A granule of a soil-borne disease special medicine and fertilizer and a preparation method thereof

Abstract

The application belongs to the technical field of medicine and fertilizer, and particularly relates to a special medicine and fertilizer granule for soil-borne diseases and a preparation method thereof. The granule is composed of a fungicidal effective component, a zinc-based slow-release material mixed carrier, a fertilizer effective component and the like. The zinc-based slow-release material mixed carrier is a complex of a chelate of at least one of polysaccharides such as chitosan, carboxymethyl chitosan and pectin and calcium chloride and a zinc-based slow-release material metal organic framework, ZIF-8. The medicine and fertilizer granule has the advantages that the zinc-based slow-release material metal organic framework ZIF-8 is used as a main slow-release carrier, the effective components of the pesticide and the fertilizer are prolonged in duration, the prevention and treatment effect on the soil-borne diseases is enhanced, the preparation method is simple, the disease prevention and treatment and the topdressing are simultaneously effective when applied, and the intensity and frequency of the farmers in applying the pesticide and the fertilizer are reduced.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of medicine and fertilizer, and particularly relates to a preparation method of a medicine and fertilizer granule special for soil-borne diseases and application thereof. BACKGROUND

[0002] With the continuous planting of crops and the development of protected land, the harm caused by soil-borne diseases of crops is increasing year by year. Soil-borne diseases include diseases caused by pathogenic bacteria, fungi, nematodes and viruses, and usually have the characteristics of multiple pathogen types, wide host range, strong concealment, fast transmission speed, large damage area and difficult control. If not intervened in time, it may lead to crop failure, which will cause serious yield and economic losses. Therefore, effectively preventing and controlling the occurrence of soil-borne diseases of crops has become an urgent problem to be solved to improve crop yield.

[0003] Due to the strong infectivity and concealment of soil-borne diseases, it is very difficult to prevent and control them. At present, the methods for preventing and controlling soil-borne diseases include screening of disease-resistant crop varieties, biological control, soil physical disinfection, chemical pesticide control and the like. The currently screened resistant varieties do not have permanent disease resistance and are prone to produce new pathogenic strains under conditions conducive to soil-borne diseases. Biological control is environmentally friendly and can replace or reduce the use of chemical pesticides, but its field application is relatively small. Soil physical disinfection often causes other pollution to the soil.

[0004] At present, the most effective method for preventing and controlling soil-borne diseases is chemical pesticide control, and seed dressing is a good control method, but its effect will be weakened in the later growth period of crops. Therefore, it is necessary to combine pre-sowing seed dressing, post-spraying treatment and other control methods for comprehensive prevention and control. However, long-term use of chemical pesticides may lead to drug resistance of diseases, influence on the environment and other negative problems.

[0005] In the traditional growth cycle of crops, disease control and fertilizer application are parallel operations, which increases the workload of farmers and easily leads to unreasonable use of pesticides and fertilizers, poor disease control effect and the like. SUMMARY

[0006] Therefore, in order to solve the problem, the application aims to provide a medicine and fertilizer granule special for soil-borne diseases and a preparation method thereof.

[0007] In order to achieve the above-mentioned purpose, the application adopts the following technical solutions.

[0008] The first technical purpose of the present application is to provide a soil-borne disease special medicine and fertilizer granule, which comprises the following components: pesticide fungicidal active ingredient, zinc-based slow-release material mixed carrier, fertilizer active ingredient, etc., wherein the zinc-based slow-release material mixed carrier is a complex of at least one of polysaccharides such as chitosan, carboxymethyl chitosan and pectin and calcium chloride and a composite of zinc-based slow-release material metal organic framework-zeolitic imidazolate framework ZIF-8.

[0009] Optionally, the pesticide fungicidal active ingredient refers to a fungicidal pesticide active ingredient with systemicity, and the mass percentage is 0.15%-0.4%.

[0010] Optionally, the fertilizer active ingredient contains macroelements (nitrogen, phosphorus and potassium) and other trace elements, and the mass percentage is 15%-21%; the macroelements can be selected from potassium dihydrogen phosphate, potassium chloride, urea, ammonium nitrate, etc.

[0011] Further, the contained trace element is zinc element, which is contained in the zinc-based slow-release material component.

[0012] Optionally, the raw material for synthesizing the metal organic framework-zeolitic imidazolate framework ZIF-8 is dimethyl imidazole and zinc salt, and the zinc salt can be zinc nitrate or zinc acetate and the corresponding hydrate thereof.

[0013] It should be noted that the present application combines the slow-release material-metal organic framework-zeolitic imidazolate framework ZIF-8 with the fertilizer granule, and based on the compounding of fungicides and fertilizers, the soil-borne disease prevention and control effect and the prevention and control period are increased, and the disease prevention ability and the growth promotion function of crops are improved, and the soil-borne disease resistance of crops is improved.

[0014] The preparation method of the medicine and fertilizer granule is as follows:

[0015] Step 1) first select one of polysaccharides such as chitosan, carboxymethyl chitosan and pectin to configure a polysaccharide aqueous solution with a mass percentage of 2%-3%, and add the fertilizer active ingredient containing nitrogen, phosphorus and potassium, the zinc salt of zinc nitrate or zinc acetate and the corresponding hydrate thereof, Tween 80 or Span 80 to the polysaccharide solution according to the mass percentages of 15%-21%, 2.2%-4.4% (relative to the mass of the polysaccharide aqueous solution) and 0.5% respectively and fully dissolve to obtain solution 1;

[0016] Step 2) weigh the pesticide active ingredient with a mass percentage of 0.15%-0.4% and dissolve it in a small amount of dimethyl sulfoxide, slowly add it to solution 1 under high-speed stirring, fully stir to obtain solution 2;

[0017] Step 3) weigh 12.5g of dimethyl imidazole and dissolve it in 200mL of saturated calcium chloride aqueous solution to obtain solution 3;

[0018] Step 4) drop solution 2 into solution 3 to form microspheres and continue to react for 3-5 hours to make the reaction sufficient;

[0019] Step 5) collect the microspheres prepared in step (4) and dry to obtain the soil-borne disease special fertilizer granules.

[0020] By changing the amount of zinc salt added, fertilizer granules with different internal structures can be obtained; and by changing the size of the outlet of the dropping pipe in step 4, fertilizer granules of different sizes can be obtained.

[0021] Compared with the prior art, the beneficial effects of the present application are:

[0022] The application discloses soil-borne disease special fertilizer granules and a preparation method thereof, which utilizes metal organic framework-zeolite imidazolate framework ZIF-8 as a slow-release carrier of the fertilizer granules, slows down the migration speed of pesticide effective components and fertilizer effective components in the environment, achieves a more long-acting soil-borne disease prevention and treatment effect, and slows down the application frequency of corresponding pesticides and fertilizers. BRIEF DESCRIPTION OF DRAWINGS

[0023] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained without creative labor on the basis of the provided drawings.

[0024] Figure 1 is a graph showing the influence of different zinc salt types and addition amounts on the internal structure of the granules.

[0025] Figure 2 is a fertilizer granule of different sizes obtained by controlling the outlet of the dropping pipe. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present application will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the present application, not all. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0027] Here, the special term "embodiment" as explained in any embodiment does not necessarily mean that it is superior or better than other embodiments. In the performance index test of the embodiments of the present application, unless otherwise specified, the conventional test method in the art is adopted. It should be understood that the terms described in the present application are only for describing the specific embodiments, and are not used to limit the disclosure of the present application.

[0028] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; methods and techniques similar to those specifically described herein are conventional methods and techniques adopted by those skilled in the art.

[0029] For a better understanding of the present application, numerous specific details are given in the following embodiments. It will be understood by those skilled in the art that the present application can be implemented without certain specific details. In the embodiments, some methods, means, instruments, devices and the like which are well known to those skilled in the art are not described in detail in order to highlight the essence of the present application.

[0030] The technical features disclosed in the embodiments of the present application can be combined arbitrarily without conflict, and the resulting technical solutions belong to the content disclosed in the embodiments of the present application.

[0031] The application discloses a special medicine and fertilizer granule for soil-borne diseases and a preparation method thereof.

[0032] For a better understanding of the present application, the following embodiments are further described in detail, but it should not be understood as limiting the present application. Some non-essential improvements and adjustments made by those skilled in the art according to the above content are also regarded as falling within the protection scope of the present application.

[0033] Example 1: 0.2% thifluzamide medicine and fertilizer granule

[0034] The above medicine and fertilizer granule comprises the following components with the weight percentage: thifluzamide 0.2%, urea 5%, potassium hydrogen phosphate 4%, potassium chloride 6%, and the carrier makes up 100%.

[0035] Step 1) 2.0 g of chitosan, 95.5 g of deionized water, 0.5 g of Tween 80 and 2.0 g of acetic acid are mixed to form a 2% chitosan aqueous solution by mass percentage; urea 3.5 g, potassium hydrogen phosphate 2.8 g and potassium chloride 4.2 g are added to the solution, dissolved and stirred uniformly, then 2.2 g of zinc acetate dihydrate is added and stirred to disperse uniformly to obtain solution 1;

[0036] Step 2) 0.61 g of thifluzamide technical material is weighed and dissolved in 3 mL of dimethyl sulfoxide, slowly added dropwise into the rapidly stirred solution 1, fully stirred and then ultrasonicated to remove all bubbles in the solution to obtain solution 2;

[0037] Step 3) 12.5 g of dimethyl imidazole is dissolved in 200 mL of saturated calcium chloride aqueous solution to obtain solution 3;

[0038] Step 4) Under room temperature, solution 2 is added dropwise into solution 3 under stirring to form microspheres, and the stirring is continued for 3-5 hours to ensure the reaction is complete;

[0039] Step 5) After the microspheres are collected and the surface liquid is removed, drying is performed to obtain the fertilizer granules.

[0040] Example 2: 0.4% thifluzamide fertilizer granules

[0041] The above-mentioned fertilizer granules comprise the following components with the following weight percentages: thifluzamide 0.4%, ammonium nitrate 5%, potassium phosphate dibasic 4%, potassium chloride 6%, and the carrier makes up 100%.

[0042] Step 1) 2.0 g of carboxymethyl chitosan, 95.5 g of deionized water, 0.5 g of Tween 80, and 2.0 g of acetic acid are mixed to form a 2% carboxymethyl chitosan aqueous solution; 3.5 g of ammonium nitrate, 2.8 g of potassium phosphate dibasic, and 4.2 g of potassium chloride are added to the solution, dissolved and stirred uniformly, and then 2.2 g of zinc acetate dihydrate is added and stirred to disperse uniformly to obtain solution 1;

[0043] Step 2) 1.22 g of thifluzamide technical material is weighed, dissolved in 3 mL of dimethyl sulfoxide, slowly added dropwise into rapidly stirred solution 1, and after sufficient stirring, ultrasonic is performed to remove all bubbles in the solution to obtain solution 2;

[0044] Step 3) 12.5 g of dimethyl imidazole is dissolved in 200 mL of saturated calcium chloride aqueous solution to obtain solution 3;

[0045] Step 4) Under room temperature, solution 2 is added dropwise into solution 3 under stirring to form microspheres, and the stirring is continued for 3-5 hours to ensure the reaction is complete;

[0046] Step 5) After the microspheres are collected and the surface liquid is removed, drying is performed to obtain the fertilizer granules.

[0047] Example 3: 0.15% tebuconazole fertilizer granules

[0048] The above-mentioned fertilizer granules comprise the following components with the following weight percentages: tebuconazole 0.15%, urea 5%, potassium phosphate dibasic 5%, potassium chloride 6%, and the carrier makes up 100%.

[0049] Step 1) 3.0 g of chitosan, 94.5 g of deionized water, 0.5 g of Tween 80, and 2.0 g of acetic acid are mixed to form a 3% chitosan aqueous solution; 3.5 g of urea, 3.5 g of potassium phosphate dibasic, and 4.2 g of potassium chloride are added to the solution, dissolved and stirred uniformly, and then 3.5 g of zinc nitrate hexahydrate is added and stirred to disperse uniformly to obtain solution 1;

[0050] Step 2) 0.46 g of tebuconazole technical material was weighed and dissolved in 3 mL of dimethyl sulfoxide, which was slowly added dropwise into the rapidly stirred solution 1, and after sufficient stirring, ultrasonic was applied until all the bubbles in the solution were removed to obtain solution 2;

[0051] Step 3) 12.5 g of dimethyl imidazole was dissolved in 200 mL of saturated calcium chloride aqueous solution to obtain solution 3;

[0052] Step 4) Under room temperature conditions, solution 2 was added dropwise into solution 3 under stirring to form microspheres, and the stirring was continued for 3-5 hours to ensure sufficient reaction;

[0053] Step 5) The microspheres were collected and the surface liquid was removed, and then dried to obtain the fertilizer granules.

[0054] Example 4: 0.3% tebuconazole fertilizer granules

[0055] The above-mentioned fertilizer granules comprise the following components with the following weight percentage: tebuconazole 0.3%, urea 7%, di-potassium hydrogen phosphate 7%, potassium chloride 7%, and the carrier makes up 100%.

[0056] Step 1) 2.0 g of pectin, 95.5 g of deionized water, 0.5 g of Span 80 and 2.0 g of acetic acid were mixed to form a 2% mass percentage pectin aqueous solution; 4.9 g of urea, 4.9 g of di-potassium hydrogen phosphate and 4.9 g of potassium chloride were added to the solution, dissolved and stirred uniformly, and then 3.5 g of zinc acetate was added and stirred to disperse uniformly to obtain solution 1;

[0057] Step 2) 0.92 g of tebuconazole technical material was weighed and dissolved in 3 mL of dimethyl sulfoxide, which was slowly added dropwise into the rapidly stirred solution 1, and after sufficient stirring, ultrasonic was applied until all the bubbles in the solution were removed to obtain solution 2;

[0058] Step 3) 12.5 g of dimethyl imidazole was dissolved in 200 mL of saturated calcium chloride aqueous solution to obtain solution 3;

[0059] Step 4) Under room temperature conditions, solution 2 was added dropwise into solution 3 under stirring to form microspheres, and the stirring was continued for 3-5 hours to ensure sufficient reaction;

[0060] Step 5) The microspheres were collected and the surface liquid was removed, and then dried to obtain the fertilizer granules.

[0061] As Figure 1It can be seen that a large number of large cavity structures are formed inside the granules at a lower zinc salt addition, and the space distribution inside the granules is uneven. At an addition amount of 4.4%, whether zinc acetate dihydrate or zinc nitrate hexahydrate, the granules present a uniform honeycomb structure inside, which can keep the granules uniform and consistent, and the fine and uniform cavities can ensure the uniformity of the release dynamics of the pesticide active ingredients or fertilizer elements, and is conducive to the stable performance of the product.

[0062] In order to further prove the beneficial effects of the present application and better understand the present application, the technical features disclosed in the present application are further illustrated by the following application test examples, but it should not be understood as limiting the present application. Other improvements made by those skilled in the art without creative work based on the above disclosure are also considered to fall within the protection scope of the present application.

[0063] Test Example 1: Field control effect test of thifluzamide pesticide fertilizer granules on peanut white thread blight

[0064] Test site: a peanut field of a farmer in Judong Town, Yangxi County, Yangjiang City, Guangdong Province, the land is flat, and peanuts have been planted for more than 5 years, and the peanut white thread blight has been more serious in recent years.

[0065] Test design: at the same time as a certain brand of thifluzamide granules on the market, the plot area is 50m 2 , randomly arranged test area groups, three repetitions for each treatment. The pesticide fertilizer is applied by seedling stage scattering, and the amount of each mu is 10 kg of Example 1 (10 kg), 5 kg of Example 2, and the control group uses the same amount of thifluzamide as Examples 1 and 2. Normal irrigation water, 30d, 45d and 60d after the application of pesticide fertilizer, respectively, investigate, five-point random sampling to calculate the peanut white thread blight control effect.

[0066] The disease index grading standard is as follows: 0 level: no symptoms on the plant; 1 level: disease spots on the inoculated stem base; 3 level: wilting and shriveling on the stem base, and 1 / 3 or less of the plant showing systemic symptoms (wilting, death, wilting, etc.), and there are few mycelia on the soil surface; 5 level: 2 / 3 or less of the plant showing systemic symptoms (wilting, death, wilting, etc.), and there are a large number of mycelia or sclerotia on the soil surface; 7 level: 2 / 3 or more of the plant showing systemic symptoms (wilting, death, wilting, etc.); 9 level: the plant completely withers and dies.

[0067] Disease incidence (%) = number of diseased plants / total number of plants investigated × 100%

[0068] Disease index = Σ (number of diseased plants × corresponding level) / (total number of plants investigated × highest level) × 100

[0069] Control effect (%) = (disease index of water control - disease index of treatment / disease index of water control) × 100

[0070] Table 1 Field control effect of thifluzamide pesticide fertilizer granules on peanut sclerotinia blight

[0071] Treatment / control effect 30 days after treatment 45 days after treatment 60 days after treatment Control 85.4％ 79.3％ 73.9％ Example 1 89.5％ 85.4％ 79.6％ Example 2 88.7％ 84.6％ 80.1％

[0072] As shown in Table 1, the pesticide fertilizer granules of the present application use slow-release materials as carriers, and can exhibit long-term disease control effect when used for the prevention and control of soil-borne peanut sclerotinia blight, can reduce the total use amount of pesticide active ingredients, reduce the physical expenditure of farmers in disease prevention and control, and protect the yield and quality of agricultural products.

[0073] Test Example 2: Field control effect test of pentazocine pesticide fertilizer granules on wheat foot rot

[0074] Test site: a wheat field of a farmer in Shuanghe Town, Queshan County, Zhumadian City, Henan Province, flat land, planted spring wheat for more than 5 years, and the wheat foot rot began to aggravate three years ago.

[0075] Test design: simultaneously applied with a certain brand of pentazocole granules on the market, plot area 25m 2 , randomly arranged test area groups, three replicates per treatment. Adopting pre-sowing trenching for pesticide fertilizer, measuring 20 kg of Example 4 and 10 kg of Example 5 per mu, and the control group using the same amount of pentazocole as Example 4 and Example 5. Investigate the occurrence of wheat foot rot at the wheat booting stage and maturity stage respectively, 100 plants are randomly sampled at each point (edge row is not taken) in each plot, and the number of wheat foot rot plants is recorded respectively, and the disease incidence and control effect are calculated.

[0076] Control effect = (disease incidence of control - disease incidence of treatment) / disease incidence of control x 100%

[0077] Table 2 Field control effect of pentazocole pesticide fertilizer granules on wheat foot rot

[0078] Treatment / control effect At the booting stage At the mature stage Control 74.28％ 71.44％ Example 4 80.43％ 78.96％ Example 5 81.33％ 78.68％

[0079] As shown in Table 2, the pesticide fertilizer granules of the present application use slow-release materials as carriers, and have good control effect when used for the prevention and control of soil-borne wheat foot rot, and the effect is better than that of the marketized dosage form.

[0080] The above description of the disclosed embodiments enables a person skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to these embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A special granular pesticide and fertilizer formulation for soil-borne diseases, characterized in that, It contains the following components: pesticide bactericidal active ingredient, zinc-based slow-release material mixed carrier, and fertilizer active ingredient; among which, The active ingredient in the pesticide is a systemic fungicidal active ingredient, and its mass percentage is 0.15%-0.4%. The effective components of the fertilizer include nitrogen, phosphorus, potassium and other trace elements, which account for 15%-21% by mass. The preparation method of the soil-borne disease-specific fertilizer granules specifically includes the following steps: (1) Prepare a polysaccharide aqueous solution with a mass percentage of 2%-3%, and add the fertilizer active ingredients, zinc salt, Tween 80 or Span 80 to the polysaccharide solution and dissolve them completely to obtain solution 1; The polysaccharide is at least one of chitosan, carboxymethyl chitosan, and pectin; The zinc salt is zinc nitrate or zinc acetate and their corresponding hydrates; The amount of zinc salt used is 4.4% by mass of the polysaccharide aqueous solution; (2) Dissolve the active ingredient of pesticide in dimethyl sulfoxide, and then slowly add it to solution 1 under high-speed stirring. After stirring thoroughly, solution 2 is obtained. (3) Weigh dimethylimidazolium and dissolve it in a saturated calcium chloride aqueous solution to obtain solution 3; (4) Add solution 2 dropwise to solution 3 to react and form microspheres, and continue the reaction for 3-5 hours to ensure that the reaction is complete; (5) Collect the microspheres prepared in step (4) and dry them to obtain the soil-borne disease-specific fertilizer granules.

2. The soil-borne disease-specific fertilizer granule according to claim 1, characterized in that, The amount of Tween 80 or Span 80 used is 0.5% by mass of the polysaccharide aqueous solution; the ratio of dimethylimidazole to saturated calcium chloride aqueous solution is 12.5g:200mL.

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