CN1327771C - Tolclofos emulsion and its preparation method - Google Patents
Tolclofos emulsion and its preparation method Download PDFInfo
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- CN1327771C CN1327771C CNB03150664XA CN03150664A CN1327771C CN 1327771 C CN1327771 C CN 1327771C CN B03150664X A CNB03150664X A CN B03150664XA CN 03150664 A CN03150664 A CN 03150664A CN 1327771 C CN1327771 C CN 1327771C
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- methyl
- tolclofos
- tolelofos
- microemulsion
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Abstract
The present invention discloses a tolclofos-methyl microemulsion and a preparation method thereof, which is composed of the following components with certain weight percentage contents: 5% to 25% of the tolclofos-methyl, 5% to 15% of a nonionic surfactant, 5% to 15% of an anionic surfactant, 10% to 30% of solvent and water accounting for the rest amount of the tolclofos-methyl emulsion. Because the present invention is a nanometer agricultural chemical, the particle size of the emulsion is in a transition region between atom clusters and macroscopic objects, and the number of atoms on surface, surface area and surface energy can be increased fast; the number of the atoms on the surface is large, so the agricultural chemical has an unsaturated property, the physical properties and the chemical properties of the tolclofos-methyl are greatly different with the physical properties and the chemical properties of large macroscopic granules, and the tolclofos-methyl has high chemical activity. The tolclofos-methyl microemulsion of the present invention has high absorption speed and strong targeting action, the application amount of the tolclofos-methyl microemulsion is considerably reduced, so agricultural production cost is reduced; in addition, because the water is adopted as solvent, poisonous and harmful solvent, such as toluene, etc. is reduced, and environment pollution caused by the use of the agricultural chemical is reduced.
Description
Technical field
The present invention relates to a kind of plant protection product, be specifically related to a kind of microemulsion of bactericide, more specifically relate to a kind of tolelofos-methyl microemulsion and preparation method thereof.
Background technology
Tolelofos-methyl, adopted name: tolclofos-methyl (BSI, E-ISO, (m) F-ISO); Chemical name: O-2,6-two chloro-are right-tolyl O, O-dimethyl disulfide substituted phosphate.Pure product are colourless crystallization, and former medicine is colourless to the light brown solid, 78～80 ℃ of fusing points.This product is phosphorous series bactericidal agent, various germs such as Fungi Imperfecti, Basidiomycetes and Ascomycetes all there is very strong bactericidal activity, seedling blight, stalk break, snow mold etc. there are good control efficiency, have special effect as damping off to plants such as cotton, potato, beets.Because suction-operated is strong, be difficult for running off, in soil, have certain lasting period, gram spills by seed dressing, dipping and soil and uses.
Tolelofos-methyl can be used for foliage spray and seed treatment effectively.Because the awkward water-soluble organic compound of tolelofos-methyl, therefore, the product of traditional tolelofos-methyl is wetting powder or missible oil, and the granularity of pulvis is big, and the absorption ratio of plant is low, be sprayed on the plant after, be detained and manifest serious, cause environmental pollution; And missible oil is owing to contain a large amount of poisonous, hazardous solvent toluene or dimethylbenzene etc., can produce greatly human body and environment during use and pollute.Therefore research and development will be that institute of agricultural sector ten minutes expected with water by the tolelofos-methyl micro emulsion formulation of dispersion medium, also be the directions that develops the green ecotypical agricultural.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of tolelofos-methyl microemulsion and preparation method thereof, to overcome the above-mentioned defective that prior art exists, satisfy the needs of relevant department.
Technical conceive of the present invention is such:
Because the awkward water-soluble organic compound of tolelofos-methyl only is made into the preparation that can be scattered in fully in the water and just can uses in agricultural production.According to the physical and chemical performance that it had, can select for use the less solvent of certain emulsifier and environmental pollution to prepare the microemulsion that can be scattered in the water, for this reason, the inventor is by a large amount of experiments, filter out the emulsifier and the solvent that can be used for preparing the tolelofos-methyl micro emulsion, proposed following technical scheme:
A kind of tolelofos-methyl microemulsion is characterized in that, component and weight percent content comprise:
Tolelofos-methyl 5～25%
Non-ionic surface active agent 5～15%
Anion surfactant 5～15%
Solvent 10～30%
Water surplus
According to the present invention, because the formation condition of micro emulsion relies on and in the adding of long-chain alcohol, the present invention also adopts C simultaneously
3～C
5Alcohol is coagent, also contains 2～8% ethylene glycol and/or 0.5～2% sodium acetate in the above-mentioned tolelofos-methyl microemulsion, to improve stability of emulsion.
Preferred content is:
Tolelofos-methyl 10～20%
Non-ionic surface active agent 6～10%
Anion surfactant 5～10%
Solvent 5～20%
Ethylene glycol 4～6%
Sodium acetate 0.8～1.5%
Water surplus
Wherein:
Said non-ionic surface active agent preferred nonionic surfactants is one or more among polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, castor oil polyoxyethylene ether, phenol derivatives polyoxyethylene/polyoxypropylene base ether, polyoxyethylene carboxylate, SYNPERONIC PE/F68, agricultural newborn 400#, 600#, 1600#, 1601#, the 1602# etc., above surfactant product is the commercially available prod, digests the product that companies such as learning Co., Ltd produces as adopting chemical plant, Lvshun, Nanjing, Nanjing petrochemical industry Co., Ltd, Liaoyang Austria.
In the preferred calcium dodecyl benzene sulfonate of said anion surfactant, sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid disodium, the sodium lignin sulfonate one or more;
A kind of in the preferred cyclohexanone of said solvent, methyl alcohol, ethanol, cyclohexane, the dichloroethane etc. and or more than one.
Tolelofos-methyl preparation of microemulsion method of the present invention comprises the steps:
Under 10～70 ℃ temperature, stirring and emulsifying thing to be mixed promptly obtains said microemulsion after becoming the liquid of homogeneous transparent with above-mentioned various definite raw materials.The product that is obtained, appearance transparent, product is stable 54 ± 1 ℃ of heat storages, and 0 ± 1 ℃ of cold storage is stable, and product is not stratified, emulsion fineness＜0.1um.
Because the present invention is a kind of nano pesticide, particle diameter is in the transitional region of cluster and macro object boundary, the atomicity on surface, surface area and surface can will increase sharply, the atomicity that is in the surface is more, have undersaturated character, the physicochemical property of tolelofos-methyl will have bigger different with big macroscopic particles, and very big chemism is arranged.The result who produces this nano effect is that tolelofos-methyl has greatly changed to the crop pest control effect.Tolelofos-methyl microemulsion of the present invention is because its grain fineness reaches nanoscale, so have and absorb fast and have extremely strong targeting, amount of application reduces greatly, has not only reduced agriculture production cost, has alleviated simultaneously because of the big environmental pollution that produces of formulation rate.
Embodiment
Embodiment 1
It is as follows to fill a prescription:
Tolelofos-methyl 20%
SYNPERONIC PE/F68 7%
Calcium dodecyl benzene sulfonate 6%
Cyclohexanone 6～8%
Ethylene glycol 4～6%
Sodium acetate 0.8～1.5%
Water surplus
In emulsion reactor, in 40 ℃ of following stirring and emulsifying, the cooling back obtains tolelofos-methyl microemulsion of the present invention when treating that solution becomes homogeneous transparent liquid with the material of said ratio.
Embodiment 2
The product of embodiment 1 carries out carrying out under low-temperature stability test and 54 ± 1 ℃ heat stabilization test (carry out according to pesticide test heat is store and cold storage is tested) at 0 ± 1 ℃ respectively according to the method for pesticidal preparations standard code and found that this product is without any oil/aqueous phase separation phenomenon, also do not have any solid and separate out, product meets the stability test requirement after after tested.
Embodiment 3
Microemulsion of the present invention is adopted " the methyl using method of bibliographical information such as agricultural chemicals commodity handbook is carried out the test of seed treatment consumption, and its result is as follows:
Table 1 20% tolelofos-methyl microemulsion control beet seedling damping off result of the test
| The medicament title | Seed dressing consumption % | Incidence of disease % | Average attack rate % | Control efficiency % | ||
| 1 district | 2 districts | 3 districts | ||||
| 20% tolelofos-methyl micro emulsion | 2.0 | 0.2 | 0.1 | 0.2 | 0.17 | 99.6 |
| 25% tolelofos-methyl micro emulsion | 3.0 | 0.00 | 0.10 | 0.00 | 0.03 | 99.9 |
| 20% tolelofos-methyl wetting powder | 3.0 | 15.68 | 17.52 | 16.47 | 16.56 | 59.79 |
| 20% tolelofos-methyl missible oil | 3.0 | 18.26 | 18.31 | 17.42 | 18.00 | 56.29 |
| Contrast | Clear water | 42.5 | 39.5 | 41.55 | 41.18 | |
Table 2 20% tolelofos-methyl microemulsion control cotton seedling blight result of the test
| The medicament title | Seed dressing consumption % | Incidence of disease % | Average attack rate % | Control efficiency % | ||
| 1 district | 2 districts | 3 districts | ||||
| 20% tolelofos-methyl micro emulsion | 1.0 | 0.22 | 0.32 | 0.37 | 0.30 | 99.0 |
| 25% tolelofos-methyl micro emulsion | 2.0 | 0.15 | 0.17 | 0.09 | 0.14 | 99.5 |
| 20% tolelofos-methyl wetting powder | 2.0 | 13.49 | 15.87 | 14.12 | 14.49 | 53.0 |
| 20% tolelofos-methyl missible oil | 2.0 | 16.57 | 17.28 | 14.88 | 16.24 | 47.35 |
| Contrast | Clear water | 32.56 | 30.11 | 29.88 | 30.85 | |
Claims (3)
1. tolelofos-methyl microemulsion is characterized in that component and weight percent content comprise:
Tolelofos-methyl 5～25%
Non-ionic surface active agent 5～15%
Anion surfactant 5～15%
Solvent 10～30%
Ethylene glycol 2～8%
Sodium acetate 0.5～2%
Water surplus.
Non-ionic surface active agent is more than one among polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, castor oil polyoxyethylene ether, phenol derivatives polyoxyethylene/polyoxypropylene base ether, polyoxyethylene carboxylate, SYNPERONIC PE/F68, agricultural newborn 400#, 600#, 1600#, 1601# or the 1602#, and anion surfactant is more than one in calcium dodecyl benzene sulfonate, sodium alkyl sulfonate, alkyl diphenyl ether disulphonic acid disodium or the sodium lignin sulfonate.
2. the tolelofos-methyl microemulsion is characterized in that component and weight percent content are
Tolelofos-methyl 10～20%
Non-ionic surface active agent 6～10%
Anion surfactant 5～10%
Solvent 5～20%
Ethylene glycol 4～6%
Sodium acetate 0.8～1.5%
Water surplus.
3. tolelofos-methyl preparation of microemulsion method according to claim 1 and 2, it is characterized in that comprising the steps: with above-mentioned various raw materials that under 10～70 ℃ temperature stirring and emulsifying thing to be mixed promptly obtains said microemulsion after becoming the liquid of homogeneous transparent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03150664XA CN1327771C (en) | 2003-08-29 | 2003-08-29 | Tolclofos emulsion and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB03150664XA CN1327771C (en) | 2003-08-29 | 2003-08-29 | Tolclofos emulsion and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1493192A CN1493192A (en) | 2004-05-05 |
| CN1327771C true CN1327771C (en) | 2007-07-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB03150664XA Expired - Fee Related CN1327771C (en) | 2003-08-29 | 2003-08-29 | Tolclofos emulsion and its preparation method |
Country Status (1)
| Country | Link |
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| CN (1) | CN1327771C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306874C (en) * | 2004-11-18 | 2007-03-28 | 上海工程技术大学 | Nuisance free seed additive for preventing vegetable sprout term disease |
| CN102337183B (en) * | 2010-07-27 | 2013-06-05 | 上海浦泰化工有限公司 | High-speed paper machine system cleaning agent and concentrated liquid thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820699A (en) * | 1987-10-13 | 1989-04-11 | Sandoz, Ltd. | Novel bactericidal use |
| JPH02295906A (en) * | 1989-05-09 | 1990-12-06 | Sumitomo Chem Co Ltd | Agricultural chemical preparation having improved odor |
-
2003
- 2003-08-29 CN CNB03150664XA patent/CN1327771C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4820699A (en) * | 1987-10-13 | 1989-04-11 | Sandoz, Ltd. | Novel bactericidal use |
| JPH02295906A (en) * | 1989-05-09 | 1990-12-06 | Sumitomo Chem Co Ltd | Agricultural chemical preparation having improved odor |
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| Publication number | Publication date |
|---|---|
| CN1493192A (en) | 2004-05-05 |
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