[summary of the invention]
The object of the invention is to solve the problem of the undesirable and herbicide resistance of actual preventive effect of the prior art, provide a kind of efficient, low toxicity, quick-acting is good and the lasting period is long, is conducive to the composition pesticide of the wheat weeds comprehensive regulation.
The present invention has adopted following technical scheme: a kind of herbicidal composition containing alkynes oxalic acid and AC322140.Other titles of described alkynes oxalic acid (Clodinafop-propargyl): clodinafop-propargyl, top, Mai Ji, chemical name: (R)-2-[4-(the fluoro-2-pyridine of the chloro-3-of 5-oxygen base) phenoxy group] propionic acid alkynes propyl ester, structural formula is:
Other titles of described AC322140 (Cyclosulfamuron): gold autumn, chemical name: 1-[2-(cyclopropyl carbonyl) phenyl amino sulfonyl]-3-(4,6-SDM-2-yl) urea, structural formula is:
In herbicidal composition of the present invention, active component weight ratio is alkynes oxalic acid: AC322140=3:32~24:1, be preferably 3:8~6:1, more preferably 3:2, the weight percentage of two active components in herbicidal composition is 5~80%, surplus is various auxiliary agents conventional in the Pesticide formulation processes such as carrier, solvent, emulsifier, dispersant, wetting agent, and concrete composition and consumption require to do simple experiment according to formula and determine.
Described herbicidal composition can be prepared into according to the method for well known to a person skilled in the art the various formulations of the applicable agricultural uses such as wetting powder, water dispersible granules, suspending agent, and most preferred dosage form is wetting powder.
Adjuvant used comprising when composition is made wetting powder:
Dispersant can be one or more in lignosulfonates, polycarboxylate, alkylnaphthalene sulfonate, neopelex, alkyl polyoxyethylene ether sulfonate, alkylphenol-polyethenoxy base ether formaldehyde condensation products, and consumption is 1~12% of preparation total amount;
Wetting agent can be one or more in lauryl sodium sulfate, Teepol, fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether, sorbitan fatty acid ester APEO, and consumption is 1~8% of preparation total amount;
Appropriate carrier can be one or more in kaolin, diatomite, attapulgite, bentonite, white carbon.
Adjuvant used comprising when composition is made water dispersible granules:
Dispersant can be one or more in polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate, alkylphenol polyoxyethylene, alkyl polyoxyethylene ether sulfonate, and consumption is 1~10% of preparation total amount;
Wetting agent can be one or more in naphthalene sulfonate, lauryl sodium sulfate, sorbitan fatty acid ester polyoxyethylene ether, alkylsulfonate, and consumption is 1~8% of preparation total amount;
Disintegrant can be one or more in ammonium sulfate, urea, starch and derivative thereof, low-substituted hydroxypropyl cellulose, polyvinylpyrrolidone, sodium alginate, and consumption is 1~5% of preparation total amount;
Adhesive can be one or more in hydroxyethylcellulose, soluble starch, polyethylene glycol, methylcellulose, polycarboxylic acid and water-soluble high-molecular compound sodium carboxymethylcellulose, polyvinyl alcohol, and consumption is 0.1~3% of preparation total amount;
Appropriate carrier can be one or more in white carbon, kaolin, bentonite, precipitated calcium carbonate, gypsum, attapulgite, urea, sucrose.
Adjuvant used comprising when composition is made suspending agent:
Dispersant can be one or more in polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate, TERSPERSE2425, alkylphenol polyoxyethylene, and consumption is 1~8% of preparation total amount;
Wetting agent can be one or more in alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, alkylphenol-polyethenoxy base ether phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, naphthalene sulfonate, and consumption is 0.1~5% of preparation total amount;
Thickener can be one or more in xanthans, carboxymethyl cellulose, Sodium Polyacrylate, bentonite, aluminium-magnesium silicate, and consumption is 0.1~0.5% of preparation total amount;
Antifreezing agent can be one or more in ethylene glycol, propane diols, glycerine, urea, and consumption is 2~6% of preparation total amount;
Preservative can be one or more in formaldehyde, sorbic acid, Sodium Benzoate, and consumption is 0.1~2% of preparation total amount;
Defoamer can be silicone based defoamer, and consumption is 0.1~0.2% of preparation total amount;
Appropriate amount of deionized water.
The present invention possesses following beneficial effect:
1, Herbicidal combinations provided by the invention, expand the herbicide spectrum of alkynes oxalic acid and AC322140 single dose, in certain ratio range, show synergistic function, the control efficiency of composition has had raising than single dose, reduce the using dosage of agricultural chemicals, reduced drug cost and the agricultural chemicals adverse effect to ecotope.
2, Herbicidal combinations provided by the invention, rapidly, the lasting period is long, easy to use, time saving and energy saving in drug effect performance, and it applies huge economic benefit and social benefit.
3, Herbicidal combinations provided by the invention, can reduce the resistance risk that long-term use single herbicide produces, and extends medicament service life, to the comprehensive regulation important in inhibiting of Weed Resistance.
4, Herbicidal combinations provided by the invention is low to crop, toxicity to man and livestock, can in the situation that not injuring crop, kill multiple weeds, safer to crop.
[embodiment]
Product of the present invention and application are described by following specific embodiment, but should not be construed as limitation of the present invention.Without departing from the spirit and substance of the case in the present invention, the amendment of method of the present invention, step or condition etc. being made or replacement all belong to scope of the present invention.
Example of formulations 1:50% alkynes oxalic acid AC322140 wetting powder
Method by frequent above-mentioned raw materials regulation for wetting powder, i.e. front mixing, air-flow crushing, rear mixing, obtain 50% alkynes oxalic acid AC322140 wetting powder.
Example of formulations 2:70% alkynes oxalic acid AC322140 wetting powder
Method by frequent above-mentioned raw materials regulation for wetting powder, i.e. front mixing, air-flow crushing, rear mixing, obtain 70% alkynes oxalic acid AC322140 wetting powder.
Example of formulations 3:30% alkynes oxalic acid AC322140 water dispersible granules
Method by frequent above-mentioned raw materials regulation for water dispersible granules, i.e. front mixing, air-flow crushing, rear mixing, the kneading that adds water, granulation, screening, obtain 30% alkynes oxalic acid AC322140 water dispersible granules.
Example of formulations 4:11% alkynes oxalic acid AC322140 water dispersible granules
Method by frequent above-mentioned raw materials regulation for water dispersible granules, i.e. front mixing, air-flow crushing, rear mixing, the kneading that adds water, granulation, screening, obtain 11% alkynes oxalic acid AC322140 water dispersible granules.
Example of formulations 5:25% alkynes oxalic acid AC322140 suspending agent
Method by frequent above-mentioned raw materials regulation for suspending agent, high speed shear is disperseed, sand milling is pulverized, mediation, obtains 25% alkynes oxalic acid AC322140 suspending agent.
Example of formulations 6:10% alkynes oxalic acid AC322140 suspending agent
Method by frequent above-mentioned raw materials regulation for suspending agent, high speed shear is disperseed, sand milling is pulverized, mediation, obtains 10% alkynes oxalic acid AC322140 suspending agent.
The raw embodiment 1 that surveys
Alkynes oxalic acid and AC322140 cauline leaf are processed synergy toxicity determination test
In order to prevent and treat wheat paddock broad leaved weed and the grassy weed in agricultural production, inventor has carried out indoor virulence testing research with alkynes oxalic acid and two kinds of compositions of AC322140, concrete grammar is: indoor pot method is carried out cauline leaf processing, and experiment is with reference to " farm-chemical indoor determination experiment criterion weed killer herbicide Part IV ".
1, experimental condition
(1) for examination weeds
Clearvers, broadcast ma wormwood artemisia, amur foxtail, wild oat
(2) reagent agent
Alkynes oxalic acid
AC322140
2, examination material is prepared
Cultivation for examination weeds adopts potted plant cultivation.By 11 × 12cm plastic basin, by air-dry the soil that did not use the wheat paddock of weed killer herbicide to adopt back, fill basin after sieving, quantitative 4/5 place of dry ground in basin, P in soil H value 7.0, the content of organic matter 1.2%.Adopt basin alms bowl bottom infiltrating irrigation mode to make soil completely moistening.By amur foxtail, wild oat that last year, field gathered, broadcast ma wormwood artemisia, clearvers seed gibberellin soaks 24h, clear water clean after with dark gauze shading, is placed in the culture dish that is covered with gauze, water is moistening carries out vernalization, after seed shows money or valuables one carries unintentionally, sows.Each approximately 50 the even program requests of amur foxtail and wild oat are at soil surface, earthing 0.5~1.0cm, clearvers and broadcast the every basin of ma wormwood artemisia and broadcast 30~40, earthing 1~2mm, be placed in cellar culture in greenhouse, in incubation, keep ground moistening with the moisturizing of basin alms bowl bottom infiltrating irrigation mode.After weeds emerge, amur foxtail and the every basin of wild oat are decided to be to 20 strains, broadcast the every basin of ma wormwood artemisia and clearvers and be decided to be 10 strains.
3, test is processed
46 processing are established in this test altogether, wherein alkynes oxalic acid establish 15,30,45,60,75g a.i./hm
25 dosage processing, AC322140 establishes 8,16,24,32,40g a.i./hm
25 dosage processing.The two mixedly establishes 7 assembly than processing alkynes oxalic acid and AC322140: 3:128,3:32,3:8,3:2,6:1,24:1,96:1, dosage is respectively 12,24,36,48,60g a.i./hm
2, separately establish 1 clear water contrast, amount to 46 processing, repeat for 4 times.
4, test method
The dispenser time limit fixes on carries out cauline leaf spraying and processes when weeds grew to for 2.5~5 leaf phase, be placed in spray medicine (ASS-4 type pesticide spraying system, DG8003 shower nozzle, atomisation pressure 2.75MPA in tower, spouting liquid 30Kg/ mu), treat that natural air drying is placed on cultivation in greenhouse and observes.
5, data survey and statistical analysis
After processing, observe and record the growth conditions of weeds, process after 30 days, investigation weed control efficacy, records respectively the strain number of weeds, calculates weeds strain preventive effect.By the linear regression analysis between probability value and the logarithm value of series concentration of preventive effect, calculate the ED of each processing
50and correlation coefficient, evaluate the biologically active of each processing to weeds, the abundant method of utilization Sun Yun calculates the co-toxicity coefficient of different medicament proportionings, evaluates the synergy situation of different proportionings, determines alkynes oxalic acid and AC322140 optimum activity ratio.
The abundant method computing formula of Sun Yun:
In formula: E---strain preventive effect;
C---contrast weeds acrial part weeds strain number;
T---process weeds acrial part weeds strain number.
In formula: ATI---mixture actual measurement toxicity index;
The ED of S---standard herbicide
50, unit is a gram per hectare (g a.i./hm
2);
The ED of M---mixture
50, unit is a gram per hectare (g a.i./hm
2).
TTI=TI
A×P
A+TI
B×P
B……………………………………………(3)
In formula: TTI---the theoretical toxicity index of mixture;
TI
a---A medicament toxicity index;
P
a---the percentage composition of A medicament in mixture, unit is percentage (%);
TI
b---B medicament toxicity index;
P
b---the percentage composition of B medicament in mixture, unit is percentage (%).
In formula: CTC---co-toxicity coefficient;
ATI---mixture actual measurement toxicity index;
The theoretical toxicity index of TTI---mixture.
Co-toxicity coefficient CTC >=120 of built agent show as synergistic effect; CTC≤80 show as antagonism; 80 < CTC < 120 show as summation action.
6, result of the test: in Table 1-4
Table 1 alkynes oxalic acid and AC322140 mixture control weeds of wheat clearvers virulence
Table 2 alkynes oxalic acid and AC322140 mixture control weeds of wheat are broadcast ma wormwood artemisia virulence
Table 3 alkynes oxalic acid and AC322140 mixture control weeds of wheat amur foxtail virulence
Table 4 alkynes oxalic acid and AC322140 mixture control weeds of wheat wild oat virulence
Toxicity Determination result shows: alkynes oxalic acid shows as and is added or synergistic effect weeds with AC322140 is mixed in the scope of weight ratio 3:128~96:1, in the scope of weight ratio 3:32~24:1, use with and have good synergistic effect, mixed in the scope of weight ratio 3:8~6:1 have obvious synergistic effect, expanded control of weeds spectrum.
The raw embodiment 2 that surveys
The composite cauline leaf of alkynes oxalic acid and AC322140 is processed the Security test test to wheat
Process the safety to wheat in order to study the composite cauline leaf of alkynes oxalic acid and AC322140, for the rational mixture of alkynes oxalic acid and AC322140 provides scientific basis, inventor has done following test, test is with reference to the agricultural industry criteria NY/T1155.8-2007 of People's Republic of China (PRC) farm-chemical indoor determination experiment criterion-weed killer herbicide, the 8th part: the safety testing cauline leaf spray-on process of crop.
1, experimental condition
(1) for studying thing
Wheat breed: No. 19, Jimai
(2) for examination weeds
Clearvers
(3) reagent agent
Alkynes oxalic acid
AC322140
2, examination material is prepared
(1) for studying thing
Adopt greenhouse pot culture method for the cultivation that studies thing, by 11 × 12cm plastic basin, put in culturing pot, by not using, the soil of adopting back in the wheat paddock of weed killer herbicide was air-dry, after sieving, filled basin, quantitative 4/5 place of dry ground in basin, P in soil H value 7.0, the content of organic matter 1.2%.After adopting basin alms bowl bottom infiltrating irrigation mode to make soil completely moistening, wheat seed is quantitatively broadcasted sowing in soil surface, earthing 0.5~1.0cm, with the moisturizing of basin alms bowl bottom infiltrating irrigation mode, keeps soil fully moistening.
(2) for examination weeds
Cultivation for examination weeds adopts greenhouse pot culture method, by 11 × 12cm plastic basin, puts in culturing pot, by not using, the soil of adopting back in the wheat paddock of weed killer herbicide was air-dry, after sieving, filled basin, quantitative 4/5 place of dry ground in basin, P in soil H value 7.0, the content of organic matter 1.2%.After adopting basin alms bowl bottom infiltrating irrigation mode to make soil completely moistening, quantitatively broadcast sowing in soil surface for examination weed seed pretreated, earthing 1~2mm, with the moisturizing of basin alms bowl bottom infiltrating irrigation mode, keeps soil fully moistening, clearvers is decided to be to 20 strains after weeds emerge.
3, experimental scheme
(1) weeds dispenser dosage
36 processing are established in test altogether, wherein alkynes oxalic acid establish 2.75,5.5,11,22,44g a.i./hm
25 dosage processing, AC322140 establishes 1.5,3,6,12,24g a.i./hm
25 dosage processing.The two mixedly establishes 5 assembly than processing alkynes oxalic acid and AC322140: 3:32,3:8,3:2,6:1,24:1, dosage is respectively 2.5,5,10,20,40g a.i./hm
2, separately establish 1 clear water contrast, amount to 36 processing, repeat 4 times.
(2) crop dispenser dosage
36 processing are established in test altogether, wherein alkynes oxalic acid establish 70,100,130,160,190g a.i./hm
25 dosage processing, AC322140 establishes 50,75,100,125,150g a.i./hm
25 dosage processing.The two mixedly establishes 5 assembly than processing alkynes oxalic acid and AC322140: 3:32,3:8,3:2,6:1,24:1, dosage is respectively 60,90,120,150,180g a.i./hm
2, separately establish 1 clear water contrast, amount to 36 processing, repeat 4 times.
4, application method
The dispenser time limit carries out cauline leaf spraying and processes while fixing on 3~4 leaf phases of wheat, 2.5~5 leaf phase of weeds, be placed in dispenser (ASS-4 type pesticide spraying system in spray tower, DG8003 shower nozzle, atomisation pressure 2.75MPA, spouting liquid 30Kg/ mu), treat that natural air drying is placed on cultivation in greenhouse and observes.
5, data survey and statistical analysis
(1) crop investigation
After dispenser, investigate each processing wheat and have or not symptom of chemical damage, record in detail symptom of chemical damage if having, within after medicine 20 days, measure each processing wheat fresh weight, calculate fresh weight inhibiting rate, the safety with clear and definite test medicine to wheat.
(2) weeds investigation
After dispenser, record in detail the symptom of being injured (as growth inhibition, chlorosis, deformity etc.) of weeds, after medicine 20 days, weigh each processing weeds acrial part fresh weight, adopt growth inhibition assay to calculate the fresh weight preventive effect of weeds.
(3) growth inhibition assay computing formula
In formula:
E-fresh weight preventive effect, unit is percentage (%);
T
0-contrast weeds acrial part fresh weight, unit is gram;
T
1-processing weeds acrial parts fresh weight, unit is gram.
(4) selectivity index computational methods
6, results and analysis is in Table 5-7
The preventive effect of table 5 alkynes oxalic acid mixtures' ratios different from AC322140 to clearvers
The safety of table 6 alkynes oxalic acid mixtures' ratios different from AC322140 to wheat
The selectivity index of table 7 alkynes oxalic acid mixtures' ratios different from AC322140 to wheat
Note: in table 7 data be by market demand DPS2000 data handling system in table 5, table 6 (Tang Qiyi, Feng Mingguang. Practical Statistic analysis and DPS data handling system [M] thereof. Beijing: Science Press, 2002.188-201) calculate.
In the time of selectivity index >=4, represent that the selectivity of medicament between crops and weeds is very high, in the time of 2≤selectivity index < 4, represent that medicament has selectivity between crops and weeds, in the time of selectivity index < 2, represent the poor selectivity of medicament between crops and weeds.Security test test to wheat shows: alkynes oxalic acid is greater than 2 with AC322140 is mixed in the scope of weight ratio 3:32~24:1 to wheat selectivity index, to wheat safety.
The raw embodiment 3 that surveys
Eliminating weed in wheat field field control effectiveness test I:
1, test is processed
8 processing are established in test, repeat for 4 times, process community for totally 32,20 square metres of every processing community areas, and random district group is arranged.(1)~(5) 50% alkynes oxalic acid AC322140 wetting powder (Shandong Binnong Technology Co., Ltd.'s production) is reagent agent, and 15% alkynes oxalic acid wetting powder and 10% AC322140 wetting powder are contrast medicament.Every mu is watered 30 kilograms, adopts 552 third type sprayers (0.7mm aperture) even spraying.Field main weeds has clearvers, broadcasts ma wormwood artemisia, shepherd's purse, hard grass, amur foxtail, wild oat etc.
2, pilot project and method
(1) safety: after dispenser, the situation of growing of investigation wheat, evaluates the safety of reagent agent to wheat.
(2) herbicidal effect: every community is got 4 points at random, 1/4 square metre of every some investigation, after medicine 30 days, record respectively weeds kind and strain number, calculate weeds strain preventive effect.
3, result of the test
(1) safety: dispenser " Invest, Then Investigate ", chemicals treatment district Plant Height in Wheat, Ye Se and blank district are basically identical, show that reagent agent (1)~(5) 50% alkynes oxalic acid AC322140 wetting powder is all to wheat safety.
(2) herbicidal effect: in table 8
30 days various weed control efficacies after table 8 medicine
As shown in Table 8,50% alkynes oxalic acid AC322140 wetting powder of different proportionings between 86.65~95.00%, is all better than contrasting medicament 15% alkynes oxalic acid wetting powder and 10% AC322140 wetting powder (weeds strain preventive effect is respectively 59.92% and 61.92%) to common weed strain preventive effect.Explanation thus, alkynes oxalic acid and AC322140 are within the scope of weight ratio 3:32~24:1, and the weeds common to wheat paddock have preventive effect, and the lasting period is greater than one month, substantially can control the wheat paddock crop smothering in whole vegetative period, and this herbicidal composition is to wheat safety.
Eliminating weed in wheat field field control effectiveness test II:
1, test is processed
(1) 5% alkynes oxalic acid AC322140 wetting powder (3:2) 120g/ mu
(2) 50% alkynes oxalic acid AC322140 wetting powder (3:2) 12g/ mus
(3) 75% alkynes oxalic acid AC322140 wetting powder (3:2) 8g/ mus
3 processing are established in test, repeat for 4 times, process community for totally 12,20 square metres of every processing community areas, and random district group is arranged.(1)~(3) alkynes oxalic acid AC322140 wetting powder (Shandong Binnong Technology Co., Ltd.'s production) is reagent agent, and every mu is watered 30 kilograms, adopts 552 third type sprayers (0.7mm aperture) even spraying.Field main weeds has clearvers, broadcasts ma wormwood artemisia, shepherd's purse, hard grass, amur foxtail, wild oat etc.
2, pilot project and method
Herbicidal effect: every community is got 4 points at random, investigates 1/4 square metre at every, and after dispenser, 30 days investigation weed control efficacies, record respectively weeds kind and strain number, calculate weeds strain preventive effect.
3, result of the test: herbicidal effect is in table 9
30 days various weed control efficacies after table 9 medicine
Note: (1) 5% alkynes oxalic acid AC322140 wetting powder (3:2)
(2) 50% alkynes oxalic acid AC322140 wetting powders (3:2)
(3) 75% alkynes oxalic acid AC322140 wetting powders (3:2)
As shown in Table 9, in the time that the weight ratio of alkynes oxalic acid and AC322140 is 3:2, the alkynes oxalic acid AC322140 wetting powder of different content to common weed strain preventive effect all more than 94%, while showing that alkynes oxalic acid and AC322140 weight ratio are optimal proportion, the herbicidal composition of different activities component content all has significant preventive effect to weeds.
In sum, component of the present invention is reasonable, the activity that preventive effect is better than each component while using separately, grass family and broad leaved weed are all had to good preventive effect, expanded control of weeds spectrum, delayed the generation of herbicide resistance, to crop safety, meet the security requirement of pesticidal preparations.