CN103997889B - Water-based suspension emulsion - Google Patents
Water-based suspension emulsion Download PDFInfo
- Publication number
- CN103997889B CN103997889B CN201180075604.7A CN201180075604A CN103997889B CN 103997889 B CN103997889 B CN 103997889B CN 201180075604 A CN201180075604 A CN 201180075604A CN 103997889 B CN103997889 B CN 103997889B
- Authority
- CN
- China
- Prior art keywords
- water
- suspension emulsion
- lufenuron
- cyhalothrin
- active component
- 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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- 239000000725 suspension Substances 0.000 title claims abstract description 96
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000000839 emulsion Substances 0.000 title claims abstract description 78
- 239000005912 Lufenuron Substances 0.000 claims abstract description 62
- 229960000521 lufenuron Drugs 0.000 claims abstract description 62
- PWPJGUXAGUPAHP-UHFFFAOYSA-N lufenuron Chemical compound C1=C(Cl)C(OC(F)(F)C(C(F)(F)F)F)=CC(Cl)=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F PWPJGUXAGUPAHP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000005903 Gamma-cyhalothrin Substances 0.000 claims abstract description 49
- ZXQYGBMAQZUVMI-GCMPRSNUSA-N gamma-cyhalothrin Chemical compound CC1(C)[C@@H](\C=C(/Cl)C(F)(F)F)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-GCMPRSNUSA-N 0.000 claims abstract description 49
- 238000002360 preparation method Methods 0.000 claims description 57
- 239000000203 mixture Substances 0.000 claims description 45
- 239000003921 oil Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 24
- 239000002270 dispersing agent Substances 0.000 claims description 23
- ZXQYGBMAQZUVMI-RDDWSQKMSA-N (1S)-cis-(alphaR)-cyhalothrin Chemical compound CC1(C)[C@H](\C=C(/Cl)C(F)(F)F)[C@@H]1C(=O)O[C@@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-RDDWSQKMSA-N 0.000 claims description 20
- 239000005910 lambda-Cyhalothrin Substances 0.000 claims description 20
- 239000003995 emulsifying agent Substances 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000002562 thickening agent Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 239000011324 bead Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 150000004676 glycans Chemical class 0.000 claims description 4
- 229920001282 polysaccharide Polymers 0.000 claims description 4
- 239000005017 polysaccharide Substances 0.000 claims description 4
- 239000001294 propane Substances 0.000 claims description 4
- 239000000230 xanthan gum Substances 0.000 claims description 4
- 229920001285 xanthan gum Polymers 0.000 claims description 4
- 229940082509 xanthan gum Drugs 0.000 claims description 4
- 235000010493 xanthan gum Nutrition 0.000 claims description 4
- 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 3
- 229920000578 graft copolymer Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 5
- 239000004615 ingredient Substances 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 30
- 238000003860 storage Methods 0.000 description 25
- 238000012360 testing method Methods 0.000 description 15
- 239000000047 product Substances 0.000 description 11
- 238000007796 conventional method Methods 0.000 description 10
- 238000007865 diluting Methods 0.000 description 10
- 239000003814 drug Substances 0.000 description 10
- 239000004562 water dispersible granule Substances 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 239000000375 suspending agent Substances 0.000 description 9
- 239000007764 o/w emulsion Substances 0.000 description 8
- 239000004563 wettable powder Substances 0.000 description 8
- -1 micro emulsionAgent Substances 0.000 description 7
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 6
- 231100000674 Phytotoxicity Toxicity 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 239000013530 defoamer Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 5
- 239000012872 agrochemical composition Substances 0.000 description 5
- 230000002528 anti-freeze Effects 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 231100000419 toxicity Toxicity 0.000 description 5
- 230000001988 toxicity Effects 0.000 description 5
- 210000000481 breast Anatomy 0.000 description 4
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002728 pyrethroid Substances 0.000 description 4
- 241000238631 Hexapoda Species 0.000 description 3
- HRYILSDLIGTCOP-UHFFFAOYSA-N N-benzoylurea Chemical compound NC(=O)NC(=O)C1=CC=CC=C1 HRYILSDLIGTCOP-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000013065 commercial product Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000005338 heat storage Methods 0.000 description 3
- 239000003094 microcapsule Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 244000257790 Brassica carinata Species 0.000 description 2
- 235000005156 Brassica carinata Nutrition 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000005906 Imidacloprid Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 241000607479 Yersinia pestis Species 0.000 description 2
- BQODPTQLXVVEJG-UHFFFAOYSA-N [O].C=C Chemical group [O].C=C BQODPTQLXVVEJG-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229940056881 imidacloprid Drugs 0.000 description 2
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 2
- 230000000749 insecticidal effect Effects 0.000 description 2
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 description 2
- 229940073769 methyl oleate Drugs 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 231100000208 phytotoxic Toxicity 0.000 description 2
- 230000000885 phytotoxic effect Effects 0.000 description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 2
- 229920000053 polysorbate 80 Polymers 0.000 description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 2
- 239000010458 rotten stone Substances 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- ZOCSXAVNDGMNBV-UHFFFAOYSA-N 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-[(trifluoromethyl)sulfinyl]-1H-pyrazole-3-carbonitrile Chemical compound NC1=C(S(=O)C(F)(F)F)C(C#N)=NN1C1=C(Cl)C=C(C(F)(F)F)C=C1Cl ZOCSXAVNDGMNBV-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 102100035683 Axin-2 Human genes 0.000 description 1
- 101700047552 Axin-2 Proteins 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005944 Chlorpyrifos Substances 0.000 description 1
- 101100379079 Emericella variicolor andA gene Proteins 0.000 description 1
- 239000005899 Fipronil Substances 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- BJVCAPVVVPZVHB-UHFFFAOYSA-N O=C1NC=CC1C1CCCCC1 Chemical class O=C1NC=CC1C1CCCCC1 BJVCAPVVVPZVHB-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000008052 alkyl sulfonates Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- WMGSQTMJHBYJMQ-UHFFFAOYSA-N aluminum;magnesium;silicate Chemical compound [Mg+2].[Al+3].[O-][Si]([O-])([O-])[O-] WMGSQTMJHBYJMQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical compound CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- ZXQYGBMAQZUVMI-UNOMPAQXSA-N cyhalothrin Chemical compound CC1(C)C(\C=C(/Cl)C(F)(F)F)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-UNOMPAQXSA-N 0.000 description 1
- 230000007682 dermal toxicity Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000004495 emulsifiable concentrate Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 229940013764 fipronil Drugs 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000010413 gardening Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000026731 phosphorylation Effects 0.000 description 1
- 238000006366 phosphorylation reaction Methods 0.000 description 1
- 239000003123 plant toxin Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 231100000438 skin toxicity Toxicity 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000004546 suspension concentrate Substances 0.000 description 1
- 239000004548 suspo-emulsion Substances 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 230000009466 transformation Effects 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<
- A01N47/34—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
Abstract
The present invention provides water-based suspension emulsion (SE) product now, and it comprises suspended solid component lufenuron and the gamma cyhalothrin as emulgate ingredient.
Description
Technical field
The present invention now provides a kind of water-based suspension emulsion (suspoemulsion, SE) product of novelty, and it comprises as outstandingFloat the lufenuron (Lufenuron) of solid constituent and the gamma cyhalothrin (Lambda-as emulgate ingredientcyhalothrin)。
Background technology
Gamma cyhalothrin is the isomers S-alpha-cyano-3-phenoxy benzyl 1R by racemic ratio, cis-3-(Z-2-is chloro-3,3,3-trifluoropropyl-1-alkene-1-yl)-2,2-dimethyl cyclopropane carboxylic acid ester and R-alpha-cyano-3-phenoxy benzyl 1S,Cis-3-(Z-2-chloro-3,3,3-trifluoropropyl-1-alkene-1-yl)-2, the enantiomer of 2-dimethyl cyclopropane carboxylic acid ester kills compositionThe adopted name of the ISO approval of worm active component. Before desinsection product gamma cyhalothrin, be mixed with missible oil(emusifiableconcentrate). The product that contains gamma cyhalothrin of intending being used for agricultural or gardening is conventionally with noteVolume trade mark KARATE sells.
Lufenuron is that chemical name is N-[[[2, the chloro-4-of 5-bis-(1,1,2,3,3,3-hexafluoro propoxyl group) phenyl] amino]Carbonyl]-2, the adopted name of the ISO approval of the active insecticidal components of 6-difluorobenzamide. Lufenuron is generally with missible oil(emulsificableconcentrate, EC) dosage form is sold. Due to the characteristic of lufenuron, contain and exceed 5% lufenuronMissible oil dilute with water after easily crystallization.
In recent years, expect improve usefulness, widen insecticidal spectrum by two or more products of combined administration, and postpone rightThe resistance of pesticide. CN1176589 has described the pre-mixing agent of benzoyl urea agricultural chemicals and pyrethroid (pyrethroid)(premix). This combination is maintained the efficient and hypotoxicity of benzoyl urea agricultural chemicals, and unlike pyrethroid toolThere is the resistance to the action of a drug. The combination of benzoyl urea and pyrethroid has high application effect, extensively uses scope and grow duration, spyBe not applicable to prevention and kill the insect that the resistance to the action of a drug is strong. The pre-mixing agent that this patent is mentioned can be mixed with missible oil, oil-suspending agent, micro emulsionAgent, water-dispersible granule and microcapsules. But these patents do not provide or instruct the side of these preparations of preparing this pre-mixing agentMethod. And this patent does not provide environment storage stability data yet. With the base that is combined as of lufenuron and gamma cyhalothrinThe commercial product of plinth is not easy to obtain with missible oil, oil-suspending agent, microemulsion, water-dispersible granule and microcapsules.
Generally speaking, the formulated in combination of lufenuron or gamma cyhalothrin can be become to missible oil. But, according to inventor'sExperience, in said composition, the content of lufenuron should be less than 5%, to avoid the crystallization of lufenuron in the time diluting. Therefore, in compositionThe pre-mixing agent with high-load (exceeding 5%) lufenuron is not suitable for being mixed with missible oil. On the other hand, missible oil needs a large amount of organic moltenAgent (as aromatic hydrocarbon, chlorinated hydrocabon etc.), effectively to prepare active component. But known such organic solvent has toxicity and lifeState toxicology property, produces toxicity and ecological toxicity problem. For this conventional formulation, ICAMA (the Ministry of Agriculture) cancelsThe registration of missible oil. Other country (as Europe and Brazil) has improved the registered standard of missible oil.
According to inventor's experience, lufenuron is unstable in emulsion. The emulsion system of lufenuron and gamma cyhalothrinAgent is easily crystallization under environment storage requirement.
With regard to single gamma cyhalothrin preparation, some eco-friendly preparations are just under development. CN101828571Gamma cyhalothrin concentrated suspension (suspensionconcentrate) has been described. CN101167471 has described efficientlyLambda-cyhalothrin water-dispersible granules. CN1600099 has described gamma cyhalothrin wettable powder. At these preparationsIn, gamma cyhalothrin is easily separated out due to the low melting point of this active component in fine gtinding and crushing process; Institute obtainsThese compositions that obtain generally cannot be shown good dispersiveness and pot-life, particularly because the active component of low melting point existsIn environment storage temperature (5 DEG C to 50 DEG C), experience phase transformation causes caking and crystal growth.
CN1836513, WO2005096820, WO2002028186, CN1274530 and WO9522902 disclose and have contained admittedlyBody active component (as Frontline (fipronil) or Imidacloprid (imidacloprid)) and liquid actives are (as efficient chlorine fluorineCyano chrysanthemate or chlopyrifos (chlorpyrifos)) composition, wherein said composition is mixed with the spraying of oil emu, super low loadingAgent, oil in water emulsion, microemulsion, wettable powder, water-dispersible granules, dry suspending agent (drysuspensition),Granule, aqueous pharmaceutical, wettable powder, aerosol, concentrated suspension and missible oil. Although these patents usually disclose agricultureThe various preparations of the combination of medicine active component, comprise water-dispersible granules, concentrated suspension and wettable powder. These patentsDo not provide or instruct preparation this water-dispersible granules composition, concentrated suspension composition and wettable powder compositionMethod. Commercial product based on combinations thereof is not easy with water-dispersible granules composition, concentrated suspension composition and canWP composition obtains. As noted above, for the combination of above pesticide activity component, prepare water-dispersible granules,The standard method of concentrated suspension and wettable powder may not be feasible, and can not provide desirable composition, because such groupCompound does not have the due good dispersion of water-dispersible granules, concentrated suspension and wettable powder, stability, storage lifeLimit and other characteristic. So wettable powder, concentrated suspension and water-dispersible granules are not suitable for lufenuron and efficientThe pre-mixing agent of lambda-cyhalothrin because gamma cyhalothrin due to the low melting point of this active component easily at fine gtinding andIn crushing process, separate out.
Microcapsule formulation can solve the low melting point problem of gamma cyhalothrin, and lufenuron and gamma cyhalothrinPre-mixing agent can be mixed with ZC, it is the mix preparation of gamma cyhalothrin CS and lufenuron SC. But, the cost of said preparationToo high and its production process complexity. This commercial product is not easy to obtain.
Very expect to provide the composition of eco-friendly lufenuron and gamma cyhalothrin; Providing can be in compositionComprising 5% above lufenuron is also useful so that the more composition of efficient to be provided. In addition provide in environment storage requirement (5,DEG C to 50 DEG C) lower stable and in the time of dilution also stable composition be also very important.
Summary of the invention
The present invention now provides novel water-based suspension emulsion (SE) product, its comprise as the lufenuron of suspended solid component andAs the gamma cyhalothrin of emulgate ingredient.
The present invention also provides eco-friendly suspension emulsion composition.
The present invention also provides novel water-based suspension emulsion, and it can comprise suspension emulsion composition, described suspension emulsion compositionCan in said composition, contain more than 5% lufenuron so that more effective to be provided.
The present invention also provides novel water-based suspension emulsion, its show simultaneously height physics and chemistry stability andMobility especially, in the temperature range of-5 DEG C to 54 DEG C, is not wherein observed crystalline polamer and caking after storage.
The present invention also provides novel water-based suspension emulsion, its all performance before and after the temperature range storage of-5 DEG C to 54 DEG CGo out dispersiveness and suspension, wherein after storage, do not observe crystalline polamer.
Therefore, first aspect, the invention provides water-based suspension emulsion, it is characterized in that comprising following component:
(a) disperse oil phase, it comprises:
(i) as the gamma cyhalothrin of the first active component,
(ii) at least one solvent, is wherein dissolved with gamma cyhalothrin;
(b) continuous water, it comprises:
(i) as the lufenuron of the second active component,
(ii) water, is wherein suspended with lufenuron.
Oil phase (component (a)) can comprise one or more of solvents and other additive.
Water (component (b)) also can comprise (iii) one or more of dispersants and other additive continuously.
On the other hand, the invention provides the method for the preparation of aforementioned water-based suspension emulsion, it is characterized in that comprising followingStep:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: by the water of active component, dispersant and aequum being mixed to prepare the particle of lufenuron active componentDispersion in continuous water; And
Step 3: the water producing in the oil phase producing in step 1 and step 2 is merged.
Or it comprises the following steps:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: the Lambda-Cyhalothrin in step 1 is added in water with high shear, obtains efficient cyhalothrinEster EW phase;
Step 3: by the water of active component, dispersant and aequum is mixed to prepare described lufenuron active component itThe dispersion of particle in continuous water; And
Step 4: the water producing in the oil in water emulsion phase producing in step 2 and step 3 is merged.
The present invention also provides the purposes of above-mentioned suspension emulsion and the method for on the scene processed insect, and it comprises uses this outstanding breastAgent.
Detailed Description Of The Invention
Suspension emulsion (SE) is the combination of a kind of missible oil (EC) of component and the concentrated suspension (SC) of another kind of component. EC phaseIt is the phase that the first active component dissolves in oil. SC is the suspending agent of another active component in water. In the time that the two mixes, willWater is as the continuous phase in emulsion (carrying the oil droplet as the decentralized photo that contains a kind of active component), with another active componentSuspended particulate mixes. Generally speaking, SC and the SE therefore producing comprise other component (for example dispersant) in addition, to help suspensionThe stability of agent and therefore whole system.
First aspect, the invention provides water-based suspension emulsion, it is characterized in that comprising following component:
(a) disperse oil phase, it comprises:
(i) as the gamma cyhalothrin of the first active component,
(ii) at least one solvent, is wherein dissolved with gamma cyhalothrin;
(b) continuous water, it comprises:
(i) as the lufenuron of the second active component,
(ii) water, is wherein suspended with lufenuron.
On the other hand, the invention provides the method for the preparation of aforementioned water-based suspension emulsion, it is characterized in that comprising followingStep:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: by the water of active component, dispersant and aequum being mixed to prepare the particle of lufenuron active componentDispersion in continuous water; And
Step 3: the water producing in the oil phase producing in step 1 and step 2 is merged.
Or it comprises the following steps:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: the Lambda-Cyhalothrin in step 1 is added in water with high shear, makes efficient cyhalothrinEster EW phase;
Step 3: by the water of active component, dispersant and aequum is mixed to prepare described lufenuron active component itThe dispersion of particle in continuous water; And
Step 4: the water producing in the oil phase producing in step 2 and step 3 is merged.
Suspension emulsion of the present invention can use technology well known by persons skilled in the art to produce in known manner.
Suspension emulsion of the present invention can comprise one or more of solvents in component (a). Applicable solvent has aromatic hydrocarbon, oleic acidMethyl esters, 1-METHYLPYRROLIDONE, propene carbonate, NOP, cyclohexyl-1-pyrrolidones, alkane, different alkaneThe mixture of hydrocarbon and cycloalkane. Applicable solvent can business obtain.
Suspension emulsion of the present invention can comprise one or more of emulsifying agents in component (a). Be included in the present compositionIn applicable emulsifying agent be also known in the art and can business obtain. Applicable emulsifying agent comprises ion and nonionic breastAgent the two, for example fatty acid ester, aliphatic alcohol ester, ether, alkylsulfonate/ester and arylsulphonate/ester. The surface that other is applicableActive emulsifier can be also known to those skilled in the art.
Suspension emulsion of the present invention can comprise one or more of suitable dispersants in component (b). According to of the present inventionSuspension emulsion preferably comprises the mixture of two kinds of different dispersants. Preferred dispersant is following substances:
Methacrylic acid-methyl methacrylate-polyethyleneglycol-graft copolymer, for example, with title4913Those that (from Uniqema) and Tersperse2500 (HuntsmanSurfactant) are commercially available;
Tristyrylphenol ethoxylates (Tristyrylphenolethoxylate), on average has 16 to 60 (preferably16 to 50) individual oxygen ethylene unit; In addition, the tristyrylphenol ethoxylates of sulphation or phosphorylation (on average has 6 to 20(preferably 7 to 16) individual oxygen ethylene unit), and the salt of these materials; Wherein can specifically mention known to title SoprophorFLK (from Rhodia), Soprophor3D33 (from Rhodia) and SoprophorS/40-P (from Rhodia) are commercially availableProduct; And
Expoxy propane/epoxyethane block copolymer (has the polyoxyethylene unit of at least 40 % by mole, center polyoxy thirdAlkene part preferably has 1500 to 2000 molecular weight). For example, can mention with title PluronicPE10100 (fromBASF), PluronicPE10500 (from BASF) and the commercially available product of Pluronic6800 (from BASF). Think above-mentionedSurfactant is that system is brought stability.
Except said components, composition can comprise one or more of other additives as required. Be included in preparationIn additive be known in the art and be commonly used. Can be included in suitable the adding in the suspension emulsion according to the present inventionAdd agent and be all the usual preparation adjuvant using, as defoamer, emulsifying agent, antifreeze, anticorrisive agent, antioxidant, colouring agent,Thickener and inert filler.
Applicable defoamer is included in all substances that conventionally can be used for this object in agrochemical composition. Particularly preferablyDefoamer be the mixture of dimethyl silicone polymer and perfluoroalkyl phosphonic acids, the silicone that for example can obtain from GE or ComptonDefoamer.
Applicable anticorrisive agent is included in all substances that conventionally can be used for this object in this type of agrochemical composition. CanThe suitable example of mentioning comprises(from BayerAG) and(from BayerAG).
Applicable antioxidant is all substances that conventionally can be used for this object in agrochemical composition. Be preferably fourthHydroxy toluene.
Applicable inert filler be included in agrochemical composition, conventionally can be used for this object and do not serve as thickeningThe all substances of agent. Be preferably inorganic particle (for example carbonate, silicates and oxides) and organic substance (for example urea/firstAldehyde condensate). For example, can mention kaolin, rutile, tripoli, tripoli fine powder, silica gel, natural and synthetic silicate andTalcum.
Applicable thickener is included in all substances that conventionally can be used for this object in agrochemical composition. For example xanthanAcid glue, PVOH, cellulose, clay hydration silicate, aluminium-magnesium silicate or its mixture. Moreover such thickener is this areaKnown and can business obtain.
In addition, also comprise according to suspension emulsion of the present invention the water being present in aqueous components (b).
Can in relatively wide scope, change according to the content of each component in suspension emulsion of the present invention. Therefore, can depositThe concentration of component conventionally as follows:
Be generally by weight 1% to 40% from the reactive compound of the group (i) of (a), be preferably by weight 5% to20％；
Be generally by weight 1% to 40% from the reactive compound of the group (i) of (b), be preferably by weight 5% to20％；
Be generally by weight 1% to 30% from the solvent of the group (ii) of (a), be preferably by weight 5% to 20%;
From the group (ii) of (b) according to the present invention in suspension emulsion water content can on a large scale, change.
Determine according to other component, water content is generally by weight 25% to 80%;
Be generally by weight 1% to 10% from the dispersant of the group (iii) of (b), be preferably by weight 1% to5％；
Can use any applicable method preparation according to suspension emulsion of the present invention. Preferred preparation preferably passes through with dirtyJourney preparation:
Step 1: by active component is mixed to prepare Lambda-Cyhalothrin with solvent together with suitable emulsifying agentPhase;
Step 2: by the water of active component, dispersant and aequum being mixed to prepare the particle of lufenuron active componentDispersion in continuous water;
By active component lufenuron for example, together with applicable dispersant and other additive (antifreeze and defoamer) andThe water of aequum tentatively mixes, and usage level agitation beads grinding machine fine gtinding is to maintain technological parameter, for example, remain flatAll particle diameter d50 is no more than 3 microns and nearly all particle d90 and is no more than 6 microns.
Step 3: the water producing in the EC producing in step 1 being added to step 2 under the stirring that continues Best Times amountXiang Zhong.
Step 4: previously prepared good thickener (as polysaccharide or xanthan gum), makes its aquation and be ready for as stepIn rapid 5 subsequent steps of mentioning, add.
Step 5: appropriate thickener (as the glue in step 4 (gum)) is added in the mixture in step 3 and continues to stirMix, until mixture becomes uniform suspending agent.
Preferred preparation is also preferably prepared by following flow process:
Step 1: by active component is mixed to prepare Lambda-Cyhalothrin with solvent together with suitable emulsifying agentPhase;
Step 2: the Lambda-Cyhalothrin in step 1 is added in water with high shear, obtains efficient cyhalothrinEster EW phase;
Step 3: by the water of active component, dispersant and aequum being mixed to prepare the particle of lufenuron active componentDispersion in continuous water;
By active component lufenuron for example, together with suitable dispersant and other additive (antifreeze and defoamer) andThe water of aequum tentatively mixes, and usage level agitation beads grinding machine fine gtinding is to maintain technological parameter, for example, remain flatAll particle diameter d50 is no more than 3 microns and nearly all particle d90 and is no more than 6 microns.
Step 4: produce in the oil in water emulsion producing in step 2 being added to step 3 under the stirring that continues Best Times amountIn raw water.
Step 5: previously prepared good thickener (as polysaccharide or xanthan gum), makes its aquation and be ready in conductIn the subsequent step that step 6 is mentioned, add.
The 6th step: appropriate thickener (as the glue in step 5) is added in the mixture in step 4 and continued and stir, untilMixture becomes uniform suspending agent.
The low tempertaure storage stability of 7 days is placed in test suspension agent at-5 DEG C, places the high temperature storage of 14 days at 54 DEG CStability, and at 30 DEG C, dilute the stability of latter 24 hours.
Suspension emulsion according to the present invention is such preparation, even if it still keeps stable after high temperature or freezing lower storage,Do not observe crystalline growth. After dilute with water, they are convertible into even spraying liquid, and do not find because the activity of spray liquid becomesPoint crystallization and the nozzle blockage that causes. These spray liquids are applicable to using by conventional method (as sprayed or pouring into).
The rate of application excursion of the suspension emulsion according to the present invention is wider, and concentration depends on the amount of active component in compositionWith draft purposes, it can be determined by those of skill in the art.
On the other hand, the invention provides the method for Control pests in place (particularly insect), the method comprise toThe above-mentioned preparation of effective dose is used in this place.
In addition, the present invention also provides the purposes of above-mentioned concentrate formulation Control pests in place.
These suspension emulsions of the present invention have all represented the physical and chemical stability of improvement in most cases, especiallyIn-5 ° to 54 DEG C temperature ranges, lay up period is not observed crystalline polamer. Said preparation or eco-friendly.
The advantage of preparation of the present invention is, can use the stability of pesticide formulation of viable commercial concentration, and without any aobviousOutstanding or harmful crystallization forms.
Compared with commercially available E.C., preparation of the present invention demonstrates low phytotoxicity.
Suspension emulsion preparation of the present invention is nonflammable, dermal toxicity is low and skin irritation is low advantage in addition.
Finally, suspension emulsion preparation of the present invention can be considered to be on ecological toxicity safety, because they are by safety and basicThe composition preparation of inertia. Result is not only useful preparation, and preparation also meets the tight of U.S. EPA (State Bueau of Environmental Protection)Lattice require and the European standard of controlling VOC.
Although will describe the present invention in conjunction with some preferred embodiment in following examples, should be appreciated that it alsoBe not intended to limit the invention to these specific embodiments. On the contrary, it be intended to contain can be included in by appended right wantAsk all replacement schemes, amendment and equivalent in the present invention's the scope that book limits. Therefore, (it comprises excellent following examplesThe embodiment of choosing) will be used for illustrating enforcement of the present invention, details shown in being to be understood that is for for example and only for exampleProperty the present invention's preferred embodiment is discussed, propose these embodiment and be considered to the most useful and hold intelligible pass most to provideIn the description of method and principle of the present invention and concept aspect.
Preparation Example
Embodiment 1
Be prepared as follows suspension emulsion preparation:
A) prepare the missible oil of gamma cyhalothrin phase:
By active component gamma cyhalothrin (JiangsuYoushiChemistry, the excellent scholar's chemistry in Jiangsu) and oleic acidMethyl esters (Clariant) at room temperature mixes. After being left standstill 30 minutes, add emulsifier EL 360 (Clariant), and stir straightTo forming uniform solution.
B) prepare the discrete particles of lufenuron (ShanghaiStone, Shanghai stone) active component in continuous water:
| Component | Composition (gram) | Remarks |
| The former medicine of lufenuron (Shanghai stone) | 5 (by sterlings) | Active component |
| Soprophor BSU(Rhodia) | 0.5 | Dispersant |
| Soprophor FLK(Rhodia) | 1.5 | Dispersant |
| Propane diols (DOW) | 4 | Antifreeze |
| Rhodopol 23/W(Rhodia) | 0.15 | Thickener |
| Silicone oil (Degussa) | 0.5 | Defoamer |
| Water | Complement to 100 | Supporting agent |
Active component lufenuron is added with other together with applicable dispersant SoprophorBSU and SoprophorFLKAdd agent (for example antifreeze and defoamer) and the water of aequum and tentatively mix, and usage level agitation beads grinding machine is by its essenceFine lapping to be to maintain technological parameter, for example, maintain average grain diameter d50 and be no more than 3 microns and nearly all particle d90 and be no more than 6Micron.
C) prepare suspension emulsion
Under the stirring of the lasting Best Times amount of room temperature, oil phase (a) is added in water (b). Then, by appropriate thickenerGlue (Rhodopol23/W) adds in said mixture and continues stirring, hangs until this mixture at room temperature becomes uniformlyFloating agent. Low tempertaure storage stability (5 DEG C), the high-temperature storage stability (54 DEG C) and rare at 30 DEG C of this suspending agent are testedStability while releasing.
Embodiment 2
Be prepared as follows suspension emulsion preparation:
A) prepare the oil in water emulsion of gamma cyhalothrin EW phase:
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 8 (by sterlings) | Active component |
| Propene carbonate (Local) | 8 | Solvent |
| Atlox4912(Croda) | 2 | Emulsifying agent |
| Tween 80 (Croda) | 0.3 | Emulsifying agent |
At room temperature active component gamma cyhalothrin is mixed with Solvesso100. After being left standstill 30 minutes, addEnter emulsifier EL 360 and stir until form homogeneous solution. Then, with high shear, Lambda-Cyhalothrin is added to waterIn, obtain gamma cyhalothrin EW phase.
B) prepare the discrete particles of lufenuron in continuous water:
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 1.
C) suspension emulsion
Under the stirring that continues Best Times amount, oil-in-water phase (a) is added in water (b). Then, by appropriate thickeningAgent glue adds in said mixture and continues stirring, until mixture becomes uniform suspending agent. Test the low temperature of suspending agentBin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 3
Be prepared as follows suspension emulsion preparation:
A) prepare the missible oil of gamma cyhalothrin phase:
With having prepared the missible oil of gamma cyhalothrin with a) the contained identical general fashion of embodiment 1.
B) prepare the discrete particles of lufenuron in continuous water
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 1.
C) suspension emulsion
With having prepared suspension emulsion with c) the contained identical general procedure of embodiment 1. Test the low temperature of this suspending agentBin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 4
Be prepared as follows suspension emulsion preparation:
A) prepare the missible oil of Lambda-Cyhalothrin phase:
With having prepared the missible oil of gamma cyhalothrin with a) the contained identical general fashion of embodiment 1.
B) prepare the discrete particles of lufenuron in continuous water:
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 1.
C) suspension emulsion
With having prepared suspension emulsion with c) the contained identical general flow of embodiment 1. Test the low temperature of this suspending agentBin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 5
Be prepared as follows suspension emulsion preparation:
A) prepare the oil in water emulsion of gamma cyhalothrin EW phase
With having prepared the oil-in-water breast of gamma cyhalothrin EW phase with a) the contained identical general fashion of embodiment 2Agent.
B) prepare the discrete particles of lufenuron in continuous water:
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 2.
C) suspension emulsion
With having prepared suspension emulsion with c) the contained identical general procedure of embodiment 2. Test the low temperature of this suspending agentBin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 6
Be prepared as follows suspension emulsion preparation:
A) prepare the oil in water emulsion of gamma cyhalothrin EW phase
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 5 (by sterlings) | Active component |
| Methyl oleate (Clariant) | 5 | Solvent |
| Alkamuls OR/36 | 2 | Emulsifying agent |
With having prepared the oil-in-water breast of gamma cyhalothrin EW phase with a) the contained identical general fashion of embodiment 2Agent.
B) prepare the discrete particles of lufenuron in continuous water:
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 2.
C) suspension emulsion
With having prepared suspension emulsion with c) the contained identical general procedure of embodiment 2. Test the low temperature of this suspending agentBin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 7
Be prepared as follows suspension emulsion preparation:
A) prepare the missible oil of Lambda-Cyhalothrin phase
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 1 (by sterling) | Active component |
| Propene carbonate (Local) | 1 | Solvent |
| Atlox4912(Croda) | 2 | Emulsifying agent |
| Tween 80(Croda) | 0.3 | Emulsifying agent |
Prepared the missible oil of gamma cyhalothrin with the identical general fashion contained with embodiment 1 (a).
B) prepare the discrete particles of lufenuron in continuous water:
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 1.
C) suspension emulsion
Use the identical general procedure contained with embodiment 1 it (c) to prepare suspension emulsion. Test the low of this suspending agentTemperature bin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 8
Be prepared as follows suspension emulsion preparation:
A) prepare the oil in water emulsion of gamma cyhalothrin EW phase
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 30 (by sterlings) | Active component |
| Corn oil | 30 | Solvent |
| Alkamuls OR/36 | 3 | Emulsifying agent |
With having prepared the oil-in-water breast of gamma cyhalothrin EW phase with a) the contained identical general fashion of embodiment 2Agent.
B) prepare the discrete particles of lufenuron in continuous water
With having carried out the preparation of the concentrated suspension of lufenuron with b) the contained identical conventional method of embodiment 2.
C) suspension emulsion
Use with c) the contained identical general procedure of embodiment 2 and prepared suspension emulsion. Test the low of this suspending agentTemperature bin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 9
Be prepared as follows suspension emulsion preparation:
A) prepare the emulsifiable concentrates of Lambda-Cyhalothrin phase
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 40 (by sterlings) | Active component |
| Methyl oleate | 40 | Solvent |
| Alkamuls OR/36 | 3 | Emulsifying agent |
With having prepared the missible oil of gamma cyhalothrin with a) the contained identical general fashion of embodiment 1.
B) prepare the discrete particles of lufenuron in continuous water:
Use with b) the contained identical conventional method of embodiment 1 and carried out the preparation of the concentrated suspension of lufenuron.
C) suspension emulsion
Use with c) the contained identical general procedure of embodiment 1 and prepared suspension emulsion. Test the low of this suspending agentTemperature bin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Embodiment 10
Be prepared as follows suspension emulsion preparation:
A) prepare the oil in water emulsion of gamma cyhalothrin EW phase
| Component | Composition (gram) | Remarks |
| The former medicine of gamma cyhalothrin | 15 (by sterlings) | Active component |
| Propene carbonate | 15 | Solvent |
| Alkamuls OR/36 | 3 | Emulsifying agent |
With having prepared the oil-in-water breast of gamma cyhalothrin EW phase with a) the contained identical general fashion of embodiment 2Agent.
B) prepare the discrete particles of lufenuron in continuous water:
Use with b) the contained identical conventional method of embodiment 2 and carried out the preparation of the concentrated suspension of lufenuron.
C) suspension emulsion
Use with c) the contained identical general procedure of embodiment 2 and prepared suspension emulsion. Test the low of this suspending agentTemperature bin stability (5 DEG C), high-temperature storage stability (54 DEG C) and the stability while diluting at 30 DEG C.
Stability test result
Low-temperature stability and the heat-storage stability of sample are tested. In Cryo Equipment, at-5 DEG C, test 7 daysLow-temperature stability. In baking oven, at 54 DEG C, test the heat-storage stability of 14 days. Complete after test, said preparation is passed through342 order mesh screens filter, and observe the mobility of preparation and the formation of crystal.
In addition, that sample is taken out and remain on surrounding environment one from 54 DEG C is existing to the storage of having observed two days later to promoteResemble.
Also by sample at-5 DEG C low tempertaure storage and at 54 DEG C, determined before and after heat-storage preparation suspension and pointLoose sex expression. 1 gram of sample is added to 250 milliliters of graduated cylinders that contain standard hard water (CIPACDwater). If sample existsIn cylinder, sink fast, represent the bad dispersibility of sample. If sample can be dispersed in water at once, represent the dispersiveness of sampleGood. Then, cover lid by upper and lower graduated cylinder jolting 10 times, then leaves standstill 1 minute by graduated cylinder. If the solid of sedimentation is many, thatThe suspension of this sample is poor. If the solid of sedimentation is micro-, the suspension of this sample is good so.
Suspension emulsion preparation of the present invention has following characteristics:
Phytotoxicity test result
Carried out checking relatively phytotoxic experiment with following sample according to the present invention, and comparative experiments is based on citySell lufenuron 50EC (Match, Syngenta) product and gamma cyhalothrin 120EC (KARATE, Syngeta) product. PressThe seriousness of symptom, test sample is sorted out as follows:
0 grade: plant-less toxicity
1 grade: slight phytotoxicity
2 grades: serious phytotoxicity
Detect the phytotoxic experiment demonstration of preparation, the preparation of embodiment 1 to 10 all presents the plant poison of 0 stageProperty. Show that with the comparative experiments of commercially available lufenuron 50EC product and gamma cyhalothrin 120EC this product introduction goes out 2 stagesPhytotoxicity. Generally speaking, the phytotoxicity of the present invention's suspension emulsion preparation is significantly lower than commercially available EC product.
Can find out from above contained experimental data, suspension emulsion preparation according to the present invention all has good under low temperature and high temperatureGood mobility and bin stability. In addition, suspension emulsion has good dividing at-5 DEG C of low tempertaure storages with before and after 54 DEG C of heat-storagesLoose property and suspension. Moreover the phytotoxicity that preparation of the present invention demonstrates is significantly lower than commercially available EC preparation.
Claims (16)
1. a water-based suspension emulsion, is characterized in that comprising following component:
(a) disperse oil phase, it comprises:
(i) as the gamma cyhalothrin of the first active component
(ii) at least one solvent, is wherein dissolved with gamma cyhalothrin
(b) continuous water, it comprises:
(i) as the lufenuron of the second active component
(ii) water, is wherein suspended with lufenuron.
2. suspension emulsion claimed in claim 1, is characterized in that comprising gamma cyhalothrin and the conduct as emulgate ingredientThe lufenuron of suspending components.
3. suspension emulsion claimed in claim 1, is characterized in that component (b) also comprises:
(iii) at least one dispersant.
4. suspension emulsion claimed in claim 3, wherein described at least one dispersant in component (b) it (iii) is selected from methylAcrylic acid-methyl methacrylate-polyethyleneglycol-graft copolymer, tristyrylphenol ethoxylates and/or haveExpoxy propane/epoxyethane block copolymer of 10% to 50%EO.
5. suspension emulsion claimed in claim 4, wherein said expoxy propane/epoxyethane block copolymer has 20% to 50%EO.
6. suspension emulsion claimed in claim 4, wherein said expoxy propane/epoxyethane block copolymer has 30% to 40%EO.
7. for the preparation of the method for suspension emulsion described in any one in claim 1 to 6, it is characterized in that comprising the following steps:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: connecting by the particle that the water of active component, dispersant and aequum is mixed prepare lufenuron active componentDispersion in continuous water; And
Step 3: the water producing in the oil phase producing in step 1 and step 2 is merged.
8. for the preparation of the method for suspension emulsion described in any one in claim 1 to 6, it is characterized in that comprising the following steps:
Step 1: by active component and suitable solvent are prepared to Lambda-Cyhalothrin phase;
Step 2: the Lambda-Cyhalothrin in step 1 is added in water with high shear, obtains gamma cyhalothrin EWPhase
Step 3: by the water of active component, dispersant and aequum being mixed to prepare the particle of described lufenuron active componentDispersion in continuous water; And
Step 4: the water producing in the oil-in-water phase producing in step 2 and step 3 is merged.
9. for the preparation of the method for suspension emulsion described in any one in claim 1 to 6, it is characterized in that comprising the following steps:
Step 1: by active component is mixed to prepare Lambda-Cyhalothrin phase with solvent together with suitable emulsifying agent;
Step 2: by the water of active component, dispersant and aequum being mixed to prepare the particle of described lufenuron active componentDispersion in continuous water;
Step 3: step 2 produces continuing under the continuous stirring of Best Times amount, the described EC producing in step 1 to be added toWater;
Step 4: previously prepared thickener, makes its aquation and be ready in the subsequent step of mentioning as step 5 and addAdd;
Step 5: appropriate described thickener is added to the mixture in step 3 and continues to stir, until described mixture becomesSuspending agent uniformly.
10. method claimed in claim 9, wherein said thickener is polysaccharide or xanthan gum.
The method of 11. claims 9, wherein in step 2, described in mixing by usage level agitation beads grinding machine fine gtindingComponent is to maintain technological parameter.
The method of 12. claims 9, wherein in step 2, described in mixing by usage level agitation beads grinding machine fine gtindingComponent is no more than 3 microns and all particle d90 and is no more than 6 microns to maintain average grain diameter d50.
13. methods for the preparation of suspension emulsion described in any one in claim 1 to 6, is characterized in that comprising the following steps:
Step 1: by active component is mixed to prepare Lambda-Cyhalothrin phase with solvent together with suitable emulsifying agent;
Step 2: the Lambda-Cyhalothrin in step 1 is added in water with high shear, obtains gamma cyhalothrin EWPhase;
Step 3: connecting by the particle that the water of active component, dispersant and aequum is mixed prepare lufenuron active componentDispersion in continuous water;
Step 4: continue under the continuous stirring of Best Times amount, the O/w emulsion in step 2 to be added in step 3 described inWater;
Step 5: previously prepared thickener, makes its aquation and be ready in the subsequent step of mentioning as step 6 and addAdd;
The 6th step: appropriate described thickener is added to the mixture in step 4 and continues to stir, until described mixture becomesSuspending agent uniformly.
Method described in 14. claims 13, wherein said thickener is polysaccharide or xanthan gum.
The method of 15. claims 13, wherein, in step 3, mixes institute by usage level agitation beads grinding machine fine gtindingState component to maintain technological parameter.
The method of 16. claims 13, wherein, in step 3, mixes institute by usage level agitation beads grinding machine fine gtindingStating component is no more than 3 microns and all particle d90 and is no more than 6 microns to maintain average grain diameter d50.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2011/084191 WO2013091154A1 (en) | 2011-12-19 | 2011-12-19 | A novel aqueous suspoemulsion |
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| CN103997889B true CN103997889B (en) | 2016-05-11 |
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| CN (1) | CN103997889B (en) |
| FR (1) | FR2984079B1 (en) |
| PH (1) | PH12014501191B1 (en) |
| TW (1) | TWI543709B (en) |
| WO (1) | WO2013091154A1 (en) |
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| BR102013021474A8 (en) * | 2013-08-22 | 2019-05-21 | Rotam Agrochem Int Co Ltd | new aqueous suspoemulsion and a process for preparing it |
| US10881100B2 (en) * | 2014-01-29 | 2021-01-05 | Rotam Agrochem International Company Limited Chai Wan | Aqueous suspoemulsion containing lambda-cyhalothrin and methods for making and using the same |
| GB202202303D0 (en) * | 2022-02-21 | 2022-04-06 | Upl Corporation Ltd | Stable agrochemical compositon |
| WO2024057330A1 (en) * | 2022-09-13 | 2024-03-21 | Redson Retail & Reality Pvt. Ltd | Insecticidal composition |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1911035A (en) * | 2005-08-12 | 2007-02-14 | 南京第一农药有限公司 | Synergistic compound pesticide contg. high efficiency cyfluthrin and lurfenuron, and its application |
| CN101697733A (en) * | 2009-09-30 | 2010-04-28 | 深圳诺普信农化股份有限公司 | Lufenuron-containing aqueous emulsion and preparation method thereof |
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| WO2005096820A1 (en) * | 2004-03-25 | 2005-10-20 | Fmc Corporation | Liquid termiticide compositions of pyrethroids and a neonicitinoids |
| TWI524844B (en) * | 2008-05-12 | 2016-03-11 | 先正達合夥公司 | Pesticidal compositions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1911035A (en) * | 2005-08-12 | 2007-02-14 | 南京第一农药有限公司 | Synergistic compound pesticide contg. high efficiency cyfluthrin and lurfenuron, and its application |
| CN101697733A (en) * | 2009-09-30 | 2010-04-28 | 深圳诺普信农化股份有限公司 | Lufenuron-containing aqueous emulsion and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 第八章 悬浮乳剂;刘步林主编;《农药剂型加工技术》;化学工业出版社;19981031;第343-349页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| PH12014501191A1 (en) | 2014-09-08 |
| TWI543709B (en) | 2016-08-01 |
| FR2984079B1 (en) | 2015-12-25 |
| WO2013091154A1 (en) | 2013-06-27 |
| FR2984079A1 (en) | 2013-06-21 |
| PH12014501191B1 (en) | 2014-09-08 |
| TW201325451A (en) | 2013-07-01 |
| CN103997889A (en) | 2014-08-20 |
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