CN109699653A - Epoxiconazole aqueous suspension agent and preparation method thereof - Google Patents
Epoxiconazole aqueous suspension agent and preparation method thereof Download PDFInfo
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- CN109699653A CN109699653A CN201910100128.8A CN201910100128A CN109699653A CN 109699653 A CN109699653 A CN 109699653A CN 201910100128 A CN201910100128 A CN 201910100128A CN 109699653 A CN109699653 A CN 109699653A
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Abstract
The invention discloses a kind of epoxiconazole aqueous suspension agents and preparation method thereof, are made of weight percent following components: epoxiconazole 10~30%, dispersing agent and wetting agent 4~7%, thickener 3~5%, defoaming agent 0.5~1%, antifreezing agent 3~6%, adjusting pH value is 5~8, and water complements to 100%；Wherein the dispersing agent is tristyrylphenol polyoxyethylene ether sulfuric acid dipersant；The wetting agent is selected from one of NP series nonylphenol polyoxyethylene ether, AEO series fatty alcohol polyoxyethylene ether, macromolecule EO-PO block copolymer, alkyl phenol polyoxyethylene ether, styrylphenol polyethenoxy ether or two or more combinations.Significantly reduce in suspending agent processing that (cold) the storage stability of heat is poor, foam is more, automatic bad dispersibility and the problems such as Ostwald ripening.
Description
Technical field
The present invention relates to a kind of broad-spectrum fungicides, specifically, being about a kind of epoxiconazole aqueous suspension agent and its system
Preparation Method.
Background technique
Epoxiconazole is a kind of absorbability triazole bactericidal agent, fluorine is contained in structure, activity is high, and toxicity is low, and wide sterilization spectrum is held
The effect phase is longer, can by inhibit pathogen ergosterol synthesis, hinder germ cell wall formation, and be currently known
Fungicide compare, can more effectively inhibit disease fungus.All fourth matter enzymatic activitys that crop can be improved simultaneously, lead to fungi haustorium
It shrinks, inhibits germ intrusion, which becomes unique in triazole bactericidal agent.
The epoxiconazole dosage form of domestic market sale is mainly missible oil, water dispersible granules, aqueous suspension agent.Because missible oil is wanted
Using a large amount of organic solvent, a large amount of organic solvent causes pollution to environment, with people's environmental consciousness and security knowledge
Continuous enhancing, the formulations of pesticide develop towards water baseization, thus pesticide suspension concentrate increasingly by the favour of people and
Pay attention to.Agricultural chemicals suspension agent be by be slightly soluble in water or solid-state raw medicine not soluble in water and various auxiliary agents in an aqueous medium disperse homogenizing and
The multiphase dispersion of formation, belongs to thermodynamic unstable system.Due to being to use water as solvent, missible oil and wettable are avoided
Pulvis can exempt the trouble that Multiple Pesticides active constituent uses preceding bucket to mix because of environmental pollution caused by organic solvent and dust, but
It is that epoxiconazole aqueous suspension agent is easy to appear that (cold) the storage stability of heat is poor, foam is more, self-dispersing is poor, Ovshinsky is ripe in process
The problems such as change, the serious development and utilization for hindering suspending agent.
Summary of the invention
In view of the above shortcomings of the prior art, the first object of the present invention is to provide a kind of epoxiconazole aqueous suspension agent, this
The second of invention is designed to provide the preparation method of this kind of epoxiconazole aqueous suspension agent, significantly reduces hot (cold) in suspending agent processing
Store that stability is poor, foam is more, automatic bad dispersibility and the problems such as Ostwald ripening.
In order to realize above-mentioned the first purpose of technology, present invention employs the following technical solutions: a kind of epoxiconazole aqueous suspension
Agent, it is characterised in that: be made of weight percent following components:
Wherein the dispersing agent is tristyrylphenol polyoxyethylene ether sulfuric acid dipersant；
The wetting agent is selected from NP series nonylphenol polyoxyethylene ether, AEO series fatty alcohol polyoxyethylene ether, macromolecule
One of EO-PO block copolymer, alkyl phenol polyoxyethylene ether, styrylphenol polyethenoxy ether are two or more
Combination.
Using the above scheme: epoxiconazole is prepared as a kind of systemic fungicide with protection and therapeutic effect
Organic solvent is not used, the pollution to environment is reduced using water as dispersed phase at aqueous suspension agent.Aqueous suspension agent uses water
As the dispersed phase of system, the dimethylbenzene of traditional missible oil is replaced with water, the epoxiconazole missible oil of the organic solvents such as toluene processing can be with
The viscosity for significantly reducing aqueous suspension agent increases its stability and reduces the pollution to environment；Granule dust is not generated, convenient for adding
The harm to worker can be reduced while work.
The present invention is using tristyrylphenol polyoxyethylene ether sulfuric acid dipersant as auxiliary agent, hydrophobic main chain Long carbon chain
It is adsorbed on epoxiconazole particle surface, prevents from reuniting between particle；Sulfate group and ethylene oxide hydrophilic radical and water isopolarity
Solvent has good compatibility, and so as to stable for extended periods of time, viscosity is effectively reduced, improves suspensibility.With NP series nonyl
Base phenol polyethenoxy ether, AEO series fatty alcohol polyoxyethylene ether, macromolecule EO-PO block copolymer, alkylphenol-polyethenoxy
The wetting agents such as ether, styrylphenol polyethenoxy ether compounding, interaction are complemented each other, and are formed inclusion property aqueous suspension, are made agriculture
Migration is small in the soil for medicine, does not pollute to underground water, produces and uses safety.It significantly reduces hot (cold) in suspending agent processing
Store that stability is poor, foam is more, automatic bad dispersibility and the problems such as Ostwald ripening.Prepare stable epoxiconazole aqueous suspension agent.This
Invention epoxiconazole aqueous suspension agent viscosity is low, and room temperature topples over residue < 0.5%, partial size at 3 μm hereinafter, cloud disperses in water,
95% or more suspensibility；Heat storage stability is high, and viscosity change is little after heat storage, topples over residue < 1.0%, and suspensibility is high.
Additive amount by controlling thickener can effectively control the viscosity of suspending agent, improve self-dispersing, prevent Ovshinsky
Ripening phenomenon.
In above scheme: the percentage composition of the dispersing agent is 3%-5%, and the percentage composition of wetting agent is 1%-4%.Make
Dispersion effect it is more preferable, stability is more preferable.
In above scheme: the thickener is selected from sodium carboxymethylcellulose, aluminium-magnesium silicate, hydroxymethyl cellulose, ethoxy
One or more of cellulose, methylcellulose or polyvinyl alcohol, xanthan gum XG.
In above scheme: the defoaming agent be selected from silicone oil, silicone compound, Cl0-20 saturated fat acids compound,
C8-10 at least one of the fatty alcohols.
In above scheme: the antifreezing agent is in ethylene glycol, glycerine, propylene glycol, polyethylene glycol, sorbierite or urea
It is one or more of.
In above scheme: the pH adjusting agent is in triethylamine, sodium hydroxide, ammonium hydroxide, acetic acid, citric acid or phosphoric acid
It is one or more of.
The second object of the present invention is achieved in that the preparation method of the epoxiconazole aqueous suspension agent, feature exist
In being prepared according to the following steps:
(1), deionized water, wetting agent, dispersing agent, antifreezing agent, pH adjusting agent, defoaming agent is proportionally added into be mixed
It is even, add epoxiconazole and etc. quality zirconium oxide bead, be sanded, be sanded temperature control at 40 DEG C hereinafter, partial size reaches flat
Stop being sanded behind equal partial size≤3 μm；
(2), in step 1 products therefrom, thickener is added, continues grinding and obtains epoxiconazole aqueous suspension agent.
In step (1), the revolving speed of sand milling is 1000-1500r/min.
In step (2), the revolving speed of sand milling is 500-800r/min, and the sand milling time is 5-20min.
When preparing epoxiconazole aqueous suspension agent using first plus wetting, dispersing agent etc. are ground to after certain partial size and add thickening again
Agent not only prevents the network-like structure of thickener to be destroyed under high shear, has ensured the effect of thickener, and can mention
The self-dispersing of high epoxiconazole aqueous suspension agent keeps the good of aqueous suspension agent to divide certainly while so that the viscosity of epoxiconazole is obtained control
Dissipate property and stability.
The invention has the advantages that
(1), it is compounded with the wetting agent that tristyrylphenol polyoxyethylene ether sulfuric acid dipersant and the present invention select
Epoxiconazole aqueous suspension agent is processed, improves the suspensibility of epoxiconazole aqueous suspension agent, heat storage stability, and pass through control thickener
Additive amount can effectively control the viscosity of suspending agent, improve self-dispersing, prevent Ostwald ripening phenomenon.
(2), it using novel processing technology, is used when preparing epoxiconazole aqueous suspension agent and first adds the grinding such as profit, hygroscopic water powder
Thickener is added again after to certain partial size, the network-like structure of thickener is not only prevented to be destroyed under high shear, is ensured
The effect of thickener, and the self-dispersing of epoxiconazole aqueous suspension agent can be improved, control the viscosity of epoxiconazole same
When keep aqueous suspension agent good self-dispersing and stability.
(3) aqueous suspension agent uses dispersed phase of the water as system, and the dimethylbenzene of traditional missible oil is replaced with water, and toluene etc. is organic
The epoxiconazole missible oil of solvent processing, can be significantly reduced the viscosity of aqueous suspension agent, increases its stability and reduces to environment
Pollution；Water dispersible granules are compared simultaneously, do not generate granule dust, the harm to worker can be reduced while easy to process.
(4) the wetting agent compounding selected with tristyrylphenol polyoxyethylene ether sulfuric acid dipersant and the present invention adds
Work epoxiconazole aqueous suspension agent enhances the stability of aqueous suspension agent, forms inclusion property aqueous suspension, makes pesticide migration in the soil
It is small, underground water is not polluted, produces and uses safety.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
The preparation of 1 10% tricyclazole aqueous suspension agent of embodiment
Each component content (by weight) is epoxiconazole raw drug 10%, tristyrylphenol polyoxyethylene ether sulfuric acid salinity
Powder 3% (Shanghai is big high molecular material Co., Ltd), (Shanghai is big height to macromolecule EO-PO block copolymer dispersant 1%
Molecular material Co., Ltd), thickener xanthan gum XG (2%) 3%, defoaming agent organosilicon 0.5%, (the Aladdin examination of ethylene glycol 3%
Agent Shanghai Co., Ltd), adjusting pH value with triethanolamine is 7-8.Add deionized water to l00%.
Tristyrylphenol polyoxyethylene ether sulfuric acid dipersant, macromolecule EO- is added in the first step in deionized water
After PO block copolymer dispersant, ethylene glycol, organic silicon defoamer are mixed evenly, be added epoxiconazole raw drug and etc. quality
Zirconium oxide bead is sanded, revolving speed 1200in, and temperature control is sanded at 40 DEG C hereinafter, partial size stops after reaching 3 μm of requirement <
It is sanded.
Second step is added the xanthan gum thickener that mass concentration is 2%, revolving speed is reduced in first step products therefrom
700r/min stops being sanded, obtains 10% epoxiconazole aqueous suspension agent after grinding 10min.
The key technical indexes is as follows:
Effective content: 10%；Appearance: white uniformity liquid；Average grain diameter: 2.56 μm；System stability: qualified；It freezes
Melt examination: qualified；Heat storage stability dispersibility: qualified；Dispersibility: disperse in water at cloud；Suspensibility: 97.50%.
Heat storage stabilization is referred to storing 14d at 54 ± 2 DEG C, be carried out later to its average grain diameter, suspensibility, dispersibility
Test.Average grain diameter is 2.56 μm before the present embodiment heat is store, and is 2.89 μm after heat storage；Heat storage front and back is white uniformity liquid,
Limited content is 10%；Suspensibility is 97.5% before heat is store, and is 95.31% after heat storage.Illustrate that heat storage heat storage stability is qualified.
The preparation of 2 20% epoxiconazole aqueous suspension agent of embodiment
Each component content (by weight) is epoxiconazole raw drug 20%, tristyrylphenol polyoxyethylene ether sulfate
4% (Shanghai is big high molecular material Co., Ltd)；Alkyl phenol polyoxyethylene ether 2%；Thickener sodium carboxymethylcellulose 4%,
Defoaming agent silicone compound 0.5%, antifreezing agent glycerine 4% (Aladdin reagent Shanghai Co., Ltd) adjust pH with ammonium hydroxide
Value is 7-8.Add deionized water to l00%.Specific preparation is carried out by embodiment 1.
The key technical indexes: average grain diameter is 2.62 μm before heat is store, and is 3.04 μm after heat storage；Heat storage front and back is white equal
Even liquid, limited content are 20%；Suspensibility is 96.24% before heat is store, and is 95.13% after heat storage.Illustrate heat storage stability
It is qualified.
Effective content: 20%；Appearance: white uniformity liquid；Average grain diameter: 2.62 μm；System stability: qualified；It freezes
Melt examination: qualified；Heat storage stability dispersibility: qualified；Dispersibility: disperse in water at cloud；Suspensibility: 96.24%.
The preparation of 3 30% epoxiconazole aqueous suspension agent of embodiment
Each component content (by weight) is epoxiconazole raw drug 30%, tristyrylphenol polyoxyethylene ether sulfuric acid salinity
Powder 5% (Shanghai is big high molecular material Co., Ltd)；(Shanghai is big macromolecule to styrylphenol polyethenoxy ether 2%
Materials Co., Ltd)；Thickener aluminium-magnesium silicate 5%, Cl0-20 saturated fat acids compound 1%, antifreezing agent polyethylene glycol and
Ethylene glycol 6% (Aladdin reagent Shanghai Co., Ltd), adjusting pH value with sodium hydroxide is 7-8.Add deionized water to l00%.
Specific preparation is carried out by embodiment 1.
The key technical indexes: average grain diameter is 2.83 μm before heat is store, and is 3.26 μm after heat storage；Heat storage front and back is white equal
Even liquid, limited content are 30%；Suspensibility is 95.48% before heat is store, and is 94.29% after heat storage.Illustrate heat storage stability
It is qualified.
Effective content: 30%；Appearance: white uniformity liquid；Average grain diameter: 2.83 μm；System stability: qualified；It freezes
Melt examination: qualified；Heat storage stability dispersibility: qualified；Dispersibility: disperse in water at cloud；Suspensibility: 95.48%.
Embodiment 4
The preparation of 25% epoxiconazole aqueous suspension agent
Each component content (by weight) is epoxiconazole raw drug 25%, tristyrylphenol polyoxyethylene ether sulfate
3% (Shanghai is big high molecular material Co., Ltd)；NP series nonylphenol polyoxyethylene ether 4%；Thickener hydroxyethyl cellulose
4%, defoaming agent C8-10 fatty alcohols compound 0.8%, antifreezing agent sorbierite 5% is 5-6 with lemon acid for adjusting pH value.Add
Ionized water is to l00%.Specific preparation is carried out by embodiment 1.
The key technical indexes: average grain diameter is 2.38 μm before heat is store, and is 2.59 μm after heat storage；Heat storage front and back is white equal
Even liquid, limited content are 25%；Suspensibility is 97.34% before heat is store, and is 96.73% after heat storage.Illustrate heat storage stability
It is qualified.
Effective content: 25%；Appearance: white uniformity liquid；Average grain diameter: 2.38 μm；System stability: qualified；It freezes
Melt examination: qualified；Heat storage stability dispersibility: qualified；Dispersibility: disperse in water at cloud；Suspensibility: 97.34%.
Embodiment 5
The preparation of 28% epoxiconazole aqueous suspension agent
Each component content (by weight) is epoxiconazole raw drug 28%, tristyrylphenol polyoxyethylene ether sulfate
4% (Shanghai is big high molecular material Co., Ltd)；AEO series fatty alcohol polyoxyethylene ether 2%；Thickener methylcellulose or
Polyvinyl alcohol 3%, defoaming agent C8-10 fatty alcohols compound 0.7%, antifreezing agent urea 4% are with acetic acid or phosphorus acid for adjusting pH value
5-6.Add deionized water to l00%.Specific preparation is carried out by embodiment 1.
The key technical indexes: average grain diameter is 2.79 μm before heat is store, and is 3.12 μm after heat storage；Heat storage front and back is white equal
Even liquid, limited content are 28%；Suspensibility is 97.58% before heat is store, and is 96.21% after heat storage.Illustrate heat storage stability
It is qualified.
Effective content: 28%；Appearance: white uniformity liquid；Average grain diameter: 2.79 μm；System stability: qualified；It freezes
Melt examination: qualified；Heat storage stability dispersibility: qualified；Dispersibility: disperse in water at cloud；Suspensibility: 97.58%.
It is found by embodiment, which has smaller difference when pH is 5-6 and 7-8, and properties meet
Standard, properties of product are stablized, and illustrate that this suspending agents systems is more stable under the conditions of weak acid or weak base, are suitable for different condition,
It is pervasive to answer extensively.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that；It still may be used
To modify to technical solution documented by previous embodiment, or some or all of the technical features are equal
Replacement.And these are modified or replaceed, the model for technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses, should all cover within the scope of the claims and the description of the invention.
Claims (9)
1. a kind of epoxiconazole aqueous suspension agent, it is characterised in that: be made of weight percent following components:
Wherein the dispersing agent is tristyrylphenol polyoxyethylene ether sulfuric acid dipersant；
The wetting agent is selected from NP series nonylphenol polyoxyethylene ether, AEO series fatty alcohol polyoxyethylene ether, macromolecule EO-PO
One of block copolymer, alkyl phenol polyoxyethylene ether, styrylphenol polyethenoxy ether or two or more combinations.
2. epoxiconazole aqueous suspension agent according to claim 1, it is characterised in that: the percentage composition of the dispersing agent is 3%-
5%, the percentage composition of wetting agent is 1%-4%.
3. epoxiconazole aqueous suspension agent according to claim 1 or claim 2, it is characterised in that: the thickener is selected from carboxymethyl cellulose
One of plain sodium, aluminium-magnesium silicate, hydroxymethyl cellulose, hydroxyethyl cellulose, methylcellulose or polyvinyl alcohol, xanthan gum XG
Or it is several.
4. epoxiconazole aqueous suspension agent according to claim 3, it is characterised in that: the defoaming agent is selected from silicone oil, silicone
Close object, Cl0-20 saturated fat acids compound, C8-10 at least one of the fatty alcohols.
5. epoxiconazole aqueous suspension agent according to claim 4, it is characterised in that: the antifreezing agent be selected from ethylene glycol, glycerine,
One or more of propylene glycol, polyethylene glycol, sorbierite or urea.
6. epoxiconazole aqueous suspension agent according to claim 5, it is characterised in that: the pH adjusting agent is selected from triethylamine, hydrogen-oxygen
Change one or more of sodium, ammonium hydroxide, acetic acid, citric acid or phosphoric acid.
7. the preparation method of epoxiconazole aqueous suspension agent described in any one of claims 1-6, which is characterized in that according to the following steps
Preparation:
(1), deionized water, wetting agent, dispersing agent, antifreezing agent, pH adjusting agent, defoaming agent is proportionally added into be mixed evenly,
Add epoxiconazole and etc. quality zirconium oxide bead, be sanded, be sanded temperature control at 40 DEG C hereinafter, partial size reaches average grain
Stop being sanded behind diameter≤3 μm；
(2), in step (1) products therefrom, thickener is added, continues grinding and obtains epoxiconazole aqueous suspension agent.
8. the preparation method of epoxiconazole aqueous suspension agent according to claim 7, it is characterised in that: in step (1), sand milling turns
Speed is 1000-1500r/min.
9. the preparation method of epoxiconazole aqueous suspension agent according to claim 8, it is characterised in that: in step (2), sand milling turns
Speed is 500-800r/min, and the sand milling time is 5-20min.
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