A glufosinate-ammonium salt soluble liquid containing a composite plant source synergistic adjuvant and a preparation method thereof

CN122804795APending Publication Date: 2026-09-25LIER CROPSCIENCE CO LTD
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Patent Information

Application Number
CN202611174947.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-08-04
Publication Date
2026-09-25

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Technical Problem

为克服现有10%精草铵膦铵盐水剂除草见效慢、大龄杂草防效差、低温药效不足、合成助剂难降解、茶皂素发泡严重易堵喷头、冷热贮易分层的技术问题,本发明提供一种稳定、低泡、增效显著、绿色低污染的植物源增效可溶液剂及其制备工艺

Benefits of technology

1、冬青提取物富含天然冬青苷,属于低泡型天然两亲物质,可显著降低药液表面张力,喷雾后在杂草叶面快速铺展、吸附滞留,减少药液滚落流失;区别于茶皂素,几乎无泡沫,适配各类喷雾器械;

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Abstract

The application discloses a kind of phosphinothricin ammonium salt soluble liquid containing composite plant source synergist and a preparation method thereof, and the preparation is prepared into homogeneous transparent soluble liquid by using phosphinothricin ammonium salt as herbicidal active component, collocating extract of ilex aquifolium, rosemary essential oil composite plant source synergic system, and being compounded with dissolving agent, penetrating agent, hydrolytic stabilizer, pH buffer and deionized water.The obtained preparation can significantly reduce the surface tension of liquid medicine, spread, adsorb and stay on the leaf surface of weeds after spraying, reduce the rolling loss of liquid medicine, improve the conduction speed of pesticide in plant, quickly reach the root system, and reduce the probability of perennial weed regrowth.The composite plant source synergist has excellent mutual solubility, does not produce foaming and precipitation problems, optimizes the interface compatibility of system, reduces the hydrolysis of active ingredient, and improves the cold and hot storage stability of preparation.
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Description

Technical Field

[0001] This invention belongs to the field of pesticide formulations, and in particular relates to a soluble form of glufosinate-ammonium salt and its preparation method. Background Technology

[0002] Glufosinate-ammonium salt is a non-selective herbicide belonging to the glutamine synthase inhibitor class. Its mechanism of action is to inhibit nitrogen metabolism in weeds, leading to the accumulation of ammonium ions in the plant, causing poisoning and death. This ingredient has no systemic activity in the soil, is safe for subsequent crops, and is widely applicable for weed control in orchards of cash crops and non-arable land. Currently, the mainstream registered specification on the market is 10% glutfosinate-ammonium salt soluble concentrate. This formulation has good water solubility and is easy to use, making it the current mainstream formulation.

[0003] Existing synergistic systems for conventional 10% glufosinate-ammonium salt soluble concentrates often employ synthetic chemical surfactants such as fatty alcohol ethers, alkyl glycosides, and polycarboxylates, which have several technical drawbacks: First, these synthetic adjuvants only provide basic wetting and cannot effectively break down the dense waxy cuticle layer on weed surfaces, making it difficult for the solution to penetrate deeply into weed tissues. This results in lower efficacy against older weeds (over 20cm in height) and perennial deep-rooted weeds, leading to a higher rate of weed regrowth after application. Second, at low temperatures (below 18℃), the synthetic surfactants... The surface activity of the agent is significantly reduced, the spreading and penetration ability of the pesticide solution is weakened, and the weeding speed is slow when applied in spring and autumn at low temperatures. It usually takes 7 to 10 days for obvious poisoning symptoms to appear. Third, the biodegradation cycle of petroleum-based synthetic adjuvants is relatively long. Long-term and continuous application can easily accumulate in the soil surface layer, destroying the soil microbial community structure, which does not meet the requirements of pesticide reduction and green ecological agriculture development. Fourth, the compatibility between synthetic adjuvants and glufosinate-ammonium salt aqueous solution is limited. Long-term storage can easily cause slight turbidity, layering and other appearance deterioration, affecting the physicochemical stability during the shelf life.

[0004] Existing plant-derived synergistic technologies often use tea saponin as a natural wetting and dispersing agent. However, tea saponin also has unavoidable drawbacks: it has extremely strong foaming properties, and when large motorized sprayers are used in the field, the foam overflows and easily clogs the filters and nozzles, seriously affecting the application efficiency; high amounts of tea saponin are prone to precipitating flocculent substances when stored at low temperatures, which damages the stability of the formulation; and tea saponin has a plant-like odor, resulting in poor sensory quality of the formulation.

[0005] Currently, there is a lack of low-foaming plant-derived synergistic systems that do not contain tea saponins and are compatible with 10% glufoam-phosphonium salt soluble concentrates. The wetting ability of single plant essential oils is insufficient, and the dewaxing effect of single plant extracts is poor, making it difficult to achieve stable and efficient synergistic effects.

[0006] Purpose of the invention To overcome the technical problems of existing 10% glufosinate-ammonium salt solutions, such as slow weed control, poor efficacy against older weeds, insufficient efficacy at low temperatures, difficulty in degrading synthetic adjuvants, severe foaming of tea saponins leading to nozzle clogging, and easy stratification during cold and hot storage, this invention provides a stable, low-foaming, significantly synergistic, green, and low-pollution plant-derived synergistic soluble concentrate and its preparation process. Summary of the Invention

[0007] This invention provides a low-foaming, plant-derived, synergistic 10% glufoam-phosphonium salt soluble concentrate formulated with wintergreen extract and rosemary essential oil, free of tea saponins, which combines synergistic effects, low-temperature adaptability, low-foaming ease of use, storage stability, and environmental friendliness.

[0008] Specifically, this invention provides a 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, comprising the following components by mass percentage: 10.94% glufosinate-ammonium salt technical grade; 2.5-7.0% compound plant-derived synergistic adjuvant; 3.0-9.0% solubilizer; 1.0-3.5% penetration enhancer; 0.2-1.2% hydrolysis stabilizer; 0.1-0.6% pH buffer adjuster; and the balance being deionized water; the total mass fraction of all components is 100%; and the effective content of glufosinate-ammonium in the formulation is consistently 10%.

[0009] Preferably, the compound plant-derived synergist is composed of wintergreen extract and rosemary essential oil in a mass ratio of 2:1 to 4:1; the wintergreen extract has an active ingredient content of ≥90%, and the rosemary essential oil has a total terpenoid + phenolic active ingredient content of ≥85%; The co-solvent is one or more of propylene glycol, ethylene glycol, and propylene glycol methyl ether; the penetration aid is C8-C10 fatty alcohol polyoxyethylene ether; the hydrolysis stabilizer is either sodium benzoate or sodium bisulfite; the pH buffer adjuster is glacial acetic acid or dilute ammonia to adjust the pH of the preparation to 5.0-6.8.

[0010] The method for preparing the wintergreen extract of the present invention includes the following steps: preparing wintergreen ( Ilex chinensis The leaves were chopped and extracted in a microwave extraction vessel using 75% ethanol solution under microwave reflux for 60 min. The extract was separated, concentrated, and then used to obtain holly glycoside extract. The holly glycoside extract was dissolved again with 10 times its weight of 75% ethanol solution, filtered through 100-mesh activated carbon, and the filtrate was collected. The pH of the solution was adjusted to 6.5 with 0.1 mol / L hydrochloric acid solution, and NaCl was added to saturate the solution. The mixture was cooled to 4°C to precipitate, filtered, collected, and dried to obtain holly extract. The rated power of the microwave reflux extraction was 800W, and the extraction temperature was 15°C.

[0011] The preparation method of rosemary essential oil of the present invention refers to patent CN201710660289. The specific method includes the following steps: (1) soaking fresh rosemary branches and leaves in water and then grinding them to obtain rosemary slurry; the mass ratio of fresh rosemary branches and leaves to water is 1:3; (2) treating the rosemary slurry obtained in step (1) to obtain rosemary slurry after cell wall breaking; the cell wall breaking method is enzymatic hydrolysis; the enzyme used for enzymatic hydrolysis is a complex enzyme with a mass ratio of cellulase with an enzyme activity of 450,000 U / g and pectinase with an enzyme activity of 450,000 U / g, which is 1:1; (3) distilling the rosemary slurry obtained in step (2) using a rotary distillation apparatus to obtain a rosemary oil-water mixture and a residue-liquid mixture; (4) separating the oil and water in the rosemary oil-water mixture obtained in step (3) to obtain rosemary essential oil.

[0012] More preferably, the present invention provides a 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, characterized in that the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, wintergreen extract 3.2%, rosemary essential oil 1.1%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water 66.55%.

[0013] This invention also provides a method for preparing a 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, characterized by comprising the following steps: Step 1: Weigh each component according to its weight percentage and set aside.

[0014] Step 2: At 20-30℃ and a stirring speed of 300-500 r / min, add metered deionized water to the stirred tank, add glufosinate-ammonium salt technical material, and continue stirring for 15-20 min until the solid is completely dissolved to obtain a transparent active mother liquor. Step 3: Add the cosolvent, penetration enhancer, and hydrolysis stabilizer to the mother liquor in sequence, and stir for 10 minutes to mix evenly; Step 4: Slowly drip the pre-mixed wintergreen extract and rosemary essential oil complex plant-derived synergist into the system and stir continuously for 15 minutes until the system is homogeneous and transparent. Step 5: Add pH buffer to adjust the pH of the system to 5.0-6.8, and keep warm and stir for 20 minutes; Step 6: Let stand naturally for 25-35 minutes to defoam, then filter with a 200-mesh filter to remove trace impurities. After testing the effective ingredients and stability, fill the solution to obtain the finished product.

[0015] The preparation method of this invention requires no heating or high-temperature reaction process, and the production environment is at normal pressure and temperature, making it safe and efficient.

[0016] This invention also provides the use of a 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant. The soluble concentrate is used for controlling annual and perennial weeds in orchards, tea gardens, wastelands, and non-cultivated land along highways. When using, the dosage is 200-300 mL per acre, diluted in 30 kg of water and sprayed evenly on the leaves. Target weeds include annual and perennial weeds such as ryegrass, Kentucky bluegrass, alfalfa, white clover, goosegrass, foxtail grass, purslane, cocklebur, reeds, fleabane, and knotweed.

[0017] Beneficial technical effects This invention relates to a 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant. This synergistic system utilizes a binary, tea-free saponin-free plant-derived compound synergistic system of wintergreen extract and rosemary essential oil. This synergistic system has the following advantages: 1. Holly extract is rich in natural holly glycosides, which are low-foaming natural amphiphilic substances. It can significantly reduce the surface tension of the pesticide solution, spread quickly on the leaves of weeds after spraying, absorb and retain the pesticide, and reduce the rolling and loss of the pesticide solution. Unlike tea saponin, it produces almost no foam and is suitable for various spraying equipment. 2. The α-pinene and oxalic acid components in rosemary essential oil can dissolve and destroy the waxy layer and cuticle barrier of the weed epidermis, forming a penetration channel for the herbicide and accelerating the entry of glufosinate into the thin-walled cells of the weed across the epidermis. 3. When holly extract is combined with rosemary essential oil, a composite interface film is formed, which enhances the conduction speed of the agent in the plant, allowing it to quickly reach the root system and reduce the probability of perennial weeds turning green again. 4. Both wintergreen extract and rosemary essential oil are natural plant extracts that are easily and completely degraded by soil microorganisms, leaving no residue or secondary pollution. They are safe for bees, earthworms, and other beneficial organisms in the environment. 5. The compound plant-derived adjuvants have excellent miscibility, do not cause foaming or precipitation problems, optimize the interfacial compatibility of the system, reduce the hydrolysis of active ingredients, and improve the stability of the formulation under cold and hot storage. Detailed Implementation

[0018] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0019] The specific sources of the chemical substances used in the examples are as follows: Glufosinate-ammonium salt: actual purity 91.4wt%, Wuhan Pushida Biotechnology Co., Ltd.

[0020] Wintergreen extract: This invention is prepared in-house, and the specific method is described in the invention content section.

[0021] Rosemary essential oil: This invention is prepared in-house, and the specific method is described in the invention content section.

[0022] Ethylene glycol: Jinan Kosmai New Materials Co., Ltd.

[0023] C8-C10 fatty alcohol polyoxyethylene ether: Jiangsu Haian Petrochemical Plant, model number E1003.

[0024] Sodium bisulfite: Nantong Runfeng Petrochemical Co., Ltd.

[0025] Glacial acetic acid: Nanjing Zhongchun Biotechnology Co., Ltd.

[0026] Carrageenan: purity 99wt%, Shandong Fengtai Biotechnology Co., Ltd., model FT11.

[0027] Synergen ME adjuvant: Synergen from Clariant TM A series of additives, model number Synergen ME.

[0028] Isomer C13 fatty alcohol polyoxyethylene ether MULTISO 13-100: Sasol's MULTISO series product, model MULTISO 13-100.

[0029] Fatty alcohol polyoxyethylene ether phosphate monoester: Chenrun Chemical, model number ODP.

[0030] SAG 1572 defoamer: Momentive Advanced Materials, Inc., USA, model SAG 1572.

[0031] I. Formulation Examples Example 1 A 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, wintergreen extract 3.2%, rosemary essential oil 1.1%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water to make up to 100%.

[0032] The preparation method is as follows: Step 1: Weigh each component according to its weight percentage and set aside.

[0033] Step 2: At 25°C and a stirring speed of 400 r / min, add metered deionized water to the stirred tank, add glufosinate-ammonium salt technical material, and continue stirring for 20 min until the solid is completely dissolved to obtain a transparent active mother liquor. Step 3: Add the cosolvent, penetration enhancer, and hydrolysis stabilizer to the mother liquor in sequence, and stir for 10 minutes to mix evenly; Step 4: Slowly drip the pre-mixed wintergreen extract and rosemary essential oil complex plant-derived synergist into the system and stir continuously for 15 minutes until the system is homogeneous and transparent. Step 5: Add pH buffer to adjust the pH of the system to 6.5, and keep warm and stir for 20 minutes; Step 6: Let stand naturally for 30 minutes to defoam, then filter with a 200-mesh filter to remove trace impurities. After testing the effective ingredients and stability, fill the solution to obtain the finished soluble liquid.

[0034] Example 2 A 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, wintergreen extract 4.6%, rosemary essential oil 2.3%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water to make up to 100%.

[0035] The preparation method is the same as in Example 1.

[0036] Example 3 A 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, wintergreen extract 4%, rosemary essential oil 1%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water to make up to 100%.

[0037] The preparation method is the same as in Example 1.

[0038] Comparative Example 1 A 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, holly extract 4.3%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water to make up to 100%.

[0039] The preparation method is the same as in Example 1.

[0040] Comparative Example 2 A 10% glufosinate-ammonium salt soluble concentrate containing a compound plant-derived synergistic adjuvant, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, rosemary essential oil 4.3%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water to make up to 100%.

[0041] The preparation method is the same as in Example 1.

[0042] Comparative Example 3 A 10wt% glufosinate-ammonium salt soluble concentrate, wherein the mass percentage of each component in the formulation is as follows: glufosinate-ammonium salt 10.94%, Synergen ME adjuvant 6%, isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100 8%, SAG 1572 defoamer 0.2%, composite fatty alcohol polyoxyethylene ether phosphate monoester 70%, 10wt% hydrochloric acid 0.1%, and deionized water to make up to 100%.

[0043] The preparation method is as follows: Weigh 109.4g of glufosinate-ammonium salt, 60g of Synergen ME adjuvant, 80g of isomeric C13 fatty alcohol polyoxyethylene ether MULTISO 13-100, and 2g of SAG 1572 defoamer, and add them to 700g of composite fatty alcohol polyoxyethylene ether phosphate monoester solution. Stir at room temperature for 30 minutes, add 10wt% hydrochloric acid to adjust the pH to 7.5, add water to make up to 1000g, and continue stirring for 15 minutes until clear and transparent. After testing and filling, the glufosinate-ammonium salt soluble concentrate is obtained.

[0044] II. Application Test Cases 2.1 Surface tension and contact angle tests In the following examples and comparative examples, the surface tension of the pesticide solution was measured using a surface tension meter. Only when the surface tension of the pesticide solution is lower than the surface free energy of the target crop can the pesticide solution wet and spread on the target surface.

[0045] In the following examples and comparative examples, the liquid-solid interface contact angle was measured: a contact angle meter was used to measure the contact angle formed when the pesticide droplet landed on the target crop. When the liquid and solid come into contact, the free energy of the system decreases. The amount of decrease in free energy reflects the degree of wetting of the liquid on the target crop. The smaller the contact angle, the stronger the wetting ability of the selected target, the better the spreadability of the pesticide on the target crop, and the higher the pesticide utilization rate.

[0046] Take 1 gram of each sample from the examples and comparative examples, and then dilute them with water by 300 times, 500 times, 1000 times and 1500 times respectively. Measure the surface tension value of each dilution, and drop the dilution onto the leaves of alfalfa plants to measure the contact angle. The results are shown in Table 1.

[0047] Table 1. Test results of surface tension and contact angle of each agent.

[0048] Conclusion: The data above show that the surface tension and contact angle of Example 1 (a blend of wintergreen extract and rosemary essential oil) were significantly lower than those of the comparative examples at all dilution ratios, and the advantage became more pronounced with increasing dilution ratio. Under the same total active ingredient content (4.3%), the wetting performance of the blended system (3.2% + 1.1%) was far superior to that of the single plant-derived components (Comparative Examples 1 and 2), indicating a significant synergistic effect. At high dilutions (e.g., 1500×), the contact angle of Example 1 only increased slightly, while the comparative examples deteriorated sharply, proving its low critical micelle concentration, making it more suitable for low-concentration application in the field. All indicators of Example 1 are superior to those of the traditional chemical adjuvant system (Comparative Example 3), combining environmental friendliness and high efficiency. It is evident that the formulation system of this invention can significantly reduce the surface tension of the drug solution and significantly improve the wetting and spreading ability of droplets on the target leaf surface. It is especially suitable for application scenarios with reduced dosage and enhanced efficacy under high dilution. Its comprehensive performance is superior to single plant-derived adjuvants and traditional chemical adjuvants, and it has significant application prospects for reduced dosage and enhanced efficacy.

[0049] 2.2 Field efficacy trials To clarify the final effect of adding adjuvants that reduce the surface tension of pesticide liquid formulations to pesticide formulations, a field efficacy test for weed control in orchards was conducted in Taoyuan Base, Shexian County, Anhui Province in June 2026. The test was conducted in accordance with the GB / T17980-2000 guidelines for field efficacy tests of pesticides.

[0050] 2.2.1 Test reagents Control agents: Example 1, Comparative Examples 1-3 and water control.

[0051] 2.2.2 Test subjects The orchard was severely infested with ryegrass, Kentucky bluegrass, alfalfa, and white clover. Barnyard grass, goosegrass, crabgrass, foxtail grass, and knotweed were also present. The perennial broadleaf weed, fleabane, was sporadically present. At the time of application, weed coverage in each treatment plot was over 95%, with plant height ranging from 25-55 cm.

[0052] 2.2.3 Experimental Design The experiment included four treatments, each with a control group (CK). Each plot was 30 square meters in size and replicated four times. The plots for different treatments were arranged in a completely randomized block design.

[0053] The comparative and example samples were diluted and sprayed at the same dilution ratio, with a formulation dosage of 150 mL / mu and a spray volume of 30 L / mu. 2.2.4 Survey methods and efficacy evaluation methods The control effect of each treatment was investigated 10 days and 30 days after application. A 5-point sampling method was used, with each point covering 0.5 square meters. The type, number of plants, and fresh weight of weeds were recorded, and the weed control effect was calculated.

[0054] Formula for calculating prevention and control effect: Control efficacy (%) = (Number of weeds in control group - Number of weeds in treatment group) / Number of weeds in control group × 100% Fresh weight control efficacy (%) = (fresh weight of weeds in control group - fresh weight of weeds in treatment group) / fresh weight of weeds in control group × 100%.

[0055] The control group refers to the blank control with water, and the treatment group refers to the area treated with the above-mentioned test reagents.

[0056] Table 2 Results of field efficacy trials for each treatment 10 days after application.

[0057] Table 3. Results of field efficacy trials for each treatment 30 days after application.

[0058] Total weeds refer to all weeds within the surveyed area.

[0059] Conclusion: Based on the weed control efficacy data at 10 and 30 days post-application, Example 1 showed significantly superior efficacy compared to the three comparative examples at all time points, against different weed species, and in terms of both plant control efficacy and fresh weight control efficacy. This advantage continued to increase over time. At 10 days post-application, Example 1 achieved a plant control efficacy of 86.5% and a fresh weight control efficacy of 86.8% against total weeds, while the plant control efficacy of Comparative Examples 1 to 3 ranged only from 76.0% to 79.7%, and the fresh weight control efficacy ranged only from 78.3% to 80.4%, a difference of approximately 7 to 10 percentage points. At 30 days post-application, the plant control efficacy of Example 1 increased to 92.8%, and the fresh weight control efficacy reached a high of 95.4%, while the fresh weight control efficacy of the comparative examples remained at around 81% to 82%. This means that Example 1's fresh weight control efficacy at 30 days was nearly 13 percentage points higher than that of Comparative Example 3. The fresh weight control efficacy of Example 1 increased by nearly 9 percentage points from 10 days to 30 days, while the increase in the comparative examples was generally only 2 to 3 percentage points. This fully demonstrates that the compound adjuvant not only improved the initial rapid effect, but more importantly, significantly enhanced the residual effect of the agent, and could effectively inhibit the regeneration and fresh weight accumulation of weeds.

[0060] In terms of efficacy against different target weeds, Example 1 showed very balanced performance against ryegrass and alfalfa, with fresh weight control efficacy of 90.8% and 92.3% respectively 30 days after application, showing no selectivity bias. This indicates that the adjuvant system has a good absorption-promoting effect on both grasses and broadleaf weeds, demonstrating excellent broad-spectrum efficacy. Comparative Example 1 (containing only holly extract) and Comparative Example 2 (containing only rosemary essential oil) showed similar values ​​in various efficacy metrics, such as 81.3% and 81.0% of total fresh weight control efficacy at 30 days, essentially at the same level, but both were significantly lower than that of Example 1, which combined the two. Since the total amount of plant-derived adjuvants added in Example 1 and the two comparative examples was the same, this indicates a synergistic effect between holly extract and rosemary essential oil, and the combined use of these two adjuvants resulted in a herbicidal activity enhancement that is incomparable to that of a single component. In addition, Comparative Example 3 uses a traditional chemical adjuvant system, and its 30-day total weed fresh weight control efficacy is 82.6%, which is slightly better than that of a single plant-derived adjuvant, but still significantly lower than that of Example 1 (95.4%). This indicates that the compound plant-derived adjuvant not only has advantages in terms of environmental protection, but also surpasses conventional chemical adjuvants in actual weed control effect.

[0061] Furthermore, when the above field efficacy results are correlated with the measured surface tension and contact angle data of the formulation, Example 1 exhibited the lowest surface tension and smallest contact angle at all dilution ratios. This means that the herbicide solution has optimal spreadability and wettability on weed leaves, forming a more uniform herbicide film and more effectively penetrating the leaf cuticle to enter the plant. It is precisely this excellent physical property that provides the foundation for the full absorption and rapid translocation of glufosinate-ammonium salt, thereby translating into higher control efficacy per plant and fresh weight in the field.

[0062] In summary, the compound plant-derived synergistic adjuvant system, formulated with holly extract and rosemary essential oil at a ratio of 3.2% and 1.1%, synergistically reduces surface tension and enhances leaf adhesion and penetration, maximizing the herbicidal activity of glufosinate-ammonium salts while maintaining both rapid and sustained effects. It demonstrates excellent performance against both grasses and broadleaf weeds. At the same dosage of active ingredients, this formulation significantly outperforms single plant-derived adjuvants and traditional chemical adjuvants, making it a highly valuable, dosage-reduced, and synergistic adjuvant solution for widespread application.

Claims

1. A soluble form of glufosinate-ammonium salt containing a compound plant-derived synergistic adjuvant, characterized in that, It is composed of the following components by mass percentage: 5-20% glufosinate-ammonium technical grade; 2.5-7.0% compound plant-derived synergistic adjuvant; 3.0-9.0% solubilizer; 1.0-3.5% penetration enhancer; 0.2-1.2% hydrolysis stabilizer; 0.1-0.6% pH buffer; the balance is deionized water; the total mass fraction of all components is 100%.

2. The soluble form of glufosinate-ammonium salt containing a compound plant-derived synergist according to claim 1, characterized in that: The compound plant-derived synergist is composed of holly extract and rosemary essential oil in a mass ratio of 2:1 to 4:1; the holly extract has an active ingredient content of ≥90%, and the rosemary essential oil has a total terpenes + phenolic active ingredients content of ≥85%.

3. The soluble form of glufosinate-ammonium salt containing a compound plant-derived synergist according to claim 1, characterized in that: The co-solvent is one or more of propylene glycol, ethylene glycol, and propylene glycol methyl ether; the penetration aid is C8-C10 fatty alcohol polyoxyethylene ether; the hydrolysis stabilizer is either sodium benzoate or sodium bisulfite; the pH buffer adjuster is glacial acetic acid or dilute ammonia to adjust the pH of the preparation to 5.0-6.

8.

4. The soluble form of glufosinate-ammonium salt containing a compound plant-derived synergist according to claim 1, characterized in that, The mass percentages of each component in the soluble liquid are as follows: glufosinate-ammonium salt 10.94%, wintergreen extract 3.2%, rosemary essential oil 1.1%, ethylene glycol 5.5%, C8-10 fatty alcohol polyoxyethylene ether 2.2%, sodium benzoate 0.6%, glacial acetic acid 0.25%, and deionized water 66.55%.

5. The method for preparing the soluble form of glufosinate-ammonium salt containing a compound plant-derived synergist as described in any one of claims 1 to 4, characterized in that, Includes the following steps: Step 1: At room temperature (20-30℃) and stirring speed (300-500 r / min), add metered deionized water to the stirred tank, add glufosinate-ammonium salt technical material, and stir continuously for 15-20 min until the solid is completely dissolved to obtain a transparent active mother liquor. Step 2: Add the cosolvent, penetration enhancer, and hydrolysis stabilizer to the mother liquor in sequence, and stir for 10 minutes to mix evenly; Step 3: Slowly drip the pre-mixed wintergreen extract and rosemary essential oil complex plant-derived synergist into the system and stir continuously for 15 minutes until the system is homogeneous and transparent. Step 4: Add pH buffer to adjust the pH of the system to 5.0-6.8, and keep warm and stir for 20 minutes; Step 5: Let stand naturally for 25-35 minutes to defoam, then filter with a 200-mesh filter to remove trace impurities. After testing the effective ingredients and stability, fill the solution to obtain the finished soluble liquid.

6. The preparation method according to claim 5, characterized in that: The entire process requires no heating or high-temperature reaction steps, and the production environment is at normal pressure and temperature.

7. The application of the soluble agent according to claim 1 in weed control in orchards, tea gardens, wastelands, and non-cultivated land along highways, characterized in that: The dosage of the preparation is 200-300 mL per mu, diluted with 30 kg of water and sprayed evenly on the leaves. The target pests include ryegrass, Kentucky bluegrass, alfalfa, white clover, goosegrass, foxtail grass, purslane, cocklebur, reeds, fleabane, and knotweed.

Citation Information

Patent Citations

  • A method for extracting rosemary essential oil and antioxidants from rosemary

    CN107686773B