CN109169646A - Oil-suspending agent and preparation method thereof can be dispersed in a kind of dinotefuran - Google Patents
Oil-suspending agent and preparation method thereof can be dispersed in a kind of dinotefuran Download PDFInfo
- Publication number
- CN109169646A CN109169646A CN201811199895.0A CN201811199895A CN109169646A CN 109169646 A CN109169646 A CN 109169646A CN 201811199895 A CN201811199895 A CN 201811199895A CN 109169646 A CN109169646 A CN 109169646A
- Authority
- CN
- China
- Prior art keywords
- dinotefuran
- oil
- emulsifier
- preparation
- agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- YKBZOVFACRVRJN-UHFFFAOYSA-N dinotefuran Chemical compound [O-][N+](=O)\N=C(/NC)NCC1CCOC1 YKBZOVFACRVRJN-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 239000000375 suspending agent Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000003921 oil Substances 0.000 claims abstract description 88
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000002270 dispersing agent Substances 0.000 claims abstract description 46
- 239000002562 thickening agent Substances 0.000 claims abstract description 40
- 239000000839 emulsion Substances 0.000 claims abstract description 19
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 238000004945 emulsification Methods 0.000 claims abstract description 6
- 235000019198 oils Nutrition 0.000 claims description 84
- 239000000470 constituent Substances 0.000 claims description 41
- -1 methylamino Avermectin Chemical compound 0.000 claims description 29
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 28
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 28
- 239000003963 antioxidant agent Substances 0.000 claims description 19
- 230000003078 antioxidant effect Effects 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 150000002191 fatty alcohols Chemical class 0.000 claims description 12
- 239000003002 pH adjusting agent Substances 0.000 claims description 12
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 9
- 229920005646 polycarboxylate Polymers 0.000 claims description 9
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical group CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims description 8
- 229920001400 block copolymer Polymers 0.000 claims description 8
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 claims description 8
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 claims description 8
- 229940073769 methyl oleate Drugs 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- 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 7
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 claims description 7
- SPSPIUSUWPLVKD-UHFFFAOYSA-N 2,3-dibutyl-6-methylphenol Chemical compound CCCCC1=CC=C(C)C(O)=C1CCCC SPSPIUSUWPLVKD-UHFFFAOYSA-N 0.000 claims description 6
- 239000005660 Abamectin Substances 0.000 claims description 6
- 229960000892 attapulgite Drugs 0.000 claims description 6
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 6
- 229960000878 docusate sodium Drugs 0.000 claims description 6
- 239000002480 mineral oil Substances 0.000 claims description 6
- 235000010446 mineral oil Nutrition 0.000 claims description 6
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 claims description 6
- 229910052625 palygorskite Inorganic materials 0.000 claims description 6
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 claims description 6
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 5
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 239000000600 sorbitol Substances 0.000 claims description 5
- 239000004255 Butylated hydroxyanisole Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005903 Gamma-cyhalothrin Substances 0.000 claims description 4
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 4
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 claims description 4
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical compound [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 claims description 4
- 235000019282 butylated hydroxyanisole Nutrition 0.000 claims description 4
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 4
- 229940043253 butylated hydroxyanisole Drugs 0.000 claims description 4
- 239000002285 corn oil Substances 0.000 claims description 4
- 235000005687 corn oil Nutrition 0.000 claims description 4
- 239000006071 cream Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- ZXQYGBMAQZUVMI-GCMPRSNUSA-N gamma-cyhalothrin Chemical compound CC1(C)[C@@H](\C=C(/Cl)C(F)(F)F)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-GCMPRSNUSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 239000001739 pinus spp. Substances 0.000 claims description 4
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000004250 tert-Butylhydroquinone Substances 0.000 claims description 4
- 235000019281 tert-butylhydroquinone Nutrition 0.000 claims description 4
- 229940036248 turpentine Drugs 0.000 claims description 4
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 4
- 239000008158 vegetable oil Substances 0.000 claims description 4
- 239000004615 ingredient Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 244000068988 Glycine max Species 0.000 claims description 2
- 235000010469 Glycine max Nutrition 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 2
- DNIKXCUKOGVNIO-UHFFFAOYSA-N formaldehyde;phenol;styrene Chemical compound O=C.OC1=CC=CC=C1.C=CC1=CC=CC=C1 DNIKXCUKOGVNIO-UHFFFAOYSA-N 0.000 claims description 2
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 claims 1
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 claims 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 claims 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- 229920005610 lignin Polymers 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 27
- 239000002245 particle Substances 0.000 abstract description 14
- 238000003860 storage Methods 0.000 abstract description 9
- 230000000857 drug effect Effects 0.000 abstract description 8
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000003090 pesticide formulation Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 29
- 239000008367 deionised water Substances 0.000 description 26
- 229910021641 deionized water Inorganic materials 0.000 description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 20
- 235000006708 antioxidants Nutrition 0.000 description 15
- 238000010907 mechanical stirring Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- 229920001732 Lignosulfonate Polymers 0.000 description 7
- 229960001777 castor oil Drugs 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 235000012424 soybean oil Nutrition 0.000 description 6
- 239000003549 soybean oil Substances 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](NC)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000004996 alkyl benzenes Chemical group 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000013641 positive control Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- JBDFNORUNVZONM-UHFFFAOYSA-N 4-octoxy-4-oxo-3-sulfobutanoic acid Chemical compound CCCCCCCCOC(=O)C(S(O)(=O)=O)CC(O)=O JBDFNORUNVZONM-UHFFFAOYSA-N 0.000 description 1
- 241000931705 Cicada Species 0.000 description 1
- 241001498622 Cixius wagneri Species 0.000 description 1
- 241000254173 Coleoptera Species 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 241000257303 Hymenoptera Species 0.000 description 1
- 241000255777 Lepidoptera Species 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 241001556089 Nilaparvata lugens Species 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 240000000528 Ricinus communis Species 0.000 description 1
- 235000004443 Ricinus communis Nutrition 0.000 description 1
- 241000176086 Sogatella furcifera Species 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- VVUBWCWVDFCEOP-UHFFFAOYSA-N benzene;styrene Chemical compound C1=CC=CC=C1.C=CC1=CC=CC=C1 VVUBWCWVDFCEOP-UHFFFAOYSA-N 0.000 description 1
- 235000021329 brown rice Nutrition 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- UZRCGISJYYLJMA-UHFFFAOYSA-N phenol;styrene Chemical compound OC1=CC=CC=C1.C=CC1=CC=CC=C1 UZRCGISJYYLJMA-UHFFFAOYSA-N 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000001032 spinal nerve Anatomy 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to Pesticide formulation technical fields, and in particular to oil-suspending agent and preparation method thereof can be dispersed in a kind of dinotefuran.The preparation method of oil-suspending agent can be dispersed in dinotefuran provided by the present invention, comprising: a) in a heated condition, dinotefuran, the first emulsifier, dispersing agent and water is mixed, dissolution obtains dinotefuran aqua；B) the second emulsifier, thickener and oil base are mixed, obtains miscible oil；C) under high-speed stirred state, the dinotefuran aqua of step a) is added in the miscible oil of step b), emulsification obtains W/O emulsion.The present invention, which takes water as a solvent, is pre-dissolved dinotefuran, and then emulsion dispersion forms W/O emulsion into oil base, so that the dinotefuran diameter of particle being precipitated in drop is nanoscale, excellent storage stability, diffusion velocity is fast, and drug effect is high.
Description
Technical field
The invention belongs to Pesticide formulation technical fields, and in particular to oil-suspending agent and its system can be dispersed in a kind of dinotefuran
Preparation Method.
Background technique
Dinotefuran, for the third generation nicotinic insecticide of Mitsui chemical company exploitation, desinsection wide spectrum is nicotinic Acetyl
The excitant of choline receptor transmits the cynapse for influencing insect CNS by spinal nerves, has to tag and make with stomach toxicity
With and there is brilliant interior suction osmosis.Dinotefuran is fool proof to mammal, birds and aquatile, to crop without medicine
Evil, the various pests such as Semiptera, Lepidoptera, coleoptera, Diptera, Hymenoptera can be prevented and treated, to Brown Planthopper, white backed planthopper,
Small brown rice planthopper, night tail cicada etc. have very high preventive effect.
Dinotefuran belongs to a kind of slightly solubility active constituent, is neither easy to be dissolved in water isopolarity solvent, in 25 DEG C of water
Solubility be only 40g/L, be also not easily dissolved in medium and small polar solvent.For slightly solubility active constituent, in the formulation
Partial size it is smaller, the particle number of dispersion is more, and surface area is bigger, the drug effect of performance bigger with the contact area of target organisms
It is bigger.
Dispersible oil-suspending agent is the high dispersive stable suspersion system with non-aqueous system (oil base) for decentralized medium, is with one
Class can be used as builder through overtesting and not pollute a kind of dosage form of the oils of crop as dilution carrier, and it is living that pesticide can be improved
The permeability and absorbability of property ingredient, there is good synergistic effect.Currently, using dinotefuran as the dispersible oil of main active
Suspending agent mainly uses direct polishing or sand-blast, pesticide activity component, dispersing agent and other auxiliary agents is mixed, pre-dispersed
It is ground later, or is placed on grinding distribution in sand mill in pre-dispersed.However, can be divided as made from the above method
The particle diameter distribution for dissipating active constituent in oil-suspending agent is wide, and for partial size often at 0.5 μm or more, drug effect is low, and storage stability is poor, and sand
During mill between sanding media (bead, zirconium pearl), sanding media and cavity inner wall mutually collide, rub, filtering nothing can be generated
The stability of oil-suspending agent can be dispersed in the mechanical admixture that method is rejected, the impurity effect of introducing.Chinese patent 201610739132.5
Disclosing a kind of dinotefuran can be dispersed oil-suspending agent and preparation method thereof, and using direct polishing, preparation partial size is 2~4 μm.
Summary of the invention
The main purpose of the present invention is to provide the preparation methods that oil-suspending agent can be dispersed in a kind of dinotefuran, it is intended to solve existing
Dinotefuran diameter of particle is larger in the preparation for having preparation process to obtain, and drug effect is low, introduces the technical problems such as mechanical admixture.
In order to solve the above-mentioned technical problem, an aspect of of the present present invention, providing a kind of dinotefuran can be dispersed oil-suspending agent
Preparation method, comprising:
A) in a heated condition, dinotefuran, the first emulsifier, dispersing agent and water are mixed, dissolution obtains dinotefuran water
Agent；
B) the second emulsifier, thickener and oil base are mixed, obtains miscible oil；
C) under high-speed stirred state, the dinotefuran aqua of step a) is added in the miscible oil of step b), is emulsified
To W/O emulsion.
On the other hand, the present invention also provides a kind of dinotefuran, and oil-suspending agent can be dispersed, and is W/O emulsion, the W/O cream
Contain nanoscale dinotefuran crystal fine grain in the drop of shape liquid；
Preparing raw material by it is in terms of 100 parts by weight, comprising: 5~30 parts of dinotefuran；Second 0~30 part of active constituent；Cream
8~20 parts of agent；2~4 parts of dispersing agent；5~15 parts of water；0~3 part of thickener；0~1 part of antioxidant；PH adjusting agent 0~0.3
Part；Oil base is supplied.
In the technical solution of the present invention, by using the dinotefuran characteristic that solubility increased dramatically in the hot water, using water
Dinotefuran is dissolved as solvent, then the first emulsifier and dispersing agent are added in the aqueous solution of dinotefuran and carry out pre-dispersed, shape
At the dinotefuran aqua of homogeneous phase, then dinotefuran aqua is added in miscible oil mix under high-speed stirred state and is stirred
It mixes；During stirring, dinotefuran aqua occurs to emulsify and formed with ultra-fine nanosized liquid droplets in miscible oil
W/O emulsion, simultaneously as temperature decline causes dinotefuran to form nucleus in nanosized liquid droplets, so that system of the present invention
The partial size of active constituent in agent more refines, and reaches nanoscale.
Compared with prior art, the present invention, which takes water as a solvent, is pre-dissolved dinotefuran, and then emulsion dispersion forms W/O into oil base
Emulsion drop, so that dinotefuran diameter of particle is nanoscale, excellent storage stability, diffusion velocity is fast, and drug effect is high；The present invention utilizes
Water reduces environmental pollution as solvent, saves cost of material, safe ready, and water or interface stability agent, and there is thickening to make
With enhancing preparation stored stability substitutes part oil base, reduces cost.
Specific embodiment
Larger in order to solve dinotefuran diameter of particle in the preparation that existing preparation process obtains, drug effect is low, it is mechanical miscellaneous to introduce
The technical problems such as matter.The embodiment of the invention provides the preparation methods that oil-suspending agent can be dispersed in a kind of dinotefuran, and water is used to make
For solvent, and the preparation of the dinotefuran particle containing ultra-fine grain diameter is made, excellent storage stability, diffusion velocity is fast, and drug effect is high.
The preparation method of oil-suspending agent can be dispersed in a kind of dinotefuran of the invention, comprising:
A) in a heated condition, dinotefuran, the first emulsifier, dispersing agent and water are mixed, dissolution obtains dinotefuran water
Agent；
B) the second emulsifier, thickener and oil base are mixed, obtains miscible oil；
C) under high-speed stirred state, the dinotefuran aqua of step a) is added in the miscible oil of step b), is emulsified
To W/O emulsion.
In the above-mentioned technical solutions, solubility of the dinotefuran in 25 DEG C of water is only 40g/L, when water temperature is greater than 60 DEG C,
Solubility is greater than 2000g/L, and the embodiment of the present invention is by using using the dinotefuran characteristic that solubility increased dramatically in the hot water
Water dissolves dinotefuran as solvent, and environmentally protective, production and application is highly-safe.
The present invention is pre-dispersed by will carry out in the first emulsifier and the aqueous solution of dispersing agent addition dinotefuran, and is made
The dinotefuran aqua of one phase；Then, dinotefuran aqua is added in miscible oil under high-speed stirred state and carries out continuing stirring；
During stirring, dinotefuran aqua occurs to emulsify in miscible oil and forms the W/O with ultra-fine nanosized liquid droplets
Emulsion, simultaneously as temperature decline causes dinotefuran to form nucleus in nanosized liquid droplets.It overcomes and passes through in the prior art
It is wide that active constituent particle diameter distribution in dispersible oil-suspending agent obtained is directly sanded, the poor problem of storage stability, and avoid
Introducing mechanical admixture, high production efficiency, stability are good.Thus, the preparation as made from above-mentioned preparation method, active constituent
Grain diameter nano, particle diameter distribution is narrow, and excellent storage stability, diffusion velocity is fast, and drug effect is high.
Further, the dinotefuran of step a) of the present invention and emulsifying dispersant be added to the water the sequence of mixing without successively it
Point；Moreover, the water as solvent can heat in advance, can also be heated again after dinotefuran and water mixing, or in furan
Worm amine and emulsifying dispersant are all heated with after water mixing again.
In some currently preferred embodiments of the present invention, step a) specifically: dinotefuran is dissolved by heating in water, is added the
One emulsifier and dispersing agent mix, and obtain dinotefuran aqua.
In other some preferred embodiments, step a) specifically: by dinotefuran, the first emulsifier, dispersing agent and water
Mixing dissolves by heating, and forms dinotefuran aqua；Or are as follows: the first emulsifier, dispersing agent, dinotefuran are sequentially added in the hot water,
Dissolution mixing, forms dinotefuran aqua.
High-speed stirred is primarily to enable dinotefuran aqua fully emulsified in miscible oil, and it is enough to form partial size
Small W/O emulsion droplet, improving dinotefuran of the embodiment of the present invention can be dispersed the stability of oil-suspending agent.
Preferably, the revolving speed of step c) high-speed stirred is in 500~10000rpm or more；Mixing time is in 0.5h or more.
As the revolving speed high-speed stirred 0.5h to be greater than 10000rpm, emulsifying effectiveness is optimal, and W/O emulsion system is relatively stable,
Situations such as being less prone to particle sedimentation layering.
The linear velocity of dinotefuran aqua addition miscible oil is excessive to be easy to cause emulsification pretreatment insufficient, so that size droplet diameter
It is bigger than normal, however, the linear velocity of dinotefuran aqua addition miscible oil is too small and production efficiency can be reduced.
Preferably, it is 10~50m/min that the linear velocity of miscible oil, which is added, in dinotefuran aqua in step c).
The water solubility of dinotefuran is poor, and when temperature is lower than 50 DEG C, solubility in water is lower, and dissolution dinotefuran needs
More water are added, water is excessive to be easy to cause the dispersible oil-suspending agent of the embodiment of the present invention feeding-up, and leads to size droplet diameter
It is excessive, reduce the stability of W/O emulsion.
Preferably, the temperature that step a) is dissolved by heating is 50~80 DEG C.
The problems such as in emulsion process, the dosage of water is excessive, is easy to cause demulsification, drop big, system retrogradation, when water and the
The mass ratio of one emulsifier is (5~15): when (8~12), can avoid that the demulsification as caused by excess moisture, drop is excessive and body
The problems such as being retrogradation, guarantees the stability and particle size of preparation, and then guarantees the dinotefuran particle fine in drop.Work as water
When being greater than 15:8 with the mass ratio of the first emulsifier, W/O emulsion is feeding-up, and size droplet diameter is excessive, and stability reduces.
Preferably, dinotefuran, water, the first emulsifier and dispersing agent mass ratio be (5~30): (5~15): (8~
12): (2~4).
Further, the mass ratio of miscible oil and dinotefuran aqua is 1:(0.1~1), conducive to W/O lotion is formed, protect
It is complete to demonstrate,prove water emulsification, obtains nanometer particle.
In embodiments of the present invention, step b) further includes being added: the second active constituent, antioxidant and pH is added and adjusts
Agent；
Second active constituent, antioxidant, pH adjusting agent, the second emulsifier and thickener mass ratio be preferably 1:(0~
2): (0~0.5): (0.1~10): (0.1~2).
In some preferred embodiments, go back while being added in step b): the second active constituent, antioxidant and pH are adjusted
Agent；Second active constituent, antioxidant, pH adjusting agent, the second emulsifier and thickener mass ratio be 1:(0.1~2):
(0.01~0.5): (0.1~10): (0.1~2).
In other preferred embodiments, goes back while being added in step b): the second active constituent and antioxidant；Second is living
Property ingredient, antioxidant, the second emulsifier and thickener mass ratio be 1:(0.1~2): (0.1~10): (0.1~2)；
Or are as follows: it goes back while being added in step b): the second active constituent and pH adjusting agent；Second active constituent, pH are adjusted
The mass ratio of agent, the second emulsifier and thickener is 1:(0.01~0.5): (0.1~10): (0.1~2).
Further, the second active constituent of the embodiment of the present invention is preferably emamectin-benzoate, AVM hereinafter
Any one in rhzomorph, Nylar, gamma cyhalothrin and chlopyrifos.
By previous experiments optimal screening, emamectin-benzoate, avermectin, Nylar, efficient chlorine fluorine
Cyano chrysanthemate and chlopyrifos oil-soluble are good, can be dissolved in oil base, and have synergistic function with dinotefuran.
Antioxidant is added, can prevent active constituent oxidation by air from decomposing.Preferably, the embodiment of the present invention is anti-
Oxidant is preferably one of dibutyl hydroxy toluene, butylated hydroxy anisole and tert-butylhydroquinone or a variety of.
Dibutyl hydroxy toluene, butylated hydroxy anisole and tert-butylhydroquinone have stronger oxidation resistance, and
Oil-soluble is good, can be dissolved in oil base.
Fractions of active ingredient is stablized within the scope of specific pH, is easy to decompose beyond pH range.Preferably, the present invention is real
The pH adjusting agent for applying example is preferably one of hydrochloric acid, glacial acetic acid and citric acid or a variety of.
Hydrochloric acid, glacial acetic acid and citric acid have the sour effect of preferable tune, and hydrochloric acid, glacial acetic acid room temperature are that mobility is preferable
Liquid, is solid under citric acid room temperature, and when use facilitates measurement to use, convenient for operation.
In embodiments of the present invention, the first emulsifier and the second emulsifier are each independently selected from alkylbenzene sulfonate, two
Octyl sulfosuccinate, fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, anhydrous sorbitol polyoxyethylene polyoxy third
One of alkene, styryl phenyl polyoxyethylene ether and styrene phenol formaldehyde resin polyoxyethylene ether are a variety of；
First emulsifier is different from the second emulsifier.
Further, the first emulsifier is preferably alkylbenzene sulfonate, dioctyl sulfosuccinate, fatty alcohol polyoxy second
Alkene ether, castor oil polyoxyethylene ether, anhydrous sorbitol polyoxyethylene polyoxypropylene, styryl phenyl polyoxyethylene ether and benzene second
One of alkene phenol formaldehyde resin polyoxyethylene ether.
Second emulsifier is preferably alkylbenzene sulfonate, dioctyl sulfosuccinate, fatty alcohol polyoxyethylene ether, castor-oil plant
Oily polyoxyethylene ether, anhydrous sorbitol polyoxyethylene polyoxypropylene, styryl phenyl polyoxyethylene ether and styrene phenol first
One or both of urea formaldehyde polyoxyethylene ether.
In embodiments of the present invention, it is poly- to be selected from lignosulfonates, polycarboxylate, naphthalene sulfonate and polyoxyethylene for dispersing agent
One of oxypropylene block copolymer is a variety of.Lignosulfonates, polycarboxylate, naphthalene sulfonate and polyoxyethylene polyoxy third
Alkene block copolymer there is preferable drop to stick dispersion effect dinotefuran, and good compatibility, and can compound with most of emulsifier makes
With.
In embodiments of the present invention, thickener in white carbon black, attapulgite, aluminium-magnesium silicate and organobentonite one
Kind is a variety of.White carbon black, attapulgite, aluminium-magnesium silicate and the adjustable dispersible oil-suspending agent of organobentonite viscosity, shape
At tridimensional network, stabilization of solid particle, and then delayed fallout.
In embodiments of the present invention, oil base is preferably trimethylbenzene, S-100 (No. 100 solvent naphthas), S-150 (No. 150 solvents
Oil), S-200 (No. 200 solvent naphthas), sec-Butyl Acetate, methyl oleate, turpentine-based vegetable oil, soybean oil, corn oil and mineral oil
One of or it is a variety of, property stablize, source is wide, and viscosity is low, and safety is higher.
Based on above-mentioned preparation method, the present invention also provides a kind of dinotefuran, and oil-suspending agent can be dispersed, and is W/O emulsion,
Contain nanoscale dinotefuran crystal fine grain in the drop of W/O emulsion；
Preparing raw material by it is in terms of 100 parts by weight, comprising: 5~30 parts of dinotefuran；Second 0~30 part of active constituent；Cream
8~20 parts of agent；2~4 parts of dispersing agent；5~15 parts of water；0~3 part of thickener；0~1 part of antioxidant；PH adjusting agent 0~0.3
Part；Oil base is supplied；
Second active constituent is selected from emamectin-benzoate, avermectin, Nylar, gamma cyhalothrin
With any one in chlopyrifos.
Further, the partial size of the dinotefuran crystal fine grain in W/O of embodiment of the present invention emulsion in drop be 200nm~
500nm。
Further, emulsifier be selected from alkylbenzene sulfonate, dioctyl sulfosuccinate, fatty alcohol polyoxyethylene ether,
Castor oil polyoxyethylene ether, anhydrous sorbitol polyoxyethylene polyoxypropylene, styryl phenyl polyoxyethylene ether and styrene benzene
One of fluosite polyoxyethylene ether is or a variety of；And/or
Dispersing agent is selected from lignosulfonates, polycarboxylate, naphthalene sulfonate and polyoxyethylene polyoxypropylene block copolymer
One of or it is a variety of；And/or
Thickener is selected from one of white carbon black, attapulgite, aluminium-magnesium silicate and organobentonite or a variety of；And/or
Antioxidant is selected from one of dibutyl hydroxy toluene, butylated hydroxy anisole and tert-butylhydroquinone or more
Kind；And/or
PH adjusting agent is selected from one of hydrochloric acid, glacial acetic acid and citric acid or a variety of；And/or
Oil base is selected from trimethylbenzene, S-100, S-150, S-200, sec-Butyl Acetate, methyl oleate, turpentine-based vegetable oil, big
One of soya-bean oil, corn oil and mineral oil are a variety of.
In order to which technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Specific embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to
It explains the present invention, is not intended to limit the present invention.
Embodiment 1
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 1:
Table 1
Its prepare the following steps are included:
S11, dinotefuran and deionized water are mixed, 56 DEG C is heated under 1000rpm stirring, so that dinotefuran is completely molten
Solution is in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S12, the second emulsifier, thickener and oil base are mixed, mechanical stirring obtains miscella to uniform at 800 rpm
Agent；
The dinotefuran aqua of step S11 is added dropwise to by S13, the high-speed stirred at 10000rpm by the linear velocity of 10m/min
It is persistently stirred in the miscible oil of step S12, obtains that oil-suspending agent can be dispersed containing 5% dinotefuran.
Embodiment 2
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 2:
Table 2
| Component | Content | Remarks |
| Dinotefuran | 5% | First active constituent |
| Methylaminoemamectin benzoate | 1% | Second active constituent |
| Deionized water | 5% | Solvent |
| Fatty alcohol polyoxyethylene ether | 8% | First emulsifier |
| Alkylbenzene sulfonate | 3% | Second emulsifier |
| Lignosulfonates | 2% | Dispersing agent |
| Organobentonite | 1% | Thickener |
| White carbon black | 2% | Thickener |
| Dibutyl hydroxy toluene | 1% | Antioxidant |
| Trimethylbenzene | 5% | Oil base |
| Methyl oleate | Supply 100% | Oil base |
Its prepare the following steps are included:
S21, dinotefuran and deionized water are mixed, 56 DEG C is heated under 500rpm stirring, so that dinotefuran is completely molten
Solution is in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S22, the second active constituent, the second emulsifier, thickener, antioxidant and oil base are mixed, the machine at 1000rpm
Tool is stirred until homogeneous, and obtains miscible oil；
The dinotefuran aqua of step S21 is added dropwise to by S23, the high-speed stirred at 8000rpm by the linear velocity of 30m/min
It is persistently stirred in the miscible oil of step S22, it is outstanding to obtain the dispersible oil containing 6% dinotefuran emamectin-benzoate
Floating agent.
Embodiment 3
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 3:
Table 3
| Component | Content | Remarks |
| Dinotefuran | 10% | First active constituent |
| Distilled water | 8% | Solvent |
| Styryl phenol polyethenoxy ether | 10% | First emulsifier |
| Alkylbenzene sulfonate | 4% | Second emulsifier |
| Polycarboxylate | 2% | Dispersing agent |
| Attapulgite | 2% | Thickener |
| Soybean oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S31, dinotefuran and solvent are mixed, 58 DEG C is heated under 500rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S32, the second emulsifier, thickener and oil base are mixed, mechanical stirring obtains miscella to uniform at 700rpm
Agent；
The dinotefuran aqua of step S31 is added dropwise to by S33, the high-speed stirred at 10000rpm by the linear velocity of 50m/min
In the miscible oil of step S32, obtain that oil-suspending agent can be dispersed containing 10% dinotefuran.
Embodiment 4
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 4:
Table 4
| Component | Content | Remarks |
| Dinotefuran | 10% | First active constituent |
| Avermectin | 2% | Second active constituent |
| Distilled water | 8% | Solvent |
| Styryl phenol polyethenoxy ether | 10% | First emulsifier |
| Alkylbenzene sulfonate | 4% | Second emulsifier |
| Polycarboxylate | 2% | Dispersing agent |
| Attapulgite | 2% | Thickener |
| Dibutyl hydroxy toluene | 1% | Antioxidant |
| Sec-Butyl Acetate | 10% | Oil base |
| Soybean oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S41, dinotefuran and solvent are mixed, 58 DEG C is heated under 1000rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S42, the second active constituent, the second emulsifier, thickener, antioxidant and oil base are mixed, at 600 rpm machine
Tool is stirred until homogeneous, and obtains miscible oil；
S43, under 8000rpm high-speed stirred, the dinotefuran aqua of step S41 is added dropwise to by the linear velocity of 40m/min
It is persistently stirred in the miscible oil of step S42, obtains that oil-suspending agent can be dispersed containing 12% dinotefuran avermectin.
Embodiment 5
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 5:
Table 5
| Component | Content | Remarks |
| Dinotefuran | 15% | First active constituent |
| Distilled water | 10% | Solvent |
| Fatty alcohol polyoxyethylene ether | 8% | First emulsifier |
| Sorbierite polyoxy ether | 4% | Second emulsifier |
| Alkylbenzene sulfonate | 3% | Second emulsifier |
| Naphthalene sulfonate | 2% | Dispersing agent |
| Organobentonite | 1.5% | Thickener |
| Mineral oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S51, dinotefuran and solvent are mixed, 58 DEG C is heated under 9000rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S52, the second emulsifier, thickener and oil base are mixed, mechanical stirring is mixed to uniform at 1000rpm
Finish；
The dinotefuran aqua of step S31 is added dropwise to by S53, the high-speed stirred at 20000rpm by the linear velocity of 30m/min
In the miscible oil of step S32, obtain that oil-suspending agent can be dispersed containing 15% dinotefuran.
Embodiment 6
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 6:
Table 6
Its prepare the following steps are included:
S61, dinotefuran and solvent are mixed, 58 DEG C is heated under 700rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S62, the second reactive compound, the second emulsifier, thickener and oil base are mixed, in 600rpm mechanical stirring to equal
It is even, obtain miscible oil；
S63, under 10000rpm high-speed stirred, the dinotefuran aqua of step S61 is added dropwise to by the linear velocity of 40m/min
In the miscible oil of step S62, obtain that oil-suspending agent can be dispersed containing 20% dinotefuran Nylar.
Embodiment 7
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 7:
Table 7
| Component | Content | Remarks |
| Dinotefuran | 20% | First active constituent |
| Distilled water | 10% | Solvent |
| Fatty alcohol polyoxyethylene ether | 8% | First emulsifier |
| Alkylbenzene sulfonate | 5% | Second emulsifier |
| Polyoxyethylene polyoxypropylene block copolymer | 4% | Dispersing agent |
| White carbon black | 1% | Thickener |
| Soybean oil | 20% | Oil base |
| Methyl oleate | Supply 100% | Oil base |
Its prepare the following steps are included:
S71, dinotefuran and solvent are mixed, 62 DEG C is heated under 500rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S72, the second emulsifier, thickener and oil base are mixed, mechanical stirring obtains miscella to uniform at 700rpm
Agent；
S73, under 20000rpm high-speed stirred, the dinotefuran aqua of step S71 is added dropwise to by the linear velocity of 30m/min
In the miscible oil of step S72, obtain that oil-suspending agent can be dispersed containing 20% dinotefuran.
Embodiment 8
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 8:
Table 8
Its prepare the following steps are included:
S81, dinotefuran and solvent are mixed, 62 DEG C is heated under 500rpm stirring, so that dinotefuran is dissolved completely in
In deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S82, the second reactive compound, the second emulsifier, thickener, pH adjusting agent and oil base are mixed, at 1000rpm
Mechanical stirring obtains miscible oil to uniform；
S83, under 10000rpm high-speed stirred, the dinotefuran aqua of step S81 is added dropwise to by the linear velocity of 20m/min
In the miscible oil of step S82, obtain that oil-suspending agent can be dispersed containing 24% dinotefuran gamma cyhalothrin.
Embodiment 9
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 9:
Table 9
| Component | Content | Remarks |
| Dinotefuran | 25% | First active constituent |
| Deionized water | 13% | Solvent |
| Styryl phenol polyethenoxy ether | 8% | First emulsifier |
| Alkylbenzene sulfonate | 4% | Second emulsifier |
| Castor oil polyoxyethylene ether | 3% | Second emulsifier |
| Polycarboxylate | 2% | Dispersing agent |
| Organobentonite | 1% | Thickener |
| Soybean oil | 15% | Oil base |
| Mineral oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S91, dinotefuran and deionized water are mixed, 70 DEG C is heated under 500rpm stirring, so that dinotefuran is completely molten
Solution is in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S92, the second emulsifier, thickener and oil base are mixed, mechanical stirring obtains miscella to uniform at 600 rpm
Agent；
S93, under 20000rpm high-speed stirred, the dinotefuran aqua of step S91 is added dropwise to by the linear velocity of 40m/min
In the miscible oil of step S92, obtain that oil-suspending agent can be dispersed containing 25% dinotefuran.
Embodiment 10
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 10:
Table 10
| Component | Content | Remarks |
| Dinotefuran | 20% | First active constituent |
| Nylar | 10% | Second active constituent |
| Deionized water | 12% | Solvent |
| Styryl phenol polyethenoxy ether | 8% | First emulsifier |
| Alkylbenzene sulfonate | 4% | Second emulsifier |
| Castor oil polyoxyethylene ether | 3% | Second emulsifier |
| Polycarboxylate | 2% | Dispersing agent |
| Organobentonite | 1% | Thickener |
| S-150 | 15% | Oil base |
| Methyl oleate | Supply 100% | Oil base |
Its prepare the following steps are included:
S101, dinotefuran and deionized water are mixed, 70 DEG C is heated under 700rpm stirring, so that dinotefuran is completely molten
Solution is in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S102, the second active constituent, the second emulsifier, thickener and oil base are mixed, mechanical stirring is extremely at 900rpm
Uniformly, miscible oil is obtained；
S103, under 20000rpm high-speed stirred, the dinotefuran aqua of step S101 is added dropwise to the mixing of step S102
In finish, obtain that oil-suspending agent can be dispersed containing 30% dinotefuran Nylar.
Embodiment 11
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 11:
Table 11
| Component | Content | Remarks |
| Dinotefuran | 30% | First active constituent |
| Deionized water | 15% | Solvent |
| Fatty alcohol polyoxyethylene ether | 12% | First emulsifier |
| Dioctyl sulfosuccinate | 8% | Second emulsifier |
| Polyoxyethylene polyoxypropylene block copolymer | 2% | Dispersing agent |
| Lignosulfonates | 2% | Dispersing agent |
| Organobentonite | 0.5% | Thickener |
| Mineral oil | 15% | Oil base |
| Methyl oleate | Supply 100% | Oil base |
Its prepare the following steps are included:
S111, dinotefuran and deionized water are mixed, 70 DEG C is heated under 700rpm stirring, so that dinotefuran is completely molten
Solution is in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S112, the second emulsifier, thickener and oil base are mixed, mechanical stirring is mixed to uniform at 900rpm
Finish；
S113, under 15000rpm high-speed stirred, by the dinotefuran aqua of step S111 by 50m/min linear velocity be added dropwise
In the miscible oil for entering step S112, obtain that oil-suspending agent can be dispersed containing 30% dinotefuran.
Embodiment 12
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 12:
Table 12
| Component | Content | Remarks |
| Dinotefuran | 15% | First active constituent |
| Chlopyrifos | 15% | Second active constituent |
| Deionized water | 8% | Solvent |
| Fatty alcohol polyoxyethylene ether | 12% | First emulsifier |
| Dioctyl sulfosuccinate | 8% | Second emulsifier |
| Polyoxyethylene polyoxypropylene block copolymer | 2% | Dispersing agent |
| Lignosulfonates | 2% | Dispersing agent |
| Organobentonite | 1.5% | Thickener |
| S-200 | 15% | Oil base |
| Corn oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S121, dinotefuran and deionized water are mixed, 65 DEG C is heated under 1000rpm stirring, so that dinotefuran is complete
It is dissolved in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S122, the second active constituent, the second emulsifier, thickener and oil base are mixed, mechanical stirring is extremely at 900rpm
Uniformly, miscible oil is obtained；
S123, under 10000rpm high-speed stirred, by the dinotefuran aqua of step S121 by 40m/min linear velocity be added dropwise
In the miscible oil for entering step S122, obtain that oil-suspending agent can be dispersed containing 30% dinotefuran chlopyrifos.
Embodiment 13
A kind of dispersible oil-suspending agent of dinotefuran is present embodiments provided, formula such as the following table 13:
Table 13
| Component | Content | Remarks |
| Dinotefuran | 10% | First active constituent |
| Chlopyrifos | 30% | Second active constituent |
| Deionized water | 8% | Solvent |
| Fatty alcohol polyoxyethylene ether | 12% | First emulsifier |
| Alkylbenzene sulfonate | 8% | Second emulsifier |
| Polyoxyethylene polyoxypropylene block copolymer | 2% | Dispersing agent |
| Lignosulfonates | 2% | Dispersing agent |
| Organobentonite | 1.5% | Thickener |
| White carbon black | 1.5% | Thickener |
| S-200 | 20% | Oil base |
| Turpentine-based vegetable oil | Supply 100% | Oil base |
Its prepare the following steps are included:
S131, dinotefuran and deionized water are mixed, 60 DEG C is heated under 1000rpm stirring, so that dinotefuran is complete
It is dissolved in deionized water；The first emulsifier is added and dispersing agent continues to stir, obtains dinotefuran aqua；
S132, the second active constituent, the second emulsifier, thickener and oil base are mixed, mechanical stirring is extremely at 700rpm
Uniformly, miscible oil is obtained；
S133, under 10000rpm high-speed stirred, by the dinotefuran aqua of step S131 by 30m/min linear velocity be added dropwise
In the miscible oil for entering step S132, obtain that oil-suspending agent can be dispersed containing 40% dinotefuran chlopyrifos.
Comparative example 1
Oil-suspending agent can be dispersed in 10% dinotefuran, is prepared using sand-blast, is formulated as follows:
By weight percentage 100% meter, weighs 10% dinotefuran, polycarboxylate 2%, styryl phenol polyethenoxy ether
8%, alkylbenzene sulfonate 4%, castor oil polyoxyethylene ether 3%, organobentonite 2%, white carbon black 2%, methyl oleate are supplied
100%.
Preparation method: said components being sufficiently mixed and are placed on grinding distribution in sand mill, and being sanded to partial size is 5 μm of left sides
Oil-suspending agent can be dispersed after refiltering up to 10% dinotefuran in the right side.
Comparative example 2
Oil-suspending agent can be dispersed in 20% dinotefuran, is prepared using sand-blast, is formulated as follows:
By weight percentage 100% meter, it is total to weigh 20% dinotefuran, naphthalene sulfonate 2%, polyoxyethylene polyoxypropylene block
Polymers 2%, fatty alcohol polyoxyethylene ether 8%, sorbierite polyoxy ether 4%, alkylbenzene sulfonate 3%, organobentonite 1%,
White carbon black 1%, soybean oil 100%.
Preparation method: said components being sufficiently mixed and are placed on grinding distribution in sand mill, and being sanded to partial size is 5 μm of left sides
Oil-suspending agent can be dispersed after refiltering up to 20% dinotefuran in the right side.
Test case
The dinotefuran of Example 1~13 can be dispersed oil-suspending agent and carry out stability test, including heat-storage test and cold
Jelly storage test after storing 14 days under the conditions of 54 DEG C and storing 7 days respectively under the conditions of -5 DEG C, is observed appearance after storing, is hanged
Floating rate, dispersibility, partial size.
Wherein, oil-suspending agent and 20% dinotefuran can be dispersed with 10% dinotefuran that comparative example 1 and comparative example 2 respectively obtain
Dispersible oil-suspending agent is compared as positive control.
Table 14 and table 15 are test result, and as shown in the results, oil-suspending agent can be dispersed in the dinotefuran of the embodiment of the present invention
Appearance is uniform, good fluidity, cold and hot storage qualified stability.It is compared with positive control, the dinotefuran of the embodiment of the present invention
Oil-suspending agent can be dispersed better than the dinotefuran of sand-blast preparation in the storage stability of dispersible oil-suspending agent, with excellent cold and hot
Stability is store, oil-suspending agent can be dispersed also superior to dinotefuran prepared by sand-blast in the project indicators such as partial size, suspensibility.
Table 14
Table 15
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. the preparation method that oil-suspending agent can be dispersed in a kind of dinotefuran characterized by comprising
A) in a heated condition, dinotefuran, the first emulsifier, dispersing agent and water are mixed, dissolution obtains dinotefuran aqua；
B) the second emulsifier, thickener and oil base are mixed, obtains miscible oil；
C) under high-speed stirred state, the dinotefuran aqua of step a) is added in the miscible oil of step b), emulsification obtains W/O
Emulsion.
2. preparation method according to claim 1, which is characterized in that the revolving speed of the step c) high-speed stirred 500~
10000rpm or more；Mixing time is in 0.5h or more.
3. preparation method according to claim 1, which is characterized in that the temperature of the step a) heating for dissolving is 50~80
℃。
4. preparation method according to any one of claims 1 to 3, which is characterized in that the dinotefuran, water, the first emulsification
The mass ratio of agent and dispersing agent is (5~30): (5~15): (8~12): (2~4).
5. preparation method according to any one of claims 1 to 3, which is characterized in that the miscible oil and the furan worm
The mass ratio of aqueous amine agent is 1:(0.1~1).
6. preparation method according to any one of claims 1 to 3, which is characterized in that step b) further include: it is living to be added second
Property ingredient, antioxidant and pH adjusting agent；
Second active constituent, antioxidant, pH adjusting agent, the second emulsifier and thickener mass ratio be 1:(0~2):
(0~0.5): (0.1~10): (0.1~2).
7. preparation method according to claim 6, which is characterized in that second active constituent is selected from methylamino Avermectin
Any one in plain benzoate, avermectin, Nylar, gamma cyhalothrin and chlopyrifos；And/or
The antioxidant is selected from one of dibutyl hydroxy toluene, butylated hydroxy anisole and tert-butylhydroquinone or more
Kind；And/or
The pH adjusting agent is selected from one of hydrochloric acid, glacial acetic acid and citric acid or a variety of.
8. preparation method according to any one of claims 1 to 3, which is characterized in that first emulsifier and the second cream
Agent is each independently selected from alkylbenzene sulfonate, dioctyl sulfosuccinate, fatty alcohol polyoxyethylene ether, castor oil polyoxy
Vinethene, anhydrous sorbitol polyoxyethylene polyoxypropylene, styryl phenyl polyoxyethylene ether and styrene phenol formaldehyde resin
One of polyoxyethylene ether is a variety of；
First emulsifier is different from the second emulsifier.
9. preparation method according to any one of claims 1 to 3, which is characterized in that the dispersing agent is selected from sulfomethylated lignin
One of hydrochlorate, polycarboxylate, naphthalene sulfonate and polyoxyethylene polyoxypropylene block copolymer are a variety of；And/or
The thickener is selected from one of white carbon black, attapulgite, aluminium-magnesium silicate and organobentonite or a variety of；And/or
The oil base is selected from trimethylbenzene, S-100, S-150, S-200, sec-Butyl Acetate, methyl oleate, turpentine-based vegetable oil, big
One of soya-bean oil, corn oil and mineral oil are a variety of.
10. oil-suspending agent can be dispersed in a kind of dinotefuran, which is characterized in that be W/O emulsion, in the drop of the W/O emulsion
Contain nanoscale dinotefuran crystal fine grain；
Preparing raw material by it is in terms of 100 parts by weight, comprising: 5~30 parts of dinotefuran；Second 0~30 part of active constituent；Emulsifier
8~20 parts；2~4 parts of dispersing agent；5~15 parts of water；0~3 part of thickener；0~1 part of antioxidant；0~0.3 part of pH adjusting agent；
Oil base is supplied.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811199895.0A CN109169646B (en) | 2018-10-15 | 2018-10-15 | Dinotefuran dispersible oil suspending agent and preparation method thereof |
| AU2019360278A AU2019360278A1 (en) | 2018-10-15 | 2019-09-10 | Dinotefuran oil-based suspension concentrate and preparation method therefor |
| PCT/CN2019/105168 WO2020078145A1 (en) | 2018-10-15 | 2019-09-10 | Dinotefuran oil-based suspension concentrate and preparation method therefor |
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| CN201811199895.0A CN109169646B (en) | 2018-10-15 | 2018-10-15 | Dinotefuran dispersible oil suspending agent and preparation method thereof |
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| CN109169646B CN109169646B (en) | 2020-12-29 |
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| Country | Link |
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| CN (1) | CN109169646B (en) |
| AU (1) | AU2019360278A1 (en) |
| WO (1) | WO2020078145A1 (en) |
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| WO2020078145A1 (en) * | 2018-10-15 | 2020-04-23 | 深圳诺普信农化股份有限公司 | Dinotefuran oil-based suspension concentrate and preparation method therefor |
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| CN115104620B (en) * | 2021-08-13 | 2023-08-11 | 山东恒利达生物科技有限公司 | Furannicotine insecticidal composition and application thereof |
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| DE102005048539A1 (en) * | 2005-10-11 | 2007-04-12 | Bayer Cropscience Ag | Suspension concentrates based on oil |
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| CN104126602B (en) * | 2014-08-18 | 2016-06-22 | 陕西上格之路生物科学有限公司 | A kind of dispersible oil-suspending agent containing pymetrozine and MTI-446 |
| CN109315420B (en) * | 2018-10-15 | 2021-10-19 | 深圳诺普信农化股份有限公司 | Dinotefuran oil suspension hot fogging concentrate and preparation method thereof |
| CN109169646B (en) * | 2018-10-15 | 2020-12-29 | 深圳诺普信农化股份有限公司 | Dinotefuran dispersible oil suspending agent and preparation method thereof |
| CN109221226B (en) * | 2018-10-15 | 2021-03-12 | 深圳诺普信农化股份有限公司 | Dinotefuran dispersible oil suspending agent for flight control and preparation method thereof |
| CN109463392B (en) * | 2018-10-15 | 2021-05-14 | 深圳诺普信农化股份有限公司 | Dinotefuran oil-based seed coating agent and preparation method thereof |
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2018
- 2018-10-15 CN CN201811199895.0A patent/CN109169646B/en active Active
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- 2019-09-10 WO PCT/CN2019/105168 patent/WO2020078145A1/en active Application Filing
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| AU2019360278A1 (en) | 2021-01-07 |
| WO2020078145A1 (en) | 2020-04-23 |
| CN109169646B (en) | 2020-12-29 |
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