Summary of the invention
The technical problem to be solved in the present invention is: at bactericide resistance and pedo relict problem in actual applications, the bactericide that filters out two kinds of different sterilizing mechanismses carries out composite, and to improve the bactericidal agent for preventing and treating effect, delaying drug resistance produces, reduce amount of application, reduce the control cost.
For solving the problems of the technologies described above, the invention provides a kind of bactericidal composition, said composition comprises A and two kinds of active ingredients of B, and active component A is SSF 126 (Metominostrobin), and active component B is for being selected from Prochloraz (Prochloraz).The inventor finds that by test above-mentioned bactericidal composition synergy is obvious, the more important thing is that amount of application reduces, and reduces use cost.It is different with the compound structure type of B component to contain component A, and mechanism of action is different, and both are composite can to enlarge fungicidal spectrum, and can delay generation and the development speed of pathogen resistance to a certain extent, and does not have cross resistance between component A and the B component.
Another object of the present invention provides the preparation method who comprises two kinds of effective constituents A and B bactericidal composition and prevents and treats the application of crop pest at agriculture field.
In the above-mentioned bactericidal composition, the weight ratio between weight two components of component A and B component is 0.02~50.According to the physicochemical property between the component and practical application, the preferred weight ratio of active component SSF 126 (A) and active component Prochloraz (B) is 0.05~30, and A and two kinds of active components of B account for the 5-90% of bactericide gross weight.
The invention provides the purposes of bactericidal composition in controlling plant diseases of being formed by component A (SSF 126) and B component (Prochloraz), as SSF 126 and Prochloraz is composite that rice blast is had very high preventive effect.
Above-mentioned composition also comprises carrier, auxiliary agent and/or surfactant.In the process of using, can mix auxiliary agent commonly used.
Proper auxiliary agent can be solid or liquid, and they are material commonly used in the formulation process normally, mineral matter natural or regeneration for example, solvent, dispersant, wetting agent, adhesive, thickener, adhesive or fertilizer.
The application process of the present composition comprises the acrial part, particularly leaf portion or blade face that composition of the present invention is used for the plant growth.The frequency of using and amount of application depend on biology and the weather life condition of pathogene.Can be with the growth place of plant, as the rice field, soak with the liquid preparation of composition, perhaps composition is applied in the soil with solid form, as with particle form (soil application), composition can be by soil (systemic action) in plant root enters plant corpus.
These compositions can only comprise active component and use, also can be mixed together use with additive, therefore composition of the present invention can be prepared into various formulations, for example wetting powder, suspending agent, oil-suspending agent, water dispersible granules, aqueous emulsion, microemulsion.According to the character of these compositions and use purpose and the ambient conditions that composition will reach, can select with composition with spraying, atomizing, dust, broadcast sowing or sprinkle the method for watering etc. and so on and use.
Available known method can become various formulations with preparation of compositions of the present invention, active ingredient and auxiliary agent as solvent, solid carrier, can evenly can be mixed, grind when needing with surfactant, is prepared into needed formulation.
Above-mentioned solvent can be selected from aromatic hydrocarbon, preferably contains 8-12 carbon atom, as the benzene of xylene mixture or replacement, phthalate, sad as Dibutyl phthalate or phthalandione two, fat hydrocarbon, as cyclohexane or paraffin, pure and mild ethylene glycol and their ether and ester, as ethanol, ethylene glycol, glycol monomethyl methyl; Ketone, as cyclohexanone, the solvent of strong polarity, as the N-N-methyl-2-2-pyrrolidone N-, dimethyl sulfoxide (DMSO) or dimethyl formamide and vegetable oil or vegetable oil are as soybean oil.
Above-mentioned solid carrier, but as being used for the normally natural minerals filler of pulvis and dispersant, for example talcum, kaolin, montmorillonite or atlapulgite.In order to manage the physical property of composition, also can add polymolecularity silicic acid or polymolecularity adsorpting polymerization thing carrier, for example granular absorption carrier or non-absorption carrier, suitable granular absorption carrier is porous type, as float stone, bentonite or bentonite; Suitable non-absorption carrier such as calcite or sand.In addition, can use the granular material of being prefabricated into of a large amount of inorganic in nature or organic character as carrier, particularly dolomite.
Chemical property according to the active ingredient in the composition of the present invention, suitable surfactant is lignin sulfonic acid, naphthalene sulfonic acids, phenolsulfonic acid, alkali salt or amine salt, alkylaryl sulfonates, alkyl sulfate, alkylsulfonate, aliphatic alcohol sulfate, fatty acid and sulphated fatty alcohol glycol ether also have the condensation product of sulfonated naphthalene and naphthalene derivatives and formaldehyde, the condensation product of naphthalene or naphthalene sulfonic acids and phenol and formaldehyde, NONIN HS 240, the ethoxylation isooctylphenol, octyl phenol, nonyl phenol, alkylaryl polyglycol ether, tributyl benzene polyglycol ether, three stearyl phenyl polyglycol ethers, alkyl aryl polyether alcohol, ethoxylated castor oil, polyoxyethylene alkyl ether, the ethylene oxide condensation product, the ethoxylation polyoxypropylene, lauric acid polyglycol ether acetal, sorbitol ester, lignin sulfite waste liquor and methylcellulose.
Two kinds of active ingredients show as synergistic effect in the composition of the present invention, and the specific activity of said composition is used the activity expection summation of individualized compound, and the independent activity of individualized compound is more remarkable.Synergistic effect shows as and allows that amount of application reduces, wideer antifungal control spectrum, instant effect, more lasting control efficiency, by only once or minority use better control plant harmful fungoid several times and widened the possible administration interval time.These characteristics are special needs in the plant epiphyte control practice process.
Other characteristics that show of bactericidal composition of the present invention mainly show as: 1, because two single thinner architectural differences of this composition are very big, the mechanism of action is different fully, there is not cross resistance, can delays two single agent and use the resistance problem that produces separately; 2, composition of the present invention is good to crop safety, preventive effect.Through evidence, microbicide compositions chemical property of the present invention is stable, and synergy is remarkable, and controlling object is shown tangible synergy and complementation.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explaining the present invention, and be not used in restriction the present invention, all any modifications of making within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within protection scope of the present invention.
Percentage all is weight percentage in all prescriptions of following examples.The processing technology of the various preparations of the present composition is prior art, can change to some extent according to different situations.
One, formulation prepares embodiment
(1) processing of water dispersible granules and embodiment
Active component SSF 126 and Prochloraz, auxiliary agent and filler are mixed in the ratio of filling a prescription, be ground into wetting powder through air-flow, add a certain amount of water mixing extruder grain again, make the water dispersible granules product after the drying screening.
Embodiment 1:86% SSF 126 Prochloraz water dispersible granules
SSF 126 82%, Prochloraz 4%, dodecyl sodium sulfate 3%, Negel 2%, ammonium sulfate 2%, precipitated calcium carbonate complements to 100%.
Embodiment 2:65% SSF 126 Prochloraz water dispersible granules
SSF 126 3%, Prochloraz 62%, methyl naphthalene sulfonate formaldehyde condensate 5%, sodium lignin sulfonate 3%, lauryl sodium sulfate 4%, diatomite complements to 100%.
(2) processing of suspending agent and embodiment
The ratio of each component such as active component SSF 126 and Prochloraz, dispersant, wetting agent, thickener and water in prescription mixed, after sand milling and/or high speed shear, obtain semi-finished product, add water after the analysis and mix to filter and get product.
Embodiment 3:35% SSF 126 Prochloraz suspending agent
SSF 126 30%, Prochloraz 5%, sodium lignin sulfonate 7%, xanthans 0.8%, bentonite 3%, Magnesiumaluminumsilicate 1%, ethylene glycol 4%, water complements to 100%.
Embodiment 4:18% SSF 126 Prochloraz suspending agent
SSF 126 6%, Prochloraz 12%, methyl naphthalene sulfonate formaldehyde condensate 6%, bentonite 4%, glycerine 5%, water complements to 100%.
(3) processing of wetting powder and embodiment
The active component SSF 126 is fully mixed in proportion with Prochloraz, various auxiliary agent and filler etc., after ultrafine crusher is pulverized, make wetting powder.
Embodiment 5:45% SSF 126 Prochloraz wetting powder
SSF 126 25%, Prochloraz 20%, calcium lignosulfonate 7%, neopelex 12%, bentonite 16%, attapulgite complements to 100%.
Embodiment 6:76% SSF 126 Prochloraz wetting powder
SSF 126 73%, Prochloraz 3%, alkyl polyoxy ethyl ether sulfonate 1% draws back powder 4%, bentonite 1.5%, white carbon 5%, diatomite complements to 100%.
Embodiment 7:58% SSF 126 Prochloraz wetting powder
SSF 126 4%, Prochloraz 54%, alkylsulfonate 6%, sodium lignin sulfonate 6%, white carbon 11%, kaolin complements to 100%.
(4) processing of microemulsion and embodiment
SSF 126 and Prochloraz fully after the dissolving, are stirred in solvent, add emulsifier, builder and antifreeze simultaneously, treat above-mentioned system mixing after, again water is slowly added in the above-mentioned mixed liquor, can be made into the microemulsion of different content after fully stirring.
Embodiment 8:12% SSF 126 Prochloraz microemulsion
SSF 126 4%, Prochloraz 8%, acetone 15%, compound sodium nitrophenolate 0.5%, alkyl polyoxyethylene ether and polyoxyethylene nonylphenol ether 5%, propane diols 1%, urea 2%, water complements to 100%.
Embodiment 9:16% SSF 126 Prochloraz microemulsion
SSF 126 12%, Prochloraz 4%, polyoxyethylene carboxylate and phenethyl phenol polyethenoxy ether 4%, glycerine 2%, methyl alcohol 11%, azone 1%, water complements to 100%.
(5) processing of aqueous emulsion and embodiment
In the emulsification still, SSF 126 and Prochloraz, solvent, auxiliary agent are mixed under mechanical agitation, drop into emulsifier then and stabilizing agent stirs, add water at last, under 100-12000 rev/min rotating speed, stirred 10-30 minute, make it to become the product of even emulsus.
Embodiment 10:30% SSF 126 prochloraz aqueous emulsion
SSF 126 18%, Prochloraz 12%, N-repefral 4%, nonyl phenol benzene oxygen vinethene 3%, 2,6-di-tert-butyl-4-methy phenol 2%, ethylene glycol 3%, polyvinyl alcohol 1%, Sodium Benzoate 1%, silicone defoaming agent 0.8%, water complements to 100%.
Embodiment 11:45% SSF 126 prochloraz aqueous emulsion
SSF 126 8%, Prochloraz 37%, butylated hydroxy anisole 4%, poly-isosuccinic acid acid anhydride-ethylene glycol copolymer 3%, propane diols 2%, xanthans 3%, polyvinyl alcohol 1%, silicone defoaming agent 1.2%, water complements to 100%.
(6) processing of oil-suspending agent and embodiment
Active component SSF 126 and each component such as Prochloraz, dispersant, stabilizing agent, defoamer and solvent are mixed in the ratio of prescription, put into the grinding of sand milling still after, send into the interior mixing of homogeneous blender and get product.
Embodiment 12:15% SSF 126 Prochloraz oil-suspending agent
SSF 126 5%, Prochloraz 10%, sodium lignin sulfonate 8%, bentonite 4%, xanthans 1%, silicone defoaming agent 2%, soybean oil complements to 100%.
Embodiment 13:28% SSF 126 Prochloraz oil-suspending agent
SSF 126 24%, Prochloraz 4% draws back powder 8%, bentonite 5%, organic silicone 2%, machine oil complements to 100%.
Two, drug effect demonstration test
(1) biologicall test embodiment 1
1, SSF 126 and Prochloraz are composite tests the rice blast toxicity test
Subjects: rice blast fungus (pick up from the field and through separation and purification)
Test method: pot-culture method.Choose the paddy rice seedling in tri-leaf period of growth potential unanimity, every basin 2 young plants, 5 basins are selected in each processing for use.Pyricularia oryzae is cultivated at tomato juice oat agar medium, wash spore with sterile water after producing spore, be made into the spore suspension of 1 * 105 spore/ml after double gauze filters, spray inoculation puts black plastic sack and preserves moisture and cultivate 24h on for the examination rice seedling after the inoculation equably.Behind the inoculation 24h, carry out chemicals treatment, each medicament arranges about 25 ℃, cultivate under the condition of relative moisture 〉=90%, behind the 7d according to the incidence of the whole strain blade of morbidity grade scale investigation of rice blast, as the standard medicament, calculate disease index and control efficiency with SSF 126.
Control efficiency is converted into probability value (y), and soup is done height (μ g/ml) and is converted logarithm value (x) to, calculates concentration EC50 in virulence equation and the inhibition with method of least squares, calculates the toxicity index level co-toxicity coefficient (CTC) of medicament according to the abundant method of Sun Yun.Toxicity test the results are shown in Table 1.
Actual measurement toxicity index (ATI)=(standard medicament EC50/ reagent agent EC50) * 100
The percentage composition of B in percentage composition+B medicament toxicity index * mixture of A in theoretical toxicity index (TTI)=A medicament toxicity index * mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (the ATI)/theoretical toxicity index (TTI) of mixture] * 100
CTC≤80, the composition performance is antagonism, 80<CTC<120, the composition performance is summation action, CTC 〉=120, the composition performance is synergistic effect.
The composite toxicity test interpretation of result to rice blast of the different proportionings with Prochloraz of table 1 SSF 126
The medicament title |
EC
50(μg/ml)
|
ATI |
TTI |
Co-toxicity coefficient (CTC) |
SSF 126 |
6.25 |
100.00 |
/ |
/ |
Prochloraz |
7.41 |
84.34 |
/ |
/ |
Proportioning SSF 126: Prochloraz=50: 1 |
2.7633 |
226.18 |
98.69 |
229.18 |
Proportioning SSF 126: Prochloraz=30: 1 |
2.4731 |
252.72 |
99.53 |
253.91 |
Proportioning SSF 126: Prochloraz=10: 1 |
2.2819 |
273.89 |
98.49 |
278.09 |
Proportioning SSF 126: Prochloraz=1: 1 |
2.1856 |
285.96 |
92.17 |
310.25 |
Proportioning SSF 126: Prochloraz=1: 10 |
2.7526 |
227.06 |
94.82 |
239.46 |
Proportioning SSF 126: Prochloraz=1: 30 |
3.2025 |
195.16 |
84.81 |
230.11 |
Proportioning SSF 126: Prochloraz=1: 50 |
3.4132 |
183.11 |
84.65 |
216.32 |
Result's (table 1) shows, SSF 126 and Prochloraz are between proportioning 50: 1~1: 50 (being ratio 50~0.02), and co-toxicity coefficient illustrates that all more than 200 the composite control to rice blast of SSF 126 and Prochloraz has significant synergies.
(2) field control effectiveness test
1, adopt the method for parallel test to verify SSF 126 and the composite field control effect to rice blast of Prochloraz.
(1) test site: test arrangement is at abutment farm, east, Dafeng City paddy field, and the plot is smooth, and rice blast morbidity throughout the year is heavier, and rice seedling is in tillering stage;
(2) test method: at the initial stage of a disease, carry out the spraying first time immediately, carry out the dispenser second time after 7 days, each handles 4 residential quarters, each residential quarter 20 square meter.10 days investigation statistics incidences behind the medicine before medicine and for the second time, 5 random sampling in each residential quarter, every some investigation 5 strain paddy rice, disease index and control efficiency are calculated in the lesion area of every blade accounts for blade area on the whole strain paddy rice of investigation percentage and classification.
Expection preventive effect (%)=X+Y-XY/100 (wherein, X, Y are single agent preventive effect)
Grade scale:
0 grade: no scab;
1 grade: leaf spot lesion is less than 5, and length is less than 1cm;
3 grades: leaf spot lesion 6-10, part scab length is greater than 1cm;
5 grades: leaf spot lesion 11-25, the part scab is linked to be sheet, and lesion area accounts for the 10-25% of leaf area;
7 grades: leaf spot lesion is more than 26, and scab is linked to be sheet, and lesion area accounts for the 26-50% of leaf area;
9 grades: scab is linked to be sheet, lesion area account for leaf area more than 50% or full leaf withered.
The composite field efficiency test result to rice blast of table 3 SSF 126 and Prochloraz
Measurement result (table 3) shows, the composite preventive effect to the control rice blast of SSF 126 and Prochloraz obviously improves, and illustrates that the two compositely has significant synergistic effect to rice blast.