CN114642212B - Suspending agent containing terbuthylazine and fenpyrad and preparation method thereof - Google Patents
Suspending agent containing terbuthylazine and fenpyrad and preparation method thereof Download PDFInfo
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- CN114642212B CN114642212B CN202210415620.6A CN202210415620A CN114642212B CN 114642212 B CN114642212 B CN 114642212B CN 202210415620 A CN202210415620 A CN 202210415620A CN 114642212 B CN114642212 B CN 114642212B
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- CN
- China
- Prior art keywords
- terbuthylazine
- agent
- agents
- fenpyrad
- suspension containing
- Prior art date
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- FZXISNSWEXTPMF-UHFFFAOYSA-N terbutylazine Chemical compound CCNC1=NC(Cl)=NC(NC(C)(C)C)=N1 FZXISNSWEXTPMF-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000005621 Terbuthylazine Substances 0.000 title claims abstract description 44
- 239000000375 suspending agent Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 239000000725 suspension Substances 0.000 claims abstract description 24
- 239000000080 wetting agent Substances 0.000 claims abstract description 23
- 239000004480 active ingredient Substances 0.000 claims abstract description 17
- 239000002562 thickening agent Substances 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 24
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 23
- 239000013530 defoamer Substances 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 16
- 239000003755 preservative agent Substances 0.000 claims description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- 229920000570 polyether Polymers 0.000 claims description 14
- 230000002335 preservative effect Effects 0.000 claims description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 12
- TVFWYUWNQVRQRG-UHFFFAOYSA-N 2,3,4-tris(2-phenylethenyl)phenol Chemical compound C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 TVFWYUWNQVRQRG-UHFFFAOYSA-N 0.000 claims description 11
- -1 alkyl naphthalene sulfonate formaldehyde Chemical compound 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 7
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 230000002528 anti-freeze Effects 0.000 claims description 6
- 150000002191 fatty alcohols Chemical class 0.000 claims description 6
- 239000000230 xanthan gum Substances 0.000 claims description 6
- 229920001285 xanthan gum Polymers 0.000 claims description 6
- 229940082509 xanthan gum Drugs 0.000 claims description 6
- 235000010493 xanthan gum Nutrition 0.000 claims description 6
- 229920001732 Lignosulfonate Polymers 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 240000007263 Pinus koraiensis Species 0.000 claims description 3
- 235000011615 Pinus koraiensis Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- NHFDKKSSQWCEES-UHFFFAOYSA-N dihydrogen phosphate;tris(2-hydroxyethyl)azanium Chemical compound OP(O)(O)=O.OCCN(CCO)CCO NHFDKKSSQWCEES-UHFFFAOYSA-N 0.000 claims description 3
- 229920002866 paraformaldehyde Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 230000001502 supplementing effect Effects 0.000 claims description 2
- KJADKKWYZYXHBB-XBWDGYHZSA-N Topiramic acid Chemical compound C1O[C@@]2(COS(N)(=O)=O)OC(C)(C)O[C@H]2[C@@H]2OC(C)(C)O[C@@H]21 KJADKKWYZYXHBB-XBWDGYHZSA-N 0.000 claims 6
- 229960004394 topiramate Drugs 0.000 claims 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 125000003827 glycol group Chemical group 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000004546 suspension concentrate Substances 0.000 claims 1
- IYMLUHWAJFXAQP-UHFFFAOYSA-N topramezone Chemical compound CC1=C(C(=O)C2=C(N(C)N=C2)O)C=CC(S(C)(=O)=O)=C1C1=NOCC1 IYMLUHWAJFXAQP-UHFFFAOYSA-N 0.000 claims 1
- 241000196324 Embryophyta Species 0.000 abstract description 23
- 239000000575 pesticide Substances 0.000 abstract description 11
- 239000003814 drug Substances 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 2
- 230000000857 drug effect Effects 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 9
- 238000009472 formulation Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 244000234609 Portulaca oleracea Species 0.000 description 3
- 239000007900 aqueous suspension Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- RZRILSWMGXWSJY-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;sulfuric acid Chemical compound OS(O)(=O)=O.OCCN(CCO)CCO RZRILSWMGXWSJY-UHFFFAOYSA-N 0.000 description 2
- 239000005592 Penoxsulam Substances 0.000 description 2
- 241000227425 Pieris rapae crucivora Species 0.000 description 2
- 235000001855 Portulaca oleracea Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 240000008042 Zea mays Species 0.000 description 2
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 2
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 235000005822 corn Nutrition 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005338 heat storage Methods 0.000 description 2
- 230000002363 herbicidal effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- MFSWTRQUCLNFOM-UHFFFAOYSA-N methyl 2-(4-{[3-chloro-5-(trifluoromethyl)pyridin-2-yl]oxy}phenoxy)propanoate Chemical group C1=CC(OC(C)C(=O)OC)=CC=C1OC1=NC=C(C(F)(F)F)C=C1Cl MFSWTRQUCLNFOM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- JPMIIZHYYWMHDT-UHFFFAOYSA-N octhilinone Chemical compound CCCCCCCCN1SC=CC1=O JPMIIZHYYWMHDT-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000004260 weight control Methods 0.000 description 2
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 1
- CASLETQIYIQFTQ-UHFFFAOYSA-N 3-[[5-(difluoromethoxy)-1-methyl-3-(trifluoromethyl)pyrazol-4-yl]methylsulfonyl]-5,5-dimethyl-4h-1,2-oxazole Chemical compound CN1N=C(C(F)(F)F)C(CS(=O)(=O)C=2CC(C)(C)ON=2)=C1OC(F)F CASLETQIYIQFTQ-UHFFFAOYSA-N 0.000 description 1
- 241000219144 Abutilon Species 0.000 description 1
- 241000219318 Amaranthus Species 0.000 description 1
- 235000017060 Arachis glabrata Nutrition 0.000 description 1
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- 208000003643 Callosities Diseases 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000001602 Digitaria X umfolozi Nutrition 0.000 description 1
- 235000017898 Digitaria ciliaris Nutrition 0.000 description 1
- 235000005476 Digitaria cruciata Nutrition 0.000 description 1
- 235000006830 Digitaria didactyla Nutrition 0.000 description 1
- 235000005804 Digitaria eriantha ssp. eriantha Nutrition 0.000 description 1
- 235000010823 Digitaria sanguinalis Nutrition 0.000 description 1
- 244000025670 Eleusine indica Species 0.000 description 1
- 235000014716 Eleusine indica Nutrition 0.000 description 1
- 238000012424 Freeze-thaw process Methods 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
- 244000020551 Helianthus annuus Species 0.000 description 1
- 235000003222 Helianthus annuus Nutrition 0.000 description 1
- 206010020649 Hyperkeratosis Diseases 0.000 description 1
- ROKXSHQOEYMQJR-UHFFFAOYSA-N N.C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 Chemical compound N.C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 ROKXSHQOEYMQJR-UHFFFAOYSA-N 0.000 description 1
- SYJGKVOENHZYMQ-UHFFFAOYSA-N Penoxsulam Chemical compound N1=C2C(OC)=CN=C(OC)N2N=C1NS(=O)(=O)C1=C(OCC(F)F)C=CC=C1C(F)(F)F SYJGKVOENHZYMQ-UHFFFAOYSA-N 0.000 description 1
- 239000005820 Prochloraz Substances 0.000 description 1
- 241000219053 Rumex Species 0.000 description 1
- 235000010086 Setaria viridis var. viridis Nutrition 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 240000006394 Sorghum bicolor Species 0.000 description 1
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 1
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 241000219094 Vitaceae Species 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007798 antifreeze agent Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 125000004786 difluoromethoxy group Chemical group [H]C(F)(F)O* 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 244000230342 green foxtail Species 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- CTAPFRYPJLPFDF-UHFFFAOYSA-N isoxazole Chemical compound C=1C=NOC=1 CTAPFRYPJLPFDF-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 230000003285 pharmacodynamic effect Effects 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- TVLSRXXIMLFWEO-UHFFFAOYSA-N prochloraz Chemical compound C1=CN=CN1C(=O)N(CCC)CCOC1=C(Cl)C=C(Cl)C=C1Cl TVLSRXXIMLFWEO-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- 238000009333 weeding Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
- A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
- A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
-
- 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
- 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
- A01N25/24—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—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 characterised by the surfactants
-
- 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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a suspending agent containing terbuthylazine and fenpyrad, which comprises the following components in percentage by mass: 40-60% of active ingredient, 4-10% of dispersing agent, 1-5% of wetting agent, 0.1-4% of thickening agent and 0.2-3% of defoaming agent; the active ingredients comprise terbuthylazine and metazopyr. The invention prepares the terbuthylazine and the fenpyrad into the suspending agent, and expands the weed killing spectrum. The dispersing agent is preferably selected, so that the problems of high product viscosity and easy creaming and bottoming during storage are effectively solved, the problems of product skinning are solved by preferably selecting the wetting agent and the antifreezing agent, the stability of the product under the low-temperature condition is improved, and the technical difficulty of the high-content suspending agent is overcome. The prepared suspending agent ensures higher suspension rate in water, and proper wetting agent is added, the drug holding capacity on the plant surface is increased, so that the drug effect is more remarkable, and the pollution of pesticides to the environment is reduced.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a suspending agent containing terbuthylazine and fenpyrad and a preparation method thereof.
Background
Terbuthylazine, chemical name: 2-chloro-4-terbutamino-6-ethylamino-1, 3, 5-triazine, terbutazine is a selective systemic conduction herbicide, can be absorbed from roots before germination, can also permeate into plants from stems and leaves, is transported into green leaves to inhibit photosynthesis, and generally has better effect on the weeds which just germinate. The weeding composition is suitable for crops such as corns, sorghum, soybeans, pomace fruit trees, oranges, grapes and the like, can prevent and remove annual broadleaf weeds and grassy weeds, has better effect on broadleaf weeds than grassy weeds, and has poor effect on perennial weeds.
The terbuthylazine is singly used, the use amount is large, and broadleaf weeds can not be effectively prevented and removed.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a suspending agent containing terbuthylazine and metazopyr and a preparation method thereof, and the prepared suspending agent has higher stability.
The invention provides a suspending agent containing terbuthylazine and fenpyrad, which comprises the following components in percentage by mass:
40 to 60 percent of active ingredient, 4 to 10 percent of dispersing agent, 1 to 5 percent of wetting agent, 0.1 to 4 percent of thickening agent and 0.2 to 3 percent of defoaming agent;
the active ingredients comprise terbuthylazine and metazopyr.
Penoxsulam (Pyroxasulfone), chemical name: 3- [5- (difluoromethoxy) -1-methyl-3- (trifluoromethyl) pyrazol-4-ylmethyl sulfonyl ] -4, 5-dihydro-5, 5-dimethyl-1, 2-isoxazole belongs to novel isoxazole herbicides, has wide application crops, is mainly used for crops such as corn, cotton, peanut, wheat, sunflower and the like, and can effectively prevent and remove broadleaf weeds such as green bristlegrass, crabgrass, barnyard and the like, amaranthus, stramonium, eggplant and abutilon and the like.
According to the invention, terbuthylazine and metazopyr are compounded, the synergistic effect of terbuthylazine and metazopyr is exerted, and the suspension formulation is obtained. In the process of producing and preparing a suspension formulation, the terbuthylazine and the fenpyrad have different properties, the terbuthylazine has strong lipophilicity, the risk of particle aggregation exists in the formulation, the density of the fenpyrad raw medicine is higher, and the risk of sedimentation exists in the formulation, so that the two formulations are difficult to prepare as a high-content water suspension. Meanwhile, the content is higher, the water content is lower, and the wetting and mixing of the slurry are difficult; meanwhile, in the suspending agent with high content, the wetting and dispersing agent cannot be well adsorbed and evenly dispersed on the surfaces of the raw medicine particles, so that the viscosity of the system is higher, and the surface layer is easy to crust; in the suspending agent with high concentration, the probability of particle movement collision is larger than that of the suspending agent with low concentration, the intermolecular distance is short, particles are gathered, the conditions of skinning and bottom formation are easy to occur during storage, and the fluidity of the product is poor. In order to solve the problems, the invention adjusts the composition and the proportion of auxiliary agents aiming at specific suspension formulations, finally solves the problems of skinning and bottoming, and ensures the stability of the preparation under the low-temperature condition.
In the invention, the suspending agent containing terbuthylazine and fenpyrad can also comprise an antifreezing agent and/or a preservative.
The mass content of the antifreezing agent is preferably 3-10%.
The mass content of the preservative is preferably 0.1% -2%.
Preferably, the suspending agent containing terbuthylazine and fenpyrad comprises the following components in percentage by mass:
40-60% of active ingredients, 4-10% of dispersing agents, 1-5% of wetting agents, 0.1-4% of thickening agents, 0.2-3% of defoaming agents, 3-10% of antifreezing agents and 0.1-2% of preservatives; the deionized water is used for supplementing 100 percent;
the active ingredients comprise terbuthylazine and metazopyr.
The mass ratio of the terbuthylazine to the fenpyrad is preferably (1-11): 1, more preferably (1 to 6): 1, more preferably (1 to 4.5): 1, may specifically be 1:1, 1.5:1, 2.67:1, 4.5:1, 9:1, 10:1, 11:1, or a range value with any of the above values as an upper or lower limit.
The mass content of terbuthylazine is preferably 20% to 55%, more preferably 20% to 45%, and may specifically be 20%, 30%, 40%, 45%, 50%, 55%, or a range having any of the above values as an upper limit or a lower limit.
The mass content of the haloxyfop-methyl is preferably 5% to 20%, more preferably 10% to 20%, and may specifically be 5%, 10%, 15%, 20%, or a range having any of the above values as an upper limit or a lower limit.
The content of the dispersant is preferably 4% to 10%, more preferably 4% to 8%, and specifically may be 4%, 5%, 6%, 7%, 8%, 9%, 10%, or a range having any of the above values as an upper limit or a lower limit.
The dispersing agent preferably comprises one or more of lignosulfonate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, styrene acrylic acid copolymer, styrene maleic anhydride copolymer sodium salt, alkyl naphthalene sulfonate formaldehyde condensate, tristyrylphenol polyoxyethylene ether sulfate ammonium salt and methyl methacrylate copolyoxyethylene ether; more preferably one or more of lignosulfonate, styrene acrylic acid copolymer, methyl methacrylate copolyoxyethylene ether, tristyrylphenol polyoxyethylene ether sulfate triethanolamine salt, tristyrylphenol polyoxyethylene ether sulfate ammonium salt, and alkyl naphthalene sulfonate formaldehyde condensate; further, a mixed dispersant of methyl methacrylate polyoxyethylene ether and an ammonium salt of tristyrylphenol polyoxyethylene ether sulfate is preferable, and the mass ratio of the methyl methacrylate polyoxyethylene ether to the ammonium salt of tristyrylphenol polyoxyethylene ether sulfate is preferably 1 (1 to 5), more preferably 1:2.
Preferably, the dispersing agent comprises a first dispersing agent and a second dispersing agent, wherein the first dispersing agent is selected from lignin sulfonate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt or tristyrylphenol polyoxyethylene ether sulfate ammonium salt; the second dispersant is selected from styrene acrylic copolymer, alkyl naphthalene sulfonate formaldehyde condensate or methyl methacrylate copolymerized polyoxyethylene ether.
The mass ratio of the first dispersant to the second dispersant is preferably (1-2): 1, the number of the components is 1, specifically, the ratio can be 1:1, 1.67:1 or 2:1.
In some embodiments of the invention, the dispersant is selected from the group consisting of lignosulfonate 2% + styrene acrylic acid copolymer 2% combination.
In some embodiments of the invention, the dispersant is selected from the group consisting of a 5% + alkyl naphthalene sulfonate formaldehyde condensate 3% combination of tristyrylphenol polyoxyethylene ether sulfate triethanolamine salt.
In some embodiments of the invention, the dispersant is selected from the group consisting of a 4% + methyl methacrylate co-polyoxyethylene ether 2% combination of an ammonium tristyrylphenol polyoxyethylene ether sulfate salt.
The mass content of the wetting agent is preferably 1% to 5%, and specifically may be 1%, 2%, 3%, 4%, 5%, or a range having any of the above values as an upper limit or a lower limit.
The wetting agent preferably comprises one or more of propylene oxide-ethylene oxide block polyether, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether and lauryl fatty alcohol polyoxyethylene ether; more preferably propylene oxide-ethylene oxide block polyether or fatty alcohol polyoxyethylene ether, and still more preferably propylene oxide-ethylene oxide block polyether 2%.
In some embodiments of the present invention, the wetting agent is selected from 5% of propylene oxide-ethylene oxide block polyether.
In some embodiments of the invention, the wetting agent is selected from the group consisting of propylene oxide-ethylene oxide block polyethers 2%.
In some embodiments of the invention, the wetting agent is selected from the group consisting of fatty alcohol polyoxyethylene ether 1%.
The invention reduces the viscosity of the product by selecting specific dispersing agent and wetting agent for compounding, improves the stability of the dosage form, is favorable for wetting target plants by liquid medicine, and effectively solves the problem of bottom formation by higher suspension rate and moderate product viscosity.
The mass content of the thickener is preferably 0.1% to 4%, and specifically may be 0.1%, 0.15%, 1%, 3%, 4%, or a range having any of the above values as an upper limit or a lower limit.
The thickener preferably comprises one or more of magnesium aluminum silicate, organic bentonite, xanthan gum and common white carbon black, and more preferably common white carbon black or xanthan gum.
In some embodiments of the invention, the thickener is selected from the group consisting of 0.1% xanthan gum.
In some embodiments of the invention, the thickener is selected from xanthan gum 0.15%.
In some embodiments of the invention, the thickener is selected from the group consisting of 4% of ordinary white carbon.
The mass content of the defoaming agent is preferably 0.2 to 3%, more preferably 0.2 to 0.5%, and specifically may be 0.2%, 0.5%, 1%, 3%, or a range having any of the above values as an upper limit or a lower limit.
The defoamer preferably comprises one or more of polyether defoamer, organosilicon defoamer and polyether modified polysiloxane defoamer, more preferably polyether defoamer or organosilicon defoamer;
in some embodiments of the invention, the defoamer is a polyether defoamer of 0.5%.
In some embodiments of the invention, the defoamer is a silicone defoamer of 0.2%.
The mass content of the antifreeze is preferably 3% to 10%, more preferably 3% to 7%, and particularly may be 3%, 4%, 5%, 7%, or a range having any of the above values as an upper limit or a lower limit.
The antifreeze agent preferably comprises one or more of urea, ethylene glycol, propylene glycol and glycerol, more preferably ethylene glycol or glycerol. The invention selects the specific antifreezing agent, so that the product is not frozen in a low-temperature environment and has good storage stability.
In some embodiments of the invention, the antifreeze is selected from ethylene glycol 3%.
In some embodiments of the invention, the antifreeze is selected from ethylene glycol 5%.
In some embodiments of the invention, the antifreeze is selected from glycerol 4%.
The mass content of the preservative is preferably 0.1% to 2%, more preferably 0.1% to 1.5%, and specifically may be 0.1%, 0.5%, 1.5%, 2%, or a range having any of the above values as an upper limit or a lower limit.
The preservative preferably comprises one or more of kathon, paraformaldehyde, sodium benzoate, more preferably kathon.
In some embodiments of the invention, the preservative is selected from sodium benzoate 1.5%.
In some embodiments of the invention, the preservative is selected from 0.1% of pinus koraiensis.
In some embodiments of the invention, the preservative is selected from 0.5% paraformaldehyde.
When the suspending agent is an aqueous suspending agent, the system is 100% complemented with deionized water.
The percentages in the present invention are weight percentages unless otherwise indicated.
The invention provides a preparation method of the suspension containing terbuthylazine and fenpyrad, which comprises the following steps:
uniformly mixing a wetting agent, a dispersing agent, a preservative, a defoaming agent, an antifreezing agent and water, then adding a thickening agent and an active ingredient under a high-speed shearing condition, uniformly mixing, and grinding to obtain the suspension containing terbuthylazine and fenpyrad.
Preferably, the high-speed shearing speed is 1000-10000 r/min.
Preferably, the thickener and the active ingredient are added, and then sheared for 10-30 min to uniformly mix the system.
Preferably, the grinding is specifically grinding until the particle size D90 of the mixture is smaller than 6 μm.
In the present invention, the grinding may be performed by any grinding method known in the art, for example, grinding may be performed under zirconia bead sanding medium. After grinding, the particles were measured by a laser particle size distribution analyzer until the particle diameter D90 was less than 6. Mu.m.
Compared with the prior art, the invention provides a suspending agent containing terbuthylazine and metazopyr, which comprises the following components in percentage by mass: 40-60% of active ingredients, 4-10% of dispersing agents, 1-5% of wetting agents, 0.1-4% of thickening agents, 0.2-3% of defoaming agents, 3-10% of antifreezing agents and 0.1-2% of preservatives; the active ingredients comprise terbuthylazine and metazopyr.
The invention firstly compounds terbuthylazine and the haloxyfop-methyl and prepares the suspending agent, wherein the terbutryn-penoxsulam suspending agent has higher content, the use amount of terbuthylazine is reduced by adding the active ingredient of the fenpyrad through compounding, and the weed control spectrum is enlarged. The problems of high product viscosity, easy creaming during storage and bottom formation are effectively solved by optimizing the dispersing agent, and the problems of product skinning are solved by optimizing the wetting agent. After production and during transportation, the product may be exposed to freezing temperatures. Freezing of the suspending agent may lead to irreversible changes, and thus the ability of the formulation to resist repeated freeze-thaw processes is an important property in assessing product stability. The stability of the product under low temperature conditions is improved by the preferential antifreezing agent. The prepared suspending agent ensures higher suspension rate in water, meets the requirements of mechanical operation in the market, and adds a proper wetting agent to increase the drug holding capacity on the plant surface and reduce the pesticide loss, so that the pesticide effect is more obvious, and the pollution of the pesticide to the environment is also reduced. The preparation process is simple and convenient, is environment-friendly and pollution-free, and has good market application prospect.
Detailed Description
In order to further illustrate the present invention, the suspending agent containing terbuthylazine and metazopyr and the preparation method thereof provided by the present invention are described in detail below with reference to examples.
Examples 1 to 7
According to the proportion of tables 1-2, uniformly mixing a wetting agent, a dispersing agent, a preservative, a defoaming agent, an antifreezing agent and water, then adding a thickening agent and an active ingredient under the high-speed shearing condition of 1000-10000 r/min, shearing for 10-30 min to uniformly mix the systems, and grinding until the particle size D90 of the mixture is smaller than 6 mu m to obtain the suspension containing terbuthylazine and fenpyr-diethyl.
Comparative example 1
According to the proportions in Table 2, the method was the same as in examples 1 to 7, preparing a suspending agent containing terbuthylazine and fenpyrad.
Table 1 examples 1 to 4 ratios of the respective raw materials
Table 2 proportions of the raw materials of examples 5 to 7 and comparative example 1
Performance detection
The properties of the aqueous suspensions prepared in the above examples and comparative examples were examined, and the results are shown in Table 3 below. Wherein, the suspension rate is detected according to the GB/T14825-2006 pesticide suspension rate determination method; the pourability is detected according to the GB/T31737-2015 pesticide pourability detection method; the wet sieve test is carried out according to an MT 185 measurement method, and the skinning condition of the sample is judged according to the wet sieve residue; viscosity was measured according to CIPAC method MT 192. Freeze-thaw stability measurement criteria: the freeze-thaw stability test was performed at four cycles between room temperature (20+ -2deg.C) and (-10+ -2deg.C), each cycle being 18h frozen and 6h thawed.
TABLE 3 Properties of aqueous suspension prepared by compounding terbuthylazine and Prochloraz
As is clear from Table 3, the product of comparative example 1 has higher viscosity, and a large amount of skinning occurs when the glass bottle passes through the filament glass bottle and is thermally stored at 54 ℃, the residual amount of the wet sieve which does not pass through the 200-mesh sieve reaches 10%, the bottom of the bottle has the phenomenon of caking, the fluidity of the appearance is poor, the sample is thickened, and the suspension rate is also greatly reduced. Examples 3,5, 6 and 7 have higher viscosity, slightly lower quality after heat storage, less than 2% of wet sieve passing through a 200-mesh sieve, lower suspension rate and meet FAO standard; examples 1,2 and 4 were better in quality, examples 1 and 2 were better in fluidity at normal temperature, and had little skinning after heat storage, less than 1%, with example 4 being the best in quality. In the freeze-thawing stability test, the suspension rates of examples 2, 3 and 7 are lower, the recovery fluidity of examples 1, 4,5 and 6 is better, and the suspension rate of example 4 is highest. Indicating that the preferred adjuvants play a critical role in product quality.
Field test
The test was carried out in a greenhouse from Shandong province, shandong WeiFang Rumex, chemical industry Co., ltd. Selecting commercially available 50% terbuthylazine suspending agent, 40% metazopyr suspending agent and pesticide combination of the invention of example 4 and comparative example 1, mixing into a medicinal liquid according to mass concentration of test design after conversion of field area and basin area for later use, and using g a.i/hm 2 The amount of pesticide applied was calculated using clear water as a control. Selecting plump and uniform gramineous weed brome seeds and broadleaf weed purslane seeds, respectively sowing 20 seeds, and then uniformly covering. After treatment, the cells were incubated in a greenhouse, and 3 groups were repeated for each treatment. The bottom of the pot is irrigated to completely moisten soil and the pesticide is applied after emergence of seedlings.
After the application, the victim symptoms of the brome and the purslane are observed regularly, the residual plant numbers and the fresh weight parts on the ground of the brome and the purslane are counted after the application for 21 days, and the plant control effect and the fresh weight control effect of each treatment are calculated according to the following formula.
Plant control (%) = (number of weed plants in control group-number of weed plants in treatment group)/number of weed plants in control group x 100%; fresh weight control (%) = (fresh weight of control group weed-fresh weight of treated group weed)/fresh weight of control group weed x 100%;
TABLE 4 data of pharmacodynamic experiments
Table 5 raw data recording table of drug effect
The results show that the matching of active components in the pesticide composition reduces the dosage of herbicide so as to reduce the cost of the pesticide, and meanwhile, the matching of auxiliary agents such as wetting agent, antifreezing agent and the like is optimized, so that the problem of easy skinning of the product is solved, and the stability of the product is improved.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (10)
1. A suspending agent containing terbuthylazine and metazopyr, which comprises the following components in percentage by mass:
40-60% of active ingredients, 4-10% of dispersing agents, 1-5% of wetting agents, 0.1-4% of thickening agents and 0.2-3% of defoaming agents;
the active ingredients comprise terbuthylazine and metazopyr;
the dispersing agent comprises a first dispersing agent and a second dispersing agent, wherein the first dispersing agent is selected from lignin sulfonate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt or tristyrylphenol polyoxyethylene ether sulfate ammonium salt; the second dispersant is selected from styrene acrylic acid copolymer, alkyl naphthalene sulfonate formaldehyde condensate or methyl methacrylate copolymerized polyoxyethylene ether;
the mass ratio of the first dispersing agent to the second dispersing agent is (1-2): 1.
2. the suspension containing terbuthylazine and topiramate according to claim 1, further comprising: antifreeze and/or preservative.
3. The suspension containing terbuthylazine and topiramate according to claim 2, characterized by comprising, in mass content:
40-60% of active ingredients, 4-10% of dispersing agents, 1-5% of wetting agents, 0.1-4% of thickening agents, 0.2-3% of defoaming agents, 3-10% of antifreezing agents and 0.1-2% of preservatives; the deionized water is used for supplementing 100 percent;
the active ingredients comprise terbuthylazine and metazopyr.
4. The suspension containing terbuthylazine and topiramate according to claim 1, wherein said wetting agent comprises one or more of propylene oxide-ethylene oxide block polyether, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene polyoxypropylene ether, lauryl fatty alcohol polyoxyethylene ether.
5. The suspension containing terbuthylazine and topiramate according to claim 4, wherein said wetting agent is selected from propylene oxide-ethylene oxide block polyethers or fatty alcohol-polyoxyethylene ethers.
6. The suspension containing terbuthylazine and topiramate according to claim 1, wherein said thickener comprises one or more of magnesium aluminum silicate, organic bentonite, xanthan gum and ordinary white carbon black;
the defoamer comprises one or more of polyether defoamer, organic silicon defoamer and polyether modified polysiloxane defoamer.
7. The suspension containing terbuthylazine and topramezone according to claim 6, wherein said thickener is selected from the group consisting of plain white carbon black and xanthan gum;
the defoamer is selected from polyether defoamer or organosilicon defoamer.
8. The suspension containing terbuthylazine and fenpyrad according to claim 2, characterized in that the antifreeze comprises one or more of urea, ethylene glycol, propylene glycol, glycerol;
the preservative comprises one or more of pinus koraiensis, paraformaldehyde and sodium benzoate.
9. The suspension concentrate containing terbuthylazine and topiramate according to claim 8, wherein,
the antifreezing agent is selected from glycol or glycerol;
the preservative is selected from the group consisting of pinus koraiensis.
10. The preparation method of the suspension containing terbuthylazine and fenpyrad according to any one of claims 1-9, comprising the following steps:
uniformly mixing a wetting agent, a dispersing agent, a preservative, a defoaming agent, an antifreezing agent and water, then adding a thickening agent and an active ingredient under a high-speed shearing condition, uniformly mixing, and grinding to obtain the suspension containing terbuthylazine and fenpyrad.
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BR102022012950-9A BR102022012950A2 (en) | 2022-04-20 | 2022-06-29 | SUSPENSION CONCENTRATE CONTAINING TERBUTHYLAZINE AND PYROXASULFONE AND METHOD OF PREPARATION THEREOF |
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CN103202308A (en) * | 2006-12-21 | 2013-07-17 | 组合化学工业株式会社 | Herbicide composition |
CN109526973A (en) * | 2018-12-14 | 2019-03-29 | 青岛清原化合物有限公司 | Ternary weeding composition and its application comprising sulfone pyrrole grass azoles |
CN112931517A (en) * | 2019-12-11 | 2021-06-11 | 北京颖泰嘉和生物科技股份有限公司 | Herbicide composition and application thereof |
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CN103202308A (en) * | 2006-12-21 | 2013-07-17 | 组合化学工业株式会社 | Herbicide composition |
CN109526973A (en) * | 2018-12-14 | 2019-03-29 | 青岛清原化合物有限公司 | Ternary weeding composition and its application comprising sulfone pyrrole grass azoles |
CN112931517A (en) * | 2019-12-11 | 2021-06-11 | 北京颖泰嘉和生物科技股份有限公司 | Herbicide composition and application thereof |
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