CN114557350B - Stable and high-control-efficiency herbicide and application thereof - Google Patents
Stable and high-control-efficiency herbicide and application thereof Download PDFInfo
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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
- A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
- A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
- A01N39/04—Aryloxy-acetic acids; Derivatives thereof
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The application relates to the technical field of herbicides, in particular to a stable and high-control-efficiency herbicide and application thereof. The raw materials of the herbicide comprise active components, wherein the active components comprise sodium 2-methyl-4-chloride and oxadiazon. The herbicide provided by the application has the following advantages: (1) The herbicide can prevent and remove weeds efficiently, and has important significance for improving the yield of grains in unit area and reducing economic loss caused by grass damage. (2) The herbicide has the advantages of easily available raw materials, simple and convenient process and strong practicability, and can be widely applied to the technical field of weeding. (3) The herbicide is especially suitable for preventing and killing annual weeds, has high safety and has no phytotoxicity to crops. (4) The herbicide has strong stability, and the decomposition rate of active components stored for a long time under high temperature condition is lower than 1%.
Description
Technical Field
The application relates to the technical field of herbicides, in particular to a stable and high-control-efficiency herbicide and application thereof.
Background
The population growth and grain supply balance are important challenges facing human beings in the 21 st century, the cultivated land area is continuously reduced due to environmental deterioration, insect damage, grass damage and other factors while the population is continuously growing, and the use of pesticides to promote the grain yield per unit area is an effective way for promoting the agricultural development in new environments. The herbicide is a chemical agent capable of thoroughly or selectively killing weeds, and plays an important role in controlling farmland weeds and killing non-agro-cultivated weeds or shrubs. According to different modes of action, herbicides can be classified into selective herbicides and biocidal herbicides, wherein the biocidal herbicides are toxic to all plants and are mainly used before sowing, and the use conditions are harsh; the selective herbicide can eliminate weeds without damaging seedlings and has wider application range. The proportion of the herbicide in the three pesticides (bactericides, pesticides and herbicides) in China is far lower than the world leading level, the domestic herbicide has very strong dependence on foreign varieties, and the technology development and production application of the herbicide have very important stand value for meeting the sustainable development requirement of modern agriculture in China. Chinese patent CN2015188397. X discloses a composition containing 2-methyl-4-sodium chloride and cyclohexenone herbicide, wherein the 2-methyl-4-sodium chloride and the cyclohexenone are adopted as active ingredients to exert the weeding effect, and the method reduces the negative influence of pesticides on the environment by controlling the mass ratio of the 2-methyl-4-sodium chloride to the cyclohexenone to achieve the effects of less herbicide consumption and less residue. The method is environment-friendly, but the herbicide has poor stability, and active ingredients are easy to escape and decompose and cannot be stored at a higher temperature for a long time. Based on the above, a herbicide with high stability and high safety and capable of effectively preventing and killing weeds is explored and is a problem to be solved in the field.
Disclosure of Invention
The herbicide provided by the application solves the problems of low herbicide weeding efficiency, poor storage stability and safety in the prior art, and realizes the herbicide with high stability, strong safety and high weed control efficiency.
The first aspect of the application provides a stable and high-control herbicide, which comprises active components including 2-methyl-4-chloro sodium and oxadiazon.
In a preferred embodiment, the active ingredient comprises 20-30% by weight of the total herbicide.
In a preferred embodiment, the weight ratio of the sodium 2-methyl-4-chloride to the oxadiazon is (3-30): (9-21).
In a preferred embodiment, the weight ratio of the sodium 2-methyl-4-chloride to the oxadiazon is (6-21): (12-20).
In a preferred embodiment, the raw materials of the herbicide further comprise 3-7% of an emulsifying agent, 3-10% of a small molecule polyol, 0.05-1% of microbial polysaccharide, 0.2-1% of an antifoaming agent and the balance of a solvent in percentage by weight.
In a preferred embodiment, the emulsifier comprises at least one of a polymeric polycarboxylate, alkylphenol ethoxylates, alkylbenzene sulfonates, fatty alcohol ethoxylates, polyol fatty acid esters, and phosphates.
In a preferred embodiment, the microbial polysaccharide comprises at least one of xanthan gum, gellan gum, pullulan, and thermogel.
In a preferred embodiment, the defoamer comprises a silicone compound.
In a preferred embodiment, the weight ratio of the active ingredient, emulsifier and small molecule polyol is (3.4-6): 1: (0.8-1.5).
In a second aspect, the present application provides the use of a stable, highly effective herbicide for the control of annual weeds.
The beneficial effects are that:
the herbicide provided by the application has the following advantages:
(1) The herbicide can prevent and remove weeds efficiently, and has important significance for improving the yield of grains in unit area and reducing economic loss caused by grass damage.
(2) The herbicide has the advantages of easily available raw materials, simple and convenient process and strong practicability, and can be widely applied to the technical field of weeding.
(3) The herbicide is especially suitable for preventing and killing annual weeds, has high safety and no phytotoxicity to crops.
(4) The herbicide has strong stability, and the decomposition rate of active components is lower than 1% under the condition of high-temperature long-term storage.
Description of the drawings:
FIG. 1.2 toxicity measurement results of sodium methyl 4 chloride, oxadiazon and mixed combination thereof on herba Andrographitis;
FIG. 2.2 toxicity measurement results of sodium methyl 4 chloride, oxadiazon and mixed combination thereof on snakehead intestines;
FIG. 3.2 toxicity measurement results of methyl 4 sodium chloride, oxadiazon and its compounding combination on barnyard grass;
FIG. 4.2 toxicity measurement results of methyl 4 sodium chloride, oxadiazon and its compounding combination on rhizoma et radix Valerianae;
fig. 5.2 raw data of toxicity measurement results of sodium methyl 4 chloride, oxadiazon and mixed combination thereof on herba Andrographitis;
FIG. 6.2 raw data of toxicity measurements of sodium methyl 4 chloride, oxadiazon, and compounded combinations thereof on snakehead intestines;
fig. 7.2 raw data of toxicity measurement results of sodium methyl 4 chloride, oxadiazon and mixed combination thereof on barnyard grass;
fig. 8.2 raw data of toxicity measurements of sodium methyl 4 chloride, oxadiazon and compounded combinations thereof on garrulous cyperus.
Detailed Description
The contents of the present application can be more easily understood by referring to the following detailed description of preferred embodiments of the present application and examples included. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification, definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified element, step or component. If used in a claim, such phrase will cause the claim to be closed, such that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the claim body, rather than immediately following the subject, it is limited to only the elements described in that clause; other elements are not excluded from the stated claims as a whole.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
The singular forms include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or event may or may not occur, and that the description includes both cases where the event occurs and cases where the event does not.
Approximating language, in the specification and claims, may be applied to modify an amount that would not limit the application to the specific amount, but would include an acceptable portion that would be close to the amount without resulting in a change in the basic function involved. Accordingly, the modification of a numerical value with "about", "about" or the like means that the present application is not limited to the precise numerical value. In some examples, the approximating language may correspond to the precision of an instrument for measuring the value. In the description and claims of the application, the range limitations may be combined and/or interchanged, if not otherwise specified, including all the sub-ranges subsumed therein.
Furthermore, the indefinite articles "a" and "an" preceding an element or component of the application are not limited to the requirements of the number of elements or components (i.e. the number of occurrences). Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component also includes the plural reference unless the amount is obvious to the singular reference.
"Polymer" means a polymeric compound prepared by polymerizing monomers of the same or different types. The generic term "polymer" encompasses the terms "homopolymer", "copolymer", "terpolymer" and "interpolymer". "interpolymer" means a polymer prepared by the polymerization of at least two different monomers. The generic term "interpolymer" includes the term "copolymer" (which is typically employed to refer to polymers prepared from two different monomers) and the term "terpolymer" (which is typically employed to refer to polymers prepared from three different monomers). It also includes polymers made by polymerizing more monomers. "blend" means a polymer formed by the co-mixing of two or more polymers by physical or chemical means.
In order to solve the problems, the first aspect of the application provides a stable and high-control herbicide, which comprises active components including sodium 2-methyl-4-chloride and oxadiazon.
In some preferred embodiments, the active component comprises 20-30% by weight of the total herbicide.
In some preferred embodiments, the weight ratio of the sodium 2-methyl-4-chloride to the oxadiazon is (3-30): (9-21).
Further preferably, the weight ratio of the 2-methyl-4-chloro sodium to the oxadiazon is (6-21): (12-20).
Still more preferably, the weight ratio of the 2-methyl-4-chloro sodium to the oxadiazon is 7:18.
as the world population grows, the demand for food is increasing day by day, and increasing the yield per unit area of crops is a prominent problem facing humans. The farmland grass damage is a main cause of crop yield reduction, the global agricultural loss caused by grass damage reaches over 900 hundred million dollars each year, under the background, the herbicide becomes the most rapid development type in the agricultural chemicals nowadays, and the reasonable use of the herbicide can effectively promote the agricultural development. The application discovers that the active components of the herbicide are compounded by 2-methyl-4-chloro sodium and oxadiazon, so that weeds can be effectively eliminated; the two active components are suspected to act together, and the two active components can be quickly diffused to the soil surface layer when applied to the crop water layer to form a closed medicinal film, so that the germination of targeted weeds can be effectively inhibited, the active components can enter the weed plant body from the root, the stem and the leaf, the normal physiological activities and hormone balance of the plant body are interfered, and the effective prevention and removal of the weeds are achieved. The application surprisingly discovers that the weight ratio of 2-methyl-4-chloro sodium to oxadiazon in the active component is (6-21): and (12-20), the herbicide has synergistic effect on annual weeds such as glossodes anatipestifer, snakehead intestines and barnyard grass, and the plant control effect on various weeds reaches more than 90% after the herbicide is applied.
In some preferred embodiments, the herbicide raw materials further comprise, by weight, 3-7% of an emulsifier, 3-10% of a small molecule polyol, 0.05-1% of a microbial polysaccharide, 0.2-1% of a defoaming agent, and the balance of a solvent.
In some preferred embodiments, the emulsifier comprises at least one of a polymeric polycarboxylate, alkylphenol ethoxylates, alkylbenzene sulfonates, fatty alcohol ethoxylates, polyol fatty acid esters, phosphates.
Further preferably, the emulsifier is a polymeric polycarboxylate.
The addition of the 2-methyl-4-chlorosodium and the oxadiazon in the herbicide effectively improves the control effect of the product, but the stability of the herbicide is greatly influenced by external factors, and particularly when the temperature is high, the decomposition rate of active ingredients in the herbicide is high, so that the actual control effect of the herbicide is limited. The application adds components such as emulsifying agent, defoaming agent and the like into the herbicide, so that the active components can be kept in a uniformly dispersed state in the solvent so as to facilitate the spraying application, thereby improving the preventing and removing effect of the herbicide and improving the stability of the herbicide to a certain extent. Traditional organic micromolecular dispersing agents stabilize active ingredients in a system mainly through electrostatic repulsion and steric hindrance, but the smaller relative molecular mass makes the dispersing effect of the organic micromolecular dispersing agents on the active ingredients not firm enough, and the organic micromolecular dispersing agents are unstable in storage after being applied to herbicides. The application surprisingly discovers that the high molecular polycarboxylate has stronger affinity with the active components in the system, the active components with stable double-electric-layer structure are easy to form in suspension in the presence of microbial polysaccharide and micromolecular polyalcohol, meanwhile, the solvation chain segment of the high molecular polycarboxylate is moderate, the moderate steric hindrance effect is exerted in the system, the aggregation of molecules such as 2-methyl-4-sodium chloride, oxadiazon and the like is effectively prevented, and the decomposition rate of the active components is obviously reduced after the herbicide is stored for a long time at high temperature.
In some preferred embodiments, the microbial polysaccharide comprises at least one of xanthan gum, gellan gum, pullulan, and thermogel.
In some preferred embodiments, the defoamer comprises a silicone compound.
In some preferred embodiments, the weight ratio of the active ingredient, emulsifier and small molecule polyol is (3.4-6): 1: (0.8-1.5).
The application, through adjusting the kinds, the addition amount and the like of the raw materials such as the active component, the emulsifier, the micromolecular polyol and the like repeatedly and continuously, unexpectedly discovers that when the weight ratio of the active component, the emulsifier and the micromolecular polyol is (3.4-6): 1: (0.8-1.5), the herbicide can have high stability and high control performance, and is suspected that active components in the herbicide, emulsifying agents, micromolecular polyalcohol, microbial polysaccharide and the like can be fully compatible under the condition, the herbicide keeps moderate fluidity, the normal metabolic process of weeds is effectively interfered after the herbicide is applied to farmlands, enzyme synthesis in weed plants is hindered, the growth and development of the weeds and the metabolic process variation are caused, the growth is stopped, the plant control effect of the herbicide on annual weeds such as barnyard grass, arrowhead, long-period rain flowers and the like can reach more than 98 percent after the herbicide is applied for 40 days, and the total fresh weight control performance can reach more than 99.9 percent; meanwhile, the stable suspending agent state obviously inhibits the precipitation of the 2-methyl-4-sodium chloride and the oxadiazon, the decomposition rate of the effective components of the herbicide is lower than 1% after the herbicide is stored for 2 weeks at 54 ℃, and the stability of the herbicide is obviously improved.
In some preferred embodiments, the small molecule polyols include, but are not limited to, ethylene glycol, propylene glycol, 1, 2-butanediol, 1, 4-butanediol, 1, 6-hexanediol.
In some preferred embodiments, the herbicide is applied at a dosage of 70-130 mL/mu.
In general, the improvement of the herbicide control effect is accompanied by the generation of phytotoxicity to the growth of plants in rice areas, and further has adverse effects on crops such as rice, such as fading, deformity, dwarfing and the like, and the herbicide is easy to become a rice remover when a little is careless. According to the application, a large number of experimental debugging shows that when the application dosage is controlled to be 70-130 mL/mu under the conditions, annual weeds such as the glossodes canadensis, the snakehead intestines and the barnyard grass can be prevented and removed efficiently, meanwhile, the negative effects on rice in a treatment area are weakened, the rice grows normally after application, and the symptoms such as dwarfing, malformation and tillering reduction are avoided, so that the compatibility of herbicide and a thicker waxy layer on the surface of crop leaves such as rice, wheat is suspected to be reduced under the conditions, and the affinity to weeds such as the glossodes canadensis and the barnyard grass is stronger, so that crop injury is restrained, and meanwhile, the herbicide plant can be effectively acted on the weeds; the herbicide has high weed control effect and high stability and simultaneously maintains reliable safety effect on crops through the control of the herbicide components and the application amount.
In some preferred embodiments, the preparation steps of the herbicide comprise adding the active components and the solvent into a reaction vessel according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering, and discharging to obtain the finished product.
In a second aspect, the present application provides the use of a stable, highly effective herbicide for the control of annual weeds. Examples of annual weeds include glossodes canadensis, eclipta alba, barnyard grass, arrowhead, longhead, and the like.
Examples
In order to better understand the above technical solution, the following describes the above technical solution in detail with reference to specific embodiments. It is noted herein that the following examples are given solely for the purpose of further illustration and are not to be construed as limitations on the scope of the application, as will be apparent to those skilled in the art in light of the foregoing disclosure. In addition, the raw materials used are commercially available, and the extraction methods of the extracts are conventional extraction methods, unless otherwise specified.
Example 1.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
The herbicide is applied at a dosage of 70 mL/mu.
Example 2.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
The application dosage of the herbicide is 100 mL/mu.
Example 3.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
The herbicide is applied at a dosage of 130 mL/mu.
Example 4.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
The herbicide is applied at a dosage of 200 mL/mu.
Control group:
an herbicide, specifically 55% propisochlor EC, purchased from halbine farmer chemical technology limited; the application dosage of the herbicide is 65 mL/mu.
Example 5.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 7 weight percent of emulsifier, 8 weight percent of micromolecular polyol, 0.3 weight percent of microbial polysaccharide, 0.8 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 6.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 4 weight percent of emulsifier, 4 weight percent of micromolecular polyol, 0.1 weight percent of microbial polysaccharide, 0.3 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 7.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises, by weight, 35% of an active component, 5% of an emulsifier, 6% of a small molecule polyol, 0.15% of microbial polysaccharide, 0.4% of a defoaming agent and the balance of a solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 9.8:25.2.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 8.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is sodium dodecyl benzene sulfonate; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 9.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 10 weight percent of emulsifier, 6 weight percent of small molecule polyol, 0.15 weight percent of polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 10.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of small molecule polyol, 0.15 weight percent of polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecule polyol is glycol with CAS number of 107-21-1.
The polysaccharide is carrageenan, and is purchased from Hebei Runfu Biotechnology Co.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Example 11.
The embodiment provides a stable and high-control-efficiency herbicide, which comprises 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent.
The active components are 2-methyl-4-sodium chloride (CAS number is 3653-48-3) and oxadiazon (CAS number is 19666-30-9), and the weight ratio of the 2-methyl-4-sodium chloride to the oxadiazon is 7:18.
the small molecular polyol is methyl glycol, and the CAS number is 57-55-6.
The microbial polysaccharide is xanthan gum, and is purchased from Shandong Han Linjun International trade company Limited.
The emulsifier is high molecular polycarboxylate, and is purchased from Jiangsu qingyu chemical industry Co., ltd, and the model is SP-SC3266; the defoamer is a polysiloxane compound and is purchased from Jiangsu four new technology application research institute, inc., model G-20A.
The solvent is deionized water.
The preparation method of the herbicide comprises the steps of adding the active components and the solvent into a reaction container according to the formula amount, stirring and dissolving, then adding the emulsifier, the micromolecular polyol, the microbial polysaccharide and the defoamer, continuously stirring uniformly, filtering and discharging to obtain the finished product.
Performance test method
1. Indoor toxicity measurement:
(1) Preparing a medicament:
2 methyl 4 sodium chloride solution: accurately weighing 0.0330g of 92% 2-methyl-4-sodium chloride crude drug, dissolving with 0.2mLDMF, adding 80mL of clear water containing 0.1% Tween 80, uniformly stirring to obtain 600g of 2-methyl-4-sodium chloride solution with a.i./ha, and diluting with water to 300, 210, 140, 70 and 30g of a.i./ha gradient concentration.
Oxadiazon solution: accurately weighing 0.03200 g of 95% oxadiazon raw medicine, dissolving with 0.2mLDMF, adding 80mL of clear water containing 0.1% Tween 80, uniformly stirring, preparing 600g of a.i./ha oxadiazon solution, and diluting with water to obtain gradient concentration of 210, 180, 150, 120 and 90g of a.i./ha.
Blank control solution: 0.2mLDMF with 80mL of water containing 0.1% Tween 80.
The 92% of the 2-methyl-4-chloro sodium technical and the 95% of the oxadiazon technical are provided by Harbin farmer chemical technology Co.
(2) Toxicity test:
irrigation (NY/T1155.5-2006): the method comprises the steps of filling quantitative soil into a porcelain bowl with the height of 6cm and the diameter of 9cm, irrigating from the top of the porcelain bowl to enable the soil to be in a wet state, sowing 15-20 pre-treated target weed seeds to be tested into the porcelain bowl, covering fine soil with the thickness of 0.5-1 cm, culturing in a greenhouse for 24 hours, then carrying out medicament irrigation treatment, wherein each bowl is provided with 1mL of medicament irrigation solution, each treatment is repeated for 4 times, and the treatment without medicament is set as a control. Culturing the treated test material in a greenhouse, periodically observing the emergence and growth conditions of target weeds, visually observing target victimization symptoms and growth inhibition conditions after 21d, weighing fresh weight of overground parts, and evaluating the virulence of the medicament on the target weeds according to the target fresh weight inhibition rate.
Fresh weight inhibition ratio P (%) = (control fresh weight-treated fresh weight)/control fresh weight x 100%
(3) And (3) data processing:
the combined action mode of herbicide is evaluated according to the Gowing method (NY/T1155.7-2006), and the specific formula is as follows:
E 0 =X+Y-XY/100
x is fresh weight inhibition rate of 2-methyl-4-chloro sodium to target weeds when the single dose is used; y is the fresh weight inhibition rate of oxadiazon on target weeds when a certain dosage is used singly; e (E) 0 The pesticide is 2 methyl 4 sodium chloride, and the theoretical value of the fresh weight inhibition rate of the target weed, namely the theoretical prevention effect, is obtained when two medicaments are mixed; e is an actual measurement value of the fresh weight inhibition rate of target weeds when the 2-methyl-4-sodium chloride and the oxadiazon are mixed, namely the actual prevention effect.
Evaluation criteria: when E-E 0 >The synergistic effect is shown at 10 percent, and the E-E is less than or equal to-10 percent 0 At 10% or less, expressed as additive effect, when E-E 0 <-10% expressed as antagonism.
All experimental data were analyzed using DPS v7.05 statistical software.
The original data and the prevention effect result of the toxicity test are shown in the attached drawings of the specification.
(4) Experimental results:
indoor toxicity test results (see the attached drawing of the specification) show that the 2-methyl-4-sodium chloride and oxadiazon have additive effects on weeding effects of the glossoside, the snakehead intestines, the barnyard grass and the crushed rice sedge in 25 tested mixed combinations, the combined weeding effect intensity of the combined weeding effect is different according to the proportion and the weed types, and the growth inhibition effect of the glossoside, the snakehead intestines, the barnyard grass and the crushed rice sedge is the best in the mixed combination of 70+180. The method comprises the following steps:
for the glossoside, the 2-methyl-4-chloro sodium and oxadiazon are mixed with 70+180E-E 0 A value of 6.05%;
E-E of mixture of 2-methyl-4-chloro sodium and oxadiazon with 70+180 for snakehead intestines 0 A value of 6.81%;
for barnyard grass, the 2-methyl-4-chloro sodium and oxadiazon are mixed in the ratio of 70+180Compounded E-E 0 A value of 5.89%;
E-E of 70+180 mixture of 2-methyl-4-chloro sodium and oxadiazon for crushed Misha 0 The value is 7.71%.2. Field efficacy test:
the herbicide obtained in examples 1 to 4 and the control group was verified for weed control effect on transplanted paddy fields. The novel smooth village paddy field is experimentally arranged in a sub-ditch street of an urban area, is flat in experimental land and consistent in cultivation condition, is in a single-row single-tank mode, has the organic matter content of 2.8mg/g and has the pH value of 6.8. The dosage for administration in accordance with the embodiments is uniformly administered by the spray method. The application time is 7 days before transplanting the rice for 5 months and 20 days, when the rice field is leveled and raked to be muddy water or clear water, the herbicide of the example 1-4 and the herbicide of the control group are diluted to be 3 liters per mu by adding water and uniformly mixed, and then the herbicide is uniformly applied to a water layer of 5-7cm, the water layer of 3-5cm is preserved after transplanting, and the water is kept for 10 days, so that the rice Miao Xinshe is prevented from being submerged. 5 months and 27 days, the rice seedling has the specification of 30 multiplied by 12cm, 3.5 to 4 leaves of the rice are transplanted, and the plant height of the rice is 15 to 16cm. And setting a blank control (without adding herbicide) to perform transplanting cultivation on the transplanted paddy field.
The residual weed plant numbers are investigated respectively 20 days and 40 days after the application, and the plant prevention effect is calculated; and investigating fresh weight of weed land, and calculating fresh weight control effect.
Plant control effect X% = (number of weed plants in blank control area-number of residual living weed plants in treatment area)/number of weed plants in pre-drug treatment area X100%.
Fresh weight control Y% = (fresh weight of live weed in control area-fresh weight of live weed in treatment area)/fresh weight of live weed in control area x 100%.
The herbicide control effects of the transplanted paddy field barnyard grass, arrowhead and longflowers were calculated according to the above formula for examples 1 to 4 and the control group (see tables 1 to 4). The latin name of barnyard grass is Echinochloacsgalli (L.) Beauv, the latin name of Cremastra indicum is Sagittaria trifolia L., and the latin name of Leptoradix Itali is Monochoriakorgakuw ii. Wherein treatment number 1 corresponds to the herbicide of example 1, treatment number 2 corresponds to the herbicide of example 2, treatment number 3 corresponds to the herbicide of example 3, treatment number 4 corresponds to the herbicide of example 4, and treatment number 5 corresponds to the herbicide of the control group.
Safety: and (5) observing whether the rice in each treatment area has phytotoxicity or not on the 10 th day (7 th day of 6 months) after the rice transplanting.
The temperature of the medicine is 10-19 ℃ and the relative humidity is 27-75% in the day of application, and the medicine is breeze and cloudy.
3. Decomposition rate of active component:
the herbicides obtained in examples 1 to 11 were stored at 54±2 ℃ for 14 days, and the content of the active ingredient before and after storage was analyzed by a liquid chromatograph, and the decomposition rate = (content before storage-content after storage)/content before storage×100%.
Performance test data
TABLE 1 field efficacy test plant control Effect (%) -20 days after application
TABLE 2 field efficacy test plant control Effect (%) -40 days after application
Table 3 field efficacy experiment fresh weight control Effect (%) -20 days after administration
Table 4 field efficacy experiment fresh weight control Effect (%) -40 days after administration
TABLE 5 safety results of field efficacy
Safety of | |
Example 1 | The rice does not have the phytotoxicity symptoms of fading, malformation, dwarfing and the like |
Example 2 | The rice does not have the phytotoxicity symptoms of fading, malformation, dwarfing and the like |
Example 3 | The rice does not have the phytotoxicity symptoms of fading, malformation, dwarfing and the like |
Example 4 | The rice is slightly dwarfed and reduced in tillering |
TABLE 6 stability test results for the herbicides of examples 1-11
And (3) analyzing a drug effect test result:
checking the plant control effect 20 days after the application: the plant control effect of the 25% dimethyl sodium oxadiazon suspending agent per mu is 93.9% -100% for barnyard grass treated by 70mL, 100mL, 130mL and 200mL, 91.7% -100% for Indian arrowhead, and 88.9% -100% for longhairy antenoron. The total plant control effect on the weeds is 93.1-100.0%. Compared with the total control effect of 55% of the control medicament, namely 100%, the control effect of 130mL and 200mL of the test medicament, namely 25% of the dimethyl sodium oxadiazon suspending agent is consistent with the control effect of the control medicament, and the control effect of 70mL and 100mL of the test medicament is slightly lower than the control effect of a control medicament treatment area.
Plant control investigation 40 days after application: the 25% dimethyl sodium oxadiazon suspending agent is treated with 70mL, 100mL, 130mL and 200mL to have a plant control effect on barnyard grass of 70.9-100.0%, a plant control effect on Indian arrowhead of 86.7-100.0% and a plant control effect on longhead of 88.1-100.0%. The total plant control effect on the weeds is 74.3-100.0%. The total control effect of the control medicament 55% of the propisochlor-oxadiazon EC is 100%, compared with the total control effect of the control medicament 55% of the propisochlor-oxadiazon EC, the control effect of the test medicament 25% of the dimethyl sodium-oxadiazon suspending agent per mu is 100mL, 130mL and 200mL identical or close to the control medicament control effect, and the control effect of the per mu 70mL is slightly lower than the control medicament treatment area control effect.
Fresh weight adjustment 40 days after administration: the fresh weight control trend is consistent with the plant control trend, the fresh weight control effect of the 25% dimethyl sodium oxadiazon suspending agent per mu treated by 70mL, 100mL, 130mL and 200mL is 98.7% -100.0%, the plant control effect of the wild arrowhead is 97.9% -100.0%, and the plant control effect of the long-rain flower is 94.7% -100.0%. The total plant control effect on the weeds is 98.2-100.0%. The total control effect of the control medicament 55% of the propisochlor-oxadiazon EC is 100%.
It can be seen that the test agent 25% dimethyl sodium oxadiazon suspending agent has low control effect on the growth of the new barnyard grass in the late 70mL dosage per mu, and the control effect on barnyard grass is lower than that of the barnyard grass treated with 100mL, 130mL and 200mL per mu. The 25% dimethyl sodium oxadiazon suspending agent has good control effect on annual gramineae and broadleaf weeds by 100mL, 130mL and 200mL treatment, and is equivalent to the control effect of 55% propyl oxadiazon EC serving as a control agent.
Difference significance analysis results: the difference between the treatment of the test medicament 25% dimethyl sodium oxadiazon suspending agent mu with 100mL, 130mL and 200mL is not obvious 20 days after the medicament application, and the total plant prevention effect and the total fresh weight prevention effect of the test medicament 25% dimethyl sodium oxadiazon suspending agent mu with 70mL are obvious under the condition of 5% obvious level and extremely obvious under the condition of 1% obvious level. The prevention effect of the test agent 25% dimethyl sodium oxadiazon suspending agent is not obviously different from that of the control agent 55% propisochlor oxadiazon EC when the test agent 25% dimethyl sodium oxadiazon suspending agent is treated by 100mL, 130mL or 200mL, and the prevention effect of the test agent 25% dimethyl sodium oxadiazon suspending agent is obviously different from that of the control agent when the test agent 25% dimethyl sodium oxadiazon suspending agent is treated by 70 mL.
The test agent 25% dimethyl sodium oxadiazon suspending agent can effectively prevent and remove weeds such as Tian Baicao, tulip, long-rain flowers and the like in the rice transplanting, the dosage is preferably 100-130 mL/mu, the total plant prevention effect is 98.8% -100% after 40 days after application, the total fresh weight prevention effect is 99.9% -100%, the prevention and removal effect is relatively ideal, and further expansion of demonstration application is recommended.
Finally, it is pointed out that the foregoing examples are illustrative only and serve to explain some of the features of the method according to the application. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the application. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (1)
1. The herbicide with high stability and high control efficiency is characterized by comprising 25 weight percent of active component, 5 weight percent of emulsifier, 6 weight percent of micromolecular polyol, 0.15 weight percent of microbial polysaccharide, 0.4 weight percent of defoamer and the balance of solvent;
the active components are 2 methyl 4 sodium chloride and oxadiazon, and the weight ratio of the 2 methyl 4 sodium chloride to the oxadiazon is 7:18;
the small molecule polyol is glycol;
the microbial polysaccharide is xanthan gum;
the emulsifier is high molecular polycarboxylate, and the model is SP-SC3266; the defoaming agent is a polysiloxane compound, and the model is G-20A;
the solvent is deionized water;
the preparation method of the herbicide comprises the steps of adding active components and a solvent into a reaction container according to the formula amount, stirring and dissolving, then adding an emulsifier, micromolecular polyol, microbial polysaccharide and a defoaming agent, continuously stirring uniformly, filtering, and discharging to obtain a finished product;
the application dosage of the herbicide is 70-130 mL/mu.
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