A high-efficiency herbicidal microemulsion and its preparation method

Abstract

The present invention relates to the field of A0N33, and in particular to a microemulsion for efficient weed control and a preparation method thereof. The raw materials of the microemulsion include at least 10-30wt% of an active ingredient; the active ingredient includes an active ingredient A and an active ingredient B; the active ingredient A is glufosinate-ammonium; the active ingredient B is oxyfluorfen. The microemulsion provided by the present invention has the following advantages: using oxyfluorfen and glufosinate-ammonium in a weight ratio of 2.8:14.2 or 3:18 as active ingredients, it is possible to achieve a low-dose, high-efficiency weed control effect, greatly saving the weed control cost, improving the weed control efficiency, and having a positive significance for promoting the development of herbicide technology.

Description

Technical Field

[0001] The present invention relates to the field of A0N33, and in particular to a highly effective herbicidal microemulsion and a preparation method thereof. Background Art

[0002] According to different weed control methods, weed control methods are mainly divided into physical weed control, chemical weed control, biological weed control and integrated control. Among them, chemical weed control is widely used in modern agricultural production operations because of its high efficiency, time controllable, saving manpower and material resources, and high economic effect. However, traditional chemical herbicides are used in huge quantities and are highly toxic, which is not conducive to the sustainable development of the ecological environment. For example, the photosynthetic inhibitor herbicide paraquat, although it has a good weed control effect, the toxicity problems it causes have restricted its use by national regulatory authorities; for example, sulfonylurea and sulfonamide herbicides were once favored for their broad-spectrum weed control and high activity, but with long-term use, the weed resistance problem it brings is becoming increasingly serious.

[0003] Chinese patent CN201810826066.4 discloses a glufosinate-ammonium, quizalofop-p-butyl, and oxyfluorfen-butyl herbicide composition, which achieves the technical effect of high herbicidal activity and low weed resistance through the joint action of glufosinate-ammonium, quizalofop-p-butyl, oxyfluorfen-butyl and polycarboxylates, sodium lauryl sulfate, kaolin, etc.; however, the herbicide has many components, poor compatibility of the formulation system, and the herbicide has the defect of poor stability. Chinese patent CN201810250928.3 discloses a special surfactant for glufosinate-ammonium and oxyfluorfen-butyl, which solves the problem of poor stability of the herbicide, but the prior art uses methyl oleate as a solvent, and oxyfluorfen-butyl has poor solubility in methyl oleate, poor stability of the microemulsion, and difficulty in fully exerting the efficacy.

[0004] With the development of agricultural technology, the requirements for herbicides to develop in the direction of low dosage, low residue, low resistance and high safety are getting higher and higher. Based on this, exploring a broad-spectrum, high-efficiency and long-lasting herbicide has become an urgent problem to be solved in this field. Summary of the invention

[0005] The present invention solves the technical problems of poor stability of herbicide compositions in high-salt environments, high-dose, high-residue, high-resistance and low-safety of herbicides in the prior art by providing a microemulsion for high-efficiency weed control, thereby realizing a herbicide with broad-spectrum, high-efficiency and long-lasting effect.

[0006] The main reason for the above problems in the prior art is that the characteristics of glufosinate-ammonium and oxyfluorfen are determined as follows:

[0007] Glufosinate:

[0008] ISO common name: glufosinate-ammonium

[0009] CA Registration Number: 77182-82-2,53369-07-6

[0010] Chemical name: (RS)-2-amino-4-(hydroxymethyloxy)butyric acid ammonium

[0011] Structural formula:

[0012] Molecular formula: C5H 15 N2O4P

[0013] Relative molecular mass: 198.16 (according to 2001 International Relative Atomic Mass)

[0014] Biological activity: Weed killer

[0015] Melting point: 215℃

[0016] Vapor pressure (20℃): <0.1mPa

[0017] Solubility: 1370g / L in water (22°C), lower solubility in general organic solvents

[0018] Stability: easily soluble in water, low solubility in organic solvents; stable to light, hydrolyzed at pH 5-9.

[0019] Oxyfluorfen:

[0020] ISO common name: Oxyfluorfen

[0021] CA Registration Number: 42874-03-3

[0022] Chemical name: 2-chloro-α, α, α-trifluoro-p-tolyl-3-ethoxy-4-nitrophenyl ether.

[0023] Structural formula:

[0024] Molecular formula: C 15 H 11 C l F3NO4

[0025] Relative molecular mass: 361.7 (according to 2001 International Relative Atomic Mass)

[0026] Biological activity: Weed killer

[0027] Physical and chemical properties: The pure product is a white crystalline solid, and the original drug is brown. MP84~85℃, BP250~300℃, flash point 93.35℃, vapor pressure 0.267×10 -3 Pa (25℃), relative density 1.04~1.06 (25℃). Easily soluble in organic solvents such as acetone, ethanol, xylene, dichloroethylene, etc., solubility in water <0.1mg / L (25℃). Unstable when exposed to light.

[0028] From the structure and solubility characteristics of glufosinate and oxyfluorfen, it can be seen that glufosinate is an organic ammonium salt with high solubility in water but very low solubility in organic solvents. Oxyfluorfen has high solubility in organic solvents but very low solubility in water. The aqueous solution of glufosinate itself belongs to a high-salt aqueous solution system after the ammonium ions in glufosinate are released. As is known to all, high-salt water systems have extremely strong destructive power against both anions and general non-ions. Therefore, general anions / non-ions become clear and transparent after dissolving oxyfluorfen, but stratification, turbidity or flocculation occurs after adding the glufosinate aqueous solution. Fig.13 As shown, after the water phase and the oil phase are prepared separately by the conventional preparation process, the water phase is added to the oil phase, and the two phases can be kept for a period of time at room temperature, but cannot be fully compatible after heat storage, resulting in stratification. In order to increase the stability of the preparation and solve the turbidity, flocculation and crystallization problems of the preparation at room temperature and low temperature, the present invention utilizes the characteristics of free ammonium ions of glufosinate and the need for anionic non-ions to maintain stability in aqueous solution, selects a hydrophilic and lipophilic amphoteric surface regulator, and utilizes its hydrophilic and lipophilic properties to enhance the stability of the preparation.

[0029] In order to solve the above problems, the first aspect of the present invention provides a highly effective herbicidal microemulsion, wherein the raw materials of the microemulsion include at least 10-30wt% of an effective ingredient;

[0030] In some preferred embodiments, the active ingredients include active ingredient A and active ingredient B; active ingredient A is glufosinate-ammonium; and active ingredient B is oxyfluorfen.

[0031] More preferably, the active ingredient B is oxyfluorfen, and the weight ratio of oxyfluorfen to glufosinate is (1-5):(15-25).

[0032] More preferably, the weight ratio of oxyfluorfen to glufosinate is 2.8:14.2 or 3:18.

[0033] Traditional herbicides have low weed control efficiency and are easily washed away by rainwater. They need to be applied in large doses to achieve the expected control effect, but this is accompanied by strong weed resistance, forming a vicious circle in the weed control process. The present invention selects oxyfluorfen and glufosinate ammonium for compounding, adopts a diphenyl ether herbicide and a contact type organophosphorus herbicide for mixed action, and acts on weeds simultaneously in different action modes, achieving a broad-spectrum and efficient weed control effect on the one hand, and effectively delaying the weed resistance on the other hand, and is particularly suitable for the control of weeds in non-cultivated land. The reason is that oxyfluorfen and glufosinate work together. On the one hand, they can destroy the permeability of weed plant cells, inhibit the formation of essential enzymes for the synthesis of tetrapyrrole compounds in plant cells, cause physiological activity disorders of weed cells, accelerate aging and eventually wilt and fall off; on the other hand, they hinder the reaction activity of plant nitrogen metabolism control enzymes, so that the toxic ammonia released by the life activities of weed plants cannot be effectively eliminated, causing metabolic disorders of nutrient elements of weed plants, insufficient supply of essential amino acids, and the transfer of nutrients and energy in plants cannot proceed normally, so that weeds are effectively eliminated. The present invention has found through a large number of experimental screenings that when the weight ratio of oxyfluorfen and glufosinate is (1-5): (15-25), especially 3:18, it has a significant synergistic effect on annual weeds (especially Amaranthus spinulosa, Chenopodium album, Crabgrass and Setaria viridis). Under this condition, the microemulsion has a good conduction effect on weeds, oxyfluorfen and glufosinate give full play to the blocking mechanism, effectively delay the resistance of weeds, reduce the dosage while efficiently killing weeds, and reduce economic costs and environmental pressures.

[0034] In some preferred embodiments, the raw materials of the microemulsion include, by weight percentage: 10-30% of active ingredient, 10-30% of surface regulator, 5-18% of cosolvent, 7-16% of solvent A, and the balance of water.

[0035] In some preferred embodiments, the surface conditioner includes at least one of a hydrophilic and lipophilic amphoteric additive, an anionic surfactant and a nonionic surfactant, and more preferably a hydrophilic and lipophilic amphoteric additive.

[0036] In some preferred embodiments, the hydrophilic and lipophilic amphoteric additives include one or more of amino acid type amphoteric surfactants, betaine type amphoteric surfactants, imidazoline type amphoteric surfactants, and amine oxide type amphoteric surfactants.

[0037] Examples of the amine oxide type amphoteric surfactant include, but are not limited to, octadecyl dihydroxyethyl amine oxide, tetradecyl dihydroxyethyl amine oxide, stearyl amide propyl amine oxide, and cocoamidopropyl amine oxide.

[0038] In some preferred embodiments, the hydrophilic and lipophilic amphoteric additive is a mixture of castor oil polyoxyethylene ether and calcium dodecylbenzene sulfonate.

[0039] In some preferred embodiments, the anionic surfactant includes a combination of one or more of stearate, sodium di(laureth-7) citrate, sodium laureth-11 carboxylate, alkyl sulfonates, alkylbenzene sulfonates, alkylnaphthalene sulfonates, and succinate sulfonates.

[0040] In some preferred embodiments, the nonionic surfactant includes a combination of one or more of alkyl glycosides, long-chain fatty alcohol polyoxyethylene ethers, alkylphenol polyoxyethylene ethers, fatty acid polyoxyethylene esters, polyoxyethylene alkylamines, and polyoxyethylene alkylamides.

[0041] Oxyfluorfen-butyl-glufosinate microemulsion has the characteristics of significant herbicidal effect and low toxicity to non-target organisms, but its stability is still affected by complex external factors, which in turn affects the effective effect of the microemulsion when used in the field; the control of the stability of the microemulsion becomes an important factor in ensuring its preventive effect. After a large number of experimental attempts, the present invention selects specific hydrophilic and lipophilic amphoteric adjuvants for use in combination with non-silicon defoaming agents, which can suppress the overflow of effective ingredients in the microemulsion to a large extent. The reason may be that under this condition, the oil phase and water phase raw materials can be fully compatible under the action of emulsifiers, cyclohexanone and other substances, and the surface tension of various phases in the microemulsion is improved to the greatest extent. The amphoteric surfactant has both anionic and cationic or nonionic and cationic structures in the same molecular structure, so that the microemulsion can form a uniform dispersed microemulsion system under low energy drive, and the decomposition trend of the microemulsion is significantly suppressed, and the stability is improved. Fig.14 As shown, different surfactants are selected in the preparation process. After the water phase and the oil phase are prepared separately by conventional preparation methods, the water phase is added to the oil phase. The preparation becomes turbid after heat storage. This shows that the upper limit of the transparent temperature of adding different auxiliary agents is low. Turbidity occurs after heating, and it is difficult to ensure that the preparation is stable at (-5 to 60 degrees Celsius). This application effectively solves this problem by selecting specific amphoteric surfactants, coordinating the active ingredients and auxiliary agents. Fig.15 As shown, microemulsions containing glufosinate and oxyfluorfen are prone to flocculation and precipitation problems under low temperature conditions. Different surface regulators are selected during the preparation process. After the water phase and the oil phase are prepared separately using the conventional preparation process, the water phase is added to the oil phase. The preparation becomes turbid after cold storage, indicating that the lower limit of the transparent temperature of adding different adjuvants is low. Turbidity and crystal precipitation are prone to occur after cooling. The effect of the surfactant adjuvant is difficult to fully exert, and it is difficult to ensure that the preparation is stable at (-5 to 60 degrees Celsius). The microemulsion obtained by selecting specific adjuvants in this application no longer precipitates crystals under refrigeration, and the temperature below the transparent temperature can be maintained at -5°C for about 2 days.

[0042] Note: Fig.14Sample d corresponds to the solution of Example 6, and the formula of samples abc is the same as that of Example 6, except that the type of surface conditioner is replaced. Fig.15 The formula of the abcd samples is the same as that of Example 6, except that the type of surface conditioner is replaced.

[0043] In some preferred embodiments, the raw materials of the microemulsion further include 0.001-0.1% of a defoaming agent.

[0044] In some preferred embodiments, the defoaming agent is a silicone defoaming agent and / or a non-silicon defoaming agent.

[0045] The addition of emulsifiers can promote the compatibility of the oil phase and the aqueous phase system, but it will inevitably produce a large amount of foam, affecting the efficacy of the herbicide. The addition of defoamers can inhibit the generation of foam, but the addition of traditional silicone defoamers will make the microemulsion system turbid and reduce stability. The addition of different types of defoamers has a great influence on the stability of the microemulsion. Improper addition of defoamers will cause the product to be stratified or turbid (especially if the amount of silicon-containing defoamers added at room temperature is slightly larger, stratification will occur). After a lot of research, the present application found that the defoamer is preferably a non-silicon defoamer. The present invention adds a very small amount of non-silicon defoamer, which solves the technical bottleneck of flocculation and turbidity of microemulsions, and interacts with specific effective ingredients, surface regulators, etc. to give the microemulsion excellent transparency. The resulting microemulsion has the characteristics of not being easy to flocculate and become turbid, and having stable properties, which further promotes the efficacy of the herbicide.

[0046] In some preferred embodiments, the co-solvent has a flash point of 20-65°C and a boiling point of 130-165°C.

[0047] More preferably, the co-solvent is cyclohexanone, which has a flash point of 43°C and a boiling point of 156°C.

[0048] In some preferred embodiments, the solvent A is solvent oil, and the boiling range of the solvent oil is 60-200°C.

[0049] Examples of solvent oil with a boiling range of 60 to 200° C. include, but are not limited to, 100# solvent oil, 150# solvent oil, and 200# solvent oil.

[0050] In some preferred embodiments, the defoamer is a non-silicone defoamer; further preferably, it is a combination of one or more of a high-carbon alcohol emulsion defoamer and a silicon-free polyether defoamer.

[0051] The second aspect of the present invention provides a method for preparing a highly effective herbicidal microemulsion, the preparation steps of the microemulsion comprising:

[0052] S1. Add active ingredient A, cosolvent, solvent A to reactor A and stir to dissolve evenly;

[0053] S2. Sequentially add the emulsifier and defoamer to the reactor A and stir to obtain a mixture;

[0054] S3. The active ingredient B and water were added to the reactor B and stirred to obtain a mixture II;

[0055] S4. Add the mixture 2 to the mixture 1 and stir evenly to obtain a mixture 3;

[0056] S5. Filter the mixed material three, discharging and packaging to obtain the finished product.

[0057] Further preferably, the preparation steps of the microemulsion include:

[0058] S1. Add oxyfluorfen, cyclohexanone and solvent A to reactor A and stir for 10-60 min;

[0059] S2. Sequentially add the emulsifier and defoamer to the reactor A and stir for 10-30 min to obtain a mixture;

[0060] S3. Add glufosinate and water to reactor B and stir for 10-60 min to obtain a mixture II;

[0061] S4. Use a diaphragm pump to pump the mixture 2 into the mixture 1, stir for 10-45 minutes, and obtain the mixture 3;

[0062] S5. Filter the mixed material three, discharging and packaging to obtain the finished product.

[0063] The present invention has been found through painstaking experimental research that, under the premise that the active ingredients are oxyfluorfen and glufosinate, the surface regulator is a hydrophilic and lipophilic amphoteric adjuvant, and the defoamer is a non-silicone defoamer, the two active ingredients are first dissolved using solvent A and deionized water respectively, and then further mixed, the stability of the microemulsion is further improved, no active ingredient decomposes after 14 days of high temperature storage, no precipitate or oily matter is precipitated after being placed at a low temperature of -20°C, and the microemulsion remains clear and transparent. Generally, the stability of the product obtained by compounding the oil-soluble active ingredient and the water-soluble active ingredient is poor, and the oil phase and the water phase raw materials are difficult to be compatible at a temperature below -6°C. The present invention unexpectedly discovered during the preparation process that the microemulsion formulation system composed of specific raw materials, after being processed by the above-mentioned process of dissolving and then mixing separately, and mixing in a specific configuration order, the two active sites of the hydrophilic and lipophilic amphiphilic additives in the system can anchor ionic compounds on the one hand, and on the other hand, due to the barrier and anchoring effect of the non-ionic structure, the system is easy to form a colloidal double layer, preventing the mutual collision of the oil phase components in the solvent, and the compatibility of different phases in the microemulsion is improved. It can be stably stored at -20°C, and the microemulsion is not prone to flocculation and turbidity, which effectively ensures that the effect of the ethosulfate-butyl-glufosinate microemulsion is fully exerted, and the practical application value of the ethosulfate-butyl-glufosinate microemulsion is improved. In the experimental exploration, it was found that by adjusting the order of adding the oil phase and the water phase, it was found that the preparation process of adding the water phase to the oil phase had a significantly better transparent temperature range than that of adding the oil phase to the water phase, and could remain transparent and stable at 54 degrees Celsius (see Fig.16 ). During the same period, the order of adding the refrigerated samples was adjusted and it was found that the effect of this method was significantly better than the other one.

[0064] The present invention is a stem and leaf treatment herbicide prepared by mixing two agents with different action mechanisms, oxyfluorfen and glufosinate ammonium. The unique "one seal and one kill" weeding mechanism makes the product have the characteristics of wide weed killing spectrum, fast weed killing speed, long lasting effect period, rainwater erosion resistance, etc., and has good control effect on non-cultivated weeds. Field tests in three places over two years show that after using 21% oxyfluorfen·glufosinate ammonium microemulsion 200-250 ml / mu, the average fresh weight control effect and the average plant control effect can reach 94%, and the product has good applicability. The control effect of the control agent oxyfluorfen and glufosinate ammonium is not as good as the control effect of the mixed preparation. The use of 21% oxyfluorfen·glufosinate ammonium microemulsion can reduce the dosage of the active ingredients oxyfluorfen and glufosinate ammonium used alone. The reduced dosage can delay the drug resistance of weeds. At the same time, the low dosage of the active ingredients also reduces the drug cost of farmers. In addition, 21% oxyfluoride-phosphine ammonium microemulsion can not only replace the eliminated highly toxic pesticide paraquat, but also replace sulfonylurea and sulfonamide herbicides with relatively serious resistance.

[0065] Beneficial effects:

[0066] The microemulsion provided by the present invention has the following advantages:

[0067] (1) Using oxyfluorfen and glufosinate-ammonium in a weight ratio of 2.8:14.2 as active ingredients can achieve a low-dose, high-efficiency weed control effect, greatly saving weed control costs and improving weed control efficiency;

[0068] (2) The compatibility of the water phase and the oil phase in the microemulsion was improved by using a specific surface modifier and a defoaming agent, and the obtained microemulsion could be stably stored at -20°C;

[0069] (3) Using specific raw materials and specific preparation processes to promote the uniform dispersion of the raw materials in the microemulsion, the microemulsion has low foaming properties and can maintain a stable and uniform clear and transparent state without turbidity;

[0070] (4) The raw materials of the present invention are easily available and the process is simple. On the one hand, it can kill weeds on a broad spectrum. On the other hand, it is more convenient to transport and use, and is suitable for mass production and promotion, which has positive significance for promoting the development of herbicide technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0071] Figure 1 .Original data of the toxicity test results of glufosinate-ammonium, oxyfluorfen and their mixed combinations on Amaranthus spinulosa;

[0072] Figure 2 .Original data of the toxicity test results of glufosinate, oxyfluorfen and their mixed combinations on Chenopodium album;

[0073] Figure 3 .Original data of the toxicity test results of glufosinate-ammonium, oxyfluorfen and their mixed combinations against Digitaria;

[0074] Figure 4 .Original data of the toxicity test results of glufosinate-ammonium, oxyfluorfen and their mixed combinations on Setaria viridis;

[0075] Figure 5 .Schematic diagram of the plot for field efficacy test (Sichuan);

[0076] Figure 6 . Weather conditions at the test site on the day of pesticide application in winter 2019 (Sichuan);

[0077] Figure 7 .Meteorological data table during the field efficacy test in winter 2019 (Sichuan);

[0078] Figure 8 .Weather conditions at the test site on the day of pesticide application in spring 2020 (Sichuan);

[0079] Figure 9. Meteorological data table during the field efficacy test in spring 2020 (Sichuan);

[0080] Fig.10 .Schematic diagram of the plot for field efficacy test (Shanghai);

[0081] Fig.11 . Weather conditions at the test site on the day of pesticide application in winter 2019 (Shanghai);

[0082] Fig.12 .Meteorological data table during the field efficacy test in winter 2019 (Shanghai).

[0083] Fig.13 .The effect diagram of conventional preparation of glufosinate-ammonium and oxyfluorfen;

[0084] Fig.14 .The thermal storage stability effect diagram of microemulsions with different surface modifiers added; wherein a is a polymer of methyl ethylene oxide and butyl ether ethylene oxide (Nouryon), b is a quaternary ammonium salt derivative (Solvay), c is an ethoxylated tallow alkylamine (Huntsman), and d is a mixture of castor oil polyoxyethylene ether and calcium dodecylbenzene sulfonate (corresponding to Example 6);

[0085] Fig.15 . The cold storage stability effect diagram of microemulsions with different surface modifiers added; wherein a is an acrylic polymer (Yunfa CP120), b is a polymer of methyl ethylene oxide and butyl ether ethylene oxide, c is a quaternary ammonium salt derivative, and d is an ethoxylated tallow alkylamine (Solvay);

[0086] Fig.16 .Microemulsion prepared by adding oil phase to water phase (the left picture shows the results of hot storage stability test, and the right picture shows the results of cold storage stability test) DETAILED DESCRIPTION

[0087] Examples 1-8

[0088] Examples 1-8 provide highly effective herbicidal microemulsions, the raw material compositions of which are shown in Table 1.0 below (in weight percentage).

[0089] Table 1.0 Formulation composition and physicochemical properties of Examples 1-8

[0090]

[0091] The hydrophilic and lipophilic amphoteric additive is specifically a mixture of castor oil polyoxyethylene ether and calcium dodecylbenzene sulfonate, which is derived from Solvay SA (me06).

[0092] The non-silicon defoaming agent is specifically DE-R023, which comes from Hefei Yueguan New Materials Co., Ltd.

[0093] The organosilicon defoamer is specifically THIX-278, which comes from Yantai Hengxin Chemical Technology Co., Ltd.

[0094] The amount of the defoamer added in Examples 1 to 8 is 0.1 wt %.

[0095] The solvent oil is s-150 aromatic solvent oil.

[0096] The steps for preparing the highly effective herbicidal microemulsions described in Examples 1-8 include:

[0097] S1. Add oxyfluorfen, cyclohexanone and solvent A into reactor A and stir for 30 min;

[0098] S2. The surface conditioning agent was added to the reactor A and stirred for 30 min to obtain a mixture;

[0099] S3. Add glufosinate, water and defoamer to reactor B and stir for 20 min to obtain a mixture II;

[0100] S4. Use a diaphragm pump to pump mixture 2 into mixture 1 and stir for 30 minutes to obtain mixture 3;

[0101] S5. Filter the mixed material three, discharging and packaging to obtain the finished product.

[0102] Note: The storage time of the microemulsions of Examples 1-8 at 54°C and -20°C is 14 days and 7 days respectively.

[0103] Performance Testing Methods

[0104] 1. Formulation screening test

[0105] 1. Purpose of the experiment

[0106] The herbicidal effects of glufosinate, oxyfluorfen and their different mixed combinations on Amaranthus spinulosa, Chenopodium album, Digitaria sanguinea and Setaria viridis were determined under greenhouse potted conditions, and their combined effects were evaluated, in order to provide a scientific basis for the formulation development of the agents and the field efficacy trials for pesticide registration.

[0107] 2 Test conditions

[0108] 2.1 Test targets

[0109] Amaranthus spinosus L., Chenopodium album L., Digitariasan guinalis L., Setaria viridis (L.) Beauv. are all stored in the weed seed storage bank of the Pesticide Bioassay Research Center of Hunan Research Institute of Chemical Industry.

[0110] 2.2 Culture conditions

[0111] The culture conditions of the test targets and the post-test targets were a temperature of 20±5°C and a relative humidity of 65±5%.

[0112] 2.3 Instruments and Equipment

[0113] Electronic balance, beaker, pipette, measuring cylinder, crop sprayer, etc.

[0114] 3 Experimental design

[0115] 3.1 Test Agents

[0116] Glufosinate-ammonium 98% technical and oxyfurofen 95% technical were both provided by Shanghai Yuelian Chemical Co., Ltd.

[0117] 3.2 Preparation of medicine

[0118] Glufosinate solution: Accurately weigh 0.0300 g of 98% glufosinate technical, dissolve it in 0.2 mL of DMF, add 80 mL of water containing 0.1% Tween 80 emulsifier, stir evenly to prepare a glufosinate solution of 580 g ai / ha, and then dilute it with water to concentrations of 460, 350, 240, and 150 g ai / ha for later use.

[0119] Oxyfluorfen solution: Accurately weigh 0.0032 g of 95% oxyfluorfen technical, dissolve it in 0.2 mL DMF, add 80 mL of clean water containing 0.1% Tween 80 emulsifier, stir evenly to prepare 60 g ai. / ha oxyfluorfen solution, and then dilute with clean water to concentrations of 50, 40, 32, and 24 g ai / ha for later use.

[0120] Blank control solution: 0.2 mL DMF plus 80 mL of water containing 0.1% Tween 80 emulsifier.

[0121] 4 Test methods

[0122] The potted stem and leaf spray method (NY / T1155.4-2006) was used: a plastic pot with a height of 6 cm and a diameter of 9 cm was filled with a certain amount of soil, 15 to 20 target weed seeds were sown in the plastic pot, covered with 0.5 to 1 cm thick fine soil and placed in a greenhouse for routine cultivation. After the weeds emerged, the seedlings were thinned and the weeds were fixed to ensure the uniform density of the weeds. When Amaranthus spinulosus grew to the 4-leaf stage, Chenopodium album to the 4-leaf stage, Digitaria to the 2-leaf stage, and Setaria officinalis to the 2-leaf stage, the stem and leaf spray treatment was carried out, 1 mL of the solution was sprayed per pot, and each treatment was repeated 4 times, and the treatment without the agent was set as the control. After treatment, the test materials were placed in the greenhouse for cultivation, and the growth of the target weeds was observed regularly. After 15 days, the target damage symptoms and growth inhibition were visually observed, and the fresh weight of the aboveground part was weighed. The toxicity of the agent to the target weeds was evaluated by the target fresh weight inhibition rate.

[0123] 5. Data investigation and statistical analysis

[0124] 5.1 Survey Methods

[0125] Fifteen days after the experimental treatment, the target damage symptoms and growth inhibition were visually observed, the fresh weight of the above-ground part was weighed, and the fresh weight inhibition rate (%) was calculated.

[0126] Fresh weight inhibition rate P (%) = (control fresh weight - treatment fresh weight) / control fresh weight × 100

[0127] 5.2 Methods for evaluating combined effects

[0128] The combined action mode of herbicides was evaluated according to the Gowing method (NY / T 1155.7-2006), and the formula is as follows: E0 = X + Y - XY / 100

[0129] Wherein, X is the fresh weight inhibition rate of target weeds when glufosinate ammonium is used alone at a certain dose; Y is the fresh weight inhibition rate of target weeds when oxyfluorfen is used alone at a certain dose; E0 is the theoretical value of the fresh weight inhibition rate of target weeds when glufosinate ammonium and oxyfluorfen are mixed; E is the measured value of the fresh weight inhibition rate of target weeds when glufosinate ammonium and oxyfluorfen are mixed.

[0130] Evaluation criteria: When E-E0>10%, it indicates a synergistic effect; when -10%≤E-E0≤10%, it indicates an additive effect; and when E-E0<-10%, it indicates an antagonistic effect.

[0131] 5.3 Data Statistical Analysis

[0132] All experimental data were analyzed using SAS6.12 statistical software.

[0133] 6. Toxicity assay results

[0134] See Tables 1-4.

[0135] Summary: The test results show that glufosinate and oxyfluorfen are mixed in the following order: 150+20, 150+30, 150+40, 150+50, 150+60, 240+20, 240+30, 240+40, 240+50, 240+60, 350+20, 350+30, 350+40, 350+50, 350+60, 460+20, 460+30, The mixing ratios of 460+40, 460+50, 460+60, 580+20, 580+30, 580+40, 580+50, and 580+60 showed additive effects on the weed control of Amaranthus spinulosa, Chenopodium album, Digitaria sanguinalis, and Setaria viridis. Among them, the mixing combination of 240+40 (i.e., the active ingredient ratio of glufosinate to oxyfluorfen is 6:1) had the best additive effect on Amaranthus spinulosa, Chenopodium album, Digitaria sanguinalis, and Setaria viridis.

[0136] The microemulsion formed by mixing the active ingredients oxyfluorfen and glufosinate ammonium can achieve better weed control effects when mixed in two different modes of action; the two different mechanisms of action can delay drug resistance when mixed; the mixture of the two can enhance the effect; and the cost can be reduced by reducing the amount of medicine used, thereby reducing environmental hazards and the development of drug resistance.

[0137] Table 1. Results of toxicity test of glufosinate, oxyfluorfen and their mixed combinations against Amaranthus spinulosa

[0138]

[0139] Table 2. Toxicity test results of glufosinate, oxyfluorfen and their mixed combinations to Chenopodium album

[0140]

[0141] Table 3. Results of toxicity test of glufosinate, oxyfluorfen and their mixed combinations against Digitaria

[0142]

[0143] Table 4. Results of toxicity test of glufosinate, oxyfluorfen and their mixed combinations to Setaria viridis

[0144]

[0145] 2. Field efficacy test

[0146] A.Winter 2019 (Sichuan)

[0147] 1 Test conditions

[0148] 1.1 Crops and targets: Crops / non-arable land

[0149] Target / weeds / main weeds include Stellaria media (L.) Cyr., Cardamine hirsute L., Gnaphalium affine D. Don, Polypogon fugax Nees ex Steud, etc.

[0150] 1. Experimental conditions: The experiment was conducted in Jinguang Village, Yuexing Town, Dongpo District, Meishan City, Sichuan Province from November 7, 2019 to December 17, 2019. The weeds in the experimental field were serious, and the main weeds were: scutellaria baicalensis, chickweed, cardamine, and scurvy. When the pesticide was applied, the number of scutellaria baicalensis was about 200 plants / m 2 , height 5-10cm; Chickweed 230 plants / m, height about 3-15cm; Cardamom about 300 plants / m', height 5-10cm. The field is mud loam, pH value 5.5, organic matter content about 1.60%, fertility level is medium.

[0151] 2.1 Drug Test Drug: The microemulsion provided in Example 6 was sourced from Shanghai Yuelian Chemical Co., Ltd.

[0152] Control reagent A: 240 g / L oxyfluorfen emulsifiable concentrate, sourced from Shanghai Huiguang Environmental Technology Co., Ltd.

[0153] Control reagent B: 80% glufosinate soluble granules, sourced from Shanghai Yuelian Chemical Co., Ltd.

[0154] Test treatment:

[0155] Table 5. Experimental treatment and control information

[0156] Among them, the reagents of treatments A to C correspond to the test reagents (ie, Example 6), the reagents of treatments D and E correspond to the control reagents A and B, and the reagent of treatment F corresponds to clean water.

[0157] 2.2 Community Arrangement

[0158] 2.2.1 Plot arrangement: Plots are arranged in random blocks, see Figure 5 .

[0159] 2.2.2 Plot area and replication: 4 replications, plot area 30m 2 There are protection lines in the community.

[0160] 2.3 Application method

[0161] 2.3.1 Time and frequency of application: Spray the stems and leaves once on November 7, 2019 when weeds are growing vigorously.

[0162] 2.3.2 Equipment and application method: The secondary dilution method is used to prepare the liquid medicine. The main preparation tools are: balance, measuring cylinder, pipette, glass rod, etc. Use HD400 sprayer for spraying, the spray pressure is 0.2-0.4MPa, the spray hole diameter is 1mm, and the water consumption per plot is about 2 liters.

[0163] 2.3.3 Meteorological data: see Figure 6 and Figure 7 .

[0164] 2.3.4 Soil data: Mud loam, pH 5.5, organic matter content about 1.60%, medium fertility. 2.3.5 Control of non-target organisms: No other pesticides were applied during the test.

[0165] 3 Investigation and Results

[0166] 3.1 Survey method: Plant protection effect, random sampling at 3 points in each plot, 0.25m per point 2 For weed control effect, each tiller was counted as one weed plant. For fresh weight control effect, three random sampling points were selected in each plot, with a density of 0.25 m 2 , weigh the fresh weight of the weeds.

[0167] 3.2 Survey time and frequency: Visually inspect weed mortality 9 days after application, investigate plant efficacy 25 days after application, and investigate plant and fresh weight efficacy 40 days after application. Specific time: November 16, 2019, December 2, 2019, and December 17, 2019.

[0168] 3.3 This test complies with the "Quality Management Standards for Pesticide Registration Tests", and is based on the "Guidelines for Pesticide Field Efficacy Tests" GB / T 17980.51-2000 and S0P-TM-001a "Herbicide Tests". The calculation formula is as follows:

[0169] Control effect of weeds per plant·fresh weight (%) = (number of weeds per plant·fresh weight in the control area - number of weeds per plant·fresh weight in the treatment area) / number of weeds per plant·fresh weight in the control area × 100

[0170] 3.4 Effects on other organisms: No significant effects of the test agent on other organisms were observed during the test.

[0171] 3.5 Test results

[0172] 3.5.1 Control effect: The average control effect is shown in Table 6-8.

[0173] Table 6. Table of efficacy of pesticides in controlling weeds in non-cultivated land 25 days after use (Dongpo District, Sichuan Province, 2019) Plants / 0.75m 2

[0174]

[0175] Table 7. Table of efficacy of pesticides in controlling weeds in non-cultivated land 40 days after use (Dongpo District, Sichuan Province, 2019) Plants / 0.75m 2

[0176]

[0177] Table 8. Fresh weight control effect of pesticides on weeds in non-cultivated land 40 days after use (Dongpo District, Sichuan Province, 2019) g / 0.75m 2

[0178]

[0179] The data in Tables 6-8 are the averages of 4 repetitions. The variance analysis was processed by DPS (version v7.05). Letters represent significant differences (uppercase 0.01 level, lowercase 0.05 level, DMRT method).

[0180] 3.5.2 Safety: The surrounding organisms were safe during the test and no symptoms of pesticide damage were observed.

[0181] The test results show that 21% oxyfluorfen·glufosinate microemulsion can control weeds in non-cultivated land, and has good control effects on chickweed, cardamine, scurf grass, and corydalis. Chickweed, cardamine, scurf grass, and corydalis are sensitive weeds. Oxyfluorfen cannot effectively kill weeds in non-cultivated land at the test dose, but can significantly inhibit weed growth, showing a certain control effect; glufosinate can significantly kill weeds in non-cultivated land and inhibit weed growth at the test dose, but its comprehensive control ability is slightly lower than that of 21% oxyfluorfen·glufosinate microemulsion. During the test, the surrounding organisms were safe and no phytotoxicity symptoms were observed. 21% oxyfluorfen·glufosinate microemulsion can be used to control weeds in non-cultivated land.

[0182] B. Spring 2020 (Sichuan)

[0183] 1 Test conditions

[0184] 1.1 Crops and targets: Crops / non-arable land

[0185] Target / weeds / major weeds include Digitaria sanguinalis (L.) Scop., Conyza canadensis (L.) Cron q., Solanum nigrum L., Alternanthera philoxeroides (Mart.) Griseb., etc.

[0186] 1.2 Experimental conditions: The experiment was conducted from April 2, 2020 to May 12, 2020 in an idle field requisitioned by the government of Tianku Village, Jinjiang Township, Pengshan District, Meishan City, Sichuan Province. The field had been abandoned for half a year, and the weeds were serious. The main weeds were: Digitaria, Erigeron cantoniensis, Solanum nigrum, Alternanthera philoxeroides, etc. The field was mud loam with a pH value of 6.2, an organic matter content of 1.68%, and a medium-low fertility level.

[0187] 2.1 Drug and reagent treatment and 2.2 Community arrangement are the same as the implementation method in winter 2019 (Sichuan).

[0188] 2.3 Application method

[0189] 2.3.1 Application time and frequency: On April 2, 2020, the stems and leaves were sprayed once during the vigorous growth period of weeds. 2.3.2 Equipment and application method: The solution was prepared by the secondary dilution method. The main preparation tools are: balance, measuring cylinder, pipette, glass rod, etc. Use Linong HD 400 sprayer for spraying, the spray pressure is 0.2-0.4MPa, the nozzle diameter is 1mm, and the water consumption per plot is about 2.75L. For detailed information, see Figure 9.

[0190] 2.3.3 Weather data: On April 2, 2020, there was light rain in the early morning, and it was cloudy when the pesticide was applied, which did not affect the test. For detailed information, see Figure 8 .

[0191] 2.3.4 Soil data: loam, pH 6.2, organic matter content 1.68%, medium to low fertility level.

[0192] 2.3.5 Prevention of non-target organisms: No other agents were administered during the trial.

[0193] 3 Investigation and Results

[0194] 3.1 Survey method: Plant protection effect, random sampling at 4 points in each plot, 0.25m 2 For weed control efficiency, each tiller was counted as one weed plant. For fresh weight control efficiency, four random sampling points were selected in each plot, with a density of 0.25 m 2 , weigh the fresh weight of the weeds.

[0195] 3.2 Survey time and frequency: Visually inspect weed mortality 14 days after application, investigate plant efficacy 25 days after application, and investigate plant and fresh weight efficacy 40 days after application. Specific time: April 16, 2020, April 27, 2020, and May 12, 2020.

[0196] 3.3 The calculation formula for prevention effectiveness is the same as that for the winter of 2019.

[0197] 3.4 Effects on other organisms: No effects of the test agent on other organisms were observed during the experiment.

[0198] 3.5 Test results

[0199] 3.5.1 Control effect: The average control effect is shown in Table 9-11, and the original data is shown in Figure 11-13 .

[0200] Table 9. Table of efficacy of pesticides in controlling weeds in non-cultivated land 25 days after use (Pengshan, Sichuan, 2020) Plants / 1m 2

[0201]

[0202] Table 10. Table of efficacy of pesticides in controlling weeds in non-cultivated land 40 days after use (Pengshan, Sichuan, 2020) Plants / 1m 2

[0203]

[0204] Table 11. Table of the efficacy of pesticides in controlling weeds in non-cultivated land after 40 fresh weight (Pengshan, Sichuan, 2020) g / 1m 2

[0205]

[0206] The data in Tables 9-11 are the averages of 4 repetitions, and the variance analysis was processed by DPS (version v7.05). Letters represent significant differences (uppercase 0.01 level, lowercase 0.05 level, DMRT method).

[0207] The test results show that 21% oxyfluorfen-glufosinate microemulsion can control weeds in non-cultivated land, and has a good control effect on crabgrass, Erigeron candidum, Solanum nigrum, and Alternanthera philoxeroides. Oxyfluorfen cannot effectively kill weeds in non-cultivated land at the test dose, but it can significantly inhibit weed growth, showing a certain control effect; glufosinate can significantly kill weeds in non-cultivated land and inhibit weed growth at the test dose, and it has a strong persistence effect, and can still maintain a high control effect after 40 days. During the test, the surrounding organisms were safe and no symptoms of phytotoxicity were observed. 21% oxyfluorfen-glufosinate microemulsion can be used to control weeds in non-cultivated land.

[0208] 3.5.2 Safety: The surrounding organisms were safe during the test and no symptoms of pesticide damage were observed.

[0209] C. Winter 2019 (Shanghai)

[0210] 1. Pharmacy:

[0211] Same as 2019 Winter (Sichuan) Pharmacy.

[0212] 2. Chemical treatment

[0213] Table 12. Drug handling information

[0214]

[0215] 3 Test conditions

[0216] 3.1 Experimental crops and subjects

[0217] Test crops: non-arable land, main weeds are: ground grass weeds - Polypogon fugax, Poa annua, Eleusine indica, broadleaf weeds - Veronica didyma, Cerastium arvense, Elephantopus scaber. 3.2 Test environment and facility cultivation conditions

[0218] The experiment was conducted in an abandoned woodland in Lixi Team, Huayi Village, Huaxin Town, Qingpu District, Shanghai. When the medicine was used on December 15, 2019, the weeds were in their vigorous growth period and the density was relatively high.

[0219] 4.2 Area, number and arrangement of plots

[0220] The test area is 720m 2 , 30m long from north to south, 20m wide from east to west, area of ​​each plot: 6m (length) × 5m (width) = 30m 2 The experiment has 6 treatments, each treatment is repeated 4 times, with a total of 24 plots. The test agent, control agent, and water control treatments are randomly arranged by block group. Fig.10 .

[0221] 4.3 Application method

[0222] 4.3.1 Spraying method

[0223] First, use clean water to calibrate the water requirement of the clean water control, and use the droplets of liquid on the leaves and stems as the standard. The water requirement for each plot is 1.8L. Pour each prepared dose of the drug into the sprayer, add to the required water, and spray each plot evenly.

[0224] 4.3.2 Weighing instruments and pesticide application equipment

[0225] 4.3.2.1 Measuring instruments: electronic balance, measuring cup, and measuring cylinder.

[0226] 4.3.2.2 Application equipment

[0227] The Guardian 3WJD-18 electric electrostatic sprayer uses a fan-shaped nozzle specially designed for herbicides. After calibration, the flow rate error rate is ≤10%.

[0228] 4.3.3 Application time and frequency

[0229] The application time was the afternoon of December 15, 2019, when the weeds in the non-cultivated land were in the late stage of vigorous growth. The application was carried out once in total. The application was carried out around 5:00-7:30 pm.

[0230] 4.3.4 Usage capacity

[0231] 1.8 liters per plot, equivalent to 40 liters per mu and 600 liters per hectare.

[0232] 5. Investigation, recording and measurement methods

[0233] 5.1 Meteorological and soil data

[0234] 5.1.1 Meteorological data Meteorological data can be found in Fig.11 , Fig.12 During this period, there were no severe climatic factors affecting the test results.

[0235] 5.1.2 Soil data The soil type is loamy clay, and the pH value and organic matter content were not measured.

[0236] 5.1.3 No field management data.

[0237] 5.2 Survey methods, time and frequency

[0238] 5.2.1 Survey Methods

[0239] The sampling method is 4 points on the diagonal of each plot, and each point is framed by 0.5m*0.5m lead wire for 0.25m 2 , investigate the number of weeds in the frame (the number of tillers is used for grass weeds, and the total number of large-leaf broad-leaf weeds, "earthengrass", is investigated because of its uneven distribution). Investigate the base number before applying the medicine, investigate the number of residual weeds after applying the medicine, and measure the fresh weight of the weeds for the last time. Calculate the control effect.

[0240] 5.2.2 Survey time and frequency

[0241] Investigate the base number before applying the medicine, investigate the number of residual weeds 14 and 28 days after applying the medicine, and measure the fresh weight 28 days after applying the medicine.

[0242] 5.2.3 Calculation method of drug efficacy

[0243] 5.2.3.1 Calculation formula for drug efficacy

[0244] Reduction rate % = (number of weeds before treatment - number of remaining weeds after treatment) / number of weeds before treatment × 100

[0245] Plant control efficiency % = (% weed reduction rate in the pesticide treatment area - % weed reduction rate in the water control area) / (100 - % weed reduction rate in the water control area) × 100

[0246] Fresh weight control effect % = (fresh weight of weeds in the clear water control area - fresh weight of weeds in the pesticide treatment area) / fresh weight of weeds in the clear water control area × 100

[0247] 5.2.3.2 Statistical methods

[0248] The average value was retained to one decimal place, and the control effect value was retained to two decimal places. The Duncan's new multiple range (DMRT) method was used to statistically analyze the test data for differences in efficacy among treatments, and significance tests were performed at p = 0.05 and 0.01.

[0249] 5.3 No direct impact on crops.

[0250] 5.4 Impact on other organisms

[0251] 5.4.1 Impact on other non-targets

[0252] No significant effects of the test agents on non-target organisms were observed.

[0253] 5.4.2 Impact on other non-target beneficial organisms

[0254] No effect on beneficial organisms.

[0255] 6. Test results

[0256] Table 13 Results of pesticides for controlling weeds in non-cultivated land (14 days after application)

[0257]

[0258]

[0259] Table 14. Results of pesticides for controlling weeds in non-cultivated land (28 days after application)

[0260]

[0261] AB and ab indicate significant differences at the 0.05 and 0.01 levels, respectively.

[0262] 7 Conclusion

[0263] The tested agent has excellent weed control effect at a dosage of 150-250 ml / mu, and the total weed control effect and fresh weight control effect are both above 98.00% 28 days after application. The control effect is equivalent to that of the control single agent 80% glufosinate SG at a conventional dosage, and is higher than that of the control single agent 240g / L oxyfluorfen EC at a conventional dosage, with a very significant difference. The recommended dosage is: 150-200 ml / mu of preparation, 472.4-630 g / hectare of active ingredient, and evenly sprayed by stem and leaf spraying during the peak growth period of weeds in non-arable land.

[0264] 8 Trial Quality and Effectiveness Analysis

[0265] This test was strictly carried out according to the test plan, and the weeds in each treatment were evenly distributed in the field. The target biomass also met the test requirements. The test results truly reflected the control effect level of the tested agent. The test results were valid.

[0266] 9. Test Deviation and Evaluation

[0267] There were no deviations during the test that affected the test results.

[0268] D-F. The same method was used to conduct efficacy tests in Jiangsu in 2020, Hunan in 2019, and Hunan in 2020. The test results of Sichuan, Shanghai, Jiangsu, and Hunan from 2019 to 2020 are summarized in Tables 15-16.

[0269] Table 15. Average plant protection effect in field trials in three locations over two years

[0270]

[0271] Table 16. Average fresh weight control effect of field trials in three locations over two years

[0272]

[0273] Field trials in three places over two years have shown that the average fresh weight control effect and the average plant control effect can reach 94% after using 21% oxyfluoride·glufosinate microemulsion 200-250 ml / mu, which has good applicability. The control effect and fresh weight control effect of the control agent 240 g / L oxyfluoride emulsifiable concentrate 40 ml / mu are 59.97% and 65.21% respectively; the fresh weight control effect and plant control effect of 80% glufosinate soluble granules 60 g / mu are 92% and 93% respectively. The control effect of the control agent is not as good as that of the mixed preparation.

[0274] Through two years of field trials in three places, it can be seen that after the two are mixed, the dosage of the active ingredients oxyfluorfen and glufosinate ammonium is reduced. The reduced dosage can also delay the resistance of weeds. At the same time, the low dosage of active ingredients also reduces the cost of farmers' use of drugs.

[0275] 3. Physical and chemical performance test

[0276] 1. Emulsion stability: Referring to GB / T 1603-2001, add 100mL 30℃±2℃ standard hard water into a 250mL beaker, then add 5mL sample of Example 6, stir with a glass rod at 2.5±0.5r / s for 30s, transfer to a 100mL measuring cylinder, put the measuring cylinder into a 30℃±2℃ constant temperature water bath, and let stand for 1h. No floating (cream), sinking oil and precipitation are observed, and the test result is qualified.

[0277] 2. Persistent foaming property: Referring to GB / T 28137-2011, add standard hard water (20±5℃) to the measuring cylinder to the 180mL mark, add 1.0g of the sample of Example 6, add hard water to the mark 9cm±0.1cm from the bottom of the measuring cylinder stopper, cover the lid, and turn the measuring cylinder upside down 180° 30 times (2s each time) with the middle of the measuring cylinder as the center. Put it vertically on the test bench and let it stand: record the foam volume at 1min±10s. Repeat the measurement three times, and the results are 48.0mL, 48.0mL, 48.0mL, and the average value is 48.0mL.

[0278] 3. Thermal storage stability: Referring to GB / T 19136-2003, the sample of Example 6 was sealed and placed in a 54°C oven for 14 days. The quality and pH of the sample were tested within 24 hours, and the results were measured three times in parallel and recorded in Tables 17-18. At the same time, the decomposition rate of the active ingredients of the sample was measured, and the decomposition rates of oxyfluorfen and glufosinate were both 0%.

[0279] Table 17. Sample mass changes before and after thermal storage

[0280]

[0281] Table 18. pH changes of samples before and after thermal storage

[0282]

[0283] 4. Cold storage stability: Referring to GB / T 19137-2003, the sample of Example 6 was placed at 0°C for 1 hour and the appearance was observed to see if there was any change. After continuing to store at 0°C for 7 days, the volume of the precipitate at the bottom was recorded. No precipitate was observed, and the test result was qualified.

Claims

1. A highly effective herbicidal microemulsion, characterized in that: According to weight percentage, the raw materials of the microemulsion include: 10-30% of active ingredient, 10-30% of surface regulator, 5-18% of cosolvent, 0.001-0.1% of defoamer, 7-16% of solvent, and water to make up the balance; The active ingredients include active ingredient A and active ingredient B; active ingredient A is glufosinate-ammonium; active ingredient B is oxyfluorfen; The weight ratio of oxyfluorfen to glufosinate is 2.8:14.2 or 3:18; The surface conditioning agent is a hydrophilic and lipophilic amphoteric additive, specifically a mixture of castor oil polyoxyethylene ether and calcium dodecylbenzene sulfonate; The defoamer is a non-silicone defoamer, including a combination of one or more of a high-carbon alcohol emulsion defoamer and a silicon-free polyether defoamer; The cosolvent is cyclohexanone.

2. A method for preparing the highly effective herbicidal microemulsion according to claim 1, characterized in that: The preparation steps of the microemulsion include: S1. Add oxyfluorfen, cyclohexanone and solvent to reactor A and stir for 10-60 min; S2. The surface conditioning agent was sequentially added to the reactor A and stirred for 10-30min to obtain a mixture; S3. Add glufosinate, water and defoamer to reactor B and stir for 10-60 min to obtain a mixture II; S4. Use a diaphragm pump to pump mixture 2 into mixture 1, stir for 10-45 minutes, and obtain mixture 3; S5. Filter the mixed material three, discharging and packaging to obtain the finished product.

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