CN114097784B - Emulsifiable concentrate containing metolachlor and sulfenamide and preparation method thereof - Google Patents
Emulsifiable concentrate containing metolachlor and sulfenamide and preparation method thereof Download PDFInfo
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- CN114097784B CN114097784B CN202111527232.9A CN202111527232A CN114097784B CN 114097784 B CN114097784 B CN 114097784B CN 202111527232 A CN202111527232 A CN 202111527232A CN 114097784 B CN114097784 B CN 114097784B
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- sulfenamide
- metolachlor
- emulsifiable concentrate
- preparation
- ether
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- WVQBLGZPHOPPFO-UHFFFAOYSA-N 2-chloro-N-(2-ethyl-6-methylphenyl)-N-(1-methoxypropan-2-yl)acetamide Chemical compound CCC1=CC=CC(C)=C1N(C(C)COC)C(=O)CCl WVQBLGZPHOPPFO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical compound [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 239000004495 emulsifiable concentrate Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 9
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 9
- DMAXMXPDVWTIRV-UHFFFAOYSA-N 2-(2-phenylethyl)phenol Chemical compound OC1=CC=CC=C1CCC1=CC=CC=C1 DMAXMXPDVWTIRV-UHFFFAOYSA-N 0.000 claims description 7
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 6
- -1 tridecyl fatty alcohol Chemical class 0.000 claims description 5
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims description 4
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 claims description 4
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 claims description 4
- 229940073769 methyl oleate Drugs 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- HNXNKTMIVROLTK-UHFFFAOYSA-N n,n-dimethyldecanamide Chemical compound CCCCCCCCCC(=O)N(C)C HNXNKTMIVROLTK-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000003995 emulsifying agent Substances 0.000 abstract description 13
- 239000004480 active ingredient Substances 0.000 abstract description 11
- 238000009472 formulation Methods 0.000 abstract description 10
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000006184 cosolvent Substances 0.000 abstract description 5
- 239000000839 emulsion Substances 0.000 abstract description 5
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 230000001804 emulsifying effect Effects 0.000 abstract description 3
- 239000000575 pesticide Substances 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 2
- 239000006071 cream Substances 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 19
- 238000011282 treatment Methods 0.000 description 14
- 244000068988 Glycine max Species 0.000 description 13
- 235000010469 Glycine max Nutrition 0.000 description 13
- 238000012360 testing method Methods 0.000 description 8
- 239000003814 drug Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 238000009333 weeding Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 230000002363 herbicidal effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 1
- 240000006995 Abutilon theophrasti Species 0.000 description 1
- 240000006740 Cichorium endivia Species 0.000 description 1
- 241000233838 Commelina Species 0.000 description 1
- 240000004230 Cyperus compressus Species 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
- 206010059866 Drug resistance Diseases 0.000 description 1
- 244000058871 Echinochloa crus-galli Species 0.000 description 1
- 244000025670 Eleusine indica Species 0.000 description 1
- 235000014716 Eleusine indica Nutrition 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 244000170916 Paeonia officinalis Species 0.000 description 1
- 235000006484 Paeonia officinalis Nutrition 0.000 description 1
- 231100000674 Phytotoxicity Toxicity 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229940064734 aminobenzoate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000003733 chicria Nutrition 0.000 description 1
- BIKACRYIQSLICJ-UHFFFAOYSA-N cloransulam-methyl Chemical group N=1N2C(OCC)=NC(F)=CC2=NC=1S(=O)(=O)NC1=C(Cl)C=CC=C1C(=O)OC BIKACRYIQSLICJ-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940095130 dimethyl capramide Drugs 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- PNJUHWYLFGZTIK-UHFFFAOYSA-N dodecyl benzenesulfonate;2-(2-hydroxyethylamino)ethanol Chemical compound OCCNCCO.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 PNJUHWYLFGZTIK-UHFFFAOYSA-N 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- OORLZFUTLGXMEF-UHFFFAOYSA-N sulfentrazone Chemical compound O=C1N(C(F)F)C(C)=NN1C1=CC(NS(C)(=O)=O)=C(Cl)C=C1Cl OORLZFUTLGXMEF-UHFFFAOYSA-N 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 238000004260 weight control Methods 0.000 description 1
- 239000008096 xylene Substances 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
-
- 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
-
- 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
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- 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)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of pesticides, in particular to emulsifiable concentrate containing refined metolachlor and sulfenamide and a preparation method thereof. The cream comprises an active ingredient, an emulsifier, a cosolvent and a solvent; the active ingredients consist of metolachlor and sulfenamide. The emulsion of the invention improves the stability of the formulation through the optimization of the auxiliary agent, meets the water quality of different areas, and has the advantages of good emulsifying dispersibility and high stability.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to emulsifiable concentrate containing refined metolachlor and sulfenamide and a preparation method thereof.
Background
Metolachlor (S-metaachlor), chemical name: 2-chloro-N- (2-ethyl-6-methylphenyl) -N- [ (1R) -2-methoxy-1-methylethyl ] acetamide belongs to amide selective pre-emergence herbicide, is suitable for post-sowing seedling or pre-transplanting soil treatment of dry land crops, and can prevent and kill annual gramineous weeds, partial dicotyledonous weeds and annual sedge weeds.
Sulfenamide (cloransulam-methyl), chemical name: methyl 3-chloro-2- (5-ethoxy-7-fluoro [1,2,4] triazol [1,5-c ] pyrimidin-2-ylsulfonyl) aminobenzoate belongs to sulfonamide herbicides and is mainly used for preventing and removing broadleaf weeds by spraying stems and leaves of soybean fields.
Herbicide varieties containing a single active ingredient often suffer from varying degrees of deficiencies in agricultural pest control, such as: the weeding spectrum is narrow, weeds are easy to generate drug resistance after continuous use, and the pollution to the environment can be aggravated after the weeding composition is used for a plurality of times. The combination of the metolachlor and the sulfenamide in the prior art CN108235985A, CN109561687A, CN107920529A, CN109566632A, CN108235985A and other patents already discloses that the synergistic effect among active components in the composition is proved, so that the weeding composition can be used for expanding the weeding composition and delaying the weed resistance.
However, the existing composition formulations of the metolachlor and the sulfenamide in the market are suspension emulsions, no emulsifiable concentrate formulation exists, the suspension emulsion has poorer quality stability compared with the emulsifiable concentrate formulation, the processing technology has higher requirements, the production cost is higher, the composition is easily influenced by environmental changes in the marine transportation process, the phenomena of caking, creaming, particle size growth, water separation and the like are easy to occur at high temperature, the crystallization risk exists at low temperature, and the drug effect is seriously influenced.
Disclosure of Invention
In view of the above, the invention provides an emulsifiable concentrate containing the fine metolachlor and the sulfenamide and a preparation method thereof. The emulsion improves the stability of the formulation through the optimization of the auxiliary agent, meets the water quality of different areas, and has the advantages of good emulsifying dispersibility and high stability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a missible oil containing metolachlor and sulfenamide, which comprises active ingredients, an emulsifying agent, a cosolvent and a solvent; the active ingredients consist of metolachlor and sulfenamide.
Preferably, the mass percentages of the components are as follows:
in the active ingredients, the mass ratio of the metolachlor to the sulfenamide is (1-8): 1.
preferably, the mass percentages of the components are as follows:
preferably, the mass percentages of the components are as follows:
preferably, the emulsifier is one or more of phenethyl phenol polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, dodecylbenzene sulfonate, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene polyoxypropylene ether.
Preferably, the emulsifier is one or more of phenethyl phenol polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, calcium dodecyl benzene sulfonate, diethanolamine dodecyl benzene sulfonate, castor oil polyoxyethylene ether or fatty alcohol polyoxyethylene ether.
More preferably, the emulsifier is a combination of three emulsifiers, and consists of a first emulsifier calcium dodecyl benzene sulfonate, a second emulsifier phenethyl phenol polyoxyethylene polyoxypropylene ether and a third emulsifier isomeric tridecyl fatty alcohol polyoxyethylene ether. The first, second and third emulsifiers are preferably used in an amount of 1 to 6:1-9:1 mass ratio, and more preferably 1 to 6:4-9:1, more preferably 1:9: 1. 6:4: 1. 4:5: 1. 3:6: 1. 2:7: 1. 5:8: 1. 6:7:1 or 5:8:0.5 mass ratio, most preferably 5:8:1 mass ratio.
According to the invention, through optimizing the auxiliary agent, the stability of the product is improved, the high-low temperature range of-10 ℃ to 54 ℃ can be tolerated, and the influence of environmental change in the transportation process is effectively solved; meanwhile, the invention can resist different water qualities such as C water, D water, 3WHO water and the like, meets the use requirements of different countries and regions, and is favorable for wide popularization and application; and the invention has excellent drug effect.
Preferably, the cosolvent is one or more of methyl oleate, biodiesel or solvent oil. Methyl oleate is preferred.
Preferably, the solvent is one or more of ethanol, acetone, N-dimethyl capramide or cyclohexanone. N, N-dimethyldecanoamide is preferred.
The invention also provides a preparation method of the emulsifiable concentrate, which comprises the following steps: uniformly mixing the solvent, the cosolvent and the active ingredients, heating and preserving heat until the raw materials are completely dissolved; finally adding the emulsifying agent and stirring uniformly.
Preferably, the temperature of the heat preservation is 45-55 ℃.
The invention has the following beneficial effects:
1) The pesticide composition provided by the invention has the advantages of simple processing technology, good product stability, convenience in use and excellent drug effect performance.
2) The invention carries out a large amount of screening work on the auxiliary agent system, finally obtains the system with the optimal matching degree among the components, improves the stability of the dosage form, meets the water quality of different areas, and has the advantages of good emulsifying dispersibility and high stability.
Detailed Description
The invention discloses an emulsifiable concentrate containing metolachlor and sulfenamide and a preparation method thereof, and a person skilled in the art can refer to the content of the emulsifiable concentrate and properly improve the technological parameters. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the methods and applications described herein, and in the practice and application of the techniques of this invention, without departing from the spirit or scope of the invention.
Metolachlor essence: the pure product is colorless liquid, and the industrial product is brown oily liquid. Melting point: -61.1 ℃, boiling point: 334 ℃, relative density (water=1): 1.117, saturated vapor pressure: 1.8mPa (25 ℃ C.). Solubility: water solubility 488mg/L (25 ℃ C.) miscible with benzene, xylene, toluene, octanol and methylene chloride, hexane, dimethylformamide, methanol, dichloroethane, insoluble in ethylene glycol, propanol and petroleum ether.
Sulfenamide: the pure product is a brown yellow solid. Melting point 121-123 deg.C, relative density 1.34 (20 deg.C) and vapor pressure 1.3X10 -4 Pa (25 ℃), dissociation constant pKa6.56. Is soluble in most polar organic solvents such as acetone, and has a solubility of 11mg/L (pH=6), 0.78 (pH=7), and 16 (pH=7.5) in water at 25deg.C. The half life in soil is 110-280 d.
Chinese and english names of active ingredients and partial adjuvants:
the following percentages are by weight unless otherwise indicated.
The raw materials or auxiliary materials used in the invention can be purchased from the market.
The invention is further illustrated by the following examples:
examples 1 to 10 and comparative example 1
The formulations of the examples and comparative examples are shown in the following table:
TABLE 1
The preparation method comprises the following steps: uniformly mixing the solvent, the cosolvent and the active ingredients, heating and preserving heat to 45-55 ℃ until the raw materials are completely dissolved; finally adding the emulsifying agent and stirring uniformly.
Test example 1 Performance test
The properties of the emulsifiable concentrates prepared in the above examples and comparative examples were examined, and the results are shown in table 2 below. Wherein, the emulsion stability is detected according to the GB/T1603-1979 determination method, and the spontaneous dispersibility in water is detected according to the GB/T32775-2016 determination method.
TABLE 2 Performance of emulsifiable concentrate products containing the combination of the active ingredients of metolachlor and sulfenamide
As is clear from Table 2, in examples 7, 8, 9 and 10, spontaneous dispersibility in water was slightly poor, and a small amount of precipitation occurred in cold storage at-10 ℃; examples 1,2, 3, 4, 5, 6 are preferred, preferably the adjuvants and co-solvents, solvents play a critical role in the quality of the product.
Example 11
The mass percentage of the emulsifier was adjusted on the basis of the formulation (group a) of example 1, which was as follows:
TABLE 3 Table 3
Test example 2 performance test the performance of the emulsifiable concentrates prepared in example 11 was tested and the results are shown in table 4 below.
Table 4 Performance of emulsifiable concentrate products containing the combination of the active ingredients of essential metolachlor and sulfenamide
Pesticide effect test of compound preparation of metolachlor and sulfenamide for controlling weeds in soybean fields in field
The test is carried out in the city of the peony river in the Heilongjiang province, the soil type is black soil, and the fertility is good. The control medicament is 960g/L of the essential metolachlor emulsifiable concentrate and 50% of the sulfenamide suspending agent. A total of 4 treatments were set up, each: treatment 1: spraying clear water and blank control; treatment 2: the refined metolachlor-sulfentrazone emulsifiable concentrates obtained in examples 1 and 7; treatment 3:960g/L of refined metolachlor emulsifiable concentrate; treatment 4:50% sulfenamide suspending agent.
Wherein, the metolachlor and sulfentrazone emulsifiable concentrates obtained in examples 1 and 7 were subjected to stem and leaf spray treatment according to the dosage of the effective component of 800 g/hectare, the stem and leaf spray treatment according to the dosage of the effective component of 1300 g/hectare was performed in treatment 3, and the stem and leaf spray treatment according to the dosage of the effective component of 540 g/hectare was performed in treatment 4.
Spraying stems and leaves of the first three leaves of the soybean, and preventing and killing weeds in soybean fields, wherein the weeds in soybean fields comprise broadleaf weeds such as dayflower, piemarker, endive and the like, and grassy weeds such as crabgrass and barnyard grass. The medicine is applied by a worker pesticide-16 knapsack manual sprayer for 1 time, 750kg of water is added according to the dosage of each hectare preparation to prepare medicine liquid, and the medicine liquid is uniformly sprayed according to the medicine liquid quantity in a converted district. With random block arrangement, 4 repetitions, cell area 50m 2 (5m×10m)。
50 days after application, the effect of each treatment on the fresh weight control effect of weeds and the effect on the safety of soybeans were investigated.
The investigation method comprises the following steps: each cell fixes 4 points, each point 0.25m 2 The fresh weight of the undelivered weeds in the area was investigated and the control effect was calculated as follows:
control effect (%) = (fresh weed weight in control zone-fresh weed weight in treated zone) ×100%/fresh weed weight in control zone
The results of controlling weeds in soybean fields are shown in Table 5 below:
table 5 results of field efficacy test of each treatment agent for controlling weeds in soybean fields
As can be seen from the test results in the table 5, after the compound formulation of the metolachlor and the sulfenamide, the compound formulation can effectively control the weeds in the soybean field for one year and multiple years, and the control effect on the weeds in the soybean field for one year and multiple years after 50 days of application is obviously better than that of 2 control medicaments, so that the synergistic effect is shown. Example 1 using the preferred adjuvant and the preferred formulation has significantly better control than example 7. According to the observation of the whole process of the field test, the soybean grows well within the test dosage range, and the phenomenon of phytotoxicity does not occur in each treatment agent, so that the soybean is safe to soybean.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. An emulsifiable concentrate containing metolachlor and sulfenamide, which is characterized by comprising the following components in percentage by mass:
55% of metolachlor, 9% of sulfenamide, 5% of calcium dodecyl benzene sulfonate, 8% of phenethyl phenol polyoxyethylene polyoxypropylene ether, 1% of isomeric tridecyl fatty alcohol polyoxyethylene ether, 8% of methyl oleate and the balance of N, N-dimethyl decyl amide.
2. A process for the preparation of an emulsifiable concentrate as claimed in claim 1, comprising: uniformly mixing N, N-dimethyl capramide, methyl oleate, metolachlor and sulfenamide, heating and preserving heat until the raw materials are completely dissolved; finally adding calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene polyoxypropylene ether, isomerism tridecyl fatty alcohol polyoxyethylene ether, and uniformly stirring.
3. The preparation method according to claim 2, wherein the temperature of the heat preservation is 45-55 ℃.
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