A spirodiclofen suspension, preparation method and application thereof

Abstract

The present application relates to the technical field of spirodiclofen pesticides, and specifically to a spirodiclofen suspension, and its preparation method and application. The suspension comprises the following components: spirodiclofen, auxiliary dispersant a, auxiliary dispersant b, defoamer, thickener, wetting agent, and the balance is water; wherein, the auxiliary dispersant a contains ester groups and amino groups, and the auxiliary dispersant b contains ether bonds and hydroxyl groups. Weigh water, defoamer, and wetting agent, mix at room temperature, and record as liquid A; weigh spirodiclofen original drug, auxiliary dispersant a, and auxiliary dispersant b, add to liquid A and mix to obtain liquid B; shear liquid B, then grind and add thickener, and mix to obtain the spirodiclofen suspension. The present application improves the storage period and high temperature stability of the spirodiclofen suspension through auxiliary dispersant a, auxiliary dispersant b, wetting agent, defoamer, and thickener, and also increases its retention time on citrus leaves, which has a positive effect on the prevention and control of citrus red spiders.

Description

Technical Field

[0001] The present application relates to the technical field of spiroclofonate pesticides, and more specifically, to a spiroclofonate suspension concentrate and a preparation method and application thereof. Background Art

[0002] With the development of agricultural modernization in my country, many regions have begun to increase the yield of their respective advantageous crops. Among them, citrus is widely distributed in Guangdong and Guangxi, Jiangsu and Zhejiang regions in my country. However, for citrus producing areas, citrus red spider is a problem that must be faced. Citrus red spider, scientifically known as Panonychus citri, is distributed in citrus producing areas in my country and around the world, posing a serious threat to citrus production safety. In my country's citrus producing areas, citrus red spider has serious generation overlap and a long damage period. It mainly causes damage by sucking young mites, nymphs and adult mites, causing the affected leaves to lose their luster, fall leaves, and drop flowers and fruits. At present, the prevention and control of citrus red spider mainly relies on spirocytobacide miticides.

[0003] Spirodiclofen is a spirocyclic tetraketone acaricide. Its sales have been increasing year by year in recent years, and it is the acaricide with the highest sales. Spirodiclofen is a non-systemic acaricide. It is mainly used to control eggs, nymphs and female adult mites through contact and stomach poisoning. Its mechanism of action is to inhibit fat synthesis in the body of harmful mites and block energy metabolism. It has no cross-resistance with conventional acaricides. Its egg-killing effect is the same as before, and it has a good protective effect on harmful mites at different developmental stages.

[0004] Regarding the existing spiroclocarp-based acaricides, the applicant found the following problems:

[0005] First of all, the main type of spirodiclofen currently used is suspension concentrate. The important indicator of suspension concentrate is suspension rate. The suspension rate has a relatively high efficacy. The main problem of spirodiclofen suspension concentrate is the problem of particle size growth during long-term storage. As the particle size increases, the suspension rate of spirodiclofen decreases rapidly, so its efficacy will gradually decrease over time.

[0006] Secondly, spirodiclofen is toxic to bees, fish, silkworms and other organisms. When using it, the less the better while achieving the mite-killing effect. However, the existing spirodiclofen is limited by its own adhesion on crop leaves. Its efficacy will begin to decline within 72 hours after spraying, and it will completely lose its efficacy about 14 days after application. In order to ensure its insecticidal ability, the adjacent spraying cycle of spirodiclofen is often very short, which will cause a certain degree of damage to the ecological environment where citrus is located.

[0007] In view of the above technical problems, it is necessary to propose a spirodiclofen suspension with high suspension rate, strong stability, strong wettability and excellent retention on citrus leaves. Summary of the invention

[0008] In order to improve the problems of low suspension rate, poor stability, short residence time and poor wettability of spiroclofonate in the related art, the present application provides a spiroclofonate suspension and a preparation method and application thereof.

[0009] In the first aspect, the present application provides a spirodiclofen suspension, which adopts the following technical solution:

[0010] A spirodiclofen suspension, comprising the following components in weight percentage: 10-24wt% spirodiclofen, 4-5wt% auxiliary dispersant a, 1-2wt% auxiliary dispersant b, 0.2-0.5wt% defoamer, 0.2-0.5wt% thickener, 0.2-0.5wt% wetting agent, and the balance is water;

[0011] The auxiliary dispersant a contains an ester group and an amino group, and the auxiliary dispersant b contains an ether bond and a hydroxyl group.

[0012] In a specific embodiment, the auxiliary dispersant a further contains an unsaturated bond in addition to the carbon-oxygen double bond, and the unsaturated bond includes a carbon-carbon double bond.

[0013] In a specific embodiment, the auxiliary dispersant a is aminoacrylate.

[0014] In a specific embodiment, the auxiliary dispersant b further contains a carbon chain not less than C8.

[0015] In a specific embodiment, the auxiliary dispersant b is polyoxyethylene ether.

[0016] In a specific embodiment, the wetting agent is an amide wetting agent used in the pesticide field, including any one or more of formamide, acetamide, propionamide, N-methyl-2-pyrrolidone, and N,N-dimethylformamide.

[0017] In a specific embodiment, the defoaming agent is a polysiloxane defoaming agent used in the pesticide field, including any one or more of methyl silicone oil, ethyl silicone oil, amino silicone oil, mercapto silicone oil, hexamethylcyclooctasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclotetrasiloxane, and octamethyltetrasiloxane.

[0018] In a specific embodiment, the thickener is a thickener used in the pesticide field, including any one of xanthan gum, hydroxypropyl cellulose or polyvinyl pyrrolidone.

[0019] In a second aspect, the present application provides a method for preparing a spirodiclofen suspension, using the following technical solution:

[0020] A method for preparing a spirodiclofen suspension comprises the following steps:

[0021] Weigh water, defoamer and wetting agent according to weight percentage, mix well at room temperature, and record as liquid A;

[0022] Weigh spirodiclofen technical, auxiliary dispersant a, and auxiliary dispersant b according to weight percentage, add to solution A and mix well to obtain solution B;

[0023] Liquid B is subjected to high-speed shearing for 3-5 minutes, and then ground to particles with an average particle size of 3-5 μm. Finally, a thickener is added according to weight percentage, and the mixture is mixed to obtain the spirodiclofen suspension.

[0024] In a third aspect, the present application provides an application of a spiroclofen suspension for controlling citrus red spider mites.

[0025] In summary, the present application has the following beneficial effects: the present application improves the storage period and high temperature stability of the spirodiclofen suspension by using auxiliary dispersant a, auxiliary dispersant b, wetting agent, defoaming agent and thickener, while also increasing its wettability and retention time on citrus leaves, properly optimizing the technical problems in the prior art, and having a positive effect on the prevention and control of citrus red spider mites. At the same time, it also reduces the damage of spirodiclofen to the ecological environment around citrus planting areas, which has significant practical significance. DETAILED DESCRIPTION

[0026] The present application is further described in detail below with reference to the embodiments.

[0027] As a drug for controlling citrus spider mites, spirodiclofen is mainly used in suspensions, and an important indicator of suspensions is the suspension rate. The higher the suspension rate, the more stable the active ingredients of spirodiclofen are in the drug system. The lower the suspension rate, the more aggregation and deposition of spirodiclofen molecules occur, and the particle size increases, thereby reducing its efficacy. When using existing spirodiclofen, there are technical problems such as the increase in particle size after long-term use and the increase in particle size as the storage temperature increases, thereby reducing the suspension rate. The applicant mainly studied a large number of literatures and combined with actual experiments to find that although spirodiclofen molecules are soluble in water, they have poor stability and are easily affected by external temperature and storage time. The main reason may be that in the spirodiclofen suspension, spirodiclofen mainly forms a suspension in the form of suspended particles with a particle size of about 5 μm. As the temperature increases, the probability of collision between particles increases, thereby leading to the aggregation of particles; the storage time causes the effect of spirodiclofen suspension to deteriorate, which is also a similar mechanism. Therefore, in order to increase the stability of the spirodiclofen suspension, it is necessary to use spirodiclofen as the base and supplement it with an auxiliary agent with good dispersibility, and use the auxiliary agent with good dispersibility to stably disperse spirodiclofen in the system.

[0028] Based on the above ideas, the applicant found through a large number of experiments that adding auxiliary dispersant a and auxiliary dispersant b to jointly construct a dispersion system can make the spirodiclofen suspension stable and long-lasting. It should be noted that auxiliary dispersant a and auxiliary dispersant b are only used to distinguish the two dispersants, and are simply classified in combination with the functional groups or functions of the optional dispersants. There is no order of precedence, nor is there a subordinate or primary and secondary relationship. All practices that reverse, change and transform their names without creative thinking are within the scope of protection of this application. At first, the applicant added two commonly used dispersants: polyethylene glycol and acrylate, and found that they can indeed have some dispersion effects, but the effect is minimal, and there is no substantial improvement in the storage time of spirodiclofen. Later, the applicant considered increasing the types and number of functional groups that form hydrogen bonds, and found through experiments that when the auxiliary dispersant a contains amino and ester groups in the molecule, and the auxiliary dispersant b contains hydroxyl and ether bonds in the molecule, the improvement of the storage stability of spirodiclofen is greater than that of polyethylene glycol and acrylate. On this basis, the applicant also found that when auxiliary dispersant b is present, if auxiliary dispersant a is diethyl aminopropionate, the dispersion effect is very unstable, sometimes the dispersion effect is not obvious, and sometimes even the storage stability of spirodiclofen is reduced. When auxiliary dispersant a is replaced with ethyl aminoacrylate, the storage stability of spirodiclofen is significantly improved. The reason may be that diethyl aminopropionate already contains a carbon-oxygen double bond. If another carbon-oxygen double bond is formed at the conjugated position of the ester group, it will certainly disperse the electron cloud density and stabilize the ester group. However, the electron distribution of the carbon-oxygen double bond is more inclined to form hydrogen bonds or intermolecular forces with water molecules, and lose or weaken the original intention of interacting with the groups in the spirodiclofen molecule. Therefore, the priority of diethyl aminopropionate to form hydrogen bonds or intermolecular forces with water molecules over the formation of hydrogen bonds or intermolecular forces with spirodiclofen is random as the conditions change. Therefore, the dispersion effect of diethyl aminoacrylate on spirodiclofen is unstable. Combined with the functional groups of auxiliary dispersant a, it can be inferred that in order to maintain molecular polarity and reduce the interaction between auxiliary dispersant a and water, it is best to have an electron-rich carbon-carbon unsaturated bond, preferably a carbon-carbon double bond, at the conjugated position of the ester group of auxiliary dispersant a. Therefore, after theoretical analysis and actual experimental results, auxiliary dispersant a is preferably amino acrylate. For auxiliary dispersant b, the applicant found that when auxiliary dispersant a was used alone, it had a certain dispersing effect, but it was not significant. Therefore, another auxiliary agent with dispersing effect was needed to cooperate with a to achieve the dispersing effect on spirodiclofen.In the initial experiments, the applicant found that the auxiliary dispersants a and b contain amino groups, ester groups, non-carbon oxygen unsaturated bonds, hydroxyl groups, and ether bonds, which "pull" and disperse the small particles of spirodiclofen into the water, achieving a "hand-in-hand" dispersion effect, thereby preparing a relatively stable suspension concentrate. Initially, the applicant used a small molecule auxiliary dispersant b, most of which were C4 / C5 / C6 carbon chains. After a large number of experiments and with the help of a laser particle size analyzer, it was found that if the carbon chain length of the auxiliary dispersant b was too small, the small molecule auxiliary dispersants a and b would tend to be more "encapsulated" rather than "dispersed", so that the solubility of some small pieces of spirodiclofen would increase and approach complete dissolution, while most of the spirodiclofen would be almost freely suspended in the system. During the storage stability experiment, the amount of spirodiclofen precipitation was significant, resulting in its suspension rate being similar to that without the addition of auxiliary agents, or even worse. When the applicant switched to compounds with carbon chains longer than C8, it was found that polyoxyethylene ethers with a carbon chain length of not less than C8 could form a more stable spatial structure. This spatial structure could reduce the collision and aggregation between the component molecules, thereby facilitating the improvement of the suspension rate of spirodiclofen. At the same time, polyoxyethylene ethers with a carbon chain length of not less than C8 could generate stronger van der Waals forces and dispersion forces, thereby increasing the interaction between b and spirodiclofen molecules, thereby increasing the suspension rate of spirodiclofen and the stability of the system.

[0029] So far, the defect of storage stability of spirodiclofen has been optimized. However, in my country, citrus is grown in a wide area, especially in Guangdong and Guangxi, where the temperature is high all year round. Fruit farmers usually use spirodiclofen immediately after purchase because the suspension of spirodiclofen has poor heat resistance. The higher the temperature, the greater the chance of aggregation and precipitation of spirodiclofen. This disadvantage of aggregation under high temperature seems to limit the use of spirodiclofen to some extent. For example, spraying at high temperature at noon, storing indoors with high room temperature, and storing in direct sunlight may all reduce the efficacy of spirodiclofen. After preliminarily determining the most preferred auxiliary dispersants a and b, the applicant conducted further experiments to reproduce the effect of the two on the stability of spirodiclofen. In the reproduction experiment, the applicant found that auxiliary dispersants a and b significantly improved the stability of spirodiclofen. This significant improvement was not only reflected in the storage time, but also in the heat resistance and activity retention. Through the synergistic cooperation of auxiliary dispersants a and b, the initial aggregation temperature of the spirodiclofen suspension was increased by about 5°C. The applicant combined the synergistic mechanism of auxiliary dispersants a and b, and analyzed the relevant literature, and the reason may be (Take the auxiliary dispersant a as aminoacrylate and the auxiliary dispersant b as polyoxyethylene ether as an example): First, the polarity of aminoacrylate and polyoxyethylene ether is compatible with spirodiclofen, and can produce strong interactions with spirodiclofen molecules. This interaction based on polarity and hydrogen bonding can make aminoacrylate and polyoxyethylene ether adsorb on the polar groups of spirodiclofen molecules, forming a relatively stable protective layer with a certain closed structure; at the same time, in terms of surface tension, the surface tension of aminoacrylate and polyoxyethylene ether is small, so that the two can better penetrate into the spirodiclofen molecules, thereby improving the dispersibility and stability of spirodiclofen suspension. In addition, in terms of stability, aminoacrylate molecules contain amino and acrylate groups, and the interaction between these groups can make it have certain flexibility and ductility. At the same time, aminoacrylate also has a low glass transition temperature, which makes it have good flexibility and ductility in a wide temperature range. And polyoxyethylene ether molecules contain multiple ether bonds, and the interaction between these ether bonds can also make it have certain flexibility and ductility. In addition, polyoxyethylene ether also has a low crystallization temperature and high molecular chain flexibility, which makes it have good flexibility and ductility in a wide temperature range. When amino acrylate and polyoxyethylene ether form a protective film, their flexibility and ductility can complement each other, further improving the overall performance of the protective film. This flexibility and ductility allows the protective film to change with the temperature and pressure of the system, thereby better adapting to changes in the system. When the temperature of the system rises, the protective film can expand with the change of temperature to prevent the aggregation and precipitation of spirodiclofen molecules. At the same time, the protective film can also reduce the temperature of the system by absorbing heat, thereby preventing the suspended particles of spirodiclofen from being precipitated by heat.

[0030] In order to further increase the storage effect and stability of the spiroclofoam suspension, the applicant also added a defoamer, a thickener and a wetting agent to the components. Among them, the wetting agent, the defoamer and the thickener can be selected from the defoamers, wetting agents and thickeners commonly used in the spiroclofoam suspension in the pesticide field. For example, the wetting agent can be an amide wetting agent, specifically formamide, acetamide, propionamide, N-methyl-2-pyrrolidone, N,N-dimethylformamide, the defoamer can be a polysiloxane defoamer with excellent performance, specifically methyl silicone oil, ethyl silicone oil, amino silicone oil, mercapto silicone oil, hexamethylcyclooctasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclotetrasiloxane, octamethyltetrasiloxane, and the thickener can be an auxiliary agent for increasing viscosity, specifically xanthan gum, hydroxypropyl cellulose or polyvinyl pyrrolidone. When the applicant selected the defoamer, the thickener and the wetting agent, it was found that when the wetting agent was a mixture of N-methyl-2-pyrrolidone and N,N-dimethylformamide, the defoamer was a mixture of mercaptosilicone oil and octamethyltetrasiloxane, and the thickener was xanthan gum, the stability of the spirodiclofen suspension during and after the preparation was improved, especially the wettability on citrus leaves was significantly improved. This means that when the defoamer, the wetting agent and the thickener are the above substances, the spirodiclofen suspension of the present application can increase the adhesion on the citrus leaves, the degree of decline in efficacy after spraying for 72 hours is small, the spraying cycle of spirodiclofen will also be increased, and the damage of spirodiclofen to the ecological environment is reduced.

[0031] In summary, the present application improves the storage period and high temperature stability of the spirodiclofen suspension by using auxiliary dispersant a, auxiliary dispersant b, wetting agent, defoaming agent and thickener, while also increasing its wettability and retention time on citrus leaves, properly optimizing the technical problems in the prior art, and having a positive effect on the prevention and control of citrus red spider mites. At the same time, it also reduces the damage of spirodiclofen to the ecological environment around citrus planting areas, which has significant practical significance.

[0032] The solution of the present application is further explained below in conjunction with specific embodiments.

[0033] Example

[0034] Example 1

[0035] The present application provides a spirodiclofen suspension, the preparation method of which comprises the following steps:

[0036] 1. Weigh 84.4wt% water, 0.2wt% defoamer, and 0.2wt% wetting agent, mix at 60r / min for 15min at room temperature, and record it as liquid A;

[0037] 2. Weigh 10wt% of spirodiclofen technical, 4wt% of auxiliary dispersant a, and 1wt% of auxiliary dispersant b, add them into solution A, and mix at 60r / min for 15min to obtain solution B;

[0038] 3. Liquid B was sheared at high speed for 3 minutes using a T-25 shearing machine, and then ground using a sand mill until the average particle size of the particles was 3-5 μm. Finally, 0.2 wt% of a thickener was added and mixed at 60 r / min for 15 minutes to obtain a spirodiclofen suspension.

[0039] In this embodiment 1, the auxiliary dispersant a is amino ethyl acrylate, the auxiliary dispersant b is polyoxyethylene ether, the wetting agent is N-methyl-2-pyrrolidone and N,N-dimethylformamide compounded in a weight ratio of 1:2, the defoaming agent is mercapto silicone oil and octamethyltetrasiloxane compounded in a weight ratio of 1:1, and the thickener is xanthan gum.

[0040] Example 2

[0041] The present application provides a spirodiclofen suspension, the preparation method of which comprises the following steps:

[0042] 1. Weigh 78.6wt% water, 0.3wt% defoamer, and 0.3wt% wetting agent, mix at 70r / min for 12min at room temperature, and record it as liquid A;

[0043] 2. Weigh 15wt% of spirodiclofen technical, 4.2wt% of auxiliary dispersant a, and 1.3wt% of auxiliary dispersant b, add them to solution A, and mix at 70r / min for 12min to obtain solution B;

[0044] 3. Liquid B was sheared at high speed for 4 minutes using a T-25 shearing machine, and then ground using a sand mill until the average particle size of the particles was 3-5 μm. Finally, 0.3 wt % of a thickener was added and mixed at 70 r / min for 12 minutes to obtain a spirodiclofen suspension.

[0045] The types of the auxiliary agents in this embodiment are the same as those in embodiment 1, and the only difference is the dosage.

[0046] Example 3

[0047] The present application provides a spirodiclofen suspension, the preparation method of which comprises the following steps:

[0048] 1. Weigh 76.2wt% water, 0.4wt% defoamer, and 0.4wt% wetting agent, mix at 70r / min for 13min at room temperature, and record it as liquid A;

[0049] 2. Weigh 18wt% of spirodiclofen technical, 4.6wt% of auxiliary dispersant a, and 1.4wt% of auxiliary dispersant b, add to solution A, and mix at 70r / min for 13min to obtain solution B;

[0050] 3. Liquid B was sheared at high speed for 4 minutes using a T-25 shearing machine, and then ground using a sand mill until the average particle size of the particles was 3-5 μm. Finally, 0.4 wt% of a thickener was added and mixed at 70 r / min for 13 minutes to obtain a spirodiclofen suspension.

[0051] The types of the auxiliary agents in this embodiment are the same as those in embodiment 1, and the only difference is the dosage.

[0052] Example 4

[0053] The present application provides a spirodiclofen suspension, the preparation method of which comprises the following steps:

[0054] 1. Weigh 70.2wt% water, 0.4wt% defoamer, and 0.4wt% wetting agent, mix at 70r / min for 14min at room temperature, and record it as liquid A;

[0055] 2. Weigh 22wt% of spirodiclofen technical, 4.8wt% of auxiliary dispersant a, and 1.8wt% of auxiliary dispersant b, add them to solution A, and mix at 70r / min for 13min to obtain solution B;

[0056] 3. Liquid B was sheared at high speed for 4 minutes using a T-25 shearing machine, and then ground using a sand mill until the average particle size of the particles was 3-5 μm. Finally, 0.4 wt% of a thickener was added and mixed at 70 r / min for 13 minutes to obtain a spirodiclofen suspension.

[0057] The types of the auxiliary agents in this embodiment are the same as those in embodiment 1, and the only difference is the dosage.

[0058] Example 5

[0059] The present application provides a spirodiclofen suspension, the preparation method of which comprises the following steps:

[0060] 1. Weigh 67.5wt% water, 0.5wt% defoamer, and 0.5wt% wetting agent, and mix at 80r / min for 10min at room temperature, which is called liquid A;

[0061] 2. Weigh 24wt% of spirodiclofen technical, 5wt% of auxiliary dispersant a, and 2wt% of auxiliary dispersant b, add them into solution A, and mix at 80r / min for 10min to obtain solution B;

[0062] 3. Liquid B was sheared at high speed for 5 minutes using a T-25 shearing machine, and then ground using a sand mill until the average particle size of the particles was 3-5 μm. Finally, 0.5 wt % of a thickener was added and mixed at 80 r / min for 10 minutes to obtain a spirodiclofen suspension.

[0063] The types of the auxiliary agents in this embodiment are the same as those in embodiment 1, and the only difference is the dosage.

[0064] Embodiment 6-8

[0065] Compared with Example 1, Examples 6 to 8 differ in that the defoaming agents are different, as shown in Table 1.

[0066] Table 1

[0067]

[0068] Embodiments 9 to 11

[0069] Compared with Example 1, Examples 9 to 11 differ in that the wetting agents are different, as shown in Table 2.

[0070] Table 2

[0071]

[0072] Embodiment 12-13

[0073] Compared with Example 1, Examples 12 to 13 differ in that the thickeners are different, as shown in Table 3.

[0074] Table 3

[0075]

[0076] Comparative Example 1

[0077] Compared with Example 1, the present application is different in that the auxiliary dispersant a of the present application is diethyl aminopropionate.

[0078] Comparative Example 2

[0079] Compared with Example 1, the present application is different in that the auxiliary dispersant b of the present application is diethylene glycol.

[0080] Comparative Example 3

[0081] Compared with Example 1, the present application is different in that the auxiliary dispersant b of the present application is triethylene glycol.

[0082] The above embodiments and comparative examples were subjected to performance testing. The test results are shown in Tables 4 and 5. The following are some of the main test indicators and corresponding test methods:

[0083] 1. Suspension rate: Test in accordance with the relevant provisions of GB / T 14825-2006.

[0084] 2. Storage stability:

[0085] 1. Thermal storage stability: Referring to the relevant provisions of GB / T 19136-2021, 20 ml of the emulsion prepared in each embodiment and comparative example was taken, placed in an ampoule, sealed, and stored in a constant temperature box at 54±2°C for 14 days, and its performance was tested.

[0086] 2. Cold storage stability: Referring to the relevant provisions of GB / T 19137-2003, 20 ml of the emulsion prepared in the corresponding examples and comparative examples were placed in an ampoule, sealed, and cold stored at -5°C. After 24 hours, the ampoule was returned to room temperature and its performance was tested after melting.

[0087] 3. Biological detection of duration of drug efficacy: Samples of insect-infested citrus trees were selected, with each embodiment and comparative example as the sample, and the insect population reduction rate was calculated according to the application method, investigation time and method disclosed in the article "Effectiveness Experiment of Different Agents for Controlling Citrus Red Spider" in Volume 33, Issue 5 of "Southern Horticulture", so as to characterize the duration of drug efficacy of each embodiment and comparative example.

[0088] Table 4

[0089]

[0090] Table 5

[0091]

[0092] Result analysis:

[0093] Combining the test results of Table 4 and Table 5, as well as Examples 1 to 5, it can be seen that the auxiliary dispersants a and b of Examples 1 to 5 have a more significant effect on increasing the suspension rate of the spirodiclofen aqueous system, and have good heat storage stability and cold storage stability. In addition, no heat-resistant or cold-resistant adjuvant is required to be added to the components. The storage stability of the spirodiclofen suspension is increased by relying on the dispersion and film-forming effects of the auxiliary dispersants a and b. At the same time, Examples 1 to 5 also have good wettability and residual drug effect time: Combining Table 5, it can be seen that in the process of 14 days to 28 days after the application of the drug, the insect population reduction rate of Examples 1 to 5 is mostly increasing (only the insect population rate of Example 2 on the 28th day decreased, but combined with the derivation rate of citrus red spider, it can be seen that the drug effect of Example 2 continued to decay from 14 days to 28 days after the application of the drug, and completely failed in the period close to 28 days of the application of the drug. If the drug effect of Example 2 fails after 14 days of the application, The insect population decay rate after 28 days of application will certainly be much less than 85%). Therefore, the present application provides a spirodiclofen suspension with high suspension rate, stable storage, long efficacy time and long application cycle through the synergistic cooperation between auxiliary dispersant a, auxiliary dispersant b and other auxiliary components. Combined with the existing available field tests, the insect population decay rate of Examples 1 to 5 after 28 days of application is also extremely excellent, which greatly improves the technical problems of poor wettability, poor residual efficacy and short application cycle of ordinary spirodiclofen acaricides.

[0094] Combining Examples 6 to 13 with Example 1, it can be seen that the types of auxiliary agents in Example 1 of the present application are the most preferred, but not the only choice. The use of the other auxiliary agents disclosed in this application can also achieve good results, but the test results are not as good as those in Example 1.

[0095] Instructions for use and precautions:

[0096] 1. The spirodiclofen suspension provided in the present application should be applied at the early stage of citrus red spider mite damage, and the front and back sides of crop leaves, fruit surfaces, tree trunks, branches, etc. should be fully and evenly coated with the drug during application.

[0097] 2. This application only needs to be applied once in each growing season of citrus trees, with a safe interval of 30 days; do not apply the pesticide on windy days or 1 hour before rain.

[0098] 3. This application is not recommended for use in combination with other agents with different mechanisms to prevent the mites from developing drug resistance.

[0099] 4. This application is toxic to bees, fish and other aquatic organisms, and silkworms. Avoid affecting the surrounding bee colonies during application. It is forbidden to use it near flowering plants, silkworm rooms and mulberry gardens. Keep away from aquaculture areas, rivers and ponds, and it is forbidden to wash the application equipment in rivers and ponds. It is forbidden to use it in areas where natural enemies such as trichogrammatids are released.

[0100] 5. When preparing and using this product, you should wear protective clothing, gloves and masks. Smoking and eating are strictly prohibited.

[0101] 6. Pregnant and lactating women are prohibited from using this product.

[0102] 7. After using the medicine, wash your hands, face, other exposed body parts, and clothes contaminated by the medicine with soap and plenty of water.

[0103] 8. Empty bottles after use should be properly disposed of and should not be used for other purposes or discarded at will.

[0104] 9. It is prohibited to release natural enemies such as trichogrammatids in the area.

[0105] 10. It is prohibited to raise fish, shrimps and crabs in rice fields, and the pesticide solution after application is prohibited to be discharged into the water body.

[0106] 11. This product should be stored in a dry, cool, ventilated, rainproof place, away from fire or heat sources. Keep it out of reach of children and unauthorized persons and lock it. Do not store or transport it together with other commodities such as food, beverages, grain, feed, etc.

[0107] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A spirodiclofen suspension, characterized in that: The invention comprises the following components in percentage by weight: 10-24 wt% of spirodiclofen, 4-5 wt% of auxiliary dispersant a, 1-2 wt% of auxiliary dispersant b, 0.2-0.5 wt% of defoamer, 0.2-0.5 wt% of thickener, 0.2-0.5 wt% of wetting agent, and the balance is water; Wherein, the auxiliary dispersant a is amino ethyl acrylate, and the auxiliary dispersant b is polyoxyethylene ether.

2. The spirodiclofen suspension concentrate according to claim 1, characterized in that: The wetting agent is an amide wetting agent used in the pesticide field, including any one or more of formamide, acetamide, propionamide, N-methyl-2-pyrrolidone, and N,N-dimethylformamide.

3. The spirodiclofen suspension concentrate according to claim 1, characterized in that: The defoamer is a polysiloxane defoamer used in the pesticide field, including any one or more of methyl silicone oil, ethyl silicone oil, amino silicone oil, mercapto silicone oil, hexamethylcyclooctasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclotetrasiloxane, and octamethyltetrasiloxane.

4. The spirodiclofen suspension concentrate according to claim 1, characterized in that: The thickener is a thickener used in the field of pesticides, including any one of xanthan gum, hydroxypropyl cellulose or polyvinyl pyrrolidone.

5. The method for preparing a spirodiclofen suspension concentrate according to any one of claims 1 to 4, characterized in that: The steps include: Weigh water, defoamer and wetting agent according to weight percentage, mix well at room temperature, and record as liquid A; Weigh spirodiclofen technical, auxiliary dispersant a, and auxiliary dispersant b according to weight percentage, add to solution A and mix well to obtain solution B; Liquid B is subjected to high-speed shearing for 3-5 minutes, and then ground to particles with an average particle size of 3-5 μm. Finally, a thickener is added according to weight percentage, and the mixture is mixed to obtain the spirodiclofen suspension.

6. The use of a spirodiclofen suspension concentrate according to any one of claims 1 to 4, characterized in that: Used for the control of citrus red spider mites.

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