CN115624032A - Preparation method of prochloraz-epoxiconazole water emulsion - Google Patents
Preparation method of prochloraz-epoxiconazole water emulsion Download PDFInfo
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- CN115624032A CN115624032A CN202210817082.3A CN202210817082A CN115624032A CN 115624032 A CN115624032 A CN 115624032A CN 202210817082 A CN202210817082 A CN 202210817082A CN 115624032 A CN115624032 A CN 115624032A
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- CN
- China
- Prior art keywords
- prochloraz
- epoxiconazole
- water
- phase
- polyoxyethylene ether
- 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.)
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000005767 Epoxiconazole Substances 0.000 title claims abstract description 46
- 239000000839 emulsion Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- ZMYFCFLJBGAQRS-IRXDYDNUSA-N (2R,3S)-epoxiconazole Chemical compound C1=CC(F)=CC=C1[C@@]1(CN2N=CN=C2)[C@H](C=2C(=CC=CC=2)Cl)O1 ZMYFCFLJBGAQRS-IRXDYDNUSA-N 0.000 claims abstract description 20
- 239000005820 Prochloraz Substances 0.000 claims abstract description 20
- 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 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 11
- 238000010008 shearing Methods 0.000 claims abstract description 11
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 27
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 27
- 239000003921 oil Substances 0.000 claims description 17
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 12
- 239000003814 drug Substances 0.000 claims description 11
- 229940079593 drug Drugs 0.000 claims description 11
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 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 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- 239000004359 castor oil Substances 0.000 claims description 5
- 235000019438 castor oil Nutrition 0.000 claims description 5
- 150000002191 fatty alcohols Chemical class 0.000 claims description 5
- 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 5
- 238000003756 stirring Methods 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- 238000007710 freezing Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 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 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 2
- 229950004959 sorbitan oleate Drugs 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 239000003760 tallow Substances 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims 3
- VHGFAEBHLBZCIX-UHFFFAOYSA-N 2-dodecylbenzenesulfonate;2-hydroxyethylazanium Chemical compound NCCO.CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O VHGFAEBHLBZCIX-UHFFFAOYSA-N 0.000 claims 1
- YZYASTRURKBPPS-UHFFFAOYSA-N C(CCC(=O)OCCCCCC(C)C)(=O)OCCCCCC(C)C.[Na] Chemical compound C(CCC(=O)OCCCCCC(C)C)(=O)OCCCCCC(C)C.[Na] YZYASTRURKBPPS-UHFFFAOYSA-N 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 239000004557 technical material Substances 0.000 claims 1
- 239000007798 antifreeze agent Substances 0.000 abstract 1
- 239000000375 suspending agent Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000002994 raw material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- KLIIGADLHUOXPS-UHFFFAOYSA-N 2-(1,2,2-triphenylethenyl)phenol Chemical compound OC1=CC=CC=C1C(C=1C=CC=CC=1)=C(C=1C=CC=CC=1)C1=CC=CC=C1 KLIIGADLHUOXPS-UHFFFAOYSA-N 0.000 description 3
- 229920005682 EO-PO block copolymer Polymers 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000003899 bactericide agent Substances 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 244000052616 bacterial pathogen Species 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 229940002612 prodrug Drugs 0.000 description 2
- 239000000651 prodrug Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- BLHFWIFQKPTLCY-UHFFFAOYSA-N 2-aminoethanol dodecyl benzenesulfonate Chemical compound NCCO.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 BLHFWIFQKPTLCY-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 102000012286 Chitinases Human genes 0.000 description 1
- 108010022172 Chitinases Proteins 0.000 description 1
- BOLQUPOXTWHXIX-UHFFFAOYSA-N OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 Chemical compound OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 BOLQUPOXTWHXIX-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002528 anti-freeze Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- MQKXWEJVDDRQKK-UHFFFAOYSA-N bis(6-methylheptyl) butanedioate Chemical compound CC(C)CCCCCOC(=O)CCC(=O)OCCCCCC(C)C MQKXWEJVDDRQKK-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- -1 diphenylvinyl phenol formaldehyde Chemical compound 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008029 eradication Effects 0.000 description 1
- 230000008686 ergosterol biosynthesis Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 244000053095 fungal pathogen Species 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 230000009545 invasion Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 235000010493 xanthan gum Nutrition 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues 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
- 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
- A01N43/64—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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
-
- 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)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
Abstract
The invention discloses a preparation method of prochloraz-epoxiconazole aqueous emulsion, which comprises the following components: 5-25wt% of prochloraz technical, 5-25wt% of epoxiconazole technical, 2-10wt% of emulsifier, 5-20 wt% of anti-precipitation agent, 0.5-10wt% of antifreeze agent and the balance of water. The epoxiconazole is dissolved in the heated prochloraz by a hot melting method, then the emulsifier and the anti-precipitation agent are added to prepare an oil phase, and the antifreezing agent and water are weighed to prepare a water phase. And then adding the water phase into the oil phase for reverse-phase high-speed shearing to obtain the prochloraz-epoxiconazole water emulsion.
Description
Technical Field
The invention belongs to the technical field of pesticide chemical preparations, and particularly relates to a preparation method of prochloraz-epoxiconazole aqueous emulsion.
Background
Prochloraz is an imidazole broad-spectrum pesticide bactericide, has the functions of treatment and eradication, and has the conductivity and no systemic action. Epoxiconazole is a triazole fungicide with broad spectrum, high efficiency, low toxicity and systemic property. Can inhibit the synthesis of ergosterol of pathogenic bacteria, and compared with the existing bactericide, the bactericide can more effectively inhibit pathogenic fungi. Epoxiconazole can improve the chitinase activity of crops, cause the contraction of fungal haustorium and inhibit the invasion of pathogenic bacteria. The epoxiconazole and the prochloraz are compounded, so that at present, suspending agents and microemulsions are mainly used in the market, the efficacy of the suspending agents is poorer than that of the suspending agents, the microemulsions use more organic solvents, the cost is high, and the environment is easily polluted.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of prochloraz-epoxiconazole aqueous emulsion aiming at the defects of the prior art.
The technical scheme is as follows: the preparation method of the prochloraz-epoxiconazole water emulsion comprises 5-25wt% of prochloraz raw drug, 5-25wt% of epoxiconazole raw drug, 2-10wt% of emulsifier, 5-20 wt% of anti-precipitation agent, 0.5-10wt% of antifreezing agent and the balance of water; dissolving epoxiconazole raw drug in heated prochloraz raw drug by a hot melting method, adding an emulsifier and an anti-precipitation agent to prepare an oil phase, and weighing an antifreezing agent and water to prepare a water phase; and then adding the water phase into the oil phase for reverse-phase high-speed shearing to obtain the prochloraz-epoxiconazole water emulsion.
Further, as a preferred embodiment, the emulsifier is one or more of triphenylvinyl phenol polyoxyethylene ether, triphenylvinyl phenol polyoxyethylene polyoxypropylene ether, diphenylvinyl phenol formaldehyde resin polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic acid ether polyoxyethylene ether, tallow amine polyoxyethylene ether, alkyl polyglycoside, sorbitan oleate, calcium dodecylbenzene sulfonate, dodecylbenzene sulfonate ethanolamine salt, diisooctyl succinate sodium sulfonate, and triphenylvinyl phenol polyoxyethylene ether phosphate triethanolamine salt.
Further, as a preferred embodiment, the anti-precipitation agent is one or more of solvent naphtha S-150#, methyl pyrrolidone, dimethyl sulfoxide, cyclohexanone or n-octanol.
Further, as a preferred embodiment, the antifreeze is selected from one or more of ethylene glycol, glycerol, propylene glycol and urea.
Further, as a preferred embodiment, the method specifically comprises the following steps:
1) Weighing prochloraz raw drug according to a specified ratio, heating to 50-65 ℃, adding epoxiconazole, stirring for dissolving, and then adding an emulsifier and an anti-precipitation agent to prepare an oil phase;
2) Weighing the anti-freezing agent and the water according to a specified ratio, and uniformly stirring to obtain a water phase;
3) And transferring the weighed water phase into the oil phase for one time, and performing reverse phase shearing and high-speed shearing to obtain the prochloraz-epoxiconazole water emulsion.
Further, as a preferred embodiment, the heating temperature in the step 1) is 50 to 65 ℃.
Further, as a preferred embodiment, the shearing mode is a reverse phase emulsification method, and the water phase is transferred into the oil phase at one time.
Has the advantages that: the invention has the advantages of less auxiliary agent, no or little solvent used for dissolving the epoxiconazole technical product by a hot melting method, safety, environmental protection and low cost, and increases the low temperature and the normal storage stability of the product.
Detailed Description
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to the examples.
Example 1: a preparation method of prochloraz-epoxiconazole water emulsion.
10% prochloraz-5% epoxiconazole water emulsion: weighing 10g of prochloraz raw material, heating to 50 ℃, adding 5g of epoxiconazole raw material after the prochloraz is melted, carrying out hot melting, then adding 3g of castor oil polyoxyethylene ether, 2g of fatty alcohol polyoxyethylene ether, 1g of tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt and 5g of cyclohexanone, and uniformly stirring to prepare an oil phase; weighing 5g of propylene glycol and 100 g of water as a complementary system to prepare a water phase, and transferring the water phase into an oil phase at one time to be sheared at a high speed to form stable aqueous emulsion.
Example 2: a preparation method of prochloraz-epoxiconazole water emulsion.
15% of prochloraz and 10% of epoxiconazole emulsion in water: weighing 15g of prochloraz original drug, heating to 50 ℃, adding 10g of epoxiconazole original drug after the prochloraz is melted, carrying out hot melting, adding 3g of castor oil polyoxyethylene ether, 2g of fatty alcohol polyoxyethylene ether, 1g of tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, 1g of ethylene oxide-propylene oxide block copolymer and 5g of cyclohexanone, and preparing into an oil phase; weighing 5g of propylene glycol and 100 g of water complementing system to prepare a water phase, and transferring the water phase into an oil phase at one time for high-speed shearing to form stable aqueous emulsion.
Example 3: a preparation method of prochloraz-epoxiconazole aqueous emulsion.
25% of prochloraz and 15% of epoxiconazole emulsion in water: weighing 25g of prochloraz raw material, heating to 50 ℃, adding 15g of epoxiconazole raw material after the prochloraz is melted, carrying out hot melting, adding 4g of tristyrylphenol polyoxyethylene ether, 3g of castor oil polyoxyethylene ether, 2g of tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, 1g of ethylene oxide-propylene oxide block copolymer emulsifier and 10g of cyclohexanone, and preparing into an oil phase; 5g of propylene glycol is weighed, 100 g of water foot-tonifying system is prepared into a water phase, and the water phase is transferred into an oil phase at one time and cut at high speed to form stable aqueous emulsion.
Prochloraz prodrugs described in examples 1-3 were purchased from: less chemical Co., ltd.
The epoxiconazole prodrugs described in examples 1 to 3 were purchased from: andao Maihufeng (Jiangsu) Ltd.
And (3) detecting the low-temperature stability, namely testing the low-temperature stability of the samples of the examples 1-3 and the existing suspending agent products at 0 ℃, 5 ℃ and 10 ℃ respectively. The lower the temperature, the unfrozen product, indicating that the product has good freezing resistance. The product is stored in an oven at 54 ℃ for 2 weeks, and the thermal storage stability is tested, and no water and oil are separated out, so that the product quality is stable, and the results are shown in table 1. The results in table 1 show that the sample of the prochloraz-epoxiconazole aqueous emulsion of the invention in the scheme 1-3 has better low-temperature and thermal storage stability than the control sample of prochloraz-epoxiconazole suspending agent.
TABLE 1 comparison of the low-temperature and thermal storage stability results of the samples of examples 1-3 with those of the same suspending agent type
The control effect test shows that the control effect is investigated on 7 days and 14 days after the application of the pesticide by diluting the schemes 1 to 3 with water by 1500 times and spraying the diluted solutions to the rice sheath blight diseases, and the control effect is shown in table 2.
Test results show that the prochloraz-epoxiconazole water emulsion has obvious effect of preventing and treating rice sheath blight, and is obviously higher than a control sample prochloraz-epoxiconazole suspending agent.
TABLE 2 comparison of control effect test results of samples in examples 1 to 3 with similar suspending agent products
Wherein the suspending agent-like control samples in this example were derived from: jiangsu Jian Nonghua GmbH; the preparation method specifically comprises the following steps: weighing the following components in percentage by weight: 10% of prochloraz original drug, 5% of epoxiconazole original drug, 2% of dispersing agent EO-PO block copolymer, 3% of dispersing agent triphenylethylene phenol polyoxyethylene ether phosphate triethanolamine, 2% of wetting agent fatty alcohol polyoxyethylene ether, 1% of wetting agent lauryl sodium sulfate, 0.15% of thickening agent xanthan gum, 5% of white carbon black, 0.2% of preservative isothiazolinone, 5% of antifreezing agent glycerol and the balance of water; shearing at low temperature (5-20 deg.C), and sanding to obtain 15% prochloraz-epoxiconazole suspension.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited to the invention itself. Various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A preparation method of prochloraz-epoxiconazole aqueous emulsion is characterized by comprising the following steps: 5-25wt% of prochloraz technical, 5-25wt% of epoxiconazole technical, 2-10wt% of emulsifier, 5-20 wt% of anti-precipitation agent, 0.5-10wt% of antifreezing agent and the balance of water; dissolving epoxiconazole raw drug in heated prochloraz raw drug by a hot melting method, adding an emulsifier and an anti-precipitation agent to prepare an oil phase, and weighing an antifreezing agent and water to prepare a water phase; and then adding the water phase into the oil phase for reverse-phase high-speed shearing to obtain the prochloraz-epoxiconazole water emulsion.
2. The preparation method of prochloraz-epoxiconazole water emulsion according to claim 1, which is characterized in that: the emulsifier is one or more of tristyrylphenol polyoxyethylene ether, tristyrylphenol polyoxyethylene polyoxypropylene ether, distyrylphenol formaldehyde resin polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, oleic ether polyoxyethylene ether, tallow amine polyoxyethylene ether, alkyl polyglycoside, sorbitan oleate, calcium dodecyl benzene sulfonate, dodecyl benzene sulfonic acid ethanolamine salt, sodium diisooctyl succinate sulfonate and tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt.
3. The preparation method of prochloraz-epoxiconazole water emulsion according to claim 1 or 2, which is characterized in that: the anti-precipitation agent is one or more of solvent naphtha S-150#, methyl pyrrolidone, dimethyl sulfoxide, cyclohexanone or n-octanol.
4. The preparation method of prochloraz-epoxiconazole water emulsion according to claim 1 or 2, which is characterized in that: the antifreezing agent is one or more selected from ethylene glycol, glycerol, propylene glycol and urea.
5. The preparation method of prochloraz-epoxiconazole water emulsion according to claim 1, which is characterized in that: the method specifically comprises the following steps:
1) Weighing prochloraz technical material according to a specified ratio, heating to 50-65 ℃, adding epoxiconazole, stirring for dissolving, and then adding an emulsifier and an anti-precipitation agent to prepare an oil phase;
2) Weighing the anti-freezing agent and the water according to a specified ratio, and uniformly stirring to obtain a water phase;
3) And transferring the weighed water phase into the oil phase for one time, and performing reverse phase shearing and high-speed shearing to obtain the prochloraz-epoxiconazole water emulsion.
6. The method for preparing prochloraz-epoxiconazole aqueous emulsion according to claim 5, wherein: the heating temperature of the step 1) is 50-65 ℃.
7. The preparation method of prochloraz-epoxiconazole water emulsion according to claim 5, which is characterized in that: the shearing mode is a reverse phase emulsification method, and the water phase is transferred into the oil phase at one time.
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