Ultra-low volume liquid formulations containing sodium p-chlorophenoxyacetic acid, process for their preparation and use

Abstract

The present application relates to the technical field of pesticide preparation, in particular to a super low volume liquid preparation containing sodium p-chlorophenoxyacetic acid, a preparation method and application. The components are as follows in mass percentage: 0.01-1% of sodium p-chlorophenoxyacetic acid, 3-5% of plant small molecule signal peptide, 1-5% of organic silicon, 3-10% of nano silicon dioxide, 30-50% of ethylene glycol, 10-20% of nutrient elements, and water to make up to 100%. The organic silicon component includes at least one polyether modified polysiloxane and at least one polyether compound. The super low volume preparation containing sodium p-chlorophenoxyacetic acid has good stability, strong anti-evaporation and sedimentation capacity, and can improve the absorption and utilization rate of the plant surface. When applied to crops, it can promote yield increase, has higher efficiency than conventional soluble liquid preparation, and has better yield increase effect.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of pesticide preparation, in particular to a super low volume liquid agent containing sodium p-chlorophenoxyacetic acid, a preparation method and application. BACKGROUND

[0002] Pesticide super low volume spraying technology is a pesticide application technology with extremely low liquid application amount per unit area. The pesticide application amount per mu for field crops is usually less than 0.3 liters, which is suitable for use in water-deficient and inconvenient water-fetching areas. The technology uses drift and cumulative spraying, which is several tens of times more efficient than conventional targeted spraying. It is a major technical innovation to adapt to modern agricultural production, improve pesticide efficacy and work efficiency, and reduce pesticide use and environmental pollution. With the continuous advancement of agricultural scale and modernization in China, unmanned aerial vehicle (UAV) spraying technology is rapidly developing and being popularized in China, and the demand for pesticide products in the form of super low volume liquid agent is increasing.

[0003] However, the super low volume liquid agent has certain limitations: 1. The super low volume spraying has high dispersity, and the formed droplets have a small particle size, generally 50-100 μm, are easy to drift, have a large surface area, and have a high evaporation rate. Therefore, a solvent with low volatility must be selected. Commonly used solvents include isopropyl alcohol, dimethylbenzene, cyclohexanone, solvent oil, naphtha, solvent naphtha, power kerosene, dimethylformamide, isophorone, and hexamethyl phosphoramide. Although the super low volume liquid agent prepared from such solvents has a small unit area usage amount, it still pollutes the environment, especially in high-temperature weather, and poses a safety risk to crops and users; 2. The pesticide preparations for super low volume use in China are still developed, detected, standardized, and managed according to ordinary spraying methods. The registered pesticide preparations are used in the form of super low volume liquid agent after dilution. The diluted pesticide solution may have precipitation, crystallization, and flocculation, and the UAV nozzle is easy to be blocked, resulting in failure of the UAV spraying equipment to work normally.

[0004] Sodium p-chlorophenoxyacetate is a phenoxyacetic acid compound with a molecular formula of C8H6ClNaO3 and a relative molecular mass of 208.6. The pure product is usually colorless crystals, and the technical product is white crystals with a slight phenolic odor. It is mainly used as an auxin plant growth regulator to regulate the growth of crops such as tomatoes and lychees, and has the effects of preventing flower and fruit drop, improving fruit setting rate, accelerating the growth and development of young fruits, and increasing yield. However, sodium p-chlorophenoxyacetate is an ionic crystal. According to the principle of similarity of shape, non-polar solvents cannot overcome the ionic bond effect, and the hydrophobic part is not enough to drive the dissolution of sodium p-chlorophenoxyacetate. Therefore, it is difficult to prepare a traditional super low volume liquid agent from sodium p-chlorophenoxyacetate.

[0005] The sodium p-chlorophenoxyacetate is easily soluble in water, but water has high volatility, especially in high temperature, dry or windy environment, the tiny mist droplets (usually less than 50 microns in diameter) can evaporate quickly before reaching the target surface, resulting in loss of active ingredients; and water has poor wettability and adhesion to hydrophobic surfaces, which can cause liquid loss, reduce the deposition efficiency of the pesticide on the target, and affect the control effect; in low temperature environment (such as winter or high altitude area), water-based spray may freeze, clog the nozzle or damage the equipment; water-based mist droplets are easily affected by wind and drift, which can cause pollution to non-target areas (such as adjacent crops, water sources), and increase the ecological and pesticide damage risk.

[0006] Therefore, based on the contradiction between the sodium p-chlorophenoxyacetate and the properties of the traditional ultra-low volume liquid, it is difficult to prepare a stable ultra-low volume liquid although there is a wide demand for agricultural application. SUMMARY

[0007] The present application provides an ultra-low volume liquid containing sodium p-chlorophenoxyacetate, a preparation method and application to solve the defects in the prior art. Through a large number of experiments and formula research, the present application has prepared an ultra-low volume liquid containing sodium p-chlorophenoxyacetate with good stability, strong anti-evaporation performance and deposition capacity, and improved absorption and utilization rate on the plant surface. The application of the ultra-low volume liquid containing sodium p-chlorophenoxyacetate in crops can promote yield increase, and has higher efficiency and better yield increase effect than conventional soluble liquid.

[0008] To achieve the above-mentioned purpose, the present application adopts the following technical solutions:

[0009] In a first aspect, the present application provides an ultra-low volume liquid containing sodium p-chlorophenoxyacetate, the components of which are as follows in mass percentage: 0.01-1% of sodium p-chlorophenoxyacetate, 3-5% of plant small molecule signal peptide, 1-5% of silicone, 3-10% of nano-silicon dioxide, 30-50% of ethylene glycol, 10-20% of nutrient elements, and water to make up to 100%; the silicone component includes at least one polyether modified polysiloxane and at least one polyether compound.

[0010] Preferably, the plant small molecule signal peptide is selected from one or more of RALF (Rapid Alkalinization Factor), CIF (Casparian strip Integrity Factor), EPF (Epidermal Patterning Factor), EPFL (Epidermal Patterning Factor Like), PEP (Plant Elicitor Peptide), and yeast peptide containing amino acids.

[0011] Preferably, the plant small molecule signal peptide is a yeast peptide containing amino acids, and the mass ratio of the amino acids to the yeast peptide is 3:17.

[0012] Preferably, the organosilicon is a combination of a polyether-modified silicone oil and a polyether.

[0013] Preferably, the mass ratio of the polyether-modified silicone oil to the polyether is 2:1.

[0014] Preferably, the nano-silicon dioxide has a particle size of 100-200 nm.

[0015] Preferably, the nutrient element contains boron and zinc.

[0016] Preferably, the mass ratio of the boron-containing nutrient element to the zinc-containing nutrient element is (1-2):1.

[0017] In some embodiments of the present application, the mass fraction of the sodium p-chlorophenoxyacetic acid in the ultra-low volume liquid is any one or a value between any two of 0.01%, 0.05%, 0.1%, 0.5%, and 1.0%; and the mass fraction of the nano-silicon dioxide in the ultra-low volume liquid is any one or a value between any two of 3%, 5%, and 10%.

[0018] In a second aspect, the present application provides a preparation method of the ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid, which comprises: dissolving sodium p-chlorophenoxyacetic acid in water, heating, dissolving nutrient elements and plant small molecule signal peptides, and then adding ethylene glycol, organosilicon, and nano-silicon dioxide to obtain a mixture.

[0019] In a third aspect, the present application provides an application of the ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid in promoting crop yield.

[0020] Preferably, the crop is any one of wheat and rice.

[0021] Preferably, the application is to promote crop spike differentiation, increase the number of grains per spike, and increase the thousand-grain weight.

[0022] Preferably, the effective component dosage of the ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid is 0.04-0.1 g / acre. In some embodiments of the present application, the effective component dosage of the ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid is any one or a value between any two of 0.04 g / acre, 0.05 g / acre, 0.08 g / acre, and 0.1 g / acre.

[0023] The present application has the following beneficial effects:

[0024] In order to overcome the contradiction between sodium p-chlorophenoxyacetic acid and the traditional ultra-low volume liquid properties, and to prepare an ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid with excellent performance, the present application creatively found that the sodium p-chlorophenoxyacetic acid, plant small molecule signal peptide, organic silicon, nano silicon dioxide, ethylene glycol, nutrient elements and water as components can be prepared into an ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid with good stability, strong anti-evaporation and anti-drift ability, and can improve the absorption and utilization rate of the plant surface. The application of the ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid in crops can promote yield increase, and the efficiency is higher than that of the conventional soluble liquid, and the yield increase effect is better. The above components interact with each other, and have a profound synergistic effect on the efficiency, stability and mode of action of the whole ultra-low volume liquid system, and the components act as follows:

[0025] Plant small molecule signal peptide: sodium p-chlorophenoxyacetic acid is a synthetic growth regulator, which mainly regulates the endogenous hormone level of plants by external application, and the addition of plant small molecule signal peptide can act as a signal molecule, which is recognized and combined by the cytoplasmic membrane receptor kinase at a very low concentration, opens the downstream signal transduction pathway, mediates the intercellular, intertissue and interorgan communication, thereby regulates the plant growth, development and stress response, so that the same or even better effect can be achieved at a lower concentration of sodium p-chlorophenoxyacetic acid, and the amount of chemical pesticides is reduced; in addition, the ultra-low volume liquid droplets are very fine, mainly adhering to the leaf surface, and need effective penetration and conduction, and the small peptide has strong affinity and penetration, can quickly enter the plant body, promote and accelerate the stem thickening and leaf expansion, and improve the photosynthesis area; and due to the presence of organic silicon and nano silicon dioxide in the system, the stability problem of the peptide material is effectively solved, and the efficient delivery and leaf penetration of the active ingredient are ensured.

[0026] Organic silicon: the organic silicon of the component has good hydrolysis resistance, which meets the long-term storage stability requirement of the ultra-low volume liquid; and the organic silicon has a low surface tension, which can greatly reduce the static and dynamic surface tension of the liquid, so that it is much lower than the critical surface tension of the plant leaf surface, so that the very fine droplets can quickly wet the hydrophobic leaf surface, immediately spread to form a liquid film, reduce the rebound, significantly improve the settling rate and effective adhesion amount of the liquid, and lay a foundation for subsequent absorption.

[0027] Nano-silica: The core role of nano-silica in the system is its unique nano effect and interface characteristics. First, with its high specific surface area, mesoporous structure and abundant surface hydroxyl groups, nano-silica can efficiently load sodium p-chlorophenoxyacetic acid and plant small molecule signal peptide through physical adsorption (van der Waals force) and hydrogen bond chemical action to form a stable complex. This structure not only effectively protects the active ingredients from hydrolytic degradation, but also realizes the controlled release of the drug through interface interaction, prolonging the effective period; secondly, the polyether modified polysiloxane in organosilicon can be anchored on the surface of nano-silica particles, which can inhibit the spontaneous agglomeration of nano-particles through steric hindrance effect, ensuring its uniform dispersion in the preparation, and fully exerting the function of nano-carrier; in addition, nano-silica significantly enhances the deposition and adhesion performance of the drug solution on the leaf surface, its small particle size (<100 nm) and surface properties can improve the adhesion of fog droplets on the plant wax layer, reduce the loss of rainwater washing; at the same time, the small size effect helps the active ingredients to penetrate the plant stomata or epidermal barrier, thereby significantly improving the permeability and bioavailability of the drug.

[0028] Ethylene glycol: As a component with a high mass percentage in the formula, ethylene glycol constitutes the base solvent of the system, responsible for dissolving sodium p-chlorophenoxyacetic acid, plant small molecule signal peptide and other water-soluble nutrients, ensuring the sufficient dissolution and long-term chemical stability of these polar or ionic components, preventing precipitation, crystallization and drug efficacy decline due to poor solubility. The polyether segment in the combination of ethylene glycol and organosilicon has good compatibility, as a bridge, it reconciles the contradiction between the hydrophobic part of organosilicon and water, ensuring the formation of a uniform and stable solution system environment, solving the problem of traditional oil-based ultra-low volume liquid solvent that cannot dissolve polar pesticides and biological agents, and the high risk of phytotoxicity; in addition, ethylene glycol is a solvent with high boiling point, low vapor pressure and low volatility, which can effectively inhibit the rapid evaporation of water in the fog droplets during spraying, stabilize the ultra-low volume spray particle size, thereby greatly reducing the drift loss of fog droplets and improving the adhesion per unit area; moreover, ethylene glycol itself has a certain permeability, which can assist the organosilicon component to wet the plant leaf wax layer, creating favorable conditions for the subsequent penetration and absorption of sodium p-chlorophenoxyacetic acid and signal peptide, and providing a suitable dispersion medium for nano-silica particles, its viscosity helps to slow down the settling rate of nano-particles, and cooperates with organosilicon to maintain the state of nano-silica.

[0029] Nutritional elements: Nutritional supplement elements commonly used for crops during flowering and fruiting period, used in conjunction with spraying to promote pollen germination, improve seed setting rate and enhance the stress resistance of crops; the sodium p-chlorophenoxyacetic acid ultra-low volume liquid of the present invention integrates the nutritional elements such as boron and zinc required during the jointing and booting stage and the flowering stage of wheat, which can reduce the number of pesticide applications and save manpower and resources. BRIEF DESCRIPTION OF DRAWINGS

[0030] Figure 1 Schematic diagram for water-sensitive paper setting during the deposition amount test process of effect example 3;

[0031] Figure 2 Schematic diagram for pesticide spraying process during the deposition amount test process of effect example 3;

[0032] Figure 3 Photo diagram for the deposition amount test process of effect example 3. DETAILED DESCRIPTION

[0033] In order for those skilled in the art to better understand the technical solutions of the application, the application will be further described in detail below with reference to the specific embodiments.

[0034] The medicines used in the following examples and sources are as follows:

[0035] Sodium parachlorophenoxyacetate, content 97%, provided by Sichuan Runer Technology Co., Ltd.;

[0036] Yeast peptide containing amino acids (YYP), amino acid content 15%, yeast peptide content 85%, yeast peptide containing amino acids hydrolyzed amino acid content ≥85%, molecular weight 180-1000 accounting for >85%, provided by Shenzhen Leyeisheng Ecological Technology Co., Ltd.;

[0037] Organic silicon TIS358, containing polyether modified silicone oil 60%, CAS No: 67674-67-3, molecular formula C7H 22 O2Si3, molecular weight 222.505, surface tension 20.0-23.0 mN / m; containing polyether 30%, CAS No: 27274-31-3; provided by Jiangxi Tian Sheng New Material Co., Ltd.;

[0038] Nano silicon dioxide, particle size 100-200 nm, molecular weight: ~20 million, viscosity (20℃): 150-200 mPa·s (cP), pH value: 6.5, provided by Shanghai Tongjiang Chemical Co., Ltd.;

[0039] Ethylene glycol, content 100%, provided by Chengdu Chengzheng Chemical Co., Ltd.;

[0040] Sodium polyborate, content 99.8%, provided by Sichuan Runer Technology Co., Ltd.;

[0041] EDTA-zinc, content 99%, provided by Sichuan Runer Technology Co., Ltd.;

[0042] Cocamide propyl betaine (CAB35), solid content 35%, pH value 5.5-7.5, provided by Chengdu Ke Hongda Technology Co., Ltd.

[0043] Example 1-5 sodium parachlorophenoxyacetate ultra-low volume liquid

[0044] The formula of each component of the sodium p-chlorophenoxyacetic acid ultra-low volume liquid is shown in Table 1.

[0045] Table 1. Formula composition of sodium p-chlorophenoxyacetic acid ultra-low volume liquid

[0046]

[0047] The preparation method of the sodium p-chlorophenoxyacetic acid ultra-low volume liquid of Examples 1-5 and Comparative Examples 1-3 is as follows:

[0048] According to the proportioning of Table 1, each raw material is weighed, and pure water is added to a preparation kettle containing sodium p-chlorophenoxyacetate. The kettle is heated to 70°C, and sodium polyborate, EDTA-zinc, and YPP are added in sequence and stirred to dissolve. After the solid materials are completely dissolved, ethylene glycol, silicone TIS358, and nano-silicon dioxide are added, and the mixture is stirred and mixed uniformly. The temperature is lowered to room temperature, and the mixture is filtered using 200-mesh filter cloth to obtain the product.

[0049] Comparative Example 4: 1% sodium p-chlorophenoxyacetate soluble concentrate

[0050] The formula of the 1% sodium p-chlorophenoxyacetate soluble concentrate is shown in Table 2.

[0051] Table 2. Formula composition of 1% sodium p-chlorophenoxyacetate soluble concentrate

[0052]

[0053] The preparation method of the 1% sodium p-chlorophenoxyacetate soluble concentrate described in Comparative Example 4 is as follows:

[0054] After dissolving sodium p-chlorophenoxyacetate in pure water, ethylene glycol and CAB35 are added and stirred uniformly to obtain the product.

[0055] Effect Example 1: Quality index and stability test

[0056] Referring to the "Pesticide Ultra-Low Volume Liquid Product Standard Writing Specification" (HG / T 2467.20-2003) and the "Pesticide Ambient Temperature Storage Stability Test General Rules" (NY / T 1427-2016), the products of the examples and comparative examples are subjected to quality index detection and stability test, and the detection results are shown in Tables 3-11:

[0057] Table 3. Quality index and preparation stability test detection results of Example 1 ultra-low volume liquid

[0058]

[0059] Table 4. Quality index and preparation stability test detection results of Example 2 ultra-low volume liquid

[0060]

[0061] Table 5. Quality indicators and test results of the preparation stability test of the ultra-low volume liquid of Example 3

[0062]

[0063] Table 6. Quality indicators and test results of the preparation stability test of the ultra-low volume liquid of Example 4

[0064]

[0065] Table 7. Quality indicators and test results of the preparation stability test of the ultra-low volume liquid of Example 5

[0066]

[0067] Table 8. Quality indicators and test results of the preparation stability test of the sodium p-chlorophenoxyacetate ultra-low volume liquid of Comparative Example 1

[0068]

[0069] Table 9. Quality indicators and test results of the preparation stability test of the sodium p-chlorophenoxyacetate ultra-low volume liquid of Comparative Example 2

[0070]

[0071] Table 10. Quality indicators and test results of the preparation stability test of the sodium p-chlorophenoxyacetate ultra-low volume liquid of Comparative Example 3

[0072]

[0073] Table 11. Quality indicators and test results of the preparation stability test of the sodium p-chlorophenoxyacetate soluble liquid of Comparative Example 4

[0074]

[0075] From the analysis of the quality indicator test data in Tables 3-11, the quality stability of the sodium p-chlorophenoxyacetate ultra-low volume liquid prepared in the examples is excellent after 2 years of storage at room temperature; if the plant small molecule signal peptide, ethylene glycol, and nano-silicon dioxide are missing from the formulation of the ultra-low volume liquid, the decomposition rate of the preparation will be affected to varying degrees; the 2-year storage decomposition rate of the sodium p-chlorophenoxyacetate soluble liquid of Comparative Example 4 is >5%, the surface tension value is large (greater than 50 mN / m), and the surface tension value increases with longer storage time, indicating that the wetting and adhesion effect of the formulation on the surface of the crop is poor.

[0076] Effect Example 2 Anti-evaporation rate test (filter paper hanging method)

[0077] Experimental method: qualitative filter paper with copper wire ring, diameter 11 cm, pre-weighed, recorded as m0, 0.8-1.0 ml of drug solution was taken with a syringe, evenly dropped on the qualitative filter paper, so that the filtrate was completely wet, immediately weighed, that is, m1, hung in a constant temperature box at 30℃±1℃, 20 min later, weighed again, recorded as m2, all the weight of the pre-copper wire ring was removed, the volatile rate of the drug solution was calculated.

[0078] Data analysis: according to the calculated volatile rate of the drug solution, the volatile rate greater than 30% is strong, 10-30% is medium, and less than 10% is weak. That is, the anti-evaporation rate <70% is weak, 70%-90% is medium, and >90% is strong. Set up 9 groups of parallel samples, and take the average value as the anti-evaporation rate.

[0079] Volatile rate = 1-(m2-m0) / (m1-m0)*100%, anti-evaporation rate = 1-volatile rate.

[0080] The anti-evaporation rate test was carried out on example 2 and example 3 and comparative examples 1-4, and the results are shown in tables 12-17:

[0081] Table 12. Anti-evaporation rate test results of example 2

[0082]

[0083] Table 13. Anti-evaporation rate test results of example 3

[0084]

[0085] Table 14. Anti-evaporation rate test results of comparative example 1

[0086]

[0087] Table 15. Anti-evaporation rate test results of comparative example 2

[0088]

[0089] Table 16. Anti-evaporation rate test results of comparative example 3

[0090]

[0091] Table 17. Anti-evaporation rate test results of comparative example 4

[0092]

[0093] From Table 12 to Table 17, it can be seen that the average anti-evaporation rate of the ultra-low volume liquid agent obtained by the embodiment of the application can be as high as 95% or more, and the anti-evaporation capacity is strong; if the plant small molecule signal peptide, ethylene glycol, nano-silicon dioxide and other components are missing in the formula of the ultra-low volume liquid agent, the anti-evaporation capacity of the preparation will be weakened to different degrees; the anti-evaporation capacity of the soluble liquid agent prepared in Comparative Example 4 is weak, far lower than that of the ultra-low volume liquid agent of the application.

[0094] Effect Example 3 deposition amount test

[0095] The pesticide deposition amount refers to the amount of pesticide deposited on a unit area of the target after application, and the unit of measurement is μl / cm², which is a core evaluation parameter of pesticide application effect. The value thereof reflects the effective utilization rate of pesticide in the application process, and is affected by factors such as surface tension of the target, leaf angle, spray distance and the like.

[0096] Test agent:

[0097] Treatment 1, water control;

[0098] Treatment 2, 1% sodium p-chlorophenoxyacetic acid soluble liquid agent (Comparative Example 4), according to the low volume spraying standard, the amount of pesticide per mu is 20 ml, and water is added to 100 ml, diluted 5 times;

[0099] Treatment 3, 0.05% ultra-low volume liquid agent (Example 2), according to the ultra-low volume spraying, the amount of pesticide per mu is 100 ml;

[0100] Treatment 4, 1% ultra-low volume liquid agent (Example 5), according to the amount of pesticide per mu of 20 ml, the amount of water per mu of 100 ml, diluted 5 times;

[0101] Treatment 5: 0.05% ultra-low volume liquid agent (Comparative Example 1), according to the ultra-low volume spraying, the amount of pesticide per mu is 100 ml;

[0102] Treatment 6: 0.05% ultra-low volume liquid agent (Comparative Example 2), according to the ultra-low volume spraying, the amount of pesticide per mu is 100 ml;

[0103] Treatment 7: 0.05% ultra-low volume liquid agent (Comparative Example 3), according to the ultra-low volume spraying, the amount of pesticide per mu is 100 ml;

[0104] Experimental method: select 5 30-meter open land, insert bamboo poles at intervals of 50 cm, the top end of the bamboo pole is parallel to the ground and clamps the water-sensitive paper, each bamboo pole is spaced 50 cm apart, a total of 12 points (see Figure 1 and Figure 3 shown). The pesticide spraying process is shown in Figure 2 and Figure 3After the spraying was completed, the water sensitive papers were introduced into the computer one by one through the scanner, and the image after scanning was analyzed by the droplet deposition analysis system, so as to obtain the data of droplet particle size and deposition amount of the droplets on each water sensitive paper. The average deposition amount was calculated by removing the maximum and minimum collection points of the droplet density in each treatment group. The droplet particle size was represented by volume DV10 (the particle size corresponding to the cumulative particle size distribution of 10%), DV50 and DV90. The parameters of the unmanned aerial vehicle operation were as follows:

[0105] Table 18. Operation parameters

[0106]

[0107] Deposition amount test data:

[0108] Table 19. Deposition amount test of clean water

[0109]

[0110] Table 20. Deposition amount test of sodium p-chlorophenoxyacetic acid soluble concentrate of Comparative Example 4

[0111]

[0112] Table 21. Deposition amount test of sodium p-chlorophenoxyacetic acid ultra-low volume liquid of Example 2

[0113]

[0114] Table 22. Deposition amount test of sodium p-chlorophenoxyacetic acid ultra-low volume liquid of Example 5

[0115]

[0116] Table 23. Deposition amount test of ultra-low volume liquid of Comparative Example 1

[0117]

[0118] Table 24. Deposition amount test of ultra-low volume liquid of Comparative Example 2

[0119]

[0120] Table 25. Deposition amount test of ultra-low volume liquid of Comparative Example 3

[0121]

[0122] Table 26. Influence of sodium p-chlorophenoxyacetic acid soluble concentrate and ultra-low volume liquid on deposition amount

[0123]

[0124] From the above table data, the spray particle size of the ultra-low volume liquid is smaller, the coverage is higher, and the deposition amount is higher, thereby improving the plant absorption utilization rate and improving the drug efficacy.

[0125] Example 4 drug efficacy test

[0126] 1. 0.01% sodium p-chlorophenoxyacetic acid super low volume liquid to promote wheat yield test

[0127] 1.1 Test time: October 26, 2024 to November 8, 2024.

[0128] 1.2 Test site: Yuntong Village, Santai County, Mianyang City, Sichuan Province.

[0129] 1.3 Test object: Mianmai 112.

[0130] 1.4 Test site treatment: Select a small wheat plot with consistent variety, uniform growth, no obvious pests and diseases, and relatively flat as the test plot, sow at the above time, and the wheat is at the jointing and budding stage when spraying. The plot has adequate and evenly distributed fertility, no obvious pests and diseases, and the grower has not used other types of yield-increasing agents; the soil is loam.

[0131] 1.5 Test agent: 0.01% sodium p-chlorophenoxyacetic acid ultra-low volume liquid prepared in Example 1; 1% sodium p-chlorophenoxyacetic acid soluble liquid prepared in Comparative Example 4; sodium polyborate; EDTA-zinc; plant small molecule signal peptide YPP.

[0132] 1.6 Test period: wheat jointing stage, flowering stage.

[0133] The settings of each treatment group are shown in Table 27.

[0134] Table 27. Test design

[0135]

[0136] 1.7 Method of application: Treatment 1 and Treatment 2 are soluble liquids, low-volume spraying is used, the plot area is 0.5 mu, and the repetition is 2 times; Treatment 3 and 4 are ultra-low volume liquids, ultra-low volume spraying is used, the plot area is 0.5 mu, and the repetition is 2 times; the plot area of the blank control is 0.5 mu; the bamboo sticks are bound with adhesive tape to separate each treatment, and the marks are made.

[0137] 1.8 Test basis: Refer to GB / T 17980.132-2004

[0138] 1.9 Investigation method:

[0139] Crop yield calculation method:

[0140] Randomly select 5 points in each plot, and select 1 m 2The above indexes are measured. 20 spikes of wheat are randomly selected from each point to measure spike length, spike grain number, effective spike number (spike grain number > 5), determine the yield of the sampling point, thousand-grain weight (5 repetitions are randomly selected from each plot to measure), and calculate the theoretical yield per mu and yield increase rate.

[0141] Data statistical analysis: DPS6.55 (Duncan) statistical software is used for analysis. According to the test data, average effective spike number C1, average spike grain number C2, average thousand-grain weight C3, and theoretical yield increase rate C4 are calculated.

[0142] Effective spike number per mu: In the range of the wheat test field, 1 square meter is randomly selected to measure the effective spike number (spike grain number > 5), and the average value is calculated to obtain the effective spike number per mu.

[0143] Spike grain number: 20 spikes of wheat are randomly selected from each plot to investigate the spike grain number (small spikes with less than 5 grains are removed).

[0144] Thousand-grain weight: After using the water floating method, 100 grains are weighed repeatedly 3 times, and the average value of the similar 2 times is the hundred-grain weight, which is multiplied by 10 to obtain the thousand-grain weight.

[0145] Theoretical yield (kg / mu) = unit area spike number (spikes / m 2 ) × 667m 2 × average spike grain number × thousand-grain weight (g) ÷ 10 -6 × 85% (wherein, 10 -6 is the unit conversion coefficient).

[0146] Increase or yield increase rate calculation method:

[0147] Yield increase rate (%) = (treatment group yield - control group yield) / control group yield × 100%.

[0148] Safety evaluation method of the drug:

[0149] Observe whether the drug affects the normal growth of wheat, whether there are leaf yellowing, scorching, dry tips, etc.

[0150] “+” mild phytotoxicity appears on the leaves, which does not affect crop growth;

[0151] “++” obvious phytotoxicity appears on the leaves, but it can recover and does not affect crop yield

[0152] “+++” severe phytotoxicity appears on the leaves, which affects the normal growth of crops and causes a certain degree of loss to crop yield and quality.

[0153] 1.10 Test results

[0154] (1) Safety evaluation

[0155] Table 28. Safety evaluation of sodium p-chlorophenoxyacetate on wheat

[0156]

[0157] As can be seen from Table 28, using 0.01% sodium p-chlorophenoxyacetate ultra-low volume liquid and 1% sodium p-chlorophenoxyacetate soluble liquid at the jointing and booting stages of wheat seedlings is safe, and no phytotoxicity was observed in each treatment of the test.

[0158] Table 29. Results of sodium p-chlorophenoxyacetate wheat yield-increasing test

[0159]

[0160] Table 30. Effect of sodium p-chlorophenoxyacetate on wheat quality

[0161]

[0162] As can be seen from Table 29, treatment group 1 (1% sodium p-chlorophenoxyacetate soluble liquid 10 ml / acre), containing 0.1 g / acre of active ingredient sodium p-chlorophenoxyacetate; treatment group 2 (1% sodium p-chlorophenoxyacetate soluble liquid 20 ml / acre), containing 0.2 g / acre of active ingredient sodium p-chlorophenoxyacetate; treatment group 3 (0.01% sodium p-chlorophenoxyacetate ultra-low volume liquid 400 ml / acre), containing 0.04 g / acre of active ingredient sodium p-chlorophenoxyacetate; treatment group 4 (0.01% sodium p-chlorophenoxyacetate ultra-low volume liquid 800 ml / acre), containing 0.08 g / acre of active ingredient sodium p-chlorophenoxyacetate; it can be seen that at the jointing and flowering stages of wheat, the use amount of ultra-low volume liquid per mu is lower, which can promote the increase of effective ear number, improve the seed setting rate, increase the thousand-grain weight, and the effect of promoting yield increase is significantly better than that of low-volume spraying of soluble liquid. Compared with treatment group 2 (1% sodium p-chlorophenoxyacetate soluble liquid 20 ml / acre), treatment group 3 (0.01% sodium p-chlorophenoxyacetate ultra-low volume liquid 400 ml / acre) reduces the use amount per mu by 5 times, but still has a significant effect on promoting the increase of effective ear number, improving the seed setting rate, increasing the thousand-grain weight, and promoting yield increase.

[0163] As can be seen from Table 30, the use of sodium p-chlorophenoxyacetate ultra-low volume liquid at the jointing and flowering stages of wheat promotes the increase of wheat yield without affecting the quality of wheat.

[0164] 2. 0.05% sodium p-chlorophenoxyacetic acid super low volume liquid to promote wheat yield test

[0165] 2.1 Test time: March 29, 2024 to May 24, 2024.

[0166] 2.2 Test site: Qianrenzhuang, Guanzhen Township, Xinxian County, Henan Province.

[0167] 2.3 Test subject: Amy 189.

[0168] 2.4 Experimental field treatment: Guoguang Kuliman fertilizer was used as base fertilizer in the experimental plots. No pesticides were used afterward. There was a small amount of sheath blight in the field. Field management was average. There were no obvious pests. The soil was loam. The previous crop was corn.

[0169] 2.5 Test reagents: 0.05% sodium p-chlorophenoxyacetate ultra-low volume liquid prepared in Example 2; 1% sodium p-chlorophenoxyacetate soluble liquid prepared in Comparative Example 4; sodium polyborate; EDTA-zinc; plant small molecule signal peptide YPP.

[0170] 2.6 Application period: March 29, 2024 and April 20, 2024, at the growth stage of the wheat: jointing stage and flowering stage.

[0171] The settings for each processing group are shown in Table 31.

[0172] Table 31. Experimental Design

[0173]

[0174] 2.7 Application method: Same as 1.7.

[0175] 2.8 Test basis: Same as 1.8.

[0176] 2.9 Survey Methodology:

[0177] Effective number of ears per mu: Within the wheat experimental field, randomly select 1 square meter, measure the effective number of ears (number of grains per ear > 5), and calculate the average value to determine the effective number of ears per mu.

[0178] Number of grains per spike: Ten wheat spikes were randomly selected from each plot, and the number of grains per spike was investigated (spikes with fewer than 5 grains were excluded).

[0179] 1000-grain weight: After using the water flotation method, randomly select 100 grains and weigh them. Repeat this process 3 times. The average of the two closest weighings is the 100-grain weight. Multiply this by 10 to get the 1000-grain weight.

[0180] Theoretical yield (kg / mu) = Number of ears per unit area (ears / m²) 2 ) × 667m 2 × Average number of grains per ear × 1000-grain weight (g) ÷ 10 -6 ×85% (of which, 10) -6 (Unit conversion factor).

[0181] Method for calculating the increase or production rate:

[0182] Increase in yield (%) = (yield of treatment group - yield of control group) / yield of control group × 100%.

[0183] Safety evaluation method of drug:

[0184] Observe whether the agent affects the normal growth of wheat, whether there are leaf yellowing, scorching, dry tip and other phenomena.

[0185] “+” leaf mild phytotoxicity, no effect on crop growth;

[0186] “++” leaf obvious phytotoxicity, but can recover, no effect on crop yield

[0187] “+++” leaf serious phytotoxicity, affecting the normal growth of crops, causing a certain degree of loss to the yield and quality of crops.

[0188] 2.10 Test results

[0189] (1) Safety evaluation results

[0190] Table 32. Safety evaluation of sodium p-chlorophenoxyacetate on wheat

[0191]

[0192] As can be seen from Table 32, the use of 0.05% sodium p-chlorophenoxyacetate ultra-low volume liquid and 1% sodium p-chlorophenoxyacetate soluble liquid at the jointing and squaring stage of wheat is safe, and no phytotoxicity is observed in each treatment.

[0193] Table 33. Results of sodium p-chlorophenoxyacetate wheat yield-increasing test

[0194]

[0195] Table 34. Effect of sodium p-chlorophenoxyacetate on wheat quality

[0196]

[0197] As shown in Table 33, treatment group 1 (1% sodium p-chlorophenoxyacetic acid soluble liquid 10 ml / acre) contains 0.1 g / acre of active ingredient sodium p-chlorophenoxyacetic acid; treatment group 4 (0.05% sodium p-chlorophenoxyacetic acid ultra-low volume liquid 200 ml / acre) contains 0.1 g / acre of active ingredient sodium p-chlorophenoxyacetic acid. It can be seen that under the same amount of drug per mu at the jointing stage and flowering stage of wheat, the ultra-low volume liquid promotes the increase of effective ear number, improves the seed setting rate, increases the thousand-grain weight, and the effect of promoting yield increase is significantly better than that of low volume spraying of soluble liquid. Treatment group 3 (0.05% sodium p-chlorophenoxyacetic acid ultra-low volume liquid reduces the amount of drug per mu to 100 ml / acre), i.e. 0.05 g / acre of active ingredient sodium p-chlorophenoxyacetic acid, compared with treatment group 2 (1% sodium p-chlorophenoxyacetic acid soluble liquid 20 ml / acre), i.e. 0.2 g / acre of active ingredient sodium p-chlorophenoxyacetic acid, the amount of drug per mu of ultra-low volume liquid is reduced by 4 times, and there is still a significant effect in promoting the increase of effective ear number, improving the seed setting rate, increasing the thousand-grain weight, and promoting yield increase.

[0198] As shown in Table 34, the sodium p-chlorophenoxyacetic acid ultra-low volume liquid promotes the increase of wheat yield, and has no effect on the quality of wheat.

[0199] 3. 1% sodium p-chlorophenoxyacetic acid super low volume liquid to promote wheat yield test

[0200] 3.1 Test time: April 10, 2024 to June 5, 2024.

[0201] 3.2 Test site: Liulou Town, Wenshang County, Jining City, Shandong Province.

[0202] 3.3 Test object: Zhongmai 578.

[0203] 3.4 Test site treatment: The wheat was at the booting stage, the wheat grew well, the soil type was loess, the management level was medium, and there were some weeds in the field. Drug treatment: the first drug treatment time was April 10, 2024. The second drug treatment time was April 25, 2024.

[0204] 3.5 Test drug: 1% sodium p-chlorophenoxyacetic acid ultra-low volume liquid prepared in Example 5; 1% sodium p-chlorophenoxyacetic acid soluble liquid prepared in Comparative Example 4; polyborate sodium; EDTA-zinc; plant small molecule signal peptide YPP.

[0205] 3.6 Usage period: jointing stage and flowering stage of wheat.

[0206] The settings of each treatment group are shown in Table 12.

[0207] Table 35. Test design

[0208]

[0209] 3.7 Drug application method: same as 1.7.

[0210] 3.8 Test basis: same as 1.8.

[0211] 3.9 Investigation method:

[0212] Effective ear number per mu: In the range of the wheat test field, 1 square meter was randomly selected, and the effective ear number (grain number per ear > 5) was measured to calculate the average value of the effective ear number per mu.

[0213] Grain number per ear: 10 wheat ears were randomly selected from each plot, and the grain number per ear was investigated (excluding small ears with less than 5 grains).

[0214] Thousand-grain weight: After using the water floating method, 100 grains were counted and weighed, repeated 3 times, and the average value of the similar 2 times was the hundred-grain weight, multiplied by 10 to get the thousand-grain weight.

[0215] Theoretical yield (kg / mu) = unit area ear number (ears / m 2 ) × 667m 2 × average grain number per ear × thousand-grain weight (g) ÷ 10 -6 × 85% (wherein, 10 -6 is the unit conversion coefficient).

[0216] Increase or yield increase rate calculation method:

[0217] Yield increase rate (%) = (treatment group yield - control group yield) / control group yield × 100%.

[0218] Safety evaluation method of drug:

[0219] Observe whether the pesticide affects the normal growth of wheat, whether there are leaf yellowing, scorching, dry tips, etc.

[0220] “+” Light pesticide damage on leaves, which does not affect crop growth;

[0221] “++” Obvious pesticide damage on leaves, but can recover, which does not affect crop yield

[0222] “+++” Severe pesticide damage on leaves, which affects the normal growth of crops and causes a certain degree of loss to crop yield and quality.

[0223] 3.10 Test results

[0224] (1) Safety evaluation results

[0225] Table 36. Safety evaluation of sodium p-chlorophenoxyacetate on wheat

[0226]

[0227] Table 36 can be seen, in the wheat jointing stage using 1% sodium p-chlorophenoxyacetic acid ultra-low volume liquid, 1% sodium p-chlorophenoxyacetic acid soluble liquid is safe, the test did not observe the phytotoxicity of each treatment.

[0228] Table 37. Sodium p-chlorophenoxyacetate wheat yield-increasing test results

[0229]

[0230] Table 38. Effect of sodium p-chlorophenoxyacetate on wheat quality

[0231]

[0232] Table 37 can be seen, treatment group 1 (1% sodium p-chlorophenoxyacetate soluble liquid 10 ml / acre), containing 0.1 g / acre of active ingredient sodium p-chlorophenoxyacetate; treatment group 4 (1% sodium p-chlorophenoxyacetate ultra-low volume liquid 10 ml / acre), containing 0.1 g / acre of active ingredient sodium p-chlorophenoxyacetate, can be seen, in the same acreage of wheat jointing stage, the ultra-low volume liquid promotes the increase of effective ear number, improves the seed setting rate, increases the thousand-grain weight, and the effect of promoting yield increase is significantly better than that of the low volume spray of the soluble liquid. Treatment group 3 (1% sodium p-chlorophenoxyacetate ultra-low volume liquid reduces the acreage of drug to 5 ml / acre), that is, the active ingredient sodium p-chlorophenoxyacetate is 0.05 g / acre, compared with treatment group 2 (1% sodium p-chlorophenoxyacetate soluble liquid 20 ml / acre), that is, the active ingredient sodium p-chlorophenoxyacetate is 0.2 g / acre, the ultra-low volume liquid reduces the acreage of drug by 4 times, and still has a significant effect on promoting the increase of effective ear number, improving the seed setting rate, increasing the thousand-grain weight, and promoting yield increase.

[0233] Table 38 can be seen, sodium p-chlorophenoxyacetate promotes the increase of wheat yield, and has no effect on the quality of wheat.

[0234] The above is only a preferred embodiment of the present application, it should be noted that the above preferred embodiment should not be regarded as a limitation of the present application, the protection scope of the present application should be limited by the scope defined by the claims. For ordinary skilled in the art, without departing from the spirit and scope of the present application, a number of improvements and refinements can also be made, which improvements and refinements should also be regarded as the protection scope of the present application.

Claims

1. An ultra-low volume liquid formulation containing sodium p-chlorophenoxyacetic acid, characterized in that, The components are as follows in mass percentage: 0.01-1% of sodium p-chlorophenoxyacetate, 3-5% of plant small molecule signal peptide, 1-5% of organic silicon, 3-10% of nano-silicon dioxide, 30-50% of ethylene glycol, 10-20% of nutritional elements, and water to make up to 100%; the organic silicon component comprises at least one polyether modified polysiloxane and at least one polyether compound; the plant small molecule signal peptide is selected from one or more of RALF, CIF, EPF, EPFL, PEP, and yeast peptide containing amino acid.

2. The ultra-low volume liquid formulation according to claim 1, characterized in that, The organic silicon is a combination of polyether modified silicone oil and polyether.

3. The ultra-low volume liquid formulation according to claim 1, characterized in that, The nano-silicon dioxide has a particle size of 100-200 nm.

4. The ultra-low volume liquid formulation according to claim 1, characterized in that, The nutritional elements are nutritional elements containing boron elements and zinc elements.

5. A process for the preparation of ultra-low volume liquid containing sodium p-chlorophenoxyacetic acid as claimed in any one of claims 1 to 4, characterized in that, The application further relates to a preparation method of the p-chlorophenoxyacetate-containing ultra-low volume liquid agent. The sodium p-chlorophenoxyacetate is dissolved in water and heated, the nutritional elements and the plant small molecule signal peptide are dissolved, and after the solid materials are completely dissolved, the ethylene glycol, the organic silicon and the nano-silicon dioxide are mixed to obtain the p-chlorophenoxyacetate-containing ultra-low volume liquid agent.

6. Application of the p-chlorophenoxyacetate-containing ultra-low volume liquid agent in promoting crop yield according to any one of claims 1-4.

7. Use according to claim 6, characterized in that, The crop is selected from any one of wheat and rice.

8. Use according to claim 7, characterized in that, The application is to promote crop spike differentiation, increase the number of grains per spike and the thousand-grain weight.

9. Use according to claim 6, characterized in that, The effective component dosage of the p-chlorophenoxyacetate-containing ultra-low volume liquid agent is 0.04-0.1 g / mu.

Images