CN101632355B - Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof - Google Patents
Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a pesticide water dispersible granule containing an organic silicon surface active agent and a preparation method thereof. The preparation method comprises the following steps: pulverizing one or more pesticide active components, a wetting agent, a dispersing agent, a disintegrating agent, a stabilizing agent and a carrier through an air flow and then sufficiently stirring and uniformly mixing the materials; then sequentially adding an organic silicon surface active agent, a defoaming agent and an adhesive aqueous solution as well as uniformly stirring the materials; kneading the materials in a kneading machine to prepare a plastic material; conveying the plastic material into an extrusion granulator to granulate; and obtaining a water dispersible granule finished product through drying and sieving. The pesticide preparation of the invention has good wettability, stronger adhesive power and expansion capability and excellent infiltrability and can obviously improve the utilization rate and the drug effect of the pesticide.
Description
Technical field:
The present invention relates to pesticide field, more specifically relate to the method for using of a kind of novel agrochemical auxiliary agent in pesticide water dispersible granules and the preparation method of this water dispersible granules.
Background technology:
Using the pesticide control disease pest and weed is to guarantee the indispensable means of agricultural product good quality and high output.The modern formulations of pesticide are to water baseization, ultramicronising, no dust and sustained release development, and wherein being transformed to water dispersible granules by wetting powder is exactly one of main direction of agricultural chemicals development.Pesticide water dispersible granules can reduce the consumption of organic solvent, the dust pollution that does not have wettable powder and pulvis to bring again, and reduced pesticide producing and cost of transportation, safer, more environmental protection has become a kind of very important formulation in the pesticidal preparations.Agricultural chemicals will be brought into play high service efficiency, at first will make pesticide solution on target substance, fully sprawl and be detained.This just requires soup to have lower surface tension, has good wetability and permeability on the target surface.Otherwise will cause fluid loss, will inevitably influence drug effect like this, directly environment caused serious pollution.Simultaneously, if drug effect is not high, the peasant will inevitably strengthen dispenser dynamics and intensity, has both caused the increase of agricultural chemicals use cost, has also caused the severe overweight of residue of pesticide.Therefore, improving the agricultural chemicals availability is to reduce drug cost, reduces environmental pollution, reduces the basic of residue of pesticide.
Organosilicon table surfactant is existing more patent report in other field, does not still have disclosed patent at present but in pesticide field, use.Compare with conventional surfactant, organic silicon surfactant can effectively reduce the surface tension of water, reduces the contact angle of soup and biological target, has the infiltration capacity that good wetability, stronger adhesion, superpower extended capability are become reconciled.Soup is arrived be difficult to wetting place, increase the spraying coverage rate, promote the soup fast Absorption.Can improve simultaneously the resistance of rainwater washing against ability of soup, improve the effective rate of utilization of agricultural chemicals, reduce the agricultural chemicals injected volume.As a kind of novel, insecticides adjuvant efficiently, it has broad application prospects in pesticide industry.
Therefore, in the present invention novel surfactant-organic silicon surfactant is joined in the pesticide water dispersible granules, made a kind of physical stability, chemical stability, all good pesticide water dispersible granules of preparation effect property.
Technology contents:
The objective of the invention is to propose a kind of pesticide water dispersible granules that contains organic silicon surfactant and preparation method thereof.
Pesticide water dispersible granules of the present invention is made up of pesticidal active substance, organic silicon surfactant, auxiliary element and filler.
Pesticidal active substance wherein is for being selected from insecticide AVM, Affirm (Merck Co.), emamectin-benzoate, worm hydrazides, Imidacloprid, butyl ether urea, fly eradication amine, Acetamiprid, decis, fluorine worm nitrile; Bactericide is selected from Difenoconazole, propiconazole, nitrile bacterium azoles, triazolone, dimethomorph, phonetic mould amine, tmtd, mancozeb, Flusilazole; Herbicide nicosulfuron, tribenuron-methyl, Quizalotop-ethyl, napropamide, atrazine; In miticide four mite piperazines, azacyclotin, fenbutatin oxide, the pyridaben one or more.
Organic silicon surfactant wherein can be to well known to a person skilled in the art those.Preferably has T type structure, by all being the skeleton that siloxanes forms that methylates, with the trisiloxanes of one or more polyethers tail.The more preferably Silwet408, Silwet625, the Silwet618 SilwetPD that produce of GE company, and Silwet806, the Boost that Doro Elaneo company produces, or the Sylgard309 that produces of Doco Corning company etc.Concrete general structure does
Pesticide water dispersible granules of the present invention also contains auxiliary element.Described auxiliary element wetting agent can be selected from fatty acid sulfate salt; Alkylbenzenesulfonate; Dialkyl group succinate sulfonate sodium; α-Xi Jihuangsuanyan; Fatty alcohol APES succinate monoester sulfonate; Fatty acid amide N methyl taurine sodium salt; Lauryl alcohol polyethylene glycol oxide base ether sodium sulfate; APES sulphate; Single two Negel; Sodium lignin sulfonate; The butyl biphenyl natrium phenolsulfonicum; Phenolsulfonic acid formaldehyde condensation products sodium salt; Phosphate ester salt; Morwet EFW; Morwet DB; Morwet B; Morwet IP; Morwet 3028; Among the Morwet 3008 one or more
Dispersant can be selected from sodium lignin sulfonate; Calcium lignosulfonate; Alkyl polyoxyethylene ether sulfonate; The polyoxyethylene poly-oxygen propylene aether block copolymer; The APES formaldehyde condensation products; Petroleum sodium sulfonate; Aliphatic alcohol polyoxyvinethene phosphate; Benzyl naphthalenesulfonate formaldehyde condensation compound (dispersing agent C NF); 1-methyl naphthalene sulfonate formaldehyde condensate (Dispersant MF); Desugar condensation sodium lignin sulfonate (dispersant M); Di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate (dispersant NNO); Morwet D-425; MorwetD-110; Morwet D-450; Among the Morwet D-500 one or more.。
Adhesive can be selected from any or several kinds in starch, gelatin, gum Arabic, polyvinylpyrrolidone (PVP), CMC, hydroxyethylcellulose, methylcellulose, polyethylene glycol, polyvinyl alcohol, glucose, the sucrose.
Stabilizing agent can be selected from one or more in chloropropylene oxide, pyrogallol, butyl glycidyl ether, potassium sorbate, Sodium Benzoate, epoxidised soybean oil, linseed oil, BHA, BHT, citric acid, PABA, castor oil, olive oil, hydroquinones, bisnaphthol, the salicylic acid.
Antifoaming agent can be selected from silicone emulsion, organic modified polyorganosiloxane, tributyl phosphate, sorbitan mono-laurate, glyceryl monoricinoleate, C10-20 saturated fat acids, C8-10 aliphatic alcohols, SAG1522; SAG1577; SAG1572; SAG1538, SAG471, one or more among the SAG5693.
Disintegrant can be selected from one or more in ammonium sulfate, urea, polyvinylpyrrolidone, sodium sulphate, starch and derivative thereof, cellulose, sodium bicarbonate, bay acid alcohol sodium sulphate, sodium alginate, sodium chloride, the bentonite.
Filler can be selected from one or more in kaolin, white carbon, attapulgite, potter's clay, bentonite, montmorillonite, calcium carbonate, diatomite, dolomite, the talcum.
The pesticide water dispersible granules that contains organic silicon surfactant of the present invention consists of by weight by pesticide activity component 1%～80%, organic silicon surfactant 1%～25%, and auxiliary element and filler are formed.
Further, the composition of pesticide water dispersible granules of the present invention is by weight:
Pesticide activity component 1%～80% wetting agent 0.5%～20%
Organic silicon surfactant 1%～25% dispersant 0.5%～20%
Antifoaming agent 0.3%～5.0% adhesive 0.3%～10%
Disintegrant 0～5.0% stabilizing agent 0～10%
Filler 2%～90%.
Pesticide water dispersible granules of the present invention can prepare through following method:
Earlier pesticide activity component and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Pesticide water dispersible granules of the present invention is owing to the particle that pesticide activity component is processed into a certain size; And added organic silicon surfactant therein; Thereby have the following advantages: (1) is solvent-free few with dust, and environmental pollution is little, to the producer and user and Environmental security; (2) intensity of enough hardness is arranged, prevent that product from producing the dust that exceeds standard during packing, storing; (3) certain shape and fineness are arranged, density is big, and good fluidity glutinously connects, do not lump, sticking wall, practices thrift cost, packs easily; (4) have low surface tension after the said preparation spraying, good in the target surface wettability, sprawl with infiltration capacity by force, be distributed in the target surface with fine particle, help improving drug effect; (5) the organosilicon auxiliary agent can make soup arrival be difficult to wetting place, increases the spraying coverage rate, promotes the soup fast Absorption.Improve the resistance of rainwater washing against ability of soup, improve the effective rate of utilization of agricultural chemicals, reduce the agricultural chemicals injected volume.
The invention provides a kind of efficient, low toxicity, pesticide water dispersible granules that biological effective rate of utilization is high, comparatively friendly to environment.Solvent-free and the dust of said preparation; Environmental pollution is few; And novel surfactant-organic silicon surfactant is incorporated in the processing of pesticide water dispersible granules; By the physics peptizaiton of wetting dispersing agent and comminution by gas stream, form a kind of physical stability, chemical stability, all good pesticide water dispersible granules of preparation effect property, can pesticide activity component be dispersed in the water during use.Preparation technology of the present invention is simple, and production cost is low.
Embodiment:
Essence for a better understanding of the present invention specifies technology contents of the present invention with instance below, but content of the present invention is not limited thereto.
One: 5% Affirm (Merck Co.) water dispersible granules of embodiment
Each constituent content is Affirm (Merck Co.) 5%, dispersant Morwet D-4254%, wetting agent Morwet EFW 2% by weight, and organic silicon surfactant Silwet408 8%, silicone defoaming agent SAG1522 1%, disintegrant sodium sulphate 10.0%, adhesive CMC 1%, stabilizing agent BHT 1%, filler kaolin complement to 100%.
The preparation process is: earlier pesticide activity component Affirm (Merck Co.) and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Two: 10% difenoconazole water dispersible granules of embodiment
Each constituent content is Difenoconazole 10%, dispersant Morwet D-4253%, wetting agent Morwet EFW 3% by weight, and organic silicon surfactant Silwet408 6%, silicone defoaming agent silicone emulsion 0.5%, disintegrant urea 10.0%, adhesive hydroxyethylcellulose 1%, stabilizing agent Sodium Benzoate 1%, filler kaolin complement to 100%.
The preparation process is: earlier pesticide activity component Affirm (Merck Co.) and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Three: 69% mancozeb dimethomorph water dispersion granulas of embodiment
Each constituent content is mancozeb 60%, dimethomorph 9%, dispersant MorwetD-450 3%, wetting agent Morwet 3,008 2% by weight, organic silicon surfactant Silwet618 8%, antifoaming agent SAG1577 1%, disintegrant urea 5.0%, adhesive gelatin 1%, stabilizing agent Sodium Benzoate 1%, filler white carbon 100%.
The preparation process is: earlier pesticide activity component mancozeb, dimethomorph and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Four: 75% fly eradication amine of embodiment water dispersible granules
Each constituent content is fly eradication amine 75%, dispersant Morwet D-450 4%, wetting agent Morwet 3,028 2% by weight, and organic silicon surfactant Silwet408 8%, silicone defoaming agent silicone emulsion 0.5%, disintegrant sodium sulphate 5.0%, adhesive polyvinylpyrrolidone 1%, stabilizing agent potassium sorbate 0.5%, filler white carbon complement to 100%.
The preparation process is: earlier pesticide activity component fly eradication amine and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Five: 80% water dispersible granule of nicosulfuron of embodiment
Each constituent content is nicosulfuron 80%, dispersant Morwet D-500 3%, wetting agent Morwet 3,028 2% by weight, and organic silicon surfactant Silwet408 6%, silicone defoaming agent SAG1577 1%, disintegrant urea 5.0%, adhesive polyvinylpyrrolidone 0.5%, stabilizing agent Sodium Benzoate 1%, filler white carbon complement to 100%.
The preparation process is: earlier pesticide activity component nicosulfuron and wetting agent, dispersant, disintegrant, stabilizing agent, carrier are fully mixed behind comminution by gas stream; Add organic silicon surfactant, antifoaming agent and the adhesive aqueous solution then successively; Stir while adding evenly; In kneader, mediate, process plastic material.Send this material to extruding granulator at last and carry out granulation.Obtain the water dispersible granules finished product through dry, screening.
Embodiment six: the evaluation of preparation physicochemical property effect property
To adding the preparation of organic silicon surfactant described in the present invention, the assay method of each item evaluation index is following: (in the following experiment, CK all adopts the white carbon of equivalent to substitute organic silicon surfactant, all the other recipe ingredients and according to the invention same)
1, surface tension (Υ)
The mensuration of medical liquid surface tension adopts platinum plate method.When the surface tension of soup was lower than the surface free energy of target, soup just might and be sprawled at the target moistened surface.
2, dynamic contact angle (θ)
Dynamic contact angle adopts contact angle measurement to measure, and adopts video method.The soup that dynamic contact angle is little is strong to wettability on the selected target.
3, drop expanding area (S)
The mensuration of drop expanding area adopts integration method.The drop expanding area has directly been represented the extended capability of soup on the target surface, and the drop expanding area is big, shows that the preparation spreadability is good.
Table 1 preparation effect property of the present invention evaluation (dilution 1000 *)
| The mensuration project | CK | FORMULATION EXAMPLE 1 |
| Surface tension (mN/m) | 38.64 | ?22.8 |
| Contact angle during 30s (°) | 58.2 | ?32.6 |
| Expansion radius (mm) during 30s | 2.48 | ?3.80 |
The effect property evaluation of table 2 preparation of the present invention (dilution 1000 *)
| The mensuration project | CK | FORMULATION EXAMPLE 2 |
| Surface tension (mN/m) | 37.2 | ?22.6 |
| Contact angle during 30s (°) | 65.5 | ?38.7 |
| Expansion radius (mm) during 30s | 2.64 | ?3.78 |
The effect property evaluation of table 3 preparation of the present invention (dilution 1000 *)
| The mensuration project | CK | FORMULATION EXAMPLE 3 |
| Surface tension (mN/m) | 38.4 | ?22.1 |
| Contact angle during 30s (°) | 62.8 | ?40.5 |
| Expansion radius (mm) during 30s | 2.69 | ?3.87 |
The effect property evaluation of table 4 preparation of the present invention (dilution 1000 *)
| The mensuration project | CK | FORMULATION EXAMPLE 4 |
| Surface tension (mN/m) | 39.4 | ?22.3 |
| Contact angle during 30s (°) | 58.1 | ?34.3 |
| Expansion radius (mm) during 30s | 2.95 | ?3.99 |
The effect property evaluation of table 5 preparation of the present invention (dilution 1000 *)
| The mensuration project | CK | FORMULATION EXAMPLE 5 |
| Surface tension (mN/m) | 36.7 | ?21.6 |
| Contact angle during 30s (°) | 56.8 | ?35.2 |
| Expansion radius (mm) during 30s | 2.78 | ?3.46 |
Can find out that from above mensuration result surface tension, the contact angles and wetting time that preparation can reduce soup is effectively shone in the preparation comparison that is added with organic silicon surface active agent, increases the expanding area of drop.
Embodiment seven: preparation field efficacy control efficiency is estimated
The pesticide water dispersible granules that adopts the present invention to produce for checking is further compared the advance that does not add the pesticide water dispersible granules that organic silicon surfactant produces, and has carried out field control effectiveness test respectively, and employing method and result are exemplified below said.Below in the experiment, CK adopts the white carbon of equivalent to substitute organic silicon surfactant, all the other recipe ingredients and according to the invention same.
1,5% Affirm (Merck Co.) water dispersible granules field control effectiveness test
Trial crops is a wild cabbage, and controlling object is a beet armyworm 1-2 instar larvae, with 3000 times of preparation dilutions, restrains even spraying by mu with amount of formulation 10, dispenser once, each handles triplicate, 2 days and 7 days investigation prevention effects behind the medicine, the result sees the following form.
Table 6 5% Affirm (Merck Co.) water dispersible granules control beet armyworm effect relatively
2,10% difenoconazole water dispersible granule field control effectiveness test
Trial crops is a tomato, and controlling object is an early blight, with 3000 times of preparation dilutions, with amount of formulation 10 gram even spraying, in the dispenser of early blight their early stage once, executes medicine for the second time after 7 days, altogether the dispenser secondary by mu.Each handles triplicate, for the first time 7 days and 7 days preventive effects behind the medicine for the second time behind the medicine of investigation respectively, and the result sees the following form.
Table 7 10% difenoconazole water dispersible granule is prevented and treated the early blight effect relatively
3,69% mancozeb dimethomorph water dispersion granula field control effectiveness test
Trial crops is a cucumber, and controlling object is a downy mildew, with 600 times of preparation dilutions, with amount of formulation 100 gram even spraying, in the dispenser of downy mildew their early stage once, executes medicine for the second time after 7 days by mu, executes medicine for the third time after 14 days, and dispenser is three times altogether.Each handles triplicate, investigates for the third time 7 days preventive effects behind the medicine, and the result sees the following form.
Table 8 69% mancozeb dimethomorph water dispersion granula is prevented and treated the downy mildew effect relatively
Claims (5)
1. pesticide water dispersible granules; It is 5% Affirm (Merck Co.) water dispersible granules; Wherein each constituent content is by weight: Affirm (Merck Co.) 5%, dispersant Morwet D-4254%, wetting agent Morwet EFW 2%, organic silicon surfactant Silwet4088%, silicone defoaming agent SAG15221%, disintegrant sodium sulphate 10.0%, adhesive CMC 1%, stabilizing agent BHT 1%, filler kaolin complement to 100%.
2. pesticide water dispersible granules; It is 10% difenoconazole water dispersible granule; Wherein each constituent content is by weight: Difenoconazole 10%, dispersant Morwet D-4253%, wetting agent Morwet EFW 3%, organic silicon surfactant Silwet4086%, silicone defoaming agent silicone emulsion 0.5%, disintegrant urea 10.0%, adhesive hydroxyethylcellulose 1%, stabilizing agent Sodium Benzoate 1%, filler kaolin complement to 100%.
3. pesticide water dispersible granules; It is 69% mancozeb dimethomorph water dispersion granula; Wherein each constituent content is by weight: mancozeb 60%, dimethomorph 9%, dispersant MorwetD-4503%, wetting agent Morwet 30082%, organic silicon surfactant Silwet6188%, antifoaming agent SAG15771%, disintegrant urea 5.0%, adhesive gelatin 1%, stabilizing agent Sodium Benzoate 1%, filler white carbon 100%.
4. pesticide water dispersible granules; It is 75% fly eradication amine water dispersible granules; Wherein each constituent content is by weight: fly eradication amine 75%, dispersant Morwet D-4504%, wetting agent Morwet 30282%, organic silicon surfactant Silwet4088%, silicone defoaming agent silicone emulsion 0.5%, disintegrant sodium sulphate 5.0%, adhesive polyvinylpyrrolidone 1%, stabilizing agent potassium sorbate 0.5%, filler white carbon complement to 100%.
5. pesticide water dispersible granules; It is 80% water dispersible granule of nicosulfuron; Wherein each constituent content is by weight: nicosulfuron 80%, dispersant Morwet D-5003%, wetting agent Morwet 30282%, organic silicon surfactant Silwet4086%, silicone defoaming agent SAG15771%, disintegrant urea 5.0%, adhesive polyvinylpyrrolidone 0.5%, stabilizing agent Sodium Benzoate 1%, filler white carbon complement to 100%.
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