CN105284888B - A kind of bactericidal composition containing oxalic acid copper diacetonamine - Google Patents
A kind of bactericidal composition containing oxalic acid copper diacetonamine Download PDFInfo
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Abstract
The invention discloses a kind of bactericidal composition containing oxalic acid copper diacetonamine, including the first active component and the second active component, the weight ratio of the first active component and the second active component is 1:15~10:1, the first active component is oxalic acid copper diacetonamine, and the second active component is sulphur.The present composition can be configured to agriculturally allow water dispersible granules, wettable powder, suspending agent or the dispersible oil-suspending agent used, to alternaria leaf spot of apple, apple marssonina leaf spot, apple mildew, cucumber downy mildew, powdery mildew of cucumber, the late blight of potato have preferable preventive effect.Present invention efficiently solves the problem of alone oxalic acid copper diacetonamine or undesirable above-mentioned protective fungicide preventive effect, the two compounding has significant synergies and good to crop safety, slow down the generation of resistance.
Description
Present patent application is patent CN104351243A divisional application.
Patent name：A kind of bactericidal composition containing oxalic acid copper diacetonamine
Number of patent application：201410620595.0
Patent application day：On November 06th, 2014
Technical field
The invention belongs to technical field of compounded pesticide, is related to a kind of bactericidal composition, and in particular to one kind is with oxalic acid dipropyl
Ketoamine copper is as the first active component, protective fungicide zineb, Mancozeb, Carbatene, ambam, Propineb, Fu Mei
Binary built bactericidal composition of the sterilization components such as double, ziram, Bravo, sulphur, dimethachlon as the second active component.This
The preparation formulation and its that have further related to the bactericidal composition are invented in application agriculturally.
Background technology
Copper agent is one of disinfectant use in agriculture type the most ancient, has has a broad antifungal spectrum, to be not likely to produce the resistance to the action of a drug etc. excellent
Point.Based on the usage history of the inorganic copper agent of Kocide SD, copper sulphate etc. more than 200 years, but due to its be difficult to by
Biodegradation, it is long-term a large amount of using accumulation of the copper in soil has been had resulted in, can be to the normal growth and soil function of plant
Have undesirable effect.At present, the utilization of organic copper agent, it has also become the hot topic of disinfectant use in agriculture production, organic copper agent
To crop safety, nuisanceless.
Inst. of Pesticides, Xibei Univ. of Agricultural ＆. Forestry Science ＆. Technolo leads to using two acetone isolated in Qinling Mountains streptomycete zymotic fluid as raw material
Cross to its structural modification, synthesize a kind of new compound --- oxalic acid copper diacetonamine.This is a kind of new organocopper compound,
Toxicity shows that it shows good bacteriostatic activity to various agricultural pathogen, table of field test results it is bright its to cucumber cream
The crop diseases such as mildew, the late blight of potato, alternaria leaf spot of apple have good prevention effect.
Protective fungicide refers to before infection process crop, the first dispenser in crop surface, prevents germ from invading, and rises
To protective effect.After protective fungicide use, one layer of ventilative, permeable, printing opacity compactness protection can be formed in crop surface
Medicine film, this layer of diaphragm can suppress the sprouting and invasion of germ spore, so as to reach the effect of sterilizing disease-preventing.This series bactericidal agent pair
The crop disease preventive effect for having infected and having fallen ill is very poor, and often and systemic fungicide mixture use can be only achieved preferable preventive effect.
Common protective fungicide has zineb, Mancozeb, Carbatene, ambam, Propineb, thiram, ziram, hundred bacterium
Clearly, sulphur, dimethachlon etc..
Zineb, English common name zineb, chemical name is zinc ethylenebisdithiocarbamate, is broad spectrum activity, protection
Property bactericide.The mechanism of action of zineb is to destroy coacetylase, so as to influence the oxidation of aliphatic acid.Active ingredient chemical property compared with
Vivaciously, different sulphur gas cyanogen compound is easily oxidized in water, has stronger suppression to make the enzyme for containing-SH bases in pathogen body
With, and germ spore can be directly killed, suppress the germination of spore, prevent in germ invaded plantses body, but to invaded plantses
The mycelial lethal effect of internal cause of disease is smaller.It is mainly used in preventing and treating the crops such as wheat class, vegetables, grape, fruit tree and tobacco
A variety of fungal diseases, can prevent and treat Chinese cabbage, cucumber downy mildew, anthracnose of tomato, the late blight of potato, fruit white rot of grape, black spot,
Apple, pear scab.
Mancozeb, English common name mancozeb, chemical name are the network of the double dithiocarbamates formyl manganese of ethylene and zinc
Salt is closed, is a kind of excellent protective fungicide, belongs to low-toxin farm chemicals.Its bactericidal range is wide, is not likely to produce the resistance to the action of a drug, prevention effect
It is substantially better than other same series bactericidal agents.At present, domestic most composite bactericides are formulated with Mancozeb processing, manganese,
Zinc microelement has obvious rush to strengthen to crop, production-increasing function, to preventing and treating pear scab, alternaria leaf spot of apple, vegetable category epidemic disease
Disease, downy mildew, field crop rust and other effects are notable, steady quality, reliable.
Carbatene, English common name metiram, chemical name are double (the two thiocarbamate esters) zinc (2 of three [ammonia] ethene
+))] [tetrahydrochysene-Isosorbide-5-Nitrae, the thiophene diazocines -3,8- of 7- bis- connect dithione], it is a kind of condensate, belongs to benzimidazole protectiveness
Bactericide.Carbatene can prevent the sprouting of germ spore, suppress the elongation of germ germ tube, germ can not be infected plant tissue,
There is good preventive effect to various diseases caused by Oomycete fungal, be mainly used in preventing and treating vegetable downy mildew, anthracnose, brown spot
Deng.
Ambam, English common name amobam, chemical name are ethylene bisdithiocarbamic ammonium, organic sulphur preparation,
Sterling is clear crystal, water-soluble.Controlling disease mainly shields, and because decoction can penetrate into plant epidermis, has concurrently and controls again
Treatment acts on.The mechanism of action is and the trace element (in such as enzyme or coenzyme contained iron) needed for normal metabolic processes in somatic cells
Chelation compound is formed, makes metabolism not normal.Ambam belongs to less toxic bactericide, and effect is strong, and concentration is low, is made generally in
45% or 50% aqueous solution, wide sterilization spectrum is effective to various crop fungal disease, is available for seed treatment, foliar spray and soil
Earth sterilizes, for preventing and treating bacterial blight of rice, banded sclerotial blight, rice blast, cucumber downy mildew, powdery mildew, sweet potato black rot, cotton charcoal
The various crop diseases such as subcutaneous ulcer disease, corn northern leaf blight and southern leaf blight, while plant growth can also be promoted.
Propineb, English common name propineb, chemical name are acrylic bisdithiocarbamic zinc, are Bayer public affairs
The protective fungicide for the broad spectrum activity developed is taken charge of, mechanism of action is the oxidation for suppressing pyruvic acid in pathogen body.Propineb
The morning of downy mildew and tomato, potato to crops such as vegetables, grape, tobacco and hops, late blight have excellent guarantor
The effect of shield property, and also have certain inhibitory action to the disease of powdery mildew, rust and Botrytis.
Thiram, English common name thiram, chemical name are tetramethyl thiuram disulfide, broad spectrum activity organic sulfur class
Bactericide, there is good protective effect, be mainly used in seed and soil treatment, available for preventing and treating Cereal smut and a variety of
The seedling blight of crop, it can also be used to prevent and treat the disease of some fruit trees and vegetables.
Ziram, English common name ziram, chemical name are double-(dimethyl-thiocarbamic acid) zinc, are a kind of high
Effect, broad spectrum activity have the bactericide of protective effect, and main mechanism is made with the enzyme of the base Han-SH in pathogen body
With normal metabolism being destroyed, for fruit tree anthracnose, blossom rot, scab, brown rot, powdery mildew etc..Ziram belongs to
Low-toxin farm chemicals, to people and animals' low toxicity, to fish high poison, there is stimulation to skin, eyes and the upper respiratory tract, to plant safety, nothing
Pollution.
Bravo, English common name chlorothalonil, chemical name are that (2,4,5,6- tetra- is chloro- for daconil M
1,3- benzene dicarbonitrile), it is a kind of less toxic wide spectrum, protective fungicide.The mechanism of action of Bravo for can with fungal cell
Glyceraldehyde 3-phosphate dehydrogenase is had an effect, and is combined with the protein containing cysteine in the enzyme, so as to destroy the enzyme
Activity, the metabolism of fungal cell is set to be damaged and lose vitality.Bravo does not have uptake and translocation effect, is sprayed onto plant
After upper, there can be good tackness on body surface, be not easy to be fallen by rain drop erosion, therefore the drug effect phase is longer.
Sulphur, English common name sulfur, non-internal-absorting protective fungicide, no therapeutic effect.The mechanism of action of sulphur
For respiration inhibitor, electron transfer process between germ helium reduction system cytochrome b and c is acted on, captures electronics, disturbed
Normally " oxidationreduction ".Sulphur can be used for wheat, beet, vegetables such as cucumber, eggplant etc., fruit tree for example apple, Lee, peach, grape,
The preventing and treating of the crop diseases such as citrus, matrimony vine.The controlling object of sulphur is wheat powdery mildew, rust, smut, head blight, melon
Powdery mildew, apple, pears, peach scab, uncinula necator etc..Sulphur is in addition to bactericidal activity, also with acaricidal action, such as
For preventing and treating phyllocoptruta oleivora etc..
Dimethachlon, English common name dimetachlone, chemical name are N- (3,5- dichlorophenyl) succimide, tool
Have eradicant fungicide, a therapeutic action, longevity of residure length, China from 2002 initially as sclerotinia sclerotiorum pathogen to carbendazim
The surrogate-data technique for producing resistance area uses, due to being found that sclerotinia sclerotiorum pathogen to dimethachlon in production in recent years
The phenomenon that sensitiveness reduces, therefore individually use it to preventing and treating sclerotinia sclerotiorum and still suffer from larger risk.Therefore, the bactericide is entered
The rational compounding of row, it is significant to reducing resistance risk.
Inventor is found by experiment that, by oxalic acid copper diacetonamine and protective fungicide zineb, Mancozeb, Dai Sen
A kind of compounding in connection, ambam, Propineb, thiram, ziram, Bravo, sulphur, dimethachlon, has significant synergy
Effect, prevention effect can be significantly improved, reduce dosage, expanded preventing and treating spectrum, reduce cost accounting, delayed drug-fast production
It is raw, to crop safety.
The content of the invention
It is an object of the invention to provide one kind compounding component it is reasonable, synergistic effect is notable, and bactericidal effect is good, drug cost
It is low, it is not likely to produce the resistance to the action of a drug and to the agricultural bactericidal composition of crop safety.
Second object of the present invention is to provide the system of the binary built bactericidal composition containing oxalic acid copper diacetonamine
Agent formulation.
Third object of the present invention is to provide application of the above-mentioned bactericidal composition on preventing and treating corps diseases.
To achieve the above object, this invention takes following technical scheme：
A kind of bactericidal composition containing oxalic acid copper diacetonamine, including the first active component and the second active component, the
The weight of one active component and the second active component ratio is 1:15~10:1, first active component is oxalic acid diacetonamine
Copper, second active component are selected from protective fungicide zineb, Mancozeb, Carbatene, ambam, Propineb, Fu Mei
One kind in double, ziram, Bravo, sulphur, dimethachlon.
Further, in bactericidal composition of the present invention, the content of the first active component and the second active component
Sum is the 5%~90% of the bactericidal composition gross weight.
Further, the formulation of the bactericidal composition containing oxalic acid copper diacetonamine be water dispersible granules, wettable powder,
Suspending agent or dispersible oil-suspending agent.
Further, purposes of the bactericidal composition containing oxalic acid copper diacetonamine on preventing and treating corps diseases.
As the preferred of technical scheme, the corps diseases are alternaria leaf spot of apple, apple marssonina leaf spot, apple white powder
Disease, cucumber downy mildew, powdery mildew of cucumber, the late blight of potato.
Compared with single use oxalic acid copper diacetonamine respectively or above-mentioned protective fungicide, beneficial to effect caused by the present invention
Fruit is mainly reflected in following aspect：
(1) the second active component of bactericidal composition of the present invention is from zineb, Mancozeb, Carbatene, Dai Sen
One kind in ammonium, Propineb, thiram, ziram, Bravo, sulphur, dimethachlon.These protective fungicides crop at home
Used more generally in the preventing and treating of disease, and usage amount is larger.Largely apply above-mentioned protective fungicide, a variety of diseases for a long time
Opportunistic pathogen is to which creating the stronger resistance to the action of a drug so that and the prevention effect of these protective fungicides of single administration is poor, but this
The important kind that several bactericide belong in protective fungicide, also it is difficult to substitute in a short time, therefore should examines really
Consider the resistance problems of above-mentioned bactericide.Oxalic acid copper diacetonamine is as a kind of new organic copper fungicide kind, and it is to crop
The preventing and treating of disease is based on protective effect.The present invention is by the different oxalic acid copper diacetonamine of the mechanism of action and above-mentioned protective fungicide
The effect of one kind in agent carries out binary built, and this also is to continue with playing above-mentioned bactericide and the effective side for slowing down resistance
Method.The activity and bactericidal effect of the bactericidal composition are not the simple superposition of each component activity, but have significant synergistic effect.
In addition, the advantages of bactericidal composition is also manifested by, component is reasonable, and bactericidal effect is good, and drug cost is low, to crop safety
It is good, the generation of delaying drug resistance.
(2) bactericidal composition of the present invention expands preventing and treating spectrum, significantly improves the multiple diseases of multiple kinds of crops
Prevent effect, especially to alternaria leaf spot of apple, apple marssonina leaf spot, apple mildew, cucumber downy mildew, powdery mildew of cucumber,
The preventive effect of the late blight of potato is preferable.
(3) bactericidal composition of the present invention can be prepared as water dispersible granules, wettable powder, suspending agent or can divide
The preparation of the different dosage forms such as oil-suspending agent is dissipated, each preparation is good to crop safety, meets the security requirement of pesticidal preparations.
Embodiment
In order that the purpose of the present invention, technical scheme and beneficial effect are more clearly understood, with reference to embodiments, to this
Invention is further elaborated.
(1) preparation prepares part
Bactericidal composition containing oxalic acid copper diacetonamine can be configured to water dispersible granules, wettable powder, suspending agent
Or the formulation such as dispersible oil-suspending agent.When preparing above-mentioned different dosage forms, to those skilled in the art, except needs
Outside containing fungicide active ingredient for the election, it is also necessary to select a variety of auxiliary agents, can select to use different agricultures as needed
Medicine preparation auxiliary element (auxiliary agent).The auxiliary element can be decentralized medium, dispersant, emulsifying agent, wetting agent, thickener,
One or more in defoamer, antifreezing agent, disintegrant, binding agent, filler etc..
For water dispersible granules, those skilled in the art are very familiar with completing the present invention using corresponding auxiliary agent.It is scattered
Agent from polycarboxylate (TERSPERSE 2700, T36, GY-D06 etc.), lignosulfonates, it is a kind of in alkylnaphthalene sulfonate or
It is a variety of；Wetting agent is from one or more in alkyl sulfate, alkylsulfonate, naphthalene sulfonate；Disintegrant is from ammonium sulfate, sulphur
It is one or more in sour sodium, polyvinylpyrrolidone, starch and its derivative, bentonite；Binding agent from starch, glucose,
One or more in polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, sucrose；Filler is from diatomite, kaolin, white
Carbon black, fine particle calcium carbonate, talcum powder, attapulgite, clay are one or more.
When preparing corresponding wettable powder, workable auxiliary agent has：Dispersant selects polycarboxylic acid salt
(TERSPERSE2700, T36, GY-D06 etc.), lignin sulfonate (Ufoxane 3A, Borresperse NA,
Borresperse CA-SA etc.), naphthalene and alkyl naphthalene formaldehyde condensate sulfonates class (NNO, MF, Morwet D-425, Tamol
NN, TERSPERSE2020 etc.), Nekal BX (nekal), EO-PO block polyether class (polyoxyethylene polyoxypropylenes
Block copolymer), alkylphenol-polyethenoxy base ether phosphate, alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfate (SOPA)
Middle one or more；Wetting agent is from Sulfates (K-12), Sulfonates (ABS-Na, BX, Terwet1004 etc.), compound profit
It is one or more in humectant (Morwet EFW)；Filler is from diatomite, kaolin, fine particle calcium carbonate, talcum powder, white carbon, concave convex rod
One or more in soil, clay, ammonium sulfate, urea, sucrose, glucose, cornstarch, sodium sulphate, sodium polyphosphate.
When preparing corresponding suspending agent, workable auxiliary agent has：Dispersant such as polycarboxylate, lignosulfonates, alkane
It is a kind of in base naphthalene sulfonate (dispersing agent NNO), TERSPERSE 2020 (Huntsman Corporation of the U.S. produces, alkyl naphthalene sulfonic acid salt)
It is or a variety of；Emulsifying agent such as Nongru-700 # (common names：Alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201, this disk -60# it is (logical
With name：Span60), Tween-60 # (common names：Polyoxyethylene sorbitan stearate), agriculture breast
1601# (common names：Triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer), (U.S.'s Hensels of TERSPERSE 4894
Step company produce) in one or more；Wetting agent such as alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfate, alkyl phenol gather
Oxyethylene group ether phosphate, phenethyl phenol polyoxyethylene groups ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate,
It is one or more in TERSPERSE 2500 (Huntsman Corporation of U.S. product)；Thickener such as xanthans, polyvinyl alcohol, swelling
It is one or more in soil, aluminium-magnesium silicate；It is one or more in preservative such as formaldehyde, benzoic acid, sodium benzoate；Stabilizer such as epoxy
It is one or more in soybean oil, epoxychloropropane, triphenyl phosphate；Defoamer such as organic silicon defoamer；Antifreezing agent such as second two
It is one or more in alcohol, propane diols, glycerine, urea, inorganic salts such as sodium chloride；Water is deionized water.
When preparing corresponding dispersible oil-suspending agent, workable auxiliary agent has：Emulsifying agent selects BY (castor oil polyoxy second
Alkene ether) serial emulsifying agent (BY-110, BY-125, BY-140), calcium dodecyl benzene sulfonate, AEO, agriculture breast
700# (common names：Alkyl phenol formaldehyde resin polyoxyethylene ether), agriculture breast 2201, this disk -60# (common names：Sorbitol anhydride list is stearic
Acid esters), Tween-60 # (common names：Sorbitan monostearate APEO), agriculture breast 1601# (common names：Phenethyl
Phenol polyoxyethylene poly-oxygen propylene aether), the one or more in TERSPERSE 4894 (Huntsman Corporation of U.S. product)；It is scattered
Agent is from polycarboxylate, lignosulfonates, EO-PO block copolymers (polyoxyethylene polyoxypropylene block copolymer), phosphoric acid
Ester and its esters, Sulfonates, alkylnaphthalene sulfonate (dispersing agent NNO), (Huntsman Corporation of the U.S. goes out TERSPERSE 2020
Product, alkyl naphthalene sulfonic acid salt) in one or more；Wetting agent selects alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfuric acid
Salt, APES phosphate, phenethyl phenol polyoxyethylene groups ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene
One or more in sulfonate, TERSPERSE 2500 (Huntsman Corporation of U.S. product)；Thickener from gas-phase silica,
One or more in polyvinyl alcohol, organobentonite, attapulgite, aluminium-magnesium silicate；Stabilizer from organic acid, organic base,
One or more in esters, alcohols, antioxidant, epoxychloropropane, tall oil；Decentralized medium is from soybean oil, rapeseed oil, cotton
Seed oil, corn oil, castor oil, palm oil, epoxidized soybean oil, methyl oleate and its esterification oils, diesel oil, machine oil, mineral oil,
It is and a kind of or more in esters solvent such as repefral, dibutyl phthalate, ethyl acetate, methyl benzoate
Kind.
The bactericidal composition of the present invention includes the first active component and the second active component, and the first active component is oxalic acid two
Acetone amine copper, the second active component are one kind in protective fungicide.The weight of first active component and the second active component
Than for 1:15~10:1, and the content sum of the first active component and the second active component is the bactericidal composition gross weight
5%~90%.As a preferred embodiment, the second active component protective fungicide be selected from zineb, Mancozeb,
One kind in Carbatene, ambam, Propineb, thiram, ziram, Bravo, sulphur, dimethachlon.
It should be noted that the active ingredient (or active component) in each example of formulations of subordinate is weight after folding hundred.
Example of formulations 1
Weigh 30 grams of oxalic acid copper diacetonamines, 450 grams of zineb, 30 grams of GY-D06 (polycarboxylate), 25 grams of alkylnaphthalene sulphurs
Hydrochlorate, 15 grams of Nekal BXs (nekal), 20 grams of K-12 (lauryl sodium sulfate), 25 grams of PVA (molecular weight
2000), 25 grams of sodium sulphate, attapulgite supply 1000 grams.The method i.e. mixing of the frequent regulation water intaking dispersible granule of above-mentioned raw materials,
Ultra micro air-flow crushing, mixing, granulation step, produce active constituent content and dissipated for 48% oxalic acid copper diacetonamine zineb moisture
Granula.
Example of formulations 2
Weigh 50 grams of oxalic acid copper diacetonamines, 500 grams of Mancozebs, 30 grams of TERSPERSE 2700 (polycarboxylate, U.S.
Huntsman Corporation produce), 25 grams of dispersing agent NNOs (alkylnaphthalene sulfonate formaldehyde condensation products), 20 grams of Nekal BX (dibutyl naphthalene sulphurs
Sour sodium), 20 grams of K-12 (lauryl sodium sulfate), kaolin add to 1000 grams.The frequent regulation water intaking dispersible granule of above-mentioned raw materials
Method be mixing, ultra micro air-flow crushing, mixing, granulation step, it is 55% oxalic acid diacetonamine to produce active constituent content
Copper mancozeb water dispersible granule.
Example of formulations 3
Weigh 100 grams of oxalic acid copper diacetonamines, 500 grams of Carbatenes, 40 grams of T36 (polycarboxylate), 20 grams of dispersing agent NNOs
(alkylnaphthalene sulfonate formaldehyde condensation products), 30 grams of Nekal BXs (nekal), 20 grams of K-12 (dodecyl sulphates
Sodium), 25 grams of sodium carboxymethylcelluloses, 60 grams of sodium sulphate, talcum powder add to 1000 grams.The frequent regulation water intaking dispersible granule of above-mentioned raw materials
The method of agent is mixing, ultra micro air-flow crushing, mixing, granulation step, and it is 60% oxalic acid diacetonamine to produce active constituent content
Copper Carbatene water dispersible granules.
Example of formulations 4
Weigh 100 grams of oxalic acid copper diacetonamines, 300 grams of ambam, 35 grams of GY-D06,35 grams of nekals, 30
Gram lauryl sodium sulfate, talcum powder are filled up to 1000 grams.Above-mentioned raw materials are blended, ultra micro air-flow crushing, hybrid technique step,
It is 40% oxalic acid copper diacetonamine ambam wettable powder to be prepared into active constituent content.
Example of formulations 5
Weigh 400 grams of oxalic acid copper diacetonamines, 500 grams of Propinebs, 10 grams of alkylphenol-polyethenoxy base ether phosphates, 10 grams
Alkylnaphthalene sulfonate formaldehyde condensation products (TERSPERSE2020), 10 grams of lauryl sodium sulfate, cornstarch are filled up to 1000
Gram.Above-mentioned raw materials are blended, ultra micro air-flow crushing, hybrid technique step, and it is 90% oxalic acid dipropyl to be prepared into active constituent content
Ketoamine copper Wettable propineb powder.
Agent embodiment 6
Weigh 250 grams of oxalic acid copper diacetonamines, 250 grams of thiram, 20 grams of alkylphenol-polyethenoxy base ether phosphates, 15 grams
Tamol NN (alkylnaphthalene sulfonate formaldehyde condensation products), 15 grams of alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfate
(SOPA), 20 grams of ABS-Na, sodium polyphosphate add to 1000 grams.Above-mentioned raw materials are blended, and active ingredient is made after air-flow crushing
Content is 50% oxalic acid copper diacetonamine thiram wettable powder.
Example of formulations 7
Weigh 250 grams of oxalic acid copper diacetonamines, 200 grams of ziram, 40 grams of this disk -60#, 25 grams of alkylphenol-polyethenoxy bases
Ether phosphate, 25 grams of dispersing agent NNOs, 15 grams of bentonites, 5 grams of polyvinyl alcohol, 45 grams of propane diols, 7 grams of benzoic acid, 10 grams of organosilicons
Defoamer (trade name：S-29 Nanjing "four news" (new ideas applied chemistry product company produce), deionized water add to 1000 grams.Above-mentioned raw materials are through mixed
Close, high speed shear disperses 30min, and it is that 45% oxalic acid copper diacetonamine good fortune is beautiful that active constituent content is made after being sanded with sand mill
Zincium suspension agent.
Example of formulations 8
Weigh 300 grams of oxalic acid copper diacetonamines, 100 grams of Bravos, 30 grams of Tween-60 #, 20 grams of alkyl sulfates, 25 grams
Lignosulfonates, 22 grams of aluminium-magnesium silicates, 5 grams of polyvinyl alcohol, 45 grams of glycerine, 8 grams of sodium benzoates, 7 grams of organic silicon defoamer (business
The name of an article：S-29 Nanjing "four news" (new ideas applied chemistry product company produce), deionized water add to 1000 grams.Above-mentioned raw materials are blended, cut at a high speed
Cutting dissipates 30min, and it is 40% oxalic acid copper diacetonamine Bravo suspending agent that active constituent content is made after being sanded with sand mill.
Example of formulations 9
Weigh 40 grams of oxalic acid copper diacetonamines, 10 grams of sulphur, 20 grams of alkylphenol-polyethenoxy base ether formaldehyde condensation products sulfuric acid
Salt, 40 grams of polyoxyethylene polyoxypropylene block copolymers, 50 grams of AEOs, 25 grams of Nongru-700 #, 25 gram 12
Alkyl benzene calcium sulfonate, 8 grams of attapulgites, 12 grams of aluminium-magnesium silicates, 15 grams of BHT (BHT, antioxidant), cottonseed
Oil supplies 1000 grams.Above-mentioned raw materials are blended, and it is 5% to be sanded with sand mill and active constituent content is made less than 5um to particle diameter
The dispersible oil-suspending agent of oxalic acid copper diacetonamine sulphur.
Example of formulations 10
Weigh 500 grams of oxalic acid copper diacetonamines, 100 grams of dimethachlons, 40 grams of calcium dodecyl benzene sulfonates, 35 grams
TERSPERSE2020 (Huntsman Corporation of the U.S. produces, alkyl naphthalene sulfonic acid salt), 50 grams of (U.S.'s Hensels of TERSPERSE 4894
The company of stepping produces), 40 grams of Nongru-700 #, 25 grams of organobentonites, 25 grams of tall oils, epoxidized soybean oil supplies 1000 grams.It is above-mentioned
Raw material is blended, and it is 60% oxalic acid copper diacetonamine to be sanded with sand mill and active constituent content is made less than 5um to particle diameter
The dispersible oil-suspending agent of dimethachlon.
Example of formulations 11
Weigh 350 grams of oxalic acid copper diacetonamines, 50 grams of zineb, 25 grams of this disk -60#, 55 grams of BY-140,35 grams of castor oil
APEO, 40 grams of agriculture breast 1601#, 25 grams of TERSPERSE 4894 (Huntsman Corporation of U.S. product), 10 grams of attapulgites,
15 grams of polyvinyl alcohol, 15 grams of BHT (BHT, antioxidant), repefral supplies 1000 grams.On
It is blended to state raw material, it is 40% oxalic acid diacetonamine to be sanded with sand mill and active constituent content is made less than 5um to particle diameter
The dispersible oil-suspending agent of copper zineb.
Example of formulations 12
500 grams of oxalic acid copper diacetonamines, 50 grams of Mancozebs are weighed, (U.S.'s Hensel steps public affairs to 35 grams of TERSPERSE 2500
Department produces), 40 grams of BY-110,50 grams of sorbitan monostearates, 35 grams of phenethyl phenol polyoxyethylene poly-oxygen propylene aethers, 30
Gram AEO, 15 grams of polyvinyl alcohol, 10 grams of attapulgites, 25 grams of epoxychloropropane, methyl benzoate are supplied
1000 grams.Above-mentioned raw materials are blended, and it is 55% oxalic acid two to be sanded with sand mill and active constituent content is made less than 5um to particle diameter
The dispersible oil-suspending agent of acetone amine copper Mancozeb.
(2) Biometric portion
1st, indoor virulence experimental section
Toxicity Determination experiment 1：Powdery mildew of cucumber Toxicity Determination
In order to prevent and treat the vegetables in agricultural production, fruit tree, wheat, strawberry, the powdery mildew on flowers, inventor is with oxalic acid two
The synergy that acetone amine copper has carried out mutual compounding with protective fungicide zineb, thiram, sulphur is studied, and specific method is：
Subjects are cucumber powdery mildew's pathogen (Sphaerotheca fuliginea).The experiment that active compound is configured to need
Medicament, test method reference《People's Republic of China's farm-chemical indoor determinations of agricultural industry criteria NY/T1156.11-2008
The part of test rule bactericide the 11st：Prevent and treat cucurbits powdery mildew experiment pot-culture method》.
First by single dose and each Mixed Pharmacy set 5 various concentrations gradients (preventive effect in the range of 5%~90% by etc.
Set than series).With the pure water added with a small amount of surfactant (Tween 80), wash to take and cover with Powdery Mildew cucumber leaves
Fresh spores, filtered with double gauze, spore concentration is made as 1 × 105The suspension of individual spore/milliliter, it is standby.Often handle 3
Basin, 4 repetitions, and set the processing for not containing effect composition containing only solvent and surfactant and make blank control.Use spore suspension
Liquid 24h before chemicals treatment is inoculated with, and decoction is uniformly sprayed in blade face to whole wettings, standby after decoction natural air drying.Connect
Kind and chemicals treatment after potted plant cucumber natural air drying, then move to thermostatic chamber, 7 cultivated under conditions of 20 DEG C~24 DEG C of temperature
My god~10 days.When blank control disease leaf rate reaches more than 80%, incidence is managed in classification investigation everywhere, is often handled and is at least investigated
30 leaves, grade scale are：
0 grade：It is disease-free；
1 grade：Lesion area accounts for less than the 5% of full wafer leaf area；
3 grades：Lesion area accounts for the 6%~15% of full wafer leaf area；
5 grades：Lesion area accounts for the 16%~25% of full wafer leaf area；
7 grades：Lesion area accounts for the 26%~50% of full wafer leaf area；
9 grades：Lesion area accounts for the 50%~75% of full wafer leaf area；
11 grades：Lesion area accounts for more than the 75% of full wafer leaf area.
Computational methods：
Disease index=∑ (the sick numbers of sheets at different levels × relative value of series)/(investigation total leaf number × 11) × 100
Prevention effect (%)=[(control disease index-processing disease index)/control disease index] × 100
By the linear regression analysis between the probit value of preventive effect and the logarithm value of series concentration, the EC of each medicament is obtained50
Value, the co-toxicity coefficient (CTC) of mixture is calculated with the abundant methods of Sun Yun, activity of the reagent agent to germ is evaluated with this.
The co-toxicity coefficient (CTC) >=120 of complex preparation shows as synergistic effect；CTC≤80 show as antagonism；80 ＜
CTC ＜ 120 show as summation action.
The result of the test that Toxicity Determination tests 1 (powdery mildew of cucumber Toxicity Determination) is shown in Table 1-1 to table 1-3.
Table 1-1 oxalic acid copper diacetonamines combine the Toxicity Determination to powdery mildew of cucumber with zineb
Table 1-2 oxalic acid copper diacetonamines combine the Toxicity Determination to powdery mildew of cucumber with thiram
Table 1-3 oxalic acid copper diacetonamines combine the Toxicity Determination to powdery mildew of cucumber with sulphur
Toxicity Determination result (table 1-1 to table 1-3) shows：Oxalic acid copper diacetonamine respectively with zineb, thiram,
One kind in sulphur, using weight ratio as 1:15~10:1 it is mixed have preferable virulence to cucumber powdery mildew's pathogen, have significant increasing
Effect acts on.
Toxicity Determination experiment 2：Alternaria leaf spot of apple Toxicity Determination
In order to prevent and treat the alternaria leaf spot of apple in agricultural production, inventor with oxalic acid copper diacetonamine respectively with Dai Sen
Connection, Bravo, dimethachlon have carried out the synergy research of mutual compounding, and specific method is：
Subjects are alternaria leaf spot of apple (Alternaria alternaria f.sp mali).Active compound is prepared
Into the test medicine of needs, single dose and each Mixed Pharmacy are set into 5 various concentrations gradients (on the basis of pilot study result
On, bacteriostasis rate is set in the range of 5%~90% by geometric progression).If clear water compares, it is repeated 3 times.Experiment is given birth to using mycelia
Long performance rate method, by cultured pathogen, aseptically with a diameter of 5mm card punch, bacteria cake is cut from colony edge, used
Bacteria cake is connected on the culture medium flat plate of different agents concentration by transfer needle, is put 28 DEG C, is cultivated in saturated humidity incubator；Treat control group
When bacterium colony covers with, colony diameter is measured, the percentage that each chemicals treatment suppresses mycelial growth is calculated, passes through the probit value of inhibiting rate
Linear regression analysis between the logarithm value of series concentration, obtain the EC of each medicament50Value, being total to for mixture is calculated with the abundant methods of Sun Yun
Malicious coefficient (CTC), activity of the reagent agent to germ is evaluated with this.
The co-toxicity coefficient (CTC) >=120 of complex preparation shows as synergistic effect；CTC≤80 show as antagonism；80 ＜
CTC ＜ 120 show as summation action.
Alternaria leaf spot of apple Toxicity Determination the results are shown in Table 2-1 to table 2-3.
Table 2-1 oxalic acid copper diacetonamines combine the Toxicity Determination to alternaria leaf spot of apple with Carbatene
Table 2-2 oxalic acid copper diacetonamines combine the Toxicity Determination to alternaria leaf spot of apple with Bravo
Table 2-3 oxalic acid copper diacetonamines combine the Toxicity Determination to alternaria leaf spot of apple with dimethachlon
Toxicity Determination result (table 2-1 to table 2-3) shows：Oxalic acid copper diacetonamine respectively with Carbatene, Bravo,
One kind in dimethachlon, using weight ratio as 1:15~10:1 it is mixed have preferable virulence to alternaria leaf spot of apple, have significantly
Synergistic effect.
Toxicity Determination experiment 3：Cucumber downy mildew Toxicity Determination
In order to prevent and treat the vegetables in agricultural production, fruit tree downy mildew, inventor with oxalic acid copper diacetonamine and Mancozeb,
Ambam, Propineb have carried out the synergy research of mutual compounding, and specific method is：
Experiment uses bacterium of downy mildew of cucumber (Pseudoperonospora cubensis) as test object.Active compound is prepared
Into the test medicine of needs, test method reference《People's Republic of China's agricultural industry criteria NY/T1156.3-2006》.
Set 5 various concentrations gradients (antibacterial on the basis of pilot study result single dose and each Mixed Pharmacy first
Rate is set in the range of 5%~90% by geometric progression).Experiment target bacterium is to pick up from the field leaf position of 4 leaves~6 from up to down
Bacterium of downy mildew of cucumber blade, the Pseudoperonospora cubensis sporangium at the lower blade back side is washed with 4 DEG C of distillations, being made into suspension, (concentration controls
At every milliliter 1 × 105Individual~1 × 107Individual sporangium), deposit at 4 DEG C standby；Decoction is uniformly sprayed in the healthy leaves back side,
After decoction natural air drying, by each processing blade and blade backwards to upper, it is emitted on after being marked by processing in moisture preservation box.Experiment sets not drug containing
Blank control is made in the processing of agent.Vacuum side of blade is inoculated in the ready μ L of Fresh spores capsule suspension drop 10.Connect per blade
The drop of kind 4, often processing are no less than 5 leaves.Ware lid is covered after inoculation, growth cabinet is placed in or has the humidistat of illumination, daily
Continuous illumination/dark 12h alternatings, temperature are 17 DEG C~22 DEG C, are cultivated under conditions of relative humidity more than 90%.Depending on processing and sky
White control incidence measures and records lesion diameter, and unit is millimeter (mm), calculates prevention effect.Pass through the machine of prevention effect
Linear regression analysis between rate value and the logarithm value of series concentration, obtain the EC of each medicament50Value, mixture is calculated with the abundant methods of Sun Yun
Co-toxicity coefficient (CTC), activity of the reagent agent to germ is evaluated with this.
The co-toxicity coefficient (CTC) >=120 of complex preparation shows as synergistic effect；CTC≤80 show as antagonism；80 ＜
CTC ＜ 120 show as summation action.
Cucumber downy mildew Toxicity Determination the results are shown in Table 3-1 to table 3-3.
Table 3-1 oxalic acid copper diacetonamines combine the Toxicity Determination to cucumber downy mildew with Mancozeb
Table 3-2 oxalic acid copper diacetonamines combine the Toxicity Determination to cucumber downy mildew with ambam
Table 3-3 oxalic acid copper diacetonamines combine the Toxicity Determination to cucumber downy mildew with Propineb
Toxicity Determination result (table 3-1 to table 3-3) shows：Oxalic acid copper diacetonamine respectively with Mancozeb, Dai Sen
One kind in ammonium, Propineb, using weight ratio as 1:15~10:1 it is mixed have preferable virulence to cucumber downy mildew, have significant
Synergistic effect.
2. field test part
Biological Examples 1：Prevent and treat alternaria leaf spot of apple field test
(the 60% oxalic acid copper diacetonamine Carbatene moisture of example of formulations 3 has been carried out in Shaanxi Province's Weinan City within 2013
Shot agent), example of formulations 8 (40% oxalic acid copper diacetonamine Bravo suspending agent), (60% oxalic acid two of example of formulations 10
The dispersible oil-suspending agent of acetone amine copper dimethachlon) preventing and treating alternaria leaf spot of apple field test.
Test method reference《Pesticide field efficacy medicine test criterion (two) bactericidal agent for preventing and treating alternaria leaf spot of apple test of pesticide effectiveness
GB/T 17980.124-2004》.Experiment is located at Weinan City Fuping County, and soil is clay, and physical features 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 14 years, distance between rows and hills be 5m ×
6m, the garden spot defoliation occur heavier over the years.Test medicine and extension rate are shown in Table 4, separately set blank control, often handle 4 times
Repeat, per 3 trees of plot area, totally 44 cells, random district's groups arrange.Using conventional spray-on process, blade positive and negative are uniformly sprayed
It is wet.When blade begins to see, second of dispenser in 14 days, common dispenser is twice for first time dispenser.
Investigation and statistical method：
After second of dispenser 14 days carry out disease index investigation, per cell investigate 2 plants tree, every plant divide east, south, west, north,
Middle different azimuth is each to fix 2 young sprouts, investigates its whole blade, record total number of sheets, the sick number of sheets at different levels and sick series, calculates the state of an illness
Index.
Grade scale is:
0 grade, disease-free spot；
1 grade, lesion area accounts for less than the 10% of whole leaf area；
3 grades, lesion area accounts for the 11%~25% of whole leaf area；
5 grades, lesion area accounts for the 26%~40% of whole leaf area；
7 grades, lesion area accounts for the 41%~65% of whole leaf area；
9 grades, lesion area accounts for more than the 65% of whole leaf area.
Disease index and prevention effect computational methods：
Disease index=Σ (the sick numbers of sheets at different levels × relative value of series)/(investigation total number of sheets × 9) × 100
Prevention effect (%)=[(disease index after disease index-chemicals treatment district dispenser after blank district dispenser)/it is empty
Disease index after white check plot dispenser] × 100
Table 4 prevents and treats alternaria leaf spot of apple field test results
Table of field test results is bright：60% 1000 times of oxalic acid copper diacetonamine Carbatene water dispersible granules, 1500 times,
40% 1500 times of oxalic acid copper diacetonamine Bravo suspending agent, 2000 times, 60% oxalic acid copper diacetonamine dimethachlon can divide
Dissipate 2500 times of oil-suspending agent, 3000 times, have good preventive effect to alternaria leaf spot of apple, hence it is evident that better than 30% oxalic acid diacetonamine
1000 times of copper wettable powder, 70% 700 times of Carbatene water dispersible granules, 75% 500 times of Bravo wettable powder, 40% bacterium
The net wettable powder 2000 of core to the preventive effect of alternaria leaf spot of apple, reaches the pole level of signifiance (in detail with the preventive effect difference of single dose again
It is shown in Table 4).
Security survey to apple tree, observe within some days after the 1st day and medicine after spray every time, each chemicals treatment is to apple
Tree occurs without poisoning phenomenon.Experiment also found that three kinds of Mixed Pharmacies also have anti-well to apple marssonina leaf spot, apple mildew
Effect.
After result of the test shows oxalic acid copper diacetonamine and Carbatene, Bravo, dimethachlon mixture, hence it is evident that improve to apple
The prevention effect of fruit spot defoliation, dosage and drug cost are reduced, be preventing and treating apple spot to Apple Growth safety
Defoliation and apple marssonina leaf spot, the favourable agents of apple mildew.
Biological Examples 2：Prevent and treat late blight of potato field test
7~August in 2014 in Fugu County of Shaanxi Province has carried out example of formulations 1, and (48% oxalic acid copper diacetonamine is for gloomy
Zinc water dispersible granules), example of formulations 2 (55% oxalic acid copper diacetonamine mancozeb water dispersible granule), example of formulations 6
(50% oxalic acid copper diacetonamine thiram wettable powder) prevents and treats late blight of potato field test.Test method reference
《Pesticide field efficacy medicine test criterion (one) bactericidal agent for preventing and treating late blight of potato GB/T 17980.34-2000》.
Test arrangement starts incidence of leaf occur, test medicine and dilution times in the plot of morbidity weight over the years in July, 2014
Number is shown in Table 5, separately sets blank control, often handles 4 repetitions, and per the ㎡ of plot area 25, totally 44 cells, random district's groups arrange.Adopt
With conventional spray-on process, blade positive and negative uniformly squirt, liter/mu of decoction dosage 50.First time dispenser is when blade begins to see, 14 days
Second of dispenser, common dispenser is twice.
Investigation and statistical method：
Disease index investigation is carried out within 14 days after second of dispenser, per the 5 points of samplings of cell diagonal, every investigation 2~3
Strain, whole blades are investigated, record total number of sheets, the sick number of sheets at different levels and sick series, calculate disease index.
Grade scale is:
0 grade, disease-free spot；
1 grade, lesion area accounts for less than the 5% of whole leaf area；
3 grades, lesion area accounts for the 6%~10% of whole leaf area；
5 grades, lesion area accounts for the 11%~20% of whole leaf area；
7 grades, lesion area accounts for the 21%~50% of whole leaf area；
9 grades, lesion area accounts for more than the 50% of whole leaf area.
Disease index and prevention effect computational methods：
Disease index=Σ (the sick numbers of sheets at different levels × relative value of series)/(investigation total number of sheets × 9) × 100
Prevention effect (%)=[(disease index after disease index-chemicals treatment district dispenser after blank district dispenser)/it is empty
Disease index after white check plot dispenser] × 100
Table 5 prevents and treats late blight of potato field test results
Table of field test results is bright：48% 1500 times 2000 times of oxalic acid copper diacetonamine water dispersion granules agent of dithane,
55% 1000 times of oxalic acid copper diacetonamine mancozeb water dispersible granule, 1500 times, 50% oxalic acid copper diacetonamine good fortune is beautiful
Double 2000 times of wettable powders, 2500 times, have good preventive effect to the late blight of potato, hence it is evident that better than 30% oxalic acid diacetonamine
1000 times of copper wettable powder, 80% 800 times of Zineb wettable powder, 80% 600 times of mancozeb wettable powder, 25%
Thiram wettable powder 600 to the preventive effect of the late blight of potato, reaches the pole level of signifiance with the preventive effect difference of single dose and (referred to again
Table 5).
Security survey to potato, observe within some days after the 1st day and medicine after spray every time, each chemicals treatment is to Ma Ling
Potato occurs without poisoning phenomenon.
Result of the test shows oxalic acid copper diacetonamine and one kind in protective fungicide zineb, Mancozeb, thiram
After mixture, hence it is evident that improve the prevention effect to the late blight of potato, dosage and drug cost are reduced, to potato growth
Safety, it is the favourable agents for preventing and treating the late blight of potato.
In summary, composition of the invention is to use oxalic acid copper diacetonamine and protective fungicide zineb, Dai Sen
Two kinds of a kind of composition in MnZn, Carbatene, ambam, Propineb, thiram, ziram, Bravo, sulphur, dimethachlon
Active component compound scheme, its activity and bactericidal effect are not the simple superposition of each component activity, with existing unitary agent phase
Than, in addition to significant bactericidal effect, and there is significant synergistic effect, it is good to crop safety, meet pesticidal preparations
Security requirement.
Claims (5)
1. a kind of bactericidal composition containing oxalic acid copper diacetonamine, it is characterised in that lived including the first active component and second
Property composition, the weight ratio of the first active component and the second active component is 1:15~10:1, first active component is oxalic acid
Copper diacetonamine, second active component are sulphur.
2. the bactericidal composition according to claim 1 containing oxalic acid copper diacetonamine, it is characterised in that described first lives
Property composition and the second active component content sum be the bactericidal composition gross weight 5%~90%.
3. the bactericidal composition according to claim 1 or 2 containing oxalic acid copper diacetonamine, the agent of the bactericidal composition
Type is water dispersible granules, wettable powder, suspending agent or dispersible oil-suspending agent.
4. the bactericidal composition according to claim 3 containing oxalic acid copper diacetonamine, the bactericidal composition is used to prevent
Control corps diseases.
5. the bactericidal composition according to claim 4 containing oxalic acid copper diacetonamine, it is characterised in that the crops
Disease is alternaria leaf spot of apple, apple marssonina leaf spot, apple mildew, cucumber downy mildew, powdery mildew of cucumber, potato late blight
Disease.
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| CN101310597A (en) * | 2007-05-21 | 2008-11-26 | 西北农林科技大学农药研究所 | Agricultural antiseptic |
| CN101310600A (en) * | 2007-05-21 | 2008-11-26 | 西北农林科技大学农药研究所 | Sterilization composition |
| CN101456873A (en) * | 2007-12-14 | 2009-06-17 | 西北农林科技大学农药研究所 | Agricultural bactericidal agent |
| CN101768175A (en) * | 2008-12-31 | 2010-07-07 | 西北农林科技大学农药研究所 | Agricultural fungicide of oxalic acid copper diacetonamine |
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| CN1345539A (en) * | 2000-09-28 | 2002-04-24 | 赵晓武 | Disease-proofing pesticide--relative bactericide and cupric sulfate compounded soluble powder agent |
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| CN101310597A (en) * | 2007-05-21 | 2008-11-26 | 西北农林科技大学农药研究所 | Agricultural antiseptic |
| CN101310600A (en) * | 2007-05-21 | 2008-11-26 | 西北农林科技大学农药研究所 | Sterilization composition |
| CN101456873A (en) * | 2007-12-14 | 2009-06-17 | 西北农林科技大学农药研究所 | Agricultural bactericidal agent |
| CN101768175A (en) * | 2008-12-31 | 2010-07-07 | 西北农林科技大学农药研究所 | Agricultural fungicide of oxalic acid copper diacetonamine |
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