CN101697733B - Lufenuron-containing aqueous emulsion and preparation method thereof - Google Patents
Lufenuron-containing aqueous emulsion and preparation method thereof Download PDFInfo
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- CN101697733B CN101697733B CN200910190682.6A CN200910190682A CN101697733B CN 101697733 B CN101697733 B CN 101697733B CN 200910190682 A CN200910190682 A CN 200910190682A CN 101697733 B CN101697733 B CN 101697733B
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- aqueous emulsion
- lufenuron
- emulsifier
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- 239000000839 emulsion Substances 0.000 title claims abstract description 48
- 239000005912 Lufenuron Substances 0.000 title claims abstract description 36
- 229960000521 lufenuron Drugs 0.000 title claims abstract description 36
- 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 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004945 emulsification Methods 0.000 title 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 28
- -1 alkyl phthalate esters Chemical class 0.000 claims abstract description 27
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 12
- 239000002608 ionic liquid Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 150000002148 esters Chemical class 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 31
- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Natural products C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000003112 inhibitor Substances 0.000 claims description 9
- 239000002562 thickening agent Substances 0.000 claims description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 8
- 239000010452 phosphate Substances 0.000 claims description 8
- 229920001983 poloxamer Polymers 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005903 Gamma-cyhalothrin Substances 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 6
- ZXQYGBMAQZUVMI-GCMPRSNUSA-N gamma-cyhalothrin Chemical group CC1(C)[C@@H](\C=C(/Cl)C(F)(F)F)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-GCMPRSNUSA-N 0.000 claims description 6
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- 239000004359 castor oil Substances 0.000 claims description 4
- 235000019438 castor oil Nutrition 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 4
- 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 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 4
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 3
- 230000002528 anti-freeze Effects 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 claims description 2
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical class CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 claims description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 claims description 2
- 229910016467 AlCl 4 Inorganic materials 0.000 claims description 2
- OWYSSKOUATWAAO-UHFFFAOYSA-N C1(=CC=CC=C1)C=1C(=C(C(=C(C1)O)C=C)C1=CC=CC=C1)C1=CC=CC=C1 Chemical compound C1(=CC=CC=C1)C=1C(=C(C(=C(C1)O)C=C)C1=CC=CC=C1)C1=CC=CC=C1 OWYSSKOUATWAAO-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- WPPOGHDFAVQKLN-UHFFFAOYSA-N N-Octyl-2-pyrrolidone Chemical group CCCCCCCCN1CCCC1=O WPPOGHDFAVQKLN-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- ULQISTXYYBZJSJ-UHFFFAOYSA-N R-12-HOA Natural products CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical group CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 2
- 229920013821 hydroxy alkyl cellulose Polymers 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 239000012875 nonionic emulsifier Substances 0.000 claims description 2
- 229940055577 oleyl alcohol Drugs 0.000 claims description 2
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 claims description 2
- FFZANLXOAFSSGC-UHFFFAOYSA-N phosphide(1-) Chemical compound [P-] FFZANLXOAFSSGC-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- 229920005604 random copolymer Polymers 0.000 claims description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 2
- 239000004299 sodium benzoate Substances 0.000 claims description 2
- 235000010234 sodium benzoate Nutrition 0.000 claims description 2
- 239000004334 sorbic acid Substances 0.000 claims description 2
- 235000010199 sorbic acid Nutrition 0.000 claims description 2
- 229940075582 sorbic acid Drugs 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 2
- 229920001285 xanthan gum Polymers 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 239000002518 antifoaming agent Substances 0.000 claims 1
- 125000000373 fatty alcohol group Chemical group 0.000 claims 1
- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical group N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 abstract description 6
- 239000005875 Acetamiprid Chemical group 0.000 abstract description 6
- 239000005906 Imidacloprid Substances 0.000 abstract description 6
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical group [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 abstract description 6
- 229940056881 imidacloprid Drugs 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- KAATUXNTWXVJKI-NSHGMRRFSA-N (1R)-cis-(alphaS)-cypermethrin Chemical group CC1(C)[C@@H](C=C(Cl)Cl)[C@H]1C(=O)O[C@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-NSHGMRRFSA-N 0.000 abstract description 4
- 239000005944 Chlorpyrifos Chemical group 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- SBPBAQFWLVIOKP-UHFFFAOYSA-N chlorpyrifos Chemical group CCOP(=S)(OCC)OC1=NC(Cl)=C(Cl)C=C1Cl SBPBAQFWLVIOKP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000008346 aqueous phase Substances 0.000 abstract 3
- 239000012071 phase Substances 0.000 abstract 3
- ZXQYGBMAQZUVMI-RDDWSQKMSA-N (1S)-cis-(alphaR)-cyhalothrin Chemical group 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 abstract 1
- 125000002947 alkylene group Chemical group 0.000 abstract 1
- 125000000129 anionic group Chemical group 0.000 abstract 1
- 239000003945 anionic surfactant Substances 0.000 abstract 1
- 239000005910 lambda-Cyhalothrin Chemical group 0.000 abstract 1
- 239000002736 nonionic surfactant Substances 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 6
- 241000238631 Hexapoda Species 0.000 description 5
- 241000607479 Yersinia pestis Species 0.000 description 3
- 230000000749 insecticidal effect Effects 0.000 description 3
- 239000005946 Cypermethrin Substances 0.000 description 2
- KAATUXNTWXVJKI-UHFFFAOYSA-N cypermethrin Chemical compound CC1(C)C(C=C(Cl)Cl)C1C(=O)OC(C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 KAATUXNTWXVJKI-UHFFFAOYSA-N 0.000 description 2
- 229960005424 cypermethrin Drugs 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 241000675108 Citrus tangerina Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 241001486250 Etiella zinckenella Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 241000219146 Gossypium Species 0.000 description 1
- 241000255967 Helicoverpa zea Species 0.000 description 1
- 241000500437 Plutella xylostella Species 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 241001414989 Thysanoptera Species 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a lufenuron-containing aqueous emulsion and a preparation method thereof. The aqueous emulsion mainly comprises an active component A, an active component B, solvent, emulsifier and water, wherein the active component A is lufenuron; the active component B is imidacloprid, acetamiprid, lambda-Cyhalothrin, beta-cypermethrin or chlorpyrifos; the solvent is one or more of aromatic hydrocarbons, alkyl phthalate esters, alkylene carbonic esters, ionic liquids and N-alkyl pyrrolidones; and the emulsifier is one of mixture of anionic and nonionic surfactants. The preparation method comprises: (1) preparing an oil phase and an aqueous phase; and (2) adding the oil phase to the aqueous phase or adding the aqueous phase to the oil phase under a high-shear condition so as to obtain the aqueous emulsion. The lufenuron-containing aqueous emulsion has the advantages of high stability and small particle size.
Description
Technical field
The invention belongs to pesticidal preparations field, relate in particular to a kind of aqueous emulsion that contains lufenuron and preparation method thereof.
Background technology
Lufenuron (Lufenuron) is the novel benzoyl area kind insecticidal/acaricidal agent of one of being developed by Syngenta Co.,Ltd of Switzerland; its chemistry RS by name)-1-[2; the chloro-4-(1 of 5-bis-; 1; 2,3,3; 3-hexafluoro propoxyl group) phenyl]-3-(2,6-difluoro benzoyl) urea.This is that one has the inhibiting insect growth regulator, IGR of chitin synthesis, has unique insecticidal mechanism, by acting on insect larvae, stoping decortication process to kill off the insect pests.Lufenuron is mainly used in preventing and treating the insects such as diamond-back moth, lima bean pod borer, thrips, the blue or green worm of swallow, cotton bollworm, to crop safety, corn, vegetables, oranges and tangerines, cotton, potato, grape, Soybean and Other Crops all can be used, it is advantageous that the insect that can prevent and treat pyrethroid and organophosphorous pesticide generation resistance, be suitable for Integrated pest and administer.
Aqueous emulsion is that water-fast original liquid body or former medicine are dissolved in a kind of formulations of pesticide of water-fast organic solvent gained Solution Dispersion in water.Pesticide original medicine is made aqueous emulsion, its particle diameter can than traditional can wet-milling (WP), the particle diameter of suspending agent (SC) is less, drug effect is better, and compared with can wet-milling, aqueous emulsion without dust, endangers little to producer, user in manufacturing, using.But, because the former medicine of difference need to be selected to dissolve the solvent of former medicine and suitable emulsifier, just can be mixed with the aqueous emulsion of good stability, and current alternative solvent phase is to less, therefore, relatively difficulty of aqueous emulsion research and development at present.
The long-term use of single medicament often causes the raising of pest resistance to insecticide, increases the difficulty of control, affects the output of crop.Therefore,, by using Recompounded pesticide to increase drug effect, reduce costs, expand insecticidal spectrum, increase economic efficiency, become most countries and regional agriculturist's selection.Not yet have about lufenuron at present, occur with the report of the Recompounded pesticide aqueous emulsion of Imidacloprid or Acetamiprid or gamma cyhalothrin or beta-cypermethrin or chlopyrifos.
Summary of the invention
The object of the embodiment of the present invention is to provide a kind of high stability aqueous emulsion that contains lufenuron.
Another object of the embodiment of the present invention is to provide the preparation method of above-mentioned aqueous emulsion.
The aqueous emulsion that contains lufenuron of the embodiment of the present invention, comprises the following component according to weight percent meter:
Active components A 1%-50%
Active component B 1%-50%
Solvent 5%-50%
Emulsifier 1%-20%
Antifreezing agent 0%-8%
Thickener 0%-5%
Mould inhibitor 0%-5%
Defoamer 0%-0.5%
Water 10%-70%
Wherein, described active components A is lufenuron, active component B is the one in Imidacloprid, Acetamiprid, gamma cyhalothrin, beta-cypermethrin and chlopyrifos, and described solvent is one or more materials in aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone; Emulsifier is the mixing of one or more emulsifier in anion and nonionic surface active agent.
The preparation method of the aqueous emulsion that contains lufenuron of the embodiment of the present invention, comprises the following steps:
(1) active components A and active component B are dissolved in solvent, add or do not add the emulsifier that HLB value is 5-7, be evenly mixed to get oil phase;
The emulsifier of HLB value > 10 is mixed with water, add or not with antifreeze, defoamer, thickener, mould inhibitor, mix and obtain water;
(2) under high shear, oil phase is joined in water or by water and joined in oil phase, make aqueous emulsion.
Technique scheme, by selecting one or more materials in aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone as solvent, select the mixing of one or more emulsifier in anion and nonionic agent as emulsifier, be mixed with the pesticide emulsion in water that contains active components A and active component B, this aqueous emulsion has advantages of that stability is high, particle diameter is little (referring to table 11).
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides a kind of good stability, and the aqueous emulsion that contains lufenuron comprises the following component according to weight percent meter:
Active components A 1%-50%
Active component B 1%-50%
Solvent 5%-50%
Emulsifier 1%-20%
Antifreezing agent 0%-8%
Thickener 0%-5%
Mould inhibitor 0%-5%
Defoamer 0%-0.5%
Water 10%-70%
Wherein, active components A is lufenuron, active component B is the one in Imidacloprid, Acetamiprid, gamma cyhalothrin, beta-cypermethrin and chlopyrifos, and solvent is one or more materials in aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone; Emulsifier is the mixing of one or more emulsifier in anion and nonionic surface active agent.
Further, above-mentioned solvent weight percent is preferably 10%-30%, depending on the solvability of former medicine and different.
Further, above-mentioned phthalate solvent is repefral, diethylester, dibutyl ester and butyl benzyl ester; Alkylene carbonate kind solvent is propene carbonate and butylene; In ionic liquid kind solvent, cationic solvent has glyoxaline cation, pyridylium, alkyl ammonium cation and alkyl phosphorus cation, and anion has Cl
-, Br
-, AlCl
4 -, [BF
4]
-, [PF
6]
-, [CF
3sO
3]
-[(CF
3sO
3)
2n]
-; N-alkyl pyrrolidine ketones solvent is N-n-octyl pyrrolidones and N-dodecyl pyrrolidones; Aromatic hydrocarbon solvent is dimethylbenzene, toluene and boiling point higher than the reformed arene of 150 DEG C.Above-mentioned solvent is all the little solvent of solvability in water, is suitable for preparing aqueous emulsion.In solvability permission situation, preferentially select boiling point higher than the reformed arene of 150 DEG C, main for environmental protection and the consideration to user's health,
Further, above-mentioned reformed arene is Solvesso 100, Solvesso 150 and Solvesso 200.
Further, above-mentioned anion emulsifier has triphenyl vinyl phenol polyoxyethylene ether phosphate, the phosphate of Pluronic PE 6800 etc., nonionic emulsifier has fatty alcohol Pluronic PE 6800, oleyl alcohol and (or) hexadecanol APEO (EO 5-5.5), sorbitol anhydride monolaurate, monopalmitate, single stearyl ester, monoleate, polyoxyethylene nonylphenol ether (EO 4-20), castor oil polyoxyethylene ether (EO 12-40), poly-(12-hydroxyl stearic acid) polyoxyethylene ether block copolymers (ABA type), poly-isosuccinic acid acid anhydride-ethylene glycol copolymer etc.
Further, mentioned emulsifier weight content in aqueous emulsion is preferably 2%-10%, more preferably 3%-8% mass ratio.
There is no particular restriction for above-mentioned antifreezing agent, is the conventional antifreezing agent in this area, the combination of for example, in optional spent glycol, propane diols, glycerine and urea one or more.
There is no particular restriction for above-mentioned thickener, is this area customary thickeners, the combination that for example can select one or more materials in xanthans, hydroxy alkyl cellulose class, polyvinylpyrrolidone, polyvinyl alcohol.This thickener viscosity preferably, between 100-2000cP, makes the free-flow of material energy.
There is no particular restriction for above-mentioned mould inhibitor, is the conventional mould inhibitor in this area, and mould inhibitor is the combination of one or more materials in Sodium Benzoate, formaldehyde, sorbic acid.
There is no particular restriction for above-mentioned defoamer, is this area defoamers, for example, can select the combination of one or more materials in silicone based (as poly-alkyl silicon oxirane) and alcohols (as isooctanol).
The present invention also provides a kind of preparation method of the aqueous emulsion that contains lufenuron, comprises the following steps:
(1) active components A and active component B are dissolved in solvent, add or do not add the emulsifier that HLB value is 5-7, be evenly mixed to get oil phase;
The emulsifier of HLB value > 10 is mixed with water, add or not with antifreeze, defoamer, thickener, mould inhibitor, mix and obtain water;
(2) under high shear, oil phase is joined in water or by water and added in oil phase, make aqueous emulsion.
Above-mentionedly join in water as oil phase, high shear rates is 5000-10000 rev/min, and as water joins in oil phase, high shear rates is 4000-10000 rev/min, all can make particle diameter at the product of 0.2～10 micron.
The emulsifier that above-mentioned HLB value is 5-7 is isooctanol APEO, EO/PO random copolymer, poly-(12-hydroxy stearic acid) polyoxyethylene ether block copolymers etc. such as;
The emulsifier of HLB value > 10 is castor oil polyoxyethylene ether, alkylpolyoxyethylene, triphenylethylene phenol polyethenoxy ether phosphate, fatty alcohol Pluronic PE 6800, polyoxyethylene nonylphenol ether, Pluronic PE 6800 phosphate, poly-isosuccinic acid acid anhydride-ethylene glycol copolymer etc. such as.
Embodiment 1
Table 1.20% lufenuron Imidacloprid water emulsion formula (100 grams)
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 1a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 1b.
Embodiment 2
Table 2.40% lufenuron Imidacloprid water emulsion formula (100 grams)
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 2a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 2b.
Embodiment 3
Table 3.20% lufenuron Acetamiprid water emulsion formula (100 grams)
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 3a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 3b.
Embodiment 4
Table 4.40% lufenuron Acetamiprid water emulsion formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 4a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 4b.
Embodiment 5
Table 5.20% lufenuron gamma cyhalothrin water emulsion formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 5a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 5b.
Embodiment 6
Table 6.40% lufenuron gamma cyhalothrin water emulsion formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 6a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 6b.
Embodiment 7
Table 7.20% lufenuron high performance aqueous emulsion of cypermethrin formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 7a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 7b.
Embodiment 8
Table 8.40% lufenuron high performance aqueous emulsion of cypermethrin formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 8a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 8b.
Embodiment 9
Table 9.20% lufenuron chlorpyrifos aqueous emulsion formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 9a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 9b.
Embodiment 10
Table 10.40% lufenuron chlorpyrifos aqueous emulsion formula
Under high shear (5000-10000rpm), oil phase is added and in water, obtains sample 10a; Otherwise, under high shear (4000-10000rpm), water is added to and in oil phase, obtains sample 10b.
The indices of aqueous emulsion sample
Table 11
A. recorded by No. 2 rotor speeds 60 of ROOKFIELD DVII+Pro viscometer.
B. recorded by Ma Erwen laser fineness gage (mastersizer 2000).
From table 11, data can be found out, the aqueous emulsion in the embodiment of the present invention, and good stability, particle diameter is little.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. contain an aqueous emulsion for lufenuron, comprise the following component according to weight percent meter:
Wherein, described active components A is lufenuron, and active component B is gamma cyhalothrin, and described solvent is one or more materials in aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone; Described emulsifier is the mixing of one or more emulsifier in anion and nonionic surface active agent; Wherein, described aromatic hydrocarbons is dimethylbenzene, toluene and boiling point higher than the reformed arene of 150 DEG C, described alkyl phthalate kind solvent is repefral, diethylester, dibutyl ester and butyl benzyl ester, described alkylene carbonate kind solvent is propene carbonate and butylene, in described ionic liquid kind solvent, cationic solvent has glyoxaline cation, pyridylium, alkyl ammonium cation and alkyl phosphorus cation, and anion has Cl
-, Br
-, AlCl
4 -, [BF
4]
-, [PF
6]
-, [CF
3sO
3]
-[(CF
3sO
3)
2n]
-, described N-alkyl pyrrolidine ketones solvent is N-n-octyl pyrrolidones and N-dodecyl pyrrolidones; Described anion emulsifier is the phosphate of triphenyl vinyl phenol polyoxyethylene ether phosphate, Pluronic PE 6800, and described nonionic emulsifier is fatty alcohol Pluronic PE 6800, oleyl alcohol and (or) hexadecanol APEO, sorbitol anhydride monolaurate, monopalmitate, single stearyl ester, monoleate, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, poly-(12-hydroxyl stearic acid) polyoxyethylene ether block copolymers and poly-isosuccinic acid acid anhydride-ethylene glycol copolymer.
2. the aqueous emulsion that contains as claimed in claim 1 lufenuron, is characterized in that, wherein, described solvent weight percent is 10%-30%.
3. the aqueous emulsion that contains as claimed in claim 1 lufenuron, is characterized in that, wherein, described reformed arene is Solvesso100, Solvesso150 and Solvesso200.
4. the aqueous emulsion that contains as claimed in claim 1 lufenuron, is characterized in that, wherein, described emulsifier weight content in aqueous emulsion is 2～10%.
5. the aqueous emulsion that contains as claimed in claim 4 lufenuron, is characterized in that, wherein, described emulsifier weight content in aqueous emulsion is 3～8%.
6. the aqueous emulsion that contains as claimed in claim 1 lufenuron, is characterized in that, wherein, described antifreezing agent is one or more combination in ethylene glycol, propane diols, glycerine and urea; Thickener is the combination of one or more materials in xanthans, hydroxy alkyl cellulose class, polyvinylpyrrolidone and polyvinyl alcohol; Mould inhibitor be in Sodium Benzoate, formaldehyde, sorbic acid in the combination of one or more materials; Described defoamer is the combination of one or more materials in silicone based and alcohol defoaming agent.
7. the preparation method of the aqueous emulsion that contains lufenuron as described in claim 1 to 6 any one, comprises the following steps:
(1) active components A and active component B are dissolved in solvent, add or do not add the emulsifier that HLB value is 5-7, be evenly mixed to get oil phase;
The emulsifier of HLB value >10 is mixed with water, add or not with antifreeze, defoamer, thickener, mould inhibitor, mix and obtain water;
(2) under high shear, oil phase is joined in water or by water and joined in oil phase, make aqueous emulsion.
8. contain as claimed in claim 7 the preparation method of the aqueous emulsion of lufenuron, wherein, the emulsifier that HLB value is 5-7 is one or more in isooctanol APEO, EO/PO random copolymer and poly-(12-hydroxy stearic acid) polyoxyethylene ether block copolymers; The emulsifier of HLB value >10 is one or more in castor oil polyoxyethylene ether, alkylpolyoxyethylene, triphenylethylene phenol polyethenoxy ether phosphate, fatty alcohol Pluronic PE 6800, polyoxyethylene nonylphenol ether, Pluronic PE 6800 phosphate and poly-isosuccinic acid acid anhydride-ethylene glycol copolymer.
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| BRPI1002174A2 (en) * | 2010-06-17 | 2012-03-13 | Rotam Agrochem International Company Ltd | AGROCHEMICAL COMPOSITION, USE OF A C2-C4 DIALKYLENE GLYCOL DI- / MONO-C1-C4 Ether AQUIL, METHOD TO REDUCE EYE IRRITATION OF INSETICID FORMULATIONS, LOCAL PEST TREATMENT METHOD AND |
| CN102308788B (en) * | 2011-07-07 | 2013-10-23 | 中国农业大学 | A kind of insecticidal pesticide preparation using ionic liquid as co-solvent and preparation method thereof |
| CN102907457A (en) * | 2011-08-03 | 2013-02-06 | 龚亚慧 | Pesticidal microemulsion and preparation method thereof |
| CN103053591A (en) * | 2011-10-18 | 2013-04-24 | 南京华洲药业有限公司 | Synergistic insecticidal composition containing lufenuron and pyrethroid insecticide and its application |
| WO2013091154A1 (en) * | 2011-12-19 | 2013-06-27 | Rotam Agrochem International Co., Ltd | A novel aqueous suspoemulsion |
| CN103598176B (en) * | 2013-05-13 | 2015-03-11 | 北京农学院 | 1,2-dihydroxyl- hexacosanyl-4-one emulsion in water and preparation method thereof |
| 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 |
| WO2024057330A1 (en) * | 2022-09-13 | 2024-03-21 | Redson Retail & Reality Pvt. Ltd | Insecticidal composition |
| CN116918826A (en) * | 2023-07-17 | 2023-10-24 | 上海悦联生物科技有限公司 | A 19% high-efficiency cyhalothrin·lufenuron suspension and its preparation method |
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