene ether emulsifier is at least one of aryl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, phenolic resin polyoxyethylene ether, fatty alcohol polyoxypropylene ether, nonylphenol formaldehyde condensate polyoxyethylene ether and diphenylethylphenol formaldehyde condensate polyoxyethylene ether.
4. The pyraclostrobin and epoxiconazole microemulsion according to claim 3 wherein the aryl phenol polyoxyethylene ether is at least one of triphenylethylene phenol polyoxyethylene ether, dibenzyl diphenol polyoxyethylene ether, dibenzyl complex phenol polyoxyethylene ether, cumyl phenethyl phenol polyoxyethylene ether and dibenzyl phenol polyoxyethylene ether.
5. The pyraclostrobin and epoxiconazole microemulsion according to claim 4, wherein the fatty alcohol polyoxyethylene ether is at least one of C16-18 fatty alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether and lauryl alcohol polyoxyethylene ether.
6. The pyraclostrobin and epoxiconazole microemulsion according to claim 5 wherein the block polyether type nonionic surfactant is propylene glycol block polyether.
7. The pyraclostrobin and epoxiconazole microemulsion according to claim 6, wherein the mass ratio of the aryl phenol polyoxyethylene ether, the fatty alcohol polyoxyethylene ether, the diphenylethylphenol formaldehyde condensate polyoxyethylene ether and the propylene glycol block polyether is (6-10): (7-9): (5-10): (2-5).
8. The pyraclostrobin and epoxiconazole microemulsion according to claim 7 wherein the solvent is at least one of dimethylpropionamide, dimethylformamide and dimethyl carbonate.
9. A method for preparing pyraclostrobin and epoxiconazole microemulsions according to any one of claims 1-8, characterized in that it comprises at least the following steps:
(1) Adding the cosolvent and the solvent into a preparation kettle, opening a stirrer, adding the pyraclostrobin and the epoxiconazole, stirring, dissolving and mixing for 30-60min;
(2) Accurately weighing polyoxyethylene ether emulsifier, block polyether type nonionic surfactant and defoamer according to the feeding proportion, sequentially adding the weighed materials into a preparation kettle, and opening a stirrer to mix for 30-60min;
(3) Adding deionized water into the preparation kettle, and mixing for 30-60 min.
10. Use of pyraclostrobin and epoxiconazole microemulsions according to anyone of claims 1 to 8 for the control of northern leaf blight, wheat powdery mildew and gibberellic disease.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211584307.1A CN115885984A (en) | 2022-12-09 | 2022-12-09 | Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211584307.1A CN115885984A (en) | 2022-12-09 | 2022-12-09 | Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115885984A true CN115885984A (en) | 2023-04-04 |
Family
ID=86487895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211584307.1A Pending CN115885984A (en) | 2022-12-09 | 2022-12-09 | Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115885984A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102265879A (en) * | 2011-06-20 | 2011-12-07 | 青岛泰生生物科技有限公司 | Sterilizing microemulsion containing Pyraclostrobin and preparation method thereof |
| CN102484998A (en) * | 2010-12-02 | 2012-06-06 | 江苏丘陵地区镇江农业科学研究所 | Broad-spectrum combined bactericide |
| CN103563942A (en) * | 2012-08-05 | 2014-02-12 | 南京华洲药业有限公司 | Bactericidal composition containing pyraclostrobin and epoxiconazole and application thereof |
| CN106070273A (en) * | 2016-06-08 | 2016-11-09 | 广东中迅农科股份有限公司 | A kind of containing pyraclostrobin with the composition pesticide of epoxiconazole |
| CN108260596A (en) * | 2016-12-30 | 2018-07-10 | 山东潍坊润丰化工股份有限公司 | A kind of bactericidal composition containing pyraclostrobin and epoxiconazole, fungicide and its application |
-
2022
- 2022-12-09 CN CN202211584307.1A patent/CN115885984A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102484998A (en) * | 2010-12-02 | 2012-06-06 | 江苏丘陵地区镇江农业科学研究所 | Broad-spectrum combined bactericide |
| CN102265879A (en) * | 2011-06-20 | 2011-12-07 | 青岛泰生生物科技有限公司 | Sterilizing microemulsion containing Pyraclostrobin and preparation method thereof |
| CN103563942A (en) * | 2012-08-05 | 2014-02-12 | 南京华洲药业有限公司 | Bactericidal composition containing pyraclostrobin and epoxiconazole and application thereof |
| CN106070273A (en) * | 2016-06-08 | 2016-11-09 | 广东中迅农科股份有限公司 | A kind of containing pyraclostrobin with the composition pesticide of epoxiconazole |
| CN108260596A (en) * | 2016-12-30 | 2018-07-10 | 山东潍坊润丰化工股份有限公司 | A kind of bactericidal composition containing pyraclostrobin and epoxiconazole, fungicide and its application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101485329B (en) | Agricultural chemical composition for disinsection and use thereof | |
| CN102696601A (en) | Insecticidal composition containing flubendiamide | |
| CN107006505A (en) | A kind of composition pesticide of copper 8-hydroxyquinolinate and pyraclostrobin | |
| CN115885984A (en) | Pyraclostrobin and epoxiconazole microemulsion as well as preparation method and application thereof | |
| CN104521980A (en) | Pymetrozine-containing insecticidal composition | |
| CN116267928A (en) | Sterilization composition containing bronopol | |
| CN107232217B (en) | Bactericide composition and application thereof | |
| CN114617127A (en) | Pesticide sterilization composition and application thereof | |
| CN107347903A (en) | A kind of composition pesticide containing cycolxylidin and matrine | |
| CN103651507A (en) | Insecticidal composition containing cycolxylidin and nimbin | |
| CN111869672B (en) | Bactericidal composition and application thereof | |
| CN107711868B (en) | Bactericidal composition containing prochloraz and biological antibacterial substance HSAF and application thereof | |
| CN106508943A (en) | Bactericidal composition containing benthiavalicarb-isopropyl and prochloraz, and applications thereof | |
| CN104886122A (en) | Compound composition containing dufulin and pyrazole amide bactericide and bactericide | |
| CN104886123B (en) | Fungicidal composition containing dufulin and fluazinam and fungicide containing fungicidal composition | |
| CN110495463A (en) | The Synergistic insecticidal composition of the pyrimidine containing trifluoro-benzene and its application | |
| CN115804383B (en) | Sterilization composition for preventing and treating corn ear rot and application thereof | |
| CN114982765B (en) | Pesticide composition and preparation and application thereof | |
| CN114847292B (en) | Sterilization composition containing zoxamide and fludioxonil and application thereof | |
| CN114747582B (en) | Pesticide composition containing Isoflucypram and copper quinolinate and application thereof | |
| CN101669496A (en) | Bifenazate and milbemectin miticide composition and application thereof | |
| CN107372522A (en) | A kind of composition pesticide containing fenazaquin | |
| CN101543219A (en) | Sterilizing composite compounded by diniconazole and tea saponin, preparation method and application thereof | |
| CN106689162B (en) | A kind of bactericidal composition of second containing pheno mycin and pyraclostrobin | |
| CN104488913A (en) | Buprofezin-containing insecticidal composition |
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 |