CN108124888A - A kind of triazolone microemulsion and preparation method thereof - Google Patents
A kind of triazolone microemulsion and preparation method thereof Download PDFInfo
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- CN108124888A CN108124888A CN201810057042.7A CN201810057042A CN108124888A CN 108124888 A CN108124888 A CN 108124888A CN 201810057042 A CN201810057042 A CN 201810057042A CN 108124888 A CN108124888 A CN 108124888A
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- Prior art keywords
- triazolone
- microemulsion
- preparation
- emulsifier
- antifreeze
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
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- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of triazolone microemulsion and preparation method thereof, triazolone microemulsion contain triazolone 5 20%, solvent 5 15%, emulsifier 10 25%, antifreeze 4 10%, remaining be deionized water, the summation of raw material is 100%.Preparation method is, first triazolone is added in a heated condition after being dissolved by heating in solvent and be stirred, antifreeze and emulsifier are added in during stirring, treat above-mentioned material after mixing, accelerate mixing speed, and be slowly added to deionized water, continue thereafter with maintenance and stir and material is heated to 70 DEG C 80 DEG C, object system to be mixed switchs to O/W types from w/o type, and the bactericidal microemulsion containing triazolone is can be prepared by homogeneous liquid postcooling to room temperature.Suitable for diseases such as prevention Wheat sheath blight, powdery mildews；Method production is simple, storing safety, and to people, animal safety, effect on environment is small.
Description
Technical field
The present invention relates to a kind of agriculture chemicals fungicides more particularly to a kind of triazolone microemulsion and preparation method thereof.
Background technology
With concern of the people to living environment, it is desirable that reduce Pesticidal products and use the environmental hazard brought.To adapt to this
One social desirability in Pesticidal products exploitation, while exploitation low toxicity, efficient pesticide new variety is focused on, carries pesticidal preparations
Higher requirement is gone out, it is desirable that pesticidal preparations develop to solidification, water baseization direction.
Triazolone (Triadimefon), chemical name：1- (4- chlorophenoxies) -3,3- dimethyl -1- (1H, 1,2,4- tri-
Azoles -1- bases) -2- butanone.
Structural formula：
Empirical formula：C14H16N3O2Cl.Relative molecular mass：293.8 (based on international relative atomic masses in 1997).Physics and chemistry
Property：Colorless solid has special fragranced, 82.3 DEG C of fusing point, vapour pressure 0.02mPa (20 DEG C), 0.06mPa (25 DEG C), density
1.22 (20 DEG C), KowlogP=3.11, solubility water 64mg/L (20 DEG C), moderate is dissolved in many organic solvents, except fat hydrocarbon
In addition, dichloromethane, toluene ＞ 200, isopropanol 50-100, hexane 5-10g/L (20 DEG C) stablize, and pH3,6,9 (22 DEG C) partly decline
Phase was more than 1 year.
Action character：
It is a kind of efficient, low toxicity, low-residual, the triazole bactericidal agent that the lasting period is long, absorbability is strong.By each section of plant
After absorption, it can be conducted in plant.Have the effects that prevent to rust and powdery mildew, root out, treating, is stifling.To a variety of works
The disease of object such as Helminthosporium carbonum, wheat class moire disease, wheat leaf blight, pineapple black rot, maize head smut etc. are effectively.It is right
Fish and birds are safer.It is harmless to honeybee and natural enemy.The bactericidal mechanism principle of triazolone is extremely complex, mainly inhibits thalline
The biosynthesis of ergosterol, thus inhibit or interfere the development of thalline attachment spore and haustorium, the growth of mycelia and the shape of spore
Into.Activity is very strong in the living body, but in vitro poor effect to certain germs for triazolone.It is strong that spore is compared to the activity of mycelia.Three
Oxazolone can be with many fungicide.Insecticides (tech) ＆ Herbicides (tech) etc. now mixes current.
Patent about triazolone is concentrated mainly on is processed into breast by the mixture of triazolone or triazolone and other pesticides
Oil, wettable powder, preparation available on the market is mainly 20% missible oil, 20% wettable powder.Triazolone is processed into micro-
After emulsion, preparation cost can be largely reduced, drug effect is improved, reduces the usage amount of organic solvent and the dirt to environment
Dye so as to reduce residual of the triazolone in agricultural product, improves agricultural product quality.Therefore, " efficiently, low toxicity, safety, economy "
Triazolone microemulsion will largely substitute triazolone missible oil, and especially high added value agricultural production is produced and store in agricultural product
It plays a significant role in product production and processing.The successful development and application of triazolone microemulsion will have great social benefit and warp
Ji benefit.
Invention content
It is an object of the invention to disclose a kind of triazolone microemulsion and preparation method thereof.
Another object of the present invention is to solve the defects of above-mentioned Beijing technology or deficiency.The killing containing triazolone
The Environmental compatibility of bacterium microemulsion form is good, can embody the characteristics of triazolone is efficient, less toxic completely.
Realizing foregoing invention purpose technical solution is：It is triazolone 5-20%, solvent 5-15%, emulsifier 10-25%, freeze proof
Agent 4-10%, remaining be deionized water, the summation of raw material is 100%.
The present invention emulsifier be selected from nonylphenol polyoxyethylene ether, neopelex, calcium dodecyl benzene sulfonate,
One or more of polyoxethylene octylphenyl phenol ether.
The antifreeze of the present invention is selected from one or more of ethylene glycol, propylene glycol, glycerine, urea.
The solvent of the present invention is selected from one or more of methanol, acetone, ethyl alcohol, dimethylbenzene.
The preparation method of above-mentioned triazolone bactericidal microemulsion, which is characterized in that this method presses the original of claim 1 first
Material proportioning prepares raw material, first triazolone is added in solvent dissolves by heating in a heated condition, after triazolone fully dissolves
Be stirred, antifreeze and emulsifier added in during stirring, treats above-mentioned material after mixing, accelerate mixing speed, and slowly plus
Enter deionized water, continue thereafter with maintenance and stir and material is heated to 70 DEG C -80 DEG C, object system to be mixed switchs to O/W from w/o type
Type can be prepared by the microemulsion containing triazolone in homogeneous liquid postcooling to room temperature.
The triazolone microemulsion of the present invention is a kind of water baseization preparation, compared with prior art, the environment of dosage form
Compatibility is good, suitable for prevention Helminthosporium carbonum, wheat class moire disease, wheat leaf blight, pineapple black rot, maize head smut
Evil has germ higher control effect, and method production is simple, storing safety, and to people, animal safety, effect on environment is small.
Specific embodiment
Real row 1
5% triazolone microemulsion is prepared.5.3% kilogram of 95% triazolone active compound is weighed, adds in 5 kilograms of methanol, stirring adds
Heat makes it completely dissolved, and adds in 2 kilograms of polyoxethylene octylphenyl phenol ethers, 3 kilograms of nonylphenol polyoxyethylene ether and 1.5 under stiring
Kilogram calcium dodecyl benzene sulfonate is uniformly mixed, and is then kept stirring 2.5 kilograms of ethylene glycol of lower another addition, is existed after mixing
Deionized water is added under high-speed stirred and is assigned to 100 kg of water；It is heated to 70 DEG C after mixing, object system to be mixed turns from w/o type
For O/W types, in homogeneous liquid postcooling to room temperature to get 5% triazolone microemulsion.
Example 2
10% triazolone microemulsion is prepared.10.6 kilograms of 95% triazolone active compound is weighed, 10 kilograms of dimethylbenzene is added in, stirs
It mixes, heating makes it completely dissolved, and adds in 7 kilograms of polyoxethylene octylphenyl phenol ethers, 4 kilograms of nonylphenol polyoxyethylene ether under stiring
It with 2.5 kilograms of neopelexes, is uniformly mixed, 4 kilograms of ethylene glycol is added under stiring, after mixing in high-speed stirring
It mixes lower addition deionized water and is assigned to 100 kilograms；It is heated to 75 DEG C after mixing, object system to be mixed switchs to O/W from from w/o type
Type, in homogeneous liquid postcooling to room temperature to get 10% triazolone microemulsion.
Example 3
15% triazolone microemulsion is prepared.15.8 kilograms of 95% triazolone active compound is weighed, adds in 12 kg ethanols, is stirred,
Heating makes it completely dissolved, under stiring add in 6 kilograms of polyoxethylene octylphenyl phenol ethers, 5 kilograms of nonylphenol polyoxyethylene ether and
3.5 kilograms of neopelexes are uniformly mixed, and 4 kilograms of propylene glycol are added under stiring, after mixing in high-speed stirred
Lower addition deionized water is assigned to 100 kilograms；It is heated to 75 DEG C after mixing, object system to be mixed switchs to O/W types from from w/o type,
In homogeneous liquid postcooling to room temperature to get 15% triazolone microemulsion.
Example 4
20% triazolone microemulsion is prepared.21.1 kilograms of 95% triazolone active compound is weighed, adds in 15 kilograms of methanol, is stirred,
Heating makes it completely dissolved, and adds in 5 kilograms of polyoxethylene octylphenyl phenol ethers under stiring, 6 kilograms of nonylphenol polyoxyethylene ether and
2.5 kilograms of neopelexes are uniformly mixed, and 4 kilograms of propylene glycol are added under stiring, after mixing in high-speed stirred
Lower addition deionized water is assigned to 100 kilograms；It is heated to 75 DEG C after mixing, object system to be mixed switchs to O/W types from from w/o type,
In homogeneous liquid postcooling to room temperature to get 20% triazolone microemulsion.
Test examples 1 (preparation stability experiment)：
Stability of emulsion is tested.1mL10% triazolone microemulsions, 15% triazolone microemulsion, 20% triazolone are taken respectively
Microemulsion adds in 200mL342mg/L standard hard waters, 30 minutes is stood at 30 DEG C.Lotion keeps milky white state without grease
It suspends or solid precipitates, and can be mixed with water with arbitrary proportion.
Cold storage stability test.30mL10% triazolone microemulsions, 15% triazolone microemulsion, 20% triazolone are taken respectively
Microemulsion, sealing, which is placed in subzero 10 DEG C of refrigerators, to be freezed, and is taken out to be placed in after 24 hours and be observed at room temperature, preparation is restored by caking
It is transparent, it is repeated multiple times, it is reproducible.Separately 20% triazolone microemulsion 30mL is taken to be fitted into colourless transparent glass port grinding bottle, sealed
It is placed in 0-10 DEG C of refrigerator and refrigerates 2 weeks, preparation keeps transparent, and object solid precipitation or crystallization are precipitated.
Heat storage stability is tested.It is taken respectively by a certain amount of 10% triazolone microemulsion, 15% triazolone microemulsion, 20%
Triazolone microemulsion is fitted into vial and seals, and is stored 2 weeks under the conditions of being placed in 54 ± 2 DEG C, is weighed after taking out cooling, before storage
The sample that the quality of the pharmaceutical preparations remains unchanged afterwards detects its active constituent content.
Using the content of active ingredient triazolone in high-efficient liquid phase chromatogram technique analysis preparation.Chromatographic condition is：Chromatographic column：C18
Column；Detector：UV detector；Detection wavelength：235nm；Mobile phase：Methanol+water=75+25 (V/V)；Flow velocity：1mL/min；
Sampling volume：5uL；Quantitative approach：External standard method.
Testing result is as follows：Average resolution ratio 2.7% in 10% triazolone microemulsion；It is average in 15% triazolone microemulsion
Resolution ratio 2.5%；Average resolution ratio 2.1% in 20% triazolone microemulsion.Formulation aesthetics keep homogeneous phase transparent.Result of the test is demonstrate,proved
Bright, the microemulsion formulation heat storage stability obtained by the present invention is qualified.
Claims (5)
1. a kind of triazolone microemulsion and preparation method thereof, which is characterized in that the microemulsion contains the original of mass percent
Material：Triazolone 5-20%, solvent 5-15%, emulsifier 10-25%, antifreeze 4-10%, remaining be deionized water, raw material it is total
Be 100%.
2. the bactericidal microemulsion described in claim 1 containing triazolone, which is characterized in that the emulsifier gathers selected from nonyl phenol
One or more of ethylene oxide ether, neopelex, calcium dodecyl benzene sulfonate, polyoxethylene octylphenyl phenol ether.
3. the bactericidal microemulsion described in claim 1 containing triazolone, which is characterized in that the antifreeze be selected from ethylene glycol,
One or more of propylene glycol, glycerine, urea.
4. the bactericidal microemulsion described in claim 1 containing triazolone, which is characterized in that the solvent be selected from methanol, acetone,
One or more of ethyl alcohol, dimethylbenzene.
5. the preparation method of a kind of bactericidal microemulsion containing triazolone, which is characterized in that this method presses the raw material of claim 1 first
Proportioning prepares raw material, first triazolone is added in solvent dissolves by heating in a heated condition, it is laggard to treat that triazolone fully dissolves
Row stirring, antifreeze and emulsifier are added in during stirring, treats above-mentioned material after mixing, accelerate mixing speed, and be slowly added to
Deionized water continues thereafter with maintenance and stirs and material is heated to 70 DEG C -80 DEG C, and object system to be mixed switchs to O/W types from w/o type,
The microemulsion containing triazolone is can be prepared by homogeneous liquid postcooling to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810057042.7A CN108124888A (en) | 2018-01-22 | 2018-01-22 | A kind of triazolone microemulsion and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810057042.7A CN108124888A (en) | 2018-01-22 | 2018-01-22 | A kind of triazolone microemulsion and preparation method thereof |
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| Publication Number | Publication Date |
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| CN108124888A true CN108124888A (en) | 2018-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201810057042.7A Pending CN108124888A (en) | 2018-01-22 | 2018-01-22 | A kind of triazolone microemulsion and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101036457A (en) * | 2006-03-14 | 2007-09-19 | 北京华京五方实用纳米科技开发有限公司 | Microemulsion |
| CN101554155A (en) * | 2008-04-11 | 2009-10-14 | 北京绿色农华生物工程技术有限公司 | Triazolone microemulsion and preparation method thereof |
| CN101642095A (en) * | 2008-08-08 | 2010-02-10 | 郑州轻工业学院 | Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof |
| CN101642094A (en) * | 2008-08-08 | 2010-02-10 | 郑州轻工业学院 | Triadimefon pesticide microemulsion and preparation method thereof |
-
2018
- 2018-01-22 CN CN201810057042.7A patent/CN108124888A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101036457A (en) * | 2006-03-14 | 2007-09-19 | 北京华京五方实用纳米科技开发有限公司 | Microemulsion |
| CN101554155A (en) * | 2008-04-11 | 2009-10-14 | 北京绿色农华生物工程技术有限公司 | Triazolone microemulsion and preparation method thereof |
| CN101642095A (en) * | 2008-08-08 | 2010-02-10 | 郑州轻工业学院 | Composite bactericidal microemulsion containing triadimefon and ethylicin and preparation method thereof |
| CN101642094A (en) * | 2008-08-08 | 2010-02-10 | 郑州轻工业学院 | Triadimefon pesticide microemulsion and preparation method thereof |
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Application publication date: 20180608 |