Preparation method of water-soluble fertilizer for rice
By adding microalgae oil and mesoporous silica nanoparticles to water-soluble fertilizers, the problem of low utilization rate of traditional water-soluble fertilizers is solved, and the yield of rice and the chlorophyll content of leaves is significantly improved, and the heavy metals are reduced. absorb.
Patent Information
- Application Number
- CN202411410010.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-10
- Publication Date
- 2025-01-10
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The fertilizer utilization rate of traditional water-soluble fertilizers is low, which limits the growth and yield of rice.
Add microalgae oil to the water-soluble fertilizer and use mesoporous silica nanoparticles as carriers to prepare nanocomposite materials through steps such as emulsification and ultrasonic oscillation to improve fertilizer utilization and rice yield.
The unsaturated fatty acids, vitamins and mineral content in water-soluble fertilizers have been improved, the utilization rate of fertilizers and the growth of rice have been enhanced, the yield and chlorophyll content of leaves have been significantly improved, and the absorption of heavy metals has been reduced.
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Figure CN119285397A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of water-soluble fertilizers, and in particular to a method for preparing a water-soluble fertilizer for rice. Background Art
[0002] With the rapid development of modern agriculture, people have put forward higher requirements for the efficient use of fertilizers and the improvement of crop quality. Water-soluble fertilizer is a multi-component compound fertilizer that can be completely dissolved in water. It has the advantages of efficient absorption, balanced nutrition, flexible formula, safety and ease of use, and water and fertilizer saving.
[0003] For rice, an important food crop, the current fertilizer utilization rate of traditional water-soluble fertilizers is low and there are certain limitations in promoting rice growth. Summary of the invention
[0004] The technical task of the present invention is to address the above shortcomings and provide a method for preparing a water-soluble fertilizer for rice. By adding microalgae oil to the water-soluble fertilizer and using mesoporous silica nanoparticles as a carrier, the fertilizer utilization rate of the water-soluble fertilizer is improved, and the yield of rice can be increased, thereby solving the problem of low fertilizer utilization rate of traditional water-soluble fertilizers and limitations in rice growth.
[0005] To achieve the above object, the present invention provides the following technical solutions:
[0006] A method for preparing a water-soluble fertilizer for rice comprises the following steps:
[0007] S100, mixing the organic phase with the aqueous phase, and preparing a nanoemulsion after emulsification;
[0008] S200, mixing a surfactant with ethanol and ammonia water, adding a silicon source, stirring, filtering to obtain a solid substance, washing the solid substance and calcining to obtain mesoporous silica nanoparticles;
[0009] S300, mixing the nanoemulsion with the mesoporous silica nanoparticles, adding chloroform, and ultrasonically shaking, and after the organic reagent evaporates, obtaining a nanocomposite material;
[0010] S400, dissolving the nanocomposite material, diatomaceous earth, potassium dihydrogen phosphate, betaine, chelated magnesium, chelated zinc, and chelated manganese in deionized water, and preparing a water-soluble fertilizer by drying, crushing, and sieving.
[0011] Furthermore, in step S100, the organic phase is a mixed solution of microalgae oil and Tween 80, wherein the addition ratio of the microalgae oil and the Tween 80 is 5 to 20:1; the aqueous phase is a mixed solution of ethanol and deionized water, wherein the addition ratio of the ethanol and the deionized water is 1:31 to 65; the addition ratio of the nanoemulsion and the mesoporous silica nanoparticles is 1:1.
[0012] Further, in step 200, the surfactant is a hexadecyltrimethylammonium bromide solution, wherein the concentration of the hexadecyltrimethylammonium bromide solution is 5%;
[0013] Furthermore, in step 200, the silicon source is tetraethyl orthosilicate.
[0014] Furthermore, the addition ratio of the hexadecyltrimethylammonium bromide solution, the ethanol, the ammonia water and the tetraethyl orthosilicate is 25 ml: 25 ml: 6 ml: 1.7 g.
[0015] Furthermore, in step S300, the addition ratio of the nanoemulsion, the mesoporous silica nanoparticles and the chloroform is 100 mg: 100 μL: 1 ml.
[0016] Furthermore, in step S400, the addition ratio of the nanocomposite material, the diatomaceous earth, the potassium dihydrogen phosphate, the betaine, the chelated magnesium, the chelated zinc, the chelated manganese and the deionized water is 15:3:25:3:3:0.5:0.5:50.
[0017] Furthermore, in step S400, the drying temperature is 30-40°C.
[0018] Furthermore, in step S400, the mesh size of the sieving is 100 meshes.
[0019] Compared with the prior art, the advantages and positive effects of the present invention are:
[0020] 1. By adding microalgae oil to water-soluble fertilizer, the content of unsaturated fatty acids, vitamins and minerals in the water-soluble fertilizer is increased, the fertilizer utilization rate of the water-soluble fertilizer can be improved, and the growth and development of rice can be promoted;
[0021] 2. By using mesoporous silica nanoparticles as carriers, due to their high specific surface area, good pore structure and excellent adsorption performance, they can stably load and release the active ingredients in the microalgae oil in the water-soluble fertilizer, thereby further improving the fertilizer utilization rate of the water-soluble fertilizer;
[0022] 3. By optimizing the addition ratio of microalgae oil in water-soluble fertilizer, the fertilizer utilization rate of water-soluble fertilizer and rice yield can be improved. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0024] Figure 1 It is a schematic diagram of the process of the present invention;
[0025] Figure 2 is a transmission electron microscopy image of the nanoemulsion in Example 1;
[0026] Figure 3 This is a schematic diagram of the ultrastructure of mesoporous silica nanoparticles in Example 1;
[0027] Figure 4 Schematic diagram of the chlorophyll content curve of rice leaves measured by applying the fertilizers of Examples 1-4 and Comparative Examples 1-4. DETAILED DESCRIPTION
[0028] In order to more clearly understand the above-mentioned purpose, features and advantages of the present invention, the present invention is further described below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.
[0029] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.
[0030] Materials and sources are listed in Table 1:
[0031] Table 1 Materials and sources
[0032]
[0033]
[0034] Embodiment 1:
[0035] See also Figure 1 This embodiment provides a method for preparing a water-soluble fertilizer for rice, comprising the following steps:
[0036] S100, preparing a nanoemulsion.
[0037] Mix 5 parts of microalgae oil and 1 part of Tween 80 to obtain an organic phase; mix 1 part of ethanol and 65 parts of deionized water to obtain an aqueous phase; emulsify the organic phase and the aqueous phase under a magnetic stirrer, the emulsification conditions are 500 rpm, room temperature, and the emulsification time is 30 minutes, and then the nanoemulsion is formed after ultrasonic oscillation for 20 minutes.
[0038] S200. Prepare mesoporous silica nanoparticles.
[0039] Dissolve 1.25 g of hexadecyltrimethylammonium bromide in 25 ml of deionized water to obtain a 5% hexadecyltrimethylammonium bromide solution, then add 25 ml of ethanol and 6 ml of ammonia water to the 25 ml of 5% hexadecyltrimethylammonium bromide solution and stir, add 1.7 g of tetraethyl orthosilicate to the solution, stir at room temperature for 2 hours, filter and recover the obtained solid substance, wash the solid substance with deionized water and then calcine at a calcination temperature of 500°C for 7 hours to obtain mesoporous silica nanoparticles.
[0040] S300: preparing nanocomposite materials.
[0041] 100 uL of the nanoemulsion was mixed with 100 mg of mesoporous silica nanoparticles, and 1 ml of chloroform was added, mixed and ultrasonically vibrated for 20 min, and then placed in a fume hood to wait for the organic reagent to evaporate, thereby obtaining a nanocomposite material.
[0042] S400, preparing a water-soluble fertilizer.
[0043] Dissolve 15 parts of nanocomposite materials, 3 parts of diatomaceous earth, 25 parts of potassium dihydrogen phosphate, 3 parts of betaine, 3 parts of chelated magnesium, 0.5 parts of chelated zinc and 0.5 parts of chelated manganese in 50 parts of deionized water, mix well and dry at 30-40°C for 12 hours, crush and sieve to a mesh size of 100 to obtain a water-soluble fertilizer.
[0044] Embodiment 2:
[0045] S100, preparing nanoemulsion: mixing 10 parts of microalgae oil and 1 part of Tween 80 to obtain an organic phase. The other steps and conditions are the same as those in Example 1 and will not be described again.
[0046] S200, preparing mesoporous silica nanoparticles: the steps and conditions are the same as those in Example 1 and will not be repeated here.
[0047] S300, preparing nanocomposite materials: the steps and conditions are the same as those in Example 1, and will not be described in detail here.
[0048] S400, preparing water-soluble fertilizer: the steps and conditions are the same as those in Example 1, and will not be repeated here.
[0049] Embodiment 3:
[0050] S100, preparing a nanoemulsion: mixing 15 parts of microalgae oil and 1 part of Tween 80 to obtain an organic phase; mixing 1 part of ethanol and 31 parts of deionized water to obtain an aqueous phase; the other steps and conditions are the same as those in Example 1 and will not be repeated here.
[0051] S200, preparing mesoporous silica nanoparticles: the steps and conditions are the same as those in Example 1 and will not be repeated here.
[0052] S300, preparing nanocomposite materials: the steps and conditions are the same as those in Example 1, and will not be described in detail here.
[0053] S400, preparing water-soluble fertilizer: the steps and conditions are the same as those in Example 1, and will not be repeated here.
[0054] Embodiment 4:
[0055] S100, preparing a nanoemulsion: mixing 20 parts of microalgae oil and 1 part of Tween 80 to obtain an organic phase; mixing 1 part of ethanol and 48 parts of deionized water to obtain an aqueous phase; the other steps and conditions are the same as those in Example 1 and will not be repeated here.
[0056] S200, preparing mesoporous silica nanoparticles: the steps and conditions are the same as those in Example 1 and will not be repeated here.
[0057] S300, preparing nanocomposite materials: the steps and conditions are the same as those in Example 1, and will not be described in detail here.
[0058] S400, preparing water-soluble fertilizer: the steps and conditions are the same as those in Example 1, and will not be repeated here.
[0059] Comparative Example 1: Preparation of a blank control In this comparative example, 600 ml of deionized water was used instead of water-soluble fertilizer.
[0060] Comparative Example 2: Preparation of water-soluble fertilizer without adding nanocomposite materials. The preparation method is to dissolve 3 parts of diatomaceous earth, 25 parts of potassium dihydrogen phosphate, 3 parts of betaine, 3 parts of chelated magnesium, 0.5 parts of chelated zinc, and 0.5 parts of chelated manganese in 65 parts of deionized water, mix well and dry at a temperature of 30-40°C for 12 hours, crush and sieve to a mesh size of 100 mesh.
[0061] Comparative Example 3: Preparation of water-soluble fertilizer without adding nanoemulsion.
[0062] 1.25 g of hexadecyltrimethylammonium bromide was dissolved in an appropriate amount of 25 ml of deionized water to obtain a 5% hexadecyltrimethylammonium bromide solution, and then 25 ml of ethanol and 6 ml of ammonia water were added to the 25 ml of the 5% hexadecyltrimethylammonium bromide solution, and stirred. 1.7 g of tetraethyl orthosilicate was added to the solution, and stirred at room temperature for 2 hours. The obtained solid material was filtered and recovered, and the solid material was washed with deionized water and then calcined at a calcination temperature of 500° C. for 7 hours to obtain mesoporous silica nanoparticles;
[0063] 100 mg of mesoporous silica nanoparticles were mixed with 1 ml of chloroform and subjected to ultrasonic oscillation for 20 min, and then placed in a fume hood to wait for the organic reagent to evaporate, thereby obtaining the treated mesoporous silica nanoparticles;
[0064] 15 parts of treated mesoporous silica nanoparticles, 3 parts of diatomaceous earth, 25 parts of potassium dihydrogen phosphate, 3 parts of betaine, 3 parts of chelated magnesium, 0.5 parts of chelated zinc, and 0.5 parts of chelated manganese are dissolved in 50 parts of deionized water, mixed and dried at a drying temperature of 30-40°C for 12 hours, crushed and sieved with a mesh size of 100 to obtain a water-soluble fertilizer without adding nanoemulsion.
[0065] Comparative Example 4: Preparation of water-soluble fertilizer without adding mesoporous silica nanoparticles.
[0066] 10 parts of microalgae oil and 1 part of Tween 80 were mixed to obtain an organic phase; 1 part of ethanol and 65 parts of deionized water were mixed to obtain an aqueous phase; the organic phase and the aqueous phase were emulsified under a magnetic stirrer at 500 rpm, room temperature, and an emulsification time of 30 minutes, and then subjected to ultrasonic oscillation for 20 minutes to form a nanoemulsion;
[0067] 100uL of the nanoemulsion was mixed with 1ml of chloroform and ultrasonically vibrated for 20min, and then placed in a fume hood to wait for the organic reagent to evaporate, thereby obtaining the treated nanoemulsion;
[0068] 15 parts of the treated nanoemulsion, 3 parts of diatomaceous earth, 25 parts of potassium dihydrogen phosphate, 3 parts of betaine, 3 parts of chelated magnesium, 0.5 parts of chelated zinc, and 0.5 parts of chelated manganese are dissolved in 50 parts of deionized water, mixed and dried at a drying temperature of 30-40°C for 12 hours, crushed and sieved with a mesh size of 100 to obtain a water-soluble fertilizer without adding mesoporous silica nanoparticles.
[0069] Rice planting and fertilizer application:
[0070] Rice was planted on 8 mu of experimental land, with 200m 21000 holes were planted in one area, with 3 plants in each hole, 30 cm between rows and 20 cm in the longitudinal direction. There was one group per mu, with a total of 8 groups. Each group was 4 to 5 meters apart, and three areas were set up in each group, which were three parallel areas. During the experiment, except for the different fertilizer components and ratios, the rest of the management was the same. The specific fertilization method is shown in Table 2.
[0071] Table 2 Fertilization methods
[0072]
[0073] The chlorophyll content of fresh rice leaves was measured at the tillering stage, jointing stage, flowering stage, filling stage and maturity stage; after the rice was harvested, the element content of the rice was measured, and the weight of each area after harvest was weighed and counted to calculate the yield and thousand-grain weight. The specific detection method is as follows:
[0074] (1) Determination of element content:
[0075] Collect naturally air-dried rice, husk it and crush it into a uniform sample, accurately weigh 0.5g of sample and place it in a digestion tank, add 5ml nitric acid to digest and drive away the acid, transfer the digestion solution to a 50ml volumetric flask after cooling to room temperature, wash the digestion tank 3 times with deionized water, transfer it to a volumetric flask and adjust the volume to the scale, and mix well. The blank solution preparation method is the same as above. ICP-MS is used to determine the content of phosphorus, potassium, magnesium, zinc, manganese, silicon, chromium, cadmium, arsenic, and lead. The signal response value is the ordinate (Y) and the mass concentration of the standard product is the abscissa (X) to draw a standard curve. The element content is calculated according to the standard curve. The calculation formula is as follows.
[0076]
[0077] Wherein, C is the content of the element to be measured in the sample (mg / kg); C1 is the concentration of the element to be measured in the sample (ng / mL); C0 is the concentration of the element to be measured in the blank sample (ng / mL); V is the total volume of the sample (mL); m is the mass of the sample (g);
[0078] (2) Determination of chlorophyll content:
[0079] Three fresh rice leaves were randomly selected from each area at the tillering stage, jointing stage, flowering stage, filling stage and maturity stage, cut into pieces and mixed evenly. 5 mg of the broken samples were weighed and placed in a 50-mL centrifuge tube. 25 mL of ethanol-acetone (1:1) mixture was added and shaken well. The leaves were kept away from light for 24 h until they turned completely white. The OD645 and OD663 values were measured and the chlorophyll content (mg / g) was calculated using the formula: Chl=20.2OD645+8.02OD663.
[0080] (3) Yield determination: When rice is harvested, each area weighs and counts the rice after harvest, and the average value of each group is calculated as the yield.
[0081] (4) Determination of thousand-grain weight: 1,000 grains were randomly selected from each area and weighed, and the average value of each group was taken as the thousand-grain weight.
[0082] Figure 2 is the transmission electron microscope image of the nanoemulsion of Example 1, Figure 3 This is a schematic diagram of the ultrastructure of mesoporous silica nanoparticles in Example 1. It can be seen from the figure that the nanoemulsion and the mesoporous silica nanoparticles are evenly distributed and are spherical.
[0083] The results of the rice leaf chlorophyll content test are shown in Table 3, and the curve diagram is shown in Figure 4 , from Table 3 and Figure 4 It can be seen that the chlorophyll content of rice leaves increased first and then decreased in the same group at different periods; in the same period, compared with the water-soluble fertilizer without nanoemulsion, mesoporous silica nanoparticles, nanocomposite materials, and the control group without fertilization, the chlorophyll content of rice leaves was higher after the water-soluble fertilizer with nanocomposite materials was applied, indicating that the nanocomposite materials have a positive effect on promoting rice photosynthesis, thereby increasing the chlorophyll content of rice leaves. From the T5-T8 groups of the same period, it can be seen that the chlorophyll content of rice leaves in the T6 group is the highest, indicating that the nanocomposite water-soluble fertilizer with an appropriate amount of microalgae oil can promote the photosynthesis of rice leaves.
[0084] Table 3 Effects of different fertilization treatments on chlorophyll content in rice leaves (P<0.05)
[0085]
[0086] The effects of different fertilization treatments on the content of each element in rice are shown in Table 4. It can be seen from T1 to T5 that compared with the water-soluble fertilizer without nanoemulsion, mesoporous silica nanoparticles, nanocomposite materials, and the control group without fertilization, the mineral element (phosphorus, potassium, magnesium, zinc, manganese, silicon) content in rice significantly increased after the water-soluble fertilizer with nanocomposite materials was applied, and the heavy metal content significantly decreased, indicating that the nanocomposite material enhanced the nutrient absorption capacity of rice for water-soluble fertilizer, and can effectively prevent heavy metal ions from being absorbed by rice. From T5 to T8, it can be seen that different ratios of microalgae oil in water-soluble fertilizer have different nutrient absorption and heavy metal fixation capacities for rice. When Tween 80: microalgae oil = 1:10, ethanol: deionized water = 1:38, the water-soluble fertilizer has the best effect.
[0087] Table 4 Effects of different fertilization treatments on the content of various elements in rice (P<0.05)
[0088]
[0089] The effects of different fertilization treatments on rice yield and thousand-grain weight are shown in Table 5. From T2 to T5, it can be seen that the rice yield and thousand-grain weight of the water-soluble fertilizer with nanocomposite materials are significantly higher than those of the water-soluble fertilizer without nanoemulsion, mesoporous silica nanoparticles, or nanocomposite materials, indicating that the nanocomposite materials promote the vigorous growth of rice. From T5 to T8, it can be seen that different proportions of microalgae oil in water-soluble fertilizers have different effects on rice yield and thousand-grain weight. When Tween 80: microalgae oil = 1:10, ethanol: deionized water = 1:38, rice yield and thousand-grain weight are the highest, while too little or too much microalgae oil may inhibit the growth of rice.
[0090] Table 5 Effects of different fertilization treatments on rice yield and 1000-grain weight (P<0.05)
[0091]
[0092] Through the above specific implementations, those skilled in the art can easily implement the present invention. However, it should be understood that the present invention is not limited to the above specific implementations. On the basis of the disclosed implementations, those skilled in the art can arbitrarily combine different technical features to achieve different technical solutions.
Claims
1. A method for preparing a water-soluble fertilizer for rice, characterized in that: The following steps are involved: S100, mixing the organic phase with the aqueous phase, and preparing a nanoemulsion after emulsification; S200, mixing a surfactant with ethanol and ammonia water, adding a silicon source, stirring, filtering to obtain a solid substance, washing the solid substance and calcining to obtain mesoporous silica nanoparticles; S300, mixing the nanoemulsion with the mesoporous silica nanoparticles, adding chloroform, and ultrasonically shaking, and after the organic reagent evaporates, obtaining a nanocomposite material; S400, dissolving the nanocomposite material, diatomaceous earth, potassium dihydrogen phosphate, betaine, chelated magnesium, chelated zinc, and chelated manganese in deionized water, and preparing a water-soluble fertilizer by drying, crushing, and sieving.
2. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step S100, the organic phase is a mixed solution of microalgae oil and Tween 80, wherein the addition ratio of the microalgae oil and the Tween 80 is 5 to 20:1; the aqueous phase is a mixed solution of ethanol and deionized water, wherein the addition ratio of the ethanol and the deionized water is 1:31 to 65; the addition ratio of the nanoemulsion and the mesoporous silica nanoparticles is 1:
1.
3. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step 200, the surfactant is a cetyltrimethylammonium bromide solution, wherein the concentration of the cetyltrimethylammonium bromide solution is 5%.
4. The method for preparing a water-soluble fertilizer for rice according to claim 3, characterized in that: In step 200, the silicon source is tetraethyl orthosilicate.
5. The method for preparing a water-soluble fertilizer for rice according to claim 4, characterized in that: The addition ratio of the hexadecyltrimethylammonium bromide solution, the ethanol, the ammonia water and the tetraethyl orthosilicate is 25 ml: 25 ml: 6 ml: 1.7 g.
6. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step S300 , the nanoemulsion, the mesoporous silica nanoparticles and the chloroform are added in a ratio of 100 mg: 100 μL: 1 ml.
7. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step S400, the nanocomposite material, the diatomaceous earth, the potassium dihydrogen phosphate, the betaine, the chelated magnesium, the chelated zinc, the chelated manganese and the deionized water are added in a ratio of 15:3:25:3:3:0.5:0.5:
50.
8. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step S400, the drying temperature is 30-40°C.
9. The method for preparing a water-soluble fertilizer for rice according to claim 1, characterized in that: In step S400, the mesh size of the sieving is 100 meshes.