Slow-release pesticide fertilizer containing cyantraniliprole as well as preparation method and application thereof

Abstract

The invention provides a cyantraniliprole-containing slow-release pesticide fertilizer and a preparation method thereof. The cyantraniliprole-containing slow-release pesticide fertilizer is mainly prepared from the following raw materials: 0.01-1% of cyantraniliprole, 0.01-1% of clothianidin, 20-60% of a fertilizer, 1-5% of a dispersing aid, 1-5% of a gel, 1-5% of a coating agent, 1-15% of a solvent, 0.01-2.5% of a cladding agent and the balance of filler. The gel is used for being mixed with cyantraniliprole and clothianidin to prepare soft film pesticide fertilizer core particles; the coating agent coats the outer layer of the soft film pesticide fertilizer core particle to prepare a multi-layer slow-release pesticide fertilizer core; the fertilizer and the filler wrap the outer layer of the multi-layer slow-release pesticide-fertilizer core to prepare pesticide-fertilizer particles; the coating agent is coated on the outer layer of the pesticide-fertilizer particles. According to the invention, the technical problem of poor mixing stability of cyantraniliprole and the fertilizer can be well solved, so that the strong insecticidal advantage of cyantraniliprole can be fully played, and the quality and stability of the pesticide fertilizer can be remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of pharmaceutical fertilizers, and in particular to a slow-release pharmaceutical fertilizer containing cyantraniliprole, a preparation method thereof, and an application thereof. Background Art

[0003] At present, in the field of pharmaceutical fertilizers, the application of cyantraniliprole is still in its infancy. In particular, in terms of how to ensure the stability of cyantraniliprole in pharmaceutical fertilizers, there are still many technical problems to be solved. When cyantraniliprole is prepared into a pharmaceutical fertilizer granule with a nitrogen-containing fertilizer, a chemical reaction often occurs, resulting in an accelerated decomposition rate of cyantraniliprole and a reduced drug effect, thereby affecting its control effect. In order to solve the decomposition problem when cyantraniliprole is mixed with fertilizers, some technical attempts have been made to improve it. For example, by adjusting the fertilizer components, reducing its decomposition effect on cyantraniliprole; however, these methods still have some problems in actual application, such as adjusting the fertilizer components may affect the fertilizer effect, and the application value is not high.

[0004] In summary, developing an effective technology to prevent the decomposition of cyantraniliprole has become an urgent need for the current industry development. Summary of the Invention

[0005] The present invention provides a slow-release pharmaceutical fertilizer containing cyantraniliprole, a preparation method thereof, and an application thereof, which can better solve the technical problem of poor mixing stability between cyantraniliprole and fertilizers. In this way, both the powerful insecticidal advantages of cyantraniliprole can be fully exerted, and the quality and stability of the pharmaceutical fertilizer can be significantly improved.

[0006] To achieve the above object, the technical solution of the present invention is as follows:

[0007] A slow-release pharmaceutical fertilizer containing cyantraniliprole is mainly made from the following raw materials: 0.01-1% of cyantraniliprole, 0.01-1% of clothianidin, 20-60% of fertilizer, 1-5% of dispersion aid, 1-5% of gelling agent, 1-5% of coating agent, 1-15% of solvent, 0.01-2.5% of cladding agent, and the filler makes up 100%;

[0008] The gelling agent is used to mix with cyantraniliprole and clothianidin to form a soft film pharmaceutical fertilizer core particle;

[0009] The cladding agent is wrapped around the outer layer of the soft film pharmaceutical fertilizer core particle to form a multi-layer slow-release pharmaceutical fertilizer core;

[0010] The fertilizer and the filler are wrapped around the outer layer of the multi-layer slow-release pharmaceutical fertilizer core to form a pharmaceutical fertilizer particle;

[0011] The coating agent is wrapped around the outer layer of the pharmaceutical fertilizer particle.

[0012] Preferably, the dispersion aid is at least one of calcium dodecylbenzenesulfonate, styrylphenol polyoxyethylene ether, polysorbate, sorbitan laurate, SP-2728, SP-SC29, fatty alcohol polyoxyethylene ether, and Nekal BX;

[0013] The solvent is one or a combination of more of water, acetone, methanol, ethyl acetate, dimethylformamide, cyclohexanone, xylene, and glutaraldehyde;

[0014] The gelling agent is at least one of hypromellose, polyethylene glycol, sodium alginate, chitosan, starch, glycerol, and ethylene glycol.

[0015] Preferably, the coating agent is at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, sodium alginate, chitosan, starch, nano calcium carbonate, sodium dodecyl sulfate, and glycerol.

[0016] Preferably, the film coating agent is one or a combination of more of hypromellose, polyvinyl alcohol, polyethylene glycol, sodium alginate, chitosan, ethylene glycol, and glycerol.

[0017] The present invention also provides a preferred filler, which is a mixture of one or more of diatomite, kaolin, attapulgite, bentonite, white carbon black, and calcium carbonate.

[0018] The present invention further provides a preparation method of the slow-release pesticide-fertilizer containing cyantraniliprole as described above, including the following steps:

[0019] (1) Preparation of the soft film pesticide-fertilizer core particles: Mix and dissolve cyantraniliprole, clothianidin, the dispersion aid, and the solvent to prepare a technical drug solution, and fully mix the technical drug solution with the gelling agent. The mass ratio of the technical drug solution to the gelling agent is 1:4 to 16. Adjust the pH value of the mixed liquid to 3.0 to 6.0 to form a hydrogel, freeze-dry, and pulverize to obtain the soft film pesticide-fertilizer core particles;

[0020] (2) Preparation of the multi-layer slow-release pesticide-fertilizer core: Add the soft film pesticide-fertilizer core particles into a coating machine, and spray the coating agent on the outer layer of the soft film pesticide-fertilizer core particles at least in two times. Keep it in a heated state for pre-curing after each spraying; after the spraying is completed, dry to obtain the multi-layer slow-release pesticide-fertilizer core;

[0021] (3) Preparation of the pesticide-fertilizer particles: Fully mix the multi-layer slow-release pesticide-fertilizer core with the fertilizer and the filler to obtain a mixed material, and then add the mixed material into a granulator to make particles, dry and screen to obtain the pesticide-fertilizer particles;

[0022] (4) Coating: Mix the coating agent with water to prepare a coating solution. Subsequently, add the fertilizer and pesticide granules into a coating machine, spray the coating solution so that the coating material adheres to the surface of the fertilizer and pesticide granules, and obtain the slow-release fertilizer and pesticide after drying.

[0023] Preferably, the mass ratio of the soft film fertilizer and pesticide core particles to the coating agent is 3 - 15:1, the mass ratio of the multi-layer slow-release fertilizer and pesticide core, the fertilizer and the filler is 1:200 - 700:150 - 500, and the mass ratio of the coating agent to the fertilizer and pesticide granules is 2 - 5:100 - 2000.

[0024] Preferably, step (1) specifically includes: Mix and dissolve the cyantraniliprole and clothianidin with a dispersion aid and a solvent to prepare a technical drug solution. Take the technical drug solution and mix it fully with the freshly prepared gelling agent A, disperse it by ultrasonic wave or stirring for 20 - 60 min, then add the freshly prepared gelling agent B, mix it fully, add glacial acetic acid, adjust the pH of the system to 4.0 - 5.5 to form a hydrogel, perform freeze-drying, and obtain the soft film fertilizer and pesticide core particles after pulverization; the mass ratio of the technical drug solution, gelling agent A and gelling agent B is: 1:2 - 8:2 - 8;

[0025] The preparation method of the gelling agent A includes the following steps: Dissolve chitosan in an acidic dimethylformamide aqueous solution, the mass ratio of chitosan to the dimethylformamide aqueous solution is 1:150 - 250, the concentration of the dimethylformamide aqueous solution is 20 - 35%, the pH is 3.0 - 5.5, disperse it by ultrasonic wave or stirring until it is transparent to obtain the gelling agent A;

[0026] The preparation method of the gelling agent B includes the following steps: Dissolve sodium alginate in a dimethylformamide aqueous solution, the mass ratio of chitosan to the dimethylformamide aqueous solution is 1:150 - 250, the concentration of the dimethylformamide aqueous solution is 20 - 35%, and disperse it by ultrasonic wave or stirring until it is transparent.

[0027] Preferably, in step (2), the preparation method of the coating agent specifically includes: Add polyvinyl alcohol, polyvinylpyrrolidone, nano calcium carbonate particles / starch, sodium dodecyl sulfate and / or glycerol, and water into a container in sequence, heat it to 70 - 96 °C and stir to make it disperse evenly to obtain a mixed coating solution. After the mixed coating solution is cooled to room temperature, add a glutaraldehyde solution and stir to mix evenly to obtain the coating agent;

[0028] The mass ratio of polyvinyl alcohol, polyvinylpyrrolidone, nano calcium carbonate particles / starch, sodium dodecyl sulfate and / or glycerol, and water is 3 - 12:1 - 4:0.2 - 0.8:0.8 - 3:30 - 60; the dosage of the glutaraldehyde solution is 0.1 - 1% of the mass of the mixed coating solution, and the mass concentration is 2 - 10%.

[0029] Preferably, the sodium dodecyl sulfate and / or glycerol is sodium dodecyl sulfate and glycerol, and the mass ratio is 1:5 to 10.

[0030] Preferably, the process for preparing the coating solution specifically includes: hydroxypropyl methylcellulose and / or polyvinyl alcohol and / or sodium alginate, glycerol and / or polyethylene glycol and / or ethylene glycol, and water are sequentially added into a container, and the mass ratio of hydroxypropyl methylcellulose and / or polyvinyl alcohol and / or sodium alginate, glycerol and / or polyethylene glycol and / or ethylene glycol, and water is 1 to 6:2 to 3:90 to 100, and it is heated to 70 to 96 °C and stirred until dissolved.

[0031] The present invention further provides the application of the above-mentioned slow-release fertilizer and pesticide containing cyantraniliprole in sugarcane planting and pest control.

[0032] The present invention has the following remarkable excellent effects:

[0033] (1) In the present invention, the gelling agent is first mixed with cyantraniliprole and clothianidin, and the cyantraniliprole and clothianidin are coated by forming a three-dimensional cross-linked network relying on the physical force of the gelling agent, thereby improving the stability of cyantraniliprole and clothianidin, prolonging the drug effect time of cyantraniliprole, ensuring the use effect of the fertilizer and pesticide, and reducing the need for frequent pesticide application.

[0034] (2) In the present invention, a coating agent is wrapped around the core of the multi-layer slow-release fertilizer and pesticide, and a physical isolation layer is further constructed between the fertilizer and cyantraniliprole and clothianidin, thereby better solving the problem of poor mixing stability between cyantraniliprole and the fertilizer, and the coating agent has good forming and bonding effects, providing a good basis for more uniformly coating the fertilizer.

[0035] (3) By adopting the combined method of gel network coating and physical isolation of the coating agent, the present invention significantly improves the stability of cyantraniliprole in nitrogen-containing fertilizers, can preferably solve the technical problem of poor stability of the cyantraniliprole fertilizer and pesticide, thereby ensuring the quality and drug effect of the fertilizer and pesticide granule, significantly improving the fertilizer effect and pest control effect, more effectively killing or controlling pests, and ensuring the growth and yield of crops.

[0036] (3) The fertilizer and pesticide prepared by the present invention are added with a variety of slow-release components, so that the drug effect and fertilizer effect last for a long time, can reduce the loss and decomposition of pesticides, thereby reducing the pollution risk to the environment such as soil and water sources, conforming to the policy orientation of reducing the application amount and increasing the efficiency of chemical fertilizers and pesticides and protecting the farmland environment in China, and contributing to promoting the green development and sustainable development of agricultural production.

[0037] (4) The fertilizer and pesticide prepared by the present invention have excellent stability and long-term effectiveness, thereby reducing the number of pesticide applications and the dosage of pesticides, reducing the production cost of farmers, and improving economic benefits.

[0038] (5) The medicated fertilizer prepared by the present invention contains cyantraniliprole and clothianidin, which can reduce the insect population base in the soil and has a good preventive effect on crop pests. Especially for sugarcane borers, it can also prevent other sugarcane pests such as thrips and cutworms.

[0039] (6) The medicated fertilizer granule prepared by the present invention can be used in the environment resistant to chlorantraniliprole, which helps to improve the control effect of sugarcane pests. Specific Embodiments

[0040] The present invention will be further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the following embodiments.

[0041] In order to make the purpose, technical solution and advantages of the present invention clearer, the present invention will be further specifically described in conjunction with the following specific embodiments. According to the following embodiments, those skilled in the art can better understand the present invention and can implement it. It should be understood that the specific embodiments described herein are only used to interpret the present invention and are not used to limit the present invention. It should be particularly noted that any modifications, equivalent replacements and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention, but the embodiments cited are not used to limit the present invention.

[0042] Example 1: Preparation of Sustained-Release Medicated Fertilizer

[0043] The preparation method of the sustained-release medicated fertilizer in this example includes the following steps:

[0044] (1) Preparation of soft film medicated fertilizer core particles: 24 g of cyantraniliprole (content 95%), 96 g of clothianidin (content 95%), 50 g of polysorbate-20, and 830 g of solvent (560 g of dimethylformamide + 270 g of deionized water) are mixed and dissolved to prepare 1000 g of the original drug solution. Then, 1000 g of the original drug solution is first fully mixed with 4500 g of freshly prepared gelling agent A, ultrasonically dispersed for 30 min, and then 4500 g of freshly prepared gelling agent B is added and fully mixed. Glacial acetic acid is added to adjust the pH value of the system to 4.0 to form a hydrogel. Finally, it is freeze-dried for 12 h and pulverized to obtain soft film medicated fertilizer core particles;

[0045] Among them, the preparation method of gelling agent A includes the following steps: 25 g of chitosan is dissolved in 4950 g of acidic dimethylformamide aqueous solution (3750 g of deionized water + 1200 g of DMF), and the pH of the dimethylformamide aqueous solution is 5.0. It is ultrasonically dispersed until transparent to obtain gelling agent A;

[0046] The preparation method of gelling agent B includes the following steps: 25 g of sodium alginate is dissolved in 4975 g of dimethylformamide aqueous solution (3750 g of deionized water + 1225 g of DMF), and it is ultrasonically dispersed until transparent to obtain gelling agent B.

[0047] (2) Preparation of multi-layer sustained-release fertilizer core: 200 g of soft-film fertilizer core particles (part of the soft-film fertilizer core particles prepared in step (1)) are added to a coating machine, the coating agent is mixed with water and dispersed evenly, and then sprayed on the outer layer of the soft-film fertilizer core particles three times, using 10 g of the coating agent each time, and pre-cured by hot air at 80° C. for 5 minutes after spraying; after spraying, the particles are dried to obtain a multi-layer sustained-release fertilizer core.

[0048] Among them, the preparation method of the shelling agent specifically includes: adding 5g of polyvinyl alcohol, 1.5g of polyvinyl pyrrolidone, 0.3g of nano calcium carbonate particles, 0.1g of sodium dodecyl sulfate, 0.75g of glycerol, and 42g of water to a container in sequence, heating and stirring in a 95°C water bath to disperse them evenly to obtain a mixed shelling liquid, and after the mixed shelling liquid is cooled to room temperature, adding 0.1g of a 5% mass concentration of glutaraldehyde solution, stirring and mixing evenly to obtain a shelling agent.

[0049] (3) Preparation of the drug fertilizer granules: 200 g of the multilayer slow-release drug fertilizer core was fully mixed with 60 kg of fertilizer and 39.8 kg of kaolin to obtain a mixture, and then the mixture was added to a granulator to obtain granules, which were dried and sieved to obtain the drug fertilizer granules. After this step, the theoretical mass content of the original drug was 0.10135%, of which the content of cyantraniliprole was 0.02027% and that of clothianidin was 0.08108%.

[0050] (4) The coating agent is mixed with water to prepare a coating solution, and then 100 kg of the fertilizer granules are added to the coating machine, and 5 kg of the coating solution is sprayed to make the coating material adhere to the surface of the fertilizer granules. After drying, a slow-release fertilizer product is obtained.

[0051] The preparation process of the coating solution includes: adding 0.3 kg polyvinyl alcohol, 0.1 kg glycerol, 0.025 kg polyethylene glycol, and 4.575 kg water into a container in sequence, heating to 95° C. and stirring until dissolved.

[0052] After comprehensive calculation, the theoretical mass content of the original drug in the slow-release fertilizer is 0.10092%. (That is, the theoretical mass content of the original drug is approximately equal to 0.10%).

[0053] Comparative Example 1: Preparation of common fertilizer

[0054] In this embodiment, comparative example 1 is provided, and comparative example 1 is a common medicated fertilizer without a sustained-release component. The preparation method of the common medicated fertilizer comprises the following steps: cyantraniliprole, clothianidin original medicine, and fertilizer are fully mixed with fillers and additives in the same proportions as in the above embodiment 1, and then the materials are added to a disc granulator to obtain spherical particles; and after drying, the particles are sieved to obtain a common medicated fertilizer product.

[0055] Example 2: Decomposition Rate Test

[0056] Referring to the preparation method of Example 1, samples A1 - A8 containing different fertilizer components were prepared respectively. Referring to the preparation method of Comparative Example 1, samples B1 - B8 containing different fertilizer components were prepared respectively. Then, samples A1 - A8 and B1 - B8 were thermally stored respectively at a temperature of 54 ± 2 °C, and the decomposition rate test was carried out according to the following test method.

[0057] Test method: After 14 days of thermal storage, the test samples were taken out. After the samples were cooled to room temperature, referring to the test method of "2.3 Other Preparations" in GB / T19136 - 2003, the determination of the mass fraction of the active ingredient in the test samples was completed using high - performance liquid chromatography within 24 hours. The test results are shown in Table 1:

[0058] Table 1 Influence of Different Fertilizers on the Stability of Pharmaceutical Fertilizer Granules

[0059]

[0060] As can be seen from Table 1, for the ordinary pharmaceutical fertilizer prepared by the conventional method, the thermal storage decomposition rate of cyantraniliprole is at a relatively high level. This means that during storage, a large amount of cyantraniliprole will decompose, which will cause the content of the active ingredient in the pharmaceutical fertilizer to decrease rapidly, unable to achieve the expected effect of preventing and controlling pests and diseases, and affecting the growth and yield of crops. In sharp contrast to the ordinary pharmaceutical fertilizer, by using the method for preparing the slow - release pharmaceutical fertilizer of the present invention, the decomposition rate of cyantraniliprole in its products is significantly reduced. It can better maintain the stability of cyantraniliprole during storage and use, enabling its active ingredient to play a role more durably, thus ensuring the control effect of the pharmaceutical fertilizer on pests and diseases, meeting the needs during the growth process of crops, and providing a more reliable guarantee for agricultural production.

[0061] The slow - release pharmaceutical fertilizer prepared by the present invention can solve the technical problem of poor stability of the cyantraniliprole - containing pharmaceutical fertilizer, is more superior and practical compared with the conventional ordinary pharmaceutical fertilizer, can ensure the quality and efficacy of the pharmaceutical fertilizer granules, and meet the needs of agricultural production for pest control and pest resistance control.

[0062] Example 3: Nitrogen Nutrient Release Rate Test of Slow - Release Pharmaceutical Fertilizer and Ordinary Fertilizer

[0063] Referring to "GB / T 23348 - 2009 Slow - Release Fertilizers", the nitrogen release rate of the slow - controlled - release pharmaceutical fertilizer in the examples of the present invention was determined.

[0064] Taking the slow - release pharmaceutical fertilizers A1, A2, A3 in Example 3 and the ordinary pharmaceutical fertilizers B1, B2, B3 in Example 3 as test samples.

[0065] Table 2 Comparison Table of Nitrogen Nutrient Release Rates of Slow - Release Pharmaceutical Fertilizer and Ordinary Fertilizer

[0066]

[0067] As can be seen from Table 2, the fertilizer efficiency duration of ordinary pharmaceutical fertilizers is very short. After the nutrients are rapidly released, they can no longer provide nutrient support for crops subsequently. However, the controlled-release pharmaceutical fertilizers are different. They still have a certain nitrogen nutrient release rate at 56 d, indicating that they can continuously provide nutrients for crops such as sugarcane for a relatively long time, greatly extending the fertilizer efficiency, thereby reducing the number of fertilizations and saving labor and materials. Especially for crops with a relatively long growth cycle such as sugarcane, the slow-release pharmaceutical fertilizers can better meet the nutrient requirements of the entire growth cycle of the crops, promoting crop growth and increasing yields.

[0068] Through the data comparison in Table 2, it is fully proved the advantages of the slow-release pharmaceutical fertilizers prepared by the present invention in terms of slow-release effect, improving fertilizer utilization rate, and extending fertilizer efficiency.

[0069] Example 4: Drug release rate of controlled-release pharmaceutical fertilizers

[0070] Using the slow-release pharmaceutical fertilizer A2 in Example 3 and the ordinary pharmaceutical fertilizer B2 in Example 3 as test samples.

[0071] The dialysis bag method was used to determine the drug release rates of A2 and B2.

[0072] Take a section of dialysis bag (about 3 cm), add a certain mass of pharmaceutical fertilizer granules, then seal the dialysis bag and place it in a stoppered ground-glass Erlenmeyer flask containing 25 mL of 60% methanol aqueous solution (pH = 7). After sealing the Erlenmeyer flask, place it in a constant temperature oscillator (25 °C) and set the rotation speed to 250 rpm. At 1 d, 3 d, 5 d, 7 d, 10 d, 14 d, 28 d, 42 d, and 56 d respectively, take out 1 mL of the solution from the release medium, analyze and determine the concentration of the active ingredient in the release medium and calculate the cumulative release rate, and add 1 mL of 60% methanol aqueous solution to the Erlenmeyer flask to ensure that the total volume of the release medium remains unchanged.

[0073] Calculation formula for the cumulative release rate of the active ingredient:

[0074] where, E r represents the cumulative release rate of the active ingredient at time t, m act represents the total mass of the active ingredient in the pharmaceutical fertilizer granule, C t represents the concentration of the active ingredient in the release medium at time t, V t represents the volume of the release medium taken out each time, and V0 represents the total volume of the release medium.

[0075] Table 3 Cumulative release rates of active ingredients of slow-release pharmaceutical fertilizers and ordinary pharmaceutical fertilizers

[0076]

[0077] As can be seen from Table 3, compared with ordinary medicated fertilizers, the slow-release medicated fertilizer prepared by the present method has all its advantages. It has a significant slow-release effect. Active ingredients such as cyantraniliprole and clothianidin are not released in large amounts instantaneously like ordinary medicated fertilizers, but are released slowly. This characteristic also significantly improves the utilization rate of active ingredients, avoiding the large loss and waste caused by the rapid release of ordinary medicated fertilizers. Therefore, in actual application, the amount of medicine used can be greatly reduced, and there is no need to apply a large amount initially like ordinary medicated fertilizers to ensure the effect, thus reducing costs. In addition, ordinary medicated fertilizers often have a short drug effect, while the slow-release medicated fertilizer can continuously provide stable protection and nourishment for sugarcane in the long term. This series of advantages not only conforms to the policy of reducing the use of pesticides and chemical fertilizers promoted in China, but also guarantees the high efficiency and quality of sugarcane cultivation, protects the environment and promotes the sustainable development of agriculture.

[0078] Example 5: Control effect of medicated fertilizer granules on sugarcane borers

[0079] Samples A1 - A3 in Example 3, samples B1 - B3 in Example 3, and a commercially available 0.16% chlorantraniliprole·clothianidin sample (Zheken, produced by Guangxi Chemical Industry Research Institute Co., Ltd., with comparable nutrient content) were used as samples for the efficacy test.

[0080] Efficacy test design plan: The test plot is located in the main sugarcane production area of Jincheng Base of Guangxi Chemical Industry Research Institute Co., Ltd., Jincheng Tun, Jiangzhou District, Chongzuo City, Guangxi Zhuang Autonomous Region. The soil is sandy, the soil layer is loose, and the water and fertilizer conditions are average. 3 treatments were set in the experiment, each treatment was repeated 4 times, and a randomized block arrangement was adopted. The area of each plot was 41.6 m 2 . Isolation rows were set between blocks and between plots, and protective rows were set around. The application time of the medicine was during the soil covering stage. Small ditches were dug around the sugarcane planting rows, and the medicine was scattered into the ditches according to the set treatment dose of the medicine, and the medicine was completely covered with soil layer. The blank control plot only received soil covering treatment without applying any medicine and fertilizer.

[0081] Investigation method: 30 days after the application of the medicine, the number of all sugarcane plants in each plot was investigated respectively, and the number of dead heart seedlings was recorded.

[0082] The efficacy calculation method is as follows:

[0083] Rate of dead heart seedlings (%) = Number of dead heart seedlings / Total number of seedlings × 100%;

[0084] Control effect (%) = (Rate of dead heart seedlings in the control plot - Rate of dead heart seedlings in the treatment plot) / Rate of dead heart seedlings in the control plot × 100%.

[0085] Table 4 Control effect of medicated fertilizer granules on sugarcane borers

[0086] Pharmaceutical agent Dosage (kg / mu) Rate of dead heart seedlings (%) Control effect (%) A1 15 1.34 88.73％ A2 15 1.8 84.86％ A3 15 1.61 86.46％ B1 15 4.66 60.81％ B2 15 4.82 59.46％ B3 15 4.37 63.25％ Commercially available sample 15 1.78 85.03％ CK / 11.89 /

[0087] As can be seen from Table 4, the slow-release fertilizer-pesticide prepared by the present invention has a very significant control effect on sugarcane borers, and the control effect is greater than 84.8%. In contrast, the control effect of the ordinary fertilizer-pesticide on sugarcane borers is only so-so, far lower than that of the fertilizer-pesticide granule prepared by this method. Under the same application rate, since the original drug content in the fertilizer-pesticide used in this example is only 0.10%, the amount of drug used is reduced by 37.5%. The control effect of the slow-release fertilizer-pesticide of the present invention is still slightly better than that of the commercially available 0.16% chlorantraniliprole·clothianidin sample. Therefore, the slow-release fertilizer-pesticide of the present invention can achieve better control effects with less amount of drug used, which not only reduces the production cost, but also reduces the amount of pesticide application, realizing the goals of high efficiency, low toxicity, environmental friendliness and low risk, and conforming to the development trend of reducing the application amount and increasing the efficiency of pesticides and fertilizers in China.

[0088] Example 6: Effects of fertilizer-pesticide granules on the plant height, stem diameter growth and yield of sugarcane

[0089] Taking samples A1-A3, samples B1-B3 in Example 3 and the commercially available 0.16% chlorantraniliprole·clothianidin (N:P2O5:K2O = 15:15:15) as test samples, and preparing ordinary fertilizers (CK, without pesticides; N:P2O5:K2O = 15:15:15) for comparison (no slow-release agent is added during the granulation of ordinary fertilizers, and the extra surplus is supplemented with inert fillers such as kaolin, silica white or calcium carbonate powder, and no film coating treatment is carried out).

[0090] Test design plan: The test plot is located in the main sugarcane production area of Jincheng Base of Guangxi Chemical Industry Research Institute Co., Ltd., Jincheng Tun, Jiangzhou District, Chongzuo City, Guangxi Zhuang Autonomous Region. The soil is sandy, the soil layer is loose, and the water and fertilizer conditions are average. 3 treatments are set in the experiment, each treatment is repeated 4 times, and a randomized block arrangement is adopted. The area of each plot is 41.6m 2 . Isolation rows are set between blocks and between plots, and protection rows are set around.

[0091] The sugarcane variety is Zhongzhe 9. Mechanical operation is used for planting, and basal fertilizer is applied during planting; topdressing is carried out once during the stage of intertillage and soil cultivation. When topdressing, it is on the sugarcane row, and fertilization and soil cultivation are integrated mechanized. The plant height and stem diameter are measured once 3 months after planting, and then the growth indexes of sugarcane in each treatment are investigated once every 10d, 20d, and 30d respectively, and the yield is investigated and counted at the time of sugarcane harvest, and the relative yield increase rate and average single stem weight are calculated.

[0092] Table 5 Effects of different treatments on the plant height and stem diameter growth of sugarcane

[0093]

[0094] As can be seen from Table 5, the slow-release fertilizer for sugarcane of the present invention has a slow-release effect, which is more conducive to the growth of sugarcane. As time goes by, its effect becomes more and more significant. The indicators such as the plant height and stem diameter of sugarcane show a stable and good growth trend, and are significantly better than the commercially available samples and the control samples. At the same time, the slow-release fertilizer in this example can increase the yield of sugarcane by up to 16.11%, which is 1.76 times higher than that of the commercially available samples.

[0095] In summary, the slow-release fertilizer of the present invention has a good slow-release effect, enabling it to continuously release the active ingredients of the drug and nutrients during the growth process of sugarcane. It can not only effectively control sugarcane borers and reduce the withering rate of sugarcane, but also meet the nutrient requirements of sugarcane at different growth stages, thus helping sugarcane grow vigorously and achieving the goal of increasing production and income.

[0096] It should be noted that the above-described embodiments are only the preferred embodiments of the present invention, aiming to illustrate the technical solutions of the present invention rather than to limit them. For those skilled in the art, without departing from the materials and principles of the present invention, various forms of improvements can still be made, and these improvements should also be regarded as within the protection scope of the present invention.

Claims

1. A slow-release fertilizer containing cyantraniliprole, characterized in that: It is mainly made of the following raw materials: cyantraniliprole 0.01~1%, clothianidin 0.01~1%, fertilizer 20~60%, dispersing aid 1~5%, gelling agent 1~5%, coating agent 1~5%, solvent 1~15%, encapsulating agent 0.01~2.5%, filler 100%; The gelling agent is used to be mixed with cyantraniliprole and clothianidin to prepare soft-film fertilizer core particles; The encapsulating agent is wrapped around the outer layer of the soft film fertilizer core particle to form a multi-layer slow-release fertilizer core; The fertilizer and the filler are wrapped in the outer layer of the multi-layer slow-release medicinal fertilizer core to form medicinal fertilizer particles; The coating agent is wrapped around the outer layer of the medicinal fertilizer particles.

2. The slow-release fertilizer containing cyantraniliprole according to claim 1, characterized in that: The dispersing aid is at least one of calcium dodecylbenzene sulfonate, polyoxyethylene styrylphenol ether, polysorbate, sorbitan laurate, SP-2728, SP-SC29, fatty alcohol polyoxyethylene ether, and pull-opening powder BX; The solvent is one or more combinations of water, acetone, methanol, ethyl acetate, dimethylformamide, cyclohexanone, xylene, and glutaraldehyde; The gelling agent is at least one of hydroxypropyl methylcellulose, polyethylene glycol, sodium alginate, chitosan, starch, glycerol and ethylene glycol.

3. The slow-release fertilizer containing cyantraniliprole according to claim 1, characterized in that: The encapsulating agent is at least one of polyvinyl pyrrolidone, polyvinyl alcohol, polyethylene glycol, sodium alginate, chitosan, starch, nano calcium carbonate, sodium lauryl sulfate and glycerol.

4. The slow-release fertilizer containing cyantraniliprole according to claim 1, characterized in that: The coating agent is one or more combinations of hydroxypropyl methylcellulose, polyvinyl alcohol, polyethylene glycol, sodium alginate, chitosan, ethylene glycol, and glycerol.

5. The method for preparing the cyantraniliprole-containing slow-release fertilizer according to claims 1 to 4, characterized in that: The following steps are involved: (1) Preparation of soft-film fertilizer core particles: cyantraniliprole, clothianidin, the dispersing aid, and the solvent are mixed and dissolved to prepare a raw material solution, and the raw material solution is fully mixed with a gelling agent, wherein the mass ratio of the raw material solution to the gelling agent is 1:4-16, and the pH value of the mixed liquid is adjusted to 3.0-6.0 to form a hydrogel, and the mixture is freeze-dried and crushed to obtain soft-film fertilizer core particles; (2) Preparation of multi-layer slow-release fertilizer core: Add soft-film fertilizer core particles into a coating machine, spray the coating agent on the outer layer of the soft-film fertilizer core particles at least twice, and keep heating after each spraying to pre-solidify; after spraying, dry to obtain a multi-layer slow-release fertilizer core; (3) Preparation of the drug fertilizer granules: the multi-layer slow-release drug fertilizer core is fully mixed with the fertilizer and the filler to obtain a mixed material, and then the mixed material is added to a granulator to obtain granules, and then dried and sieved to obtain the drug fertilizer granules; (4) Coating: The coating agent is mixed with water to prepare a coating solution, and then the fertilizer granules are added to a coating machine. The coating solution is sprayed to make the coating material adhere to the surface of the fertilizer granules. After drying, a slow-release fertilizer is obtained.

6. The method for preparing a slow-release fertilizer containing cyantraniliprole according to claim 5, characterized in that: The mass ratio of the soft-film fertilizer core particles to the coating agent is 3-15:1, the mass ratio of the multi-layer slow-release fertilizer core, the fertilizer and the filler is 1:200-700:150-500, and the mass ratio of the coating agent to the fertilizer particles is 2-5:100-2000.

7. The method for preparing a slow-release fertilizer containing cyantraniliprole according to claim 5, characterized in that: The step (1) specifically comprises: mixing and dissolving cyantraniliprole, clothianidin, a dispersing aid and a solvent to prepare a raw drug solution, and taking the raw drug solution and the prepared gelling agent A to fully mix, ultrasonically or stirringly dispersing for 20 to 60 minutes, and then adding the prepared gelling agent B to fully mix, adding glacial acetic acid, adjusting the pH of the system to 4.0 to 5.5 to form a hydrogel, freeze-drying, and crushing to obtain soft film fertilizer core particles; the mass ratio of the raw drug solution, gelling agent A and gelling agent B is: 1:2 to 8:2 to 8; The preparation method of the gelling agent A comprises the following steps: dissolving chitosan in an acidic dimethylformamide aqueous solution, wherein the mass ratio of chitosan to the dimethylformamide aqueous solution is 1:150-250, the concentration of the dimethylformamide aqueous solution is 20-35%, and the pH value is 3.0-5.5, and dispersing by ultrasonic or stirring until transparent to obtain the gelling agent A; The preparation method of the gelling agent B comprises the following steps: dissolving sodium alginate in a dimethylformamide aqueous solution, wherein the mass ratio of chitosan to the dimethylformamide aqueous solution is 1:150-250, the concentration of the dimethylformamide aqueous solution is 20-35%, and dispersing by ultrasonication or stirring until transparent.

8. The method for preparing a slow-release fertilizer containing cyantraniliprole according to claim 5, characterized in that: In step (2), the preparation method of the encapsulating agent specifically comprises: adding polyvinyl alcohol, polyvinyl pyrrolidone, nano calcium carbonate particles / starch, sodium lauryl sulfate and / or glycerol, and water into a container in sequence, heating to 70-96° C. and stirring to make them dispersed evenly to obtain a mixed encapsulating liquid, and after the mixed encapsulating liquid is cooled to room temperature, adding glutaraldehyde solution, stirring and mixing to obtain an encapsulating agent; The mass ratio of polyvinyl alcohol, polyvinyl pyrrolidone, nano calcium carbonate particles / starch, sodium dodecyl sulfate and / or glycerol, and water is 3-12:1-4:0.2-0.8:0.8-3:30-60, the amount of glutaraldehyde solution is 0.1-1% of the mass of the mixed coating liquid, and the mass concentration is 2-10%.

9. The method for preparing a slow-release fertilizer containing cyantraniliprole according to claim 5, characterized in that: The process of preparing the coating solution specifically includes: adding hydroxypropyl methylcellulose and / or polyvinyl alcohol and / or sodium alginate, glycerol and / or polyethylene glycol and / or ethylene glycol, and water into a container in sequence, wherein the mass ratio of hydroxypropyl methylcellulose and / or polyvinyl alcohol and / or sodium alginate, glycerol and / or polyethylene glycol and / or ethylene glycol, and water is 1-6:2-3:90-100, heating to 70-96° C. and stirring until dissolved.

10. Use of the cyantraniliprole-containing slow-release fertilizer according to claims 1 to 4 in sugarcane planting and pest control.

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