CN105104397A - Pyraclostrobin and metiram compound water dispersible granules and preparation method thereof - Google Patents
Pyraclostrobin and metiram compound water dispersible granules and preparation method thereof Download PDFInfo
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- CN105104397A CN105104397A CN201510623949.1A CN201510623949A CN105104397A CN 105104397 A CN105104397 A CN 105104397A CN 201510623949 A CN201510623949 A CN 201510623949A CN 105104397 A CN105104397 A CN 105104397A
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Abstract
The invention relates to the technical field of controlling grape downy mildew and provides pyraclostrobin and metiram compound water dispersible granules and a preparation method thereof. The granules are made from 5 parts of pyraclostrobin, 55 parts of metiram, 6 parts of fatty alcohol sulfate salt, 3 parts of ammonium sulfate, 2 parts of polyethylene glycol, and 29 parts of kaolin. The preparation method includes: mixing the materials, pulverizing a mixture with an ultra-micro flow pulverizer to obtain wettable powder, adding the wettable powder into a fluidized bed drying granulator, allowing granulating in a fluidized bed via aqueous solution of adhesive, allowing drying in a drier, performing screening to obtain a product, performing sampling and analyzing, and metering, packaging and storing a qualified product. When the granules are 60%, the granules compounded by mixing the materials according to the ratio 1:11 has an evident synergistic range; all preparations in mixed use according to the other ratios are beyond the evident synergistic range; the granules are reasonable in design, effective in controlling grape downy mildew and have evident synergistic effect of pyraclostrobin and metiram.
Description
Technical field
The present invention relates to downy mildew of garpe Prevention Technique field, specifically relate to a kind of pyraclostrobin and Carbatene compound water dispersible granule and preparation method thereof.
Background technology
Downy mildew is the plant disease caused by the Peronosporaceae in fungi, obligatory parasitic bacteria, mainly through air-flow, water, farming and insect transmission.Germ spore germination temperature is 6 ~ 10 DEG C, is suitable for infecting temperature 15 ~ 17 DEG C, the flowers such as tree peony, Chinese herbaceous peony, Chinese rose, chrysanthemum of mainly causing harm, it cause harm wide in variety, the scope that infects is wide, almost there is generation in the whole nation.Downy mildew is general first falls ill from lower blade, and their early stage produces the water stain shape point of light green, and scab edge is not obvious, and Later development is yellow irregular scab, and during high humidity, blade back produces the mould layer of canescence, gradually becomes Dark grey.
At present, the existing bactericide for downy mildew of garpe control, such as Chinese patent " CN101647446A " discloses one " bactericidal composition containing fluopicolide and pyraclostrobin ", adopts weight ratio to be that the fluopicolide of 1:30 ~ 10:1 and pyraclostrobin carry out composite." CN102239864A " discloses one " bactericidal composition containing dimethomorph and pyraclostrobin ", adopts weight ratio to be that the dimethomorph of 50:1 ~ 1:80 and pyraclostrobin carry out composite separately Chinese patent.
Inventor verifies through long term test, and this above-mentioned several bactericide mainly exists following defect:
1), by several concrete proportioning disclosed in above-mentioned several bactericide test, find cannot play good control efficiency to the control of downy mildew of garpe.
2), for several formulations disclosed in above-mentioned several bactericide, find through verification experimental verification the defect that all there is different problem.Such as, the wetting powder not easily dispersion suspension in water of preparation, or blocking shower nozzle, the phenomenon such as reason precipitation in sprayer, cause spray irregular.
3), composite problem, by several concrete proportioning disclosed in above-mentioned several bactericide carry out virulence test, heat storage stability test and mixture co-toxicity coefficient measure find, all cannot reach obvious synergistic effect.
Summary of the invention
An object of the present invention is to provide a kind of pyraclostrobin and Carbatene compound water dispersible granule, and this water dispersible granules is reasonable in design, good to the control efficiency of downy mildew of garpe, and can realize the notable synergistic effect of pyraclostrobin and Carbatene.
For achieving the above object, present invention employs following technical scheme:
A kind of pyraclostrobin and Carbatene compound water dispersible granule, be made up of the component of following weight portion:
Pyraclostrobin is New-type wide-spectrum bactericide, and its mechanism of action is mitochondrial respiratory inhibitor, namely by stoping electro transfer in cytochrome synthesis, has protection, treatment, blade infiltration conduction.Pyraclostrobin missible oil shows there is good control efficiency to powdery mildew of cucumber, downy mildew and banana freckle, leaf spot, stalk break etc. through field control effectiveness test result.
Carbatene is mainly used in preventing and treating vegetable downy mildew, anthracnose, brown spot etc.Be control tomato early blight and potato late blight favourable agents at present, preventive effect is respectively 80% and about 90%.Mancozeb is produced to the disease of resistance, use Carbatene instead and can receive good control efficiency.Generally do foliage spray, sprayed 1 time every 7-10 days, also can be used as seed treatment.
Pyraclostrobin of the present invention and Carbatene compound water dispersible granule, its beneficial effect shows:
1) water dispersible granules that, prepared by the present invention is all obviously better than the product prepared by other proportionings in suspensibility, wet screening test etc. and heat storage stability etc.
2), verify by experiment, pyraclostrobin and Carbatene with 1:11 proportioning mixed composite 60% time pyraclostrobin and Carbatene compound water dispersible granule, notable synergistic sphere of action can be played, and the preparation that other proportioning is mixed, all cannot reach notable synergistic sphere of action.Meanwhile, the actual toxicity of different ratio does not promote along with the enhancing of theoretical toxicity, there is no regular change between actual toxicity and theoretical toxicity.
Another object of the present invention is to the preparation method that a kind of pyraclostrobin and Carbatene compound water dispersible granule are provided; raw material is mixed; be ground into wetting powder through micro jet, add in fluid-bed drying comminutor, with the aqueous solution of adhesive; granulation in the fluid bed of 50-70 DEG C; carry out drying in dryer, after screening, obtain product, then sample analysis; after qualified, metering, packaging, warehouse-in.
The preparation method of pyraclostrobin of the present invention and Carbatene compound water dispersible granule, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
Below with reference to embodiment, the present invention is described in detail.But; embodiment content is only citing made for the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
One, the preparation of pyraclostrobin and Carbatene compound water dispersible granule, and testing result, the heat storage stability result of the test of all technical of water dispersible granules prepared by each embodiment.
Embodiment 1
60% pyraclostrobin and Carbatene compound water dispersible granule, each component and weight portion as follows:
| Composition | Weight portion |
| Pyraclostrobin | 5 |
| Carbatene | 55 |
| Fatty alcohol sulfate salt | 6 |
| Ammonium sulfate | 3 |
| Polyethylene glycol | 2 |
| Kaolin | 29 |
Preparation method: raw material is mixed; wetting powder is ground into through micro jet; add in fluid-bed drying comminutor; with the aqueous solution of adhesive, granulation in the fluid bed of 50-70 DEG C, carries out drying in dryer; product is obtained after screening; then sample analysis, after qualified, metering, packaging, warehouse-in.
Embodiment 2
61% pyraclostrobin and Carbatene compound water dispersible granule, each component and weight portion as follows:
| Composition | Weight portion |
| Pyraclostrobin | 5 |
| Carbatene | 56 |
| Fatty alcohol sulfate salt | 7 |
| Ammonium sulfate | 2 |
| Polyethylene glycol | 3 |
| Kaolin | 27 |
Preparation method is with embodiment 1.
Embodiment 3
59% pyraclostrobin and Carbatene compound water dispersible granule, each component and weight portion as follows:
| Composition | Weight portion |
| Pyraclostrobin | 5 |
| Carbatene | 54 |
| Fatty alcohol sulfate salt | 5 |
| Ammonium sulfate | 1 |
| Polyethylene glycol | 1 |
| Kaolin | 34 |
Preparation method is with embodiment 1.
Embodiment 4
58% pyraclostrobin and Carbatene compound water dispersible granule, each component and weight portion as follows:
| Composition | Weight portion |
| Pyraclostrobin | 3 |
| Carbatene | 55 |
| Fatty alcohol sulfate salt | 5 |
| Ammonium sulfate | 4 |
| Polyethylene glycol | 3 |
| Kaolin | 30 |
Preparation method is with embodiment 1.
Embodiment 5
62% pyraclostrobin and Carbatene compound water dispersible granule, each component and weight portion as follows:
| Composition | Weight portion |
| Pyraclostrobin | 7 |
| Carbatene | 55 |
| Fatty alcohol sulfate salt | 7 |
| Ammonium sulfate | 2 |
| Polyethylene glycol | 3 |
| Kaolin | 26 |
Preparation method is with embodiment 1.
Pyraclostrobin prepared by embodiment 1 ~ 5 and Carbatene compound water dispersible granule, the testing result of product all technical is as shown in table 1, and product heat storage stability result of the test is as shown in table 2.
The testing result of a table 15 embodiment preparing product all technical
A table 25 embodiment preparing product heat storage stability result of the test
Can be found out by table 1 and 2, product prepared by embodiment 1 is all obviously better than the product prepared by other embodiments in suspensibility, wet screening test etc. and heat storage stability etc.
Two, toxicological information
This product rat acute per os LD
50female buck is all greater than 5000mg/kg, and rat acute is through skin LD
50female buck is all greater than 2000mg/kg.
60% azoles ether Carbatene water dispersible granules is nonirritant to rabbit skin, to rabbit eye irritation.
Sensitization rate result of the test shows, 60% azoles ether Carbatene water dispersible granules belongs to I grade of weak sensitizer.
This product does not meet the requirement providing acute inhalation toxicity to test, so acute inhalation toxicity test has been reduced or remitted in my unit application according to " agriculture chemical registration data specifies ".
According to China's agricultural chemicals acute toxicity grading criteria, 60% azoles ether Carbatene water dispersant belongs to lower toxicity agricultural chemicals.
Three, for pyraclostrobin and composite indoor biological activity (virulence) mensuration of Carbatene of downy mildew of garpe
1, experiment purpose
Be intended to measure pyraclostrobin, Carbatene and the two different proportion proportioning to the virulence of downy mildew of garpe, to judge whether the two different ratio has synergistic effect to suppression downy mildew of garpe.
2, experimental condition
2.1 for examination target
Plasmopara viticola (PowderyMildews) test strain, is provided by Zhi Bing teaching and research room of Agricultural University Of Anhui.
2.2 condition of culture
By the Pseudoperonospora cubensis strain transfer of indoor 4 DEG C of Refrigerator stores on PSA medium, cultivate in 25 DEG C of incubators and make it activate, for subsequent use after twice switching.
2.3 instrument and equipment
Electronic balance (sensibility reciprocal 0.1mg), test tube, culture dish, pressure steam sterilizer, superclean bench, biochemical cultivation case, pipettor, inoculator, card punch (internal diameter is 5mm) etc.
3, experimental scheme
3.1 examination materials prepare
Pseudoperonospora cubensis pathogen is placed in biochemical cultivation case and cultivates, for subsequent use.
3.2 medicament
The former medicine of pyraclostrobin of content 97.5%, the former medicine of Carbatene of content 85%, provides by former medicine portion of Anhui Meilan Agricultural Development Co., Ltd..
3.3 medicament preparations
5 series mass concentration are diluted to the medicament that embodiment 1-5 is prepared by acetone.
4, test method
Carry out with reference to " farm-chemical indoor determination test rule----bactericide " (NY/T1156.6-2006).In order to grope the activity of each medicament to strains tested, first carry out preliminary experiment.Cultivate be placed on the medium containing higher and low concentration medicament by mycelia under, estimate EC
50, and then according to the EC estimated
50value, is made into its EC by medium
50the pastille medium of the variable concentrations gradient of left and right is cultivated.
This test adopts plate mycelial growth rate method to measure medicament to the virulence of Pseudoperonospora cubensis.Concrete grammar is as follows: through the Pseudoperonospora cubensis bacterial strain PSA medium culture of switching activation, when bacterium colony grows to culture dish 3/4ths size, punch from edge with the card punch that internal diameter is 5mm, the mycelia block broken into is as inoculum.Respectively medicament mother liquor is added in the PSA medium of people's sterilizing thawing, fully shake up, make medicament ultimate density (calculating by active ingredient) reach variable concentrations gradient (table 1).About 15mL pastille medium poured into by every ware, if not dosing is contrast, often processes 4 repetitions.Move the mycelia block (diameter 5mm) connecing new growth central in flat board, be placed in 25 DEG C of incubators and cultivate 2d (Pseudoperonospora cubensis), 7d (Pseudoperonospora cubensis) and 15d (Pseudoperonospora cubensis).Measure colony diameter by right-angled intersection method, calculate each process net growth, mycelial growth inhibition rate.
In formula: bacterium dish diameter is 5mm.
5, data statistic analysis
Mycelial growth inhibition rate is converted into probit value (y), and drug concentration (μ g/mL) converts logarithm value (x) to, tries to achieve virulence regression equation (y=a+bx) with method of least squares.With DPS statistical software, regression analysis is carried out to the log concentration value of each single dose and different mixture and corresponding inhibiting rate probit value, calculate EC
50value and 95% confidence limit.
According to EC
50calculate the actual measurement toxicity index (ATI) of built agent, theoretical toxicity index (TTI) and co-toxicity coefficient (CTC).
Built agent actual measurement toxicity index (ATI)=single dose EC
50/ built agent EC
50× 100
Theoretical toxicity index (TTI)=A toxicity index × A content (%)+B toxicity index × B content (the %)+C toxicity index × C content (%) in built agent in built agent in built agent of built agent
Co-toxicity coefficient (CTC)=ATI/TTI × 100
Calculate medicament different ratio synergy ratio (CTC) according to the abundant method of Sun Yun, CTC≤80 are antagonism, and 80 < CTC < 120 are summation action, and CTC >=120 are synergistic effect.
6, results and analysis
The co-toxicity of water dispersible granules to downy mildew of garpe prepared by embodiment 1 shows as notable synergistic effect (co-toxicity coefficient reaches 295), and water dispersible granules prepared by embodiment 2-5 only shows as addition (co-toxicity coefficient is followed successively by 82,90,88,98) to the co-toxicity of downy mildew of garpe.
Claims (2)
1. pyraclostrobin and a Carbatene compound water dispersible granule, is characterized in that: this water dispersible granules is made up of the component of following weight portion:
2. prepare the method for pyraclostrobin and Carbatene compound water dispersible granule as claimed in claim 1 for one kind; it is characterized in that: raw material is mixed; be ground into wetting powder through micro jet, add in fluid-bed drying comminutor, with the aqueous solution of adhesive; granulation in the fluid bed of 50-70 DEG C; carry out drying in dryer, after screening, obtain product, then sample analysis; after qualified, metering, packaging, warehouse-in.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106135244A (en) * | 2016-07-19 | 2016-11-23 | 江西威力特生物科技有限公司 | Water dispersible granules that Carbatene and pyraclostrobin compound and preparation method thereof |
| CN110301448A (en) * | 2018-03-27 | 2019-10-08 | 宁夏农林科学院植物保护研究所（宁夏植物病虫害防治重点实验室） | A kind of compounding seed dressing for preventing and treating black scurf of potato |
| CN110839647A (en) * | 2019-10-24 | 2020-02-28 | 惠州市银农科技股份有限公司 | Bactericidal composition containing pyraclostrobin and metiram and preparation method thereof |
| CN114732009A (en) * | 2022-06-13 | 2022-07-12 | 山东百农思达生物科技有限公司 | Preparation method of water dispersible granules containing pyraclostrobin and dimethomorph |
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| CN103548857A (en) * | 2013-08-21 | 2014-02-05 | 陕西康禾立丰生物科技药业有限公司 | Pyraclostrobin-containing pesticide composition |
| CN104126595A (en) * | 2014-08-21 | 2014-11-05 | 陕西上格之路生物科学有限公司 | Pyraclostrobin-containing bactericide composition |
| CN104247712A (en) * | 2014-03-19 | 2014-12-31 | 陕西上格之路生物科学有限公司 | Dispersible oil suspending agent containing pyraclostrobin and mancozeb |
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Patent Citations (4)
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| CN102302025A (en) * | 2011-03-12 | 2012-01-04 | 陕西汤普森生物科技有限公司 | Bactericidal composition containing pyraclostrobin and thiocarbamate |
| CN103548857A (en) * | 2013-08-21 | 2014-02-05 | 陕西康禾立丰生物科技药业有限公司 | Pyraclostrobin-containing pesticide composition |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106135244A (en) * | 2016-07-19 | 2016-11-23 | 江西威力特生物科技有限公司 | Water dispersible granules that Carbatene and pyraclostrobin compound and preparation method thereof |
| CN110301448A (en) * | 2018-03-27 | 2019-10-08 | 宁夏农林科学院植物保护研究所（宁夏植物病虫害防治重点实验室） | A kind of compounding seed dressing for preventing and treating black scurf of potato |
| CN110839647A (en) * | 2019-10-24 | 2020-02-28 | 惠州市银农科技股份有限公司 | Bactericidal composition containing pyraclostrobin and metiram and preparation method thereof |
| CN110839647B (en) * | 2019-10-24 | 2021-07-09 | 惠州市银农科技股份有限公司 | Bactericidal composition containing pyraclostrobin and metiram and preparation method thereof |
| CN114732009A (en) * | 2022-06-13 | 2022-07-12 | 山东百农思达生物科技有限公司 | Preparation method of water dispersible granules containing pyraclostrobin and dimethomorph |
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