CN115152786A - Herbicide composition and application thereof - Google Patents
Herbicide composition and application thereof Download PDFInfo
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- CN115152786A CN115152786A CN202210774601.2A CN202210774601A CN115152786A CN 115152786 A CN115152786 A CN 115152786A CN 202210774601 A CN202210774601 A CN 202210774601A CN 115152786 A CN115152786 A CN 115152786A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
- A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
- A01N33/20—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group
- A01N33/22—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group having at least one oxygen or sulfur atom and at least one nitro group directly attached to the same aromatic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P13/00—Herbicides; Algicides
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Abstract
The invention relates to a herbicide composition and a use method thereof, and the herbicide composition containing glufosinate-ammonium comprises the following effective components: glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl; the mass ratio of the glufosinate-ammonium, the oxyfluorfen to the haloxyfop-R-methyl is 10-16. The herbicide composition disclosed by the invention is prepared by compounding the glufosinate-ammonium, the oxyfluorfen and the efficient haloxyfop-methyl, has an obvious synergistic effect, can effectively kill annual or perennial dicotyledons and gramineous weeds and field broad-leaved weeds, is longer in duration and has an obvious effect of inhibiting the green turning of weeds. When the content of the active ingredients is relatively low, a good weeding effect can be realized, the medication cost is reduced, and the environment-friendly policy requirements of national synergy and application reduction are met.
Description
Technical Field
The invention relates to the technical field of herbicides, and particularly relates to a herbicide composition and application thereof.
Background
The weeds in non-cultivated land are weeds except cultivated land, which often bring adverse effects to the life of people, and weeding by using the herbicide is the most economic and effective means in weed control. Due to the fact that the biocidal herbicides such as glyphosate and paraquat are applied singly in an excessive mode, a lot of weeds generate high drug resistance and are difficult to kill. Moreover, the weeds are quickly turned green, and the dosage of the herbicide needs to be increased to kill the weeds, so that the resistance of the weeds is further enhanced, and the large-amount application of the herbicide causes great harm to the environment. Thus, there is a need for a combination of novel herbicides that are highly effective, low residue, and low pollution.
Disclosure of Invention
The first object of the present invention is to provide a novel herbicide composition, and the second object of the present invention is to provide a method for using the herbicide composition.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a herbicide composition in a first aspect, which comprises effective components and an auxiliary agent; the effective components comprise glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl, the mass ratio of the glufosinate-ammonium to the oxyfluorfen to the haloxyfop-R-methyl is 10-16: 2-4, and the effective components in the mass ratio can effectively improve the control effect of the herbicide composition.
Preferably, the mass ratio of the glufosinate-ammonium, the oxyfluorfen and the haloxyfop-R-methyl is 11-15.
Preferably, the mass of the effective component accounts for 20-25% of the total mass of the herbicide composition.
The herbicide composition prepared by adopting the mass ratio of the glufosinate-ammonium, the oxyfluorfen and the haloxyfop-R-methyl can play a better role in synergy among the effective components, so that the control effect of the herbicide composition can be effectively improved when the content of the effective components in the herbicide composition is relatively low.
By adopting the scheme of the invention, on one hand, the content of the effective components in the herbicide composition is relatively low, and better economic benefit can be brought; on the other hand, according to the environmental protection policy requirements of national reduced application and increased efficiency, the high-efficiency benefit is obtained by using low-dose medicaments, and the future pesticide use development trend is the high-efficiency benefit.
Preferably, the dosage form of the herbicide composition is oil suspending agent, wettable powder, water dispersible granules, microemulsion or suspending agent.
Further preferably, when the formulation of the herbicide composition is the oil suspension, the adjuvant includes an emulsifier, organobentonite, and methyl oleate.
Specifically, the auxiliary agent in the oil suspending agent comprises, by mass, 10% -20% of an emulsifier, 1% -3% of organobentonite and 55% -65% of methyl oleate.
When the dosage form of the herbicide composition is the wettable powder, the auxiliary agent comprises a wetting agent, a dispersing agent, white carbon black and kaolin.
Specifically, the auxiliary agent in the wettable powder comprises 1-3% of wetting agent, 6-10% of dispersing agent, 8-12% of white carbon black and 55-60% of kaolin according to mass percentage.
When the herbicide composition is in the form of water dispersible granules, the auxiliary agent comprises a wetting agent, a dispersing agent, ammonium sulfate and corn starch.
Specifically, the auxiliary agent in the water dispersible granule comprises, by mass, 2% -4% of a wetting agent, 8% -12% of a dispersing agent, 8% -12% of ammonium sulfate and 52% -57% of corn starch.
When the herbicide composition is in the form of the microemulsion, the auxiliary agent comprises an emulsifier, a solvent and water.
Specifically, the auxiliary agent in the microemulsion comprises 15-25% of emulsifier, 20-30% of solvent and 30-35% of water in percentage by mass.
When the herbicide composition is in the form of the suspension concentrate, the adjuvants include wetting agents, dispersants, water, antifoaming agents, preservatives, antifreezes, thickeners.
Specifically, the auxiliary agent in the suspending agent comprises 1-3% of wetting agent, 2-6% of dispersing agent, 0.1-1% of defoaming agent, 0.1-1% of preservative, 3-7% of antifreezing agent, 0.1-1% of thickening agent and 63-67% of water in percentage by mass.
The herbicide composition is prepared into the dosage forms, and all the additives in all the dosage forms can generate a synergistic interaction with the active ingredients, so that the control effect of the herbicide composition is further improved.
Still further preferably, the emulsifier comprises one or more of calcium dodecylbenzene sulfonate, styrene-based polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenyl polyoxyethylene ether, styrene-based phenol formaldehyde resin polyoxyethylene-polyoxypropylene block polyether, tween 80 and fatty alcohol-polyoxyethylene ether.
The solvent comprises one or more of DMF, DMSO, toluene, xylene, benzyl alcohol, ethanol, methanol, ethylene glycol, glycerol, cyclohexanone, solvent oil, chloroform, acetone, tert-butyl alcohol and N, N-dimethyl polyvinylpyrrolidone.
The wetting agent comprises one or more of sodium dodecyl sulfate, fatty alcohol-polyoxyethylene ether, sodium butyl naphthalene sulfonate and condensation product of fatty alcohol and ethylene oxide.
The dispersing agent comprises one or more of naphthalene sulfonic acid formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate and fatty alcohol-polyoxyethylene ether.
The preservative comprises one or more of benzoic acid, sodium benzoate, sorbic acid, propionic acid and cason.
The antifreeze comprises one or more of ethylene glycol, propylene glycol and glycerol.
The defoaming agent comprises one or more of organic silicon defoaming agent and polyether defoaming agent.
The thickening agent comprises one or more of xanthan gum, magnesium aluminum silicate, bentonite, diatomite and guar gum.
The herbicide composition with different formulations is prepared according to the effective components and the auxiliary agents, and comprises the following specific components:
when the herbicide composition is an oil suspending agent, the oil suspending agent comprises the following components in percentage by total mass: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 10 to 20 percent of emulsifier, 1 to 3 percent of organic bentonite and the balance of methyl oleate.
Preferably, the oil suspending agent comprises the following components by weight percent: 11 to 15 percent of glufosinate-ammonium, 5 to 8 percent of oxyfluorfen, 2.5 to 3.5 percent of haloxyfop-R-methyl, 13 to 17 percent of emulsifier, 1.5 to 2.5 percent of organic bentonite and the balance of methyl oleate.
When the herbicide composition is a microemulsion, the microemulsion consists of the following components in percentage by total mass of the microemulsion: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 15 to 25 percent of emulsifier, 20 to 30 percent of solvent and the balance of water.
Preferably, the microemulsion consists of the following components in percentage by total mass of the microemulsion: 11 to 15 percent of glufosinate-ammonium, 5 to 8 percent of oxyfluorfen, 2.5 to 3.5 percent of haloxyfop-R-methyl, 18 to 22 percent of emulsifier, 23 to 27 percent of solvent and the balance of water.
When the dosage form of the herbicide composition is wettable powder, the wettable powder comprises the following components in percentage by total mass: 10 to 16 percent of refined glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 1 to 3 percent of wetting agent, 6 to 10 percent of dispersing agent, 8 to 12 percent of white carbon black and the balance of kaolin.
Preferably, the wettable powder comprises the following components by weight percent: 11 to 15 percent of glufosinate-ammonium, 5 to 8 percent of oxyfluorfen, 2.5 to 3.5 percent of haloxyfop-R-methyl, 1.5 to 2.5 percent of wetting agent, 7 to 9 percent of dispersing agent, 9 to 11 percent of white carbon black and the balance of kaolin.
When the herbicide composition is in the form of water dispersible granules, the water dispersible granules consist of the following components in percentage by total mass: 10 to 16 percent of refined glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 2 to 4 percent of wetting agent, 8 to 12 percent of dispersing agent, 8 to 12 percent of ammonium sulfate and the balance of corn starch.
Preferably, the water dispersible granules comprise the following components by weight percent: 11 to 15 percent of glufosinate-ammonium, 5 to 8 percent of oxyfluorfen, 2.5 to 3.5 percent of haloxyfop-R-methyl, 2.5 to 3.5 percent of wetting agent, 9 to 11 percent of dispersing agent, 9 to 11 percent of ammonium sulfate and the balance of corn starch.
When the herbicide composition is a suspending agent, the suspending agent comprises the following components by weight percent: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 1 to 3 percent of wetting agent, 2 to 6 percent of dispersing agent, 0.1 to 1 percent of defoaming agent, 0.1 to 1 percent of preservative, 3 to 7 percent of antifreezing agent, 0.1 to 1 percent of thickening agent and the balance of water.
Preferably, the suspending agent comprises the following components by weight percent of the total mass of the suspending agent: 12.5 to 15 percent of glufosinate-ammonium, 5 to 6.5 percent of oxyfluorfen, 2.5 to 3 percent of haloxyfop-R-methyl, 1.5 to 2.5 percent of wetting agent, 3 to 5 percent of dispersing agent, 0.3 to 0.7 percent of defoaming agent, 0.3 to 0.7 percent of preservative, 4 to 6 percent of antifreezing agent, 0.3 to 0.7 percent of thickening agent and the balance of water.
In a second aspect, the present invention provides a method of using a herbicidal composition for controlling annual or perennial weeds, including grasses and broadleaf weeds.
Preferably, the herbicide composition is mixed with water, and the stem and leaf spraying is carried out on the weeds. Wherein, the herbicide composition acts on the weeds in the 3-4 leaf stage, and the control effect is better.
Compared with the prior art, the invention has the following advantages:
the herbicide composition is prepared by compounding the effective components of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl, and acts on weeds, so that the weeds with drug resistance can be killed and removed efficiently, and the green turning of the weeds can be inhibited effectively. The effective components have a synergistic effect, so that a good weeding effect can be realized when the content of the effective components is relatively low, the manufacturing cost of the herbicide composition can be reduced, and the influence of the herbicide composition on the environment can be reduced.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to the following examples. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not mentioned are conventional conditions in the industry. The technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
The active ingredients of the herbicide composition provided by the invention are compounded by glufosinate-ammonium, oxyfluorfen and efficient haloxyfop-methyl, and the synergistic effect can be generated among the active ingredients, so that the control effect of the herbicide composition is improved. Wherein:
refined glufosinate-ammonium of formula C 5 H 12 NO 4 P, formula weight 181.27, chemical name 4- [ hydroxy (methyl) phosphono group]-L-homoalanine. The glufosinate-ammonium is easy to dissolve in water and organic solvent, is stable to light, has a melting point of 214-216 ℃, and is a high-efficiency, low-toxicity and non-selective contact-type phosphoric acid herbicide. The refined glufosinate-ammonium is L-type glufosinate-ammonium, which has twice the herbicidal activity of the racemic DL-type glufosinate-ammonium mixture. The glufosinate-ammonium inhibits glutamine synthetase, so that nitrogen metabolism in plants is disturbed, ammonium ions are accumulated and poisoned, chloroplast synthesis is further influenced, photosynthesis is hindered, and finally, the plants die. The refined glufosinate-ammonium has low toxicity and is safe to use. The glufosinate-ammonium is easy to degrade in soil, safe to crops, wide in weeding spectrum, high in activity and quick in weeding, and can prevent and kill more than 100 annual or perennial weeds quickly. The refined glufosinate-ammonium mainly kills weeds by contact, cannot be transferred to other places, and is safe for crops of later crops. The refined glufosinate-ammonium has very good water solubility and a stable structure, and is convenient to process, mix and use.
The oxyfluorfen has the advantages of wide herbicidal spectrum, long persistent period, low dosage, high activity and low toxicity, and can be used in combination with various herbicides, so that the herbicidal spectrum can be expanded, and the pesticide effect of the herbicides can be improved. Moreover, the oxyfluorfen is convenient to use, and can be used for pre-bud treatment and post-bud treatment of weeds.
The haloxyfop-R-methyl can be quickly absorbed by the leaves of gramineous weeds and conducted to the whole plants after being applied, thereby inhibiting the growth of plant meristems and further killing the weeds. The high-efficiency haloxyfop-R has long lasting period and very good preventing and killing effect on annual and perennial grassy weeds from the seedling stage to the tillering and heading stage. In addition, the haloxyfop-R-methyl can still show excellent weeding effect under the conditions of low temperature and drought.
According to the invention, through the compounding of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl, the active ingredients have good synergy and synergism, and can be used for preventing and treating perennial resistant plants, old weeds and the like, the prevention and treatment range is effectively improved, the lasting period is obviously prolonged, and the weed green-turning is inhibited.
In the examples of the present invention, the raw materials used are all commercially available. Wherein, the proportions of the following formulas are mass ratios.
Example 1: the raw material formula of the 15 percent of glufosinate-ammonium, 5 percent of oxyfluorfen and 2.5 percent of high-efficiency haloxyfop-methyl oil suspending agent is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain an oil suspending agent.
Example 2: the raw material formula of the oil suspending agent for preparing 13 percent of glufosinate-ammonium, 6.5 percent of oxyfluorfen and 3 percent of high-efficiency haloxyfop-methyl is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain the oil suspending agent.
Example 3: the raw material formula of the oil suspending agent comprises 11 percent of glufosinate-ammonium, 8 percent of oxyfluorfen and 3.5 percent of high-efficiency haloxyfop-methyl
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain an oil suspending agent.
Example 4:15 percent of glufosinate-ammonium, 5 percent of oxyfluorfen and 2.5 percent of high-efficiency haloxyfop-methyl wettable powder, and the raw material formula is as follows
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 15 |
| Oxyfluorfen | 5 |
| High-efficiency haloxyfop-methyl | 2.5 |
| Sodium dodecyl sulfate | 2 |
| Naphthalenesulfonic acid formaldehyde condensate | 8 |
| White carbon black | 10 |
| Kaolin clay | Make up to 100 |
Putting white carbon black, kaolin, refined glufosinate-ammonium, oxyfluorfen, high-efficiency haloxyfop-methyl, a wetting agent and a dispersing agent into a stirring kettle, uniformly stirring, and carrying out air flow crushing on the materials and mixing to prepare the wettable powder.
Example 5:13 percent of glufosinate-ammonium, 6.5 percent of oxyfluorfen and 3 percent of high-efficiency haloxyfop-methyl wettable powder, and the raw material formula is as follows
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 13 |
| Oxyfluorfen | 6.5 |
| High-efficiency haloxyfop-methyl | 3 |
| Sodium dodecyl sulfate | 2 |
| Naphthalene sulfonic acid formaldehyde condensate | 8 |
| White carbon black | 10 |
| Kaolin clay | Make up to 100 |
Putting white carbon black, kaolin, glufosinate-ammonium, oxyfluorfen, high-efficiency haloxyfop-methyl, a wetting agent and a dispersing agent into a stirring kettle, uniformly stirring, and mixing the materials after airflow crushing to prepare wettable powder.
Example 6:11 percent of glufosinate-ammonium, 8 percent of oxyfluorfen and 3.5 percent of high-efficiency haloxyfop-methyl wettable powder, and the raw material formula is as follows
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 11 |
| Oxyfluorfen | 8 |
| High-efficiency haloxyfop-methyl | 3.5 |
| Sodium dodecyl sulfate | 2 |
| Naphthalene sulfonic acid formaldehyde condensate | 8 |
| White carbon black | 10 |
| Kaolin clay | Make up to 100 |
Putting white carbon black, kaolin, refined glufosinate-ammonium, oxyfluorfen, high-efficiency haloxyfop-methyl, a wetting agent and a dispersing agent into a stirring kettle, uniformly stirring, and carrying out air flow crushing on the materials and mixing to prepare the wettable powder.
Example 7: the raw material formula of the water dispersible granule for preparing 15 percent of glufosinate-ammonium, 5 percent of oxyfluorfen and 2.5 percent of high-efficiency haloxyfop-methyl is as follows
Ammonium sulfate, corn starch, glufosinate-ammonium, oxyfluorfen, efficient haloxyfop-methyl, a wetting agent and a dispersing agent are put into a stirring kettle to be uniformly stirred, the materials are subjected to airflow crushing and then mixed to prepare semi-finished powder, the powder is added into a kneader and added with water in a certain proportion to be kneaded, and the semi-finished powder is extruded and granulated and finally dried to prepare the water dispersible granule.
Example 8: the preparation method comprises the following steps of preparing 13% of glufosinate-ammonium, 6.5% of oxyfluorfen and 3% of efficient haloxyfop-methyl water dispersible granules
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 13 |
| Oxyfluorfen | 6.5 |
| High-efficiency haloxyfop-methyl | 3 |
| Condensation products of fatty alcohols with ethylene oxide | 3 |
| Polycarboxylates | 10 |
| Ammonium sulfate | 10 |
| Corn starch | Make up to 100 |
Ammonium sulfate, corn starch, glufosinate-ammonium, oxyfluorfen, efficient haloxyfop-methyl, a wetting agent and a dispersing agent are put into a stirring kettle to be uniformly stirred, the materials are subjected to airflow crushing and then mixed to prepare semi-finished powder, the powder is added into a kneader and added with water in a certain proportion to be kneaded, and the semi-finished powder is extruded and granulated and finally dried to prepare the water dispersible granule.
Example 9: the raw material formula of the water dispersible granule for preparing 11 percent of glufosinate-ammonium, 8 percent of oxyfluorfen and 3.5 percent of high-efficiency haloxyfop-methyl is as follows
Ammonium sulfate, corn starch, glufosinate-ammonium, oxyfluorfen, efficient haloxyfop-methyl, a wetting agent and a dispersing agent are put into a stirring kettle to be uniformly stirred, the materials are subjected to airflow crushing and then mixed to prepare semi-finished powder, the powder is added into a kneader and added with water in a certain proportion to be kneaded, and the semi-finished powder is extruded and granulated and finally dried to prepare the water dispersible granule.
Example 10: the preparation method of the microemulsion of 15 percent of glufosinate-ammonium, 5 percent of oxyfluorfen and 2.5 percent of high-efficiency haloxyfop-methyl comprises the following raw material formula
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into a solvent, uniformly mixing, adding an emulsifier, uniformly stirring, adding the rest water, and stirring until clear and transparent to prepare the microemulsion.
Example 11: the preparation method of the microemulsion of 13 percent of glufosinate-ammonium, 6.5 percent of oxyfluorfen and 3 percent of high-efficiency haloxyfop-methyl comprises the following raw material formula
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into a solvent, uniformly mixing, adding an emulsifier, uniformly stirring, adding the rest water, and stirring until clear and transparent to prepare the microemulsion.
Example 12: the raw material formula of the microemulsion of 11 percent of glufosinate-ammonium, 8 percent of oxyfluorfen and 3.5 percent of high-efficiency haloxyfop-methyl is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into a solvent, uniformly mixing, adding an emulsifier, uniformly stirring, adding the rest water, and stirring until clear and transparent to prepare the microemulsion.
Example 13: the raw material formula of the suspension is as follows
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 15 |
| Oxyfluorfen | 5 |
| High-efficiency haloxyfop-methyl | 2.5 |
| Butyl naphthalene sulfonic acid sodium salt | 2 |
| Polycarboxylates | 4 |
| Organic silicon defoaming agent | 0.5 |
| Kathon | 0.5 |
| Ethylene glycol | 5 |
| Xanthan gum | 0.5 |
| Water (I) | Make up to 100 |
Adding a wetting agent, a dispersing agent, a defoaming agent, a preservative, an antifreezing agent, a thickening agent, refined glufosinate-ammonium, oxyfluorfen and efficient haloxyfop-methyl into water, stirring uniformly, and sanding by a sand mill to obtain a suspension agent with qualified particle size.
Example 14: the suspending agent of 13 percent of glufosinate-ammonium, 6.5 percent of oxyfluorfen and 3 percent of high-efficiency haloxyfop-methyl is prepared by the following raw material formula
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 13 |
| Oxyfluorfen | 6.5 |
| High-efficiency haloxyfop-methyl | 3 |
| Butyl naphthalene sulfonic acid sodium salt | 2 |
| Polycarboxylates | 4 |
| Organic silicon defoaming agent | 0.5 |
| Kathon | 0.5 |
| Ethylene glycol | 5 |
| Xanthan gum | 0.4 |
| Water (W) | Make up to 100 |
Adding a wetting agent, a dispersing agent, a defoaming agent, a preservative, an antifreezing agent, a thickening agent, refined glufosinate-ammonium, oxyfluorfen and efficient haloxyfop-methyl into water, stirring uniformly, and sanding by a sand mill to obtain a suspension agent with qualified particle size.
Example 15: the suspending agent of 11 percent of glufosinate-ammonium, 8 percent of oxyfluorfen and 3.5 percent of high-efficiency haloxyfop-methyl is prepared by the following raw material formula
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 12.5 |
| Oxyfluorfen | 6.5 |
| High-efficiency haloxyfop-methyl | 3 |
| Butyl naphthalene sulfonic acid sodium salt | 2 |
| Polycarboxylates | 4 |
| Organic silicon defoaming agent | 0.5 |
| Kathon | 0.5 |
| Ethylene glycol | 5 |
| Xanthan gum | 0.45 |
| Water (I) | Make up to 100 |
Adding a wetting agent, a dispersing agent, a defoaming agent, a preservative, an antifreezing agent, a thickening agent, refined glufosinate-ammonium, oxyfluorfen and efficient haloxyfop-methyl into water, stirring uniformly, and sanding by a sand mill to obtain a suspension agent with qualified particle size.
Comparative example 1:22.5% of refined glufosinate-ammonium SL (soluble solution) and the raw material formula is as follows
| Components | Formulation (%) |
| Refined glufosinate-ammonium | 22.5 |
| Fatty alcohol polyoxyethylene ether | 15 |
| Water (I) | Make up to 100 |
Adding the emulsifier refined glufosinate-ammonium into water, stirring, shearing and filtering to obtain the soluble agent.
Comparative example 2:22.5 percent of high-efficiency haloxyfop EC (missible oil) and the raw material formula thereof is as follows
Adding the haloxyfop-R-methyl into a solvent, stirring until the mixture is transparent, adding the auxiliary agent, and stirring uniformly to prepare the emulsifiable concentrate.
Comparative example 3:22.5 percent of oxyfluorfen SL and the raw material formula thereof is as follows
Adding oxyfluorfen into a solvent, stirring into transparent liquid, and filtering to obtain a soluble agent.
Comparative example 4:14.5 percent of refined glufosinate-ammonium and 8 percent of oxyfluorfen SL, and the raw material formula is as follows
Adding oxyfluorfen and glufosinate-ammonium into a solvent, stirring to obtain a transparent liquid, and filtering to obtain a soluble solution.
Comparative example 5:15 percent of glufosinate-ammonium and 7.5 percent of haloxyfop-R-methyl SL, and the raw material formula is as follows
Adding haloxyfop-R-methyl and glufosinate-ammonium into solvent, stirring to obtain transparent liquid, and filtering to obtain soluble liquid.
Comparative example 6:12 percent of oxyfluorfen and 10.5 percent of haloxyfop-R-methyl SL, and the raw material formula is as follows
Adding haloxyfop-methyl and oxyfluorfen into a solvent, stirring to obtain a transparent liquid, and filtering to obtain a soluble solution.
Comparative example 7:5 percent of glufosinate-ammonium, 3 percent of oxyfluorfen and 1 percent of high-efficiency haloxyfop-R OD (oil suspending agent), and the formula of the raw materials is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain the oil suspending agent.
Comparative example 8:8 percent of glufosinate-ammonium, 4 percent of oxyfluorfen and 1.5 percent of high-efficiency haloxyfop-methyl OD, and the raw material formula is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain an oil suspending agent.
Comparative example 9:18 percent of glufosinate-ammonium, 10 percent of oxyfluorfen and 5 percent of high-efficiency haloxyfop-R OD, and the raw material formula is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain the oil suspending agent.
Comparative example 10:18 percent of glufosinate-ammonium, 10 percent of oxyfluorfen and 5 percent of high-efficiency haloxyfop-methyl SC (suspending agent), and the formula of the raw materials is as follows
Adding a wetting agent, a dispersing agent, a defoaming agent, a preservative, an antifreezing agent, a thickening agent, glufosinate-ammonium, oxyfluorfen and efficient haloxyfop-methyl into water, stirring uniformly, and sanding to obtain a suspension agent with qualified particle size by a sand mill.
Comparative example 11:18 percent of glufosinate-ammonium, 10 percent of oxyfluorfen and 5 percent of high-efficiency haloxyfop WP (wettable powder), and the raw material formula is as follows
| Components | Formulation (%) |
| Refined glufosinate-ammonium | 18 |
| Oxyfluorfen | 10 |
| High-efficiency haloxyfop-methyl | 5 |
| Sodium dodecyl sulfate | 2 |
| Naphthalenesulfonic acid formaldehyde condensate | 8 |
| White carbon black | 10 |
| Kaolin clay | Make up to 100 |
Putting white carbon black, kaolin, glufosinate-ammonium, oxyfluorfen, high-efficiency haloxyfop-methyl, a wetting agent and a dispersing agent into a stirring kettle, uniformly stirring, and mixing the materials after airflow crushing to prepare wettable powder.
Comparative example 12:18 percent of glufosinate-ammonium, 10 percent of oxyfluorfen and 5 percent of high-efficiency haloxyfop-methyl WDG (water dispersible granule), and the raw material formula is as follows
| Components | Ratio (%) |
| Refined glufosinate-ammonium | 18 |
| Oxyfluorfen | 10 |
| High-efficiency haloxyfop-methyl | 5 |
| Condensation products of fatty alcohols with ethylene oxide | 3 |
| Polycarboxylates | 10 |
| Ammonium sulfate | 10 |
| Corn starch | Make up to 100 |
Ammonium sulfate, corn starch, glufosinate-ammonium, oxyfluorfen, efficient haloxyfop-methyl, a wetting agent and a dispersing agent are put into a stirring kettle to be uniformly stirred, the materials are subjected to airflow crushing and then mixed to prepare semi-finished powder, the powder is added into a kneader and added with water in a certain proportion to be kneaded, and the semi-finished powder is extruded and granulated and finally dried to prepare the water dispersible granule.
Comparative example 13:18 percent of glufosinate-ammonium, 10 percent of oxyfluorfen and 5 percent of high-efficiency haloxyfop-methyl ME (microemulsion), and the formula of the raw materials is as follows
Adding glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl into a solvent, uniformly mixing, adding an emulsifier, uniformly stirring, adding the rest water, and stirring until clear and transparent to prepare the microemulsion.
Comparative example 14:13 percent of glufosinate-ammonium, 6 percent of flumioxazin and 3.5 percent of haloxyfop-R-methyl OD, and the raw material formula is as follows
Adding glufosinate-ammonium, flumioxazin and haloxyfop-R-methyl into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain the oil suspending agent.
Comparative example 15:13 percent of refined glufosinate-ammonium, 6.5 percent of oxyfluorfen and 3-flumioxazin OD and the formula of the raw materials is as follows
Adding glufosinate-ammonium, oxyfluorfen and flumioxazin into methyl oleate, adding an emulsifier and organic bentonite, and sanding to obtain the oil suspending agent.
The herbicidal compositions in the examples and comparative examples were tested for their effectiveness, as follows:
the test field is located in an uncultivated area near the north Hua Changlu of Zhang hong city, the weeds grow naturally without human factor interference, the field weeds mainly comprise broadleaf weeds, annual and perennial grassy weeds, and the weeds comprise erigeron breviscapus, sticktight, goosegrass, common euphorbia herb and the like.
Comparative tests are carried out on examples 1-15 and comparative examples 1-15, wherein the dosage of the medicament in the invention is 100g/667m 2 Diluted 150 times for use. And (3) uniformly spraying the stem leaves, applying the medicine at 13-00 days in 3 and 22 months in 2022, wherein the weather is clear and no wind is generated during application. Blank control and 3 agent controls were designed together with 5 examples. Treatment area of 9m per cell 2 . After the application, the control effect was investigated 3 times at 3d (25 days at 3 months), 5d (27 days at 3 months) and 15d (6 days at 4 months), 1 test point was selected and fixed for each cell, and the area of the test point was 0.252m 2 And investigating the condition of weeds in each treatment plot, counting weeds with severe yellow and withered roots or killed weeds as killed weeds, recording the types and the number of the survived weeds, and calculating the control effect of each treatment.
Control effect (%) = (pre-drug weed strain-total number of weeds)/number of pre-drug weeds × 100%
The data on the effect of the herbicide compositions in the respective examples and comparative examples are shown in table 1.
TABLE 1
As is evident from the table: the comparative analysis of the data of examples 1 to 15 of the present invention and comparative examples 1 to 15 shows that:
1. the compound of the glufosinate-ammonium, the oxyfluorfen and the haloxyfop-R-methyl can prevent and control annual or perennial dicotyledons, gramineous weeds and field broad-leaved weeds.
2. The refined glufosinate-ammonium has a contact killing effect on weeds, the 3d control effect of the case containing the refined glufosinate-ammonium is better than that of the case without the refined glufosinate-ammonium, and the 3d control effect of the comparative examples 2, 3 and 6 is obviously lower than that of all the examples and other comparative examples containing the refined glufosinate-ammonium.
3. The control effect of 5d in each embodiment is better than that of 5d in each proportion, which shows that the synergistic effect of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl can obviously improve the control effect of the herbicide composition.
4. It can be seen from the examples and comparative examples that the adjuvants in the oil suspending agent (OD), wettable Powder (WP), water Dispersible Granules (WDG), microemulsion (ME), and suspending agent (SC) can generate a synergistic effect with the active ingredients, so that the 15d sustained control efficacy of the herbicide composition of these formulations is improved, wherein the control efficacy is the best when the herbicide composition is a microemulsion.
5. According to the invention, the compound of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl is adopted, under the condition that the contents of effective components are equivalent or the same, compared with the single-component glufosinate-ammonium, oxyfluorfen and haloxyfop-methyl, or the binary compound of glufosinate-ammonium, oxyfluorfen, haloxyfop-methyl and oxyfluorfen, or the compound of other effective components (such as the compound of glufosinate-ammonium, oxyfluorfen and flumioxazin, the compound of glufosinate-ammonium, oxyfluorfen and flumioxazin), the compound of glufosinate-ammonium, oxyfluorfen and haloxyfop-methyl has better control effect and has synergistic effect;
the proportion of the glufosinate-ammonium, the oxyfluorfen and the haloxyfop-R-methyl in the herbicide composition in the embodiment of the invention is better than the control effect of the glufosinate-ammonium, the oxyfluorfen and the haloxyfop-R-methyl in other proportions in the herbicide composition.
6. Although the control effects of the 15d herbicide compositions of comparative examples 9 to 13 were all higher than 90%, the control effects were not improved as compared with the examples of the present invention. In addition, the addition amount of the effective components in the comparative examples 9 to 13 is too much, which does not meet the environmental protection policy requirements of national reduction and application efficiency.
In addition, comparative examples 9 to 13 were the same as the effective ingredients in each example, and the content of the effective ingredients in comparative examples 9 to 13 was higher than that in each example, but the control effects of comparative examples 9 to 13 were slightly lower than those in each example, for the summarized reasons: 1. in comparative examples 9 to 13, the synergistic effect of the proportions of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl is inferior to the proportions of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl in the herbicide composition in the embodiment of the invention; 2. although the comparative examples 9 to 13 have high content of the active ingredients, the performance of the active ingredients on weeds such as wetting, spreading, absorption, loss, volatilization and the like is changed due to the change of the dosage and proportion of other additives, so that the control effect in the comparative examples 9 to 13 is not obviously improved.
The present invention has been described in detail in order to enable those skilled in the art to understand the invention and to practice it, and it is not intended to limit the scope of the invention, and all equivalent changes and modifications made according to the spirit of the present invention should be covered by the present invention.
Claims (10)
1. A herbicide composition is characterized by comprising effective components and an auxiliary agent; the effective components comprise glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl, and the mass ratio of the glufosinate-ammonium, the oxyfluorfen to the haloxyfop-R-methyl is 10-16.
2. A herbicide composition as claimed in claim 1, wherein the mass ratio of glufosinate-ammonium, oxyfluorfen and haloxyfop-R-methyl is 11-15.
3. The herbicide composition as claimed in claim 1, wherein the mass of the active ingredient is 20 to 25% of the total mass of the herbicide composition.
4. The herbicide composition as claimed in claim 1, wherein the herbicide composition is in the form of oil suspension, wettable powder, water dispersible granule, microemulsion or suspension.
5. The herbicide composition as claimed in claim 4, wherein when said herbicide composition is in the form of said oil-suspendable agent, said adjuvant comprises an emulsifier, an organobentonite, methyl oleate;
when the dosage form of the herbicide composition is the wettable powder, the auxiliary agent comprises a wetting agent, a dispersing agent, white carbon black and kaolin;
when the herbicide composition is in the form of water dispersible granules, the auxiliary agent comprises a wetting agent, a dispersing agent, ammonium sulfate and corn starch;
when the dosage form of the herbicide composition is the microemulsion, the auxiliary agent comprises an emulsifier, a solvent and water;
when the herbicide composition is in the form of the suspension concentrate, the adjuvants include wetting agents, dispersants, water, antifoaming agents, preservatives, antifreezes, thickeners.
6. A herbicidal composition according to claim 5, characterized in that the emulsifier comprises one or more of calcium dodecylbenzenesulfonate, styrylpolyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, phenethylphenyl polyoxyethylene ether, styrylphenol formaldehyde resin polyoxyethylene-polyoxypropylene block polyether, tween 80, fatty alcohol polyoxyethylene ether;
and/or the solvent comprises one or more of DMF, DMSO, toluene, xylene, benzyl alcohol, ethanol, methanol, ethylene glycol, glycerol, cyclohexanone, solvent oil, chloroform, acetone, tert-butyl alcohol, N-dimethyl polyvinylpyrrolidone;
and/or the wetting agent comprises one or more of sodium dodecyl sulfate, fatty alcohol-polyoxyethylene ether, sodium butylnaphthalene sulfonate, and a condensation product of fatty alcohol and ethylene oxide;
and/or the dispersing agent comprises one or more of naphthalene sulfonic acid formaldehyde condensate, polycarboxylate, sodium lignosulfonate, calcium lignosulfonate and fatty alcohol-polyoxyethylene ether;
and/or, the preservative comprises one or more of benzoic acid, sodium benzoate, sorbic acid, propionic acid, cason;
and/or the antifreeze comprises one or more of ethylene glycol, propylene glycol and glycerol;
and/or the defoaming agent comprises one or more of a silicone defoaming agent and a polyether defoaming agent;
and/or the thickener comprises one or more of xanthan gum, magnesium aluminum silicate, bentonite, diatomite and guar gum.
7. The glufosinate-ammonium-containing herbicide composition according to claim 4, wherein when the formulation of the glufosinate-ammonium-containing herbicide composition is the oil suspension, the adjuvant in the oil suspension comprises 10-20% by mass of an emulsifier, 1-3% by mass of an organobentonite, and 55-65% by mass of methyl oleate;
and/or when the herbicide composition containing glufosinate-ammonium is the microemulsion, the auxiliary agent in the microemulsion comprises 15-25% of emulsifier, 20-30% of solvent and 30-35% of water in percentage by mass;
and/or when the herbicide composition containing the glufosinate-ammonium is the wettable powder, the auxiliary agent in the wettable powder comprises 1-3% of wetting agent, 6-10% of dispersing agent, 8-12% of white carbon black and 55-60% of kaolin in percentage by mass;
and/or when the herbicide composition containing glufosinate-ammonium is in the form of water dispersible granules, the auxiliary agents in the water dispersible granules comprise 2-4% of wetting agent, 8-12% of dispersing agent, 8-12% of ammonium sulfate and 52-57% of corn starch in percentage by mass;
and/or when the herbicide composition containing glufosinate-ammonium is the suspending agent, the auxiliary agents in the suspending agent comprise 1-3% of wetting agent, 2-6% of dispersing agent, 0.1-1% of defoaming agent, 0.1-1% of preservative, 3-7% of antifreezing agent, 0.1-1% of thickening agent and 63-67% of water in percentage by mass.
8. The herbicide composition as claimed in claim 1, wherein when said herbicide composition is in the form of an oil-suspendable agent, said oil-suspendable agent is composed of, in terms of one hundred percent based on the total mass of said oil-suspendable agent: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-methyl, 10 to 20 percent of emulsifier, 1 to 3 percent of organic bentonite and the balance of methyl oleate;
when the herbicide composition is a microemulsion, the microemulsion consists of the following components in percentage by total mass of the microemulsion: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 15 to 25 percent of emulsifier, 20 to 30 percent of solvent and the balance of water;
when the dosage form of the herbicide composition is wettable powder, the wettable powder comprises the following components in percentage by total mass: 10 to 16 percent of refined glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 1 to 3 percent of wetting agent, 6 to 10 percent of dispersing agent, 8 to 12 percent of white carbon black and the balance of kaolin;
when the herbicide composition is in the form of water dispersible granules, the water dispersible granules consist of the following components in percentage by total mass: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 2 to 4 percent of wetting agent, 8 to 12 percent of dispersing agent, 8 to 12 percent of ammonium sulfate and the balance of corn starch;
when the herbicide composition is a suspending agent, the suspending agent consists of the following components in percentage by total mass: 10 to 16 percent of glufosinate-ammonium, 3 to 10 percent of oxyfluorfen, 2 to 4 percent of haloxyfop-R-methyl, 1 to 3 percent of wetting agent, 2 to 6 percent of dispersing agent, 0.1 to 1 percent of defoaming agent, 0.1 to 1 percent of preservative, 3 to 7 percent of antifreezing agent, 0.1 to 1 percent of thickening agent and the balance of water.
9. A method of using a herbicidal composition, characterized in that the herbicidal composition according to any one of claims 1 to 8 is used for controlling annual or perennial weeds, including grasses and broadleaf weeds.
10. The method of using the herbicide composition as claimed in claim 9, wherein the herbicide composition is mixed with water and sprayed on the foliage of the weeds.
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