CN104938503B - Weeding composition and preparation and application thereof - Google Patents
Weeding composition and preparation and application thereof Download PDFInfo
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- CN104938503B CN104938503B CN201510398095.1A CN201510398095A CN104938503B CN 104938503 B CN104938503 B CN 104938503B CN 201510398095 A CN201510398095 A CN 201510398095A CN 104938503 B CN104938503 B CN 104938503B
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Abstract
The invention belongs to the field of weed killers, and particularly relates to a weeding composition and a preparation and application thereof. The weeding composition comprises pyroxsulam and picolinafen. The pyroxsulam and the picolinafen are compounded, and the weeding composition which is remarkable in weeding effect and safe for wheat is obtained. The invention further provides a weed killer of the weeding composition. The weed killer is mainly used for preventing and killing off grassy weeds and broad leaf weeds in wheat fields, is remarkable in weeding effect, wide in weed control spectrum and safe for the wheat, and is an ideal weed killer for preventing and killing off resistant weeds in the wheat fields.
Description
Technical field
The invention belongs to herbicide field, more particularly to a kind of Herbicidal combinations and its preparation and application.
Background technology
Wheat is the general designation of wheat system plant, is a kind of in the grass extensively planted all over the world, in originating from
Eastern crescent fertile soil (Levant) area, is one of crops of cultivation earliest in the world.The caryopsis of wheat be the mankind staple food it
One, wear into and can make after flour the foods such as bread, steamed bun, biscuit, noodles；Beer, alcohol, vodka are can be made into after fermentation, or
Raw matter fuel.Wheat is rich in starch, protein, fat, mineral matter, calcium, iron, thiamine, riboflavin, nicotinic acid, vitamin A and dimension
Raw element C etc..
The weeds of wheat paddock occur generally, and species is various, and the wheat weedses in the north of the Yellow River and big portion in Shandong are with Descurainia sophia, shepherd's purse
Based on dish, grey dish, summer cypress, conical silene herb (rice crock), corn gromwell, the seed of cowherb, chickweed and field thistle；The Yellow River and on the south, Huaihe River,
Yangtze river basin drought stubble wheat weedses are with Descurainia sophia, Herba Galii Teneri, ox chickweed, Veronica, corn gromwell, wild oat, amur foxtail, Tian Xuan
Based on Hua, pivots storage, conical silene herb (rice crock) common vetch and field thistle, some areas wartwort is serious.Wheat After Getting Rice is with grassy weed
Such as：Amur foxtail, wild oat, not hard grass, grass, caput grass, humulus grass, Herba Galii Teneri, ox chickweed, Veronica etc..
In recent years, the control of weeds of wheat paddock was increasingly sophisticated, and wheat paddock grassy weed and broad leaved weed are mixed and got over
Come more serious, and some weeds produce resistance to conventional herbicide kind.For these situations, peasant's weeding scheme is main
The mixed spraying of the simple bucket of several herbicides of blindness in field oneself, such result be often the preventive effect difference of weeds or
Person is to produce poisoning to wheat.
The content of the invention
In view of this, it is an object of the invention to provide a kind of Herbicidal combinations and its preparation and application, present invention offer
Herbicidal combinations for weeds of wheat preventive effect significantly, and to wheat safety.
The invention provides a kind of Herbicidal combinations, including pyroxsulam and fluorine pyrrole acyl grass amine.
Preferably, the mass ratio of the pyroxsulam and fluorine pyrrole acyl grass amine is 1:2～8.
The invention provides a kind of herbicide, including the Herbicidal combinations and auxiliary agent described in above-mentioned technical proposal.
Preferably, the formulation of the herbicide is to dispersible oil-suspending agent.
Preferably, the gross mass for dispersibling pyroxsulam and fluorine pyrrole acyl grass amine in oil-suspending agent is accounted for and entirely dispersible oil
20～50wt% of suspending agent quality.
Preferably, the auxiliary agent that dispersibles in oil-suspending agent includes that emulsifying agent, defoamer, thickener, dispersant, pH are adjusted
One or more in agent, synergist and solvent.
Preferably, the herbicide includes：
Preferably, described emulsifying agent includes polyoxyethylene alkylphenol class emulsifying agent, alkylaryl APEO sulfuric acid
Salt, polyoxyethylene fatty acid ester, polyoxyethylene sorbitol acid anhydride ester, polyoxyethylene fatty alcohol class emulsifying agent, dioctyl succinate sulphur
One or more in sour sodium and EO-PO block copolymers；The defoamer includes that silicone defoamer, C8-C10 are fatty
One or more in alcohol, polyethers defoamer and fatty acid ester defoamer；The thickener include organobentonite and/or
White carbon；The dispersant includes nonionic combed polycarboxylate, alkyl polyethylene glycols dispersant, DBSA
One or more in calcium, thermally coupled distillation columns, AEO and polycarboxylate；The pH is adjusted
Agent includes one or more in sodium acid carbonate, triethanolamine, sodium lignin sulfonate, sodium carbonate and urea；The synergist bag
Include one or more in organosilicon, polyethylene glycol and polyethers；The solvent includes corn oil, soybean salad oil, peanut oil, pine
One or more in fuel-economizing, soybean oil methyl esters and methyl oleate.
The invention provides a kind of application of the herbicide described in above-mentioned technical proposal in eliminating weed in wheat field.
Preferably, the herbicide is applied in the leaf phase of wheat 3～6 and/or the leaf phase of weeds 2～5.
The invention provides a kind of Herbicidal combinations, including pyroxsulam and fluorine pyrrole acyl grass amine.
The Herbicidal combinations that the present invention is provided include pyroxsulam and fluorine pyrrole acyl grass amine.Wherein, the pyroxsulam also known as
Pyroxsulam, CAS (Chemical Abstracts Service, U.S. chemical abstract service society) accession number is 422556-
08-9, shown in its structure such as formula (I)：
Pyroxsulam is sulfonamides absorbability wheat paddock foliar herbicide, by the leaf of weeds, bud and root absorption, is then pressed down
The branched-chain amino acid synthesis of weeds processed, makes weeds depauperation, sallow, death.
In the present invention, fluorine pyrrole acyl grass amine is also known as fluorine metazachlor, CAS (Chemical Abstracts Service, the U.S.
Chemical abstracts service) accession number is 137641-05-5, shown in its structure such as formula (II)：
Fluorine pyrrole acyl grass amine is that amide-type selects contact weedicide, mainly by weeds seedling root absorption, is pressed down in weeds
Phytoene dehydrogenase processed, hinders the biosynthesis of carotenoid.
In the Herbicidal combinations that the present invention is provided, the mass ratio of the pyroxsulam and fluorine pyrrole acyl grass amine is preferably 1:2
～8, more preferably 1:3～6, most preferably 1:3～5, the most preferably 1:4.4.
Compared with prior art, the invention provides a kind of Herbicidal combinations.The Herbicidal combinations that the present invention is provided include
Pyroxsulam and fluorine pyrrole acyl grass amine.The present invention obtains herbicidal effect by the way that pyroxsulam and fluorine pyrrole acyl grass amine are compounded
Significantly, and to the Herbicidal combinations of wheat safety.Test result indicate that, herbicide is to wheat paddock by obtained in the Herbicidal combinations
Weeds have significant preventive effect, and the growth of wheat paddock is not affected, particularly by pyroxsulam and fluorine pyrrole acyl grass amine
Mass ratio is 1:Herbicide obtained in 4.4 Herbicidal combinations is best to the preventive effect of weeds of wheat.
The invention provides a kind of herbicide, including the Herbicidal combinations and auxiliary agent described in above-mentioned technical proposal.
The herbicide that the present invention is provided includes the Herbicidal combinations and auxiliary agent.The formulation of the herbicide preferably can divide
Scattered oil-suspending agent.
It is described to dispersible oil-suspending agent in being the embodiment for dispersibling oil-suspending agent in the herbicide that the present invention is provided
Middle pyroxsulam preferably accounts for the 20～50wt% for entirely dispersibling oil-suspending agent quality with the gross mass of fluorine pyrrole acyl grass amine, more preferably
Account for and entirely dispersible the 23.33～49.68% of oil-suspending agent quality, most preferably account for and entirely dispersible oil-suspending agent quality
36.72%.Wherein, content of the pyroxsulam in herbicide is preferably 2～10wt%, more preferably 4.32～
9.20wt%.Content of the fluorine pyrrole acyl grass amine in herbicide is preferably 18～45wt%, more preferably 19.01～
40.48wt%.
It is described to dispersible oil-suspending agent in being the embodiment for dispersibling oil-suspending agent in the herbicide that the present invention is provided
Middle auxiliary agent preferably includes one kind in emulsifying agent, defoamer, thickener, dispersant, pH adjusting agent, synergist and solvent or many
Kind.
In the present invention, described emulsifying agent preferably includes polyoxyethylene alkylphenol class emulsifying agent, alkylaryl polyoxy second
Alkene ether sulphate, polyoxyethylene fatty acid ester, polyoxyethylene sorbitol acid anhydride ester, polyoxyethylene fatty alcohol class emulsifying agent, butanedioic acid
One or more in dioctyl ester sodium sulfonate and EO-PO block copolymers.Wherein, the polyoxyethylene alkylphenol class emulsifying agent
Model is preferably vo/01, TX-10, TX-9 or TX-7.The model of the alkylaryl polyoxyethylene ether sulfate is preferably vo/
02nd, EO/02, SP-3462 or SOPA-270.The model of the polyoxyethylene fatty acid ester is preferably SP-3468, VO/02N, C-
280 or 5500.The model of the polyoxyethylene sorbitol acid anhydride ester is preferably SOD, polysorbas20, polysorbate40 or polysorbate60.It is described poly-
The model of oxygen ethene aliphatic alcohols emulsifying agent is preferably YUS-110, paregal O -8, paregal O -9 or paregal O -10.It is described
The model of dioctyl sodium sulfosuccinate is preferably MF-31, OT, penetrant t or 7580.The EO-PO block copolymers also known as
Polyoxyethylene polyoxypropylene block copolymer, its model is preferably 601, agriculture breast 1601, agriculture breast 1602 or peaceful breast 32.In the present invention
In, content of the emulsifying agent in herbicide is preferably 10～30wt%, more preferably 10～15wt%.
In the present invention, the defoamer includes silicone defoamer, C8-C10 fatty alcohols, polyethers defoamer and fat
One or more in fat esters of gallic acid defoamer.The model of the silicone defoamer is preferably DF-1398.In the present invention
In, content of the defoamer in herbicide is preferably 0～0.5wt%, more preferably 0.05～0.4wt%.
In the present invention, thickener includes organobentonite and/or white carbon.Wherein, the bentonite model
Preferably 838F；The model of the white carbon is preferably BH-1000.In the present invention, the thickener containing in herbicide
Amount is preferably 0～5wt%, more preferably 0.5～4.5wt%.
In the present invention, the dispersant preferably include nonionic combed polycarboxylate, alkyl polyethylene glycols dispersant,
One kind in calcium dodecyl benzene sulfonate, thermally coupled distillation columns, AEO and polycarboxylate or
It is various.Wherein, the model of the nonionic combed polycarboxylate be preferably SP-OD3472,9200, D982 or 2700.The alkane
The model of base polyethylene glycols dispersant is preferably AB600, PEG200, PEG400 or PEG1500.The type of the alkyl sulfonic acid class
Number be preferably No. 500, NN0, N or M-9.The model of the thermally coupled distillation columns is preferably YUS-60P, NP-10-
P, 655G or SC-3.The model of the AEO is preferably 2510, AEO4、AEO7Or AEO9.The polycarboxylate
Model be preferably SP-3462,2700, T/36 or GY-D800.In the present invention, content of the dispersant in herbicide
Preferably 3～10wt%, more preferably 3～8wt%.
In the present invention, the pH adjusting agent preferably includes sodium acid carbonate, triethanolamine, sodium lignin sulfonate, sodium carbonate
With one or more in urea.Wherein, the model of the sodium lignin sulfonate be preferably REXA88B, M-9, REXA88A or
NA.In the present invention, content of the pH adjusting agent in herbicide is preferably 0～5wt%, more preferably 0.6～5wt%.
In the present invention, the synergist preferably includes one or more in organic silicon, polyethylene glycol and polyethers.Its
In, the model of the organosilicon be preferably BH-100,408, L-77 or S240.The model of the polyethylene glycol is preferably
PEG200, PEG400 or PEG600.The model of the polyethers is preferably SP-400, NP-10, JFC or OP-10.In the present invention,
Content of the synergist in herbicide is preferably 2～6wt%, more preferably 4～6wt%.
In the present invention, the solvent preferably includes plant oil solvent, more preferably including corn oil, soybean salad oil,
One or more in peanut oil, turpentine oil, soybean oil methyl esters and methyl oleate.
In one embodiment that the present invention is provided, the herbicide includes the Herbicidal combinations, emulsifying agent, froth breaking
Agent, thickener, dispersant, pH adjusting agent, synergist and solvent, each component content of the weeding is:
In another embodiment that the present invention is provided, the herbicide includes the Herbicidal combinations, emulsifying agent, froth breaking
Agent, thickener, dispersant, pH adjusting agent, synergist and solvent, each component content of the weeding is:
In the present invention, the preparation technology for dispersibling oil-suspending agent is not particularly limited, preferably according to lower section
Method is prepared：
According to quality of material ratio in above-mentioned formula, pyroxsulam, fluorine pyrrole acyl grass amine and auxiliary agent are accurately weighed successively and is added to
In sand mill, it is ground.In sand grinding process, the ratio of sand material and material is preferably controlled in 0.5～2:1, more preferably control 1
～1.37:1, most preferably control 1:1；The temperature of the sand milling is preferably controlled in 30～40 DEG C；The time of the sand milling is preferred
Control is in 2～3h.The fineness of preparation is detected at the end of sand milling, until fineness of materials is reached requiring after fineness, stops sand milling, filtered
Discharging, obtains the herbicide of present invention offer.The requirement fineness of the material is preferably 3～8 μm, more preferably 4～5 μm.
To dispersible oil-suspending agent, the formulation is with non-water system (oil base) as dispersion to the formulation of the herbicide that the present invention is provided
Medium, Herbicidal combinations are processed in decentralized medium stable suspersion system using the effect of functionalized surface coagent.
Said preparation great advantage is that have good tackness and plate-out ability, resistance of rainwater washing against when in use；Simultaneously decentralized medium is plant
Thing oil or vegetable oil esters compound, it is good with environment intermiscibility, is environmental protection.
, by auxiliary agent species and ratio in reasonable selection formula, its Herbicidal combinations provided with this law can be complete for the present invention
U.S. combines, and the oil-suspending agent preparation property indices that dispersible for obtaining are stablized.Test result indicate that, the weeding that the present invention is provided
Active ingredient pyroxsulam and fluorine pyrrole acyl grass amine in agent is stable in the formulation, and resolution ratio is controlled within 5% after heat storage, two
The suspensibility of active ingredient reaches more than 90%, formulation aesthetics hierarchical control 5%～10% and bottom is without caking, emulsifies in water
Good dispersion property, viscosity is controlled within 300 centipoises, and it is qualified to topple over performance, persistent foamability control in 1 minute 30 milliliters with
Interior, wettability (200 times of dilution is determined afterwards with canvas sedimentation) can be controlled in 1 minute or so complete wetting, and preparation particle diameter reaches
To 5 microns of (D90), better stability of preparation.
The herbicide that the present invention is provided has significant preventive effect to weeds of wheat, and the growth to wheat paddock does not have shadow
Ring.Test result indicate that, adopt the herbicide of present invention offer the leaf phase of wheat seeding 3～6 and/or the leaf phase of weeds 2～5 with effectively into
Point meter dosage 3.05～10.45g/ mus are watered and carry out cauline leaf spray pesticide, after dispenser 40 days to hard grass, amur foxtail and total grass
Fresh weight preventive effect is respectively：80.98%～91.34%, 91.42%～96.28% and 87.32～93.81.After dispenser 60 days to shepherd's purse
The fresh weight preventive effect of dish, ox chickweed and total grass is respectively：54.77～71.87%, 50.66～65.23%, 53.72～68.45%；
Meanwhile, wheat growth is not affected after dispenser.
The invention provides a kind of application of above-mentioned herbicide in eliminating weed in wheat field.
In the application that the present invention is provided, using described herbicide eliminating weed in wheat field.In the present invention, it is preferred to little
The leaf phase of wheat 3～6 and/or the leaf phase of weeds 2～5 apply the herbicide.The position that the herbicide applies is plant stem-leaf.It is described
As active ingredients 3.05～10.45g/ of dosage mus are advisable the formulation rate of herbicide.
Herbicide application provided by the present invention gives herbicide and plays drug effect optimal dispenser period, wheat safe medication
The key technology information such as phase and herbicide applied amount, for herbicide certain directive significance is applied with.
The herbicide that the present invention is provided is efficient, safe and environment-friendly, is worth wideling popularize application on wheat paddock.
Specific embodiment
Oil-suspending agent formulating is dispersibled to the present invention and is processed into after preparation with reference to specific embodiment and carry out medicine
Effect test is described further：
Embodiment 1
Prepare pyroxsulam and dispersible oil-suspending agent
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.77g, polyoxyethylene alkylphenol class breast
Agent (vo/01, Luo Diya) 12g, nonionic combed polycarboxylate (space is held up in SP-OD3472, Jiangsu) 5g, dioctyl succinate sulphur
Sour sodium (MF-31, Mei Feng company) 3g, sodium acid carbonate 5g, organobentonite (838F models, sky dragon chemical industry) 0.5g, silicone
Defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon (BH-100, Guangzhou one hundred are modest) 5g, soybean salad oil 61.68g
In being added to beaker, after being uniformly mixed, in being added to the Micro Sand Mill for filling 137g Zirconia beads, start sand mill
Switch, grinding temperature control at 30～40 DEG C, grinding 2 hours after, detect preparation fineness reach after 5 microns shut down,
Filtering and discharging, obtains 7.5wt% pyroxsulams and dispersibles oil-suspending agent.Said preparation will subsequently be used for joint co-toxicity coefficient measure.
Embodiment 2
Prepare fluorine pyrrole acyl grass amine and dispersible oil-suspending agent
Successively electronic scale weighs fluorine pyrrole acyl grass amine active compound (content is 97wt%) 51.5g, polyoxyethylene alkylphenol class breast
Agent (vo/01, Luo Diya) 12g, nonionic combed polycarboxylate (space is held up in SP-OD3472, Jiangsu) 5g, dioctyl succinate sulphur
Sour sodium (MF-31, Mei Feng company) 3g, sodium acid carbonate 5g, organobentonite (838F models, sky dragon chemical industry) 0.5g, silicone
Defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon (BH-100, Guangzhou one hundred are modest) 5g, soybean salad oil 17.95g
In being added to beaker, after being uniformly mixed, in being added to the Micro Sand Mill for filling 137g Zirconia beads, start sand mill
Switch, grinding temperature control at 30～40 DEG C, grinding 2 hours after, detect preparation fineness reach after 5 microns shut down,
Filtering and discharging, that is, obtain 50wt% fluorine pyrroles acyl grass amine and dispersible oil-suspending agent.Said preparation will subsequently be used for the survey of joint co-toxicity coefficient
It is fixed.
Embodiment 3
Joint co-toxicity coefficient is determined
The synergy compounded for clear and definite pyroxsulam, fluorine pyrrole acyl grass amine and the feasibility in wheat paddock application, medicament is adopted
The single dose being processed into embodiment 1 and embodiment 2, dosage ratio is selected using the mixed mode of bucket, using greenhouse pot culture biologicall test
Method, is the percentage of control by calculating each inhibition percentage for processing aerial growth and remaining weeds, and uses Gobly methods
Evaluate the two mixed synergy type to weeds.Wherein, mixe herbicide theoretical fresh weight theory preventive effect as follows
Calculate：
E0=X+Y (100-X)/100
In formula：X dispersibles fresh weight preventive effect when oil-suspending agent (A) consumption is P to weeds for 7.5wt% pyroxsulams；Y is
50wt% fluorine pyrroles acyl grass amine dispersibles fresh weight preventive effect when oil-suspending agent (B) consumption is Q to weeds；E0For 7.5wt% pyridines sulphur grass
Amine dispersibles oil-suspending agent (A) consumption and dispersibles when oil-suspending agent (B) consumption is Q to weeds for P+50wt% fluorine pyrroles acyl grass amine
Fresh weight preventive effect.
Test result is as shown in table 1：
Medicament A, B two-spot of table 1 compounds the synergy to amur foxtail and determines (20d after medicine)
It can be seen from Table 1 that, two kinds of medicaments have activity of weeding to weeds of wheat amur foxtail.By E-E0(%) value
As can be seen that being more than theoretical preventive effect, pyroxsulam and fluorine pyrrole to the actual preventive effect of amur foxtail after two kinds of composite reagents
The suitable quality proportioning of acyl grass amine is 1:There is synergistic effect when 2～8, wherein proportioning is most preferably compounded for sequence number (14), its pyridine sulphur
The mass ratio of careless amine and fluorine pyrrole acyl grass amine is 1:4.4.
Embodiment 4
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 4.48g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 19.6g, polyoxyethylene alkylphenol class emulsifying agent (vo/01, Luo Diya) 12g, nonionic combed polycarboxylate (SP-
Space is held up in OD3472, Jiangsu) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium acid carbonate 5g, organobentonite
(838F models, sky dragon chemical industry) 0.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon (BH-
100th, Guangzhou one hundred is modest) 5g, soybean salad oil 45.37g be added in beaker, after being uniformly mixed, be added to and fill 137g oxygen
In changing the Micro Sand Mill of zirconium pearl, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, after grinding 2 hours, inspection
The fineness for surveying preparation reaches shutdown, filtering and discharging after 5 microns, that is, obtain 23.33wt% pyroxsulam fluorine pyrroles acyl grass amine
Dispersible oil-suspending agent.
Embodiment 5
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 5.51g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 24.1g, polyoxyethylene alkylphenol class emulsifying agent (vo/01, Luo Diya) 15g, nonionic combed polycarboxylate (SP-
Space is held up in OD3472, Jiangsu) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium acid carbonate (commercially available, technical grade)
5g, organobentonite (838F models, sky dragon chemical industry) 0.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest)
0.05g, organosilicon (BH-100, Guangzhou one hundred are modest) 5g, soybean salad oil 36.81g are added in beaker, after being uniformly mixed,
In being added to the Micro Sand Mill for filling 137g Zirconia beads, start the switch of sand mill, grinding temperature is controlled 30～40
DEG C, after grinding 2 hours, detecting that the fineness of preparation reaches and shut down after 5 microns, filtering and discharging obtains 28.73wt% pyridine sulphurs
Careless amine fluorine pyrrole acyl grass amine dispersibles oil-suspending agent.
Embodiment 6
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 6.53g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 28.58g, polyoxyethylene alkylphenol class emulsifying agent (vo/01, Luo Diya) 15g, nonionic combed polycarboxylate
(space is held up in SP-OD3472, Jiangsu) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium acid carbonate 5g, organic bentonite
Profit soil (838F models, sky dragon chemical industry) 0.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon
(BH-100, Guangzhou one hundred are modest) 5g, soybean salad oil 31.34g is added in beaker, after being uniformly mixed, is added to and fills
In the Micro Sand Mill of 137g Zirconia beads, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, and grinding 2 is little
Shi Hou, detects that the fineness of preparation reaches and shut down after 5 microns, filtering and discharging obtains 34.02wt% pyroxsulam fluorine pyrroles
Acyl grass amine dispersibles oil-suspending agent.
Embodiment 7
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.56g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 33.11g, polyoxyethylene alkylphenol class emulsifying agent (vo/01, Luo Diya) 15g, nonionic combed polycarboxylate
(space is held up in SP-OD3472, Jiangsu) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium acid carbonate 5g, organic bentonite
Profit soil (838F models, sky dragon chemical industry) 0.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon
(BH-100, Guangzhou one hundred are modest) 5g, soybean salad oil 25.78g is added in beaker, after being uniformly mixed, is added to and fills
In the Micro Sand Mill of 137g Zirconia beads, start the switch of sand mill, after grinding 2 hours, the fineness for detecting preparation reaches 5
Shut down after microns, filtering and discharging, that is, obtain 39.42wt% pyroxsulam fluorine pyrroles acyl grass amine and dispersible oil-suspending agent.
Embodiment 8
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 8.60g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 37.65g, alkylaryl polyoxyethylene ether sulfate (vo/02, Luo Diya) 12g, calcium dodecyl benzene sulfonate
(No. 500, Historic Area of Zhongshan in Nanjing City) 3g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, triethanolamine 2g, organobentonite
(838F models, sky dragon chemical industry) 0.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, organosilicon (BH-
100th, Guangzhou one hundred is modest) 6g, methyl oleate 27.20g be added in beaker, and after being uniformly mixed, it is added to and fills 137g oxidations
In the Micro Sand Mill of zirconium pearl, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, after grinding 2 hours, detection
The fineness of preparation reaches and shut down after 5 microns, filtering and discharging, that is, obtaining 44.82wt% pyroxsulam fluorine pyrroles acyl grass amine can
Dispersion oil-suspending agent.
Embodiment 9
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 9.53g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 41.73g, polyoxyethylene fatty acid ester (space is held up in SP-3468, Jiangsu) 14g, polycarboxylate (hold up by SP-3462, Jiangsu
Space) 8g, sodium lignin sulfonate (REXA88B, virtue dimension are real big gram) 1.5g, white carbon (BH-1000, Guangzhou lily) 1.5g, have
Machine silicon class defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.05g, polyethylene glycol (PEG200 models, Jiangsu Hai'an) 4g, turpentine
Oily 19.69g is added in beaker, after being uniformly mixed, in being added to the Micro Sand Mill for filling 137g Zirconia beads, is opened
The switch of dynamic sand mill, grinding temperature is controlled at 30～40 DEG C, and after grinding 1.5 hours, the fineness for detecting preparation reaches 5 microns of left sides
Shut down behind the right side, filtering and discharging, that is, obtain 49.68wt% pyroxsulam fluorine pyrroles acyl grass amine and dispersible oil-suspending agent.
Embodiment 10
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.05g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 30.85g, polyoxyethylene sorbitol acid anhydride ester (SOD, support receive chemistry) 10g, AEO (2510, it is prosperous
Si Mai) 4g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 5g, sodium carbonate 2g, organobentonite (838F models, day
Imperial chemical industry) 3.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.25g, polyethers (space is held up in SP-400, Jiangsu)
4g, peanut oil 33.35g are added in beaker, after being uniformly mixed, are added to the miniature sand milling for filling 137g Zirconia beads
In machine, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, after grinding 2 hours, the fineness for detecting preparation reaches 5
Shut down after microns, filtering and discharging, that is, obtain 36.72% pyroxsulam fluorine pyrrole acyl grass amine and dispersible oil-suspending agent.
Embodiment 11
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.05g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 30.85g, polyoxyethylene fatty alcohol class emulsifying agent (YUS-110, outstanding bodyguard chemistry) 11g, NPE
Phosphate (YUS-60P, outstanding bodyguard chemistry) 3.5g, EO-PO block copolymer (No. 601, the triumphant unit in Jiangsu) 2g, urea 5g, organic bentonite
Profit soil (838F models, sky dragon chemical industry) 4.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest) 0.4g, organosilicon
(BH-100, Guangzhou one hundred are modest) 5g, soybean oil methyl esters 30.70g are added in beaker, after being uniformly mixed, are added to and are filled 137
In the Micro Sand Mill of gram Zirconia beads, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, is ground 2 hours
Afterwards, detect that the fineness of preparation to reach shut down after 5 microns, filtering and discharging obtains 36.72wt% pyroxsulam fluorine pyrrole acyls
Careless amine dispersibles oil-suspending agent.
Embodiment 12
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.05g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 30.85g, alkylaryl polyoxyethylene ether sulfate (vo/02, Luo Diya) 15g, polycarboxylate (SP-3462, river
Su Qingyu) (REXA88B, virtue dimension are real for 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium lignin sulfonate
Big gram) 1.6g, white carbon (BH-1000, Guangzhou lily) 1.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred are modest)
0.2g, organosilicon (BH-100, Guangzhou one hundred are modest) 6g, methyl oleate 29.80g are added in beaker, after being uniformly mixed, are added
To in the Micro Sand Mill for filling 137g Zirconia beads, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C, ground
After 2 hours, the fineness for detecting preparation reaches shutdown, filtering and discharging after 5 microns to mill, that is, obtain 36.72wt% pyridines sulphur grass
Amine fluorine pyrrole acyl grass amine dispersibles oil-suspending agent.
Embodiment 13
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.05g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 30.85g, alkylaryl polyoxyethylene ether sulfate (vo/02, Luo Diya) 15g, polycarboxylate (SP-3462, river
Su Qingyu) (REXA88B, virtue dimension are real for 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium lignin sulfonate
Big gram) 1.6g, organobentonite (838F models, sky dragon chemical industry) 1.5g, silicone defoamer (DF-1398 models, Guangzhou one hundred
It is modest) 0.2g, polyethers (space is held up in SP-400, Jiangsu) 6g, methyl oleate 29.80g be added in beaker, after being uniformly mixed, plus
Enter in the Micro Sand Mill for filling 137g Zirconia beads, start the switch of sand mill, grinding temperature is controlled at 30～40 DEG C,
After grinding 2 hours, detect that the fineness of preparation reaches and shut down after 5 microns, filtering and discharging obtains 36.72wt% pyridines sulphur grass
Amine fluorine pyrrole acyl grass amine dispersibles oil-suspending agent.
Embodiment 14
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5wt%) 7.05g, fluorine pyrrole acyl grass amine active compound (content
For 97wt%) 30.85g, alkylaryl polyoxyethylene ether sulfate (vo/02, Luo Diya) 15g, alkyl polyethylene glycols dispersion
Agent (AB600, the prompt profit in Nanjing) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium lignin sulfonate
(REXA88B, virtue dimension are real big gram) 0.6g, organobentonite (838F models, sky dragon chemical industry) 2.0g, silicone defoamer
(DF-1398 models, Guangzhou one hundred are modest) 0.2g, polyethers (space is held up in SP-400, Jiangsu) 6g, methyl oleate 30.30g are added to beaker
In, after being uniformly mixed, in being added to the Micro Sand Mill for filling 137g Zirconia beads, start the switch of sand mill, grind
At 30～40 DEG C, after grinding 2 hours, the fineness of detection preparation reaches and shut down after 5 microns mill temperature control, filtering and discharging,
Obtain 36.72wt% pyroxsulam fluorine pyrroles acyl grass amine and dispersible oil-suspending agent.
Embodiment 15
Prepare pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide
Successively electronic scale weighs pyroxsulam active compound (content is 96.5%) 7.05g, fluorine pyrrole acyl grass amine active compound (content is
97%) 30.85g, alkylaryl polyoxyethylene ether sulfate (vo/02, Luo Diya) 15g, nonionic combed polycarboxylate (SP-
Space is held up in OD3472, Jiangsu) 5g, dioctyl sodium sulfosuccinate (MF-31, Mei Feng company) 3g, sodium lignin sulfonate (REXA88B,
Virtue dimension is real big gram) 1.0g, organobentonite (838F models, sky dragon chemical industry) 2.5g, silicone defoamer (DF-1398 types
Number, Guangzhou one hundred it is modest) 0.2g, polyethylene glycol (PEG400 models, Jiangsu Hai'an) 6g, methyl oleate 29.40g be added in beaker,
After being uniformly mixed, in being added to the Micro Sand Mill for filling 137g Zirconia beads, start the switch of sand mill, grinding temperature
At 30～40 DEG C, after grinding 2 hours, the fineness for detecting preparation reaches shutdown after 5 microns, and filtering and discharging is obtained final product for degree control
Oil-suspending agent is dispersibled to 36.72% pyroxsulam fluorine pyrrole acyl grass amine.
The indices detection of prepared pyroxsulam and fluorine pyrrole acyl grass amine complex weedicide, according to following standard method
Carry out:
The assay method of the agricultural chemicals pH value of GB/T 1601
GB/T 14825-2006 agricultural-chemical suspension rate assay methods
The pesticide powders of GB/T 16150, wettable powder fineness assay method
The agricultural chemicals heat storage stability assay methods of GB/T 19136
The agricultural chemicals low-temperature stability assay methods of GB/T 19137
GB/T 28137-2011 agricultural chemicals persistent foamability assay methods
FAO/WTO MT 180
FAO/WTO MT 148.1
The part of NYT 1860.21-2010 agricultural chemicals physical and chemical property determinings test guidance the 21st：Viscosity
Fineness is determined using laser particle analyzer.
The test result of indices is carried out to complex weedicide obtained in embodiment 4～15 as shown in table 2, table 3.
Testing result contrast in the embodiment 4～9 of table 2
The active ingredient pyroxsulam and fluorine pyrrole acyl grass amine of the herbicide provided by the data in table 2, the present invention
Stable in the formulation, resolution ratio is controlled within 5% after heat storage, and the suspensibility of two active ingredient reaches more than 90%, system
Agent outward appearance hierarchical control 5%～10% and bottom is without caking；Emulsion dispersion property is good in water, and viscosity is controlled within 300 centipoises,
Topple over performance qualified, persistent foamability is controlled within 30 milliliters within 1 minute, and (canvas sedimentation is used afterwards in 200 times of dilution to wettability
Determine) can control in 1 minute or so complete wetting, preparation particle diameter reaches 5 microns of (D90), better stability of preparation.
Testing result contrast in the embodiment 10～15 of table 3
According to indices data such as viscosity, the fineness determined in table 3, production auxiliary agent cost is considered further that, obtain the present invention
Optimum formula for example 13 formula, the content of wherein active ingredient is respectively：Pyroxsulam is 6.8wt%, fluorine pyrrole acyl grass
Amine content is 29.92wt%, and total content is:36.72wt%.
Preventive effect and security test of the herbicide of the present invention in wheat paddock
The present invention is made into formulation products by embodiment 13, comparison medicament is selected on market：7.5wt% pyroxsulam moisture
Shot agent and 50wt% fluorine pyrroles acyl grass amine suspending agent, wheat enters in 3～6 leaf phases and/or weeds in 2～5 leaf phases in wheat paddock
Row directed spraying, observes the security of the growth to wheat, while statistics is miscellaneous to weeds shepherd's purse, amur foxtail, hard grass, ox chickweed etc.
The fresh weight efficiency test result of grass.40 days fresh weight preventive effect data such as institutes of table 4 to hard grass, amur foxtail and total grass wherein after dispenser
Show；60 days anti-data to shepherd's purse, ox chickweed and total grass are as shown in table 5 after dispenser.
40 days fresh weight preventive effect data to hard grass, amur foxtail and total grass after the dispenser of table 4
60 days fresh weight preventive effect data to shepherd's purse, ox chickweed and total grass after the dispenser of table 5
As can be seen from the above two tables, herbicide obtained in embodiment 13 is to preventing and kill off winter wheat field annual grassy weeds, Yu Dong
Front or early spring (the leaf phase of wheat seeding 3～6 and/or the leaf phase of weeds 2～5) dispenser, preparation mu consumption is watered cauline leaf spraying for 10～25 grams
Dispenser.40 days fresh weight preventive effects to hard grass, amur foxtail and total grass are respectively after dispenser：80.98%～91.34%, 91.42%～
96.28% and 87.32～93.81.60 days fresh weight preventive effects to shepherd's purse, ox chickweed and total grass are respectively after dispenser：54.77～
71.87%th, 50.66～65.23%, 53.72～68.45%.
In the present embodiment, wheat growth is not affected after dispenser, illustrates the herbicide of the offer of embodiment 13 to wheat
Neoasozin is complete.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. the quality of a kind of Herbicidal combinations, including pyroxsulam and fluorine pyrrole acyl grass amine, the pyroxsulam and fluorine pyrrole acyl grass amine
Than for 1:2～8.
2. a kind of herbicide, including the Herbicidal combinations and auxiliary agent described in claim 1.
3. herbicide according to claim 2, it is characterised in that the formulation of the herbicide is to dispersible oil-suspending agent.
4. herbicide according to claim 3, it is characterised in that described to dispersible pyroxsulam and fluorine pyrrole in oil-suspending agent
The gross mass of acyl grass amine accounts for the 20～50wt% for entirely dispersibling oil-suspending agent quality.
5. herbicide according to claim 4, it is characterised in that described to dispersible auxiliary agent in oil-suspending agent and include emulsification
One or more in agent, defoamer, thickener, dispersant, pH adjusting agent, synergist and solvent.
6. herbicide according to claim 5, it is characterised in that the herbicide includes：
7. herbicide according to claim 5, it is characterised in that described emulsifying agent includes polyoxyethylene alkylphenol class breast
Agent, alkylaryl polyoxyethylene ether sulfate, polyoxyethylene fatty acid ester, polyoxyethylene sorbitol acid anhydride ester, polyoxyethylene fat
One or more in fat alcohols emulsifying agent, dioctyl sodium sulfosuccinate and EO-PO block copolymers；The defoamer includes
One or more in silicone defoamer, C8-C10 fatty alcohols, polyethers defoamer and fatty acid ester defoamer；It is described
Thickener includes organobentonite and/or white carbon；The dispersant includes nonionic combed polycarboxylate, alkyl polyethylene glycol
In class dispersant, calcium dodecyl benzene sulfonate, thermally coupled distillation columns, AEO and polycarboxylate
One or more；The pH adjusting agent is included in sodium acid carbonate, triethanolamine, sodium lignin sulfonate, sodium carbonate and urea
One or more；The synergist includes one or more in organosilicon, polyethylene glycol and polyethers；The solvent includes corn
One or more in oil, soybean salad oil, peanut oil, turpentine oil, soybean oil methyl esters and methyl oleate.
8. application of the herbicide as any one of claim 3～7 in eliminating weed in wheat field.
9. application according to claim 8, it is characterised in that apply in the leaf phase of wheat 3～6 and/or the leaf phase of weeds 2～5
The herbicide.
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| CN109221225A (en) * | 2018-09-28 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of dinotefuran synergy suspending agent and preparation method thereof |
| CN110583665B (en) * | 2019-10-17 | 2022-04-22 | 美丰农业科技(上海)有限公司 | Preparation method and application of quinclorac oil suspension herbicide |
| CN113133450B (en) * | 2020-01-17 | 2023-10-20 | 成都新朝阳作物科学股份有限公司 | Use of polyether compounds as potentiators of herbicides |
| CN111972406A (en) * | 2020-07-29 | 2020-11-24 | 南京太化化工有限公司 | Auxiliary agent for dispersible oil suspending agent and nicosulfuron dispersible oil suspending agent |
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| GB201308609D0 (en) * | 2013-05-14 | 2013-06-19 | Syngenta Ltd | Mixtures of haloalkysulfonanilide derivatives and herbicides |
| CN104488917A (en) * | 2014-11-26 | 2015-04-08 | 广东中迅农科股份有限公司 | Weeding composition containing diflufenican and pyroxsulam |
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Effective date of registration: 20190813 Address after: Room 2111, No. 2, Lane 289, Zheqiao Road, China (Shanghai) Free Trade Pilot Area, Pudong New Area, Shanghai 200000 Patentee after: Meifeng Agricultural Science and Technology (Shanghai) Co., Ltd. Address before: No. 2 Jiufengshan Road, Longwan District, Wenzhou City, Zhejiang Province, 325000 Patentee before: Maifon Agricultural Chemicals Co., Ltd. |