High-content dinotefuran aqueous solution based on hydration solubilization technology and preparation method of high-content dinotefuran aqueous solution

Abstract

The invention relates to the field of pesticide preparations, in particular to a high-content dinotefuran aqueous solution based on a hydration solubilization technology and a preparation method of the high-content dinotefuran aqueous solution. The invention discloses a high-content dinotefuran aqueous solution based on a hydration solubilization technology, which comprises the following components in percentage by weight: 1 to 25 percent of dinotefuran, 0.1 to 15 percent of hydrophilic amide cosolvent, 0.01 to 5 percent of penetration wetting agent, 0.1 to 5 percent of moisturizing anti-evaporation agent and the balance of water, the invention discloses a high-content dinotefuran aqueous solution based on a hydration solubilization technology, the content of effective components of the high-content dinotefuran aqueous solution can reach 25%, multiple hydrogen bonds are formed between a dinotefuran active compound and hydrophilic amide cosolvent molecules, and the water solubility of the active compound is greatly improved; the dinotefuran aqueous solution disclosed by the invention does not contain any organic solvent, meanwhile, the dosage of the surfactant is also greatly reduced, and the dinotefuran aqueous solution shows excellent quick killing performance on bemisia tabaci, especially German cockroaches.

Description

Technical Field

[0001] The present application relates to the field of pesticide preparations, and in particular to a high-content dinotefuran aqueous solution based on hydration solubilization technology and a preparation method thereof. Background Art

[0002] The international community is paying more and more attention to and requiring more safety of pesticides. Since the amount of solvents and adjuvants used in pesticide formulations is generally large, the secondary harm of solvents and adjuvants to humans, animals and the environment is sometimes greater than the active ingredients of the pesticides themselves.

[0003] Water-based pesticides that use water to fully or partially replace organic solvents are an important direction for the future development of pesticide formulations. Since most active ingredients of pesticides have low solubility in water and are unstable in water, there are very few varieties of aqueous pesticides.

[0004] The efficacy of pesticide formulations is related to the shape and size of the active ingredients in the formulations. The smaller the size of the active ingredient, the larger the specific surface area, the larger the contact area with the target organism, and the greater the efficacy; on the other hand, due to the small size effect, the smaller the particle size, the better the wetting and permeability. The size of the active ingredient of the aqueous solution is at the angstrom or nanometer level, so in theory, the efficacy of the aqueous solution is higher than that of other formulations.

[0005] Dinotefuran aqueous solution is a solution, which belongs to a thermodynamically stable system, has a clear and transparent appearance and good storage stability. However, aqueous emulsions, suspensions and suspoemulsions are all thermodynamically unstable systems, and there may be problems such as flocculation, stratification and crystallization during transportation and storage. In addition, the preparation method of dinotefuran aqueous solution is simple, and does not require equipment such as high-speed shear emulsification and mechanical crushing, and only slight stirring is required.

[0006] Dinotefuran is a third-generation nicotinoid insecticide developed by Mitsui Co., Ltd. of Japan. It is represented by Zhongnong Lihua and its trade name is Hu Rui. The theoretical duration of dinotefuran is 43 days. It has strong systemicity and a broad insecticide spectrum. It has excellent control effects on piercing-sucking mouthparts pests and is highly effective against pests such as Coleoptera and Diptera. The product is a white crystalline solid with a melting point of 107.5°C, stable to 150°C, and a hydrolysis DT50 of >1 year (pH 4, 7, 9). Dinotefuran has no cross-resistance with conventional insecticides, so it is particularly effective against resistant pests. In addition, dinotefuran is highly effective against sanitary pests such as cockroaches, termites, and houseflies.

[0007] The solubility of dinotefuran in water is 3.98 g / 100 g (20° C.), which is a slightly water-soluble substance and is difficult to dissolve in non-polar organic solvents such as cyclohexane and xylene. Obviously, it is difficult to prepare a high-concentration dinotefuran aqueous solution.

[0008] In the related art, when preparing the dinotefuran aqueous solution, the prepared dinotefuran technical content is low, the production cost is high and the raw materials are not environmentally friendly. The produced dinotefuran aqueous solution cannot meet the needs of industrial production.

[0009] Therefore, how to prepare an environmentally friendly dinotefuran aqueous solution with high content of dinotefuran technical, low production cost has become an urgent problem to be solved. Summary of the invention

[0010] In view of the deficiencies in the prior art, the present application provides a high-content dinotefuran aqueous solution based on hydration solubilization technology and a preparation method thereof.

[0011] In the first aspect, the present application provides a high-content dinotefuran aqueous solution based on hydration solubilization technology, which adopts the following technical solution: A high-content dinotefuran aqueous solution based on hydration solubilization technology comprises, by weight percentage, 1%-25% dinotefuran, 0.1%-15% hydrophilic amide cosolvent, 0.01%-5% penetrating wetting agent, 0.1%-5% moisturizing anti-evaporation agent, and the balance is water.

[0012] Preferably, based on weight percentage, it includes 5%-25% of dinotefuran, 3%-15% of hydrophilic amide cosolvent, 0.5%-5% of penetrating wetting agent, 0.5%-5% of moisturizing anti-evaporation agent, and the balance is water.

[0013] More preferably, based on weight percentage, it includes 5%-25% of dinotefuran, 3%-15% of hydrophilic amide cosolvent, 2%-5% of penetrating wetting agent, 1%-5% of moisturizing anti-evaporation agent, and the balance is water.

[0014] In the present application, the raw materials are improved, multiple hydrogen bonds are formed between the added dinotefuran technical and the hydrophilic amide cosolvent molecules, thereby greatly improving the water solubility of dinotefuran; the added penetrating wetting agent helps to reduce the surface tension of the system and increase the wetting and permeability; the added moisturizing anti-evaporation agent can effectively reduce the evaporation of water, which is beneficial to the precipitation and absorption of the active ingredients.

[0015] The dinotefuran aqueous solution prepared in the present application has the appearance of a colorless, clear and transparent solution, is odorless, can be diluted in any proportion, is stable for a long time, and its various physical properties meet the standard indicators stipulated by the state.

[0016] The content of dinotefuran technical drug in the dinotefuran aqueous solution disclosed in the present application can reach 25%, and the technical drug molecule forms multiple hydrogen bonds between molecules with the cosolvent, and has good water solubility; the dinotefuran aqueous solution disclosed in the present application does not contain any organic solvent, only dinotefuran technical drug, hydrophilic amide cosolvent, water and a small amount of necessary functional surfactant, which is green and environmentally friendly.

[0017] Preferably, the hydrophilic amide cosolvent is one or both of carboxylic diamide compounds and amino acids.

[0018] In the present application, by improving the raw materials, the added hydrophilic amide cosolvent has no aromatic group, is easily biodegradable, and does not contain emulsifier components such as alkylphenol polyoxyethylene ether, and has outstanding environmental friendliness. At the same time, the hydrophilic amide cosolvent component also has certain nutritional functions and can promote plant growth.

[0019] Preferably, the carbonyl diamide compound is urea.

[0020] Preferably, the amino acid is glycine and / or arginine.

[0021] Preferably, the penetrating wetting agent is one or more of isomeric decanol polyoxyethylene ether, sodium oleate, sodium linoleate or surfactant KT-50.

[0022] Preferably, the moisturizing anti-evaporation agent is one or more of ethylene glycol, propylene glycol, glycerol or hyaluronic acid.

[0023] The prepared dinotefuran aqueous solution has a colorless, clear and transparent appearance, is stable in storage, has no odor, can be quickly dispersed and diluted in water in any proportion, and has no precipitation, turbidity or stratification. The prepared dinotefuran aqueous solution has qualified hard water resistance, does not become turbid or precipitate in hard water of standard concentration, and its high-performance resistance and low-temperature resistance meet the standards.

[0024] The dinotefuran aqueous solution prepared in the present application has excellent environmental friendliness, storage stability and efficacy.

[0025] After testing, it was found that the environmentally friendly dinotefuran aqueous solution without organic solvents provided in the present application has achieved the national quality standards in various performance indicators.

[0026] In the second aspect, the present application provides a method for preparing a high-content dinotefuran aqueous solution based on hydration solubilization technology, using the following technical solution: A method for preparing a high-content dinotefuran aqueous solution based on hydration solubilization technology, the steps are as follows: Weigh each raw material according to the formula; The hydrophilic amide cosolvent, the penetrating wetting agent, the moisturizing anti-evaporation agent and water are mixed, and then dinotefuran is added, mixed, and filtered to obtain the dinotefuran aqueous solution.

[0027] The present application discloses a method for preparing a high-content dinotefuran aqueous solution based on a hydration solubilization technology. During the preparation process, no high-speed shearing treatment is required, and ordinary stirring and filtering devices can be used. The production is highly operable and convenient and simple.

[0028] The dinotefuran aqueous solution disclosed in the present application does not use any organic solvent and can be prepared by using common mixed dissolution equipment. In addition, the entire preparation process is simple in technology, short in process, and easy to operate. After the preparation is completed, it can be automatically filled without the need to purchase expensive air flow pulverizing equipment, and is extremely valuable for industrial promotion.

[0029] In a third aspect, the present application provides an application of a dinotefuran aqueous solution in preventing and controlling harmful organisms, using the following technical solution: A dinotefuran aqueous solution or use of the dinotefuran aqueous solution prepared by the method in preventing and controlling harmful organisms.

[0030] Preferably, the pests are Bemisia tabaci and German cockroach.

[0031] By adopting the above technical scheme, the dinotefuran aqueous solution prepared in the present application, the dinotefuran original drug exists completely in a molecular state after being dissolved, can be directly absorbed by plants or insects, and has an excellent control effect on whiteflies, especially German cockroaches.

[0032] In summary, the present application includes at least one of the following beneficial technical effects: (1) The present application discloses a high-content dinotefuran aqueous solution based on hydration solubilization technology and a preparation method thereof. The dinotefuran aqueous solution prepared in the present application forms multiple hydrogen bonds between the added dinotefuran technical and the hydrophilic amide cosolvent molecules, thereby greatly improving the water solubility of the technical. (2) The dinotefuran aqueous solution prepared in the present application does not contain any organic solvent, has excellent environmental friendliness, storage stability and efficacy, is stable for a long time, and its various physical properties meet the standard indicators prescribed by the state; (3) The dinotefuran aqueous solution prepared in the present application exhibits excellent rapid killing properties against whiteflies, especially German cockroaches. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a photograph of the appearance of a high-content dinotefuran aqueous solution sample prepared based on the hydration solubilization technology in Example 1; Figure 2 The liquid chromatogram of the dinotefuran aqueous solution of Example 1; Figure 3 This is the infrared spectrum of dinotefuran aqueous solution and raw materials; Figure 4 The spraying effect of domestic 40% dinotefuran WSG (a) and 15% dinotefuran aqueous solution (b) on Bemisia tabaci; Figure 5 The mortality of German cockroaches after exposure to 20% dinotefuran aqueous solution for 10 min (a) and 20 min (b) and imported 40% dinotefuran WSG for 20 min (c) and 60 min (d). DETAILED DESCRIPTION

[0034] The present invention is described below with reference to specific embodiments. It will be appreciated by those skilled in the art that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention in any way.

[0035] The experimental methods in the following examples are conventional methods unless otherwise specified. The medicinal materials, reagents, etc. used in the following examples are commercially available products unless otherwise specified.

[0036] Surfactant KT-50: sodium salt of dioctyl sulfonate succinate, manufacturer: Jiangsu Hai'an Petrochemical Plant, active ingredient content is 50%, CAS: 577-11-7; Hyaluronic acid: purchased from Sinopharm Chemical Reagent Co., Ltd.; CAS: 9004-61-9; molecular weight: 900-1200; Domestic 40% dinotefuran WSG: purchased from Chifeng Novatis Biotechnology Co., Ltd.; Imported 40% Dinotefuran WSG: purchased from BASF Europe.

[0037] The present application is further described in detail below in conjunction with embodiments and comparative examples.

[0038] Example 1: A 10% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 1 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 10 Glycine 6 Surfactant KT-50 2 Ethylene glycol 5 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding glycine, surfactant KT-50, and ethylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance. See the sample photo for details. Figure 1 .

[0039] The internal standard method was used to determine the content of the above samples on a liquid chromatograph. The quantitative results of high performance liquid chromatography showed that Figure 2 Only a single peak appeared at 3.525 minutes, which was the peak of dinotefuran technical. In addition, no peaks of other substances were observed. The dinotefuran content in the 10% dinotefuran AS sample was 10.04%, which was within the error range, indicating that the technical was effectively dissolved in water.

[0040] Example 2: A 15% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 2 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 15 Arginine 9 Surfactant KT-50 3 Hyaluronic acid 5 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding arginine, surfactant KT-50, and hyaluronic acid into a stirring tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0041] Example 3: A 20% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 3 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 20 Urea 6 Arginine 6 Surfactant KT-50 5 Propylene glycol 5 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding urea, arginine, surfactant KT-50, and propylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0042] Example 4: A 5% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 4 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 5 Glycine 3 Surfactant KT-50 2 Ethylene glycol 1 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding glycine, surfactant KT-50, and ethylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0043] Example 5: A 25% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 5 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 25 Glycine 6 Urea 9 Surfactant KT-50 5 Ethylene glycol 5 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding glycine, urea, surfactant KT-50, and ethylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0044] Example 6: A 1% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 6 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 1 Glycine 3 Surfactant KT-50 2 Ethylene glycol 1 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding glycine, surfactant KT-50, and ethylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0045] Example 7: A 1% environmentally friendly dinotefuran aqueous solution The raw material formula of dinotefuran aqueous solution is as follows: Table 6 Raw materials of dinotefuran aqueous solution Components Addition amount (w%) Dinotefuran 1 Glycine 0.1 Surfactant KT-50 0.5 Ethylene glycol 0.5 Deionized water Refill to 100 The preparation method of dinotefuran aqueous solution is as follows: (1) Prepare various raw materials for preparing 100 kg of aqueous solution according to the weight ratio of the formula; (2) respectively adding glycine, surfactant KT-50, and ethylene glycol into a stirred tank, adding deionized water, and stirring to dissolve; (3) adding dinotefuran and stirring to dissolve it to obtain a transparent solution; (4) Stir gently, let stand, and filter to obtain the target product with a transparent appearance.

[0046] Performance testing: 1. Quality inspection The dinotefuran aqueous solution prepared by the method of Examples 1-7 was subjected to quality inspection. The inspection items and methods are shown in Table 7, and the inspection results are shown in Table 8: Table 7 Test items and test methods Table 8 Test results According to Table 8, the samples prepared in Examples 1-7 were tested and found to meet the prescribed quality standards.

[0047] 2. Infrared absorption of the main functional groups of several compounds: In order to explore the mechanism of amide substances in efficiently solubilizing dinotefuran, samples of dinotefuran technical, urea as a solvent, and concentrated liquid crystals after solubilization were taken and subjected to Fourier transform infrared spectroscopy, aiming to explore the absorption of infrared light by different functional groups of the samples before and after the addition of the solvent, and then to explore the changes in each functional group and the intermolecular forces, especially the formation of hydrogen bonds.

[0048] Instrument model: Thermo Fisher Nicolet Is10, potassium bromide tablet, transmission mode; From high wavenumber to low wavenumber, it can be seen that the mixture of dinotefuran and co-solvent obtained by the concentrated solution has the same peaks as the co-solvent at wavenumbers such as 3446 (stretching vibration peak of NH), 1680 (stretching vibration peak of C=O), and 1060 (stretching vibration peak of CN), and the same absorption peaks as dinotefuran original drug at wavenumbers such as 2952 (asymmetric stretching vibration absorption peak of CH2), 2872 (symmetric stretching vibration absorption peak of CH2), 1333 (symmetric bending vibration absorption peak of CH), 1145 (stretching vibration absorption peak of C=N), and 896 (stretching vibration absorption peak of CN), and the same absorption peaks appear in the three groups of samples at wavenumbers such as 3338 (stretching vibration absorption peak of NH) and 1620 (bending vibration absorption peak of NH), indicating that the mixture after solubilization maintains the complete structure of dinotefuran and co-solvent. It is worth noting that the hydroxyl peak at 3281 of the original drug of dinotefuran disappears, and the stretching vibration absorption peak of the secondary acyl group at 1550 disappears, because the functional group forms a hydrogen bond with the hydrogen in the cosolvent molecule; and the absorption peaks of the mixture at 2981, 1333 and 1145 are slightly blue-shifted, because the formation of hydrogen bonds leads to the redistribution of the electron cloud density, which shortens the bond length and affects the vibration frequency. And no displacement of the absorption peak in a larger wavenumber range is observed, which can be concluded that multiple hydrogen bonds are formed between the original drug of dinotefuran and the amide cosolvent in the mixture, and the intermolecular hydrogen bonds are dominant, rather than the intramolecular hydrogen bonds; the test results are as follows Figure 3 The infrared absorption of the main functional groups of several compounds is shown in Table 9.

[0049] Table 9 Infrared absorption of main functional groups of several compounds 3. Performance and control effect experiments Test Example 1: Surface tension test: The samples of Examples 1-7, the domestically produced 40% dinotefuran soluble granules of the competitor and the imported 40% dinotefuran soluble granules were diluted to three concentrations of 100 times, 500 times and 1000 times, respectively, and the surface tension changes were measured. The smaller the surface tension, the better the wettability of the sample, the better the spreadability on the crop surface, and the better the control effect. The results are shown in Table 10. The results show that the surface tension of the dinotefuran aqueous solution samples (Examples 1-7) prepared in the present application is better than that of the two groups of comparative samples 40% dinotefuran soluble granules, mainly because in the process of preparing the dinotefuran aqueous solution in the present application, a high-efficiency penetrating wetting agent is added to reduce the surface tension of the product.

[0050] Table 10 Surface tension of dinotefuran aqueous solution and control sample Test Example 2: Insecticidal test I of the 15% environmentally friendly dinotefuran aqueous solution prepared in Example 2 1.1. Test name: Outdoor toxicity test of 15% dinotefuran aqueous solution against Bemisia tabaci 1.2. Targets of prevention and control: Bemisia tabaci belongs to the family Aleyrodidae in the order Homoptera. It is also known as the small white moth. It is widely distributed and is a piercing-sucking pest with strong reproductive capacity and a large population. It gathers in groups and causes damage all year round. Adults and nymphs suck tomato juice and secrete honeydew to induce sooty mold, which causes leaves to turn green, wilt, and even dry up, and fruits to become sticky and black, making vegetables lose their commercial value. It can also spread viral diseases.

[0051] 1.3. Test Agents: 1) The 15% dinotefuran aqueous solution prepared in Example 2 was set into 5 dosage groups, and the preparation was diluted with water to 1.25 mg / L, 2.5 mg / L, 5 mg / L, 10 mg / L and 20 mg / L; 2) Five dosage groups were set up for commercially available domestic 40% dinotefuran soluble granules, and the preparation was diluted with water to 0.625 mg / L, 1.25 mg / L, 2.5 mg / L, 5 mg / L and 10 mg / L.

[0052] 1.4. Preparation of medicine Accurately weigh the test reagent, directly add deionized water to dilute it, and prepare a 10000 mg / L stock solution.

[0053] According to the concentration range determined in the preliminary experiment, five concentration gradients were designed for each agent (calculated according to the active ingredient), and a clear water control was set at the same time.

[0054] 1.5 Test methods According to GB / T 17980.16-2000 "Guidelines for Field Efficacy Tests of Pesticides (I) Insecticides for Control of Greenhouse Whiteflies", five pesticide application treatments were set up, and the pesticide concentration was based on the recommended 667m 2 Dosage design: 15% dithiocarb aqueous solution 120,000 times dilution, 60,000 times dilution, 30,000 times dilution, 15,000 times dilution, 7,500 times dilution; 40% dithiocarb soluble granules 240,000 times dilution, 120,000 times dilution, 60,000 times dilution, 30,000 times dilution, 15,000 times dilution, the application amount of each treatment area is 1.5L. A control area sprayed with clean water was set up, and the control area was sprayed with 1.5L of clean water. Each treatment was repeated 3 times, with a total of 18 areas, and the area of ​​each area was 30m 2 , randomized block arrangement.

[0055] Tomato leaf area is 16-20cm 2 , at 0.01m 2 There are 5.00-6.25 tomato leaves in the test area, and there are about 30 tomato leaves during the test period. 2 On the leaves, spraying began when the number of whiteflies in the test group and the control group was about 20. According to the grading standards in Table 11, the degree of damage of whiteflies in the test group and the control group was "++".

[0056] Table 11 Damage degree of whitefly Grade classification standards <![CDATA[Every 0.01 m 2 Insect quantity on plant leaves]]> + 1 head<Insect quantity≤100 heads ++ 100 heads<Insect quantity≤400 heads +++ 400 <Insect quantity≤800 ++++ Insect quantity>800 After 24 hours, the insect mortality was investigated.

[0057] 1.6 Data Processing Use Excel software to organize data; Mortality rate (%) = number of deaths / total number of insects × 100%, Corrected mortality rate (%) = (treatment mortality rate - control mortality rate) / (1 - control mortality rate) x 100%.

[0058] 1.7 Test results: The original data on the mortality of tomato whiteflies after being treated with different concentrations of 15% dinotefuran aqueous solution and 40% dinotefuran soluble granules are shown in Table 12.

[0059] Table 12 Death of tomato whiteflies after treatment with 15% dinotefuran aqueous solution and 40% dinotefuran soluble granules (24h) As can be seen from Table 12, 24 hours after the treatment, the mortality rate of the control group was 0.8%, which is less than 5%, so there is no need to correct the mortality rate. Both 15% dinotefuran aqueous solution and 40% dinotefuran soluble granules showed good biological activity against tomato whitefly, but the efficacy of the former was significantly better than that of the latter.

[0060] 1.8 Conclusion: The toxicity of the 15% dinotefuran aqueous solution prepared by the method of the present application to Bemisia tabaci is significantly higher than that of the 40% dinotefuran soluble granules. Figure 4 .

[0061] Test Example 3: Insecticidal test II of the 25% environmentally friendly dinotefuran aqueous solution prepared in Example 5 2.1. Test name: Outdoor toxicity test of 25% dinotefuran aqueous solution against tomato whitefly 2.2. Targets of prevention and control: Bemisia tabaci belongs to the family Aleyrodidae in the order Homoptera. It is also known as the small white moth. It is widely distributed and is a piercing-sucking pest with strong reproductive capacity and a large population. It gathers in groups and causes damage all year round. Adults and nymphs suck tomato juice and secrete honeydew to induce sooty mold, which causes leaves to turn green, wilt, and even dry up, and fruits to become sticky and black, making vegetables lose their commercial value. It can also spread viral diseases.

[0062] 2.3. Test Agents: 1) The 25% dinotefuran aqueous solution prepared in Example 5 was set into 5 dosage groups, and the preparation was diluted with water to 1 mg / L, 2 mg / L, 4 mg / L, 8 mg / L and 16 mg / L; 2) Five dosage groups were set up for commercially available domestic 40% dinotefuran soluble granules, and the preparation was diluted with water to 0.625 mg / L, 1.25 mg / L, 2.5 mg / L, 5 mg / L and 10 mg / L.

[0063] 2.4. Preparation of medicine Accurately weigh the test reagent, directly add deionized water to dilute it, and prepare a 10000 mg / L stock solution.

[0064] According to the concentration range determined in the preliminary experiment, five concentration gradients were designed for each agent (calculated according to the active ingredient), and a clear water control was set at the same time.

[0065] 2.5 Test methods According to GB / T 17980.16-2000 "Guidelines for Field Efficacy Tests of Pesticides (I) Insecticides for Control of Greenhouse Whiteflies", five pesticide application treatments were set up, and the pesticide concentration was based on the recommended 667m 2Dosage design: 25% dithiocarb aqueous solution 200,000 times dilution, 100,000 times dilution, 50,000 times dilution, 25,000 times dilution, 12,500 times dilution; 40% dithiocarb soluble granules 240,000 times dilution, 120,000 times dilution, 60,000 times dilution, 30,000 times dilution, 15,000 times dilution, the application amount of each treatment area is 1.5L. A control area sprayed with clean water was set up, and the control area was sprayed with 1.5L of clean water. Each treatment was repeated 3 times, with a total of 18 areas, and the area of ​​each area was 30m 2 , randomly grouped and arranged.

[0066] The classification was performed according to the classification standard in Table 11 of Test Example 2.

[0067] 2.6 Data Processing Use Excel software to organize data; Mortality rate (%) = number of deaths / total number of insects × 100%, Corrected mortality rate (%) = (treatment mortality rate - control mortality rate) / (1 - control mortality rate) x 100%.

[0068] 2.7 Test results: The original data on the mortality of tomato whiteflies after being treated with different concentrations of 25% dinotefuran aqueous solution and 40% dinotefuran soluble granules are shown in Table 13.

[0069] Table 13 Death of tomato whitefly after treatment with 25% dinotefuran aqueous solution and 40% dinotefuran soluble granules (24h) As can be seen from Table 13, 24 hours after the treatment, the mortality rate of the control group was 1.7%, which is less than 5%, so there is no need to correct the mortality rate. Both 25% dinotefuran aqueous solution and 40% dinotefuran soluble granules showed good biological activity against tomato whitefly, but the efficacy of the former was significantly better than that of the latter.

[0070] 2.8 Conclusion: The toxicity of the 25% dinotefuran aqueous solution prepared by the method of the present application to Bemisia tabaci is significantly higher than that of the 40% dinotefuran soluble granules.

[0071] Test Example 4: Example 3 Environmentally friendly 20% dinotefuran aqueous solution insecticide test III 3.1 Test Name: Indoor spray toxicity test of 20% dinotefuran water solution on German cockroaches; 3.2. Targets of prevention and control: German cockroach; 3.3. Test Agents: The 20% dinotefuran aqueous solution of Example 3 and the imported 40% dinotefuran soluble granules; Equipment: Φ50cm×60cm glass jar with non-absorbent surface (a circle of vaseline is evenly applied on the upper side), stopwatch; Test insects: German cockroaches Blattella germanica: 10-15 day old adults, half male and half female.

[0072] 3.4 Test methods Referring to the indoor efficacy test method for registered pesticides and sanitary insecticides GB / T 13917.1-2009[3], the residual spraying effect of 20% dinotefuran aqueous solution and 40% dinotefuran soluble granules on German cockroaches was tested. Before the residual spraying board surface contact killing effect test, 20% dinotefuran aqueous solution and 40% dinotefuran soluble granules were diluted 62.5 times and 125 times respectively, and the concentration was 160 mg ai / m 2 Treat the non-absorbent board surface and let it dry for 1 hour before use. Each group of 10 German cockroaches were placed in a glass tank for contact time of 10min, 20min, 30min, 40min, 50min and 60min respectively. After recovery and feeding for 1 hour, the mortality rate of the test insects was calculated. The experiment was repeated 3 times and a blank control group was set up.

[0073] 3.5 Test results When the retention dose is 160 mg ai / m 2 When the German cockroaches were exposed to 20% dinotefuran aqueous solution for 10 minutes, the mortality rate reached 50%, and all died after 20 minutes of contact; while the mortality rate of 40% dinotefuran soluble granules was 0 after 10 minutes of contact, and only 70% after 60 minutes of contact. Similar results were repeated three times. Compared with the imported 40% dinotefuran soluble granules, 20% dinotefuran aqueous solution showed excellent rapid killing performance. Figure 5 .

[0074] Table 14 Death of German cockroaches after exposure to 20% dinotefuran aqueous solution and imported 40% dinotefuran soluble granules at different times Test Example 5: Insecticide test IV using the environmentally friendly 25% dinotefuran aqueous solution of Example 5 4.1 Test Name: Indoor spray toxicity test of 25% dinotefuran aqueous solution on German cockroaches; 4.2. Targets of prevention and control: German cockroach; 4.3. Test Agents: 25% dinotefuran aqueous solution of Example 5, imported 40% dinotefuran soluble granules; Equipment: Φ50cm×60cm glass jar with non-absorbent surface (a circle of vaseline is evenly applied on the upper side), stopwatch; Test insects: German cockroaches Blattella germanica: 10-15 day old adults, half male and half female.

[0075] 4.4 Test methods Referring to the indoor efficacy test method for registered pesticides and sanitary insecticides GB / T 13917.1-2009[3], the residual spraying effect of 25% dinotefuran aqueous solution and 40% dinotefuran soluble granules on German cockroaches was tested. Before the residual spraying board surface contact killing effect test, 25% dinotefuran aqueous solution and 40% dinotefuran soluble granules were diluted 78.125 times and 125 times, respectively, at 160 mg ai / m 2 Treat the non-absorbent board surface and let it dry for 1 hour before use. Each group of 10 German cockroaches were placed in a glass tank for contact time of 10min, 20min, 30min, 40min, 50min and 60min respectively. After recovery and feeding for 1 hour, the mortality rate of the test insects was calculated. The experiment was repeated 3 times and a blank control group was set up.

[0076] 4.5 Test results When the retention dose is 160 mg ai / m 2 When the German cockroaches were exposed to 25% dinotefuran aqueous solution for 10 minutes, the mortality rate reached 60%, and all died after 20 minutes; while the mortality rate of 40% dinotefuran soluble granules was 0 after 10 minutes, and only 70% after 60 minutes, and similar results were repeated three times. Compared with the imported 40% dinotefuran soluble granules, 25% dinotefuran aqueous solution showed excellent rapid killing performance.

[0077] Table 15 Death of German cockroaches after exposure to 25% dinotefuran aqueous solution and imported 40% dinotefuran soluble granules at different times The dinotefuran aqueous solution disclosed in the present application reduces the cost of raw materials because it does not use organic solvents. In addition, after more than a dozen indoor and field tests, the high-content dinotefuran aqueous solution without organic solvents provided in the present application has shown excellent insecticidal effects, especially in terms of sanitary insecticide, the rapid killing of German cockroaches has been improved by about 50% compared with the current imported competing products. Therefore, with the promotion and application of the environmentally friendly dinotefuran aqueous solution of the present application, significant economic and social benefits will surely be generated.

[0078] The present application illustrates the detailed method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed method, that is, it does not mean that the present invention must rely on the above-mentioned detailed method to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A high-content dinotefuran aqueous solution based on hydration solubilization technology, characterized in that: Calculated by weight percentage, it includes 1%-25% of dinotefuran, 0.1%-15% of hydrophilic amide cosolvent, 0.01%-5% of penetrating wetting agent, 0.1%-5% of moisturizing anti-evaporation agent, and the balance is water.

2. The high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 1, characterized in that: Calculated by weight percentage, it includes 5%-25% of dinotefuran, 3%-15% of hydrophilic amide cosolvent, 0.5%-5% of penetrating wetting agent, 0.5%-5% of moisturizing anti-evaporation agent, and the balance is water.

3. A high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 1 or 2, characterized in that: The hydrophilic amide cosolvent is one or two of carboxylic diamide compounds and amino acids.

4. The high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 3, characterized in that: The carbonyl diamide compound is urea.

5. The high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 3, characterized in that: The amino acids are glycine and / or arginine.

6. The high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 1, characterized in that: The penetrating wetting agent is one or more of isomeric decanol polyoxyethylene ether, sodium oleate, sodium linoleate or surfactant KT-50.

7. The high-content dinotefuran aqueous solution based on hydration solubilization technology according to claim 1, characterized in that: The moisturizing anti-evaporation agent is one or more of ethylene glycol, propylene glycol, glycerol or hyaluronic acid.

8. A method for preparing a high-content dinotefuran aqueous solution based on hydration solubilization technology, characterized in that: Here are the steps: Weigh each raw material according to the formula; The hydrophilic amide cosolvent, the penetrating wetting agent, the moisturizing anti-evaporation agent and water are mixed, and then dinotefuran is added, mixed, and filtered to obtain the dinotefuran aqueous solution.

9. Use of the dinotefuran aqueous solution according to any one of claims 1 to 7 or the dinotefuran aqueous solution prepared by the method according to claim 8 in preventing and controlling harmful organisms.

10. The use according to claim 9, characterized in that: The harmful organisms are whitefly and German cockroach.

Images