CN105123727A - Dimethomorph and pyraclostrobin compound suspending agent as well as preparation method thereof - Google Patents
Dimethomorph and pyraclostrobin compound suspending agent as well as preparation method thereof Download PDFInfo
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- CN105123727A CN105123727A CN201510623915.2A CN201510623915A CN105123727A CN 105123727 A CN105123727 A CN 105123727A CN 201510623915 A CN201510623915 A CN 201510623915A CN 105123727 A CN105123727 A CN 105123727A
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- dimethomorph
- suspending agent
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- QNBTYORWCCMPQP-JXAWBTAJSA-N (Z)-dimethomorph Chemical compound C1=C(OC)C(OC)=CC=C1C(\C=1C=CC(Cl)=CC=1)=C/C(=O)N1CCOCC1 QNBTYORWCCMPQP-JXAWBTAJSA-N 0.000 title claims abstract description 37
- 239000005761 Dimethomorph Substances 0.000 title claims abstract description 37
- 239000005869 Pyraclostrobin Substances 0.000 title claims abstract description 35
- 239000000375 suspending agent Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- -1 pyraclostrobin compound Chemical class 0.000 title abstract description 5
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000000084 colloidal system Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000004576 sand Substances 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 241000233679 Peronosporaceae Species 0.000 abstract description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 abstract description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000008367 deionised water Substances 0.000 abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 abstract description 6
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 abstract description 6
- 235000010234 sodium benzoate Nutrition 0.000 abstract description 6
- 239000004299 sodium benzoate Substances 0.000 abstract description 6
- 229920001285 xanthan gum Polymers 0.000 abstract description 6
- 230000002265 prevention Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 2
- 241000219094 Vitaceae Species 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 235000021021 grapes Nutrition 0.000 abstract 1
- 229940082509 xanthan gum Drugs 0.000 abstract 1
- 235000010493 xanthan gum Nutrition 0.000 abstract 1
- 239000000230 xanthan gum Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 17
- 239000003814 drug Substances 0.000 description 14
- 230000001988 toxicity Effects 0.000 description 11
- 231100000419 toxicity Toxicity 0.000 description 11
- 230000000844 anti-bacterial effect Effects 0.000 description 9
- 241001281805 Pseudoperonospora cubensis Species 0.000 description 8
- 239000003899 bactericide agent Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 241000723353 Chrysanthemum Species 0.000 description 7
- 235000007516 Chrysanthemum Nutrition 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000002195 synergetic effect Effects 0.000 description 7
- 238000005338 heat storage Methods 0.000 description 6
- 230000000295 complement effect Effects 0.000 description 5
- 239000013530 defoamer Substances 0.000 description 5
- 230000001018 virulence Effects 0.000 description 5
- 235000009754 Vitis X bourquina Nutrition 0.000 description 4
- 235000012333 Vitis X labruscana Nutrition 0.000 description 4
- 240000006365 Vitis vinifera Species 0.000 description 4
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- 230000009471 action Effects 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 241000700199 Cavia porcellus Species 0.000 description 2
- 239000005782 Fluopicolide Substances 0.000 description 2
- 241000233654 Oomycetes Species 0.000 description 2
- 241000283973 Oryctolagus cuniculus Species 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
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- GBOYJIHYACSLGN-UHFFFAOYSA-N fluopicolide Chemical compound ClC1=CC(C(F)(F)F)=CN=C1CNC(=O)C1=C(Cl)C=CC=C1Cl GBOYJIHYACSLGN-UHFFFAOYSA-N 0.000 description 2
- 230000009036 growth inhibition Effects 0.000 description 2
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- 238000005259 measurement Methods 0.000 description 2
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- 238000012546 transfer Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 1
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- 235000006484 Paeonia officinalis Nutrition 0.000 description 1
- 240000005001 Paeonia suffruticosa Species 0.000 description 1
- 235000003889 Paeonia suffruticosa Nutrition 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
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- 231100000605 Toxicity Class Toxicity 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to dimethomorph and pyraclostrobin compound suspending agent as well as a preparation method thereof, and relates to the technical field of the prevention and treatment of downy mildew of grapes and ornamental flowers. According to 1L of dimethomorph and pyraclostrobin compound suspending agent, the suspending agent is prepared from 320g of dimethomorph, 160g of pyraclostrobin, 30g of fatty alcohol-polyoxyethylene ether, 50g of styrylphenol polyoxyethylene ether, 5g of xanthan gum, 3g of sodium benzoate, 5g of defoaming agent and the balance of deionized water. All the raw materials are pumped into a preparation kettle to be mixed and stirred to obtain a mixture, then the mixture is primarily ground by virtue of a colloid mill and is finely ground by virtue of a sand mill, then the mixture is sampled and analyzed, and after the sample is qualified, a product is filtered, measured, packed and warehoused. When the 480g/L of dimethomorph and pyraclostrobin compound suspending agent is compounded in a compounding ratio of 2 to 1, the acting range can be obviously synergized; however, for other preparations in other compounding ratios, the synergism of the acting range cannot be achieved.
Description
Technical field
The present invention relates to the downy mildew Prevention Technique field of grape and ornamental flower, specifically relate to a kind of dimethomorph and the composite suspending agent of pyraclostrobin 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 bactericide of the existing control of the downy mildew for grape and ornamental flower, such as " CN102239864A " discloses one " bactericidal composition containing pyraclostrobin and dimethomorph ", adopts weight ratio to be that the pyraclostrobin of 50:1 ~ 1:80 and dimethomorph carry out composite Chinese patent.Separately there is Chinese patent " CN101647446A " to disclose one " bactericidal composition containing fluopicolide and dimethomorph ", adopt weight ratio to be that the fluopicolide of 1:30 ~ 10:1 and dimethomorph carry out composite.
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 that the control of the downy mildew to grape and ornamental flower cannot play good control efficiency.
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, wetting powder easily causes product to bond, not easily dispersion suspension in water, 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 dimethomorph and the composite suspending agent of pyraclostrobin, and this suspending agent is reasonable in design, good to the control efficiency of the downy mildew of grape and ornamental flower, and can realize the notable synergistic effect of dimethomorph and pyraclostrobin.
For achieving the above object, present invention employs following technical scheme:
A kind of dimethomorph and the composite suspending agent of pyraclostrobin, in 1L, this suspending agent is made up of following component:
Dimethomorph single-mindedly kills Oomycete fungal bactericide, its action character is the formation destroying cell envelope, effect is had to each stage of oomycetes history of life, particularly responsive at the formation stages of sporangiophore and egg spore, (<0.25 μ g/ml) is namely suppressed at much lower concentrations.With phenylamide medicament without cross resistance.Pyraclostrobin is New-type wide-spectrum bactericide, and its mechanism of action is mitochondrial respiratory inhibitor.Namely by stoping electro transfer in cytochrome synthesis, there is protection, treatment, blade infiltration conduction.The two compound sterilizing effect synergy, the lasting period is longer, and it is better to prevent and treat downy mildew effect.
Dimethomorph of the present invention and the composite suspending agent of pyraclostrobin, its beneficial effect shows:
1) suspending agent that, prepared by the present invention is all obviously better than the product prepared by other proportionings in suspensibility, persistent foamability, wet screening test etc. and heat storage stability etc.
2), verify by experiment, dimethomorph and pyraclostrobin with 2:1 proportioning mixed composite 480g/L time dimethomorph and the composite suspending agent of pyraclostrobin, 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 dimethomorph and the composite suspending agent of pyraclostrobin are provided, just grind after raw material suction preparation still mix and blend through colloid mill, again through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
The preparation method of dimethomorph of the present invention and the composite suspending agent of pyraclostrobin, 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 dimethomorph and the composite suspending agent of pyraclostrobin, and testing result, the heat storage stability result of the test of all technical of suspending agent prepared by each embodiment.
Embodiment 1
480g/L dimethomorph and the composite suspending agent of pyraclostrobin, each component and weight as follows:
| Composition | Weight (g) |
| Dimethomorph | 320 |
| Pyraclostrobin | 160 |
| Fatty alcohol-polyoxyethylene ether | 30 |
| Styrylphenol polyoxyethylene ether | 50 |
| Xanthans | 5 |
| Sodium Benzoate | 3 |
| Defoamer | 5 |
| Deionized water | Complement to 1L |
Preparation method: just grind after raw material suction preparation still mix and blend through colloid mill, then through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
Embodiment 2
490g/L dimethomorph and the composite suspending agent of pyraclostrobin, each component and weight as follows:
| Composition | Weight (g) |
| Dimethomorph | 325 |
| Pyraclostrobin | 165 |
| Fatty alcohol-polyoxyethylene ether | 35 |
| Styrylphenol polyoxyethylene ether | 45 |
| Xanthans | 6 |
| Sodium Benzoate | 3.5 |
| Defoamer | 4 |
| Deionized water | Complement to 1L |
Preparation method is with embodiment 1.
Embodiment 3
500g/L dimethomorph and the composite suspending agent of pyraclostrobin, each component and weight as follows:
| Composition | Weight (g) |
| Dimethomorph | 330 |
| Pyraclostrobin | 170 |
| Fatty alcohol-polyoxyethylene ether | 40 |
| Styrylphenol polyoxyethylene ether | 55 |
| Xanthans | 4 |
| Sodium Benzoate | 4 |
| Defoamer | 6 |
| Deionized water | Complement to 1L |
Preparation method is with embodiment 1.
Embodiment 4
470g/L dimethomorph and the composite suspending agent of pyraclostrobin, each component and weight as follows:
| Composition | Weight (g) |
| Dimethomorph | 315 |
| Pyraclostrobin | 155 |
| Fatty alcohol-polyoxyethylene ether | 20 |
| Styrylphenol polyoxyethylene ether | 60 |
| Xanthans | 4.5 |
| Sodium Benzoate | 2.5 |
| Defoamer | 5.5 |
| Deionized water | Complement to 1L |
Preparation method is with embodiment 1.
Embodiment 5
460g/L dimethomorph and the composite suspending agent of pyraclostrobin, each component and weight as follows:
| Composition | Weight (g) |
| Dimethomorph | 310 |
| Pyraclostrobin | 150 |
| Fatty alcohol-polyoxyethylene ether | 25 |
| Styrylphenol polyoxyethylene ether | 40 |
| Xanthans | 5.5 |
| Sodium Benzoate | 2 |
| Defoamer | 4.5 |
| Deionized water | Complement to 1L |
Preparation method is with embodiment 1.
Dimethomorph prepared by embodiment 1 ~ 5 and the composite suspending agent of pyraclostrobin, 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, persistent foamability, wet screening test etc. and heat storage stability etc.
Two, toxicological information
Rat acute per os LD
50male is 5000mg/kg, and female is 5000mg/kg, belongs to malicious class such as low grade.
Rat acute percutaneous toxicity test: LD
50femalely/male be all greater than 2000mg/kgBW, belong to malicious class such as low grade.
Rabbits with Acute eye irritant test nonirritant.
Rabbits with Acute Skin Irritation Test: skin irritatin mean scores is 0, and this sample is to guinea pig skin nonirritant.
Guinea pig skin allergy is tested: skin sensitization rate (%)=0, belongs to I grade of weak sensitizer.
According to China's pesticide toxicity grading criteria, 480 grams per liter alkene acyl pyrazoles ester suspending agents belong to hypotoxicity agricultural chemicals.
Three, measure for the composite indoor biological activity (virulence) of the dimethomorph and pyraclostrobin of viewing and admiring chrysanthemum downy mildew
1, experiment purpose
Be intended to measure dimethomorph, pyraclostrobin and the two different proportion proportioning to the virulence of viewing and admiring chrysanthemum downy mildew, to judge that the two different ratio is viewed and admired chrysanthemum downy mildew to suppression and whether had synergistic effect.
2, experimental condition
2.1 for examination target
View and admire chrysanthemum Pseudoperonospora cubensis (PowderyMildews) test strain, provided by plant protection plant pathology research department 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 dimethomorph of content 97%, the former medicine of pyraclostrobin of content 97.5%, 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
Suspending agent prepared by embodiment 1 shows as notable synergistic effect (co-toxicity coefficient reaches 289) to the co-toxicity viewing and admiring chrysanthemum downy mildew, and suspending agent prepared by embodiment 2-5 only shows as addition (co-toxicity coefficient is followed successively by 80,82,83,85) to the co-toxicity viewing and admiring chrysanthemum downy mildew.
Claims (2)
1. dimethomorph and the composite suspending agent of pyraclostrobin, it is characterized in that: in 1L, this suspending agent is made up of following component:
2. prepare the method for dimethomorph and the composite suspending agent of pyraclostrobin as claimed in claim 1 for one kind, it is characterized in that: just grind after raw material suction preparation still mix and blend through colloid mill, again through sand mill fine grinding, sample analysis, qualified rear filtration, metering, packaging, warehouse-in.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108041059A (en) * | 2017-12-12 | 2018-05-18 | 安徽国星生物化学有限公司 | A kind of suspending agent of pyraclostrobin-containing and dimethomorph |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210444A (en) * | 1996-05-09 | 1999-03-10 | 巴斯福股份公司 | Fungicidal mixtures |
| CN102239864A (en) * | 2010-05-16 | 2011-11-16 | 青岛奥迪斯生物科技有限公司 | Bactericidal composition containing pyraclostrobin and dimethomorph |
| WO2012070961A2 (en) * | 2010-11-26 | 2012-05-31 | Sapec-Agro, Sa | Fungicidal mixture |
-
2015
- 2015-09-25 CN CN201510623915.2A patent/CN105123727A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210444A (en) * | 1996-05-09 | 1999-03-10 | 巴斯福股份公司 | Fungicidal mixtures |
| CN102239864A (en) * | 2010-05-16 | 2011-11-16 | 青岛奥迪斯生物科技有限公司 | Bactericidal composition containing pyraclostrobin and dimethomorph |
| WO2012070961A2 (en) * | 2010-11-26 | 2012-05-31 | Sapec-Agro, Sa | Fungicidal mixture |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108041059A (en) * | 2017-12-12 | 2018-05-18 | 安徽国星生物化学有限公司 | A kind of suspending agent of pyraclostrobin-containing and dimethomorph |
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