CN1502237A - Diniconazole microemulsion and preparation process thereof - Google Patents

Abstract

The present invention relates to a microemulsion dosage using diniconazole as active component and its preparation method. Its composition includes (wt%) 5%-10% of diniconazole, 15%-25% of surfactant, 15%-35% of organic solvent, 5%-15% of cosolvent, and the rest is water.

Description

Alkene azoles alcohol microemulsion and preparation method thereof

Technical field

The present invention relates to alkene azoles alcohol micro-emulsion form and preparation method thereof.

Background technology

Alkene azoles alcohol (diniconazole) as active ingredient belongs to triazole type broad spectrum activity systemic fungicide.Alkene azoles alcohol is by reports such as H.Takano, and Sumitomo Chemical Co. and Valent develop.The alkene azoles alcohol mechanism of action is the demethylation effect that suppresses in the ergosterol biosynthesis.Have protection and therapeutic action.Effective to white powder germ, rest fungus, bunt germ, smut bacterium, black star germ etc., leaf spot fungi, tail spore mould, ball chamber bacterium, sclerotinite, the living beak spore of standing grain bacterium, Penicillium notatum, rhizoctonia, string spore cup fungi, black rot etc. are also had suppress effect preferably in addition.Foliar spray is mainly used in control cereal class powdery mildew, leaf rust, yellow rust, wheat glume blight, leaf spot, leaf spot blight, net blotch of barley, grape powdery mildew and black rot, apple, pear scab and powdery mildew, leaf spot of peanut and sigatoka etc.Seed treatment is used to prevent and treat bunt, smut and the stripe disease of cereal crop.

The existing wetting powder of alkene azoles alcohol formulation, missible oil etc.US5905072A discloses and has been used to prepare the adjuvant of stablizing microemulsion, wherein mentions alkene azoles alcohol as active component, but the concrete prescription of unexposed alkene azoles alcohol microemulsion, and the complicated defective of this microemulsion adjuvant existence prescription, be unfavorable on producing, using.

(microemulsion, ME) be is matrix with water to microemulsion, utilizes physicochemical liquid-in-liquid dispersions system theoretical and that method is prepared is efficient, storing safety, low pollution novel form.This formulation oil bead diameter is 10～100nm, uses no or little organic solvent, cost and missible oil quite or lower slightly, active ingredient dispersity height, drug effect is higher by 10%～30% than missible oil usually.The general water content of microemulsion has not only been saved a large amount of organic solvents more than 40%, and has alleviated the pressure to environment greatly, and is significant for protection Agro-ecology balance, more helps the sustainable development of agricultural.

Summary of the invention

The purpose of this invention is to provide a kind of is the microemulsion formulation of active ingredient with alkene azoles alcohol.

Another object of the present invention provides the preparation method of described preparation.

The said preparation active constituent content is 1%～50%, is preferably 5%～10%.Said composition also comprises 15%～25% surfactant in addition, 15%～35% organic solvent, and cosolvent 5%～15%, surplus is a water.

The surfactant that is fit to is selected from nonionic, anion and the mixed surfactant that No. 500,0201B, 0203B, 0204C, 2201, OP series, farming breast etc. have the well emulsify performance.

The organic solvent that is fit to is selected from dimethylbenzene, toluene and cyclohexanone etc.

The cosolvent that is fit to is selected from C ₁-C ₄-alcohols, for example methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol and the tert-butyl alcohol, particular methanol and ethanol.

The present invention can also contain other auxiliary element such as stabilizing agent, antifreezing agent, urge bleeding agent etc.

Antifreezing agent can be for example ethylene glycol, propane diols, glycerine, polyethylene glycol, sorbierite, urea, sucrose, glucose and one or more mixture thereof.

Short bleeding agent can be for example azone, lauryl alcohol sodium sulphate, sodium lignin sulfonate, alkylphenol polyoxyethylene etc.

This microemulsion formulation prepares in a known manner, normally active ingredient is fully mixed with components such as surfactant, solvent and water.

Formulation of the present invention is a microemulsion, and the method for optimizing of using said preparation is a foliage-spray, and formulation rate is 100～150g a.i./ha usually.

Embodiment

The present invention describes with the following example, but does not limit the present invention.

One: 5% microemulsion of example of formulations

Alkene azoles alcohol 5%

Cyclohexanone 25%

Ethanol 10%

OP-21 8％

2201 8％

Water to 100%

Alkene azoles alcohol dissolves fully with organic solvent, adds other compositions again, evenly mixes, and adds entry at last, can be made into microemulsion after fully stirring.Can be diluted to the clear liquid of any concentration to water.

Adopt the step identical, prepare following example of formulations with example of formulations one.

Two: 5% microemulsions of example of formulations

Alkene azoles alcohol 5%

Dimethylbenzene 13%

Cyclohexanone 10%

Methyl alcohol 10%

OP-21 10％

2201 10％

The newborn 500# 2% of farming

Water to 100%

Three: 8% microemulsions of example of formulations

Alkene azoles alcohol 8%

Cyclohexanone 30%

Ethanol 10%

OP-10 12％

2201 10％

Water to 100%

Four: 8% microemulsions of example of formulations

Alkene azoles alcohol 8%

Dimethylbenzene 15%

Cyclohexanone 12%

Ethanol 10%

OP-21 10％

2201 10％

The newborn 500# 2% of farming

Water to 100%

The microemulsion physicochemical property of preparation is:

Outward appearance: as clear as crystal single-phase liquid;

Transparency temperature zone: 0～60 ℃;

Low-temperature stability: following 2 weeks layering, crystallization do not occur at 0 ℃;

Stability of emulsion: with the water-reducible emulsion-stabilizing of any ratio;

Ageing stability: normal temperature is stable down.

Biologicall test embodiment one: microemulsion formulation is to the peanut Cercospora bacteria Toxicity Determination

Assay method: use the PDA medium culture for the examination pathogen.Get in the 50mL medium after dilute liquid medicine 0.5mL is added to fusion, after fully shaking up, on average pour in the culture dish of 3 90mm.After treating the medium condensation, (φ=3mm) in culture dish central authorities places the biochemical incubator of (25 ± 1) ℃ to cultivate then, when treating that mycelium has just covered with in the blank culture dish, calculates inhibiting rate to handle the mycelium diameter to insert cultured pathogen piece.

Microemulsion formulation the results are shown in Table 1 to peanut Cercospora bacteria (Cercospora arachidicola Hori) Toxicity Determination.

Table 1 5% alkene azoles alcohol microemulsion is to the toxicity test of peanut Cercospora asparagagas

Reagent agent virulence regression equation EC ₅₀(mg/L) EC ₉₀(mg/L) correlation coefficient relative virus force index

12.5% alkene azoles alcohol WP Y=5.957+0.957x 0.100 2.196 0.9832

5% alkene azoles alcohol ME Y=6.066+0.858x 0.057 1.781 0.9949 1.75

Measurement result shows, EC ₅₀Or EC ₉₀Reflect that all microemulsion suppresses active strong than wetting powder to peanut Cercospora bacteria, its relative virus force index microemulsion is 1.75 times of wetting powder.

Biologicall test embodiment two: microemulsion formulation is to the brown edge greyness of banana bacterium (sigatoka) Toxicity Determination

Microemulsion formulation the results are shown in Table 2 to the brown edge greyness of banana bacterium (Cercospora amusae Zimm) Toxicity Determination.

Table 2 5% alkene azoles alcohol microemulsion is to the indoor virulence of banana sigatoka leaf spot disease bacterium

Reagent agent virulence regression equation EC ₅₀(mg/L) EC ₉₀(mg/L) correlation coefficient relative virus force index

12.5% alkene azoles alcohol WP Y=5.207+0.734x 0.552 29.1 0.9930

5% alkene azoles alcohol ME Y=5.419+0.746x 0.274 14.3 0.9974 1.91

The relative virus force index microemulsion is 1.91 times of wetting powder.

Biologicall test embodiment three: microemulsion formulation is to the pear cucumerinum Toxicity Determination

Microemulsion formulation the results are shown in Table 3 to pear cucumerinum (Venturia pirina Aderh) Toxicity Determination.

Table 3 5% alkene azoles alcohol microemulsion is to the toxicity test of pear cucumerinum

Reagent agent virulence regression equation EC ₅₀(mg/L) correlation coefficient relative virus force index

12.5% alkene azoles alcohol WP Y=4.229+0.638x 16.15 0.9791

5% alkene azoles alcohol ME Y=4.498+0.500x 10.12 0.9844 1.60

The relative virus force index microemulsion is 1.60 times of wetting powder.

Claims (7)

1. microemulsion, it comprises following composition and content (by weight)

Alkene azoles alcohol 5～10%

Surfactant 15～25%

Organic solvent 15～35%

Cosolvent 5～15%

Surplus is a water.

2. according to the microemulsion of claim 1, wherein, surfactant is selected from: 0203B, 2201,0201B, 0204C, OP series and No. 500 and composition thereof.

3. according to the microemulsion of claim 2, wherein, organic solvent is selected from: dimethylbenzene, toluene and cyclohexanone.

4. according to arbitrary microemulsion of claim 1～3, wherein, cosolvent is selected from C ₁-C ₄-alcohols.

5. according to the microemulsion of claim 4, wherein, cosolvent is selected from methyl alcohol and ethanol.

6. according to the microemulsion of claim 5, wherein, surfactant is the mixture of OP series and 2201.

7. according to the microemulsion of claim 6, wherein, surfactant is an OP series, 2201 and the mixture of No. 500, farming breast.