CN101622987A - Emamectin benzoate microcapsule suspending agent and preparation method thereof - Google Patents
Emamectin benzoate microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN101622987A CN101622987A CN200810107286A CN200810107286A CN101622987A CN 101622987 A CN101622987 A CN 101622987A CN 200810107286 A CN200810107286 A CN 200810107286A CN 200810107286 A CN200810107286 A CN 200810107286A CN 101622987 A CN101622987 A CN 101622987A
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- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin 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](NC)[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 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000003094 microcapsule Substances 0.000 title claims abstract description 39
- 239000000375 suspending agent Substances 0.000 title claims abstract description 38
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 150000001412 amines Chemical class 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000003921 oil Substances 0.000 claims description 24
- 239000012071 phase Substances 0.000 claims description 17
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical class O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 16
- 239000012948 isocyanate Substances 0.000 claims description 16
- 150000002513 isocyanates Chemical class 0.000 claims description 16
- 229920000084 Gum arabic Polymers 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 241000978776 Senegalia senegal Species 0.000 claims description 14
- 239000000205 acacia gum Substances 0.000 claims description 14
- 235000010489 acacia gum Nutrition 0.000 claims description 14
- 239000006185 dispersion Substances 0.000 claims description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 7
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical class NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002480 mineral oil Substances 0.000 claims description 6
- 235000010446 mineral oil Nutrition 0.000 claims description 6
- 239000003755 preservative agent Substances 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 239000002562 thickening agent Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 2
- KIHBGTRZFAVZRV-UHFFFAOYSA-N 2-hydroxyoctadecanoic acid Chemical class CCCCCCCCCCCCCCCCC(O)C(O)=O KIHBGTRZFAVZRV-UHFFFAOYSA-N 0.000 claims description 2
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000008346 aqueous phase Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 229960001124 trientine Drugs 0.000 claims description 2
- 239000000575 pesticide Substances 0.000 abstract description 6
- 241000607479 Yersinia pestis Species 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 2
- 206010059866 Drug resistance Diseases 0.000 abstract 1
- KQWGXHWJMSMDJJ-UHFFFAOYSA-N cyclohexyl isocyanate Chemical compound O=C=NC1CCCCC1 KQWGXHWJMSMDJJ-UHFFFAOYSA-N 0.000 abstract 1
- JXCHMDATRWUOAP-UHFFFAOYSA-N diisocyanatomethylbenzene Chemical compound O=C=NC(N=C=O)C1=CC=CC=C1 JXCHMDATRWUOAP-UHFFFAOYSA-N 0.000 abstract 1
- 230000005923 long-lasting effect Effects 0.000 abstract 1
- 238000001782 photodegradation Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 12
- LLEMOWNGBBNAJR-UHFFFAOYSA-N biphenyl-2-ol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1 LLEMOWNGBBNAJR-UHFFFAOYSA-N 0.000 description 8
- 229960002836 biphenylol Drugs 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000004530 micro-emulsion Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000003814 drug Substances 0.000 description 6
- 238000009472 formulation Methods 0.000 description 5
- 238000006303 photolysis reaction Methods 0.000 description 5
- 230000003449 preventive effect Effects 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 241000238631 Hexapoda Species 0.000 description 3
- QFMDFTQOJHFVNR-UHFFFAOYSA-N 1-[2,2-dichloro-1-(4-ethylphenyl)ethyl]-4-ethylbenzene Chemical compound C1=CC(CC)=CC=C1C(C(Cl)Cl)C1=CC=C(CC)C=C1 QFMDFTQOJHFVNR-UHFFFAOYSA-N 0.000 description 2
- 241000256247 Spodoptera exigua Species 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 229920001983 poloxamer Polymers 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- LQIAZOCLNBBZQK-UHFFFAOYSA-N 1-(1,2-Diphosphanylethyl)pyrrolidin-2-one Chemical compound PCC(P)N1CCCC1=O LQIAZOCLNBBZQK-UHFFFAOYSA-N 0.000 description 1
- OVSKIKFHRZPJSS-UHFFFAOYSA-N 2,4-D Chemical compound OC(=O)COC1=CC=C(Cl)C=C1Cl OVSKIKFHRZPJSS-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 239000005660 Abamectin Substances 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 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 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- JCTHGPXQXLMSDK-UHFFFAOYSA-N bis(Benzyloxy)methane Chemical compound C=1C=CC=CC=1COCOCC1=CC=CC=C1 JCTHGPXQXLMSDK-UHFFFAOYSA-N 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- -1 styryl phenol Chemical compound 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000004562 water dispersible granule Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses an emamectin benzoate microcapsule suspending agent and a preparation method thereof, and relates to a pesticide and a preparation method thereof. A microencapsulated product prepared by the reaction of a mixture of toluylene diisocyanate and cyclohexyl isocyanate with amine can reduce the photodegradation rate of an effective component of emamectin benzoate in the process of storage and use, improves the stability of the effective component in the microcapsule suspending agent, further improves the utilization rate of the effective component, slows down the increasing speed of drug resistance of pests, improves the effect of controlling and preventing the pests, and has quick and long-lasting effect.
Description
Technical field
The present invention relates to a kind of agricultural chemical insecticide and preparation method thereof, relate in particular to a kind of emamectin benzoate microcapsule suspension formulation and preparation method thereof.
Background technology
Emamectin-benzoate (emamectin benzoate) is the modified outcome of farm antibiotics Avermectin B1, it has super-high-efficient, low toxicity (preparation is closely nontoxic), noresidue, advantage such as nuisanceless, insecticidal activity has improved 1-3 the order of magnitude than Avermectin, the double again action of contace poison of existing stomach poison function, active high to the larva of lepidopterous insects and other many insects and mite class, proved under low-down dosage (0.084-2g/ha) also have good effect, produced at present and go up main and the composite missible oil of making of other active ingredients, microemulsion, aqueous emulsion, formulations such as water dispersible granules.
In recent years, the microencapsulation of agricultural chemicals is long because of stability, longevity of residure that it increases active ingredient, reduce contact toxicity, peculiar smell alleviates, reduces the hazardous solvent consumption and reduction to the advantage of the aspects such as pollution of environment, be subjected to the extensive concern in pesticidal preparations field.Because photodissociation easily takes place emamectin-benzoate, especially water and some solvent can obviously quicken its photodissociation, greatly reduce its drug effect, make the microencapsulation formulation and can weaken its photodissociation characteristic, relatively have certain advantage with other formulations.
Summary of the invention
The purpose of this invention is to provide a kind of emamectin benzoate microcapsule suspending agent and preparation method thereof, the mixture of cresylene isocyanates and hexamethylene isocyanates and amine reacted obtain the microencapsulation product, can reduce the light degradation rate of effective ingredient emamectin-benzoate in storage and use, improve the stability of effective ingredient in microcapsule suspending agent, further improve utilization rate of active components, slow down resistance development.
Purpose of the present invention can realize by the following technical solutions:
A kind of emamectin benzoate microcapsule suspending agent is characterized in that: it is raw material that the oil phase of said preparation adopts the material of following weight content:
Emamectin-benzoate 0.1-20%;
The mixture 1-12% of cresylene isocyanates and hexamethylene isocyanates, preferred 2-10%;
Aliphatic hydrocarbon 10-90%, preferred 30-70%;
Oil-soluble polymeric dispersant 1-15%, preferred 3-10%;
Amine 0.1-5%, preferred 0.5-2%;
The water of said preparation is made up of water basically, the weight content of water is 15-50%, can also comprise the mixture of polyvinyl alcohol and gum Arabic in addition, and the weight content of polyvinyl alcohol and gum Arabic is respectively 0.1-3%, preferred 0.1-1%, 0.01-8%, preferred 0.05-5%;
Said preparation also can comprise the auxiliary agent of following weight content:
Emulsifier 1-8%, preferred 2-5%;
Dispersant 1-8%, preferred 2-5%;
Preservative 0.05-0.5%, preferred 0.1-0.3%;
Thickener 0.01-0.2%, preferred 0.05-0.15%.
The weight ratio of the mixture of described cresylene isocyanates and hexamethylene isocyanates is: the cresylene isocyanates: the hexamethylene isocyanates is 1: 0.3-2, preferred 1: 0.5-1.5.
Can not contain emulsifier in the described auxiliary agent.
Described aliphatic hydrocarbon comprises one or both mixtures in paraffin oil, the mineral oil.
Described oil-soluble polymeric dispersant comprises for example Agrimer AL10LC (production of ISP company), phosphoric acid ester Hordaphos 215 (production of Clariant company), polymerization hydroxy stearic acid class one or both mixtures among the Atlox LP (production of Uniqema company) for example for example of alkyl nvp copolymer class.
Described amine comprises ethylidene-1, one or both mixtures in 2-diamines, diethylenetriamines, the trien.
Described emulsifier comprises for example one or both mixtures among Atlox 4912 (production of Uniqema company), Ethylan NS-500LQ (Akzo Nobel N.V.'s production), the Pluronic PE (BASF AG's production) of non-ionic block copolymer.
Described dispersant comprises for example Baykanol SL (Bayer AG's production), polycarboxylic acid salt Tersperse 2700 (production of Huntsman company), naphthalenesulfonate Tamol NN (BASF AG's production), styryl phenol b-oxide class one or both mixtures among the Soprophor 4D 384 (Rhodia's production) for example for example for example of phenol formaldehyde (PF) condensation product class.
Described preservative comprises one or both mixtures among Preventol D2, the Preventol D7 (Bayer AG's production).
Described thickener comprises for example one or both mixtures among Kelcan S, the Manugel XG (production of ISP company) of xanthans class.
The preparation method of above-mentioned emamectin benzoate microcapsule suspending agent is characterized in that, this method comprises following processing step:
(1) preparation oil phase
At ambient temperature, behind emamectin-benzoate, aliphatic hydrocarbon, oil-soluble polymeric dispersant mixed grinding, add cresylene isocyanates and hexamethylene isocyanates while stir, make oil phase, this moment, reaction temperature raise, and the temperature that needs to raise is controlled at 20-50 ℃;
(2) preparation water
Polyvinyl alcohol and gum Arabic added make water in the entry, heating makes polyvinyl alcohol and the faster dissolving of gum Arabic, and this process should be controlled at temperature 30-100 ℃, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent
Through mixing of dispersion machine, oil phase is dispersed in aqueous phase, speed of agitator is 20000 rev/mins, temperature should be controlled at 10-40 ℃ during dispersion; Treat that temperature reduces to below 15 ℃, add amine aqueous solution, stirs while heat then, stop to heat after reaching the requirement temperature, and be incubated continuation stirring 20 hours, this process heating and temperature control is at 40-80 ℃; To be cooled to room temperature condition, add auxiliary agents such as preservative, dispersant, emulsifier, thickener, temperature can raise behind the adding auxiliary agent, and should be controlled at temperature 10-50 ℃ this moment, obtains emamectin benzoate microcapsule suspending agent.
In the described step (2), temperature preferably is controlled at 30-90 ℃ during the preparation water.
In the described step (3), dispersion temperature preferably is controlled at 10-30 ℃; Heating-up temperature preferably is controlled at 50-70 ℃; Temperature preferably is controlled at 10-40 ℃ when adding auxiliary agent.
The present invention can directly convert water dilution spraying and use.
Emamectin benzoate microcapsule suspending agent of the present invention compared with prior art, produce following beneficial effect: (1) improves the stability of effective ingredient emamectin-benzoate, improve the availability of effective ingredient, slow down the pesticide resistance growth rate of insect; (2) obviously improved pest controling effect, had concurrently quick-actingly and long-acting, (3) alternative high-toxic pesticide, and reduce the field dosage significantly effectively reduces environmental pollution and residue of pesticide.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1
(1) preparation oil phase: at ambient temperature, after 1.8g emamectin-benzoate, 20gAtloxLP and the grinding of 100g mineral oil, add 5g cresylene isocyanates and 3g hexamethylene isocyanates while stirring, this moment, reaction temperature raise, and the temperature that raises is controlled at 30 ℃;
(2) preparation water: be heated to 70 ℃, 1g polyvinyl alcohol and 6g gum Arabic are dissolved in the 130g deionized water, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent: oil phase and water mixing back are disperseed with the rotating speed of dispersion machine with 20000 rev/mins, temperature is controlled at 30 ℃ during dispersion, treat that temperature reduces to below 15 ℃, the mixture that adds 2.8g diethylenetriamines and 2.8g water, be heated to 50 ℃ while stirring, insulation was stirred 20 hours at 50 ℃, to be cooled to room temperature condition, add 0.3g Preventol D2,0.3g Preventol D7,6g Tersperse 2700,6g Pluronic PE, 8g 2%Kelcan S solution, this moment, temperature raise, temperature is controlled at 40 ℃, and finally obtaining emamectin-benzoate content is 0.6%, average grain diameter is 11.8 microns a microcapsule suspending agent.
Embodiment 2
(1) preparation oil phase: at ambient temperature, with 30g emamectin-benzoate, 200g AtloxLP and 1000g mineral oil, grind the back and add 16g cresylene isocyanates and 12g hexamethylene isocyanates while stirring, this moment, reaction temperature raise, and the temperature that raises is controlled at 40 ℃;
(2) preparation water: be heated to 70 ℃, 12g polyvinyl alcohol and 3g gum Arabic are dissolved in the 350g deionized water, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent: oil phase and water mixing back are disperseed with the rotating speed of dispersion machine with 20000 rev/mins, temperature is controlled at 40 ℃ during dispersion, treat that temperature reduces to below 20 ℃, add 20g 50% diethylenetriamines solution, be heated to 55 ℃ while stirring, maintaining the temperature at 55 ℃ stirred 20 hours, to be cooled to room temperature condition, add 0.8g Preventol D2,0.8g Preventol D7,30g Baykanol SL, 44g2%Kelcan S solution, this moment, temperature raise, temperature is controlled at 30 ℃, and finally obtaining emamectin-benzoate content is 1%, average grain diameter is 11.4 microns a microcapsule suspending agent.
Embodiment 3
(1) preparation oil phase: at ambient temperature, with 60g emamectin-benzoate, 200gAtloxLP and 1000g mineral oil, grind the back and add 16g cresylene isocyanates and 12g hexamethylene isocyanates while stirring, this moment, reaction temperature raise, and the temperature that raises is controlled at 20 ℃;
(2) preparation water: be heated to 70 ℃, 12g polyvinyl alcohol and 3g gum Arabic are dissolved in the 350g deionized water, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent: oil phase and water mixing back are disperseed with the rotating speed of dispersion machine with 20000 rev/mins, and temperature is controlled at 20 ℃ during dispersion.Treat that temperature reduces to below 20 ℃, add 20g 50% diethylenetriamines solution, be heated to 55 ℃ while stirring, maintaining the temperature at 55 ℃ stirred 20 hours, to be cooled to room temperature condition, add 0.8g Preventol D2,0.8g Preventol D7,30g Baykanol SL, 44g2%Kelcan S solution, this moment, temperature raise, temperature is controlled at 50 ℃, finally obtains emamectin-benzoate content and be 3.4%, average grain diameter is 11.4 microns microcapsule suspending agent.
Embodiment 4
(1) preparation oil phase: at ambient temperature, with 200g emamectin-benzoate, 200gAtloxLP and 1000g mineral oil, grind the back and add 47g cresylene isocyanates and 35g hexamethylene isocyanates while stirring, this moment, reaction temperature raise, and the temperature that raises is controlled at 50 ℃;
(2) preparation water: be heated to 70 ℃, 12g polyvinyl alcohol and 62g gum Arabic are dissolved in the 1300g deionized water, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent: oil phase and water are squeezed in the retort with pump respectively, disperse with the rotating speed of dispersion machine with 20000 rev/mins, temperature is controlled at 10 ℃ during dispersion, treat that temperature reduces to below 15 ℃, the mixture that adds 27.5g diethylenetriamines and 27.5g water, be heated to 50 ℃ while stirring, and 50 ℃ of insulated and stirred 20 hours, to be cooled to room temperature condition, add 2.5g Preventol D2,2.5g PreventolD7,56g Soprophor 4D 384,56g Ethylan NS-500LQ, 75g 2%Kelcan S solution, this moment, temperature raise, temperature is controlled at 30 ℃, and finally obtaining emamectin-benzoate content is 6.4%, average grain diameter is 11.8 microns a microcapsule suspending agent.
Purposes embodiment
The test of embodiment A photolysis stability
At the following irradiation different time of indoor ultraviolet light (40W), the missible oil of emamectin benzoate microcapsule suspending agent of the present invention and same amount, the degradation rate of microemulsion are as shown in table 1.
The light degradation rate of table 1 emamectin benzoate microcapsule suspending agent and missible oil, microemulsion
| Handle | 6h light degradation rate | 24h light degradation rate | 48h light degradation rate |
| Embodiment 2 | ??1.02 | ??2.13 | ??4.05 |
| 1% first dimension salt missible oil | ??4.06 | ??7.03 | ??10.27 |
| 1% first dimension salt microemulsion | ??4.55 | ??6.87 | ??12.79 |
Emamectin benzoate microcapsule suspending agent is much lower than the light degradation rate of missible oil and microemulsion as can be seen from Table 1, the visible advantage of microcapsule suspending agent aspect photolysis stability.
Embodiment B is given birth to test and is tested
Emamectin benzoate microcapsule suspending agent control brassicaceous vegetable beet armyworm test of pesticide effectiveness result of the present invention is as shown in table 2:
Table 2 emamectin benzoate microcapsule suspending agent
The control brassicaceous vegetable beet armyworm test of pesticide effectiveness is table as a result
| Handle | Concentration of treatment | Worm radix before the medicine | The 3rd day preventive effect % behind the medicine | The 7th day preventive effect % behind the medicine | The 14th day preventive effect % behind the medicine |
| Embodiment 3 | 4000 times | ??152 | ??91.63 | ??96.52 | ??98.27 |
| 2% first dimension salt missible oil | 4000 times | ??145 | ??90.85 | ??87.67 | ??83.52 |
| 2% first dimension salt microemulsion | 4000 times | ??148 | ??91.78 | ??89.56 | ??87.98 |
| Blank | ??- | ??140 | ??-2.54 | ??-7.62 | ??-18.75 |
Data are the mean value of 4 repetitions in the table 2.
As can be seen from Table 2, emamectin benzoate microcapsule suspending agent missible oil, microemulsion of the 3rd day preventive effect and same concentrations behind medicine is suitable, but the preventive effect of the 3rd day and the 7th day is apparently higher than other two kinds of formulations behind the medicine, and visible microcapsule suspending agent is in the advantage of holding the efficacious prescriptions face.
Claims (9)
1, a kind of emamectin benzoate microcapsule suspending agent is characterized in that: it is raw material that the oil phase of said preparation adopts the material of following weight content:
Emamectin-benzoate 0.1-20%;
The mixture 1-12% of cresylene isocyanates and hexamethylene isocyanates, the cresylene isocyanates: the weight ratio of hexamethylene isocyanates is 1: 0.3-2;
Aliphatic hydrocarbon 10-90%;
Oil-soluble polymeric dispersant 1-15%;
Amine 0.1-5%;
The water of said preparation is made up of water basically, and the weight content of water is 15-50%, can also comprise the mixture of polyvinyl alcohol and gum Arabic in addition, and the weight content of polyvinyl alcohol and gum Arabic is respectively 0.1-3%, 0.01-8%;
Said preparation also can comprise the auxiliary agent of following weight content:
Emulsifier 1-8%;
Dispersant 1-8%;
Preservative 0.05-0.5%;
Thickener 0.01-0.2%.
2, a kind of emamectin benzoate microcapsule suspending agent according to claim 1 is characterized in that: it is raw material that the oil phase of said preparation adopts the material of following weight content:
Emamectin-benzoate 0.1-20%;
The mixture 2-10% of cresylene isocyanates and hexamethylene isocyanates, the cresylene isocyanates: the hexamethylene isocyanates is 1: 0.5-1.5;
Aliphatic hydrocarbon 30-70%;
Oil-soluble polymeric dispersant 3-10%;
Amine 0.5-2%;
The water of said preparation is made up of water basically, and the weight content of water is 15-50%, can also comprise the mixture of polyvinyl alcohol and gum Arabic in addition, and the weight content of polyvinyl alcohol and gum Arabic is respectively 0.1-1%, 0.05-5%;
Said preparation also can comprise the auxiliary agent of following weight content:
Emulsifier 2-5%;
Dispersant 2-5%;
Preservative 0.1-0.3%;
Thickener 0.05-0.15%.
The percentage by weight of the mixture of described cresylene isocyanates and hexamethylene isocyanates is: the cresylene isocyanates: the hexamethylene isocyanates is 1: 0.3-2, preferred 1: 0.5-1.5.
3, a kind of emamectin benzoate microcapsule suspending agent according to claim 1 is characterized in that: can not contain emulsifier in the described auxiliary agent.
4, a kind of emamectin benzoate microcapsule suspending agent according to claim 1 is characterized in that: described aliphatic hydrocarbon comprises one or both mixtures in paraffin oil, the mineral oil.
5, a kind of emamectin benzoate microcapsule suspending agent according to claim 1 is characterized in that: described oil-soluble polymeric dispersant comprises one or both mixtures in alkyl nvp copolymer class, phosphoric acid ester, the polymerization hydroxy stearic acid class.
6, a kind of emamectin benzoate microcapsule suspending agent according to claim 1, it is characterized in that: described amine comprises ethylidene-1, one or both mixtures in 2-diamines, diethylenetriamines, the trien.
7, a kind of preparation method of emamectin benzoate microcapsule suspending agent is characterized in that, this method comprises following processing step:
(1) preparation oil phase
At ambient temperature, behind emamectin-benzoate, aliphatic hydrocarbon, oil-soluble polymeric dispersant mixed grinding, add cresylene isocyanates and hexamethylene isocyanates while stir, make oil phase, this moment, reaction temperature raise, and the temperature that needs to raise is controlled at 20-50 ℃;
(2) preparation water
Polyvinyl alcohol and gum Arabic added make water in the entry, heating makes polyvinyl alcohol and the faster dissolving of gum Arabic, and this process should be controlled at temperature 30-100 ℃, the frozen water cooling of dissolving back;
(3) preparation microcapsule suspending agent
Through mixing of dispersion machine, oil phase is dispersed in aqueous phase, speed of agitator is 20000 rev/mins, temperature should be controlled at 10-40 ℃ during dispersion; Treat that temperature reduces to below 15 ℃, add amine aqueous solution, stirs while heat then, stop to heat after reaching the requirement temperature, and be incubated continuation stirring 20 hours, this process heating and temperature control is at 40-80 ℃; To be cooled to room temperature condition, add auxiliary agents such as preservative, dispersant, emulsifier, thickener, temperature can raise behind the adding auxiliary agent, and should be controlled at temperature 10-50 ℃ this moment, obtains emamectin benzoate microcapsule suspending agent.
8, the preparation method of a kind of emamectin benzoate microcapsule suspending agent according to claim 7 is characterized in that: in the described step (2), temperature is controlled at 30-90 ℃ during the preparation water.
9, the preparation method of a kind of emamectin benzoate microcapsule suspending agent according to claim 7 is characterized in that: in the described step (3), dispersion temperature is controlled at 10-30 ℃; Heating and temperature control is at 50-70 ℃; Temperature is controlled at 10-40 ℃ when adding auxiliary agent.
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