CN109169675A - A kind of bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate - Google Patents

A kind of bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate Download PDF

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CN109169675A
CN109169675A CN201811147294.5A CN201811147294A CN109169675A CN 109169675 A CN109169675 A CN 109169675A CN 201811147294 A CN201811147294 A CN 201811147294A CN 109169675 A CN109169675 A CN 109169675A
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fluxapyroxad
copper
hydroxyquinolinate
apple
disease
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CN109169675B (en
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郑敬敏
张仙
黄发伟
李存治
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Shaanxi Sunger Road Bio Science Co Ltd
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Shaanxi Sunger Road Bio Science Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • A01N43/42Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings

Abstract

The invention discloses the bactericidal compositions and its application of a kind of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate, effective active composition is made of the first active constituent fluxapyroxad and the second active constituent copper 8-hydroxyquinolinate, the weight ratio of first active constituent and the second active constituent is 1:60~60:1, preferably 1:20~10:1.This composition can be configured to the suspending agent agriculturally allowed, microemulsion, aqueous emulsion, dispersible oil-suspending agent, wettable powder, dosage form of water dispersible granule.Instant component is reasonable, and bactericidal effect is good, and its activity and bactericidal effect are not the active simple superposition of each component, compared with existing single formulation, in addition to significant bactericidal effect, and have significant synergistic effect, good to crop safety.The present invention has significant control efficiency to citrus and apple disease.

Description

A kind of bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate
Technical field
The present invention relates to a kind of bactericidal compositions, by the first active constituent fluxapyroxad and the second active constituent copper 8-hydroxyquinolinate And auxiliary agent composition, belong to technical field of compounded pesticide.
Background technique
Fluxapyroxad, English name fluxapyroxad, chemical name are 3- (difluoromethyl) -1- methyl-N- (3,4,5- Trifluoro [1,1- bis- benzene] -2- base)) -1H- pyrazole-4-carboxamide.It is acid amide fungicides, it is main by inhibiting mitochondrial succinate Acid esters dehydrogenase hinders tricarboxylic acid cycle, lacks amino acid, sugar, energy reduction, interferes the division and growth of cell, have Protection and therapeutic effect.Powdery mildew, gray mold to gourd, fruit and vegetable class crop, rice sheath blight disease is efficient, to fruit tree anthracnose There is greater activity.
Copper 8-hydroxyquinolinate, English name oxine-copper, be a kind of wide spectrum, efficiently, organic copper chelate of low-residual, to true The virus such as bacterium, bacillary has good preventive and therapeutic action.By forming one layer of strict protective film in crop surface, inhibit Germ sprouts and intrusion, thus so as to achieve the aim of preventing and treating diseases to crop safety.
Applicant is through retrieving, and there is presently no the document reports of fluxapyroxad and copper 8-hydroxyquinolinate mixture, further passes through examination It issues after examination and approval now, by the different fluxapyroxad of the mechanism of action and oxine-copper composite, prevents and treats citrus and apple disease with unexpected Effect, synergistic effect is significant, dosage reduce, control cost reduce, to crop safety.
Summary of the invention
The purpose of the present invention is to provide a kind of synergistic effect is significant, bactericidal effect is good, and drug cost is low, to crop safety Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate bactericidal composition.
Another object of the present invention is to provide the bactericidal composition preparation formulations of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate.
A further object of the present invention is to provide application of the above-mentioned composition on prevention and treatment citrus and apple disease.
In order to overcome the defect of existing single formulation, the technical scheme is that solve in this way:
A) the first active constituent fluxapyroxad;
B) the second active constituent copper 8-hydroxyquinolinate;
The weight ratio of first active constituent and the second active constituent is 1:60~60:1, preferably 1:20~10:1.
A kind of bactericidal composition containing fluxapyroxad and copper 8-hydroxyquinolinate of the present invention, according to those skilled in the art of the present technique institute The preparation formulation that well known method can be prepared be suspending agent, microemulsion, aqueous emulsion, dispersible oil-suspending agent, wettable powder, Water dispersible granules.
To suspending agent, workable auxiliary agent has: dispersing agent such as polycarboxylate, lignosulfonates, alkyl naphthalene formaldehyde condensation Object sulfonate, alkylphenol-polyethenoxy base ether phosphate, alkylphenol polyoxyethylene ether sulfonate, phenethyl phenol polyoxyethylene groups Ether phosphate, alkyl polyoxyethylene ether sulfonate, polyoxyethylene polyoxypropylene base ether block copolymers, pull open powder, dodecyl One of polyoxyethylene ether phosphate etc. is a variety of;Wetting agent such as alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, Phenethyl phenol polyoxyethylene groups ether phosphate, alkyl sulfate, alkylsulfonate, alkylnaphthalene sulfonate, alkylphenol-formaldehyde resin In polyoxyethylene ether, one of triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer etc. or a variety of;Thickener is such as One in xanthan gum, polyvinyl alcohol, bentonite, aluminium-magnesium silicate, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose etc. Kind is a variety of;One of preservative such as formaldehyde, benzoic acid, sodium benzoate, potassium sorbate, isothiazolinone etc. is a variety of;Disappear Infusion such as silicone oil, silicone compound, C10-20 saturated fat acid compounds, C8-10 fatty alcohols, hexanol, butanol, octanol Deng one of or it is a variety of;Antifreezing agent such as ethylene glycol, propylene glycol, glycerine, polyethylene glycol, sorbierite, urea, inorganic salts etc. One of or it is a variety of;Water is deionized water.
To microemulsion, workable auxiliary agent has: emulsifier such as agriculture breast 500#(calcium dodecyl benzene sulfonate), Nongru-700 #, Agriculture breast 2201, this disk-60#, polysorbate60-#, TX-10, agriculture breast 1601(phenethyl phenol polyoxyethylene poly-oxygen propylene aether), agriculture breast One of 600#, agriculture breast 400# etc. or a variety of;One of assistant for emulsifying agent such as methanol, isopropanol, n-butanol, ethyl alcohol etc. is more Kind;Solvent such as cyclohexanone, N-Methyl pyrrolidone, dimethylbenzene, toluene, in solvent naphtha (trade mark: S-150, S-180, S-200) It is one or more;One of stabilizer such as triphenyl phosphite, epoxychloropropane etc. is a variety of;Water is deionized water.
To aqueous emulsion, workable auxiliary agent has: emulsifier such as Nonyl pheno (EO=10) ether phosphate, triphen second Base phenol polyoxyethylene phosphonate, Nongru-700 #(alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201#, this disk -60# (Span60), Tween-60 #(polyoxyethylene sorbitan stearate), TX-10(octyl phenol polyoxy second Alkene (10) ether), agriculture breast 1601(triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer), agriculture breast 600#, agriculture breast 400# Deng one of or it is a variety of;Solvent such as dimethylbenzene, toluene, cyclohexanone, in solvent naphtha (trade mark: S-150, S-180, S-200) It is one or more;One of stabilizer such as triphenyl phosphite, epoxychloropropane, epoxidized soybean oil etc. is a variety of;It is antifreeze One of agent such as ethylene glycol, propylene glycol, glycerol, urea, inorganic salts such as sodium chloride etc. is a variety of;Thickener such as xanthan gum, One of polyvinyl alcohol, bentonite, aluminium-magnesium silicate etc. are a variety of;Preservative such as formaldehyde, benzoic acid, one in sodium benzoate Kind is a variety of, and water is deionized water.
To dispersible oil-suspending agent, workable auxiliary agent has: dispersing agent such as polycarboxylate, lignosulfonates, alkylnaphthalene Sulfonate (dispersing agent NNO), the U.S. TERSPERSE 2020(Huntsman Corporation HUNTSMAN produce, alkyl naphthalene sulfonic acid salt) etc. One of or it is a variety of;Emulsifier such as BY(castor oil polyoxyethylene ether) series emulsifier (BY-110, BY-125, BY-140), Nongru-700 #(alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201, this disk -60#(common name: sorbitol anhydride monostearate Ester), Tween-60 #(sorbitan monostearate polyoxyethylene ether), agriculture breast 1601#(phenethyl phenol polyoxyethylene polyoxy Propylene ether), TERSPERSE 4894(Huntsman Corporation of the U.S. produce) etc. one of or it is a variety of;Wetting agent such as alkyl phenol polyoxy Vinyl ethers formaldehyde condensation products sulfate, alkyl phenol polyoxyethylene ether phosphate, phenethyl phenol polyoxyethylene groups ether phosphate, alkane Base sulfate, alkylsulfonate, naphthalene sulfonate, TERSPERSE 2500(Huntsman Corporation of the U.S. produce) etc. one of or it is more Kind;One of thickener such as white carbon black, polyvinyl alcohol, bentonite, aluminium-magnesium silicate etc. is a variety of;Antifreezing agent such as ethylene glycol, third One of glycol, glycerol, urea, inorganic salts such as sodium chloride etc. is a variety of;Decentralized medium such as soybean oil, rapeseed oil, corn One of oil, methyl oleate, diesel oil, machine oil, mineral oil etc. are a variety of.
To wettable powder, workable auxiliary agent has: dispersing agent such as polycarboxylate, lignosulfonates, polyoxyethylene is poly- Oxypropylene group ether block copolymers, alkyl naphthalene formaldehyde condensate sulfonate, alkylphenol-polyethenoxy base ether phosphate, poly alkyl alcohol One of ethylene oxide ether phosphate, alkylphenol polyoxyethylene ether sulfonate etc. are a variety of;Wetting agent such as alkyl sulfate, alkane One of base sulfonate, alkylnaphthalene sulfonate etc. are a variety of;Filler such as ammonium sulfate, urea, sucrose, glucose, diatomite, height One of ridge soil, white carbon black, light calcium, talcum powder, attapulgite, clay etc. are a variety of.
For water dispersible granules, workable auxiliary agent has: dispersing agent such as polycarboxylate (TERSPERSE 2700, T36, GY- D06 etc.), lignosulfonates, one of alkylnaphthalene sulfonate etc. or a variety of;Wetting agent such as alkyl sulfate, alkyl sulfonic acid One of salt, naphthalene sulfonate etc. are a variety of;Disintegrating agent such as ammonium sulfate, sodium sulphate, polyvinylpyrrolidone, starch and its derivative One of object, bentonite etc. are a variety of;Binder such as starch, glucose, polyvinyl alcohol, polyethylene glycol, carboxymethyl cellulose One of sodium, sucrose etc. are a variety of;Filler such as diatomite, kaolin, white carbon black, light calcium, talcum powder, attapulgite, clay Deng one of or it is a variety of.
Instant component is reasonable, and treatment plus protective effect, bactericidal effect is good, and drug cost is low, and its activity and sterilization effect The active simple superposition of fruit not instead of each component, there is significant synergistic effect, good to crop safety, meets pesticidal preparations Security requirement.The present invention has excellent control efficiency to the disease on citrus and apple.
Specific embodiment
Illustrate whether fluxapyroxad and copper 8-hydroxyquinolinate mixture have synergistic effect below by indoor toxicity test.
1, the synergy of citrus bacterial canker disease is measured.
Using the method for plate culture count, people's sterile water is added to scrape lawn after cultivating 40h on slant medium for examination bacterium Bacterium solution is made, vibrates 120s through high-speed oscillator, then be diluted to the suspension of about 50/mL of thallus number with sterile water;It will prepare Reagent agent dilution 2mL move into sterile petri dish, bacterial suspension 1.0mL is accurately added with pipette, then It is poured into NT culture medium (40-50 DEG C of liquid temperature) 10mL of thawing, shaken cultivation ware is sufficiently mixed medical fluid, thallus and culture medium, coagulates Gu 16h is cultivated under 25 DEG C of constant temperature after, detects by an unaided eye and counts the single colonie number of each processing;Each drug concentration is arranged 4 It repeats, and blank control is made with sterile water.
Bacterium colony inhibiting rate is calculated as follows:
Bacterium colony inhibiting rate (%)=(control clump count-processing clump count)/control clump count × 100.
Clump count inhibiting rate is converted into probit value, drug concentration is converted into logarithm, find out EC50 with least square method Value.Then co-toxicity coefficient (CTC) is calculated by Sun Yunpei's Method.
Survey toxicity index (ATI)=(standard agent EC50/ reagent agent EC50)×100;
In theoretical toxicity index (TTI)=A medicament toxicity index × mixture in percentage composition+B medicament toxicity index × mixture of A The percentage composition of B;
Co-toxicity coefficient (CTC)=[mixture surveys toxicity index (ATI)/mixtures theoretical toxicity index (TTI)] × 100.
When CTC≤80, then composition shows as antagonism, and as 80 < CTC < 120, then composition shows as being added and make With when CTC >=120, then composition shows as synergistic effect.
1 fluxapyroxad of table and copper 8-hydroxyquinolinate combine the indoor toxicity test to citrus bacterial canker disease
The Toxicity Determination result shows: fluxapyroxad is mixed to c itrus canker for 1:80~80:1 with weight ratio with copper 8-hydroxyquinolinate Disease has preferable virulence, and weight ratio is that 1:60~60:1 shows as synergistic effect, and 1:20~10:1 synergistic effect is especially pronounced.
2, the synergy of citrus scab is measured.
In order to prevent and treat the citrus scab in agricultural production, we have carried out mutual compounding with fluxapyroxad and copper 8-hydroxyquinolinate Synergy research, subjects be citrus scab (Sphaceloma fawcettii).Raw medicine is configured to the test needed Medicament, 5 various concentration gradients are arranged in single dose and each Mixed Pharmacy, and (on the basis of preliminary experiment result, bacteriostasis rate is 5% It is set in the range of~90% by geometric progression).If clear water compares, it is repeated 4 times.
Test uses mycelial growth rate method, is aseptically 5 mm punching with diameter by cultured pathogen Device cuts bacteria cake from colony edge, and bacteria cake is connected on the culture medium flat plate of different agents concentration with transfer needle, sets 25 DEG C, satisfies It is cultivated in humidity incubator;When control group bacterium colony covers with, colony diameter is measured, each chemicals treatment is calculated and inhibits mycelia growth Percentage finds out the EC of each medicament by the linear regression analysis between the probit value of inhibiting rate and the logarithm of series of concentrations50 Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 < CTC < 120 shows as summation action.
2 fluxapyroxad of table and copper 8-hydroxyquinolinate combine the indoor toxicity test to citrus scab
The Toxicity Determination result shows: fluxapyroxad is mixed to citrus scab for 1:80~80:1 with weight ratio with copper 8-hydroxyquinolinate Disease has preferable virulence, and weight ratio is that 1:60~60:1 shows as synergistic effect, and 1:20~10:1 synergistic effect is especially pronounced.
3, the synergy of apple disease is measured.
In order to prevent and treat the apple disease in agricultural production, we have carried out mutual compounding with fluxapyroxad and copper 8-hydroxyquinolinate Synergy research, subjects be alternaria leaf spot of apple (Alternaria alternaria f.sp mali), ring rot of apple (Botryospuaeria berengeriana), canker of apple fruit (Valsa mali), apple marssonina leaf spot (Diplocarpon mali ).Raw medicine is configured to the test medicine needed, 5 various concentration gradients are arranged (pre- in single dose and each Mixed Pharmacy On the basis of standby test result, bacteriostasis rate is set in the range of 5%~90% by geometric progression).If clear water compares, it is repeated 4 times.
Test uses mycelial growth rate method, is aseptically 5 mm punching with diameter by cultured pathogen Device cuts bacteria cake from colony edge, and bacteria cake is connected on the culture medium flat plate of different agents concentration with transfer needle, sets 28 DEG C, satisfies It is cultivated in humidity incubator;When control group bacterium colony covers with, colony diameter is measured, each chemicals treatment is calculated and inhibits mycelia growth Percentage finds out the EC of each medicament by the linear regression analysis between the probit value of inhibiting rate and the logarithm of series of concentrations50 Value calculates the co-toxicity coefficient (CTC) of mixture with Sun Yunpei's Method, evaluates reagent agent to the activity of germ with this.
The co-toxicity coefficient (CTC) >=120 of compound preparation shows as synergistic effect;CTC≤80 show as antagonism;80 < CTC < 120 shows as summation action.
Table 2-1 fluxapyroxad and copper 8-hydroxyquinolinate combine the indoor toxicity test to alternaria leaf spot of apple
Table 2-2 fluxapyroxad and copper 8-hydroxyquinolinate combine the indoor toxicity test to ring rot of apple
Table 2-3 fluxapyroxad and copper 8-hydroxyquinolinate combine the indoor toxicity test to canker of apple fruit
Table 2-4 fluxapyroxad and copper 8-hydroxyquinolinate combine the indoor toxicity test to apple marssonina leaf spot
The Toxicity Determination result shows: fluxapyroxad is mixed to apple spot for 1:80~80:1 with weight ratio with copper 8-hydroxyquinolinate Defoliation, ring rot of apple, canker of apple fruit, apple marssonina leaf spot have preferable virulence, and weight ratio is that 1:60~60:1 is shown as Synergistic effect, 1:20~10:1 synergistic effect are especially pronounced.
In order to better illustrate the present invention, the content of present invention is described further below with reference to embodiment, in formula Percentage is weight percentage.
Example of formulations 1
Weigh 10% fluxapyroxad, 15% copper 8-hydroxyquinolinate, 8% polycarboxylate, 4% alkyl polyoxyethylene ether sulfonate, 4% alkylsurfuric acid Sodium, 0.8% aluminium-magnesium silicate, 3% sorbierite, 0.5% formaldehyde, 1% silicone oil, deionized water add to 100% parts by weight.Above-mentioned raw materials are through mixed It closes, high speed shear disperses 30min, is sanded with sand mill to partial size D9025% fluxapyroxad copper 8-hydroxyquinolinate is made after less than 10 μm Suspending agent.
Example of formulations 2
Weigh 4% fluxapyroxad, 20% copper 8-hydroxyquinolinate, 5% sodium lignin sulfonate, 6% sodium naphthalene sulfonate, 5% sodium alkyl sulfate, 0.4% poly- Vinyl alcohol, 0.3% bentonite, 4% propylene glycol, 0.2% potassium sorbate, 1% butanol, deionized water add to 100% parts by weight.Above-mentioned original Material is mixed, and high speed shear disperses 30min, is sanded with sand mill to partial size D9024% fluxapyroxad is made after less than 10 μm Copper 8-hydroxyquinolinate suspending agent.
Example of formulations 3
Weigh 5% fluxapyroxad, 150% copper 8-hydroxyquinolinate, 3% agriculture breast, 2201,5% this disk -60#, 12% solvent naphtha S-180,5%N- methyl Pyrrolidones, 4% methanol are dissolved completely and are uniformly mixed, and deionized water adds to 100% parts by weight, and 20% fluorine azoles is made after stirring Bacterium amide copper 8-hydroxyquinolinate microemulsion.
Example of formulations 4
Weigh 10% fluxapyroxad, 20% copper 8-hydroxyquinolinate, 5% agriculture breast 600#, 5% agriculture breast 1601#, 10% dimethylbenzene, 6% toluene, 3% just Butanol is dissolved completely and is uniformly mixed, and deionized water adds to 100% parts by weight, and 30% fluxapyroxad quinoline is made after stirring Quinoline copper microemulsion.
Example of formulations 5
Weigh 10% fluxapyroxad, 15% copper 8-hydroxyquinolinate, 5% agriculture breast 400#, 3% agriculture breast 2201#, 2% this disk -60#, 1% epoxy chloropropionate Alkane, 1% sodium chloride, 3% cyclohexanone, 0.3% bentonite, 0.5% benzoic acid, deionized water add to 100% parts by weight.Above-mentioned raw materials warp 25% fluxapyroxad quinoline aqueous emulsion of copper is made in mixing, high speed shearing emulsification.
Example of formulations 6
Weigh 10% fluxapyroxad, 25% copper 8-hydroxyquinolinate, 4% agriculture breast 1601,2% triphenoethyl benzene phenol polyethenoxy ether phosphate, 4% Tween-60 #, 5% propylene glycol, 6% toluene, 5% cyclohexanone, 0.5% xanthan gum, 0.4% formaldehyde, deionized water add to 100% parts by weight. For above-mentioned raw materials through mixing, 35% fluxapyroxad quinoline aqueous emulsion of copper is made in high speed shearing emulsification.
Example of formulations 7
Weigh 5% fluxapyroxad, 25% copper 8-hydroxyquinolinate, 4% sodium lignin sulfonate, 4% this disk -60#, 7% BY-110,1% naphthalene sulfonic acids Sodium, 0.8% bentonite, 2.5% propylene glycol, corn oil add to 100% parts by weight.Above-mentioned raw materials are through mixing, high speed shear dispersion 30min, 30% fluxapyroxad copper 8-hydroxyquinolinate is made after being sanded with sand mill can be dispersed oil-suspending agent.
Example of formulations 8
Weigh 4% fluxapyroxad, 20% copper 8-hydroxyquinolinate, 5% sodium polycarboxylate, 3% Tween-60 #, 7% agriculture breast 2201#, 5% Nongru-700 #, 1% sodium alkyl sulfonate, 2% aluminium-magnesium silicate, 4% polyvinyl alcohol, soybean oil add to 100% parts by weight.Above-mentioned raw materials are cut at a high speed through mixing Cutting dissipates 30min, and 24% fluxapyroxad copper 8-hydroxyquinolinate is made after being sanded with sand mill can be dispersed oil-suspending agent.
Example of formulations 9
Weigh 4% fluxapyroxad, 24% copper 8-hydroxyquinolinate, 7% sodium polycarboxylate, 4% alkylphenol-polyethenoxy base ether phosphate, 2% dodecane Base sodium sulphate, white carbon black are filled up to 100% parts by weight.Above-mentioned raw materials are through mixing, ultra micro air-flow crushing, hybrid technique step system It is standby to obtain 28% fluxapyroxad copper 8-hydroxyquinolinate wettable powder.
Example of formulations 10
Weigh 5% fluxapyroxad, 30% copper 8-hydroxyquinolinate, 5% aliphatic alcohol polyoxyvinethene phosphate, the contracting of 6% alkylnaphthalene sulfonate formaldehyde Object, 2% Negel are closed, diatomite is filled up to 100% parts by weight.Above-mentioned raw materials are through mixing, ultra micro air-flow crushing, mixing Processing step is prepared into 35% fluxapyroxad copper 8-hydroxyquinolinate wettable powder.
Example of formulations 11
Weigh 15% fluxapyroxad, 30% copper 8-hydroxyquinolinate, 4% sodium lignin sulfonate, (the alkylnaphthalene sulfonate formaldehyde contracting of 5% dispersing agent NNO Close object), 2% nekal, 3% lauryl sodium sulfate, kaolin adds to 100% parts by weight.The frequent regulation of above-mentioned raw materials The method of water intaking dispersible granule i.e. mixing, ultra micro air-flow crushing, mixing, granulation step produces 45% fluxapyroxad copper 8-hydroxyquinolinate Water dispersible granules.
Example of formulations 12
Weigh 10% fluxapyroxad, 25% copper 8-hydroxyquinolinate, 4% polycarboxylate T36,6% Negel, 1.5% dibutyl naphthalenesulfonic acid Sodium, 2%K lauryl sodium sulfate, 1% sodium carboxymethylcellulose, 2% glucose, light calcium add to 100% parts by weight.Above-mentioned raw materials warp The method that routine produces water dispersible granules mixes, ultra micro air-flow crushing, mixing, granulation step produce 35% fluxapyroxad Quinoline copper water dispersion granula.
Biological Examples 1: prevention and treatment citrus bacterial canker disease field trial.
Carry out example of formulations 1(25% fluxapyroxad copper 8-hydroxyquinolinate suspending agent in Jiangxi Nanfeng County within 2018), preparation it is real Apply a 3(20% fluxapyroxad copper 8-hydroxyquinolinate microemulsion) prevention and treatment citrus bacterial canker disease field trial.
Test method is referring to " GBT 17980.103-2004 pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating mandarin orange Tangerine canker ".Using randomized blocks, 4 repetitions of every processing, every cell is for 3 plants of examination tree.Rear 14d is spent to spray the 1st medicine in thanking, Then it is spaced 7 days and sprays the 2nd, 3 medicine respectively.Application is spraying using hand backpack compression sprayer, after each application of guarantee for 24 hours Without rain, if rain to add in time.It uniformly sprays to blade, fruit, medical fluid is spent to being intended to drip.
Before application, in every cell fixed point 3 plants of trees of selection, every plant of tree investigates citrus bacterial canker disease in 4 azimuth mark tender tips Incidence is investigated the scab number on 100 blades and 50 fruits altogether, and is classified, and disease index is calculated.After last application 7 and 14d carries out investigation to 100 blades and 50 fruit incidences that mark in tender tip respectively again and to incidence of leaf (fruit It is real) it is classified, calculate disease index and preventive effect.With blade (or fruit) for unit, disease grade standard is as follows:
0 grade, disease-free spot;
L grades, every leaf (or fruit) has scab l-5;
3 grades, every leaf (or fruit) has scab 6-10;
5 grades, every leaf (or fruit) has scab 11-15;
7 grades, every leaf (or fruit) has scab 16-20;
9 grades, every leaf (or fruit) has scab 21 or more.
Disease index and control efficiency calculation method:
Disease index=Σ (the disease numbers of sheets at different levels × opposite value of series)/(investigation total number of sheets × 9) × 100
Control efficiency (%)=[disease index after disease index × chemicals treatment district application before 1-(blank district is administered)/(empty Disease index before disease index × chemicals treatment district is administered after white check plot application)] × 100
Table 3 prevents and treats citrus bacterial canker disease field test results
Table of field test results are bright: 1 dosage of example of formulations is that 125mg/kg(dilutes 2000 times) to the pre- of citrus bacterial canker disease Phase preventive effect is 67.06%, and practical preventive effect is 83.96%, reaches synergistic effect.3 dosage of example of formulations is that 100mg/kg(is dilute Release 2000 times), the expection preventive effect to citrus bacterial canker disease is 48.28%, and practical preventive effect is 67.68%, reaches synergistic effect.It is comprehensive On, the preventive effect and 10% fluxapyroxad suspending agent 50g/kg of single dose, 10% fluxapyroxad suspending agent 25mg/kg, 35% of composition The preventive effect of copper 8-hydroxyquinolinate suspending agent 75mg/kg compares, and has the function that synergy, and preventive effect difference reaches extremely significant level.
Security survey to citrus is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to mandarin tree No phytotoxicity phenomenon occurs.
Biological Examples 2: prevention and treatment citrus scab field trial.
Carry out example of formulations 5(25% fluxapyroxad quinoline aqueous emulsion of copper in Jiangxi Nanfeng County within 2018), preparation it is real Apply a 7(30% fluxapyroxad copper 8-hydroxyquinolinate can be dispersed oil-suspending agent) prevention and treatment citrus bacterial canker disease field trial.
Test method is referring to " GBT 17980.102-2004 pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating mandarin orange Tangerine shot hole ".Using randomized blocks, 4 repetitions of every processing, every cell is for 3 plants of examination tree.When blossom fall 2/3 and young fruit Then application is spaced the 2nd medicine of spray in 12 days.Application is spraying using hand backpack compression sprayer, after each application of guarantee for 24 hours Without rain, if rain to add in time.It uniformly sprays to blade, fruit, medical fluid is spent to being intended to drip.
State of an illness radix is investigated before application, 15d, 30d carry out final efficacy survey after the 2nd medicine.Every cell investigates 2 plants, Every plant by the sampling of 5 points of all directions, whole blades of 2 tips of every investigation and 6 fruits.As unit of blade or fruit, disease Mutual affection grade standard is as follows:
Leaf stage division:
It is 0 grade, disease-free;
L grades, every leaf has scab l-5;
3 grades, every leaf has scab 6-10;
5 grades, every leaf has scab 11-15;
7 grades, every leaf has scab 16-20;
9 grades, every leaf has scab 21 or more.
Fruit stage division:
It is 0 grade, disease-free;
L grades, the connected area of scab accounts for the 5% or less of entire fruit area;
3 grades, the connected area of scab accounts for the 6%~10% of entire fruit area;
5 grades, the connected area of scab accounts for the 11%~25% of entire fruit area;
7 grades, the connected area of scab accounts for the 26%~50% of entire fruit area;
9 grades, the connected area of scab accounts for 51% or more of entire fruit area.
Disease index and control efficiency calculation method:
Disease index=Σ (disease leaf (fruit) numbers at different levels × opposite value of series)/(investigating total leaf (fruit) number × 9) × 100
Control efficiency (%)=(disease index after disease index-chemicals treatment district application after blank district application)/blank control Disease index × 100 after area's application
Table 4 prevents and treats citrus scab field test results
Table of field test results are bright: 5 dosage of example of formulations be 125mg/kg(dilute 2000 times) to citrus bacterial canker disease medicine after The expection preventive effect of 15d is 61.09%, and practical preventive effect is 78.20%, reaches synergistic effect;The expection preventive effect of 30d is after medicine 49.41%, and practical preventive effect is 64.87%, reaches synergistic effect;The expection preventive effect of fruit is 49.34%, and practical preventive effect is 72.23%, reach synergistic effect.7 dosage of example of formulations is that 150mg/kg(dilutes 2000 times), after citrus bacterial canker disease medicine The expection preventive effect of 15d is 64.40%, and practical preventive effect is 81.30%, reaches synergistic effect;The expection preventive effect of 30d is after medicine 50.88%, and practical preventive effect is 67.97%, reaches synergistic effect;The expection preventive effect of fruit is 60.24%, and practical preventive effect is 75.59%, reach synergistic effect.To sum up, 10% fluxapyroxad suspending agent 25g/kg of preventive effect Yu single dose, the 10% fluorine azoles of composition Bacterium amide suspending agents 50mg/kg, 35% copper 8-hydroxyquinolinate suspending agent 75mg/kg, 35% copper 8-hydroxyquinolinate suspending agent 125mg/kg preventive effect compare Compared with having the function that synergy, preventive effect difference reaches extremely significant level.
Security survey to citrus is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to mandarin tree No phytotoxicity phenomenon occurs.
Biological Examples 3: prevention and treatment alternaria leaf spot of apple field trial.
Example of formulations 9(28% fluxapyroxad copper 8-hydroxyquinolinate wettable powder has been carried out in Shaanxi Province's Weinan City within 2017 Agent), example of formulations 11(45% fluxapyroxad quinoline copper water dispersion granula) prevention and treatment alternaria leaf spot of apple field examination It tests.
Test method is referring to " GB T17980.124-2004 pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating Alternaria leaf spot of apple pharmacodynamic test ".Test is located at Weinan City Fuping County, and soil is clay, and topography is flat, and soil fertility is uniform, pH Value 7.1, fertility is preferable, experimental field cultivation condition uniformity, and apple variety is Fuji apple, and the age of tree is 17 years, distance between rows and hills 5m ×6m.Test medicine and dosage see the table below, and separately set blank control, 4 repetitions of every processing, 2 plants of every cell trees, the random district's groups of cell Arrangement.Using conventional spray-on process, blade positive and negative are uniformly squirted.Application for the first time was carried out at 10 days after apple is thanked and spent, and 14 days It carries out being administered for second afterwards, be administered 2 times altogether.
Investigation and statistical method: every cell investigates 2 plants of trees, and every plant of point east, south, west, north, middle different direction fix 2 Young sprout, investigates its whole blade, and record total number of sheets, the sick number of sheets at different levels and sick series calculate disease index.Grade scale are as follows:
0 grade, disease-free spot;
1 grade, lesion area accounts for 10% or less entire leaf area;
3 grades, lesion area accounts for the 11%-25% of entire leaf area;
5 grades, lesion area accounts for the 26%-40% of entire leaf area;
7 grades, lesion area accounts for the 41%-65% of entire leaf area;
9 grades, lesion area accounts for 65% or more of entire leaf area.
Disease index and control efficiency calculation method:
Disease index=Σ (the disease numbers of sheets at different levels × opposite value of series)/(investigation total number of sheets × 9) × 100
Control efficiency (%)=[disease index after disease index × chemicals treatment district application before 1-(blank district is administered)/(empty Disease index before disease index × chemicals treatment district is administered after white check plot application)] × 100
Table 5 prevents and treats alternaria leaf spot of apple field test results
Table of field test results are bright: 9 dosage of example of formulations is that 140mg/kg(dilutes 2000 times) to alternaria leaf spot of apple Expection preventive effect be 66.97%, and practical preventive effect be 79.54%, reach synergistic effect.11 dosage of example of formulations is 150mg/ Kg(dilutes 3000 times), the expection preventive effect to alternaria leaf spot of apple is 75.46%, and practical preventive effect is 87.84%, reaches synergy Effect.To sum up, 10% fluxapyroxad suspending agent 20g/kg of preventive effect Yu single dose, the 10% fluxapyroxad suspending agent 50g/ of composition Kg, 35% copper 8-hydroxyquinolinate suspending agent 100mg/kg, 35% copper 8-hydroxyquinolinate suspending agent 120mg/kg preventive effect compare, reach synergistic Effect, preventive effect difference reach extremely significant level.
Security survey to apple is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to apple tree No phytotoxicity phenomenon occurs.
Biological Examples 4: prevention and treatment ring rot of apple field trial.
Carried out example of formulations 2(24% fluxapyroxad copper 8-hydroxyquinolinate suspending agent in Shaanxi Province's Weinan City within 2017), system Agent embodiment 4(30% fluxapyroxad copper 8-hydroxyquinolinate microemulsion) prevention and treatment ring rot of apple field trial.
Test method is referring to " GBT 17980.118-2004 pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating apple Fruit ring spot ".Test is located at Weinan City Fuping County, and soil is clay, and topography is flat, and soil fertility is uniform, and pH value 7.1, fertility is preferable, Experimental field cultivation condition uniformity, apple variety are Fuji apple, and the age of tree is 17 years, and distance between rows and hills is 5m × 6m.Test medicine and Dosage see the table below, and separately set blank control, 4 repetitions of every processing, 5 plants of every cell trees, the random district's groups arrangement of cell.Using conventional spray Mist method, blade positive and negative uniformly squirt.Application for the first time carries out for 10 days after apple is thanked and spent, and 14 days second application is administered altogether 2 times.
Investigation and statistical method: investigating in apple picking time, and uniform and representative 4 plants of falling ill are investigated in every processing Whole fruits and fallen fruits on apple tree, investigation fruit sum are not less than 1000, record the total number of fruits, the number of sick fruits.
Disease index and control efficiency calculation method:
Diseased fruit rate (%)=investigation the number of sick fruits/investigation the total number of fruits × 100
Control efficiency (%)=(blank district diseased fruit rate-chemicals treatment district diseased fruit rate)/blank district diseased fruit rate × 100
Table 6 prevents and treats ring rot of apple field test results
Table of field test results are bright: 2 dosage of example of formulations is that 120mg/kg(dilutes 2000 times) to the pre- of ring rot of apple Phase preventive effect is 50.33%, and practical preventive effect is 64.84%, reaches synergistic effect.4 dosage of example of formulations is that 150mg/kg(is dilute Release 2000 times), the expection preventive effect to ring rot of apple is 62.52%, and practical preventive effect is 76.12%, reaches synergistic effect.It is comprehensive On, the preventive effect and 10% fluxapyroxad suspending agent 20g/kg of single dose, 10% fluxapyroxad suspending agent 50g/kg, 35% of composition The preventive effect of copper 8-hydroxyquinolinate suspending agent 100mg/kg compares, and has the function that synergy, and preventive effect difference reaches extremely significant level.
Security survey to apple is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to apple tree No phytotoxicity phenomenon occurs.
Biological Examples 5: prevention and treatment canker of apple fruit field trial.
Carried out example of formulations 6(35% fluxapyroxad quinoline aqueous emulsion of copper in Shaanxi Province's Weinan City within 2017), system Oil-suspending agent can be dispersed in agent embodiment 8(24% fluxapyroxad copper 8-hydroxyquinolinate) prevention and treatment canker of apple fruit field trial.
Test method is referring to " GBT 17980.117-2004 pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating apple Fruit and Fungus of Pear Canker Disease ".Test is located at Weinan City Fuping County, and soil is clay, and topography is flat, and soil fertility is uniform, pH value 7.1, fertilizer Power is preferable, experimental field cultivation condition uniformity, and apple variety is Fuji apple, and the age of tree is 17 years, and distance between rows and hills is 5m × 6m.Test Medicament and dosage see the table below, and separately set blank control, and 4 repetitions of every processing, 6 plants of every cell are set, and the sick scar number of every plant of tree is no less than 8 It is a, the random district's groups arrangement of cell.Using conventional spray-on process, blade positive and negative are uniformly squirted.It is scraped before the germination of spring fruit tree and controls corruption It is rotten to spray after being ill once.
Investigation and statistical method: disease index investigation, the next spring morbidity peak period of application are carried out before spring sprays After carry out efficacy survey.Sick scar block radix is investigated before medicine, and the recurrence of the old complaint scar of each cell total Test tree is investigated after medicine, Each cell old complaint scar recurrence rate is counted, preventive effect is calculated.
Table 7 prevents and treats canker of apple fruit field test results
Table of field test results are bright: 6 dosage of example of formulations is that 140mg/kg(dilutes 2500 times) to the pre- of canker of apple fruit Phase preventive effect is 51.53%, and practical preventive effect is 70.86%, reaches synergistic effect.8 dosage of example of formulations is that 120mg/kg(is dilute Release 2000 times), the expection preventive effect to canker of apple fruit is 65.47%, and practical preventive effect is 81.43%, reaches synergistic effect.It is comprehensive On, the preventive effect and 10% fluxapyroxad suspending agent 20g/kg of single dose, 10% fluxapyroxad suspending agent 40g/kg, 35% of composition The preventive effect of copper 8-hydroxyquinolinate suspending agent 100mg/kg compares, and has the function that synergy, and preventive effect difference reaches extremely significant level.
Security survey to apple is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to apple tree No phytotoxicity phenomenon occurs.
Biological Examples 6: prevention and treatment brown spot field trial.
Example of formulations 10(35% fluxapyroxad copper 8-hydroxyquinolinate wettable powder has been carried out in Shaanxi Province's Weinan City within 2017 Agent), example of formulations 12(35% fluxapyroxad quinoline copper water dispersion granula) prevention and treatment apple marssonina leaf spot field trial.
Test is located at Weinan City Fuping County, and soil is clay, and topography is flat, and soil fertility is uniform, and pH value 7.1, fertility is preferable, examination Ground cultivation condition uniformity is tested, apple variety is Fuji apple, and the age of tree is 17 years, and distance between rows and hills is 5m × 6m.Test medicine and use Amount see the table below, and separately set blank control, 4 repetitions of every processing, 4 plants of every cell trees, the random district's groups arrangement of cell.Using conventional spraying Method, blade positive and negative uniformly squirt.Application for the first time is carried out in brown spot early stage, and second is carried out after 14 days and is administered, altogether Application 2 times.
Investigation and statistical method: every cell investigates 2 plants of trees, and every plant of point east, south, west, north, middle different direction fix 2 Young sprout, investigates its whole blade, and record total number of sheets, the sick number of sheets at different levels and sick series calculate disease index.Grade scale are as follows:
0 grade, disease-free spot;
1 grade, lesion area accounts for 10% or less entire leaf area;
3 grades, lesion area accounts for the 11%-25% of entire leaf area;
5 grades, lesion area accounts for the 26%-40% of entire leaf area;
7 grades, lesion area accounts for the 41%-65% of entire leaf area;
9 grades, lesion area accounts for 65% or more of entire leaf area.
Disease index and control efficiency calculation method:
Disease index=Σ (the disease numbers of sheets at different levels × opposite value of series)/(investigation total number of sheets × 9) × 100
Control efficiency (%)=[disease index after disease index × chemicals treatment district application before 1-(blank district is administered)/(empty Disease index before disease index × chemicals treatment district is administered after white check plot application)] × 100
Table 8 prevents and treats apple marssonina leaf spot field test results
Table of field test results are bright: 10 dosage of example of formulations is that 140mg/kg(dilutes 2500 times) to the pre- of apple marssonina leaf spot Phase preventive effect is 64.81%, and practical preventive effect is 79.71%, reaches synergistic effect.12 dosage of example of formulations is 140mg/kg (2500 times of dilution) is 69.20% to the expection preventive effect of apple marssonina leaf spot, and practical preventive effect is 83.84%, reaches synergistic effect.It is comprehensive On, the preventive effect of composition and 10% fluxapyroxad suspending agent 20mg/kg of single dose, 10% fluxapyroxad suspending agent 40mg/kg, 35% copper 8-hydroxyquinolinate suspending agent 100mg/kg, 35% copper 8-hydroxyquinolinate suspending agent 120mg/kg preventive effect compare, reach synergistic work With preventive effect difference reaches extremely significant level.
Security survey to apple is observed for several days after the 1st day and medicine after spray every time, and each chemicals treatment is to apple tree No phytotoxicity phenomenon occurs.
The above test explanation, the first active constituent fluxapyroxad and the second active constituent copper 8-hydroxyquinolinate by weight 1:60~ 60:1 compounding can be made into suspending agent, microemulsion, aqueous emulsion, dispersible oil-suspending agent, wettable powder, dosage form of water dispersible granule, There is significant control efficiency to citrus and apple disease, synergistic effect is obvious, and dosage is few, control efficiency is high, and pacifies to crop Full property is good.
In conclusion composition of the invention is using two kinds of active components compound scheme, activity and bactericidal effect are not It is the active simple superposition of each component, compared with existing single formulation, other than with significant bactericidal effect, more has significant Synergistic effect, it is good to crop safety, meet the security requirement of pesticidal preparations.

Claims (5)

1. the bactericidal composition of a kind of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate, which is characterized in that effective component is by the first active constituent Fluxapyroxad and the second active constituent copper 8-hydroxyquinolinate form, the weight ratio of the first active constituent and the second active constituent be 1:60~ 60:1.
2. the bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate according to claim 1, which is characterized in that first activity at Dividing with the weight ratio of the second active constituent is 1:20~10:1.
3. the bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate according to claim 1, which is characterized in that the composition Dosage form is suspending agent, microemulsion, aqueous emulsion, dispersible oil-suspending agent, wettable powder, water dispersible granules.
4. the bactericidal composition of Fluxapyroxad-containsterilization and copper 8-hydroxyquinolinate is on prevention and treatment citrus and apple disease according to claim 1 Purposes.
5. purposes according to claim 4, citrus disease is citrus bacterial canker disease and citrus scab, and apple disease is apple spot Point defoliation, ring rot of apple, canker of apple fruit, apple marssonina leaf spot.
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