High-content imidacloprid seed treatment agent and preparation thereof

Abstract

The invention belongs to the technical field of pesticides, and relates to a high-content imidacloprid seed treatment agent and preparation thereof. The seed treatment agent with high content of imidacloprid comprises imidacloprid, at least one auxiliary agent, other auxiliary agents and a carrier, and the auxiliary agents contain cysteine hydrochloride. The effective content of the imidacloprid in the preparation is 600g / L to 800g / L. The seed treatment agent is a preparation with imidacloprid as an effective component. The seed coating agent is suitable for insect prevention of coated seeds of high-value-added crops such as corn, wheat, soybean, rice, peanut, cotton, tobacco, potato and vegetable. Particularly, the gene can be applied to transgenic crops; the obtained seed treatment agent has remarkable advantages in the aspect of preparation technology application performance due to application of special substances and special process conditions, and can be smoothly produced without creaming and ensure the production efficiency and feasibility by adding special key substances under the condition of limited water quantity in the production process.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticides and relates to a seed treatment agent with a high content of imidacloprid and a preparation method thereof. Background Art

[0002] As a type of neonicotinoid insecticide, imidacloprid is the main force in seed treatment agents. Its mechanism of action is that it selectively binds to acetylcholine receptors as a nicotinic acetylcholine receptor agonist, competes with insect acetylcholine, blocks the normal conduction of the central nervous system, and then causes insect paralysis and death. Due to this mechanism of action, in the application of seed treatment agents, especially when high-content preparations (the overall preparation content reaches 600g / L and above) are used, there will be problems such as shearing and sanding difficulties in the early stage of the preparation process due to the obvious scarcity of water, and even paste. For imidacloprid in actual coating applications, facing the trend that domestic genetically modified crops may be released, the content of the designed preparation needs to be further improved. Therefore, the content of imidacloprid used in seed treatment agents will not be too low, so for its preparation and application, especially in the preparation and application of the production link, the paste problem caused by the scarcity of water in the early stage of shearing and sanding will be more prominent.

[0003] In the current production of high-content preparations, continuous batches are used to increase the water volume to facilitate shearing and sanding. This type of solution requires a large production volume. If the water volume in a single batch is scarce, it can only be solved by gradually adding materials, and the production process is relatively cumbersome. Summary of the invention

[0004] The purpose of the present invention is to provide a seed treatment agent with a high content of imidacloprid and its preparation method.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A seed treatment agent with a high content of imidacloprid, comprising imidacloprid, at least one adjuvant, other adjuvants and a carrier, wherein the adjuvant contains cysteine ​​hydrochloride.

[0007] The effective content of imidacloprid in the preparation is 600g / L to 800g / L.

[0008] The auxiliary agent is cysteine ​​hydrochloride or a mixture thereof with other substances; wherein the auxiliary agent accounts for 2-6% of the mass of the preparation ingredients; and the other substances are one or more of lignin sulfonate, carboxylate, and block copolymer. The lignin sulfonate includes but is not limited to sodium lignin sulfonate M-9, the carboxylate includes but is not limited to SP27001, SP2728, Atlox 4913, and the block copolymer includes but is not limited to one or more of 127FL.

[0009] The added amount of cysteine ​​hydrochloride accounts for 0.2-3% of the preparation.

[0010] When the auxiliary agent is cysteine ​​hydrochloride and block copolymer, the mass ratio of cysteine ​​hydrochloride to block copolymer is 1:3-3:1.

[0011] The mass ratio of cysteine ​​hydrochloride to block copolymer is 1:2-2:1.

[0012] The carrier is water.

[0013] Other adjuvants are for special application needs of seed treatment agents, and warning color components can also be added, such as RED FGR, RED131, etc. Some other auxiliary adjuvants are also added to improve stability, such as FM-EW.

[0014] The warning color component in the above-mentioned other auxiliary agents accounts for 0-15% (preferably 10-15%) of the preparation mass; other auxiliary auxiliary agents in other auxiliary agents account for 0-1% (preferably 0.3-1%) of the preparation mass.

[0015] A preparation method of the imidacloprid seed treatment agent comprises the following steps: preparing cysteine ​​hydrochloride into an aqueous solution, and then mixing it with the effective ingredient imidacloprid, and then mixing the other ingredients according to the above description, performing shear stirring for 20 minutes, transferring the mixture into a sand mill, sand grinding until the particle size reaches within 5 microns, pouring out the liquid, and stirring the mixture evenly.

[0016] The cysteine ​​hydrochloride is configured into an aqueous solution by preparing cysteine ​​hydrochloride in water as a 50% aqueous solution, and adjusting the pH to between 6 and 7 with sodium hydroxide.

[0017] An application of the imidacloprid seed treatment agent, wherein the agent is used as a coating seed treatment agent for high value-added crops.

[0018] The high value-added crops include corn, wheat, soybeans, rice, peanuts, cotton, tobacco, potatoes and vegetables.

[0019] The advantages of the present invention are:

[0020] The seed treatment agent of the present invention is a preparation with imidacloprid as an effective ingredient. It is suitable for use in coating seeds of high value-added crops such as corn, wheat, soybean, rice, peanut, cotton, tobacco, potato and vegetables for insect prevention. It can be particularly applied to transgenic crops; the obtained seed treatment agent has significant advantages in the application performance of formulation technology due to the application of special substances and special process conditions. In the production process, under the condition of limited water, by adding special key substances, it can be smoothly produced without paste, and production efficiency and feasibility are guaranteed.

[0021] By adding cysteine ​​hydrochloride to the seed treatment agent of the present invention, it is possible to ensure that the high-content preparation does not become paste-like during the production process through a limited pH adjustment range, while the addition of this substance in seed coating preparations has not been reported. DETAILED DESCRIPTION

[0022] The following specific examples are used to further illustrate the present invention in detail, but the present invention is by no means limited to these examples, and methods well known to those skilled in the art are all included in the scope of the present invention.

[0023] The invention prepares a high-content imidacloprid seed treatment agent, which is used for coating seeds, and prevents and controls seed-borne diseases and soil-borne diseases, that is, prevents and controls diseases and insect pests starting from crop seeds. The invention mainly and effectively solves the paste problem in the preparation process of high-content preparations.

[0024] The percentages and parts in the following examples are all by weight, and the balance is made up by the carrier, and the density is calculated as 1 g / mL. The active ingredients and auxiliary agents used are all purchased from the market.

[0025] Preparation formula example

[0026] Example 1 Group

[0027] Example 1-1 600g / L Imidacloprid seed treatment suspension

[0028] Prepare a 50% cysteine ​​hydrochloride aqueous solution, add sodium hydroxide, and adjust the pH of the aqueous solution to 6.5. According to the formula requirements, weigh 2% (actually 1%) of 50% cysteine ​​hydrochloride aqueous solution and 60% of imidacloprid, stir and mix, add 127FL 2%, M-9 1%, RED FGR 10%, FM-EW 0.5%, add water to 100%, shear and stir for 20 minutes after mixing, transfer to a sand mill and sand grind until the particle size reaches within 5 microns, measure the viscosity of the feed liquid to be 300cp, pour out the feed liquid, and stir evenly to obtain the product.

[0029] Example 1-2 600g / L Imidacloprid seed treatment suspension

[0030] According to the formula requirements, 60% of imidacloprid was weighed, stirred and mixed, and then 2% of 127FL, 1% of M-9, 10% of RED FGR, and 0.5% of FM-EW were added. Water was added to 100%, and after mixing, shear stirring was performed for 20 minutes. The mixture was transferred to a sand mill and sanded until the particle size reached within 5 microns. The viscosity of the liquid was measured to be 2000cp. After standing for 10 minutes, it became a paste.

[0031] Example 2 Group

[0032] Example 2-1 600g / L Imidacloprid seed treatment suspension

[0033] Prepare a 50% cysteine ​​hydrochloride aqueous solution, add sodium hydroxide, and adjust the pH of the aqueous solution to 6.8. According to the formula requirements, weigh 0.4% (actually 0.2%) of 50% cysteine ​​hydrochloride aqueous solution, 60% of imidacloprid, stir and mix, add 2% of SP27001, 0.6% of 127FL, 10% of RED FGR, 1% of FM-EW, add water to 100%, shear and stir for 20 minutes after mixing, transfer to a sand mill and sand grind until the particle size reaches within 5 microns, measure the viscosity of the feed liquid to be 410cp, pour out the feed liquid, and stir evenly to obtain the product.

[0034] Example 2-2 600g / L Imidacloprid seed treatment suspension

[0035] According to the formula requirements, 60% of imidacloprid was weighed, and after stirring, 2% of SP27001, 0.6% of 127FL, 10% of RED FGR, and 1% of FM-EW were added, and water was added to 100%. After mixing, shear stirring was performed for 20 minutes, and the mixture was transferred to a sand mill and sanded until the particle size reached within 5 microns. The viscosity of the liquid was measured to be 2600cp, and it was paste-formed after standing for 10 minutes.

[0036] Example 3 Group

[0037] Example 3-1 800g / L Imidacloprid seed treatment suspension

[0038] Prepare a 50% cysteine ​​hydrochloride aqueous solution, add sodium hydroxide, and adjust the pH of the aqueous solution to 6.3. According to the formula requirements, weigh 3% (actually 1.5%) of 50% cysteine ​​hydrochloride aqueous solution and 80% of imidacloprid, stir and mix, add 1% of SP2728, 0.75% of 127FL, 15% of RED FGR, and 0.5% of FM-EW, add water to 100%, shear and stir for 20 minutes after mixing, transfer to a sand mill and sand grind until the particle size reaches within 5 microns, measure the viscosity of the feed liquid to be 590cp, pour out the feed liquid, and stir evenly to obtain the product.

[0039] Example 3-2 800g / L Imidacloprid seed treatment suspension

[0040] According to the formula requirements, 80% of imidacloprid was weighed, stirred and mixed, and then 1% of SP2728, 0.75% of 127FL, 15% of RED FGR, and 0.5% of FM-EW were added. Water was added to 100%, and after mixing, shear stirring was performed for 20 minutes. The mixture was transferred to a sand mill and sanded until the particle size reached within 5 microns. The viscosity of the liquid was measured to be 2000cp. After standing for 10 minutes, it became a paste.

[0041] Example 4 Group

[0042] Example 4-1 800g / L Imidacloprid seed treatment suspension

[0043] Prepare a 50% cysteine ​​hydrochloride aqueous solution, add sodium hydroxide, and adjust the pH of the aqueous solution to 6.9. According to the formula requirements, weigh 6% (actually 3%) of 50% cysteine ​​hydrochloride aqueous solution and 80% of imidacloprid, stir and mix, add 2% Atlox 4913, 1% 127FL, 15% RED FGR, 0.3% FM-EW, add water to 100%, shear and stir for 20 minutes after mixing, transfer to a sand mill and sand grind until the particle size reaches within 5 microns, measure the viscosity of the feed liquid to be 590cp, pour out the feed liquid, and stir evenly to obtain the product.

[0044] Example 4-2 800g / L Imidacloprid seed treatment suspension

[0045] According to the formula requirements, 80% of imidacloprid was weighed, stirred and mixed, and then 2% of Atlox 4913, 1% of 127FL, 15% of RED FGR, and 0.3% of FM-EW were added. Water was added to 100%, and shear stirring was performed for 20 minutes after mixing. The mixture was transferred to a sand mill and sanded until the particle size reached less than 5 microns. The discharge liquid was viscous and paste-like, and the viscosity could not be measured.

[0046] As can be seen from the above examples, the sample of the preparation without adding cysteine ​​hydrochloride will increase in viscosity during preparation, making it difficult to pour out, and some samples will not be able to discharge, and some samples will be paste-like after being placed even if the discharging liquid is prepared. In the above cases, it is difficult to prepare high-content preparations. Through the implementation of the present technical solution, when adding a cysteine ​​hydrochloride aqueous solution and adjusting its pH to a range of 6-7, the thickening and paste problems that occur during the preparation of high-content imidacloprid preparations can be significantly improved, thereby realizing the possibility of preparation.

[0047] The key substance cysteine ​​hydrochloride has not yet been used in the field of pesticide formulations. The possible reason is that the substance cysteine ​​can block and accelerate the separation of related structures in the imidacloprid compound, thereby forming gaps between particles of different active ingredients and causing aggregation, thereby inhibiting the paste and thickening of the system.

[0048] Example 5 Biological Activity - Indoor Activity Determination

[0049] The test target is the broad bean aphid Aphis craccivora Koch, nymph, which is a sensitive strain raised indoors. The test conditions are temperature: 20-22°C, humidity: RH 60%, light: L:D=14:10. The seed coating method is adopted. Weigh the broad bean seeds with an electronic balance, 100 grams per portion, and then accurately weigh the test agent with an electronic analytical balance, and coat according to the dosage of the test design (preparation in the above embodiment: seeds). The treated seeds are naturally dried in the shade for use. Sow the treated broad bean seeds in a paper cup with a diameter of 7 cm, 1 seed per pot, manage normally under greenhouse conditions, and observe the emergence of seedlings regularly. When the broad bean seedlings grow to 2-3 cm in height, inoculate healthy broad bean aphids, 5 heads per plant. After the adults produce nymphs on the second day, remove the adults and record the insect population base. Repeat 3 times, set a blank control (CK). Place the treated test insects in the observation room, observe the test insects' reactions regularly, and investigate the number of dead and alive insects after 5 days. The corrected mortality rate was calculated using the Abbott formula. The test agents were Example 1-1, Example 1-2 and Bayer's commercial product, Gaoqiao. The test results are shown in Table 1.

[0050] Table 1. Results of indoor biological activity test of 600g / L imidacloprid seed treatment suspension against aphids for 5 days

[0051]

[0052] From the above indoor biological activity results, at higher doses, there is no difference in indoor biological activity against aphids. At medium and low doses, Example 1-1 significantly improves the mortality rate of aphids. This shows that the key substances used in this technical solution can not only improve the fluidity of the preparation, avoid problems such as thickening and paste, but also have a certain effect on improving biological activity.

[0053] For the higher activity of Example 1-1, a safety test was conducted on corn coating to ensure that the cysteine ​​hydrochloride substance used in pesticide formulations for the first time is safe for crop growth. The test results are shown in Example 6.

[0054] Example 6 Biological Activity - Safety Determination

[0055] Corn (Zea mays L.), three different varieties were selected, namely Yiyuan, Yuhe, and Benyou. Temperature: 26-28°C. Humidity: RH 60%. Light: L:D=14:10. The dosage is shown in Table 2.

[0056] Table 2 Test dose

[0057]

[0058] The seed coating method was adopted. Weigh different varieties of corn seeds with an electronic balance, 100 grams per portion, and then accurately weigh the test agent with an electronic analytical balance, and coat according to the dosage of the test design (drug: seed). The treated seeds are naturally dried in the shade for later use. The germination test method refers to the "Agricultural Industry Standard of the People's Republic of China NY / T1965.3-2013 Pesticide Safety Evaluation Criteria for Crop Part 3: Indoor Test Method for Seed Treatment Agent Safety Evaluation of Crop" and "Agricultural Industry Standard of the People's Republic of China GB / T3543.4-1995 Crop Seed Inspection Procedure Germination Test". Put 3 layers of filter paper on the bottom of the sterilized culture dish, add an equal amount of clean water to the paper bed, and make it fully absorb water, then place the treated corn seeds on the paper bed according to the number, 10 seeds per dish, 3 times, and set up a blank control. After treatment, place them in an observation room under certain conditions for culture, and observe the germination of seeds every day. When the humidity of the paper bed is too low, use a pipette to add water quantitatively. Seedling test method: The treated corn seeds were sown in plastic pots with a diameter of 25*20cm, with 3 replicates per cup of pot, and a blank control was set. The seedlings were managed normally under greenhouse conditions, and the emergence was observed and recorded regularly. The growth status and drug injury symptoms of corn were recorded, and the emergence rate, emergence potential (uniformity was expressed as standard deviation of plant height), seedling height, root length, number of roots and fresh weight between different treatments were checked and calculated. The germination test survey and statistics were regular observations after treatment. The germination rate of seeds in each treatment was investigated 4 days after treatment (the germination rate of the blank control reached about 50%), 6 days (the blank control was fully germinated) and 10 days (4 days after full germination), and the seedling length, root length and number of roots were measured in the last survey.

[0059] Germination rate calculation formula:

[0060] Germination rate (%) = number of germinated seeds / number of test seeds × 100

[0061] The investigation and statistics of the germination test were conducted under normal management after corn seed sowing, and the germination was observed and recorded 7, 14, and 21 days after germination. The growth of corn and the symptoms of pesticide damage were observed and recorded, and the germination rate, germination potential (uniformity was expressed as the standard deviation of plant height), plant height, root length, number of roots, and fresh weight among the treatments were checked and calculated, and the DPS processing software was used for significant difference analysis.

[0062] Seedling emergence rate (%) = number of seedlings / number of seeds sown × 100

[0063] EXCEL and DPS software were used to analyze the significance of the experimental data using Duncan's new multiple range method.

[0064] The safety results are shown in Table 3.

[0065] Table 3. Test results of the effect of 600 g / L imidacloprid seed treatment suspension (Example 1-1) on corn seed germination

[0066]

[0067] The results of germination test in Table 3 show that 4 days after treatment, the germination rates of the blank controls of Yiyuan, Yuhe and Benyou were 71.1%, 46.7% and 93.3%, respectively. When the dosage of Example 1-1 was 600mL / 100kg, 900mL / 100kg, 1200mL / 100kg and 1500mL / 100kg of seeds, the germination potential of each treatment was significantly not lower than that of the blank control of the same variety. 6 days after treatment, the germination rates of each treatment of Yiyuan reached more than 95.6%, and there was no difference between the treatment and the blank control. The germination rates of Yuhe at each treatment dosage were more than 97.8%, and each treatment dosage was There was no significant difference among the treatments, which was equivalent to the blank control. The germination rates of all treatments of Benyou were above 97.8%, with no significant difference compared with the blank control. Ten days after treatment, the germination rates of all varieties were basically consistent with the results at 6 days. From the germination potential, the coating treatment of the tested agents had a certain promoting effect on the germination of corn seeds. From the results of the later germination rate, the seed coating treatment had little effect on the overall germination of corn seeds. From the results of the average bud length, the bud length of varieties Yiyuen and Yuhe was significantly better than that of the blank control of the two varieties. From the average root length and root number, there was little difference between the treatments of each variety and the blank control of the same variety.

[0068] The above data measurement results show that the cysteine ​​hydrochloride substance used in this technical solution is used for the first time in the research and development of pesticide formulations. It is safe for the growth of corn crops and does not affect the germination and growth of coated seeds.

Claims

1. A seed treatment agent with a high content of imidacloprid, comprising imidacloprid, at least one adjuvant, other adjuvants and a carrier, characterized in that: The auxiliary agent contains cysteine ​​hydrochloride.

2. The seed treatment agent with a high content of imidacloprid according to claim 1, characterized in that: The effective content of imidacloprid in the preparation is 600g / L to 800g / L.

3. The seed treatment agent with a high content of imidacloprid according to claim 1 or 2, characterized in that: The auxiliary agent is cysteine ​​hydrochloride or a mixture thereof with other substances; wherein the auxiliary agent accounts for 2-6% of the mass of the preparation components; and the other substances are one or more of lignin sulfonate, carboxylate and block copolymer.

4. The seed treatment agent with a high content of imidacloprid according to claim 3, characterized in that: The added amount of cysteine ​​hydrochloride accounts for 0.2-3% of the preparation.

5. The seed treatment agent with a high content of imidacloprid according to claim 3 or 4, characterized in that: When the auxiliary agent is cysteine ​​hydrochloride and block copolymer, the mass ratio of cysteine ​​hydrochloride to block copolymer is 1:3-3:

1.

6. The seed treatment agent with a high content of imidacloprid according to claim 5, characterized in that: The mass ratio of cysteine ​​hydrochloride to block copolymer is 1:2-2:

1.

7. A method for preparing the imidacloprid seed treatment agent according to claim 1, characterized in that: The cysteine ​​hydrochloride is prepared into an aqueous solution, and then mixed with the active ingredient imidacloprid, and then the other ingredients are mixed according to the above record, and shear stirring is performed for 20 minutes, and the mixture is transferred into a sand mill and sand-ground until the particle size reaches within 5 microns, and the liquid is poured out and stirred evenly.

8. The method for preparing the imidacloprid seed treatment agent according to claim 7, wherein: The cysteine ​​hydrochloride is configured into an aqueous solution by preparing cysteine ​​hydrochloride in water as a 50% aqueous solution, and adjusting the pH to between 6 and 7 with sodium hydroxide.

9. An application of the imidacloprid seed treatment agent according to claim 1, characterized in that: The treatment agent is used as a coating seed treatment agent for high value-added crops.

10. The use of the imidacloprid seed treatment agent according to claim 9, characterized in that: The high value-added crops include corn, wheat, soybeans, rice, peanuts, cotton, tobacco, potatoes and vegetables.

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