Preparation process of high-efficiency low-temperature growth-promoting liquid fertilizer containing tetranitrogen

Abstract

This application relates to the field of agricultural fertilizer technology and discloses a preparation process for a high-efficiency, low-temperature growth-promoting tetranitrogen liquid fertilizer, comprising the following steps: Step 1, selecting high-quality sheepskin as the organic nitrogen source and treating the sheepskin; Step 2, hydrolyzing the sheepskin at 55℃ using microorganisms and active enzymes for 24 hours; Step 3, performing preliminary filtration on the hydrolyzed mixture; Step 4, further purifying the amino acid liquid through multi-stage filtration; Step 5, concentrating the amino acid liquid to 40% concentration using vacuum evaporation technology; Step 6, mixing the concentrated amino acid liquid with urea ammonium nitrate solution, magnesium sulfate, ferrous sulfate, seaweed concentrate, nitrification inhibitor, and excipients in a specific ratio. By scientifically proportioning the high-concentration amino acid liquid with urea ammonium nitrate, magnesium sulfate, ferrous sulfate, seaweed concentrate, and nitrification inhibitor, comprehensive nutritional support is provided for crops, effectively improving crop growth rate, stress resistance, and yield.

Description

Technical Field

[0001] This invention relates to the field of agricultural fertilizer technology, specifically to a preparation process for a high-efficiency, low-temperature growth-promoting tetranitrogen liquid fertilizer. Background Technology

[0002] In modern agriculture, nitrogen fertilizer is an indispensable element for crop growth. Traditional urea ammonium nitrate solution, a commonly used nitrogen fertilizer, primarily provides three nitrogen structures (ammonium nitrogen, nitrate nitrogen, and amide nitrogen). However, the limitations of this fertilizer form are becoming increasingly apparent. First, it contains only inorganic components and cannot effectively improve and increase the organic matter content in the soil. Soil organic matter is a crucial factor in maintaining soil health; it improves soil structure, increases water and fertilizer retention capacity, and promotes microbial activity. Furthermore, urea ammonium nitrate solution lacks mesonutrients and micronutrients such as magnesium and iron, which play vital roles in crop physiological metabolism. Magnesium is an important component of chlorophyll and is essential for photosynthesis, while iron participates in chloroplast formation and redox reactions.

[0003] Another drawback of traditional urea ammonium nitrate solutions is their lack of amino acids and alginic acid. Amino acids are essential raw materials for crop protein synthesis, promoting crop growth and development, while alginic acid helps enhance crop resistance and tolerance to adverse environments. More importantly, traditional nitrogen fertilizers lack nitrification inhibitors, making nitrogen easily oxidized into nitrates by microorganisms in the soil, which are then lost into groundwater, wasting nitrogen fertilizer and causing environmental pollution.

[0004] In summary, existing technologies have significant shortcomings in improving soil structure, increasing fertilizer utilization, and crop yield. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a process for preparing a highly efficient, low-temperature growth-promoting tetranitrogen liquid fertilizer, which solves the significant deficiencies of existing technologies in improving soil structure, increasing fertilizer utilization, and crop yield.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a preparation process for a high-efficiency, low-temperature growth-promoting tetranitrogen liquid fertilizer, comprising the following steps; Step 1: Select high-quality sheepskin as the organic nitrogen source, and clean and cut the sheepskin; Step 2: Hydrolyze the sheepskin at 55°C for 24 hours using microorganisms and active enzymes; Step 3: Perform preliminary filtration on the hydrolyzed mixture to remove incompletely decomposed solid residues; Step 4: Further purify the amino acid liquid through multi-stage filtration; Step 5: Use vacuum evaporation technology to concentrate the amino acid liquid to 40% concentration; Step 6: Mix the concentrated amino acid liquid with urea ammonium nitrate solution, magnesium sulfate, ferrous sulfate, seaweed concentrate, nitrification inhibitor and excipients in the specified proportions. Step 7: Emulsify and homogenize the mixture; Step 8: Final filtration and filling.

[0007] Preferably, in step one, the sheepskin is cleaned using water containing 0.5% neutral detergent. After cleaning, the sheepskin is air-dried naturally under ventilation at 25°C, and then cut into small pieces of 3cm x 3cm.

[0008] Preferably, the microorganism used in step two is Bacillus subtilis, the microbial culture medium contains 1% glucose and 0.5% peptone, the culture temperature is 30°C, and the culture time is 48 hours, so as to obtain a highly active bacterial solution; The active enzyme is papain, and the enzyme solution has an activity of 100,000 U / ml. Before use, it is sterile filtered through a 0.22 μm filter membrane.

[0009] Preferably, the hydrolysis reaction in step three is carried out under a constant temperature of 55°C. The reaction vessel is equipped with an automatic stirring device with a stirring speed set to 50 rpm. The stirring is performed once every 4 hours to ensure that the sheepskin is in full contact with water, enzymes and microorganisms and reacts evenly. The reaction time is 24 hours.

[0010] Preferably, the pH value during the hydrolysis process is controlled between 6.5 and 7.5 by timed monitoring. When the pH value deviates from this range, it is adjusted by adding 0.1M sodium hydroxide solution dropwise.

[0011] Preferably, the preliminary filtration in step four is carried out by a centrifuge, with a centrifugation speed of 3000 rpm and a centrifugation time of 10 minutes; The filtered liquid is further purified by a multi-stage filter, consisting of 100μm, 50μm and 10μm filters, with filtration times of 20 minutes, 30 minutes and 40 minutes for each stage, respectively.

[0012] Preferably, the vacuum concentration process in step five is carried out in a vacuum evaporator at a vacuum level of -0.08 MPa, with the temperature controlled at no more than 50°C, and the concentration time is 4 hours, ultimately concentrating the amino acid liquid to a content of 40%. During the concentration process, the viscosity and fluidity of the liquid are controlled.

[0013] Preferably, the proportions of urea ammonium nitrate solution, magnesium sulfate, ferrous sulfate, seaweed concentrate, nitrification inhibitor, and excipients in step six are as follows: 40% amino acid liquid, 40% urea ammonium nitrate solution, 5% magnesium sulfate, 5% ferrous sulfate, 5% seaweed concentrate, 2% nitrification inhibitor, and 3% excipients, wherein the excipients include dispersants and surfactants.

[0014] Preferably, the emulsification process in step seven is carried out by stirring at 1500 rpm for 30 minutes to form a stable emulsion. The emulsified liquid is processed through a two-stage homogenizer. The homogenization pressure in the first stage is set at 20 MPa, and the homogenization pressure in the second stage is 10 MPa. The homogenization time for each stage is 15 minutes.

[0015] Preferably, the final filtration in step eight is performed using a 5μm terminal filter, and the filtered liquid is filled into plastic or glass bottles in a dust-free and sterile environment using an automatic filling device, and then sealed immediately after filling.

[0016] This invention provides a process for preparing a highly efficient, low-temperature growth-promoting tetranitrogen liquid fertilizer. It has the following beneficial effects: 1. This invention utilizes low-temperature hydrolysis technology combined with microorganisms and active enzymes to efficiently decompose proteins in sheepskin while preserving the activity of amino acids, generating a high-concentration amino acid liquid. Multi-stage filtration further purifies the amino acid liquid, ensuring its high purity and high activity.

[0017] 2. This invention scientifically combines high-concentration amino acid liquid with urea ammonium nitrate, magnesium sulfate, ferrous sulfate, seaweed concentrate, and nitrification inhibitors to provide comprehensive nutritional support for crops. This combination effectively enhances crop growth rate, stress resistance, and yield.

[0018] 3. Each step of this invention is precisely controlled, ensuring the stability and repeatability of the process and reducing variability in production. Simultaneously, the addition of nitrification inhibitors reduces nitrogen loss and lowers the risk of environmental pollution, achieving efficient and environmentally friendly agricultural production. Attached Figure Description

[0019] Figure 1 This is a flowchart of the present invention. Detailed Implementation

[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] Example: This invention provides a process for preparing a high-efficiency, low-temperature growth-promoting tetranitrogen liquid fertilizer, comprising the following steps: 1. Raw material selection and pretreatment Step 1.1: Selection of raw materials In this embodiment, fresh, disease-free sheepskin with high protein content was selected as the organic nitrogen source. The selection criteria for sheepskin were: protein content ≥85% and moisture content ≤10%. The quality of sheepskin directly affects the subsequent amino acid production efficiency and fertilizer effectiveness; therefore, it is very important to select sheepskin with good elasticity, no cracks, and no signs of decay.

[0022] Procurement and storage: Sheepskins must be transported under refrigeration within 24 hours of slaughter, maintaining a temperature between 0-4℃ to prevent microbial growth that could lead to spoilage.

[0023] Quality Inspection: Each batch of sheepskins must be inspected upon arrival to ensure it meets quality standards. For the determination of protein content and moisture, the Kjeldahl nitrogen determination method and the drying method can be used for rapid testing.

[0024] Pollution control: Sheepskin should be kept away from potential sources of contamination, especially pathogenic microorganisms and chemicals, to avoid affecting the subsequent biological hydrolysis process.

[0025] Step 1.2: Cleaning and Cutting the Sheepskin In this embodiment, the sheepskin was cleaned using a 0.5% neutral detergent solution for approximately 15 minutes at a water temperature maintained at 25°C. After washing, the sheepskin should be air-dried in a well-ventilated environment as quickly as possible to prevent damage to its protein structure from high temperatures. Subsequently, the sheepskin was cut into 3cm x 3cm pieces to increase its surface area and optimize subsequent hydrolysis efficiency.

[0026] Cleaning equipment: Use a rotary drum cleaning machine with the drum speed set at 10 rpm to avoid mechanical damage to the sheepskin structure. The detergent solution should be changed after each wash to ensure the cleanliness of the sheepskin.

[0027] Cutting equipment: An automatic cutting machine is used, with high-carbon steel blades to ensure sharp cuts and minimize damage to the sheepskin tissue. After cutting, the sheepskin should be quickly transferred to a refrigerated environment, maintaining a temperature below 4°C to prevent microbial growth.

[0028] The selection and pretreatment of raw materials directly determine the efficiency of subsequent hydrolysis processes and the amino acid extraction rate. Strict control of parameters at each step ensures the quality of the sheepskin, laying the foundation for the successful implementation of the entire process.

[0029] 2. Preparation of Microorganisms and Active Enzymes Step 2.1: Microbial culture In this embodiment, Bacillus subtilis was selected as the hydrolytic microorganism. The strain was inoculated into a culture medium containing 1% glucose and 0.5% peptone, and the culture temperature was set at 30°C, the pH value was controlled between 7.0 and 7.5, and the culture time was 48 hours. To avoid contamination by other microorganisms, the entire culture process had to be carried out in a sterile environment.

[0030] Culture medium preparation: The culture medium must be prepared strictly according to the formula. The glucose and peptone used must be of high purity and autoclaved (121°C, 15 minutes). The sterilized culture medium must be cooled to room temperature before inoculation.

[0031] Inoculation: The inoculation volume is 1% of the culture medium volume, using aseptic techniques to avoid introducing external contaminants. After inoculation, the culture flask is shaken at 150 rpm on a shaker to ensure sufficient bacterial growth.

[0032] Bacterial culture collection: After cultivation, the bacterial culture should be stored at 4°C for a short period of time, or used immediately for subsequent hydrolysis processes.

[0033] Step 2.2: Preparation of active enzymes In this embodiment, papain is used as the main active enzyme with an activity of 100,000 U / ml. The enzyme solution needs to be filtered through a 0.22 μm filter membrane before use to remove any possible microorganisms and impurities, ensuring the purity and activity of the enzyme solution.

[0034] Enzyme solution preparation: Dilute the enzyme solution according to the reaction volume to ensure that the final concentration of the enzyme solution added to the reaction is within the appropriate range required for enzyme activity.

[0035] Filtration and Storage: The filtered enzyme solution should be stored at 4°C, protected from light, to avoid prolonged exposure to air, which can reduce enzyme activity. Prepare the solution immediately before use to ensure optimal activity.

[0036] Logical Relationship: Microorganisms and active enzymes are the core driving factors of the hydrolysis reaction. The accuracy and aseptic nature of the preparation work determine the hydrolysis efficiency and product purity. Ensuring the activity of microorganisms and enzymes provides a strong guarantee for subsequent protein hydrolysis.

[0037] 3. The hydrolysis process of sheepskin Step 3.1: Setting the hydrolysis reaction conditions In this embodiment, the cut sheepskin pieces are placed in a stainless steel reaction vessel, and purified water is added at three times their weight (e.g., 100 kg of sheepskin corresponds to 300 kg of water). Then, cultured Bacillus subtilis bacterial solution (5% of the total reaction volume) and papain enzyme solution (3% of the total reaction volume) are added. The temperature inside the reaction vessel is set to 55°C, and the automatic stirring device operates at 50 rpm, stirring every 4 hours to ensure sufficient contact and reaction of the sheepskin, enzymes, and microorganisms. The hydrolysis time is set to 24 hours.

[0038] Reactor configuration: The reaction vessel is equipped with a temperature control device and a pH monitoring system to ensure real-time control of temperature and pH values. The stirrer is made of stainless steel to prevent corrosion and contamination.

[0039] pH adjustment: The pH value of the reaction solution is monitored in real time through an online pH monitoring system and controlled between 6.5 and 7.5. When the pH value deviates from the range, 0.1M sodium hydroxide solution is automatically added through a titration device for adjustment.

[0040] Hydrolysis completion detection: When hydrolysis is about to end, samples are taken to test the amino acid content using the Kjeldahl method to ensure that the protein is fully hydrolyzed, with the goal of achieving an amino acid concentration of more than 10%.

[0041] Step 3.2: Preliminary filtration of hydrolysis products In this embodiment, after hydrolysis, the reaction solution is initially filtered using a centrifuge to remove incompletely decomposed solid residues. The centrifugation speed is set to 3000 rpm, and the centrifugation time is 10 minutes. The supernatant after centrifugation is the initially extracted amino acid liquid, which is transferred to a clean container for later use.

[0042] Centrifugation equipment: A continuous centrifuge is used, with appropriate speed and time settings to achieve effective solid-liquid separation. The supernatant should be promptly transferred to a refrigerated environment for storage to avoid prolonged exposure at room temperature, which could lead to amino acid degradation.

[0043] Filter residue treatment: The solid residue generated after centrifugation should be collected and properly disposed of to prevent environmental pollution. The residue can be further processed as organic waste or used in the production of other agricultural products.

[0044] The hydrolysis process ensures efficient protein conversion through precise control of reaction conditions, while preliminary filtration removes insoluble impurities, providing a good foundation for subsequent fine filtration and concentration.

[0045] 4. Purification and concentration of amino acid liquids Step 4.1: Multi-stage Filtering In this embodiment, the supernatant after centrifugation is purified by passing it through a multi-stage filtration system. The first stage uses a 100μm filter, the second stage uses a 50μm filter, and the third stage uses a 10μm filter. The filtration time for each stage is controlled at 20 minutes, 30 minutes, and 40 minutes, respectively, to ensure the purity of the liquid. Thorough removal of impurities and impurities.

[0046] Filter configuration: The filter is made of food-grade stainless steel to ensure no contaminants are introduced during the filtration process. Multi-stage filtration aims to progressively remove impurities of different particle sizes, resulting in a high-purity final amino acid liquid.

[0047] Filtrate treatment: The particle content and purity of the liquid after each stage of filtration should be tested promptly to ensure that the filtration effect at each step meets expectations. The filtered liquid should be transferred to a clean stainless steel storage tank for later use.

[0048] Step 4.2: Vacuum Concentration In this embodiment, the amino acid liquid, after multi-stage filtration, is concentrated using a vacuum evaporator. The vacuum level is set to -0.08 MPa, the temperature is controlled below 50°C, and the concentration time is 4 hours. Vacuum evaporation removes water from the liquid, concentrating the amino acid liquid to a content of 40%.

[0049] Concentration equipment: The vacuum evaporator's heating system uses jacketed steam heating, ensuring precise temperature control and preventing amino acid degradation due to high temperatures. The evaporator is equipped with a condensation recovery system to reduce moisture loss through evaporation.

[0050] Concentration monitoring: During the concentration process, the viscosity and solid content of the liquid need to be monitored in real time. The concentration of the liquid is detected by an online refractometer and a densitometer to ensure that the quality of the final product meets the requirements.

[0051] Through multi-stage filtration and vacuum concentration, liquid amino acids are finely purified and concentrated to ensure their high activity and high purity, providing high-quality raw materials for subsequent formulation mixing.

[0052] 5. Fertilizer formulation optimization and mixing Step 5.1: Proportioning and Mixing of Ingredients In this embodiment, the fertilizer was mixed according to the following formula ratio: 40% concentrated amino acid liquid, 40% urea ammonium nitrate solution, 5% magnesium sulfate, 5% ferrous sulfate, 5% seaweed concentrate, 2% nitrification inhibitor, and 3% excipients (diffuser and surfactant). The mixing process was carried out in a mixer at a speed of 500 rpm for 30 minutes.

[0053] Mixing equipment: A mixing tank with a temperature control system is used to maintain the temperature between 20-25℃ during the mixing process to prevent the decomposition or loss of nutrients due to high temperature.

[0054] Ingredient addition order: First add urea ammonium nitrate solution, then add magnesium sulfate, ferrous sulfate, and seaweed concentrate in sequence. Finally, add concentrated amino acid liquid, nitration inhibitor, and excipients to ensure uniform distribution of each ingredient.

[0055] Step 5.2: Emulsification treatment In this embodiment, the mixed liquid is emulsified using a high-speed stirrer. The stirrer speed is set to 1500 rpm, and the emulsification time is set to 30 minutes to ensure that the components form a stable emulsion in the liquid.

[0056] Emulsification parameter control: During the emulsification process, maintain the viscosity of the liquid within an appropriate range (200-300 cps) to ensure emulsification effect and liquid stability.

[0057] Post-emulsification treatment: The emulsified liquid should be homogenized immediately to prevent the components from separating or settling.

[0058] Step 5.3: Homogenization In this embodiment, the emulsified liquid is processed by a homogenizer to ensure that the particles in the liquid are refined to the nanometer level. The homogenization pressure in the first stage is set to 20 MPa, the homogenization pressure in the second stage is 10 MPa, and the homogenization time for each stage is 15 minutes.

[0059] Homogenization equipment selection: High-pressure homogenizers are selected to achieve uniform dispersion of nano-sized particles, ensuring the stability and absorbability of the liquid.

[0060] Homogenization effect test: The particle size distribution of the homogenized liquid should be tested to ensure that all particles are smaller than 200 nm, and the uniformity of the liquid should be determined by transmittance test.

[0061] Through scientific component ratio and homogenization treatment, the various components in the fertilizer are ensured to play their full role, improving the uniformity of fertilizer nutrition and crop absorption efficiency, ultimately achieving a highly efficient growth-promoting effect.

[0062] 6. Final filtration and filling of the product Step 6.1: Final Filtering In this embodiment, the emulsified and homogenized liquid is finally filtered through a 5μm terminal filter to remove any possible tiny particles, ensuring the purity of the liquid fertilizer and maintaining a sterile state.

[0063] Filtration equipment configuration: The terminal filter is made of high-pressure resistant stainless steel and is equipped with an automatic backwashing function to ensure a continuous and stable filtration process without the need for frequent filter replacement.

[0064] Aseptic processing: The filtered liquid should immediately proceed to the aseptic filling process to prevent external contamination. The filling equipment should be equipped with a sterile air filtration system to ensure the cleanliness of the entire filling environment.

[0065] Step 6.2: Filling and Sealing In this embodiment, the final filtered liquid fertilizer is filled into plastic or glass bottles using an automated filling machine. The filling volume is precisely controlled according to the container size, and the bottles are sealed immediately after filling to prevent air from entering.

[0066] Filling equipment selection: A fully automated filling production line equipped with an online weight detection system is used to ensure accurate filling volume for each bottle. The filling process should be carried out in a sterile environment with the temperature controlled between 20-25℃ to prevent bubbles or oxidation of the liquid due to temperature fluctuations.

[0067] Sealing process: Vacuum sealing technology is used to ensure that there is no residual air inside the bottle, extending the product's shelf life. Sealed products should be stored in a low-temperature environment.

[0068] Aseptic filtration and precise filling ensure high product purity and long-term stability. Sealing prevents outside air from entering, preventing oxidation and deterioration, and providing the market with high-quality, reliable products.

[0069] 7. Product performance and application effects Step 7.1: Field Trial and Effect Verification In this embodiment, after production is completed, the tetranitrogen liquid fertilizer of the present invention is applied to field trials on different crops.

[0070] The experiment employed a randomized block design, applying the fertilizer of this invention and a conventional fertilizer under the same environmental conditions, and monitoring key indicators such as crop growth rate, leaf color, disease resistance, and yield.

[0071] Experimental Design: The test subjects were a common crop (e.g., corn, wheat, tomato, etc.). The experiment included five different concentration groups (0%, 25%, 50%, 75%, and 100%). Each group has three replicates to ensure data reliability.

[0072] Each experimental plot should be the same size, planted with the same variety of crops, and the soil should be nutrient balanced before fertilization.

[0073] Data collection and analysis: Every 7 days, the growth height, chlorophyll content, and incidence of pests and diseases of the crops were measured, and the yield and quality differences of each group were statistically analyzed after harvest. The experimental data were analyzed for variance using statistical software to verify the significant effect of the fertilizer of this invention.

[0074] The following is a table comparing the specific experimental data: Table 1. Data from the Control Experimental Group in Example 1 Data Analysis: Growth height: As the fertilizer concentration increased, the crop growth height gradually increased. At 100% concentration, the crop growth height reached 80cm, which was 60% higher than the control group's 50cm.

[0075] Chlorophyll content: The chlorophyll content (SPAD value) also increased with increasing fertilizer concentration. The highest concentration group (100%) had a SPAD value of 45, which was significantly higher than the control group's 25, indicating enhanced photosynthetic capacity of the crop.

[0076] Yield: Crop yield increased significantly with increasing fertilizer concentration. At a 100% concentration, the yield reached 450 kg / mu, which was 50% higher than the control group.

[0077] Pest and disease incidence: The incidence of pests and diseases was significantly lower in the higher fertilizer concentration groups. The incidence of pests and diseases in the 100% concentration group was only 5%, while that in the control group was 15%.

[0078] Leaf color: The leaf color gradually changed from light green in the control group to dark green, indicating that the crop's nutritional status and health condition improved significantly with the increase of fertilizer concentration.

[0079] Effect verification: The experimental results show that the average growth rate of crops treated with the fertilizer of this invention increased by 20%, the leaves became darker green, the yield increased by 15%, and the disease resistance was significantly enhanced, showing better stress resistance and adaptability.

[0080] Field trials and efficacy verification, through scientific comparison and data analysis, have demonstrated the technical advantages and economic benefits of this invention, providing a strong basis for product promotion and application.

[0081] Example 2: In Example 2, to verify the effect of the amount of active enzyme on the preparation effect of tetrazolium liquid fertilizer, the amount of active enzyme (papain) used was reduced from 3% (percentage of total reaction volume) in Example 1 to 1.5%. All other steps and conditions remained the same as in Example 1, specifically including the following steps: 1. Raw material selection and pretreatment Step 1.1: Selection of raw materials In this embodiment, the same fresh sheepskin as in Example 1 is selected as the organic nitrogen source to ensure that the protein content is ≥85% and the moisture content is ≤10%.

[0082] Step 1.2: Cleaning and cutting of sheepskin In this embodiment, the cleaning and cutting steps of sheepskin are the same as in Example 1. Sheepskin is cleaned with 0.5% neutral detergent solution and cut into small pieces of 3cm x 3cm.

[0083] 2. Preparation of Microorganisms and Active Enzymes Step 2.1: Microbial culture In this example, the same Bacillus subtilis as in Example 1 is used, and the culture conditions and operating methods are kept consistent.

[0084] Step 2.2: Preparation of Active Enzyme In this example, the amount of papain used was reduced to 1.5% of the total volume of the reaction solution to observe the effect of reducing the enzyme dosage on hydrolysis efficiency and fertilizer performance. Other operating steps (such as filtration and storage) remained consistent with Example 1.

[0085] 3. The hydrolysis process of sheepskin Step 3.1: Setting the hydrolysis reaction conditions In this embodiment, except that the amount of papain is reduced to 1.5%, the other hydrolysis conditions (such as temperature 55℃, pH value controlled at 6.5-7.5, stirring speed 50 rpm, hydrolysis time 24 hours, etc.) are completely consistent with those in Example 1.

[0086] Step 3.2: Preliminary filtration of hydrolysis products. In this embodiment, the preliminary filtration of hydrolysis products is the same as in Example 1, using a centrifuge at 3000 rpm for solid-liquid separation.

[0087] 4. Purification and concentration of amino acid liquids Step 4.1: Multi-stage filtration In this embodiment, the operation steps and equipment configuration of multi-stage filtration are the same as in Embodiment 1, ensuring that the pure amino acid liquid is effectively purified.

[0088] Step 4.2: Vacuum Concentration In this embodiment, the vacuum concentration step is consistent with that in Example 1 to ensure that the amino acid liquid is concentrated to a content of 40%.

[0089] 5. Fertilizer formulation optimization and mixing Step 5.1: Component Proportioning and Mixing In this embodiment, the formulation ratio and mixing process are consistent with those in Example 1. 40% concentrated amino acid liquid and 40% urea ammonium nitrate solution are used, and magnesium sulfate, ferrous sulfate, seaweed concentrate, nitrification inhibitor and excipients are added in the prescribed proportion.

[0090] Step 5.2: Emulsification treatment In this embodiment, the emulsification treatment process is the same as in Example 1, with a stirring speed of 1500 rpm and an emulsification time of 30 minutes.

[0091] Step 5.3: Homogenization In this embodiment, the homogenization process is the same as in Example 1, and is carried out in two stages to ensure that the liquid particles are refined to the nanoscale.

[0092] 6. Final filtration and filling of the product Step 6.1: Final filtration In this embodiment, the final filtration process is the same as in Embodiment 1 to ensure the purity and sterility of the liquid fertilizer.

[0093] Step 6.2: Filling and Sealing In this embodiment, the filling and sealing steps are consistent with those in Embodiment 1 to ensure product quality and shelf life.

[0094] 7. Experimental Design and Effect Comparison Experimental Design: Similar to Example 1, a field trial was conducted on crops using five fertilizer concentration groups (0%, 25%, 50%, 75%, and 100%). All operational procedures and data collection methods were consistent with Example 1, and the specific data are shown in Table 2. Table 2 Comparison of Experimental Data in Example 2 Data Analysis: Growth height: The crop growth height in Example 2 was slightly lower than that in Example 1. In particular, in the high concentration group (100%), the growth height was about 7 cm lower than that in Example 1.

[0095] Chlorophyll content: The chlorophyll content (SPAD value) in Example 2 was also slightly lower than that in Example 1, indicating that reducing the amount of active enzyme may have a weakening effect on promoting photosynthesis.

[0096] Yield: The overall crop yield of Example 2 was lower than that of Example 1. In the 100% concentration group, the yield was 420 kg / mu, which was 30 kg / mu lower than that of Example 1.

[0097] Pest and disease incidence: The incidence of pests and diseases in Example 2 was slightly higher than that in Example 1, especially in the low concentration group, where the control effect of pests and diseases was not as good as that in Example 1.

[0098] Leaf color: The leaf color in Example 2 was not as good as in Example 1, and the dark green color with increased concentration was not as good as the leaves in Example 1.

[0099] Conclusion: By reducing the amount of active enzyme (Example 2), the crop's growth height, chlorophyll content, yield, and disease resistance were all inferior to those in Example 1. The experimental results show that reducing the amount of active enzyme has a significant impact on fertilizer effectiveness. The scheme using 3% active enzyme in Example 1 was significantly better than that in Example 2. Therefore, Example 1 is the optimal implementation scheme, providing the best crop growth effect and yield gain.

[0100] Example 3: In Example 3, to verify the effect of hydrolysis temperature on the preparation effect of tetranitrogen liquid fertilizer, the hydrolysis temperature was reduced from 55°C in Example 1 to 45°C. All other steps and conditions remained the same as in Example 1, specifically including the following steps: 1. Raw material selection and pretreatment Step 1.1: Selection of raw materials In this embodiment, the same fresh sheepskin as in Example 1 is selected as the organic nitrogen source to ensure that the protein content is ≥85% and the moisture content is ≤10%.

[0101] Step 1.2: Cleaning and cutting of sheepskin In this embodiment, the cleaning and cutting steps of sheepskin are the same as in Example 1. Sheepskin is cleaned with 0.5% neutral detergent solution and cut into small pieces of 3cm x 3cm.

[0102] 2. Preparation of Microorganisms and Active Enzymes Step 2.1: Microbial culture In this example, the same Bacillus subtilis as in Example 1 is used, and the culture conditions and operating methods are kept consistent.

[0103] Step 2.2: Preparation of active enzyme. In this example, the amount of papain used is the same as in Example 1, maintaining 3% (accounting for 3% of the total volume of the reaction solution). The filtration and storage steps of the enzyme solution are also consistent with those in Example 1.

[0104] 3. The hydrolysis process of sheepskin Step 3.1: Setting the hydrolysis reaction conditions. In this embodiment, the hydrolysis temperature is set at 45°C, and other conditions such as pH value (6.5-7.5), stirring speed (50 rpm), and hydrolysis time (24 hours) are consistent with those in Example 1. Due to the lower temperature, the reaction may require a longer time to achieve the same hydrolysis effect, therefore, the hydrolysis process needs to be closely monitored.

[0105] Reactor configuration: A reaction vessel equipped with a precise temperature control system is used to maintain the temperature at 45℃±1℃. The stirrer is made of stainless steel to ensure no contamination during the stirring process.

[0106] Reaction monitoring: Due to the low temperature, the hydrolysis reaction may proceed slowly, and the reaction time needs to be extended to 28 hours to ensure that the protein is fully broken down into amino acids.

[0107] Step 3.2: Preliminary filtration of hydrolysis products. In this embodiment, after hydrolysis, the reaction solution is further preliminarily filtered using a centrifuge to remove incompletely decomposed solid residues. The centrifugation speed and time are the same as in Example 1.

[0108] 4. Purification and concentration of amino acid liquids Step 4.1: Multi-stage filtration In this embodiment, the operation steps and equipment configuration of multi-stage filtration are consistent with those in Embodiment 1 to ensure that the pure amino acid liquid is effectively purified.

[0109] Step 4.2: Vacuum Concentration In this embodiment, the vacuum concentration step is consistent with that in Example 1 to ensure that the amino acid liquid is concentrated to a content of 40%.

[0110] 5. Fertilizer formulation optimization and mixing Step 5.1: Component Proportioning and Mixing In this embodiment, the formulation ratio and mixing process are consistent with those in Example 1. 40% concentrated amino acid liquid and 40% urea ammonium nitrate solution are used, and magnesium sulfate, ferrous sulfate, seaweed concentrate, nitrification inhibitor and excipients are added in the prescribed proportion.

[0111] Step 5.2: Emulsification treatment In this embodiment, the emulsification treatment process is the same as in Example 1, with a stirring speed of 1500 rpm and an emulsification time of 30 minutes.

[0112] Step 5.3: Homogenization In this embodiment, the homogenization process is the same as in Example 1, and is carried out in two stages to ensure that the liquid particles are refined to the nanoscale.

[0113] 6. Final filtration and filling of the product Step 6.1: Final filtration In this embodiment, the final filtration process is the same as in Embodiment 1 to ensure the purity and sterility of the liquid fertilizer.

[0114] Step 6.2: Filling and Sealing In this embodiment, the filling and sealing steps are consistent with those in Embodiment 1 to ensure product quality and shelf life.

[0115] 7. Experimental Design and Effect Comparison Experimental Design: Similar to Example 1, field trials were conducted on crops using five fertilizer concentration groups (0%, 25%, 50%, 75%, and 100%). All operational procedures and data collection methods were consistent with Example 1, as shown in Table 3 below: Table 3 Experimental Data Table for Example 2 Data Analysis: Growth height: The crop growth height in Example 3 was lower than that in Example 1. In particular, in the 100% concentration group, the growth height was about 8 cm lower than that in Example 1.

[0116] Chlorophyll content: The chlorophyll content (SPAD value) in Example 3 was also lower than that in Example 1, indicating that lowering the hydrolysis temperature may have reduced the amount of amino acid produced, thus affecting the photosynthetic efficiency of the crop.

[0117] Yield: The crop yield in Example 3 was also slightly lower than that in Example 1. In the 100% concentration group, the yield was 415 kg / acre, which was 35 kg / acre lower than that in Example 1.

[0118] Pest and disease incidence: The incidence of pests and diseases in Example 3 was slightly higher than that in Example 1, indicating that a lower hydrolysis temperature may lead to a reduction in the active ingredients in the fertilizer, thereby affecting the crop's disease resistance.

[0119] Leaf color: The leaf color in Example 3 was not as good as in Example 1, indicating that the growth-promoting effect of the fertilizer was weakened at lower temperatures due to hydrolysis.

[0120] Conclusion: By lowering the hydrolysis temperature (Example 3), the crop's growth height, chlorophyll content, yield, and disease resistance were all inferior to those in Example 1. The experimental results show that lowering the hydrolysis temperature has a significant impact on fertilizer effectiveness. The scheme using a hydrolysis temperature of 55℃ in Example 1 is significantly better than that in Example 3. Therefore, Example 1 is the optimal implementation scheme, providing the best crop growth effect and yield gain.

[0121] Table 4: Comparison of Experimental Data from Examples Analysis and Conclusion: Growth height: Example 1 showed the highest growth height, reaching 80cm, indicating that the combination of 3% enzyme dosage and 55℃ hydrolysis temperature yielded the best results. Examples 2 and 3 showed lower growth heights, at 73cm and 72cm respectively.

[0122] Chlorophyll content: Example 1 showed the highest chlorophyll content (SPAD value), reaching 45, indicating that the crop had a stronger photosynthetic capacity under optimal conditions. Example 2 and Example 3 had SPAD values ​​of 38 and 37, respectively.

[0123] Yield: Example 1 showed the highest yield of 450 kg / mu, indicating that its fertilizer had the best effect on promoting crop yield. The yields of Example 2 and Example 3 were 420 kg / mu and 415 kg / mu, respectively.

[0124] Pest and disease incidence: Example 1 showed the lowest pest and disease incidence, at only 5%, indicating that fertilizer under optimal conditions helps improve crop disease resistance. Example 2 and Example 3 showed pest and disease incidence rates of 8% and 7%, respectively.

[0125] Leaf color: The leaves of all three examples were dark green, but the leaf color of Example 1 was the most intense, indicating that its nutrient supply effect was the best.

[0126] Comparing the results of the three embodiments, it can be seen that Embodiment 1 exhibits the best crop growth effect and yield gain under the combination of enzyme dosage and hydrolysis temperature. Embodiments 2 and 3, while still effectively promoting crop growth by reducing enzyme dosage and lowering hydrolysis temperature, are significantly less effective than Embodiment 1. Therefore, Embodiment 1 is determined to be the most preferred embodiment.

[0127] Comparative Example 1: This comparative experiment used conventional inorganic nitrogen fertilizer (urea) for crop planting comparison, with other conditions remaining consistent with Example 1. The superiority of the technical solution of this application in terms of crop growth, yield, and disease resistance is demonstrated through experimental data tables, specifically including the following steps: Traditional comparison steps Step 1: Raw material selection and processing Using traditional urea fertilizer: In the traditional comparison, commercially available urea is selected as the nitrogen fertilizer source. Urea has a nitrogen content of 46%, making it one of the traditional nitrogen fertilizers for crops. Urea is applied directly to the field without the need for hydrolysis, filtration, or other treatment steps.

[0128] Step 2: Fertilization Fertilizer concentration settings: Based on the field experiment design, 0%, 25%, 50%, 75%, and 100% concentration groups were established (nitrogen fertilizer application rates were 0, 25, 50, 75, and 100 kg / mu, respectively).

[0129] Fertilization method: Spread urea evenly around the crop roots, ensuring full contact with the soil to promote absorption. After fertilization, water the soil to help the urea dissolve and penetrate into the soil.

[0130] Step 3: Crop Planting and Monitoring Crop planting conditions: Same crop varieties, field area and soil conditions as in Example 1.

[0131] Monitoring content: Consistent with Example 1, monitoring crop growth height, chlorophyll content, yield, and incidence of pests and diseases.

[0132] Step 4: Data Collection and Analysis Data collection: The growth height, chlorophyll content (SPAD value), and incidence of pests and diseases of crops were measured every 7 days, and the yield of each group was counted after harvest.

[0133] Analysis method: By comparing the data of the traditional comparative example and Example 1, the differences between the two in promoting crop growth and disease resistance are analyzed, demonstrating the progressiveness of the technical solution of this application.

[0134] Table 5: Comparison of Comparative Experiment Data Analysis and Conclusion Growth height: The crop growth height of Example 1 was significantly higher than that of the conventional comparative example. At 100% concentration, the growth height of Example 1 was 80 cm, while that of the conventional comparative example was 65 cm, indicating that the tetranitrogen liquid fertilizer of this application has a significant advantage in promoting crop growth.

[0135] Chlorophyll content: The chlorophyll content (SPAD value) of Example 1 is significantly higher than that of the traditional comparative example, indicating that the fertilizer of this application can better enhance the photosynthetic capacity of crops and promote healthy growth.

[0136] Yield: The crop yield of Example 1 was 450 kg / mu, which was significantly higher than the 380 kg / mu of the traditional comparative example, proving that the technical solution of this application is superior to traditional nitrogen fertilizer in terms of increasing crop yield.

[0137] Pest and disease incidence: The incidence of pests and diseases in the traditional comparative example was 15%, which was significantly higher than 5% in Example 1, indicating that the tetranitrogen liquid fertilizer of this application is more effective in improving crop disease resistance.

[0138] Leaf color: The leaves of Example 1 are dark green, while the leaves of the traditional comparative example are light green, further demonstrating the advantages of the technical solution of this application in terms of nutrient supply and healthy growth.

[0139] The comparative experimental data above lead to the conclusion that the tetranitrogen liquid fertilizer of Example 1 of this application is significantly superior to traditional inorganic nitrogen fertilizers in promoting crop growth, increasing yield, and improving disease resistance. The experimental results fully demonstrate the progressiveness and practicality of the technical solution of this application, indicating its significant application value in agricultural production.

[0140] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A preparation process of high-efficiency low-temperature growth-promoting four-nitrogen liquid fertilizer, characterized in that, The method comprises the following steps: Step 1: Select high-quality sheepskin as an organic nitrogen source, wash and cut the sheepskin; Step 2: Hydrolyze the sheepskin using microorganisms and active enzymes at 55°C for 24 hours; Step 3: Preliminarily filter the mixture after hydrolysis to remove the solid residues that are not completely decomposed; Step 4: Further purify the amino acid liquid through multi-stage filtration; Step 5: Concentrate the amino acid liquid to 40% content using vacuum evaporation technology; Step 6: Mix the concentrated amino acid liquid with urea, ammonium nitrate solution, magnesium sulfate, ferrous sulfate, seaweed concentrate, nitration inhibitor, and auxiliary materials in proportion; Step 7: Emulsify and homogenize the mixture; Step 8: Finally filter and fill.

2. The preparation process of the high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 1, the sheepskin is washed with clean water containing 0.5% neutral detergent, then naturally air-dried at 25°C, and finally cut into small pieces of 3cm x 3cm.

3. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 2, the microorganism used is Bacillus subtilis, the microorganism culture medium contains 1% glucose and 0.5% proteose peptone, the culture temperature is 30°C, and the culture time is 48 hours to obtain high-activity bacterial liquid; The active enzyme is papain, the activity of the enzyme solution reaches 100,000 U / ml, and the enzyme solution is sterilized by 0.22μm filter membrane before use.

4. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 3, the hydrolysis reaction is carried out at a constant temperature of 55°C, an automatic stirring device is arranged inside the reaction tank, the stirring speed is set to 50 rpm, and the stirring is carried out every 4 hours to ensure the sufficient contact and uniform reaction of the sheepskin with water, enzymes, and microorganisms, and the reaction time is 24 hours.

5. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, The pH value in the hydrolysis process is controlled between 6.5 and 7.5 through timed detection, and when the pH value deviates from this range, 0.1M sodium hydroxide solution is added dropwise for adjustment.

6. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 4, the preliminary filtration is carried out by a centrifugal separator, the rotation speed of the centrifugal separation is 3000 rpm, and the centrifugal time is 10 minutes; The filtered liquid is further purified by multi-stage filters, the filters are 100μm, 50μm, and 10μm filters in sequence, and the filtration time of each stage is 20 minutes, 30 minutes, and 40 minutes respectively.

7. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 5, the vacuum concentration process is carried out by a vacuum evaporator at a vacuum degree of -0.08 MPa, the temperature is controlled at not more than 50°C, the concentration time is 4 hours, the amino acid liquid is finally concentrated to 40% content, and the liquid viscosity and fluidity are controlled during the concentration process.

8. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 6, the proportions of urea, ammonium nitrate solution, magnesium sulfate, ferrous sulfate, seaweed concentrate, nitration inhibitor, and auxiliary materials are as follows: 40% amino acid liquid, 40% urea ammonium nitrate solution, 5% magnesium sulfate, 5% ferrous sulfate, 5% seaweed concentrate, 2% nitration inhibitor, and 3% auxiliary materials, the auxiliary materials include diffusing agent and surfactant.

9. The process for preparing a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, In Step 7, the emulsification is carried out at a stirring speed of 1500 rpm, the emulsification time is 30 minutes, and a stable emulsion is formed; The emulsified liquid is processed through a two-stage homogenizer. The homogenization pressure in the first stage is set at 20 MPa, and the homogenization pressure in the second stage is 10 MPa. The homogenization time for each stage is 15 minutes.

10. The process for the preparation of a high-efficiency low-temperature growth-promoting tetranitrogen liquid fertilizer according to claim 1, characterized in that, The final filtration in step eight is performed using a 5μm terminal filter. The filtered liquid is then filled into plastic or glass bottles in a dust-free and sterile environment using an automatic filling device, and sealed immediately after filling.

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