CN104115826A - Metalaxyl microcapsule water suspension and preparation method thereof - Google Patents
Metalaxyl microcapsule water suspension and preparation method thereof Download PDFInfo
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- CN104115826A CN104115826A CN201410222912.3A CN201410222912A CN104115826A CN 104115826 A CN104115826 A CN 104115826A CN 201410222912 A CN201410222912 A CN 201410222912A CN 104115826 A CN104115826 A CN 104115826A
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Abstract
The invention relates to a metalaxyl microcapsule water suspension and a preparation method thereof. The method comprises the steps of: by taking a prepolymer generated by melamine and a formaldehyde solution as a wall material, dissolving metalaxyl into a capsule-core solvent, adding an emulsifier and a wetting dispersing agent, generating a metalaxyl microcapsule through polymerization by adjusting the pH, adding a proper quantity of auxiliaries such as a viscosity adjusting agent and a dispersing agent NNO in a proper proportion, and adding water for shaking uniformly to obtain the metalaxyl microcapsule water suspension. Compared with the conventional preparation, the metalaxyl microcapsule water suspension has the characteristics that the lasting period is long; pesticides are high in effective utilization rate; the water is used as a dispersing medium, so that the metalaxyl microcapsule water suspension is low in toxicity, environment-friendly and safe to store and transport; the capsule-core effective component is high in storage and transportation stability, low in preparing and processing cost, good in market prospect and the like.
Description
Technical field
The invention belongs to formulations of pesticide manufacture field, be specifically related to taking metalaxyl as core, be coated taking melamine resin as cyst material and form microcapsules, and further make metalaxyl microcapsules SC and preparation method thereof.
Background technology
At present, the formulations of pesticide are just towards Water-borne modification, spheroidizing, functionalization, slowly-releasing, Labor-saving and the future development that becomes more meticulous, and spacetabs type formulation is generally paid attention to.Nowadays document has the report about slow release type preparation in a large number.Since first Pennwalt company of the U.S. in 1974 adopts interfacial polymerization parathion-methyl to be made to microcapsules (Penncap-M), pesticide micro capsule has become the highest one of technology content in current pesticides new formulation.Utilize microcapsules technology solid, liquid pesticidal can be coated on and in natural or synthetic macromolecule cyst material, form semi permeability or seal miniature vessel, extend drug effect, reduce high-toxic pesticide toxicity, prevent that active ingredient from decomposing and volatilization, reduce dosage, prevent drift, reduce environmental pollution, use conveniently, improve medicament selectivity and make the effects such as liquid pesticidal powdered thereby play.At present, lot of domestic and international is all at the development of being devoted to pesticide micro capsule preparation.Microcapsules granula has become one of direction of pesticides new formulation development from now on.
Microcapsules are a kind of delivery formulations of controlling, and are with polymeric membrane, agricultural chemicals to be wrapped up, and being processed into diameter is several microns of small spherolites to hundreds of micron.The principal character of this type of medicament is: (1) alleviates the murder by poisoning of high toxicity chemical substance to mammal; (2) greatly extend lasting period of same dose agricultural chemicals; (3) reduce because of the drug wastage evaporating and liquid flow causes, reduce solvent load; (4) consumption of saving medicament, reduces the toxicity to plant, alleviates the pollution to environment; (5) selectivity of raising medicine.
Metalaxyl is N-(2-methoxyl group acetyl group)-N-(2; 6-xylyl)-D; L-the third ammonia; belong to acid amide fungicides; high-efficiency low-toxicity, the longevity of residure are long; there is very strong protection and therapeutic action; belong to specificity site inhibitor; mechanism of action is synthetic the working of protein by inhibition Oomycete fungi; metalaxyl energy visible through the seed coat, along with sprouting and the growth of seed, can interiorly inhale the root, stem and leaf that is transmitted to plant; and transfer to each organ of plant with moisture in plant corpus, can do cauline leaf processing, seed treatment and soil treatment.In early blight, the late blight of control potato, black shank, positive role has been brought into play in the aspect such as downy mildew, epidemic disease of melon and fruit, vegetables.
Metalaxyl belongs to hypotoxicity bactericide.Former medicine rat acute LD50 of passing through mouth is 669 mgs/kg, acute through skin LD50>3100 milliliter/kilogram.Eyes and skin are had to slight spread effect, and to fish low toxicity, trout TLM is 100 mgs/kg (96h).
At present metalaxyl is mainly processed at home granule, wetting powder, aqua and uses, but also there are some shortcomings in the metalaxyl of these formulations in application: 1, after the dispenser of metalaxyl regular dosage form, active ingredient is subject to the environmental influence such as light, moisture, degrade relatively very fast, phase half life period on plant leaf blade is shorter, reaches and prevents and treats the repeatedly dispenser of disease requirement need; 2,, compared with conventional pesticide formulation, microcapsule formulation (microcapsule suspending agent, microcapsule powder) has the effective rate of utilization that extends the lasting period, improve agricultural chemicals, avoid agricultural chemicals to be subject to the decomposition that external environment causes to run off, alleviate the feature of toxicity and poisoning, reduction environmental pollution.Microcapsule formulation has become one of important development direction of formulations of pesticide processing.Metalaxyl is processed into microcapsules SC and is expected to address the above problem, and the at present domestic research and the application report that use melamine resin to prepare metalaxyl microcapsule formulations also do not seen.
Summary of the invention
One of object of the present invention is to provide a kind of metalaxyl microcapsules SC in order to solve above-mentioned technical problem, and it is water miscible requiring high polymer monomer, and the polymer generating is insoluble; Microcapsule wall has good heat endurance and mechanical property.Two of object of the present invention is the preparation method of a kind of metalaxyl microcapsules SC that provides above-mentioned, and the method requires that preparation process is simple, technical maturity and be convenient to industrialization.Said preparation use procedure does not need additionally to add wetting agent or other auxiliary agent, and can realize control efficiency, it can be widely used in some fungal disease of crops and economic crops, as effective especially to downy mildew, phytophthora, rotten mould fungi, can be used for the crops such as grape, capsicum, cucumber, tobacco, potato, brassicaceous vegetable and tomato.
The present invention is intended to overcome the deficiency of above-mentioned prior art, and a kind of metalaxyl microcapsules SC is provided, and solves regular dosage form and uses rear metalaxyl to be subject to such environmental effects and to cause short problem of lasting period.The invention provides a kind of cost is low, be convenient to suitability for industrialized production metalaxyl microcapsules SC formula and preparation method, thereby for the control of disease in agricultural production provides a kind of new product, be conducive to agriculture sustainable development and agriculture environmental protection.
The present invention is based on for this reason following some conceive to realize: (1) will be selected one to refuse water pocket wall material metalaxyl is coated, and reduces contacting of the latter and water; (2) for raising and the market competitiveness of regular dosage form, require cyst material cheap, be convenient to reduce preparation cost; (3) preparation technical process is simple, can under normal pressure, carry out, and environmental pollution is little, is convenient to industrialization and production control cost; (4) after metalaxyl is coated, make moisture suspending agent type, reduce the consumption of organic solvent and further reduce preparation cost; (5) formulation is identical with regular dosage form occupation mode, as suspending agent, meets peasant's medication custom, is convenient to marketing.
For achieving the above object, a kind of metalaxyl microcapsules SC of the present invention, according to percetage by weight meter, be prepared from by following raw material: 10～20% metalaxyl, 15～25% capsule heart solvent, 15～25% cyst material, 1～3% wetting dispersing agent, 1～5% emulsifier, 1～3% viscosity modifier, 1～3% antifreeze and 1～5% dispersant NNO, surplus is water, wherein, cyst material is melamine resin.
Wherein, described capsule heart solvent is preferably the one in dimethylbenzene, toluene or benzene.
Melamine resin is preferably made by polycondensation reaction with mol ratio by melamine and formaldehyde for 1: 1.5～1: 2.5.
Emulsifier is selected from the one in Greenmul5860, SMA (maleic anhydride of styrene), dodecyl sodium sulfate or the lauryl sodium sulfate that agriculture breast 600#, Nongru-700 #, agriculture breast 1601, agriculture breast 0203, Beijing Green Tai Mu Science and Technology Ltd. produce, more preferably from agriculture breast 0203.
One in Greensperse8425, Tersperse2425, dispersant KET, lauryl sodium sulfate or neopelex that wetting dispersing agent is preferably produced from Beijing Green Tai Mu Science and Technology Ltd..Wherein, Tersperse2425 is that Hensel takes the alkylnaphthalene sulfonate formaldehyde condensation products anionoid efficient general type dispersant of sending out, and there is wetting function, be mainly used in the formulations such as pesticide water dispersible granule, wetting powder, aqueous suspension agent, seed coat agent as dispersant kind.
Viscosity modifier is the one in carboxymethyl cellulose, xanthans or polyvinyl alcohol preferably, more preferably xanthans.Viscosity modifier can keep the physical stability of preparation in storage process, the viscosity of the hierarchy of control.
Antifreeze is one or more in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol or urea preferably.
Water is distilled water or deionized water.
The preparation method of a kind of metalaxyl microcapsules SC of the present invention, prepares according to following steps:
(1) preparation of performed polymer: melamine is dissolved in formaldehyde, with sodium hydroxide adjusting pH to 8～9, is warming up to 65～70 DEG C, stir 10 minutes, obtain the clear melamine resin performed polymer aqueous solution;
(2) emulsion preparation: metalaxyl is fully dissolved in capsule heart solvent, after stirring, adds emulsifier and wetting dispersing agent, fully vibration forms stable O/W emulsion;
(3) cyst wall polymerization: rotating speed is adjusted to 200～400r/min, add the melamine resin performed polymer aqueous solution, slowly add hydrochloric acid to turn down gradually the pH value of system, system final pH value is adjusted to 4.2, after polymerisation 1～1.5 hour, keep 0.5～1 hour curing cyst wall, after cyst wall fully solidifies, add sodium hydroxide to regulate pH value 6.5～7, add dispersant NNO, viscosity modifier and antifreeze, stir and make metalaxyl microcapsules SC.
The invention has the advantages that: the microcapsule coated rate of the metalaxyl microcapsules SC that (1) obtains can be up to more than 93.58%; (2) Microcapsules Size of the metalaxyl microcapsules SC obtaining, at 1～50 μ m, has the feature of pesticide suspension concentrate, and can directly be watered spraying and use, or along with irrigation water processing soil is prevented and treated corps diseases; (3) the microcapsules form of the metalaxyl microcapsules SC obtaining is good, and smooth surface is fine and close in depression, big or small homogeneous, and without adhesion, good dispersion property; (4) utilize situ aggregation method taking melamine resin as wall material, not only realized technology of preparing simple, the saccilar process time is short, on by the biologically active of embedding substance without impact, compared to interfacial polymerization, especially in mild reaction conditions, in the situation without heating, realize the encystation of high clad ratio; (5) preparation cost low, be convenient to suitability for industrialized production, thereby for the control of disease in agricultural production provides a kind of new product, be conducive to agriculture sustainable development and agriculture environmental protection.
Brief description of the drawings
Fig. 1 is the Microcapsules Size distribution map of metalaxyl microcapsules SC of the present invention;
Fig. 2 is view under the microscope of metalaxyl microcapsules SC of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
In the there-necked flask that thermometer, agitating device are housed, add melamine and formaldehyde, mol ratio is 1: 1.5, by sodium hydroxide adjusting pH value to 8, is warming up to 70 DEG C, and stirring reaction 10 minutes, obtains the melamine resin prepolymer aqueous solution.
Under normal temperature, former 5.21g96.0wt% metalaxyl medicine is dissolved in 9.0g dimethylbenzene, after stirring, add 0.7g agriculture breast 0203 and 0.4gTersperse2425 fully to vibrate and form stable O/W emulsion, turn speed to 200 revs/min, add the 14g melamine resin performed polymer aqueous solution, in 60 minutes, add watery hydrochloric acid regulation system pH to 4.2, add ammonium chloride to solidify cyst wall after 0.5 hour, sodium hydroxide regulates pH to 6.5, add 2g dispersant NNO, add again 0.2g xanthan gum solution, 4g ethylene glycol, system gross weight is reached to 50g with distilled water, stir and obtain 10wt% metalaxyl microcapsules SC.
Embodiment 2:
In the there-necked flask that thermometer, agitating device are housed, add melamine and formaldehyde, mol ratio is 1: 2, by sodium hydroxide adjusting pH value to 8.5, is warming up to 70 DEG C, and stirring reaction 10 minutes, obtains the melamine resin prepolymer aqueous solution.
Under normal temperature, former 10.42g96.0wt% metalaxyl medicine is dissolved in 18.0g dimethylbenzene, after stirring, add 1.4g agriculture breast 0203 and 0.6g neopelex, fully vibration forms stable O/W emulsion, turn speed to 300 revs/min, add the 28g melamine resin performed polymer aqueous solution, in 1.5 hours, add watery hydrochloric acid regulation system pH to 4.2, add ammonium chloride to solidify cyst wall after 0.5 hour, sodium hydroxide regulates pH to 6.5, add 2g dispersant NNO, add again 0.2g xanthan gum solution, 4g ethylene glycol, system gross weight is reached 100g by water, stir and obtain 10wt% metalaxyl microcapsules SC.
Claims (8)
1. a metalaxyl microcapsules SC, it is characterized in that according to percetage by weight meter, be prepared from by following raw material: 10～20% metalaxyl, 15～25% capsule heart solvent, 15～25% cyst material, 1～3% wetting dispersing agent, 1～5% emulsifier, 1～3% viscosity modifier, 1～3% antifreeze and 1～5% dispersant NNO, surplus is water, wherein, cyst material is melamine resin.
2. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that capsule heart solvent is the one in dimethylbenzene, toluene or benzene.
3. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that melamine resin is made by polycondensation reaction with mol ratio by melamine and formaldehyde for 1: 1.5～1: 2.5.
4. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that emulsifier is selected from one or more in agriculture breast 600#, Nongru-700 #, agriculture breast 1601, agriculture breast 0203, Greenmul5860, SMA, dodecyl sodium sulfate or lauryl sodium sulfate.
5. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that wetting dispersing agent is selected from one or more in Greensperse8425, Tersperse2425, dispersant KET, lauryl sodium sulfate or neopelex.
6. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that viscosity modifier is selected from one or more in carboxymethyl cellulose, xanthans or polyvinyl alcohol.
7. a kind of metalaxyl microcapsules SC according to claim 1, is characterized in that antifreeze is selected from one or more in ethylene glycol, propane diols, glycerine, PEG400, isopropyl alcohol or urea.
8. a preparation method for metalaxyl microcapsules SC claimed in claim 1, is characterized in that preparing according to following steps:
(1) preparation of performed polymer: melamine is dissolved in formaldehyde, with sodium hydroxide adjusting pH to 8～9, is warming up to 65～70 DEG C, stir 10 minutes, obtain the clear melamine resin performed polymer aqueous solution;
(2) emulsion preparation: metalaxyl is fully dissolved in capsule heart solvent, after stirring, adds emulsifier and wetting dispersing agent, fully vibration forms stable O/W emulsion;
(3) cyst wall polymerization: rotating speed is adjusted to 200～400r/min, add the melamine resin performed polymer aqueous solution, slowly add hydrochloric acid to turn down gradually the pH value of system, system final pH value is adjusted to 4.2, after polymerisation 1～1.5 hour, keep 0.5～1 hour curing cyst wall, after cyst wall fully solidifies, add sodium hydroxide to regulate pH value 6.5～7, add dispersant NNO, viscosity modifier and antifreeze, stir and make metalaxyl microcapsules SC.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104452277A (en) * | 2014-11-28 | 2015-03-25 | 东华大学 | Microcapsule capable of cladding 2,4-dichloro-3,5-dimethylphenol, as well as preparation and application of microcapsule |
| CN104823983A (en) * | 2015-04-30 | 2015-08-12 | 中国农业大学 | Microcapsule bactericide for controlling Botrytis cinerea and Sclerotinia scleotiorum |
| CN107258802A (en) * | 2017-08-08 | 2017-10-20 | 浙江禾本科技有限公司 | A kind of water-soluble agricultural composite Nano bactericide and preparation method thereof |
| CN111727689A (en) * | 2020-07-16 | 2020-10-02 | 榆林市农业科学研究院 | High-temperature sterilization method for pea seeds |
-
2014
- 2014-05-23 CN CN201410222912.3A patent/CN104115826A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104452277A (en) * | 2014-11-28 | 2015-03-25 | 东华大学 | Microcapsule capable of cladding 2,4-dichloro-3,5-dimethylphenol, as well as preparation and application of microcapsule |
| CN104823983A (en) * | 2015-04-30 | 2015-08-12 | 中国农业大学 | Microcapsule bactericide for controlling Botrytis cinerea and Sclerotinia scleotiorum |
| CN107258802A (en) * | 2017-08-08 | 2017-10-20 | 浙江禾本科技有限公司 | A kind of water-soluble agricultural composite Nano bactericide and preparation method thereof |
| CN111727689A (en) * | 2020-07-16 | 2020-10-02 | 榆林市农业科学研究院 | High-temperature sterilization method for pea seeds |
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Application publication date: 20141029 |