CN101642095A - Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof - Google Patents
Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof Download PDFInfo
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- CN101642095A CN101642095A CN200810140984A CN200810140984A CN101642095A CN 101642095 A CN101642095 A CN 101642095A CN 200810140984 A CN200810140984 A CN 200810140984A CN 200810140984 A CN200810140984 A CN 200810140984A CN 101642095 A CN101642095 A CN 101642095A
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- triazolone
- microemulsion
- ethylthio sulfonate
- ethyl ethylthio
- organic solvent
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Abstract
The invention discloses composite bactericidal microemulsion containing triadimefon and ethylicin, which consists of the following components in percentage by weight: 5 to 15 percent of triadimefon, 1to 5 percent of ethylicin, 5 to 25 percent of organic solvent, 15 to 25 percent of primary surfactant, 3 to 10 percent of cosurfactant, and the balance of water. The invention also discloses a methodfor preparing the microemulsion. The microemulsion is apparently transparent or almost transparent uniform liquid, has no sediments and floating oil after being diluted, has excellent cold/hot storage stability and ageing stability, high transfer efficiency, high flash point, safe production, transportation, storage and usage, less environmental pollution, low production and use cost, and high bactericidal effect.
Description
Technical field
The invention belongs to technical field of pesticide, be specifically related to a kind of composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate and preparation method thereof.
Background technology
Triazolone (triadimefon), it is peaceful to claim powder to embroider again, triadimefon, hundred bacterium ketone, hundred reasons are logical etc.Pure product are colourless crystallization, and special odor is arranged, and 82.3 ℃ of fusing points are slightly soluble in water in the time of 20 ℃, dissolve in most of organic solvent.Former powder is white to light yellow solid, and fusing point is greater than 70 ℃, and is more stable under acid and alkali condition.It is long to have efficient, wide spectrum, low-residual, the longevity of residure, the characteristics that interior absorption is strong.Be easy to be absorbed and conduction in vivo by plant corpus.Effects such as having protection concurrently, treat, root out and fumigate.Belong to the hypotoxicity bactericide.Former medicine rat acute per os LD
50Be 1000～1500 milligrams/kilogram, rat is through skin LD
50＞1000 milligrams/kilogram.Skin is had slight spread effect, and no carcinogenic, teratogenesis, mutagenesis are medium to toxicity in fish in test dose, and be harmless to honeybee and birds.Be widely used in powdery mildew and the rust of crops such as control cereal, vegetables, fruit tree, dressing seed can be prevented and treated the powdery mildew of spring, winter wheat and spring barley, the spring barley loose kernel smut, wheat stalk rot and stripe disease of barley all have control efficiency to maize head fringe blade tip rot etc.Can with various sterilization agent, insecticide and herbicide mixture, have huge Application and Development potentiality.
S-Ethyl ethylthio sulfonate (ethylicin) claims allicin, antibacterial agent 402 again, for colourless or little yellow oily liquid, the garlic stink is arranged, and high volatility has severe corrosive, dissolves in multiple organic solvent, and solvability is 1.2% in the water.140 ℃ of decomposition, 56 ℃ of boiling points (0.2mmHg), storage at normal temperature is more stable.It is a kind of broad-spectrum germicide.Its bactericidal mechanism is to contain in (S-S=O=O) group and the thalline molecule in its molecular structure-substance reaction of SH base, thereby suppresses the thalline eubolism.Medium to higher mammal toxicity.Big white mouse acute oral LD
50Be 140 mg/kg, skin is had spread effect.Plant growing is had spread effect, fast through the seed sprouting of treated with same, the growth of seedling stalwartness.
The main formulation of triazolone and S-Ethyl ethylthio sulfonate preparation is missible oil and wetting powder at present, and wherein the emulsifiable concentrate production process need consume poisonous in a large number, inflammable organic solvent, is unfavorable for safety in production, transportation and storage; The volatilization meeting of organic solvent works the mischief to environment in the use in addition.The weak point that wetting powder in use exists is when the preparation flushing liquor medicinal powder to take place easily to fly upward, and operating personnel is worked the mischief remaining medicinal powder contaminated environment in the packaging bag.In addition, the emulsifiable concentrate pesticide that with oil is medium sprays in the process being mixed with the aqueous solution, and agricultural chemicals is dispersed in the aqueous solution with the situation of the little liquid pearl of missible oil, is unfavorable for the wetting of blade face after spraying application to corps leaf surface, thereby influence drug effect, the drug effect of wetting powder also is subjected to the influence of particle size.Along with the public to the enhancing of environmental consciousness and to the demand of environmental protection agricultural chemicals, some are that the aqueous pesticide of solvent becomes formulations of pesticide main development tendency from now on water.
Summary of the invention
The objective of the invention is to overcome the triazolone of existing missible oil and wetting powder and the deficiency that the S-Ethyl ethylthio sulfonate bactericide exists, a kind of be beneficial to safety in production, transportation and storage are provided; The composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate that environmental pollution is little, drug effect is high.The present invention also provides the preparation method of this microemulsion.
The objective of the invention is to be achieved through the following technical solutions:
The composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate of the present invention, this microemulsion is composed of the following components by weight percentage:
Triazolone: 5%～15%;
S-Ethyl ethylthio sulfonate: 1%～5%;
Organic solvent: 5%～25%;
First type surface activating agent: 15%～25%;
Cosurfactant: 3%～10%;
Water: add to 100%.
Described organic solvent is selected from a kind of in cyclohexane, cyclohexanone, carrene, butanols, propyl alcohol, amylalcohol, toluene, dimethylbenzene, acetate, the ethyl acetate or the mixture of any two kinds or any two or more materials in the middle of them.
Described surfactant is selected from the mixture of any two kinds or any two or more materials in polyoxyethylene nonylphenol ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitol acid anhydride mono fatty acid ester, anhydrous sorbitol APEO stearate, Brij30, glyceryl monooleate, glycerin monostearate, neopelex, sldium lauryl sulfate, calcium stearate, the alkyl benzene calcium sulfonate.
Described cosurfactant is selected from a kind of in ethanol, normal propyl alcohol, n-butanol, n-amyl alcohol, isoamyl alcohol, glycerine, ethyl acetate, acetate, the n-butyric acie or the mixture of any two kinds or any two or more materials in the middle of them.
The preparation method of composite bactericidal microemulsion who contains triazolone and S-Ethyl ethylthio sulfonate is as follows: under the room temperature condition, by weight percentage: triazolone: 5%～15%; S-Ethyl ethylthio sulfonate: 1%～5%; Organic solvent: 5%～25%; First type surface activating agent: 15%～25%; Cosurfactant: 3～10%; Water: add to 100%, take by weighing a component; Earlier triazolone, S-Ethyl ethylthio sulfonate and organic solvent are stirred to dissolving fully, again surfactant, cosurfactant are mixed and slowly add above-mentioned mixed liquor after stirring is made into emulsifier, add the water mixing then and obtain mixed liquor, be stirred well to the microemulsion of transparent and homogeneous.
Microemulsion is to be matrix with water, by former medicine dissolving, and in the presence of surfactant and cosurfactant, the isotropism of spontaneous formation, optical clear or translucent Thermodynamically stable dispersion.The use of toxic organic solvent is avoided or significantly reduced to microemulsion, suppressed the volatilization of agricultural chemicals steam, reduced environmental pollution.When spraying, excitant and stink alleviate, and reduce the murder by poisoning to production, user and environment, are beneficial to the improvement of eco-environmental quality.Simultaneously, product is easily packed, and does not fire and does not explode, and production, transportation, storage and safe in utilization are called as " environment friendly agricultural preparation ".Because its auxiliary agent content height, emulsified particles is little, and the opening up of its soup, wetting, infiltration and filming function are better than cream preparation, so the effective rate of utilization height of its soup, and its drug effect is 1.2～1.5 times of cream preparation under identical effective dose.
The present invention substitutes a large amount of poisonous inflammable benzene kind solvents by experiment sieving and research to solvent, emulsifier, builder etc. with water, reduces product toxicity and production cost, reduces environmental pollution, improves and produces and the storing safety; Microemulsion emulsifier large usage quantity, it is little to convert water dilution back active ingredient particle, opening up of soup, wetting permeability is strong, the utilization rate of active components height, builder reduces the active ingredient actual amount, improves preventive effect and reduces the purpose of preventing and treating cost thereby play favourable with the body surface resistance in the body of elimination pest in addition.Compare with prior art, the concrete advantage of the present invention is as follows:
1, microemulsion outward appearance of the present invention is transparent or approaching transparent uniform liquid, and dilution back emulsion does not have precipitation and oil slick, and hot and cold storage stability and ageing stability tool are good, transmission efficiency height, flash-point height, production, transportation, storage and safe in utilization.
2, reduced environmental pollution, aromatic solvent content and only contains 5%～30% in the microemulsion up to 50%～70% in the conventional cream preparation, and poisonous, inflammable organic solvent amount significantly reduces, thereby has reduced the pollution to environment.
3, reduce production and use cost, improved drug effect.Because micro-emulsion pesticide is dispersion medium with water, the aboundresources cheapness.In addition, microemulsion is compared with missible oil, contains the higher surface activity agent concentration in the microemulsion system, even when being mixed with weak solution, surfactant concentrations is still higher relatively, makes that the surface tension of the aqueous solution is very low, helps the formation of the little droplet of high-ratio surface.Just, make that soup is easy to sprawl on the blade face because the low surface tension of agricultural chemicals dilution has reduced soup and the plant leaf surface contact angle that has oiliness.Simultaneously,, reduced the bounce-back of droplet on the blade face, reduced the drift of active ingredient, improved result of use or minimizing and spray consumption because the soup droplet is little.Therefore, its production and use cost are all lower.
Through test, every mu of active ingredient 8g of microemulsion of the present invention sprays the control wheat powdery mildew, and 15 days protection effects can reach 90.1% behind the medicine, and the cream preparation preventive effect of same dose has only 70.5%.Illustrate that microemulsion drug effect of the present invention obviously is better than cream preparation.
4, improved plant plugged ear survival rate.The codiaeum variegatum cuttage survival rate is had obvious facilitation, and the plugged ear survival rate can reach 95%, and has only 80% to the wettable powder with dosage, illustrates that microemulsion drug effect of the present invention obviously is better than wettable powder.Rationally use this product can stimulate crop growth, short root strong sprout, reach the purpose of increasing both production and income.
Embodiment
Below in conjunction with embodiment the present invention is made more specific description, the percentage in the example is percetage by weight.
Embodiment 1
Select following prescription: triazolone 5%; S-Ethyl ethylthio sulfonate 2%; Cyclohexanone 7%; Polyoxyethylene nonylphenol ether 12%; Alkyl benzene calcium sulfonate 3%; N-butanol 9%; Water 64%.
Preparation method: under the room temperature condition, 5kg triazolone, 2kg S-Ethyl ethylthio sulfonate are dissolved with the 7kg cyclohexanone, simultaneously 9kg n-butanol, 3kg alkyl benzene calcium sulfonate (ABS-Ca) and 12kg polyoxyethylene nonylphenol ether (Tx-10) are made into emulsifier, after the two mixes under stirring condition, stir and slowly add 64kg water down, fully stirred 30 minutes, get the homogeneous phase prescribed liquid, be 5% triazolone+2% S-Ethyl ethylthio sulfonate microemulsion.
Embodiment 2
Select following prescription: triazolone 8%; 3% S-Ethyl ethylthio sulfonate; Cyclohexanone 10%; Isoamyl alcohol 7%; Polyoxyethylene sorbitol acid anhydride mono fatty acid ester (Tween-20) 17%; Alkyl benzene calcium sulfonate (ABS-Ca) 7%; Water 48%.
Press the preparation of embodiment 1 method, be 8% triazolone+3% S-Ethyl ethylthio sulfonate microemulsion.
Embodiment 3
Select following prescription: triazolone 10%; 2.5% S-Ethyl ethylthio sulfonate; Cyclohexanone 12.5%; Ethanol 7.5%; Polyoxyethylene nonylphenol ether (Tx-10) 16%; G alkyl benzene calcium sulfonate (ABS-Ca) 7.5%; Water 44%.
Press the preparation of embodiment 1 method, be 15% triazolone+3% S-Ethyl ethylthio sulfonate microemulsion.
Embodiment 4～30
Press the proportioning shown in the table 1, earlier triazolone, S-Ethyl ethylthio sulfonate and organic solvent are stirred to dissolving fully, add the water mixing then and obtain mixed liquor, surfactant, cosurfactant are mixed slowly add above-mentioned mixed liquor after stirring is made into emulsifier again, be stirred well to the microemulsion of transparent and homogeneous.
Used wet concentration is from the water of distilled water, running water or the various different hardness of laboratory system in the embodiments of the invention.
Test the test of 1. low-temperature stabilities
Get the composite bactericidal microemulsion 20mL that contains triazolone and S-Ethyl ethylthio sulfonate of the present invention, in the clear, colorless glass port grinding bottle of packing into, sealing is placed on constant temperature 12h under-8 ± 2 ℃ of conditions, if become turbid, layering, crystallization, liquid crystal, one of them person of gelling be for defective.If do not have muddiness, layering, crystallization, liquid crystal, gelling appearance, then placed 0 ℃ of constant temperature 7 days, nothing muddiness, layering, crystallization, liquid crystal, gelling person are qualified.
Product percent of pass in the embodiment of the invention is 96.7%.
Test the test of 2. heat storage stabilities
Getting the composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate of the present invention and pack in the 10mL ampere bottle, placed under 54 ± 2 ℃ of conditions constant temperature 14 days, is qualified if do not have muddiness, layering, crystallization, liquid crystal, gelling person.
The qualification rate of the product in the embodiment of the invention is 100%.
The test 3. control wheat powdery mildew tests of pesticide effectiveness
15% triazolone+3% S-Ethyl ethylthio sulfonate the microemulsion of invention is evenly sprayed the control wheat powdery mildew for 1000 times, every mu of active ingredient 8g, emulsifiable concentrate with same dose compares, and 15 days protection effects can reach 90.1% behind the medicine, and the cream preparation preventive effect of same dose has only 70.5%.Illustrate that microemulsion drug effect of the present invention obviously is better than cream preparation.
Test 4. codiaeum variegatum cuttages test
The codiaeum variegatum cuttage survival rate is had obvious facilitation, and the plugged ear survival rate can reach 95%, and has only 80% to the wettable powder with dosage, illustrates that microemulsion drug effect of the present invention obviously is better than wettable powder.Rationally use this product can stimulate crop growth, short root strong sprout, reach the purpose of increasing both production and income.
The proportioning of each component (Kg) among table 1 embodiment
Continuous table 1
Continuous table 1
Claims (5)
1. composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate, it is characterized in that: this microemulsion is composed of the following components by weight percentage:
Triazolone: 5%～15%;
S-Ethyl ethylthio sulfonate: 1%～5%;
Organic solvent: 5%～25%;
First type surface activating agent: 15%～25%;
Cosurfactant: 3%～10%;
Water: add to 100%.
2. the composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate according to claim 1 is characterized in that: described organic solvent is selected from a kind of in cyclohexane, cyclohexanone, carrene, butanols, propyl alcohol, amylalcohol, toluene, dimethylbenzene, acetate, the ethyl acetate or the mixture of any two kinds or any two or more materials in the middle of them.
3. the composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate according to claim 1 and 2 is characterized in that: described first type surface activating agent is selected from the mixture of any two kinds or any two or more materials in polyoxyethylene nonylphenol ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitol acid anhydride mono fatty acid ester, anhydrous sorbitol APEO stearate, Brij30, glyceryl monooleate, glycerin monostearate, neopelex, sldium lauryl sulfate, calcium stearate, the alkyl benzene calcium sulfonate.
4. the composite bactericidal microemulsion that contains triazolone and S-Ethyl ethylthio sulfonate according to claim 3 is characterized in that: described cosurfactant is selected from a kind of in ethanol, normal propyl alcohol, n-butanol, n-amyl alcohol, isoamyl alcohol, glycerine, ethyl acetate, acetate, the n-butyric acie or the mixture of any two kinds or any two or more materials in the middle of them.
5. the described preparation method who contains the composite bactericidal microemulsion of triazolone and S-Ethyl ethylthio sulfonate of claim 1 is characterized in that: under the room temperature condition: triazolone: 5%～15% by weight percentage; S-Ethyl ethylthio sulfonate: 1%～5%; Organic solvent: 5%～25%; First type surface activating agent: 15%～25%; Cosurfactant: 3～10%; Water: add to 100%, take by weighing a component; Earlier triazolone, S-Ethyl ethylthio sulfonate and organic solvent are stirred to dissolving fully, again surfactant, cosurfactant are mixed and slowly add above-mentioned mixed liquor after stirring is made into emulsifier, add the water mixing then and obtain mixed liquor, be stirred well to the microemulsion of transparent and homogeneous.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200810140984A CN101642095A (en) | 2008-08-08 | 2008-08-08 | Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof |
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| CN200810140984A CN101642095A (en) | 2008-08-08 | 2008-08-08 | Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108124888A (en) * | 2018-01-22 | 2018-06-08 | 孙淑珍 | A kind of triazolone microemulsion and preparation method thereof |
| CN109757486A (en) * | 2019-02-26 | 2019-05-17 | 深圳市五谷网络科技有限公司 | A kind of citrus moss prevention and treatment composition |
| CN109997846A (en) * | 2019-04-12 | 2019-07-12 | 浙江禾本科技有限公司 | A kind of Recompounded pesticide and preparation method thereof for treating powdery mildew of strawberry |
| CN110623006A (en) * | 2019-10-15 | 2019-12-31 | 安徽省益农化工有限公司 | Bactericide containing triazolone and application thereof |
| CN111053082A (en) * | 2019-10-08 | 2020-04-24 | 海南正业中农高科股份有限公司 | Composition containing ethylicin and difenoconazole and application thereof |
| CN115191430A (en) * | 2022-06-02 | 2022-10-18 | 中国科学院化学研究所 | Application of biomass-based surfactant system as auxiliary agent in improving effective utilization rate of pesticide |
-
2008
- 2008-08-08 CN CN200810140984A patent/CN101642095A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108124888A (en) * | 2018-01-22 | 2018-06-08 | 孙淑珍 | A kind of triazolone microemulsion and preparation method thereof |
| CN109757486A (en) * | 2019-02-26 | 2019-05-17 | 深圳市五谷网络科技有限公司 | A kind of citrus moss prevention and treatment composition |
| CN109997846A (en) * | 2019-04-12 | 2019-07-12 | 浙江禾本科技有限公司 | A kind of Recompounded pesticide and preparation method thereof for treating powdery mildew of strawberry |
| CN111053082A (en) * | 2019-10-08 | 2020-04-24 | 海南正业中农高科股份有限公司 | Composition containing ethylicin and difenoconazole and application thereof |
| CN110623006A (en) * | 2019-10-15 | 2019-12-31 | 安徽省益农化工有限公司 | Bactericide containing triazolone and application thereof |
| CN115191430A (en) * | 2022-06-02 | 2022-10-18 | 中国科学院化学研究所 | Application of biomass-based surfactant system as auxiliary agent in improving effective utilization rate of pesticide |
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Application publication date: 20100210 |