Preparation method and application of antofen suspending agent

Abstract

The invention discloses a preparation method and application of an antofen suspending agent, and relates to the technical field of pesticide preparations, and the preparation method specifically comprises the following steps: S1, adding water, an anti-freezing agent, a wetting dispersant and a part of a defoaming agent, and shearing in a multifunctional dispersion sand mill in a laboratory; s2, then adding a thickening agent and an antofine active compound, and continuing shearing; s3, transferring to a vertical sand mill, and adding zirconium beads for sanding; and S4, filtering the zirconium beads after sanding is completed, adding the rest of the defoaming agent, the stabilizer and the warning coloration, and shearing and uniformly mixing to obtain the product. The antofen suspending agent is efficient and safe, can effectively prevent and treat foxtail millet poliosis, is remarkable in prevention and treatment effect, and lays a foundation for further field prevention and treatment of foxtail millet poliosis.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide preparations, and in particular to a preparation method and application of an anthophen suspension. Background Art

[0002] Millet (Setaria italica) has a long history of cultivation in my country, and its cultivation history can be traced back to more than 8,000 years ago. Millet has shown many superior characteristics in the planting process. Millet has a strong drought resistance, so it has become one of the important food crops in many northern regions. my country's millet production and millet planting area rank first in the world. The planting areas are mainly distributed in some arid and semi-arid areas, such as Northwest China, North China, Northeast China, etc. These arid and semi-arid areas are the main millet production areas in my country.

[0003] With the continuous development of millet planting in my country, the Sclerospora graminicola Millet leukoplakia caused by Sacc. Schroet has gradually become one of the important agricultural problems of millet in my country. This problem is common in the main millet producing areas. Especially since 2010, the incidence of millet leukoplakia has shown an increasing trend year by year. In recent years, in Shanxi, Shaanxi, Henan, Hebei and other provinces and regions and the Northeast, these major millet producing areas have seen a sharp decline in millet production and huge losses every year due to millet leukoplakia.

[0004] At present, metalaxyl seed dressing is the most commonly used method for preventing and controlling millet white spot disease. However, long-term single use of metalaxyl will cause millet white spot disease bacteria to develop drug resistance. Therefore, in order to delay the generation and development of millet white spot disease bacteria to metalaxyl resistance, it is urgent to accelerate the development of new agents for preventing and controlling millet white spot disease. In addition, since different pesticides have different physical and chemical properties and biological activity characteristics, the biological effects and occurrence patterns of different pests and diseases are different, and the environmental conditions for using the agents are also different, it is very necessary to develop an efficient, safe, economical and easy-to-use formulation. Based on this, the development of a new agent for preventing and controlling millet white spot disease and a suitable formulation form is very meaningful for large-scale millet cultivation. Summary of the invention

[0005] In view of the above problems, the present invention provides a preparation method and application of an anthofen suspension.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is as follows: The present invention provides a method for preparing anthofen suspension, which specifically comprises the following steps: S1: Add water, antifreeze, wetting dispersant and part of defoamer and shear in the laboratory multifunctional dispersing sand mill; S2: Then add thickener and anthophen technical and continue shearing; S3: then transferred to a vertical sand mill, and sanded with zirconium beads; S4: After sand grinding, filter the zirconium beads, add the remaining defoamer, stabilizer and warning color, shear and mix evenly to obtain 2% anthofen suspension.

[0007] Furthermore, in step S1, the antifreeze agent is glycerol; the wetting and dispersing agent is sodium lignin sulfonate and Tween 20 in a mass ratio of 1:2; the defoaming agent is an organosilicon defoaming agent; and the shearing time is 3 to 5 min. Furthermore, in step S2, the thickener is xanthan gum, and the shearing time is 5 to 10 min.

[0008] Furthermore, in step S3, the sand grinding time is 1.5 to 2 h, and the particle size is controlled within D 90 ≤5 μm.

[0009] Furthermore, the stabilizer is sodium alginate and the warning color is red color paste.

[0010] Furthermore, in the steps S1-S4, the anthofen suspension is composed of the following components in a weight / volume ratio: 2% anthofen technical, 5% antifreeze, 2% wetting dispersant, 0.5% defoamer, 0.2% thickener, 0.3% stabilizer, 1.5% warning color, and the balance is water.

[0011] That is, every 100 mL of anthofen suspension contains the following components: 2 g of anthofen technical, 5 mL of antifreeze, 2 g of wetting and dispersing agent, 0.5 mL of defoaming agent, 0.2 g of thickener, 0.3 g of stabilizer, 1.5 mL of warning color, and the balance is water.

[0012] The present invention also provides an application of anthofen suspension, wherein the anthofen suspension is applied in preventing and treating millet whitening disease.

[0013] Furthermore, the application method is specifically as follows: Antofin suspension concentrate is mixed with millet seeds for seed treatment; the weight ratio of the Antofin suspension concentrate to the millet seeds is 1:300.

[0014] The research team previously collected poisonous sand plants from the Asclepiadaceae family in Yulin, Shaanxi Province. Asclepiadaceae ) Cynanchum komarovii Al. Iljinski) successfully isolated an alkaloid compound anthophen. Studies have found that this alkaloid has the characteristics of broad bactericidal spectrum, high activity, long lasting effect, low toxicity, and safety to non-target organisms, and has a good bactericidal effect on many pathogens.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention uses anthofin as the original drug and adopts a wet grinding process to prepare a 2% anthofin suspension, which can be used as a high-efficiency, low-toxic plant-derived fungicide for preventing and treating millet white disease, is safe for millet, and is not easy to develop drug resistance. The anthofin suspension of the present invention can be evenly wrapped on the surface of the seeds, thereby ensuring the uniform exertion of the drug effect. By mixing the seeds, it can play a protective role in the seed and seedling period, and can prevent the occurrence of diseases more timely, simply and effectively; in addition, compared with other dosage forms, the suspension has less damage to the seeds and higher safety. Based on this, the anthofin suspension of the present invention is efficient and safe, can effectively prevent and treat millet white disease, and has a significant prevention and control effect, which lays a foundation for further carrying out field prevention and control of millet white disease. DETAILED DESCRIPTION

[0016] In order to make the purpose and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0017] The instruments, reagents, materials, etc. involved in the following examples, unless otherwise specified, are all conventional instruments, reagents, materials, etc. in the prior art and can be obtained through regular commercial channels. The experimental methods, detection methods, etc. involved in the following examples, unless otherwise specified, are all conventional experimental methods, detection methods, etc. in the prior art.

[0018] In this embodiment, the test materials are as follows: Millet variety for test: The millet variety for this test was “Jingu No. 21”, which was provided by the Agricultural Technology Extension Center of Hengshan District, Yulin City.

[0019] Test agents: Anthofin (purity>90%) was provided by the Plant Protection Laboratory of the School of Life Sciences of Yulin University. 35% metalaxyl powder was purchased from Zhejiang Heben Technology Co., Ltd.

[0020] Nutrient soil for testing: Use the special nutrient soil produced by Shenyang Jinzhao Biotechnology Co., Ltd.

[0021] Test reagents: sodium dodecylbenzene sulfonate (SDBS), Tween 20 (TW20), sodium lignin sulfonate MNS / 90, xanthan gum, magnesium aluminum silicate, ethylene glycol, urea, glycerin, silicone defoamer, sodium alginate, R2002SS red color paste (purchased from Taobao Tiantian Dyestuff).

[0022] The test instruments include: electronic balance, laboratory multifunctional dispersing sand mill, laboratory vertical sand mill, pH meter, electric blast drying oven, refrigerator, glass constant temperature water bath, laser particle size distribution analyzer.

[0023] The suspension test method is as follows: Active ingredient content: Determined by HPLC method. Suspension rate: According to GB / T 14825-2006. Pourability: According to GB / T31737-2015.

[0024] Example 1 This embodiment provides a method for preparing anthofen suspension, which specifically comprises the following steps: S1: Add water, antifreeze (glycerol), wetting dispersant (sodium lignin sulfonate and Tween 20 in a mass ratio of 1:2) and part of defoamer (organic silicone defoamer) and shear in a laboratory multifunctional dispersing sand mill for 3 min; S2: Then, thickener (xanthan gum) and anthophen technical were added, and shearing was continued for 5 min; S3: Then transfer to a vertical sand mill, add zirconium beads (mass ratio of material to zirconium beads is 1:1.2, diameter 0.8 mm) and sand grind for 1.5 h to control the particle size at D 90 ≤5 μm; S4: After sand grinding, filter the zirconium beads, add the remaining defoamer (organic silicone defoamer), stabilizer (sodium alginate) and warning color (R2002SS red color paste), shear and mix evenly to obtain.

[0025] Example 2 This embodiment provides a method for preparing anthofen suspension, which specifically comprises the following steps: S1: Add water, antifreeze (glycerol), wetting dispersant (sodium lignin sulfonate and Tween 20 in a mass ratio of 1:2) and part of defoamer (organic silicone defoamer) and shear in a laboratory multifunctional dispersing sand mill for 4 min; S2: Then, thickener (xanthan gum) and anthophen technical were added, and shearing was continued for 8 min; S3: Then transfer to a vertical sand mill, add zirconium beads (mass ratio of material to zirconium beads is 1:1.2, diameter 0.8 mm) and sand grind for 1.8 h to control the particle size at D 90 ≤5 μm; S4: After sand grinding, filter the zirconium beads, add the remaining defoamer (organic silicone defoamer), stabilizer (sodium alginate) and warning color (R2002SS red color paste), shear and mix evenly to obtain.

[0026] Example 3 This embodiment provides a method for preparing anthofen suspension, which specifically comprises the following steps: S1: Add water, antifreeze (glycerol), wetting dispersant (sodium lignin sulfonate and Tween 20 in a mass ratio of 1:2) and part of defoamer (organic silicone defoamer) and shear in a laboratory multifunctional dispersing sand mill for 5 min; S2: Then, thickener (xanthan gum) and anthophen technical were added, and shearing was continued for 10 min; S3: Then transfer to a vertical sand mill, add zirconium beads (mass ratio of material to zirconium beads is 1:1.2, diameter 0.8 mm) and sand grind for 2 h to control the particle size at D 90 ≤5 μm; S4: After sand grinding, filter the zirconium beads, add the remaining defoamer (organic silicone defoamer), stabilizer (sodium alginate) and warning color (R2002SS red color paste), shear and mix evenly to obtain.

[0027] Experimental Example 1: Formulation Screening 1. Screening of wetting and dispersing agents As shown in Table 1, the overall effect of the wetting and dispersing agent SDBS is poor, especially after 1% SDBS was hot stored (54℃) for 14 days, its suspension rate was 95.03%, the pourability was poor, the particle size was also large, and D 90 The wetting and dispersing agent MNS / 90 has a better effect, especially after 3% MNS / 90 was stored at 54℃ for 14 days, its suspension rate was 97.25%, the pourability was good, and the particle size D 90 The wetting and dispersing agent TW20 has the best effect, especially after 2% TW20 was hot stored (54℃) for 14 days, its suspension rate was 98.43%, the pourability was good, and the particle size D 90 is 3.99 μm.

[0028] Table 1 Screening of wetting and dispersing agents

[0029] Therefore, MNS / 90 and TW20 (1:1, 1:2, 2:1) were compounded, and the hot storage suspension rate, particle size and pourability after compounding were measured. As shown in Table 2, the effect of MNS / 90 and TW20 (1:1, 1:2) compounding was better. In particular, the effect of MNS / 90 and TW20 (1:2) compounding was the best. After hot storage (54℃) for 14 days, its suspension rate was 99.06%, the pourability was good, and the particle size D 90 It is 3.95μm.

[0030] Table 2 Screening of wetting and dispersing agent compounding

[0031] 2. Thickener screening The sedimentation rate of dispersed phase particles in the suspension is affected by the viscosity of its medium. Increasing the viscosity of the suspension medium is conducive to slowing down the sedimentation rate of the suspension particles, thereby improving the suspension stability of the suspension. As shown in Table 3, after treatment with 0.15% and 0.2% xanthan gum, the water separation rate of the preparation is 3-6%, with slight water separation and good fluidity. After treatment with 0.5%, 1.0%, and 1.5% magnesium aluminum silicate, the preparation has severe water separation and is difficult to recover. After compounding xanthan gum and magnesium aluminum silicate (0.1%+1%), the water separation rate is 21%, severe water separation, and difficult to recover. After compounding xanthan gum and magnesium aluminum silicate (0.15%+1% and 0.2%+1%), the water separation rate is 10-14%, with slight water separation and recovery by shaking. Therefore, 0.2% xanthan gum has the best thickening effect on the preparation.

[0032] Table 3 Screening of thickeners

[0033] 3. Screening of antifreeze Suspension concentrates usually use water as a dispersion medium, but when used in a low-temperature environment, the suspension concentrate may freeze, affecting the stability of the product itself, thereby affecting its use and sales. Therefore, an appropriate amount of antifreeze needs to be added during the development and preparation of the suspension concentrate to solve this problem. In order to meet the requirements for the stability of the preparation, different amounts of ethylene glycol, urea, and glycerol were selected as antifreeze agents for screening in this experiment. As can be seen from Table 4, considering the use effect and cost, 5% glycerol is the best antifreeze agent and can meet the requirements for the stability of the preparation, so glycerol was finally selected as the antifreeze agent at a dosage of 5%.

[0034] Table 4 Screening of antifreeze

[0035] 4. Screening of other components Since the wet grinding process is used to produce the seed treatment suspension in this test, a sander is used in the wet grinding process. When the sander runs at high speed, a large number of bubbles will be generated, which will inevitably affect the product viscosity and filling quality. Therefore, it is necessary to add an appropriate amount of defoamer to solve this problem. 0.5% silicone defoamer and 0.3% sodium alginate are selected as stabilizers. According to the national standard, the seed treatment suspension also needs to add a warning color. The R2002SS red color paste commonly used in the laboratory is selected as the warning color, and its dosage is 1.5%.

[0036] Experimental Example 2 Safety Test Select Jingu 21 with uniform size and fullness, and coat the 2% anthofen suspension and 35% metalaxyl powder prepared in Example 2 at a drug-to-seed ratio of 1:300, use clean water as a blank control, conduct a control test, and air-dry naturally for use. Sow the coated millet seeds in special nutrient soil, and after germination, measure the emergence rate of different treatments. After 27 days, measure the plant height, root length and stem thickness of each treatment.

[0037] As shown in Table 5, each treatment group had no effect on millet germination, and the germination rate could reach more than 95%. There was no significant difference in plant height, stem thickness, and root length between the millet treated with 2% Antofin suspension and the blank control group and the 35% metalaxyl powder treatment group. Therefore, 2% Antofin seed treatment suspension is safe for millet growth.

[0038] Table 5 Safety test of 2% Antofin suspension on millet

[0039] Note: Data are the average of three experiments, and different lowercase letters represent significant differences among treatments ( P <0.05).

[0040] Experimental Example 3 Field trial - Field control effect of 2% Antofin suspension on millet gray disease The experimental site was set up in Hancha Village, Hancha Township, Hengshan District, Yulin City, Shaanxi Province (109 o 31′51′′E, 37 o 51′11′′N; 1223 m above sea level). The experiment adopted a randomized block design mode, with a total of 3 treatment groups, namely, millet seed-dressed with 2% anthofen suspension (A), millet seed-dressed with 35% metalaxyl powder (J) and water control (CK) in Example 2. 2% anthofen suspension and 35% metalaxyl powder were evenly mixed with Jingu No. 21 seeds at a ratio of 1:300, respectively. Each treatment was repeated 4 times, with a total of 12 plots, each with a width of 4 m, a length of 5 m, and a plot area of ​​20 m 2 , the row spacing is 50 cm, the hole spacing is 11 cm, and there are 2 to 4 plants in each hole. The millet for the test was planted after seed dressing, and about 360 millet plants were maintained in each plot. On May 1, 2023, a small millet sowing machine was used for sowing. Before sowing, compound fertilizer was spread on the soil, and then the soil was loosened. The number of diseased plants in each treatment was investigated during the adult stage (Table 6), and the disease index and efficacy were calculated according to Formula 1 and Formula 2. Normal tillage and weeding were carried out during the entire growth period of millet, and no irrigation was performed. Other management measures were consistent with the local fields.

[0041] Formula 1 Formula 2 Table 6 Grading standards for millet white spot disease at mature stage

[0042] As shown in Table 7, there was no significant difference in the disease index of millet after treatment with 2% Antofin suspension and 35% Metalaxyl powder, which were significantly reduced by 74.31% and 66.79% respectively compared with the CK treatment; there were significant differences in the field control effects of different treatments on millet white spot disease ( P <0.05), the field control effect of 2% Antofin suspension on millet gray disease was 66.81%, which was significantly reduced by 10.13% compared with the chemical fungicide 35% metalaxyl.

[0043] Table 7 Field control effect of 2% Antofin suspension on millet gray disease

[0044] Note: Data are the average of three experiments, and different lowercase letters represent significant differences among treatments ( P <0.05); t test verification of control effect, * Indicates significant difference ( P <0.05).

[0045] The 2% anthofen suspension prepared in Example 1 and Example 3 was subjected to the tests of Experimental Examples 2 and 3, and the same experimental results as those of the 2% anthofen suspension prepared in Example 2 were obtained.

[0046] In summary, the best formula of the 2% Antofin seed treatment suspension in this embodiment is: by weight / volume ratio, the dosage of Antofin original drug is 2%, the dosage of glycerol is 5%, the dosage of sodium lignin sulfonate + Tween 20 (1:2) is 2%, the dosage of silicone defoamer is 0.5%, the dosage of xanthan gum is 0.2%, the dosage of sodium alginate is 0.3%, the dosage of R2002SS red color paste is 1.5%, and the balance is water. The disease index of the plants treated with 2% Antofin suspension in this embodiment is much lower than that of the control group, and the drug efficacy reaches 66.81%, and it has no effect on the emergence rate of seeds. The height, stem thickness and root length of the treated plants are all higher than those of the blank control group. Therefore, 2% Antofin suspension has a good preventive and control effect on millet white disease.

[0047] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing anthofen suspension, characterized in that: The specific steps include: S1: Add water, antifreeze, wetting dispersant and part of defoamer and shear in the laboratory multifunctional dispersing sand mill; S2: Then add thickener and anthophen technical and continue shearing; S3: then transferred to a vertical sand mill, and sanded with zirconium beads; S4: After sand grinding, filter the zirconium beads, add the remaining defoamer, stabilizer and warning color, shear and mix evenly to obtain the anthofen suspension.

2. The method for preparing an anthophenic suspension according to claim 1, wherein: In the step S1, the antifreeze agent is glycerol; the wetting and dispersing agent is sodium lignin sulfonate and Tween 20 in a mass ratio of 1:2; the defoaming agent is an organosilicon defoaming agent; and the shearing time is 3 to 5 minutes.

3. The method for preparing an anthofen suspension according to claim 1, characterized in that: In step S2, the thickener is xanthan gum, and the shearing time is 5 to 10 min.

4. The method for preparing an anthofen suspension according to claim 1, characterized in that: In step S3, the sand grinding time is 1.5 to 2 h, and the particle size is controlled within D 90 ≤5 μm.

5. The method for preparing an anthofen suspension according to claim 1, characterized in that: In step S4, the stabilizer is sodium alginate and the warning color is red color paste.

6. The method for preparing an anthofen suspension according to claim 1, characterized in that: In the steps S1-S4, the anthofen suspension is composed of the following components in a weight / volume ratio: 2% anthofen technical, 5% antifreeze, 2% wetting dispersant, 0.5% defoamer, 0.2% thickener, 0.3% stabilizer, 1.5% warning color, and the balance is water.

7. An application of anthofen suspension prepared by the method for preparing anthofen suspension according to any one of claims 1 to 6, characterized in that: The anthofin suspension is used in preventing and treating millet whitening disease.

8. The use of an anthofen suspension according to claim 7, characterized in that: The application method is specifically as follows: anthofen suspension concentrate is mixed with millet seeds for seed treatment; the weight ratio of anthofen suspension concentrate to millet seeds is 1:300.

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