Momyl soluble powder as well as preparation method and application thereof

Abstract

The invention discloses methomyl soluble powder and a preparation method and application thereof, and relates to the field of pesticides, the methomyl soluble powder comprises the following raw materials by weight: 50-95% of methomyl, 0.1-10% of a wetting dispersant, 0.1-10% of an anti-caking agent, and 0-49.8% of a filler. According to the soluble powder disclosed by the invention, the problem that methomyl soluble powder is easy to cake is reduced or eliminated by selecting auxiliaries, long-time storage is facilitated, sub-packaging is easy, the problem of dissolution stability is solved, and the methomyl soluble powder is more uniform and more stable in the use process.

Description

Technical Field

[0001] The invention relates to the technical field of pesticides, and in particular to a methomyl soluble powder, a preparation method of the methomyl soluble powder, and a use method and application of the methomyl soluble powder in preventing and controlling farmland plant pests. Background Art

[0002] Methomyl is 1-(methylthio)ethylene aminomethyl carbamate, also known as methomyl, wanling, ethoxycarb, and methomyl. It is a carbamate systemic insecticide that can effectively kill the eggs, larvae, and adults of many pests. It has dual effects of contact killing and stomach poisoning. After entering the insect body, it inhibits acetylcholinesterase, making it impossible to decompose acetylcholine, which plays an important role in insect nerve conduction, causing the nerve impulse to be unable to control transmission, causing convulsions, overexcitement, paralysis and tremors in the insect, and making it unable to feed, and eventually die. After the insect eggs come into contact with the agent, they usually cannot survive the blackhead stage, and even if they hatch, they will die soon. Methomyl is a highly toxic pesticide (harmful to the human nervous system. After poisoning, atropine 0.5-2 mg can be taken orally or intramuscularly. In severe cases, epinephrine can be added. Pralidoxime, pralidoxime, bisphosphonium chloride, and morphine are prohibited for detoxification). It can only be used on crops that have been approved and registered in my country. This drug cannot be mixed with Bordeaux mixture, lime sulfur, and pesticides containing iron or tin.

[0003] Methamidophos is a highly toxic pesticide that is harmful to the human nervous system. It will cause harm to workers during both processing and use. Therefore, reducing the toxicity of highly toxic pesticides, improving their protective effects, and reducing the amount of pesticides used are currently popular research directions.

[0004] Methomyl has unique systemic, contact and stomach poisoning effects, and is highly active against eggs, larvae and adults of pests. However, it is also found that methomyl is highly toxic and harmful to the human body. When methomyl is processed into soluble powder, it is very easy to agglomerate due to the strong moisture absorption of methomyl technical, which also affects the efficacy of the drug to a certain extent. In addition, a large amount of dust is easily generated during the production process, which poses a great threat to operators. Summary of the invention

[0005] Purpose of the Invention

[0006] In order to overcome the above-mentioned shortcomings, the purpose of the present invention is to provide a soluble powder of methomyl and a preparation method and application thereof. The present invention makes the soluble powder of methomyl not only have a high content of active ingredients but also have good performance through the selection of auxiliary agent types and auxiliary agent components; at the same time, a large amount of research and screening are carried out on production equipment, and finally the production of the soluble powder of methomyl is made cleaner and more efficient through specific mixing and crushing methods.

[0007] Solution

[0008] To achieve the purpose of the present invention, the technical solution adopted by the present invention is as follows:

[0009] In a first aspect, the present invention provides a methomyl soluble powder, which comprises the following raw materials in percentage by weight: 50-95% of methomyl, 0.1-10% of a wetting and dispersing agent, 0.1-10% of an anti-caking agent, and 0-49.8% of a filler.

[0010] Furthermore, the anti-caking agent is one or more of sodium aluminosilicate, tricalcium phosphate, silicon dioxide, microcrystalline cellulose, silicate, and calcium stearate.

[0011] Furthermore, the filler is one or more water-soluble fillers such as potassium sulfate, potassium chloride, diammonium hydrogen phosphate, urea, anhydrous sodium sulfate, and ammonium sulfate.

[0012] In the above-mentioned soluble powders, wetting and dispersing agents, anti-caking agents and fillers are collectively referred to as auxiliary agents. The function of the wetting and dispersing agent is to reduce the liquid-solid surface tension of fine particles in water, increase the ability to be wetted by water, prevent the fine particles of the active pharmaceutical ingredient from aggregating with each other, and enable them to remain evenly dispersed for a long time in the liquid-solid dispersion system formed with water. The function of the anti-caking agent is to prevent the powder from agglomerating during long-term storage. The function of the filler is to load or dilute the active pharmaceutical ingredient and adjust the product content to meet the standard.

[0013] Furthermore, it comprises the following raw materials in percentage by weight: 50-95% of methomyl, 1-10% of wetting and dispersing agent, 0.1-10% of anti-caking agent and 1-48.9% of filler.

[0014] Furthermore, it comprises the following raw materials in percentage by weight: 85-94% of methomyl, 0.5-1.5% of wetting and dispersing agent, 4.5-5.5% of anti-caking agent and 1-10% of filler.

[0015] Furthermore, it comprises the following raw materials in percentage by weight: 88-92% of methomyl, 1-1.2% of wetting and dispersing agent, 4.5-5.5% of anti-caking agent and 2-6.5% of filler.

[0016] Furthermore, it comprises the following raw materials in percentage by weight: 88-92% of methomyl, 1% of wetting and dispersing agent, 5% of anti-caking agent and 2-6% of filler.

[0017] Furthermore, it comprises the following raw materials in percentage by weight: 90% of methomyl, 1% of wetting and dispersing agent, 5% of anti-caking agent and 4% of filler.

[0018] Furthermore, it comprises the following raw materials in percentage by weight: 90% of methomyl, 51% of wetting and dispersing agent MF-5, 5% of anti-caking agent, and 4% of filler; optionally, the anti-caking agent is silicon dioxide.

[0019] Further, the filler is added to 100%.

[0020] Further, the wetting and dispersing agent is one or more of sodium lignin sulfonate, maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, alkylnaphthalenesulfonic acid formaldehyde condensate sodium salt, naphthalenesulfonic acid formaldehyde condensate sodium salt, alkyl polyoxyethylene ether sodium sulfate, ethylene oxide-propylene oxide block copolymer, polycarboxylic acid sodium salt, sodium dodecyl sulfate, sodium dodecyl ether sulfate, sodium alkylnaphthalene sulfonate, sodium α-olefin sulfonate, alkylphenol polyoxyethylene ether sodium sulfate, sodium diisobutylnaphthalene sulfonate, fatty acid sulfate, fatty acid ester sulfate, and MF-5.

[0021] The wetting and dispersing agents include sodium lauryl sulfate, sodium lauryl ether sulfate and polycarboxylic acid sodium salt.

[0022] Furthermore, the wetting and dispersing agent is MF-5 (mainly a mixture of sodium lauryl sulfate, sodium lauryl ether sulfate and sodium polycarboxylate), and the anti-caking agent is silicon dioxide.

[0023] Furthermore, the wetting and dispersing agent is naphthalenesulfonic acid formaldehyde condensate sodium salt, and the anti-caking agent is silicon dioxide.

[0024] Furthermore, the wetting and dispersing agent is sodium lignin sulfonate, and the anti-caking agent is sodium aluminosilicate.

[0025] Furthermore, the wetting and dispersing agent is alkylnaphthalenesulfonic acid formaldehyde condensate sodium salt, and the anti-caking agent is microcrystalline cellulose.

[0026] Furthermore, the wetting and dispersing agent is sodium diisobutylnaphthalene sulfonate, and the anti-caking agent is silicate.

[0027] Furthermore, the wetting and dispersing agent is sodium lauryl sulfate, and the anti-caking agent is calcium stearate.

[0028] Further, the wetting and dispersing agent is sodium lignin sulfonate and sodium alkylphenol sulfonate, and the anti-caking agent is sodium aluminosilicate;

[0029] Furthermore, the wetting and dispersing agent is polycarboxylic acid sodium salt, and the anti-caking agent is microcrystalline cellulose.

[0030] Furthermore, the wetting and dispersing agent is sodium dodecyl sulfate, naphthalenesulfonic acid formaldehyde condensate sodium salt and polycarboxylic acid sodium salt, and the anti-caking agent is silicon dioxide.

[0031] Furthermore, the silicon dioxide is white carbon black.

[0032] When the soluble powder selects the above-mentioned wetting and dispersing agent, anti-caking agent and filler, the soluble powder is tested and found that when the auxiliary agent selects the following preferred auxiliary agent, the fluidity and dissolution stability of the soluble powder are greatly improved, and the occurrence of caking is effectively avoided during long-term storage. Preferably, the wetting and dispersing agent MF-5 is mainly a mixture of sodium lauryl sulfate, sodium lauryl ether sulfate and polycarboxylate sodium salt; the anti-caking agent is white carbon black; the filler is anhydrous sodium sulfate, and the anhydrous sodium sulfate is supplemented to 100%.

[0033] Furthermore, the weight ratio of the wetting and dispersing agent to the anti-caking agent is 1:(0.5-10), optionally 1:

[0034] (0.8~5), optionally 1:(1~5), optionally 1:5.

[0035] Furthermore, the particles in the powder have a particle size of ≤75 μm reaching 99.9%.

[0036] Furthermore, the particle size distribution D[4,3] in the powder is 55 to 74 μm, optionally 60 to 72 μm, optionally 64 to 72 μm.

[0037] In the second aspect, a method for preparing the methomyl soluble powder described in the first aspect is provided, wherein methomyl, a wetting and dispersing agent, an anti-caking agent and a filler are uniformly mixed and crushed to obtain the methomyl soluble powder, and the powder is optionally crushed to a particle size of ≤ 75 μm up to 99.9%.

[0038] Further, the pulverization adopts a mechanical ultrafine pulverizer or an air flow pulverizer. Optionally, the air flow pulverizer includes one or two of a flat air flow pulverizer, a vertical circulating tube air flow pulverizer, a counter-impact air flow pulverizer, a collision air flow pulverizer, a counter-jet fluidized bed air flow pulverizer, a universal pulverizer, a turbine self-cooling pulverizer, an impact ultrafine pulverizer, an impact mill, an ultrafine impact mill and a mechanical ultrafine pulverizer.

[0039] Furthermore, secondary mixing is performed after the pulverization.

[0040] Furthermore, the machines used for mixing are one or two of a plowshare mixer, a ribbon mixer, a zero-gravity mixer, a V-type mixer, a double-helix cone mixer, a high-speed or low-speed liquid mixer, and a planetary power mixer.

[0041] In a third aspect, a method for using the methomyl soluble powder described in the first aspect or the methomyl soluble powder prepared by the preparation method described in the second aspect is provided, characterized in that the methomyl soluble powder is diluted with water and applied by spraying, and optionally, the dilution multiple is 2000-5000 times.

[0042] In a fourth aspect, there is provided a use of the soluble powder of methomyl described in the first aspect, or the soluble powder of methomyl prepared by the preparation method described in the second aspect, in controlling plant pests in farmland; optionally, the plant pests include one or more of cotton bollworm, aphids, thrips, red spiders, leaf rollers, armyworms, and Spodoptera litura, and the powder is particularly effective against cotton bollworm.

[0043] Beneficial Effects

[0044] (1) The inventors of the present invention have conducted a lot of research and screening on the auxiliary agents of the dosage form, and finally, through the selection of auxiliary agent types and auxiliary agent components, the soluble powder of methomyl not only has a high content of active ingredients but also has good performance; at the same time, a lot of research and screening were conducted on production equipment, and finally, through specific mixing and crushing methods, the production of soluble powder of methomyl was made cleaner and more efficient.

[0045] (2) The present invention uses a soluble powder of the effective active ingredient, methomyl, with a high content and a small dosage, and has a special effect on cotton bollworm and aphid pests in crop and vegetable diseases, and has a high prevention effect. The soluble powder of the present invention reduces or eliminates the problem of easy agglomeration of the soluble powder of methomyl through the selection of auxiliary agents, is conducive to long-term storage, is easy to package, solves the problem of dissolution stability, and is more uniform and more stable during use.

[0046] (3) The soluble powder of the present invention solves the problem of dust generation during the production process through a specific processing technology, and the selected equipment has low energy consumption, which improves the particle size of the product, thereby reducing the dust hazard during use and is beneficial to environmental sustainable development. DETAILED DESCRIPTION

[0047] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0048] In addition, in order to better illustrate the present invention, numerous specific details are provided in the specific embodiments below. It should be understood by those skilled in the art that the present invention can be implemented without certain specific details. In some embodiments, raw materials, schemes, methods, means, etc. well known to those skilled in the art are not described in detail, so as to highlight the main purpose of the present invention.

[0049] Unless explicitly stated otherwise, throughout the specification and claims, the term “comprise” or variations such as “include” or “comprising”, etc., will be understood to include the stated elements or components but not to exclude other elements or components.

[0050] The above-mentioned fungicide composition provides a new option for preventing and controlling plant diseases. The present disclosure is further illustrated by examples below, but the present disclosure is not limited thereto.

[0051] Methomyl in the following examples can be obtained commercially, and other adjuvants are also commercially available products.

[0052] The present invention is further described in detail below by way of examples.

[0053] Since the hygroscopicity of methomyl raw material is very strong, it is easy to produce agglomeration problems, which also affects the efficacy of the drug to a certain extent. In addition, a large amount of dust is easily generated during the production process (especially during the crushing process), which is harmful to the operators. The present invention has tried a variety of crushing methods, and it is believed that the crushing effect of mechanical ultrafine pulverizer and air flow pulverizer is relatively good. The ultrafine pulverizer has better performance in terms of production capacity, particle size distribution and dust reduction. When the particle size of particles ≤75um reaches 99.9%, the ultrafine pulverizer has a larger average particle size and less dust, as shown in Table 1, Table 2, and Table 3 respectively.

[0054] Table 1 Comparison of production capacity between mechanical ultrafine pulverizer and air flow pulverizer

[0055]

[0056] Table 2 Comparison of particle size distribution between mechanical ultrafine pulverizer and air flow pulverizer

[0057]

[0058] Test method description: Definition of D[4,3]: Both are based on volume to express the average particle size. D[4,3] is the full name of "mass-to-volume average particle size" and is abbreviated as volume average diameter. Its calculation method is to average the particle size values ​​at both ends of each particle size interval, then multiply it by the particle size distribution content percentage corresponding to this interval, and add the accumulation of each interval.

[0059] Table 3 Comparison of dust concentration between mechanical ultrafine pulverizer and air flow pulverizer

[0060]

[0061]

[0062] Dust concentration detection method: intelligent dust sampler ZGF-30SH, dust filter membrane sampling, fixed-point sampling, collect air samples for 15 minutes at a flow rate of 20L / min (GBZ / T192.1-2007).

[0063] When the soluble powder is processed in the above-mentioned way, it has been verified that the system can prepare the product in a closed system, so that the product preparation process is dust-free. Preparation in a closed system is more friendly to workers and eliminates dust hazards. Compared with air flow crushing, mechanical crushing has low energy consumption, small air volume, reduced exhaust gas volume, and can increase the particle size of the product, thereby reducing dust hazards during use; the preferred mixer is a double-helix cone mixer, and the preferred crusher is a mechanical ultrafine crusher.

[0064] The feeding of the present invention is negative pressure feeding, which is dust-free. After being mixed by the double-helix cone mixer, the materials are conveyed to the mechanical superfine pulverizer through a feeder. After being pulverized to a suitable fineness, the negative pressure materials generated by the high-speed operation of the induced draft fan enter the cyclone separator and the dust collector through a pipeline, and then enter the double-helix cone mixer. After mixing, the materials enter the automatic packaging machine to complete packaging. The entire system is a fully sealed system without negative pressure generation, dust, and is environmentally friendly.

[0065] The present invention also attempts to select different adjuvants to prepare the soluble powder of methomyl, and some embodiments are as follows:

[0066] Example 1: 50% Methomyl soluble powder

[0067] The formula is: 50% of methomyl, 10% of wetting and dispersing agent polyoxyethylene-polyoxypropylene block copolymer, 10% of anti-caking agent aluminum silicate, and filler potassium sulfate added to 100%.

[0068] The preparation method is as follows: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a coulter mixer and mix them evenly; grind them into particles with a particle size of 99.9% or less of 75 μm by an impact ultrafine grinder; and then perform secondary mixing in the coulter mixer to obtain the methomyl soluble powder after mixing evenly.

[0069] Example 2: 65% Methomyl soluble powder

[0070] The formula is: 65% of methomyl, 8.5% of wetting and dispersing agent sodium salt of alkyl naphthalene sulfonic acid formaldehyde condensate, 7.5% of anti-caking agent tricalcium phosphate, and filler ammonium sulfate added to 100%.

[0071] Preparation method: put the methomyl, wetting dispersant, anti-caking agent and filler into a double-screw cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a flat air flow mill, and then mix them for the second time in a zero-gravity mixer to obtain the methomyl soluble powder after mixing evenly.

[0072] Example 3: 75% Methomyl soluble powder

[0073] The formula is: 75% of methomyl, 6.5% of wetting and dispersing agent sodium alkyl polyoxyethylene ether sulfate, 6.5% of anti-caking agent white carbon black, and filler diammonium hydrogen phosphate added to 100%.

[0074] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a double-screw cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a collision-type airflow mill, and then mix them for the second time in a ribbon mixer to obtain the methomyl soluble powder after mixing evenly.

[0075] Example 4: 85% Methomyl soluble powder

[0076] The formula is: 85% of methomyl, 2.5% of wetting and dispersing agent sodium diisobutylnaphthalene sulfonate, 2.5% of anti-caking agent white carbon black, and filler anhydrous sodium sulfate added to 100%.

[0077] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a double-screw cone mixer and mix them evenly. After crushing them into particles with a particle size of 99.9% or less of 75 μm by a turbine self-cooling pulverizer, perform secondary mixing in a plowshare mixer and obtain the methomyl soluble powder after mixing evenly.

[0078] Example 5: 90% Methomyl Soluble Powder

[0079] The formula is: 90% of methomyl, 1.0% of wetting and dispersing agent MF-5 (mainly a mixture of sodium dodecyl sulfate + sodium dodecyl ether sulfate + sodium polycarboxylate, MF-5 purchased from Wuxi Xinying Detergent Co., Ltd.), 5.0% of anti-caking agent white carbon black, and filler anhydrous sodium sulfate added to 100%.

[0080] Preparation method: put the methomyl, wetting dispersant, anti-caking agent and filler into a double-helix cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a mechanical ultrafine grinder, mix them for the second time in the double-helix cone mixer, and obtain the methomyl soluble powder after mixing evenly.

[0081] Example 6: 90% Methomyl Soluble Powder

[0082] The formula is: 90% of methomyl, 1.0% of wetting and dispersing agent MF-5, 5% of anti-caking agent microcrystalline cellulose, and filler potassium chloride added to 100%.

[0083] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a double-helix cone mixer and mix them evenly, crush them into particles with a particle size of 99.9% or less of 75 μm by a mechanical superfine crusher, and then mix them for the second time in the double-helix cone mixer to obtain the methomyl soluble powder after mixing evenly.

[0084] Example 7: 90% Methomyl Soluble Powder

[0085] The formula is: 90% of methomyl, 1.0% of naphthalenesulfonic acid formaldehyde condensate sodium salt as wetting and dispersing agent, 5% of white carbon black as anti-caking agent, and potassium chloride as filler added to 100%.

[0086] Preparation method: put the methomyl, wetting dispersant, anti-caking agent and filler into a double-helix cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a mechanical ultrafine grinder, mix them for the second time in the double-helix cone mixer, and obtain the methomyl soluble powder after mixing evenly.

[0087] Example 8: 90% Methomyl Soluble Powder

[0088] The formula is: 90% of methomyl, 1.0% of wetting and dispersing agent sodium salt of polycarboxylate, 5% of anti-caking agent white carbon black, and potassium chloride as filler added to 100%.

[0089] Preparation method: put the methomyl, wetting dispersant, anti-caking agent and filler into a double-helix cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a mechanical ultrafine grinder, mix them for the second time in the double-helix cone mixer, and obtain the methomyl soluble powder after mixing evenly.

[0090] Example 9: 95% Methomyl Soluble Powder

[0091] The formula is: 95% of methomyl, 1% of maleic acid-acrylic acid copolymer salt as a wetting and dispersing agent, 2% of microcrystalline cellulose as an anti-caking agent, and the filler diammonium hydrogen phosphate is added to 100%.

[0092] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a ribbon mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by an ultra-fine impact mill, mix them for the second time in a ribbon mixer, and obtain the methomyl soluble powder after mixing evenly.

[0093] Example 10: 53% Methomyl soluble powder

[0094] The formula is: 53% of methomyl, 9.0% of wetting and dispersing agent polyoxyethylene-polyoxypropylene block copolymer, 9.0% of anti-caking agent calcium stearate, and filler ammonium sulfate added to 100%.

[0095] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a coulter mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by an impact ultrafine grinder, and then mix them twice in the coulter mixer to obtain the methomyl soluble powder after mixing evenly.

[0096] Example 11: 55% Methomyl Soluble Powder

[0097] The formula is: 55% of methomyl, 8.5% of wetting and dispersing agent ethylene oxide-propylene oxide block copolymer, 8.0% of anti-caking agent tricalcium phosphate, and filler ammonium sulfate added to 100%.

[0098] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a coulter mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by an impact ultrafine grinder, and then mix them twice in the coulter mixer to obtain the methomyl soluble powder after mixing evenly.

[0099] Example 12: 60% Methomyl Soluble Powder

[0100] The formula is: 60% of methomyl, 6.0% of wetting and dispersing agent sodium dodecyl sulfate, 6.5% of anti-caking agent silicate, and filler urea added to 100%.

[0101] Preparation method: put the methomyl, wetting dispersant, anti-caking agent and filler into a double-screw cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a flat air flow mill, and then mix them for the second time in a zero-gravity mixer to obtain the methomyl soluble powder after mixing evenly.

[0102] Example 13: 70% Methomyl Soluble Powder

[0103] The formula is: 70% of methomyl, 2.0% of wetting and dispersing agent sodium lauryl ether sulfate, 2.0% of sodium diisobutylnaphthalene sulfonate, 6% of anti-caking agent sodium aluminosilicate, and filler ammonium sulfate added to 100%.

[0104] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a double-screw cone mixer and mix them evenly, grind them into particles with a particle size of 99.9% or less of 75 μm by a collision-type airflow mill, and then mix them for the second time in a ribbon mixer to obtain the methomyl soluble powder after mixing evenly.

[0105] Example 14: 80% Methomyl Soluble Powder

[0106] The formula is: 80% of methomyl, 1.0% of wetting and dispersing agent sodium dodecyl sulfate + 1.0% of naphthalenesulfonic acid formaldehyde condensate sodium salt + 1.0% of polycarboxylic acid sodium salt, 5% of anti-caking agent white carbon black, and filler anhydrous sodium sulfate added to 100%.

[0107] Preparation method: put the methomyl, wetting and dispersing agent, anti-caking agent and filler into a double-screw cone mixer and mix them evenly. After crushing them into particles with a particle size of 99.9% or less of 75 μm by a turbine self-cooling pulverizer, perform secondary mixing in a plowshare mixer and obtain the methomyl soluble powder after mixing evenly.

[0108] Comparative Example 1: 90% Methomyl soluble powder

[0109] The sample was made according to Example 2 of the CN104351175A patent.

[0110] The formula is: 91% of methomyl, 4.5% of anhydrous sodium oxalate, and 4.5% of hydroxyethyl cellulose.

[0111] Preparation method: put it into the premix, mix it, and then pass it through a jet mill to grind it to 23μm (600 mesh). After the crushed materials are mixed for the second time, the soluble powder of methomyl is obtained.

[0112] Comparative Example 2: 90% Methomyl soluble powder

[0113] The formula is: 90% of methomyl, 1% of sodium lignin sulfonate, 5% of white carbon black, and potassium chloride as filler is added to 100%. The preparation method is: put methomyl, sodium lignin sulfonate, white carbon black and potassium chloride into a double-screw cone mixer and mix them evenly, crush them into 75 μm (200 meshes) with a flat air flow mill and reach 99.9%, and then mix them twice in a plowshare mixer, and after mixing evenly, the methomyl soluble powder is obtained.

[0114] Test Example 1

[0115] The quality of the methomyl soluble powders prepared in the above examples and comparative examples was tested, wherein the solubility and solution stability test method was CIPAC MT179, and the hot storage stability test method was CIPAC MT46.3.

[0116] Test method: Dissolve 5 g of the preparation in a 250 mL measuring cylinder filled with 25°C standard water. After 15 rotations and inversions and 5 minutes of standing, pour the liquid onto a 75 μm (200 mesh) sieve. The residue on the sieve is used for quantitative analysis. The method for testing the stability of the solution is to let the filtrate stand for 18 hours and then filter it again through a 75 μm (200 mesh) sieve. FAO stipulates: In the solubility and solution stability test, 5 min ≤ 1%, 18 h ≤ 0.05%, based on passing through a 200 mesh sieve, and the standard water used has a hardness of 500 ppm.

[0117] The results are shown in Table 4.

[0118] Table 4 Physical properties test of embodiments and comparative examples It can be seen from the data in Table 4 that in Examples 1-14 (especially Examples 5 to 8), compared with the comparative example, the solution stability of the soluble powder of dimethoate configured using the preferred adjuvant combination is the best. The better the solution stability, the higher the suspension of the product, the more uniform the solution, and the more uniform and stable it is during the application process.

[0119] Take the soluble powder of dimethoate prepared in the above embodiments and comparative examples to test the fluidity and slope angle of the product. Fluidity test method: The flow index of powder pesticide preparations (including wettable powders) is the number of quartz sands that need to be added so that a certain amount of powder (10-15g) can flow freely and continuously from the lower opening of a special funnel. FAO stipulates that the flow index of powder pesticide preparations is 12-15 as the best. Slope angle test method: The sample is passed through a small sieve with an aperture of about 0.5 mm and a diameter of 30 mm, and then through a funnel with an inner diameter of 5 mm at the lower opening, and evenly piled into a small cone on a small disc with a radius of 1 cm. When the cone height no longer continues to increase, measure the cone height H (cm). Take the average value of 5 times, calculate according to the following formula or look up the table, and you can get the slope angle α. The smaller the slope angle, the better the fluidity, and vice versa.

[0120] Each set of data was tested on 5 samples and the average value was calculated. The results are shown in Table 5.

[0121] Table 5 Fluidity test and slope angle test of the embodiments and comparative examples

[0122]

[0123] From the above data, it can be seen that compared with the comparative example, the preferred additive system product has the best fluidity and slope angle.

[0124] Efficacy test example 1

[0125] In order to verify the effect of the methomyl soluble powder of the present invention on controlling cotton bollworm on cotton, the experiment was carried out in Shouguang City, Shandong Province, during which there was no rain, and the insecticidal effects of the methomyl soluble powder of the embodiment and the comparative example were compared.

[0126] The experiment was conducted in a cotton planting area, where cotton was in the growth period and the insect pest eggs were in the early stage of occurrence. The experiment set up 16 treatment areas and 1 control area. The 16 treatment areas were sprayed with different examples and comparative examples of the pesticides. The pesticides were applied once with a Gongnong-16 backpack manual sprayer. The amount of 1.5 kg of the preparation was diluted with 450 kg of water per hectare to prepare the liquid medicine. The liquid medicine volume was converted into a small area for uniform spraying. The small areas were arranged in random blocks, with 3 replicates in each treatment area and a small area of ​​30 m 2(3m×10m). In addition to applying the pesticide according to the above scheme, the other planting conditions in each planting area are exactly the same. The survey method adopts five-point sampling, with 5 fixed points in each area and 5 plants fixed at each point, marked with a sign. The number of remaining insects is surveyed regularly every 3 and 7 days, and the mortality rate and control effect are calculated. The calculation formula is as follows:

[0127] The calculation method of protection effect is:

[0128] Insect population reduction rate (%) = (number of larvae before treatment - number of larvae after treatment) / number of larvae before treatment × 100%

[0129] Insect population increase rate (%) = (number of larvae after treatment - number of larvae before treatment) / number of larvae after treatment × 100%

[0130] Corrected control effect (%) = (insecticidal population reduction rate in the treated area + insect population increase rate in the control area) / (100% + insect population increase rate in the control area) × 100%

[0131] During the test, the compound preparation of the present invention had no adverse effects on cotton within the test medication range. The experimental results are shown in Table 6 below:

[0132] Table 6 Insecticidal effect of the soluble powder of methomyl in the examples and comparative examples

[0133] Dilution multiple 3 days after application 7 days after application Comparison / (％)0 (％)0 Example 1 3000 83.9 82.3 Example 2 3000 85.5 84.2 Example 3 3000 86.8 85.6 Example 4 3000 86.4 85.1 Example 5 3000 93.9 91.3 Example 6 3000 89.0 86.8 Example 7 3000 88.4 86.6 Example 8 3000 87.4 85.8 Example 9 3000 84.4 83.7 Example 10 3000 84.4 83.6 Embodiment 11 3000 83.4 82.3 Example 12 3000 83.3 81.4 Example 13 3000 83.0 81.6 Embodiment 14 3000 82.8 81.1 Comparative Example 1 3000 75.0 70.0 Comparative Example 2 3000 78.5 74.3

[0134] It can be seen from Table 6 that the soluble powder of methomyl can effectively prevent and control the occurrence of cotton bollworm, and the control effects of the preparations in the examples are better than those in the comparative examples, especially Example 5 has the best effect.

[0135] In summary, the soluble powder of methomyl of the present invention reduces or eliminates the problem of easy agglomeration of the soluble powder of methomyl through the selection of auxiliary agents, is conducive to long-term storage, is easy to pack, solves the problems of solubility and solution stability, and is more uniform and more stable during use. The soluble powder of the present invention solves the problem of dust generation during the production process through a specific processing technology, and the selected equipment has low energy consumption, improves the particle size of the product, and then reduces the dust hazard during use, which is conducive to environmental sustainable development. The soluble powder of methomyl, which is an effective active ingredient, has a high content and a small dosage, and has a special effect on cotton bollworm and aphid pests in crop and vegetable diseases, and has a high preventive effect.

[0136] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A soluble powder of methomyl, characterized in that: The invention comprises the following raw materials in percentage by weight: 50-95% of methomyl, 0.1-10% of wetting and dispersing agent, 0.1-10% of anti-caking agent and 0-49.8% of filler.

2. The methomyl soluble powder according to claim 1, characterized in that The anti-caking agent is one or more of sodium aluminosilicate, tricalcium phosphate, silicon dioxide, microcrystalline cellulose, silicate, and calcium stearate; And / or, the filler is one or more water-soluble fillers such as potassium sulfate, potassium chloride, diammonium hydrogen phosphate, urea, anhydrous sodium sulfate, and ammonium sulfate.

3. The methomyl soluble powder according to claim 1, characterized in that The invention comprises the following raw materials in percentage by weight: 50-95% of methomyl, 1-10% of wetting and dispersing agent, 0.1-10% of anti-caking agent and 1-48.9% of filler; Optionally, it comprises the following raw materials in percentage by weight: 85-94% of methomyl, 0.5-1.5% of wetting and dispersing agent, 4.5-5.5% of anti-caking agent, and 1-10% of filler; Optionally, it comprises the following raw materials in percentage by weight: 88-92% of methomyl, 1-1.2% of wetting and dispersing agent, 4.5-5.5% of anti-caking agent, and 2-6.5% of filler; Optionally, it comprises the following raw materials in percentage by weight: 88-92% of methomyl, 1% of wetting and dispersing agent, 5% of anti-caking agent, and 2-6% of filler; Optionally, it comprises the following raw materials in percentage by weight: 90% of methomyl, 1% of wetting and dispersing agent, 5% of anti-caking agent, and 4% of filler; Optionally, it comprises the following raw materials in percentage by weight: 90% of methomyl, 51% of wetting and dispersing agent MF-, 5% of anti-caking agent, and 4% of filler; Optionally, the anti-caking agent is silicon dioxide; Optionally, fillers are added up to 100%.

4. The methomyl soluble powder according to claim 1, characterized in that The wetting and dispersing agent is a mixture of one or more of sodium lignin sulfonate, maleic acid-acrylic acid copolymer salt, polyoxyethylene-polyoxypropylene block copolymer, sodium alkylphenol sulfonate, sodium salt of alkylnaphthalenesulfonic acid formaldehyde condensate, sodium salt of naphthalenesulfonic acid formaldehyde condensate, sodium alkyl polyoxyethylene ether sulfate, ethylene oxide-propylene oxide block copolymer, polycarboxylic acid sodium salt, sodium dodecyl sulfate, sodium dodecyl ether sulfate, sodium alkylnaphthalene sulfonate, sodium α-olefin sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, sodium diisobutylnaphthalene sulfonate, fatty acid sulfate, fatty acid ester sulfate, and wetting and dispersing agent MF-5; Optionally, the wetting and dispersing agent MF-5 includes sodium lauryl sulfate, sodium lauryl ether sulfate and sodium polycarboxylate; Optionally, the wetting and dispersing agent is MF-5, and the anti-caking agent is silicon dioxide; Optionally, the wetting and dispersing agent is naphthalenesulfonic acid formaldehyde condensate sodium salt, and the anti-caking agent is silicon dioxide; Optionally, the wetting and dispersing agent is sodium lignin sulfonate, and the anti-caking agent is sodium aluminosilicate; Optionally, the wetting and dispersing agent is sodium alkylphenol sulfonate, and the anti-caking agent is tricalcium phosphate; Optionally, the wetting and dispersing agent is alkylnaphthalenesulfonic acid formaldehyde condensate sodium salt, and the anti-caking agent is microcrystalline cellulose; Optionally, the wetting and dispersing agent is sodium diisobutylnaphthalene sulfonate, and the anti-caking agent is silicate; Optionally, the wetting and dispersing agent is sodium lauryl sulfate, and the anti-caking agent is calcium stearate; Optionally, the wetting and dispersing agent is sodium lignin sulfonate and sodium alkylphenol sulfonate, and the anti-caking agent is sodium aluminosilicate; Optionally, the wetting and dispersing agent is sodium polycarboxylate, and the anti-caking agent is microcrystalline cellulose; Optionally, the wetting and dispersing agent is sodium dodecyl sulfate, naphthalenesulfonic acid formaldehyde condensate sodium salt and polycarboxylic acid sodium salt, and the anti-caking agent is silicon dioxide; Optionally, the silica is white carbon black.

5. The soluble powder of methomyl according to any one of claims 1 to 4, characterized in that: The weight ratio of the wetting and dispersing agent to the anti-caking agent is 1:(0.5-10), optionally 1:(0.8-5), optionally 1:(1-5), optionally 1:

5.

6. A method for preparing the methomyl soluble powder according to any one of claims 1 to 5, characterized in that: The methomyl, wetting and dispersing agent, anti-caking agent and filler are uniformly mixed and crushed to obtain the methomyl soluble powder.

7. The preparation method according to claim 6, characterized in that: The pulverizing adopts a mechanical ultrafine pulverizer or an air flow pulverizer. Optionally, the pulverizer includes one or two of a flat air flow pulverizer, a vertical circulating tube air flow pulverizer, a counter-flow air flow pulverizer, a collision air flow pulverizer, a counter-flow fluidized bed air flow pulverizer, a universal pulverizer, a turbine self-cooling pulverizer, an impact ultrafine pulverizer, an impact mill, an ultrafine impact mill and a mechanical ultrafine pulverizer; Optionally, secondary mixing is performed after pulverization.

8. The preparation method according to claim 6 or 7, characterized in that: The machines used for mixing are one or two of a plowshare mixer, a ribbon mixer, a zero-gravity mixer, a V-type mixer, a double-screw cone mixer, a high-speed or low-speed liquid mixer, and a planetary power mixer.

9. A method for using the methomyl soluble powder according to any one of claims 1 to 5 or the methomyl soluble powder prepared by the preparation method according to any one of claims 6 to 8, characterized in that: The methomyl soluble powder is diluted with water and applied by spraying. Optionally, the dilution multiple is 2000-5000 times.

10. Use of the methomyl soluble powder according to any one of claims 1 to 5, or the methomyl soluble powder prepared by the preparation method according to any one of claims 6 to 8 in preventing and controlling plant pests in farmland; optionally, the plant pests include one or more of cotton bollworm, aphid, thrips, red spider, leaf roller, armyworm, and Spodoptera litura.

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