CN117941693A

CN117941693A - Bactericidal composition containing triazole compound

Info

Publication number: CN117941693A
Application number: CN202410117281.2A
Authority: CN
Inventors: 葛家成; 刘桂娟; 张芳; 杨志鹏; 吕文东
Original assignee: Qingdao Hailier Biotechnology Co ltd
Current assignee: Qingdao Hailier Biotechnology Co ltd
Priority date: 2024-01-29
Filing date: 2024-01-29
Publication date: 2024-04-30

Abstract

The invention relates to a sterilization composition containing triazole compounds and application thereof, and the sterilization composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is Cyclobutrifluram, the active ingredient B is a triazole compound, and the triazole compound is selected from any one of flutriafol, hexaconazole and diniconazole. The bactericidal composition or the preparation thereof can enhance the drug effect, reduce the dosage, improve the control effect and delay the development of drug resistance.

Description

Bactericidal composition containing triazole compound

Technical Field

The invention relates to the field of pesticide bactericides, in particular to a bactericidal composition containing triazole compounds.

Background

Cyclobutrifluram is a novel nicotinamide class of bactericidal nematicide developed by zhengda corporation. The plant pesticide composition has broad control spectrum, is safe and efficient, can effectively control various nematodes and main fungal diseases, and can effectively control nematodes such as root knots, beet cysts and corn short bodies on crops such as cucumber, tomato, corn and beet by direct application or seed treatment; can also effectively prevent and treat plant diseases, and has excellent preventing and treating effect on fusarium especially. Its CAS accession number: 1460292-16-3. The chemical structure is as follows:

Triazole bactericides inhibit formation of iron porphyrin iron oxygen complex by coordination of triazole ring and iron atom in iron porphyrin center in thallus, thereby inhibiting synthesis of ergosterol, and finally leading thallus to death due to cell membrane injury. The triazole bactericide mainly comprises triazolone, triadimenol, uniconazole, flutriafol, hexaconazole, diniconazole, paclobutrazol, propiconazole, difenoconazole, penconazole, myclobutanil, prothioconazole and the like.

The flutriafol is a triazole sterol demethylation inhibitor bactericide, can effectively inhibit the biosynthesis of ergosterol and cause rupture of fungal cell walls, has broad-spectrum antibacterial activity and stronger systemic property, and has good protection and treatment effects on a plurality of fungal diseases caused by basidiomycetes and ascomycetes.

Hexaconazole is a sterol demethylation inhibitor, which damages and prevents the biosynthesis of ergosterol, an important component of bacterial cell membranes, and causes the cell membranes to fail to form, and causes the death of bacteria, and has systemic, protective and therapeutic activities. Can effectively prevent diseases caused by ascomycetes, basidiomycetes and fungi imperfecti. In particular to the protection and the eradication of diseases caused by basidiomycetes and ascomycetes, such as powdery mildew, rust disease, scab, brown spot and anthracnose.

Diniconazole inhibits 14 a-demethylation in ergosterol biosynthesis of fungi, causes ergosterol deficiency, causes abnormal fungal cell membrane, and finally dies fungi, and has protecting, treating and eradicating effects.

The invention has carried out intensive research on Cyclobutrifluram applied to fungal diseases, and a large number of test results show that the reasonable compounding of Cyclobutrifluram with triazole bactericides such as flutriafol, hexaconazole and diniconazole can effectively improve the control effect. With the increasing requirements of environment and food safety and the problem of drug resistance, how to scientifically apply the pesticide, reduce the dosage of chemical pesticide and improve the pesticide effect becomes a problem which needs to be solved in the pesticide field.

Disclosure of Invention

Based on the above circumstances, the present invention aims to provide a bactericidal composition containing triazole compounds and a preparation thereof, which are mainly used for controlling plant fungal diseases, and the composition or the preparation thereof can enhance the drug effect, reduce the dosage, prolong the duration of the drug and delay the development of drug resistance.

In order to achieve the above object, the following technical scheme is provided: a bactericidal composition containing triazole compounds comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound shown in a formula (I)

The active ingredient B is a triazole compound, and the triazole compound is selected from any one of tebuconazole, hexaconazole and diniconazole;

Further, the mass ratio of the active ingredient A to the active ingredient B is 35:1-1:35;

Further, the mass ratio of the compound of the formula (I) to the flutriafol is 1:35-30:1;

further, the mass ratio of the compound of the formula (I) to the flutriafol is 1:35, 1:20, 1:12, 2:9, 1:1, 2:1, 5:1, 10:1, 24:1 and 30:1;

further, the mass ratio of the compound of the formula (I) to the flutriafol is 1:20-30:1;

Further, the mass ratio of the compound of the formula (I) to the flutriafol is 1:20, 1:12, 2:9, 1:1, 2:1, 5:1, 10:1, 24:1, 30:1

Further, the mass ratio of the compound of the formula (I) to hexaconazole is 1:30-24:1;

Further, the mass ratio of the compound of the formula (I) to hexaconazole is 1:30, 1:16, 1:8, 2:5, 1:1, 2:1, 3:1, 9:1, 25:2, 24:1;

further, the mass ratio of the compound of the formula (I) to hexaconazole is 1:16-24:1;

Further, the mass ratio of the compound of the formula (I) to hexaconazole is 1:16, 1:8, 2:5, 1:1, 2:1, 3:1, 9:1, 25:2, 24:1;

further, the mass ratio of the compound of the formula (I) to diniconazole is 1:20-35:1;

Further, the mass ratio of the compound of the formula (I) to diniconazole is 1:20, 2:25, 1:10, 1:2, 5:4, 5:2, 5:1, 12:1, 25:2, 35:1;

further, the mass ratio of the compound of the formula (I) to diniconazole is 1:20-25:2;

Further, the mass ratio of the compound of the formula (I) to diniconazole is 1:20, 2:25, 1:10, 1:2, 5:4, 5:2, 5:1, 12:1, 25:2;

Further, the sum of the contents of the active component A and the active component B in the sterilizing composition is 1 to 90 percent by weight based on 100 percent by weight of the total weight of the sterilizing composition;

Further, the sum of the contents of the active ingredient A and the active ingredient B in the sterilizing composition is preferably 5 to 80wt percent based on 100wt percent of the total weight of the sterilizing composition;

Further, the bactericidal composition comprises an agriculturally acceptable auxiliary ingredient in addition to the active ingredient, wherein the auxiliary ingredient is selected from one or more of wetting agents, dispersing agents, emulsifying agents, thickening agents, disintegrating agents, antifreezing agents, antifoaming agents, solvents, preservatives, stabilizers, synergists, binders or carriers;

Further, the wetting agent is selected from one or more of alkylbenzene sulfonate, alkyl naphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, dioctyl sodium succinate, alpha olefin sulfonate, alkylphenol ethoxylate, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, chinese honeylocust fruit powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrating agent F; and/or

Further, the dispersing agent is selected from one or more of lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerin fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or

Further, the emulsifier is one or more selected from calcium dodecyl benzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and/or

Further, the thickener is one or more selected from xanthan gum, organic bentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and/or

Further, the disintegrating agent is selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and/or

Further, the antifreezing agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and/or

Further, the defoamer is one or more selected from C ₁₀-C₂₀ saturated fatty acid compounds, silicone oil, silicone compounds and C ₈-C₁₀ fatty alcohol; and/or

Further, the solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel oil, solvent oil, vegetable oil (soybean oil, corn oil, rapeseed oil, palm oil, etc.), vegetable oil derivatives and water; and/or

Further, the preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium parahydroxybenzoate, methyl parahydroxybenzoate, pinocembrane and 1, 2-benzisothiazolin-3-one; and/or

Further, the stabilizer is selected from one or more of disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2, 6-di-tert-butyl-p-methylphenol, triethanolamine oleate, epoxidized vegetable oil, kaolin, diatomite, bentonite, attapulgite, white carbon black, talcum powder, montmorillonite and starch; and/or

Further, the synergist is selected from synergistic phosphorus and synergistic ether; and/or

Further, the carrier is selected from one or more of ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils, and vegetable oil derivatives.

Further, the dosage form of the bactericidal composition is selected from a solid preparation and/or a liquid preparation and/or a seed treatment preparation;

The solid preparation comprises powder, granules, balls, tablets, strips, wettable powder, oil dispersion powder, emulsion powder, water dispersible granules, emulsion granules, water dispersible tablets, soluble powder, soluble tablets or soluble granules;

The liquid preparation comprises a soluble agent, an oil agent, a spreading oil agent, an emulsifiable concentrate, a latex, a dispersible agent, a paste, an aqueous emulsion, an oil emulsion, a microemulsion, a lipid agent, a suspending agent, a microcapsule suspending agent, an oil suspending agent, a dispersible oil suspending agent, a suspending emulsion, a microcapsule suspension-suspending agent, a microcapsule suspension-aqueous emulsion or a microcapsule suspension-suspending emulsion;

further, the powder is a free-flowing powder preparation which is suitable for spraying or spreading and contains an active ingredient;

Further, the granule is a granular preparation with a certain particle size range and free flowing active ingredients;

further, the spherical agent is a spherical agent (generally with the diameter larger than 6 mm) containing an active ingredient;

Further, the tablet is a tablet formulation having a shape and size containing an active ingredient (typically having two planar or convex surfaces with a spacing of less than a diameter);

Further, the stick is a stick or bar-like preparation (typically a few centimeters long, a few millimeters width/diameter, i.e., a length greater than a diameter/width) containing an active ingredient;

further, the wettable powder is a powdery preparation in which the active ingredients are dispersed into suspension in water;

further, the oil dispersion powder is a powder preparation in which an active ingredient is dispersed into a suspension in an organic solvent;

Further, the emulsion powder is a powdery preparation of which the active ingredients are dissolved by an organic solvent and are wrapped in soluble or insoluble inert ingredients, and the active ingredients are dispersed in water to form oil-in-water emulsion;

further, the water dispersible granule is a granular preparation which disintegrates in water and the effective components are dispersed into suspension;

Further, the emulsion granule is a granular preparation of which the active ingredient is dissolved by an organic solvent and is wrapped in soluble or insoluble inert ingredients, and the active ingredient is dispersed in water to form oil-in-water emulsion;

Further, the water dispersible tablet is a tablet preparation which disintegrates in water and the active ingredient is dispersed into suspension;

Further, the soluble powder is a powdery preparation of which the active ingredient forms a true solution in water, and can contain inert ingredients which are insoluble in water;

further, the soluble granule is a granular preparation of which the effective component forms a true solution in water, and can contain an inert component which is insoluble in water;

Further, the soluble tablet is a tablet preparation in which the active ingredient forms a true solution in water, and may contain an inert ingredient which is insoluble in water;

Further, the soluble agent is a liquid preparation which is diluted into transparent or semitransparent containing active ingredients by water, and can contain inert ingredients which are insoluble in water;

further, the soluble agent is a colloidal preparation which is diluted into true solution by water and contains active ingredients;

Further, the oil is a liquid preparation which is diluted (or not diluted) by an organic solvent to be homogeneous and contains active ingredients;

further, the film spreading oiling agent is an oiling agent which automatically diffuses into an oil film on the water surface and contains active ingredients;

further, the emulsifiable concentrate is a homogeneous liquid preparation which is diluted and dispersed into emulsion by water and contains active ingredients;

Further, the emulsion is a latex preparation which is diluted and dispersed into emulsion by water and contains active ingredients;

further, the dispersible agent is a homogeneous liquid preparation which is diluted and dispersed into suspension containing the active ingredients by water;

furthermore, the ointment is a water-based ointment preparation containing active ingredients and capable of forming a film, and is generally used directly;

Further, the aqueous emulsion is an emulsion liquid preparation formed by the active ingredient (or organic solution thereof) in water;

Further, the oil emulsion is an emulsion liquid preparation formed by the effective component (or aqueous solution thereof) in oil;

Further, the microemulsion is a microemulsion liquid preparation with the active ingredient being transparent or semitransparent in water, and is used directly or after being diluted by water;

further, the fat agent is an oil or fat-based viscous preparation containing an active ingredient, and is generally used directly;

Further, the suspending agent is a stable suspension liquid preparation prepared by dispersing the active ingredient in water in solid particles, and is generally diluted by water;

Further, the microcapsule suspending agent is a stable suspension liquid preparation formed by dispersing microcapsules containing active ingredients in liquid;

further, the oil suspending agent is a stable suspension liquid preparation prepared by dispersing solid particles as an active ingredient in liquid, and is generally diluted by an organic solvent;

Further, the dispersible oil suspending agent is a stable suspension liquid preparation prepared by dispersing solid particles of an active ingredient in a non-aqueous medium, and is generally diluted with water for use;

further, the suspoemulsion is a heterogeneous liquid preparation in which the active ingredients are stably dispersed in a continuous water phase in the form of solid particles and water-insoluble tiny liquid drops;

Further, the microcapsule suspension-suspending agent is a stable suspension liquid preparation prepared by dispersing the effective components in water by using microcapsules and solid particles;

Further, the microcapsule suspension-water emulsion is a heterogeneous liquid preparation which is formed by stably dispersing the effective component in a continuous water phase in a microcapsule and micro droplet form;

Further, the microcapsule suspension-suspension emulsion is a heterogeneous liquid preparation with active ingredients stably dispersed in a continuous water phase in the forms of microcapsules, solid particles and tiny liquid drops;

Further, the bactericidal composition can be prepared into a preparation formulation which is acceptable in pesticide, wherein the preparation formulation is microemulsion, aqueous emulsion, suspending agent, dispersible oil suspending agent, solution, emulsifiable concentrate, suspending agent, microcapsule suspending agent, water dispersible granule, wettable powder, granule, seed treatment suspending agent and seed treatment dry powder;

further, the preparation formulation is microemulsion, emulsifiable concentrate, suspending agent, aqueous emulsion, water dispersible granule and seed treatment suspending agent.

The invention also discloses application of the bactericidal composition in preventing and controlling plant diseases;

further, the plant disease is a fungal or bacterial caused plant disease;

further, the plant disease is a fungal-caused plant disease;

Further, the plant disease caused by the fungus is wheat scab.

The invention has the beneficial effects that:

(1) The bactericidal activity is increased, the application range is enlarged, and the yield increasing effect is obvious;

(2) The development prospect is wide, the use amount of pesticides is reduced, and the agricultural cost is reduced;

(3) Safe and efficient, is safe to crops, non-target organisms, beneficial organisms and natural enemies, and has the effect of increasing yield and ensuring income.

Detailed Description

The present invention will be described in more detail with reference to the following examples, but the present invention can be embodied in various forms and should not be construed as being limited to the embodiments set forth herein.

Indoor bioassay of wheat scab

The test is based on: section 2 of the bactericide referring to the standard pesticide indoor bioassay test guidelines in the agricultural industry of the people's republic of China: test plate method for inhibiting growth of pathogenic fungi mycelium NT/T1156.2-2006.

Test pathogenic bacteria: wheat scab (Fusarium graminearum) is collected from the Henan area and separated from the wheat ears with diseases. And searching a pink mould layer on the glume base on the wheat ears, picking the pink mould layer onto a culture medium by using a toothpick, and culturing in a constant-temperature incubator for later use.

Test agent: 95% of flutriafol technical, 95% of hexaconazole technical and 96% of diniconazole technical are provided by a group research and development center.

And (3) preparation of a medicament: the test stock was dissolved in acetone and then diluted with 0.1% tween 80 in water. Preparing single-dose mother liquor respectively, setting 5 series of mass concentrations according to the mixing purpose and the medicament activity, and controlling the final content of the organic solvent to be not more than 2%.

Melting PDA culture medium with microwave oven, cooling to 50deg.C, taking 1mL of prepared medicinal liquid to be tested and 9mL of PDA culture medium according to the principle from low concentration to high concentration, adding into culture dish with diameter of 9cm, mixing, and making into tablet with corresponding concentration.

Inoculating: and (3) beating the cultured pathogenic fungi into fungus cakes by using a puncher with the diameter of 5mm under the aseptic condition, placing the fungus cakes in the central position of a culture medium after the drug-containing culture medium is solidified, sealing a culture dish by using a sealing film, culturing in an incubator at the temperature of 27 ℃, and setting a blank solution without the drug as a blank control, wherein each treatment is repeated three times.

Investigation: the growth of pathogenic hyphae was investigated according to the growth of hyphae in a blank culture dish, and after culturing for 72 hours, colony diameters were measured in centimeters (cm) with calipers. The diameter of each colony was measured vertically by the cross-over method and the average value was taken.

The hypha growth inhibition rate was calculated in percent (%) according to the following formula, and the calculated result remained two bits after the decimal point.

D＝D₁-D₂············(1)

D-colony growth diameter;

d ₁ —colony diameter;

d ₂ -diameter of the fungus cake.

I＝(D₀-D_t)/D₀*100············(2)

Wherein:

i, hypha growth inhibition rate;

d ₀ —a control colony growth diameter;

D _t —agent treated colony growth diameter.

Statistical analysis: and (3) carrying out regression analysis according to the concentration logarithmic value of each medicament and the corresponding hypha growth inhibition rate value, calculating the EC ₅₀ equivalent value of each medicament, and evaluating the activity of the test medicament on the biological test material according to the correlation coefficient R.

Grand cloud Pei method: evaluating the synergistic effect of the mixed medicaments according to the co-toxicity coefficient (CTC), wherein the compounded co-toxicity coefficient CTC is more than or equal to 120 and shows the synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.

The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):

Wherein:

ati—actual measured virulence index of the mixture;

S-EC ₅₀ of standard bactericide in milligrams per liter (mg/L);

M-EC ₅₀ of the mixture in milligrams per liter (mg/L).

TTI＝TI_A ^*P_A+TI_B ^*P_B·······(4)

Wherein:

TTI-the theoretical toxicity index of the mixture;

TI _A A agent toxicity index;

the percentage content of the P _A -A medicament in the mixture is expressed as percentage (%);

TI _B -agent toxicity index;

the percentage of the P _B -B medicament in the mixture is expressed as percentage (%).

Wherein:

Ctc—co-toxicity coefficient;

ati—actual measured virulence index of the mixture;

TTI-the theoretical toxicity index of the mixture.

Example 1

Cyclobutrifluram and flutriafol indoor biological assay for preventing and treating wheat scab

The results in Table 1 show that the EC ₅₀ of Cyclobutrifluram for preventing and treating wheat scab is 4.424mg/L, the EC ₅₀ of the flutriafol for preventing and treating wheat scab is 4.139mg/L, the Cyclobutrifluram and flutriafol sterilization compositions 1:35-30:1 all show good prevention effect, and the Cyclobutrifluram and flutriafol sterilization compositions 1:20-30:1 have co-toxicity coefficients of more than 120 and all show synergistic effect. Wherein, the maximum co-toxicity coefficient value of Cyclobutrifluram and flutriafol=1:1 is 203.752 & gt 120, and EC ₅₀ is 2.099mg/L, which shows synergistic effect.

Table 1 Cyclobutrifluram results of measuring synergistic effects of different proportions of flutriafol on wheat scab

Test agent	Regression equation	r²	EC₅₀			Co-toxicity coefficient	Action
								Biopesticide	B value.+ -. Standard error	/	(mg/L)	(ATI)	(TTI)	(CTC)	/
Cyclobutrifluram(A)	1.346±0.186	0.972	4.424(3.387～5.778)	100.000	/	/	/
								Flutriafol (B)	1.424±0.180	0.976	4.139(3.244～5.280)	106.886	/	/	/
A:B＝1:35	1.487±0.226	0.966	4.768(3.541～6.420)	92.785	106.694	86.964	Additive effect
								A:B＝1:20	1.907±0.159	0.989	2.951(2.512～3.466)	149.915	106.558	140.689	Synergistic effect
A:B＝1:12	1.996±0.215	0.983	2.669(2.151～3.313)	165.755	106.356	155.849	Synergistic effect
								A:B＝2:9	1.954±0.166	0.989	2.329(1.974～2.747)	189.953	105.634	179.822	Synergistic effect
A:B＝1:1	2.025±0.068	0.998	2.099(1.966～2.241)	210.767	103.443	203.752	Synergistic effect
								A:B＝2:1	2.049±0.192	0.987	2.424(2.017～2.913)	182.508	102.295	178.413	Synergistic effect
A:B＝5:1	2.092±0.263	0.977	2.596(2.021～3.335)	170.416	101.148	168.482	Synergistic effect
								A:B＝10:1	1.958±0.208	0.983	2.997(2.444～3.676)	147.614	100.626	146.696	Synergistic effect
A:B＝24:1	1.633±0.167	0.984	3.145(2.582～3.829)	140.668	100.275	140.281	Synergistic effect
								A:B＝30:1	1.805±0.191	0.983	3.503(2.849～4.307)	126.292	100.222	126.012	Synergistic effect

Note that: the above data were analyzed using DPS statistical analysis software, with values kept 3 bits after the decimal point, as in tables 2 and 3 below.

Example 2

Cyclobutrifluram and hexaconazole indoor biological assay for preventing and treating wheat scab

The results in Table 2 show that EC ₅₀ of hexaconazole for preventing and treating wheat scab is 2.208mg/L, cyclobutrifluram and hexaconazole sterilization composition 1:30-24:1 all show good prevention effect, and Cyclobutrifluram and hexaconazole sterilization composition 1:16-24:1 have co-toxicity coefficients of more than 120 and all show synergistic effect. Wherein, the maximum co-toxicity coefficient value of Cyclobutrifluram and hexaconazole=2:1 is 220.817 & gt 120, and EC ₅₀ is 1.491mg/L, which shows synergistic effect.

Table 2 Cyclobutrifluram results of measuring synergistic effects of different proportions of hexaconazole on wheat scab

Example 3

Cyclobutrifluram and diniconazole indoor biological assay for preventing and treating wheat scab

The results in Table 3 show that EC ₅₀ of diniconazole for preventing and treating wheat scab is 1.810mg/L, cyclobutrifluram and diniconazole sterilization composition 1:20-35:1 all show good prevention effect, and Cyclobutrifluram and diniconazole sterilization composition 1:20-25:2 co-toxicity coefficient is more than 120, and the synergistic effect is shown. Wherein, the total toxicity coefficient value of Cyclobutrifluram and diniconazole=5:2 is the maximum and is 217.892 to be more than 120, EC ₅₀ is 1.450mg/L, and the synergy is obvious.

Table 3 Cyclobutrifluram results of the determination of the synergism of different proportions of diniconazole on wheat scab

Test agent	Regression equation	r²	EC₅₀			Co-toxicity coefficient	Action
								Biopesticide	B value.+ -. Standard error	/	(mg/L)	(ATI)	(TTI)	(CTC)	/
Cyclobutrifluram(A)	1.400±0.1575	0.981	4.502(3.6216～5.597)	100.000	/	/	/
								Diniconazole (B)	1.269±0.1256	0.985	1.810(1.495～2.191)	248.729	/	/	/
A:B＝1:20	1.501±0.1061	0.992	1.498(1.300～1.726)	300.534	241.647	124.369	Synergistic effect
								A:B＝2:25	1.505±0.1147	0.991	1.447(1.240～1.688)	311.126	237.712	130.884	Synergistic effect
A:B＝1:10	1.667±0.0742	0.997	1.249(1.136～1.374)	360.448	235.208	153.246	Synergistic effect
								A:B＝1:2	1.624±0.0662	0.997	1.278(1.173～1.393)	352.269	199.153	176.884	Synergistic effect
A:B＝5:4	1.525±0.085	0.995	1.373(1.224～1.540)	327.895	166.102	197.406	Synergistic effect
								A:B＝5:2	1.562±0.1039	0.993	1.450(1.268～1.659)	310.483	142.494	217.892	Synergistic effect
A:B＝5:1	1.436±0.1734	0.978	2.177(1.725～2.747)	206.798	124.788	165.719	Synergistic effect
								A:B＝12:1	1.500±0.0831	0.995	2.503(2.2464～2.788)	179.864	111.441	161.399	Synergistic effect
A:B＝25:2	1.552±0.1241	0.990	2.767(2.3718～3.220)	162.703	111.017	146.557	Synergistic effect
								A:B＝35:1	1.579±0.1142	0.992	3.71 0(3.227～4.264)	121.348	104.131	116.533	Additive effect

Formulation examples

Preparation example 1:

40% Cyclobutrifluram. Flutriafol wettable powder (20:20)

Active component A Cyclobutrifluram is 20%, active component B flutriafol is 20%, wetting agent alkyl naphthalene sulfonate is 5.5%, dispersing agent naphthalene formaldehyde condensate sodium sulfonate is 6%, kaolin is 10%, and swelling soil is filled up to 100%. The active ingredients and the auxiliary agents are uniformly mixed, put into a mechanical pulverizer for primary pulverization, pulverized by an air flow pulverizer and uniformly mixed to obtain the 40% Cyclobutrifluram-flutriafol wettable powder.

Preparation example 2:

42% Cyclobutrifluram. Diniconazole wettable powder (30:12)

Active ingredient A Cyclobutrifluram%, active ingredient B diniconazole 12%, wetting agent alkyl naphthalene sulfonate 8%, dispersant naphthalene formaldehyde condensate sodium sulfonate 4%, kaolin 15%, bulking soil complement to 100%. The active ingredients and the auxiliary agents are uniformly mixed, put into a mechanical pulverizer for primary pulverization, pulverized by an air flow pulverizer and uniformly mixed to obtain the 42% Cyclobutrifluram-diniconazole wettable powder.

Preparation example 3:

30% Cyclobutrifluram. Flutriafol suspending agent (16:14)

Active ingredient A Cyclobutrifluram%, active ingredient B flutriafol 14%, wetting agent lignosulfonate 6%, dispersant alkyl naphthalene formaldehyde condensate sodium sulfonate 2.5%, antifreeze glycol 5%, thickener xanthan gum 0.1%, magnesium aluminium silicate 0.25% and deionized water to 100%. Adding the active ingredients, a wetting agent, a dispersing agent, an antifreezing agent and water into a stirring kettle, fully stirring, crushing the materials by a sand mill until D ₉₀ (the particle size of 90% of particles) is less than 10 mu m, pumping the materials into a high-speed shearing machine after grinding, adding a thickening agent, and shearing at high speed to obtain the 30% Cyclobutrifluram-flutriafol suspending agent after shearing.

Preparation example 4:

21% Cyclobutrifluram. Hexaconazole suspending agent (14:7)

Active component A Cyclobutrifluram%, active component B hexaconazole 7%, wetting agent lignosulfonate 4.5%, dispersant alkyl naphthalene formaldehyde condensate sodium sulfonate 3%, antifreezing agent glycol 5%, thickener organic bentonite 0.1%, magnesium aluminum silicate 0.2%, and deionized water to 100%. Adding the active ingredients, a wetting agent, a dispersing agent, an antifreezing agent and water into a stirring kettle, fully stirring, crushing the materials by a sand mill until D ₉₀ (the particle size of 90% of particles) is less than 10 mu m, pumping the materials into a high-speed shearing machine after grinding, adding a thickening agent, and shearing at high speed to obtain the 21% Cyclobutrifluram-hexaconazole suspending agent after shearing.

Preparation example 5:

24% Cyclobutrifluram diniconazole suspending agent (15:9)

Active component A Cyclobutrifluram%, active component B diniconazole 9%, wetting agent lignosulfonate 4.5%, dispersant alkyl naphthalene formaldehyde condensate sodium sulfonate 3.5%, antifreezing agent glycol 1%, glycerin 2.5%, thickener magnesium aluminum silicate 0.2% and deionized water to 100%. Adding the active ingredients, a wetting agent, a dispersing agent, an antifreezing agent and water into a stirring kettle, fully stirring, crushing the materials by a sand mill until D ₉₀ (the particle size of 90% of particles) is less than 10 mu m, pumping the materials into a high-speed shearing machine after grinding, adding a thickening agent, and shearing at high speed to obtain the 24% Cyclobutrifluram-diniconazole suspending agent after shearing.

Preparation example 6:

35% Cyclobutrifluram. Flutriafol dispersible oil suspension (15:20)

Active component A Cyclobutrifluram%, active component B flutriafol 20%, emulsifier calcium dodecyl benzene sulfonate 2.5%, alkylphenol formaldehyde resin polyoxyethylene 3%, dispersant alkylphenol polyoxyethylene 4.5%, thickener xanthan gum 2% and corn oil up to 100%. Sequentially placing the active ingredients, the surfactant and other functional additives into a reaction kettle, adding oil, uniformly mixing, shearing at high speed, sanding by a wet method, and finally homogenizing and filtering to obtain the 35% Cyclobutrifluram-flutriafol dispersible oil suspending agent.

Field efficacy test

Wheat scab field efficacy test

Test site: planting field for wheat planting in Hebei province all year round

Test time: wheat heading period of 5-12 days 2020

Test agent and dosage: the dosage is shown in Table 4.

Table 4 comparison of the amounts of the field test drugs

Test treatment: setting single dose and clear water contrast, and setting the application interval of 2 times for 10 days, wherein the spraying time is respectively the initial spike period and the flowering period of wheat. Cell trials were repeated for each treatment area 667m ². Spraying by using a conventional electric sprayer.

The investigation method comprises the following steps: a 5-point sampling site-directed investigation was used. 1m ² was investigated per treatment point and the total spike number and the number of diseased spikes was investigated 10 days before harvesting. The severity of the illness is divided by the illness state of wheat ears, and the illness state is divided into 5 grades:

Grade 0, no disease;

1 grade, the number of diseased wheat ears is less than 1/4 of the total wheat ears;

2, the number of diseased wheat ears accounts for 1/4 to 1/2 of the total wheat ears;

grade 3, the number of diseased wheat ears accounts for 1/2-3/4 of the total wheat ears;

grade 4, the number of diseased wheat ears is more than 3/4 of the total wheat ears.

Calculating the disease index according to the disease index = Σ (number of disease plants at each stage x the disease grade value)/(total number of investigation x maximum grade value);

calculating the control effect according to the control effect= (control disease index-treatment disease index)/control disease index;

The average spike number and the disease spike rate of 1m ² are calculated according to the unit area.

Samples were taken during the harvest period of wheat and after 3d of air-drying the measured yields of 667m ² per cell were determined.

Data were processed with Microsoft Excel 2003 and statistically analyzed with DPS data and checked for difference significance (Duncan method).

Example 4

Results of field efficacy test of wheat scab

The results in Table 5 show that the investigation results of 10d before harvest show that the control effects of 40% Cyclobutrifluram. Flutriafol wettable powder (20:20), 21% Cyclobutrifluram. Flutriafol suspending agent (14:7) and 24% Cyclobutrifluram. Diniconazole suspending agent (15:9) on wheat scab are 81.89%, 83.18% and 82.97% respectively; at the level of 0.01 and the level of 0.05, the three mixed medicaments have no obvious difference in preventing and treating wheat scab; compared with the control single agent 24% of the Cyclobutrifluram suspending agent, 250 g/liter of the flutriafol suspending agent, 30% of the hexaconazole suspending agent and 12.5% of the diniconazole wettable powder, the mixed preparation is obviously higher than the control single agent.

Table 5 different formulations and single dose for preventing and treating wheat scab

Note that: the processing data are calculated to be 1m ² average spike number and disease spike rate according to unit area; the% control effect in the above table is the average of each repetition; lower case letters represent a significant 5% level difference and upper case letters represent a significant 1% level difference.

TABLE 6 influence of different agents for controlling wheat scab on wheat yield

Note that: the yields in the above table are the average of each replicate; lower case letters represent a significant difference in 5% levels.

The test results of the field efficacy plot show that Cyclobutrifluram, flutriafol, hexaconazole and diniconazole are compounded in the wheat scab control process, so that the disease spike rate and the disease index are reduced, the remarkable control effect is achieved, the yield is not greatly influenced, and the mixed preparation also has an obvious yield increasing effect.

In addition, according to observation after the medicine, the wheat growth in each treatment area is normal, and no phytotoxicity phenomenon occurs, which indicates that the wheat growth of each medicine is safe under the test dosage.

Through indoor toxicity measurement and field experiments, the Cyclobutrifluram and any one of the composition selected from flutriafol, hexaconazole and diniconazole provided by the invention have very good control effect on wheat scab. The bactericidal composition or the preparation thereof obtained by compounding has remarkable prevention effect, and has the characteristics of high efficiency, broad spectrum, low residue, long lasting period, strong systemic property and the like; in addition, no phytotoxicity of the compound medicament to crops is found in the test, which proves that the production cost and the use cost can be reduced and the compound medicament is safe to crops under the condition that the sterilizing synergistic effect of the obtained sterilizing composition or preparation is improved.

While the invention has been described in detail in terms of the general description and the specific embodiments, it will be apparent to those skilled in the art that various modifications and improvements can be made thereto without departing from the spirit of the invention.

Claims

1. A sterilization composition containing triazole compounds is characterized in that: comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound shown as a formula (I) The active component B is triazole compound; the triazole compound is selected from any one of flutriafol, hexaconazole and diniconazole.

2. The bactericidal composition of claim 1, wherein the mass ratio of active ingredient a to active ingredient B is from 35:1 to 1:35.

3. The bactericidal composition of claim 1, wherein the mass ratio of the compound of formula (I) to flutriafol is 1:35-30:1; the mass ratio of the compound of the formula (I) to hexaconazole is 1:30-24:1; the mass ratio of the compound of the formula (I) to diniconazole is 1:20-35:1.

4. The bactericidal composition according to claim 1, wherein the mass ratio of the compound of formula (I) to flutriafol is 1:20-30:1; the mass ratio of the compound of the formula (I) to hexaconazole is 1:16-24:1; the mass ratio of the compound of the formula (I) to diniconazole is 1:20-25:2.

5. A bactericidal composition according to claim 1, characterized in that the sum of the contents of active ingredient a and active ingredient B in the bactericidal composition is 1-90 wt%, preferably 5-80 wt%, based on 100wt% of the total weight of the bactericidal composition.

6. The composition of claim 1, wherein the composition further comprises agriculturally acceptable auxiliary ingredients in addition to the active ingredient, the auxiliary ingredients being selected from one or more of wetting agents, dispersing agents, emulsifying agents, thickening agents, disintegrating agents, freezing point depressants, antifoaming agents, solvents, preservatives, stabilizers, synergists, binders, or carriers.

7. The bactericidal composition of claim 6, wherein the dosage form of the bactericidal composition is selected from a solid formulation and/or a liquid formulation and/or a seed treatment formulation.

8. The bactericidal composition of claim 7, wherein the bactericidal composition is formulated into a pesticidally acceptable formulation, the formulation being a microemulsion, an aqueous emulsion, a suspension, a dispersible oil suspension, a solution, an emulsifiable concentrate, a suspoemulsion, a microencapsulated suspension, a water dispersible granule, a wettable powder, a granule, a seed treatment suspension, a seed treatment dry powder;

Preferably, the preparation formulation is microemulsion, emulsifiable concentrate, suspending agent, aqueous emulsion, water dispersible granule and seed treatment suspending agent.

9. Use of the fungicidal composition as claimed in any one of claims 1 to 8 for controlling plant diseases.

10. The use according to claim 9, wherein the plant disease is a fungal or bacterial caused plant disease;

preferably, the plant disease is a fungal plant disease;

still more preferably, the fungal plant disease is wheat scab.