CN101690476B - Aqueous emulsion formulated by abamectin and indoxacarb and preparation method thereof - Google Patents
Aqueous emulsion formulated by abamectin and indoxacarb and preparation method thereof Download PDFInfo
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- CN101690476B CN101690476B CN200910040983.0A CN200910040983A CN101690476B CN 101690476 B CN101690476 B CN 101690476B CN 200910040983 A CN200910040983 A CN 200910040983A CN 101690476 B CN101690476 B CN 101690476B
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- aqueous emulsion
- indoxacarb
- surfactant
- avermectin
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- 239000000839 emulsion Substances 0.000 title claims abstract description 55
- 239000005660 Abamectin Substances 0.000 title claims abstract description 39
- 239000005907 Indoxacarb Substances 0.000 title claims abstract description 36
- VBCVPMMZEGZULK-NRFANRHFSA-N indoxacarb Chemical compound C([C@@]1(OC2)C(=O)OC)C3=CC(Cl)=CC=C3C1=NN2C(=O)N(C(=O)OC)C1=CC=C(OC(F)(F)F)C=C1 VBCVPMMZEGZULK-NRFANRHFSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.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 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 title abstract description 5
- 229950008167 abamectin Drugs 0.000 title abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound 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 34
- -1 butyl benzyl ester Chemical class 0.000 claims description 33
- 239000003814 drug Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- 239000002131 composite material Substances 0.000 claims description 15
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 11
- 239000013530 defoamer Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000004359 castor oil Substances 0.000 claims description 8
- 235000019438 castor oil Nutrition 0.000 claims description 8
- 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 8
- 239000002562 thickening agent Substances 0.000 claims description 8
- 239000003112 inhibitor Substances 0.000 claims description 7
- 229920001983 poloxamer Polymers 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002608 ionic liquid Substances 0.000 claims description 5
- 239000003002 pH adjusting agent Substances 0.000 claims description 5
- 150000002170 ethers Chemical class 0.000 claims description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 4
- NJPQAIBZIHNJDO-UHFFFAOYSA-N 1-dodecylpyrrolidin-2-one Chemical class CCCCCCCCCCCCN1CCCC1=O NJPQAIBZIHNJDO-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 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 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000003799 water insoluble solvent Substances 0.000 claims description 3
- ZZXUZKXVROWEIF-UHFFFAOYSA-N 1,2-butylene carbonate Chemical compound CCC1COC(=O)O1 ZZXUZKXVROWEIF-UHFFFAOYSA-N 0.000 claims description 2
- 229910016467 AlCl 4 Inorganic materials 0.000 claims description 2
- WPPOGHDFAVQKLN-UHFFFAOYSA-N N-Octyl-2-pyrrolidone Chemical class CCCCCCCCN1CCCC1=O WPPOGHDFAVQKLN-UHFFFAOYSA-N 0.000 claims description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- 150000003014 phosphoric acid esters Chemical group 0.000 claims description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 2
- FFZANLXOAFSSGC-UHFFFAOYSA-N phosphide(1-) Chemical compound [P-] FFZANLXOAFSSGC-UHFFFAOYSA-N 0.000 claims 1
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
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- 239000012071 phase Substances 0.000 description 65
- 239000003921 oil Substances 0.000 description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 22
- 239000002245 particle Substances 0.000 description 19
- 238000012360 testing method Methods 0.000 description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 10
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- 239000004322 Butylated hydroxytoluene Substances 0.000 description 9
- 230000006641 stabilisation Effects 0.000 description 9
- 238000011105 stabilization Methods 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 230000008859 change Effects 0.000 description 8
- 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 7
- 241000238631 Hexapoda Species 0.000 description 7
- 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 description 7
- 239000012046 mixed solvent Substances 0.000 description 7
- 239000004698 Polyethylene Substances 0.000 description 6
- RWRDLPDLKQPQOW-UHFFFAOYSA-N tetrahydropyrrole Natural products C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000002518 antifoaming agent Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 235000021317 phosphate Nutrition 0.000 description 5
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical group [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 5
- 239000004299 sodium benzoate Substances 0.000 description 5
- 235000010234 sodium benzoate Nutrition 0.000 description 5
- 229920001285 xanthan gum Polymers 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 4
- 230000000857 drug effect Effects 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- 235000011187 glycerol Nutrition 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 4
- 108010010803 Gelatin Proteins 0.000 description 3
- 241000500437 Plutella xylostella Species 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 3
- 241000607479 Yersinia pestis Species 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
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- 230000007613 environmental effect Effects 0.000 description 3
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 3
- 229920000159 gelatin Polymers 0.000 description 3
- 239000008273 gelatin Substances 0.000 description 3
- 235000019322 gelatine Nutrition 0.000 description 3
- 235000011852 gelatine desserts Nutrition 0.000 description 3
- 231100001261 hazardous Toxicity 0.000 description 3
- 239000002917 insecticide Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- ZIYVHBGGAOATLY-UHFFFAOYSA-N methylmalonic acid Chemical compound OC(=O)C(C)C(O)=O ZIYVHBGGAOATLY-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 3
- 239000004334 sorbic acid Substances 0.000 description 3
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- BOLQUPOXTWHXIX-UHFFFAOYSA-N OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 Chemical compound OC1=CC=CC=C1.C=1C=CC=CC=1C=C(C=1C=CC=CC=1)C1=CC=CC=C1 BOLQUPOXTWHXIX-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229920001400 block copolymer Polymers 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 229940095259 butylated hydroxytoluene Drugs 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
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- 239000004495 emulsifiable concentrate Substances 0.000 description 2
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- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
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- BTCSSZJGUNDROE-UHFFFAOYSA-N gamma-aminobutyric acid Chemical compound NCCCC(O)=O BTCSSZJGUNDROE-UHFFFAOYSA-N 0.000 description 2
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- 239000000575 pesticide Substances 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
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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Abstract
The invention provides an aqueous emulsion formulated by abamectin and indoxacarb, comprising the following components by mass percent: 0.1-20% of abamectin, 0.3-15% of indoxacarb, 5-50% of solvent which is insoluble in water, 0.1-20% of surface active agent and a proper amount of water. Compared with the prior art, the aqueous emulsion formulated by abamectin and indoxacarb of the invention uses relatively green and environment protective solvent, and reaches a certain stability under the coordination of corresponding surface active agent and other auxiliary agent; the pesticide effect thereof is similar with the traditional missible oil when the aqueous emulsion is used in the same dilution factor; and meanwhile a large amount of harmful solvent used in aqueous emulsion is avoided, thus avoiding the adverse effects of the harmful solvent on the environment and the health of users. The invention also relates to a preparation method of the aqueous emulsion.
Description
Technical field
The present invention relates to a kind of pesticidal preparations and preparation method thereof, especially a kind of composite aqueous emulsion and preparation method thereof.
Background technology
Aqueous emulsion is a kind of environmental protection type agricultural chemical formulation of recent domestic development, because solvent for use in preparation is than traditional missible oil much less, little to environmental hazard, to user's safety, is therefore to replace a kind of in the Water-borne modification formulation of missible oil.
Indoxacarb (Indoxacarb) is E.I.Du Pont Company's a kind of oxadiazines insecticides newly developed, have and tag and stomach poison function, all effective to each instar larvae, and with other insecticides such as organic phosphates, chrysanthemum ester classes without cross resistance, its mechanism of action is, by the sodium-ion channel in blocking-up insect nerve cell, to make nerve cell loss of function.Indoxacarb is lower to mammal, domestic animal toxicity, simultaneously very safe to the useful insects such as non-target biology in environment, be mainly used in preventing and treating the gardening pest insect on the crops such as vegetables, fruit tree, grain, cotton, especially for lepidoptera pest, have comparatively ideal control efficiency.Avermectin (Abamectin) is a kind of wide spectrum, efficient, safe macrolides antibiotics compound, has strong desinsection, kills mite, eelworm-killing activity.Avermectin has stomach toxicity and action of contace poison, without systemic action, can not ovicidal, its mechanism of action is for movable by interference insect neurophysiology, stimulate and discharge γ-aminobutyric acid, make insect central nervous system signal constantly be that motor neuron accepts, thus in several hours paralysis, food refusal, slow-action or motionlessly cause death rapidly, be widely used in the insects such as crop diamond-back moth, cabbage caterpillar such as control vegetables, fruit tree.But the long-term use of single medicament often causes the raising of pest resistance to insecticide, increase the difficulty of control, affect 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.Avermectin and indoxacarb complex preparation have synergistic effect, are mainly used in preventing and treating paddy rice rice leaf roll snout moth's larva, the insects such as Cruciferae diamond-back moth.
Pesticide original medicine is made an 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 with can compare by wet-milling, aqueous emulsion without dust, endangers little to producer, user in manufacturing, using.But aqueous emulsion solvent for use must be water insoluble, and Avermectin and indoxacarb are difficult to be dissolved in general organic solvent, therefore, make aqueous emulsion and have certain difficulty.
Not yet relevant for the more stable aqueous emulsion of Avermectin and indoxacarb, occur at present, in view of this, we provide a kind of Avermectin and the composite aqueous emulsion of indoxacarb and preparation method thereof at this.
Summary of the invention
The object of the invention is to: composite aqueous emulsion of a kind of high stability Avermectin and indoxacarb and preparation method thereof is provided.
Research and development Avermectin and the composite water emulsion formula of indoxacarb, its key problem is the selection of solvent and surfactant, inventor is researching and developing on the basis of experience in the past, through large quantity research and experiment sieving, determines that the formula of aqueous emulsion is as follows: Avermectin 0.1%-20%; Indoxacarb 0.3%-15%; Solvent 5%-50%; Surfactant 0.1%-20%; UV-protectant 0.2%-2%; Antifreezing agent 4%-12%; Thickener 0.01%-3%; Mould inhibitor 0.01%-3%; Defoamer 0.2%-0.5%; PH adjusting agent 0%-2%; Water: surplus; The percentage of above-mentioned substance is mass percent.
As a kind of improvement of Avermectin of the present invention and the composite aqueous emulsion of indoxacarb, described Avermectin and indoxacarb composite than with 0.5%-15%: 0.5%-10% for good, 1.5%-3%: 1%-2% is best.
Described solvent is all water-immiscible solvent, as being wherein a kind of or its combination in alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone, high boiling point aromatic hydrocarbons.
Described surfactant can be for phosphoric acid ester, alkylated aromatic sulfonic acid salt and the nonionic surface active agent of anion be as wherein a kind of or its combination of Pluronic PE 6800, triphenyl vinyl phenol polyoxyethylene groups ethers, castor oil polyoxyethylene ether class, polyoxyethylene nonylphenol ether class.
Described UV-protectant is butylhydroxy anisole (BHA), 2,6-Butylated Hydroxytoluene (BHT).
Described antifreezing agent is one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol, ethylene glycol monoalkyl ether (as butyl), urea.
Described thickener is one or more in xanthans, gelatin, starch, methylol (ethyl, propyl group) cellulose, polyvinylpyrrolidone, polyvinyl alcohol.
Described mould inhibitor is Sodium Benzoate, formaldehyde, BIT class, sorbic acid, the bromo-2-of 2-nitro-propyl group-1, one or more in 3-glycol.
Described defoamer is silicone based.
Described pH adjusting agent is organic and inorganic acid alkali.
For solving the problems of the technologies described above, the present invention also provides the preparation method of a kind of Avermectin and the composite aqueous emulsion of indoxacarb, it is characterized in that comprising the following steps: 1) Avermectin and the former medicine of indoxacarb are dissolved in water-insoluble solvent in, and add the surfactant of UV-protectant and/or low HLB (5-7) to obtain disperse phase; 2) surfactant, antifreeze, defoamer, thickener, mould inhibitor and the water of high HLB (> 10) are mixed to get to continuous phase; 3) under high shear, disperse phase is joined in continuous phase or by continuous phase and joined in disperse phase, make the aqueous emulsion of high stability; Wherein, the 1st) step and the 2nd) order of step can be adjusted.
Compared with prior art, the aqueous emulsion that Avermectin of the present invention and indoxacarb are composite, selects the solvent of relative environmental protection, and under the cooperation of corresponding surfactant and other auxiliary agent, has reached certain stability.While using under identical extension rate, its drug effect and traditional missible oil are similar, have avoided a large amount of hazardous solvents of using in missible oil simultaneously, have avoided the adverse effect of hazardous solvent to environment and user's health.
Embodiment
Aqueous emulsion is oil phase and the aqueous mixture utilizing in machine power shearing system, and oil phase is dispersed in water with minimum drop, and the surfactant in liquid phase and various auxiliary agent make emulsion keep stable.While preparing aqueous emulsion, include after continuous phase (water) homogeneous phase of surfactant and various auxiliary agents, under high speed shear (4000-10000 rev/min), join in disperse phase (oil phase), can make particle diameter at the product of 0.3-10 micron, or disperse phase is added in continuous phase under the condition of high shear (5000-10000 rev/min), also can makes the product of same quality.
Because Avermectin and the former medicine of indoxacarb are difficult to be dissolved in general organic solvent, therefore first need to select suitable organic solvent to be prepared into oil phase.Through the trial of lot of experiments and screening, find, the mixture of alkyl phthalate class, alkylene carbonate class, ionic liquid class, N-alkyl pyrrolidine ketone and they and high boiling point aromatic hydrocarbons etc. are applicable.
The concrete preparation method of aqueous emulsion of the present invention mainly comprises three steps: first, by Avermectin and the former medicine of indoxacarb be dissolved in water-insoluble above-mentioned solvent in, and add the surfactant of UV-protectant and/or low HLB (HLB is 5-7) to obtain dispersed phase; Then, the surfactant of high HLB (HLB > 10), antifreezing agent, defoamer, thickener, mould inhibitor etc. are mixed to get to even continuous phase with water; Finally, under high shear, disperse phase is slowly joined in continuous phase or by continuous phase and joined in disperse phase, can make particle diameter at the stable aqueous emulsion of 0.2-10 micron.
Above-mentioned phthalate solvent can be repefral, diethylester, dibutyl ester, butyl benzyl ester etc.; Alkylene carbonate kind solvent can be propylene carbonate base, butylene carbonate base etc.; In ionic liquid kind solvent, conventional cation has glyoxaline cation, pyridylium, alkyl ammonium cation, alkyl phosphorus cation etc., and conventional anion 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.; High boiling point aromatic hydrocarbon solvent is as Solvesso 100,150,200 etc.The content of solvent in aqueous emulsion is 5%-50% mass ratio, preferably 20%-50% mass ratio (depending on the solvability of former medicine and different).
Described surfactant can be anionic, nonionic, or its mixture.Applicable anion surfactant has triphenyl vinyl phenol polyoxyethylene ether phosphate, the phosphate of Pluronic PE 6800 etc., applicable non-ionic surface active agent has fatty alcohol Pluronic PE 6800 (HLB 7-16), oleyl alcohol and (or) hexadecanol APEO (5-5.5EO), sorbitol anhydride monolaurate, monopalmitate, single stearyl ester, monoleate etc., 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.Between anion and nonionic mixing or the moon/nonionic, mixing use or the moon/nonionic are used separately, and usage amount is 0.1%-20% mass ratio, and preferably 0.5%-15% mass ratio, is preferably 2%-8% mass ratio.
Because Avermectin is more responsive to light, in preparation, also need to add UV-protectant, be suitable for and have antioxidant butylhydroxy anisole (BHA), 2,6-Butylated Hydroxytoluene (BHT) etc.The content of UV-protectant in aqueous emulsion is 0.2%-2% mass ratio.
The antifreezing agent that is applicable to low-temperature stabilization has ethylene glycol, propane diols, glycerine, polyethylene glycol, ethylene glycol monoalkyl ether (as butyl), and urea is also applicable, and the usage amount of antifreezing agent is between 4%-12% mass ratio.
Thickener can be selected xanthans, gelatin, starch, methylol (ethyl, propyl group) cellulose, polyvinylpyrrolidone, polyvinyl alcohol etc., and viscosity is preferably between 100-2000cP, makes the free-flow of material energy.The consumption of thickener is 0.01%-3% mass ratio.
Mould inhibitor can be selected Sodium Benzoate, formaldehyde, BIT class, sorbic acid, the bromo-2-of 2-nitro-propyl group-1,3-glycol etc., and consumption is 0.01%-3% mass ratio.
Defoamer is silicone based, and as poly-alkyl silicon oxirane, usage amount is between 0.2%-0.5%.
Described pH adjusting agent is organic and inorganic acid alkali.
In order to make object of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only for explaining the present invention, can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any modifications of making within the spirit and principles in the present invention, be equal to replacement and improvement etc., within all should being included in 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:
By 0.5 gram of 92% Avermectin, 15 grams of 95% indoxacarbs are dissolved in 22 grams of mixed solvents that contain NOP and Solvesso 150, after solution is transparent, add 1 gram of BHT, 2 grams of loose phases of poly-(12-hydroxy stearic acid) polyoxyethylene ether block copolymers emulsified component, under high shear (5000-10000rpm), slowly join and contain 3 grams of triphen ethyl phenol APEOs (agriculture breast 600#), 0.3 gram of silicone based defoamer, 4 grams of ethylene glycol, 0.1 gram of Sodium Benzoate, in the continuous phase (water) of 0.25 gram of xanthans and 51.85 water, add rear continuation and shear a few minutes.Gained aqueous emulsion viscosity is 200cP (No. 2 rotor speeds 60 of ROOKFIELD DV-+Proviscometer record, and following examples are same), and particle diameter is 0.3-5 micron (Ma Erwen laser fineness gage records, and following examples are same).
Change feed way, above-mentioned 59.5 grams of continuous phases (water), under high shear (5000-10000rpm), are added in 40.5 grams of disperse phase, make the aqueous emulsion of equal in quality.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 2:
By 2.0 grams of 92% Avermectin, 95% 13 grams of indoxacarbs are dissolved in 25 grams of mixed solvents containing diethyl phthalate and Solvsso 200, until former medicine be dissolved into completely transparent after, add therein 1 gram of BHA, 1.5 grams of poly-isosuccinic acid acid anhydride-ethylene glycol copolymers of non-ionic surface active agent are emulsified into and disperse phase (oil phase), under high shear (5000-10000rpm), be added to and contain 4 grams of Nonyl pheno base ether (OP-20, HLB=16), 0.3 gram of silicone based defoamer, 4 grams of propane diols, 0.1 gram of formaldehyde, in the continuous phase of 0.25 gram of gelatin and 48.85 grams of water compositions, oil phase adds rear continuation and shears a few minutes, make aqueous emulsion, its viscosity is 185cP, particle diameter is 0.25-4 micron.
Change feed way, 57.5 grams of above-mentioned continuous phases, under high shear (5000-10000rpm), are added in 42.5 grams of disperse phase, shear a few minutes to make aqueous emulsion after adding again, its viscosity is 190cP, and particle diameter is 0.28-4.2 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 3:
11 grams of 5.0 grams of 92% Avermectin, 95% indoxacarb are dissolved in and contain JEFFSOL AG 1723 (alkylene carbonate class, by Huntsman company, produced) and 25.5 grams of mixed solvents of Solvesso200 in, in < 60 degree celsius temperature end heating, former medicine is dissolved into after transparence completely, adds therein 1 gram of BHT, 2.5 grams of non-ionic surface active agent castor oil polyoxyethylene ethers (By-125) to be emulsified into and disperse phase (oil phase).Under high shear (5000-10000rpm), disperse phase is added to and contains 3.5 grams of anion surfactant triphenylethylene phenol polyethenoxy ether phosphates and (with triethanolamine, neutralize, the production of Soprophor FLYou Rhdia company), in the continuous phase (water) of 0.3 gram of silicone based defoamer, 4 grams of polyethylene glycol, 0.1 gram of sorbic acid, 0.25 gram of polyvinyl alcohol, 1 gram of phosphoric acid and 45.85 grams of water compositions, oil phase adds rear continuation high shear a few minutes, and making viscosity is that 175cP, particle diameter are the aqueous emulsion of 0.3-4.6 micron.
Change feed way, 55 grams of above-mentioned waters, under high shear (5000-10000rpm), are added in 45 grams of disperse phase, add rear continuation and shear a few minutes, make aqueous emulsion, its viscosity is 183cP, and particle diameter is 0.32-5.4 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 4:
10 grams of 8.0 grams of 92% Avermectin, 95% indoxacarb are dissolved in 26.5 grams of mixed solvents that contain dodecyl pyrrolidones and Solvesso150, in < 60 degree celsius temperature end heating, make former medicine be dissolved into after transparence completely, add therein 1 gram of BHT, make it be dissolved into dispersion phase completely.Under high shear (5000-10000rpm), disperse phase is added to the non-ionic surface active agent that contains 2.5 grams of fatty alcohol Pluronic PE 6800s and mix with 1.5 grams of castor oil polyoxyethylene ethers (By-130), 0.2 gram of silicone defoaming agent, 4 grams of glycerine, the 0.1 gram of bromo-2-of 2-nitro-propyl group-1, in the continuous phase of 3-glycol, 0.25 gram of polyvinylpyrrolidone, 1.5 grams of phosphoric acid and 44.45 grams of water compositions, add rear continuation and shear a few minutes, make aqueous emulsion.Sample viscosity is 192cP after tested, and particle diameter is at 0.25-3.7 micron.
Change feed way, 54.5 grams of above-mentioned continuous phases are added in 45.5 grams of disperse phase under high shear (5000-10000rpm), continue to shear a few minutes to make aqueous emulsion after adding again, sample after testing viscosity is 190cP, and particle diameter is 0.3-3.9 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 5:
9 grams of 10 grams of 92% Avermectin, 95% indoxacarb are dissolved in to 25 grams of [C
4mim] [PF
6] in (methyl butyl imidazoles hexafluorophosphate), in < 60 degree celsius temperature ends heating, former medicine is dissolved into after transparence completely, add therein 1 gram of BHA, make it be dissolved into dispersion phase completely.Under high shear (5000-10000rpm), disperse phase is added in the continuous phase of the mixture that contains 2 grams of fatty alcohol Pluronic PE 6800s and 1.5 grams of castor oil polyoxyethylene ethers, 0.3 gram of silicone defoaming agent, 4 grams of ethylene glycol, 0.1 gram of Sodium Benzoate, 0.25 gram of xanthans, 1 gram of glacial acetic acid and 45.85 grams of water compositions, add rear continuation and shear a few minutes, make aqueous emulsion.Sample viscosity is 196cP after tested, and particle diameter is at 0.22-3.5 micron.
Change feed way, 55 grams of above-mentioned continuous phases are added in 45 grams of disperse phase under high shear (5000-10000rpm), after adding, continue shearing a few minutes makes corresponding aqueous emulsion again, and its sample after testing viscosity is 182cP, and particle diameter is 0.25-3.3 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 6:
By in 12 grams of 92% Avermectin, 7.0 grams of 25.4 grams of mixed solvents that are dissolved in containing diethyl phthalate and Solvsso 200 of 95% indoxacarb, until former medicine be dissolved into completely transparent after, add therein 1 gram of BHT, the poly-isosuccinic acid acid anhydride-ethylene glycol copolymers of 1.5 grams of non-ionic surface active agents to be emulsified into and to disperse phase (oil phase).Under high shear (5000-10000rpm), disperse phase is added in the continuous phase that contains 3 grams of dodecanol APEOs, 0.3 gram of silicone defoaming agent, 4 grams of ethylene glycol, 0.2 gram of BIT, 0.25 gram of starch, 1 gram of phosphoric acid and 44.35 grams of water compositions, oil phase adds rear continuation and shears a few minutes, make aqueous emulsion, its viscosity is 190cP, and particle diameter is 0.20-4.5 micron.
Change feed way, 53.1 grams of above-mentioned continuous phases are added in 46.9 grams of disperse phase under high shear (5000-10000rpm), shear a few minutes to make aqueous emulsion after adding again, its viscosity is 210cP, and particle diameter is 0.24-5.0 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 7:
3.0 grams of 15 grams of 92% Avermectin, 95% indoxacarb are dissolved in and contain JEFFSOL AG 1723 (alkylene carbonate class, by Huntsman company, produced) and 24.5 grams of mixed solvents of Solvesso200 in, temperature end heating 60 degrees Celsius of <, former medicine is dissolved into after transparence completely, adds therein 1 gram of BHA, 2.5 grams of non-ionic surface active agent castor oil polyoxyethylene ethers to be emulsified into and to disperse phase (oil phase).Under high shear (5000-10000rpm), disperse phase is added to and contains 3.5 grams of anion surfactant triphenylethylene phenol polyethenoxy ether phosphates and (with triethanolamine, neutralize, the production of Soprophor FLYou Rhdia company), in the continuous phase (water) of 0.3 gram of silicone defoaming agent, 4 grams of propane diols, 0.1 gram of formaldehyde, 0.25 gram of xanthans, 1.4 grams of phosphoric acid and 44.45 grams of water compositions, oil phase adds rear continuation high shear a few minutes, make aqueous emulsion, its viscosity is 185cP, and particle diameter is 0.37-4.8 micron.
Change feed way, 54 grams of above-mentioned waters are added in 46 grams of disperse phase under high shear (5000-10000rpm), add rear continuation and shear a few minutes, make aqueous emulsion, its sample viscosity is 203cP, and particle diameter is 0.35-5.5 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
Embodiment 8:
0.5 gram of 20 grams of 92% Avermectin, 95% indoxacarb is dissolved in to 25 grams of [C
4mim] [(CF
3sO
3)
2n] in the mixed solvent of (methyl butyl imidazoles trifluoromethane sulfonic acid amine salt) and Solvesso150, in < 60 degree celsius temperature end heating, former medicine is dissolved into after transparence completely, adds therein 1 gram of BHT, make it be dissolved into dispersion phase completely.Under high shear (5000-10000rpm), disperse phase is added in the continuous phase of 3 grams of fatty alcohol Pluronic PE 6800s and 2 grams of castor oil polyoxyethylene ether mixtures, 0.3 gram of silicone defoaming agent, 4 grams of glycerine, 0.1 gram of Sodium Benzoate, 0.25 gram of polyvinyl alcohol, 1 gram of glacial acetic acid and 42.85 grams of water compositions, add rear continuation and shear a few minutes, make aqueous emulsion, its viscosity is 206cP, and particle diameter is at 0.21-4.5 micron.
Change feed way, 53.5 grams of above-mentioned continuous phases are added in 46.5 grams of disperse phase under high shear (5000-10000rpm), after adding, continue again to shear a few minutes, make aqueous emulsion, its sample after testing viscosity is 192cP, and particle diameter is 0.20-3.8 micron.
Two groups of samples are deposited 7 days at 0 degree Celsius, deposit laggard line stabilization test in 14 days, without phenomenons such as layering, bleed, oil slick, occur for 54 degrees Celsius.
The aqueous emulsion making with embodiment 2 is by active ingredient 2.5g/ mu control diamond-back moth, and after medicine, the preventive effect of 3 days is 93.2%, and the preventive effect of the emulsifiable concentrate formulation of same amount under same medicine amount is 89.4%, and both differences are not remarkable.
The aqueous emulsion making with embodiment 6 is by active ingredient 2g/ mu control rice leaf roller, and after medicine, the preventive effect of 3 days is 95.8%, and the preventive effect of the emulsifiable concentrate formulation of same amount under same medicine amount is 96.1%, is more or less the same between the two.
The aqueous emulsion known by above embodiment, the Avermectin making according to the present invention and indoxacarb are composite, product cut size is substantially in 0.2-10 micron, and good stability.When aqueous emulsion of the present invention is used under identical extension rate, drug effect and traditional missible oil are similar, but without a large amount of hazardous solvents that use in missible oil, thereby have avoided the adverse effect to environment and user's health.
Claims (4)
1. an Avermectin and the composite aqueous emulsion of indoxacarb, it is characterized in that: described aqueous emulsion comprise Avermectin 0.1%-20%, indoxacarb 0.3%-15%, with water-insoluble solvent 20%-50%, surfactant 0.1%-20%, UV-protectant 0.2%-2%, antifreezing agent 4%-12%, thickener 0.01%-3%, mould inhibitor 0.01%-3%, defoamer 0.2%-0.5%, pH adjusting agent 0%-2% and excess water, be more than mass percent;
Described solvent is one or more of repefral, diethylester, dibutyl ester, butyl benzyl ester, propylene carbonate base, butylene carbonate base, ionic liquid kind solvent, N-n-octyl pyrrolidones, N-dodecyl pyrrolidones;
Cation in described ionic liquid kind solvent is one or more in glyoxaline cation, pyridylium, alkyl ammonium cation, 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 surfactant is phosphoric acid ester, alkylated aromatic sulfonic acid salt surfactant or nonionic surface active agent or its mixture of anionic;
Described nonionic surface active agent is wherein a kind of or its combination of Pluronic PE 6800, triphenyl vinyl phenol polyoxyethylene groups ethers, castor oil polyoxyethylene ether class, polyoxyethylene nonylphenol ether class.
2. the composite aqueous emulsion of Avermectin according to claim 1 and indoxacarb, is characterized in that: the composite ratio of described Avermectin and indoxacarb is 0.5%-15%: 0.5%-10% mass ratio.
3. the composite aqueous emulsion of Avermectin according to claim 1 and indoxacarb, is characterized in that: the mass ratio of described surfactant is 0.5%-15%.
4. the preparation method of a kind of Avermectin claimed in claim 1 and the composite aqueous emulsion of indoxacarb, it is characterized in that comprising the following steps: 1) Avermectin and the former medicine of indoxacarb are dissolved in water-insoluble solvent in, and adding the surfactant of UV-protectant and/or low HLB to obtain disperse phase, the surfactant of described low HLB refers to that HLB is the surfactant of 5-7; 2) surfactant of high HLB, antifreezing agent, defoamer, thickener, mould inhibitor and water are mixed to get to continuous phase, the surfactant of described high HLB refers to that HLB is the surfactant of > 10; 3) under high shear, disperse phase is joined in continuous phase or by continuous phase and joined in disperse phase, and neutralize by pH adjusting agent, make the aqueous emulsion of high stability; Wherein, the 1st) step and the 2nd) order of step in no particular order.
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| CN101263823A (en) * | 2008-05-07 | 2008-09-17 | 国家农药创制工程技术研究中心 | Indoxacarb and emamectin benzoate-chlorfenapyr pesticidal composition |
| CN101385457A (en) * | 2008-10-17 | 2009-03-18 | 广西田园生化股份有限公司 | Insecticidal composition containing avermectin and indoxacarb |
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| CN101385457A (en) * | 2008-10-17 | 2009-03-18 | 广西田园生化股份有限公司 | Insecticidal composition containing avermectin and indoxacarb |
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