CN101627767A - Emulsion in water containing lufenuron and preparation method thereof - Google Patents
Emulsion in water containing lufenuron and preparation method thereof Download PDFInfo
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- CN101627767A CN101627767A CN200910041922A CN200910041922A CN101627767A CN 101627767 A CN101627767 A CN 101627767A CN 200910041922 A CN200910041922 A CN 200910041922A CN 200910041922 A CN200910041922 A CN 200910041922A CN 101627767 A CN101627767 A CN 101627767A
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- Prior art keywords
- aqueous emulsion
- water
- solvent
- acarus tritici
- tritici urea
- Prior art date
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- 239000000839 emulsion Substances 0.000 title claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000005912 Lufenuron Substances 0.000 title abstract description 5
- 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 abstract description 5
- 229960000521 lufenuron Drugs 0.000 title abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 28
- -1 UV-protectant Substances 0.000 claims abstract description 25
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 13
- 239000002562 thickening agent Substances 0.000 claims abstract description 10
- 239000013530 defoamer Substances 0.000 claims abstract description 9
- 239000003921 oil Substances 0.000 claims description 44
- 239000012071 phase Substances 0.000 claims description 42
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 40
- 239000004202 carbamide Substances 0.000 claims description 40
- 241000934067 Acarus Species 0.000 claims description 36
- 239000008346 aqueous phase Substances 0.000 claims description 19
- 239000003814 drug Substances 0.000 claims description 18
- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Natural products C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 239000003112 inhibitor Substances 0.000 claims description 8
- 239000005660 Abamectin Substances 0.000 claims description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 6
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical group C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 claims description 6
- 150000002170 ethers Chemical class 0.000 claims description 6
- 239000002608 ionic liquid Chemical class 0.000 claims description 6
- 239000004322 Butylated hydroxytoluene Substances 0.000 claims description 5
- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical group COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000004094 surface-active agent Substances 0.000 claims description 5
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 4
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical class C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 239000003945 anionic surfactant Substances 0.000 claims description 3
- 229940095259 butylated hydroxytoluene Drugs 0.000 claims description 3
- 239000004359 castor oil Substances 0.000 claims description 3
- 235000019438 castor oil Nutrition 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 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 3
- 229920013821 hydroxy alkyl cellulose Polymers 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 3
- 235000010234 sodium benzoate Nutrition 0.000 claims description 3
- 239000004299 sodium benzoate Substances 0.000 claims description 3
- 235000010199 sorbic acid Nutrition 0.000 claims description 3
- 239000004334 sorbic acid Substances 0.000 claims description 3
- 229940075582 sorbic acid Drugs 0.000 claims description 3
- 229920001285 xanthan gum Polymers 0.000 claims description 3
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical class CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 claims description 2
- 229910016467 AlCl 4 Inorganic materials 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- WPPOGHDFAVQKLN-UHFFFAOYSA-N N-Octyl-2-pyrrolidone Chemical class CCCCCCCCN1CCCC1=O WPPOGHDFAVQKLN-UHFFFAOYSA-N 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 claims 1
- FFZANLXOAFSSGC-UHFFFAOYSA-N phosphide(1-) Chemical compound [P-] FFZANLXOAFSSGC-UHFFFAOYSA-N 0.000 claims 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003960 organic solvent Substances 0.000 abstract description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 3
- 230000036541 health Effects 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000654 additive Substances 0.000 abstract 1
- 230000002528 anti-freeze Effects 0.000 abstract 1
- 239000003429 antifungal agent Substances 0.000 abstract 1
- 229940121375 antifungal agent Drugs 0.000 abstract 1
- 238000003672 processing method Methods 0.000 abstract 1
- 239000008096 xylene Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 241000238631 Hexapoda Species 0.000 description 6
- 239000000575 pesticide Substances 0.000 description 6
- 239000012752 auxiliary agent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000009472 formulation Methods 0.000 description 4
- 241000607479 Yersinia pestis Species 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000000749 insecticidal effect Effects 0.000 description 3
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 2
- 230000000857 drug effect Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 241000675108 Citrus tangerina Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 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 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
- 241001465754 Metazoa 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
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000000129 anionic group Chemical group 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
- 229920001400 block copolymer Polymers 0.000 description 1
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 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
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 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
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicinal Preparation (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses an emulsion in water containing lufenuron and a preparation method thereof; compared with the traditional emulsion in water, the emulsion in water is different in that the emulsion in water adopts more environmentally friendly solvent in stead of traditional toluene and xylene and adds proper emulsifier, UV-protectant, thickener, antifreeze, antifungal agent, defoamer and other additives and the balance water to prepare the stable emulsion in water by certain processing methods. Compared with the traditional emulsifiable solution, the emulsion in water reduces the dosage of organic solvent which is harmful to the environment, avoids the effects of the preparation to the environment and the health of users and corresponds to the current green agricultural development direction.
Description
Technical field
The present invention relates to a kind of pesticidal preparations and preparation method thereof, especially a kind of aqueous emulsion that contains the Acarus tritici urea and preparation method thereof.
Background technology
Aqueous emulsion is an important directions of present formulations of pesticide development, is that water-fast original liquid body or former medicine are dissolved in water-fast organic solvent gained solution and are scattered in a kind of formulations of pesticide in the water.Compare with other formulation, the advantage of aqueous emulsion is low toxicity, environmental protection, nothing catch fire danger, storage and convenient transportation, and can mix with arbitrary proportion with water, shortcoming is relatively difficulty of research and development, and proper auxiliary agent and solvent are selected fewer relatively at present.Prepare suitable aqueous emulsion, pesticide original medicine must possess several conditions, and at first the solvability in the water should be relatively low, and general requirement is lower than 200mg/L, and secondly chemical stability will be got well, and is difficult for having the generation of decomposing phenomenon in water.The main points of aqueous emulsion exploitation are by the means of high shear the oil droplet of aqueous phase to be broken into micron-sized dispersity, and the adding by auxiliary agent is simultaneously carried out it chemistry parcel, reduced the repulsive interaction that the surface can or utilize the surface electrical layer and make whole aqueous emulsion system stable.The aqueous emulsion that meets cold (heat) storage stability, dilution stability, pourability, viscosity and pH value index at present is also fewer, and relevant both at home and abroad report is also few, therefore also has sizable research and development potentiality in this direction.Be today that people paid attention in conventional dosage forms such as missible oil day by day for the harm of human and livestock health and living environment, the application potential of aqueous emulsion has been pointed out the road of a light undoubtedly.
Acarus tritici urea (Lufenuron) is a kind of novel benzoyl area kind insecticidal/acaricidal agent by the exploitation of Switzerland Syngenta Co.,Ltd; its chemistry RS by name)-and 1-[2,5-two chloro-4-(1,1; 2; 3,3,3-hexafluoro propoxyl group) phenyl]-3-(2; the 6-difluoro benzoyl) urea; this is a kind of synthetic inhibiting insect growth regulator, IGR of chitin that has, and has unique insecticidal mechanism, by acting on insect larvae, stoping the decortication process to kill off the insect pests.The Acarus tritici urea is mainly used in insects such as control 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, be suitable for comprehensive insect pest and administer pyrethroid and organophosphorous pesticide generation resistance.
The long-term use of single medicament often causes the raising of pest resistance to insecticide, increases the difficulty of control, influences the output of crop.Therefore, increase drug effect, reduce cost, enlarge insecticidal spectrum, increase economic efficiency, become most of countries and regions agriculturist's selection by using Recompounded pesticide.
A kind of pesticide original medicine is made aqueous emulsion, but its particle diameter can be littler than the particle diameter of traditional wet-milling (WP), suspending agent (SC), and drug effect is better, but and compare with wet-milling, aqueous emulsion does not have dust in making, using, endanger little to producer, user.But the aqueous emulsion solvent for use has certain restriction, and Acarus tritici urea etc. then is difficult to be dissolved in the general organic solvent, therefore, makes aqueous emulsion and has certain difficulty.Mostly aqueous emulsion in the past is volatile poisonous organic solvents such as toluene, dimethylbenzene if adopting, bigger for environment and people and animals' harm, and for as Avermectin, first to tie up former medicine solvability such as salt not high, hindered the application of aqueous emulsion in these fields.
In view of this, be necessary to provide a kind of utilize the higher solvent of relative environmental protection and solvability contain lufenuron aqueous emulsion and preparation method thereof.
Summary of the invention
The objective of the invention is to: a kind of high stability aqueous emulsion that contains the Acarus tritici urea and preparation method thereof is provided.
Research and develop a kind of stable water emulsion formula, its key problem is choice of Solvent, the inventor is on the basis of in the past researching and developing experience, through big quantity research and experiment sieving, find the part water-immiscible solvent, as wherein a kind of or its combination in the aromatic hydrocarbons of reforming, alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone, be suitable as solvent and be used to prepare the aqueous emulsion that contains the Acarus tritici urea.
In view of the above, determine the prescription following (mass percent) of lufenuron aqueous emulsion: active components A: 1%-50%; Active component B:0-50%; Solvent 5%-50%; Emulsifier 1%-20%; UV-protectant 0%-3%; Antifreezing agent 0%-8%; Thickener 0%-5%; Mould inhibitor 0%-5%; Defoamer 0%-0.5%; Water: surplus; Above-mentioned active components A is the Acarus tritici urea, and active component B is an Avermectin, or first dimension salt, or capillary, or pleocidin.
Described solvent is wherein a kind of or its combination in reformation aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, the N-alkyl pyrrolidine ketone.
Described emulsifier is phosphoric acid ester anion surfactant and EO/PO block copolymer, polystyrene-based phenol polyethenoxy base ethers, castor oil polyoxyethylene ether class, polyoxyethylene nonylphenol ether class, fatty alcohol polyethenoxy ether class nonionic surface active agent, can select one of them or its combination.
Because Avermectin and first dimension salt can decompose under illumination condition, so must add the UV-protectant in containing these two kinds of formulations of active ingredients, protectant commonly used has butylhydroxy anisole (BHA) or 2,6-Butylated Hydroxytoluene (BHT).
Described antifreezing agent is a kind of or its combination in ethylene glycol, propane diols, glycerine, the urea.
Described thickener is a kind of or its combination in xanthans, hydroxy alkyl cellulose class, polyvinylpyrrolidone, the polyvinyl alcohol.
Described mould inhibitor is a kind of or its combination in Sodium Benzoate, formaldehyde, the sorbic acid.
Described defoamer is a kind of or its combination in silicone based, the alcohols.
The above-mentioned preparation method who contains the aqueous emulsion of Acarus tritici urea may further comprise the steps: 1) former medicine A or former medicine A and former medicine B are dissolved in the solvent, optionally add the emulsifier of low HLB (5-7) or do not add and obtain oil phase; 2) emulsifier, UV-protectant, antifreezing agent, defoamer, thickener, the mould inhibitor of high HLB (＞10) mixed with water obtain water; 3) under high shear, oil phase is joined aqueous phase or water is joined in the oil phase, make the aqueous emulsion of high stability; Wherein, the 1st) step and the 2nd) order in step in no particular order.
Compared with prior art, the aqueous emulsion that contains the Acarus tritici urea of the present invention is selected the solvent of relative environmental protection for use, and under the cooperation of corresponding emulsifier and other auxiliary agent, has reached certain stability.
Embodiment
Aqueous emulsion is oil phase and the aqueous mixture that utilizes in the machine power shearing system, makes oil phase be dispersed in aqueous phase with minimum drop, and surfactant in the liquid phase and various auxiliary agent make emulsion keep stable.During the preparation aqueous emulsion, after including the water homogeneous phase of surfactant and various auxiliary agents, under high speed shear (4000-10000 rev/min), join in the oil phase, can make the product of particle diameter at the 0.3-10 micron, perhaps oil phase is added to aqueous phase under the condition of high shear (5000-10000), also can makes the product of same quality.
Because former medicines such as Acarus tritici urea are difficult to be dissolved in the general organic solvent, therefore at first need to select appropriate organic solvent that it is prepared into oil phase.Through attempt finding, the mixture of alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone and they and reformation aromatic hydrocarbons etc. are applicable.
The concrete preparation method of aqueous emulsion of the present invention mainly comprised for three steps: at first, former medicine A or former medicine A and former medicine B are dissolved in the solvent, add the emulsifier of low HLB (5-7) or do not add and obtain oil phase; Then, emulsifier, antifreezing agent, defoamer, thickener, the mould inhibitor of high HLB (＞10) mixed with water obtain water; At last, under high shear, oil phase is joined aqueous phase or water is joined in the oil phase, can make the stabilize water emulsion of particle diameter at the 0.2-10 micron; Wherein, the 1st) step and the 2nd) order in step in no particular order.
Above-mentioned phthalate solvent can be repefral, diethylester, dibutyl ester, butyl benzyl ester etc.; The alkylene carbonate kind solvent can be propene carbonate, butylene etc.; Cation commonly used in the ionic liquid kind solvent has glyoxaline cation, pyridylium, alkyl ammonium cation, alkyl phosphorus cation etc., and anion commonly used has Cl
-, Br
-, AlCl
4 -, [BF
4]
-, [PF
6]
-, [CF
3SO
3]
-, [(CF
3SO
3)
2N]
-Deng; N-alkyl pyrrolidine ketones solvent can be N-n-octyl pyrrolidones, N-dodecyl pyrrolidones etc.; The reformation aromatic hydrocarbon solvent can be Solvesso 100,150,200 etc.The content of solvent in aqueous emulsion is the 5%-50% mass ratio, is preferably 10%-30% mass ratio (look the solvability of former medicine and different).
Described emulsifier can be anionic, nonionic, or its mixture.The anion surfactant that is suitable for has the triphenyl vinyl phenol polyoxyethylene ether phosphate, the phosphate of EO/PO block copolymer etc., the non-ionic surface active agent that is suitable for has fatty alcohol EO/PO block copolymer, oleyl alcohol and (or) hexadecanol APEO (EO 5-5.5), the sorbitol anhydride monolaurate, monopalmitate, single stearyl ester, monoleate etc., polyoxyethylene nonylphenol ether (EO 4-20), castor oil polyoxyethylene ether (EO 12-40), poly-(the hard ester acid of 12-hydroxyl) polyoxyethylene ether block copolymers (ABA type), poly-isosuccinic acid acid anhydride-ethylene glycol copolymer etc.Mixing use or the moon/nonionic use separately between anion and nonionic mixing or the moon/nonionic, and usage amount is the 1%-20% mass ratio, is preferably the 2%-10% mass ratio, is preferably the 3%-8% mass ratio.
The UV-protectant can be selected butylhydroxy anisole (BHA) or 2 for use, 6-Butylated Hydroxytoluene (BHT).
The antifreezing agent that is applicable to low-temperature stabilization has ethylene glycol, propane diols, glycerine, and urea also is suitable for, and the usage amount of antifreezing agent is between the 0%-8% mass ratio.
Thickener can be selected a kind of or its combination in xanthans, hydroxy alkyl cellulose class, polyvinylpyrrolidone, the polyvinyl alcohol for use, and viscosity is preferably between 100-2000cP, makes that material can free-flow.The consumption of thickener is the 0%-5% mass ratio.
Mould inhibitor can be selected a kind of or its combination in Sodium Benzoate, formaldehyde, the sorbic acid for use, and consumption is the 0%-5% mass ratio.
Defoamer can be selected for use silicone based, and as poly-alkyl silicon oxirane, alcohols such as isooctanol also are suitable for.Usage amount is between 0%-0.5%.
In order to make purpose of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to these examples absolutely not.The following stated only is the present invention embodiment preferably, only is used to explain the present invention, can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that all any modifications of being made within the spirit and principles in the present invention, be equal to replacement and improvement etc., all should be included within protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with appended claims.
Embodiment 1:
Table 1,20% Acarus tritici urea EW prescription (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 1a, otherwise, water is added to obtains sample 1b in the oil phase.
Embodiment 2:
Table 2,20% Acarus tritici urea EW prescription (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 2a, otherwise, water is added to obtains sample 2b in the oil phase.
Embodiment 3:
Table 3,40% Acarus tritici urea EW prescription (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 3a, otherwise, water is added to obtains sample 3b in the oil phase.
Embodiment 4:
Table 4,15% Avermectin Acarus tritici urea EW prescription (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 4a, otherwise, water is added to obtains sample 4b in the oil phase.
Embodiment 5:
Table 5,30% Avermectin Acarus tritici urea EW (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 5a, otherwise, water is added to obtains sample 5b in the oil phase.
Embodiment 6:
Table 6,15% first dimension Acarus tritici urea EW prescription (100 gram)
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 6a, otherwise, water is added to obtains sample 6b in the oil phase.
Embodiment 7:
Table 7,30% first dimension Acarus tritici urea EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 7a, otherwise, water is added to obtains sample 7b in the oil phase.
Embodiment 8:
Table 8,20% Acarus tritici urea capillary EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 8a, otherwise, water is added to obtains sample 8b in the oil phase.
Embodiment 9:
Table 9,30% Acarus tritici urea capillary EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 9a, otherwise, water is added to obtains sample 9b in the oil phase.
Embodiment 10:
Table 10,40% Acarus tritici urea capillary EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 10a, otherwise, water is added to obtains sample 10b in the oil phase.
Embodiment 11:
Table 11,20% Acarus tritici urea pleocidin EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 11a, otherwise, water is added to obtains sample 11b in the oil phase.
Embodiment 12:
Table 12,30% Acarus tritici urea pleocidin EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 12a, otherwise, water is added to obtains sample 12b in the oil phase.
Embodiment 13:
Table 13,40% Acarus tritici urea pleocidin EW prescription
Under high shear (5000-10000rpm), oil phase is added aqueous phase obtain sample 13a, otherwise, water is added to obtains sample 13b in the oil phase.
Every index of table 14, aqueous emulsion sample of the present invention
A. record by No. 2 rotor speeds 60 of ROOKFIELD DVII+Pro viscometer.
B. record by Ma Erwen laser particle size distribution instrument (mastersizer 2000).
By table 14 as can be seen, the aqueous emulsion that contains the Acarus tritici urea that makes according to the present invention, product cut size is less, and good stability.The preparation of aqueous emulsion of the present invention need not to use a large amount of hazardous solvents in the missible oil, thereby has avoided the adverse effect to environment and user's health.
Claims (9)
1, a kind of aqueous emulsion that contains the Acarus tritici urea is characterized in that: described aqueous emulsion is combined as solvent with wherein a kind of in reformation aromatic hydrocarbons, alkyl phthalate class, alkylene carbonate class, ionic liquid class, the N-alkyl pyrrolidine ketone or its.
2, the aqueous emulsion that contains the Acarus tritici urea according to claim 1, it is characterized in that: described aqueous emulsion is made up of according to following percentage by weight following material:
Active components A 1%-50%;
Active component B 0%-50%;
Solvent 5%-50%;
Emulsifier 1%-20%;
UV-protectant 0%-3%;
Antifreezing agent 0%-8%;
Thickener 0%-5%;
Mould inhibitor 0%-5%;
Defoamer 0%-0.5%;
Water: surplus;
Wherein, active components A is the Acarus tritici urea, and active component B is an Avermectin, or first dimension salt, or capillary, or pleocidin.
3, the aqueous emulsion that contains the Acarus tritici urea according to claim 2 is characterized in that: the better mass ratio of described solvent is 10%-30%.
4, according to each described aqueous emulsion that contains the Acarus tritici urea in the claim 1 to 3, it is characterized in that: described phthalate solvent is one or more in repefral, diethylester, dibutyl ester, the butyl benzyl ester; Described alkylene carbonate kind solvent is one or more of propylene carbonate base, butylene carbonate base; Cation in the described ionic liquid kind solvent is one or more in glyoxaline cation, pyridylium, alkyl ammonium cation, the alkyl phosphorus cation, and anion is Cl
-, Br
-, AlCl
4 -, [BF
4]
-, [PF
6]
-, [CF
3SO
3]
-, [(CF
3SO
3)
2N]
-In one or more; Described N-alkyl pyrrolidine ketones solvent is one or more of N-n-octyl pyrrolidones, N-dodecyl pyrrolidones; Described reformation aromatic hydrocarbon solvent is one or more among the Solvesso 100,150,200.
5, the aqueous emulsion that contains the Acarus tritici urea according to claim 2 is characterized in that: described emulsifier is one of in phosphoric acid ester anion surfactant and EO/PO block copolymer, polystyrene-based phenol polyethenoxy base ethers, castor oil polyoxyethylene ether class, polyoxyethylene nonylphenol ether class, the fatty alcohol polyethenoxy ether class nonionic surface active agent or its combination.
6, the aqueous emulsion that contains the Acarus tritici urea according to claim 2 is characterized in that: described UV-protectant is butylhydroxy anisole or 2, a kind of or its combination in the 6-Butylated Hydroxytoluene; Described antifreezing agent is a kind of or its combination in ethylene glycol, propane diols, glycerine, the urea; Described thickener is a kind of or its combination in xanthans, hydroxy alkyl cellulose class, polyvinylpyrrolidone, the polyvinyl alcohol; Described mould inhibitor is a kind of or its combination in Sodium Benzoate, formaldehyde, the sorbic acid; Described defoamer is a kind of or its combination in silicone based, the alcohols.
7, a kind of described preparation method who contains the aqueous emulsion of Acarus tritici urea of claim 2 for preparing is characterized in that may further comprise the steps: 1) former medicine A or former medicine A and former medicine B are dissolved in and obtain oil phase in the solvent; 2) emulsifier, UV-protectant, antifreezing agent, defoamer, thickener, the mould inhibitor of high HLB (＞10) mixed with water obtain water; 3) under high shear, oil phase is joined aqueous phase or water is joined in the oil phase, make the aqueous emulsion of high stability; Wherein, the 1st) step and the 2nd) order that goes on foot in no particular order, described former medicine A is the Acarus tritici urea.
8, the method for producing aqueous emulsion that contains the Acarus tritici urea according to claim 7 is characterized in that: according to the needs of aqueous emulsion configuration, the emulsifier that can add low HLB (5-7) in the step 1) makes oil phase.
9, according to claim 7 or the 8 described method for producing aqueous emulsion that contain the Acarus tritici urea, it is characterized in that: described former medicine B is A Wei, or first dimension salt, or capillary, or pleocidin.
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| CN101380004B (en) * | 2008-07-17 | 2011-10-19 | 张少武 | Synergistic insecticidal compositions containing spinosad and lufenuron |
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| 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 |
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