Pretreatment process for preparing liquid fertilizer by using high-purity glutamine

Abstract

The invention discloses a pretreatment process for preparing a liquid fertilizer by using high-purity glutamine, and relates to the technical field of fertilizer preparation. The specific activator combination can fully stimulate the biological activity of glutamine, citric acid adjusts the pH value of a mixed system and promotes molecular structure adjustment of glutamine, ferrous sulfate releases specific trace elements and enhances the stability of glutamine, cellulase accelerates the reaction of glutamine and decomposes impurities, and the activity of glutamine is improved. The multi-stage activation and dissolution synergism further strengthens the effect, ultrasonic-assisted activation is adopted in the first-stage activation treatment, accurate activation is carried out on a dissolution product in the previous stage, glutamine is better dissolved in a solvent under the second-stage dissolution, and the dissolution rate of glutamine is increased. The measures significantly improve the biological activity of glutamine in the prepared liquid fertilizer, thereby helping to improve the yield and quality of crops.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a pretreatment process for preparing liquid fertilizer by utilizing high-purity glutamine. Background Art

[0002] In modern agricultural production, fertilizer plays a vital role in improving crop yield and quality. With the continuous advancement of science and technology and people's increasing attention to sustainable agricultural development, the research and development of new fertilizers has become an important topic in the agricultural field. Traditional fertilizers often have some shortcomings during use. For example, the nutrient release rate of some solid fertilizers is difficult to control, which easily causes nutrient waste and environmental pollution. Although ordinary liquid fertilizers have certain advantages in terms of ease of use, there is still a lot of room for improvement in terms of stability and biological activity. Glutamine, as an important amino acid, has multiple biological functions. In the agricultural field, glutamine can promote plant growth and development, improve the stress resistance of crops, increase yield and improve quality. However, to effectively apply glutamine to the preparation of liquid fertilizers, there are a series of technical difficulties; The existing technology generally has certain defects. First, the activator combination of the existing technology is often relatively simple, and the activator combination cannot be used to stimulate the biological activity of glutamine. This leads to the difficulty in significantly improving the yield and quality of crops in agricultural production, and cannot meet the demand of modern agriculture for high-efficiency fertilizers. Secondly, the solvent composition and treatment method of the existing technology may lead to poor glutamine dissolution effect, making the liquid fertilizer often less stable. Furthermore, the screening and detection of glutamine raw materials in the existing technology may not be strict, making it difficult to ensure the quality of the raw materials and the effect of liquid fertilizers. For this reason, we propose a pretreatment process for preparing liquid fertilizers using high-purity glutamine. Summary of the invention

[0003] The object of the present invention is to provide a pretreatment process for preparing liquid fertilizer by utilizing high-purity glutamine.

[0004] In order to solve the problems raised in the above background technology, the present invention provides the following technical solution: a pretreatment process for preparing liquid fertilizer using high-purity glutamine, the pretreatment process comprising the following steps: Step 1, screening and testing high-purity glutamine raw materials, using high performance liquid chromatography to test the purity of glutamine, when the purity of glutamine does not reach 99.5%, it is purified until the concentration reaches more than 99.5%, and at the same time, the particle size of the raw material is measured using a particle size analyzer. When the particle size is not within 0.1mm-0.3mm, the raw material is screened, and glutamine particles with a particle size within the range of 0.1mm-0.3mm are retained, and particles that do not meet the requirements are removed. The water content of the raw material is determined by the drying loss method. When the water content exceeds 0.5%, the raw material is dried until the water content meets the requirements; Step 2: Weigh citric acid, ferrous sulfate and cellulase respectively, transfer the three substances into a mixing container, and stir them at a constant speed to mix them evenly to prepare an activator combination; Step 3, placing the high-purity glutamine and the activator in a stirring device for contact, and using a stirring device to stir during the contact process to make the activator and glutamine evenly mixed, and monitoring the temperature and stirring state during the mixing and contact process to ensure that the process parameters are stable; Step 4: preparing a solvent and pre-treating the solvent. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. First, the deionized water is heated, and then propylene glycol and the organic chelating agent are added in proportion. After stirring evenly, the mixed solvent is ultrasonically treated, so that the treated solvent can better dissolve glutamine and enhance the stability and efficacy of the liquid fertilizer. Step 5: dissolving the activated glutamine and the pretreated solvent in the first stage, placing the mixed system in a dissolution container, and using a stirring device to continuously stir at a speed of 100r / min-110r / min to ensure that the glutamine is uniformly dissolved in the solvent to form a preliminary solution system; Step 6: Perform the first stage of activation treatment, using ultrasonic assisted activation, an ultrasonic device with a frequency of 40kHz-50kHz and a power of 1000W, placing the solution in an ultrasonic environment, and further enhancing the biological activity of glutamine through the action of ultrasound, making the solution more stable and effective; Step seven, carry out the second stage of dissolution, adjust the temperature to 42°C-44°C, the stirring speed to 120r / min-130r / min, and the stirring time to 1.0h-1.5h, so that the glutamine activated in the first stage can be better dissolved in the solvent to form a stable liquid fertilizer base solution, laying a good foundation for subsequent processing and application.

[0005] As a further scheme of the present invention: In the step 1, for the purification treatment of glutamine, a recrystallization method is adopted, glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 55°C-60°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C-15°C to allow glutamine to crystallize and precipitate, and high-purity glutamine is obtained after filtration and drying, the screening and filtration adopts a microporous filter membrane, and the drying is carried out at a temperature of 50°C-60°C and a vacuum degree of -0.08MPa to -0.1MPa, and the drying time is 4h-5h.

[0006] As a further solution of the present invention: in the step 1, for the particle size screening of glutamine, a vibrating screening machine is used with a vibration frequency of 50 Hz-60 Hz and a mesh size of 0.1 mm and 0.3 mm, so that the retained glutamine particle size is within the range of 0.1 mm-0.3 mm.

[0007] As a further solution of the present invention: in the step 1, the drying treatment of glutamine is carried out by hot air drying at a temperature of 70°C-80°C and a wind speed of 3m / s-5m / s for 3h-4h, so that the water content of glutamine does not exceed 0.5%.

[0008] As a further solution of the present invention: in the step 2, citric acid, ferrous sulfate and cellulase are added in a ratio of 2:3:1.

[0009] As a further solution of the present invention: in the step three, the combination of glutamine and the activator needs to be stirred in a stirring device at a temperature of 40°C-50°C, the stirring speed of the stirring device is controlled at 80r / min-120r / min, and the stirring time is 2h-3h.

[0010] As a further scheme of the present invention: in the step 4, in the solvent pretreatment, the ratio of deionized water, propylene glycol and organic chelating agent is 8:1:1, the deionized water is heated to 40°C-50°C, and then propylene glycol and organic chelating agent are added, stirred evenly, and ultrasonic treatment is performed for 30min-40min, and the ultrasonic frequency is 30kHz-33kHz, which can effectively change the properties of the solvent, making it more conducive to the dissolution of glutamine and the improvement of the performance of liquid fertilizer.

[0011] As a further solution of the present invention: in the step five, during the first stage of dissolution, the temperature is controlled at 38°C-40°C, and the stirring speed is 100r / min-110r / min for 1.5h-2h.

[0012] As a further solution of the present invention: in step six, the first stage activation treatment adopts ultrasonic assisted activation, and the activation treatment is carried out at a temperature of 48°C-50°C and a time of 1.0h-1.5h.

[0013] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are: 1. The present invention uses a specific activator combination composed of citric acid, ferrous sulfate and cellulase. The biological activity of glutamine can be fully stimulated by this specific activator combination. Citric acid adjusts the pH of the mixed system to promote the adjustment of the molecular structure of glutamine. Ferrous sulfate releases specific trace elements to enhance the stability of glutamine. Cellulase accelerates the reaction of glutamine and decomposes impurities. Multi-stage activation and dissolution synergistically further enhance this effect. The first stage activation treatment adopts ultrasonic assisted activation to accurately activate the dissolution product of the previous stage. In the second stage dissolution, glutamine is better dissolved in the solvent. These measures significantly improve the biological activity of glutamine in the prepared liquid fertilizer, thereby helping to improve the yield and quality of crops. 2. The present invention uses a solvent composed of deionized water, propylene glycol and an organic chelating agent. The deionized water is first heated, and then propylene glycol and the organic chelating agent are added, stirred evenly and then ultrasonically treated. The treated solvent is treated by a specific magnetic field, which changes the molecular structure and physical properties of the solvent, is more conducive to the dissolution of glutamine, improves the dissolution speed and uniformity, and makes it less likely for the liquid fertilizer to be stratified and precipitated during storage and use, thereby ensuring the effectiveness and durability of the fertilizer, ensuring the stable quality of each batch of liquid fertilizer, providing users with reliable agricultural production inputs, and reducing agricultural production costs and risks; 3. The present invention screens and detects high-purity glutamine raw materials, strictly controls the purity, particle size and water content thereof, thereby ensuring the high quality of the raw materials. The glutamine is dissolved in a mixed solvent of ethanol and water by a recrystallization method. When the purity of the glutamine does not reach the required purity, a purification treatment is performed. When the particle size and water content do not meet the requirements, screening and drying treatment are performed, so that the raw materials meet specific standards, thereby providing a reliable basis for preparing high-quality liquid fertilizers and ensuring that they can exert good effects during use. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 A schematic diagram of the method steps in an embodiment of the present invention; Figure 2 It is a schematic diagram for comparing embodiments in the embodiments of the present invention. DETAILED DESCRIPTION

[0015] The specific embodiments of the present invention will be further described below in conjunction with the accompanying drawings. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention.

[0016] In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0017] Please see attached Figure 1 -Attached Figure 2 The present invention discloses a pretreatment process for preparing liquid fertilizer using high-purity glutamine, and the pretreatment process comprises the following steps: Step 1, screening and testing high-purity glutamine raw materials, using high performance liquid chromatography to test the purity of glutamine, when the purity of glutamine does not reach 99.5%, it is purified until the concentration reaches more than 99.5%, and at the same time, the particle size of the raw material is measured using a particle size analyzer. When the particle size is not within 0.1mm-0.3mm, the raw material is screened, and glutamine particles with a particle size within the range of 0.1mm-0.3mm are retained, and particles that do not meet the requirements are removed. The water content of the raw material is determined by the drying loss method. When the water content exceeds 0.5%, the raw material is dried until the water content meets the requirements; Step 2: Weigh citric acid, ferrous sulfate and cellulase respectively, transfer the three substances into a mixing container, and stir them at a constant speed to mix them evenly to prepare an activator combination; Step 3, placing the high-purity glutamine and the activator in a stirring device for contact, and using a stirring device to stir during the contact process to make the activator and glutamine evenly mixed, and monitoring the temperature and stirring state during the mixing and contact process to ensure that the process parameters are stable; Step 4: preparing a solvent and pre-treating the solvent. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. First, the deionized water is heated, and then propylene glycol and the organic chelating agent are added in proportion. After stirring evenly, the mixed solvent is ultrasonically treated, so that the treated solvent can better dissolve glutamine and enhance the stability and efficacy of the liquid fertilizer. Step 5: dissolving the activated glutamine and the pretreated solvent in the first stage, placing the mixed system in a dissolution container, and using a stirring device to continuously stir at a speed of 100r / min-110r / min to ensure that the glutamine is uniformly dissolved in the solvent to form a preliminary solution system; Step 6: Perform the first stage of activation treatment, using ultrasonic assisted activation, an ultrasonic device with a frequency of 40kHz-50kHz and a power of 1000W, placing the solution in an ultrasonic environment, and further enhancing the biological activity of glutamine through the action of ultrasound, making the solution more stable and effective; Step seven, carry out the second stage of dissolution, adjust the temperature to 42°C-44°C, the stirring speed to 120r / min-130r / min, and the stirring time to 1.0h-1.5h, so that the glutamine activated in the first stage can be better dissolved in the solvent to form a stable liquid fertilizer base solution, laying a good foundation for subsequent processing and application.

[0018] In one embodiment of the present invention: In step 1, for the purification of glutamine, a recrystallization method is used, glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 55°C-60°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C-15°C to allow glutamine to crystallize, and high-purity glutamine is obtained after filtration and drying, and the screening and filtration are performed using a microporous filter membrane, and the drying is performed at a temperature of 50°C-60°C and a vacuum degree of -0.08MPa to -0.1MPa, and the drying time is 4h-5h.

[0019] In one embodiment of the present invention: in step 1, for the particle size screening of glutamine, a vibrating screening machine is used with a vibration frequency of 50 Hz-60 Hz and a mesh size of 0.1 mm and 0.3 mm, so that the retained glutamine particle size is in the range of 0.1 mm-0.3 mm.

[0020] In one embodiment of the present invention: in step 1, the drying treatment of glutamine is carried out by hot air drying at a temperature of 70°C-80°C and a wind speed of 3m / s-5m / s for 3h-4h, so that the water content of glutamine does not exceed 0.5%.

[0021] In one embodiment of the present invention: in step 2, citric acid, ferrous sulfate and cellulase are added in a ratio of 2:3:1.

[0022] In one embodiment of the present invention: in step three, the combination of glutamine and the activator needs to be stirred in a stirring device at a temperature of 40°C-50°C, the stirring speed of the stirring device is controlled at 80r / min-120r / min, and the stirring time is 2h-3h.

[0023] In one embodiment of the present invention: in step 4, in the solvent pretreatment, the ratio of deionized water, propylene glycol and organic chelating agent is 8:1:1, the deionized water is heated to 40°C-50°C, and then propylene glycol and organic chelating agent are added, stirred evenly, and ultrasonic treatment is performed for 30min-40min, and the ultrasonic frequency is 30kHz-33kHz, which can effectively change the properties of the solvent, making it more conducive to the dissolution of glutamine and the improvement of the performance of liquid fertilizer.

[0024] In one embodiment of the present invention: in step five, during the first stage of dissolution, the temperature is controlled at 38°C-40°C, and the stirring speed is 100r / min-110r / min for 1.5h-2h.

[0025] In one embodiment of the present invention: in step six, the first stage activation treatment adopts ultrasonic assisted activation, and the activation treatment is carried out at a temperature of 48° C.-50° C. and a time of 1.0 h-1.5 h.

[0026] In one embodiment of the present invention: after citric acid is mixed with ferrous sulfate and cellulase at a temperature of 40°C-50°C, the pH of the mixed system can be adjusted to 4.5-5.5. In the process of contacting with high-purity glutamine, the citric acid interacts with glutamine with a specific molecular structure. The stirring speed is 80r / min-120r / min, and the action time is 2h-3h, ensuring that the citric acid fully plays the role of promoting the adjustment of the molecular structure of glutamine; In one embodiment of the present invention, during the weighing process, the amount of ferrous sulfate needs to be accurately controlled to ensure that the ratio in the activator combination is 3. When synergistically acting with citric acid and cellulase, under the conditions of a temperature of 40°C-50°C and a treatment time of 2h-3h, the stability of glutamine is enhanced by releasing specific trace elements such as iron and sulfur. The ferrous sulfate exists mainly in an ionic state in the mixed system, and the reaction rate with other substances is 0.05mol / L-0.08mol / L per minute. In one embodiment of the present invention: the ratio of cellulase in the specific activator combination is 1, and its action process is to accelerate the reaction of glutamine and decompose possible impurities such as cellulose through a specific enzymatic reaction mechanism at a temperature of 40°C-50°C and a time of 2h-3h. The activity of cellulase is affected by environmental factors. Under this process condition, its optimal active temperature range is 45°C-50°C, and when the stirring speed is 80r / min-120r / min, it can better play its role.

[0027] Example 1, please refer to the attached Figure 1 -Attached Figure 2First, the high-purity glutamine raw materials are screened and tested. The purity of glutamine is tested by high-performance liquid chromatography. If the purity of glutamine does not reach 99.5%, it is purified by recrystallization. Glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 60°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C-15°C to allow glutamine to crystallize. After filtration and drying, high-purity glutamine is obtained. The screening and filtration are performed using a microporous filter membrane. The drying is performed at a temperature of 55°C and a vacuum degree of -0.1MPa. The drying time is 5h until the concentration reaches more than 99.5%. At the same time, the particle size of the raw material is analyzed using a particle size analyzer. Measure, if the particle size is not within 0.1mm-0.3mm, the raw material is screened, and the glutamine particles with a particle size within this range are retained, and the particles that do not meet the requirements are removed. Then, the moisture content of the raw material is determined by the drying loss method. When the moisture content exceeds 0.5%, the raw material is dried until the moisture content meets the requirements. Then, citric acid, ferrous sulfate and cellulase are weighed respectively, and the three substances are transferred to a mixing container. The glutamine and activator combination needs to be stirred in a stirring device at a temperature of 50°C. The stirring speed of the stirring device is controlled at 100r / min, and the stirring time is 3h. Stir at a uniform speed to mix them evenly to prepare an activator combination. After that, the high-purity glutamine and the activator are mixed. The activator combination is placed in a stirring device for contact. During the contact process, a stirring device is used for stirring to uniformly mix the activator and glutamine. During the mixed contact process, the temperature and stirring state are monitored to ensure that the process parameters are stable. Subsequently, a solvent is prepared and the solvent is pretreated. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. In the solvent pretreatment, the ratio of deionized water, propylene glycol and the organic chelating agent is 8:1:1. The deionized water is heated to 40°C and ultrasonically treated for 30 minutes. The ultrasonic frequency is 30kHz, which can effectively change the properties of the solvent, making it more conducive to the dissolution of glutamine and the improvement of the performance of the liquid fertilizer. After stirring evenly, the mixed solvent is ultrasonically treated to make the solvent The agent can better dissolve glutamine and enhance the stability and efficacy of liquid fertilizer. Then, the activated glutamine and the pretreated solvent are dissolved in the first stage. The mixed system is placed in a dissolution container and stirred at a speed of 100r / min by a stirring device to ensure that glutamine is evenly dissolved in the solvent to form a preliminary solution system. Then, the first stage of activation treatment is carried out. Ultrasonic equipment with a frequency of 50kHz and a power of 1000W is used to place the solution in an ultrasonic environment. The biological activity of glutamine is further enhanced by the action of ultrasound, making the solution more stable and effective. Finally, the second stage of dissolution is carried out, and the temperature is adjusted to 44℃, the stirring speed is 130r / min, and the stirring time is 1.5h, so that the glutamine after the first stage of activation treatment can be better dissolved in the solvent, forming a stable liquid fertilizer base solution, laying a good foundation for subsequent processing and application.

[0028] Example 2, please refer to the attached Figure 1 -Attached Figure 2First, the high-purity glutamine raw materials are screened and tested, and the purity of glutamine is tested by high-performance liquid chromatography. If the purity of glutamine does not reach 99.5%, it is purified by recrystallization. Glutamine is dissolved in ethanol at 65°C, and then slowly cooled to 20°C to allow glutamine to crystallize. After filtration and drying, high-purity glutamine is obtained. The screening and filtration are carried out using a microporous filter membrane. The drying is carried out at a temperature of 70°C and a vacuum degree of 0.08MPa. The drying time is 4h until the concentration reaches more than 99.5%. At the same time, the particle size of the raw material is measured using a particle size analyzer. If the particle size is not between 0.1mm-0.3mm If the water content is within the range of 0.5%, the raw materials are screened, and the glutamine particles with the particle size within the range are retained, and the particles that do not meet the requirements are removed. Then, the water content of the raw materials is determined by the drying loss method. When the water content exceeds 0.5%, the raw materials are dried until the water content reaches the requirement. Then, citric acid and ferrous sulfate are weighed separately, and the two substances are transferred to a mixing container, and stirred at a uniform speed to mix them evenly to prepare an activator combination. The glutamine and activator combination needs to be stirred in a stirring device at a temperature of 40°C. The stirring speed of the stirring device is controlled at 100r / min, and the stirring time is 2.0h. After that, the high-purity glutamine and the activator combination are placed in a stirring device for contact. During the process, a stirring device is used to stir so that the activator and glutamine are evenly mixed. The temperature and stirring state are monitored during the mixed contact process to ensure that the process parameters are stable. Subsequently, a solvent is prepared and pretreated. The solvent is composed of deionized water and propylene glycol. In the solvent pretreatment, the ratio of deionized water to propylene glycol is 9:1. The deionized water is heated to 40°C and ultrasonically treated for 30 minutes at a frequency of 30kHz. After stirring evenly, the mixed solvent is ultrasonically treated to allow the solvent to better dissolve glutamine and enhance the stability and efficacy of the liquid fertilizer. The activated glutamine and the pretreated solvent are then dissolved in the first stage, and the mixed system is placed in a dissolution container. In the device, a stirring device is used to continuously stir at a speed of 100r / min to ensure that glutamine is evenly dissolved in the solvent to form a preliminary solution system. Then the first stage of activation treatment is carried out. An ultrasonic device with a frequency of 30kHz and a power of 1000W is used to place the solution in an ultrasonic environment. The biological activity of glutamine is further enhanced through the action of ultrasound, making the solution more stable and effective. Finally, the second stage of dissolution is carried out, and the temperature is adjusted to 42°C, the stirring speed is 120r / min, and the stirring time is 1.0h, so that the glutamine that has undergone the first stage of activation treatment can be better dissolved in the solvent to form a stable liquid fertilizer basic solution, laying a good foundation for subsequent processing and application.

[0029] Example 3, please refer to the attached Figure 1 -Attached Figure 2 First, the high-purity glutamine raw materials are screened and tested, and the purity of glutamine is tested by high performance liquid chromatography. If the purity of glutamine does not reach 99.5%, it is purified by recrystallization. Glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 55°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C to allow glutamine to crystallize. After filtration and drying, high-purity glutamine is obtained. The screening and filtration are performed using a microporous filter membrane, and the drying is performed at a temperature of 50°C and a vacuum degree of -0.08MPa for 5 hours until the concentration reaches 100%. Reach more than 99.5%. At the same time, use a particle size analyzer to measure the particle size of the raw material. If the particle size is not within 0.1mm-0.3mm, the raw material is screened, and the glutamine particles with a particle size within this range are retained, and the particles that do not meet the requirements are removed. Then, the moisture content of the raw material is determined by the drying loss method. When the moisture content exceeds 0.5%, the raw material is dried until the moisture content meets the requirements. Then, citric acid, ferrous sulfate and cellulase are weighed separately, and the three substances are transferred to a mixing container. The combination of glutamine and activator needs to be stirred in a stirring device at a temperature of 50°C. The stirring speed of the stirring device is controlled at 80r / min, the stirring time is 3h, and the mixture is evenly stirred to prepare an activator combination. After that, the high-purity glutamine and the activator combination are placed in a stirring device for contact. During the contact process, the stirring device is used for stirring to make the activator and glutamine evenly mixed. The temperature and stirring state are monitored during the mixed contact process to ensure that the process parameters are stable. Subsequently, a solvent is prepared and pretreated. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. In the solvent pretreatment, the ratio of deionized water, propylene glycol and the organic chelating agent is 8:1:1. The mixture is heated. Deionized water is heated to 40°C and ultrasonically treated for 30 minutes at a frequency of 30kHz, which can effectively change the properties of the solvent, making it more conducive to the dissolution of glutamine and the improvement of the performance of the liquid fertilizer. After stirring evenly, the mixed solvent is ultrasonically treated to enable the solvent to better dissolve glutamine and enhance the stability and efficacy of the liquid fertilizer. The activated glutamine and the pretreated solvent are then dissolved in the first stage, and the mixed system is placed in a dissolution container. A stirring device is used to continuously stir at a speed of 100r / min to ensure that glutamine is evenly dissolved in the solvent to form a preliminary solution system.

[0030] Example 4, please refer to the attached Figure 1 -Attached Figure 2First, the high-purity glutamine raw materials are screened and tested. The purity of glutamine is tested by high-performance liquid chromatography. If the purity of glutamine does not reach 99.5%, it is purified by recrystallization. Glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 60°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C to allow glutamine to crystallize. After filtration and drying, high-purity glutamine is obtained. The screening and filtration are performed using a microporous filter membrane and dried at a temperature of 50°C and a vacuum degree of -0.1MPa. The drying process was carried out under the following conditions, with a drying time of 5 hours until the concentration reached more than 99.5%. At the same time, a particle size analyzer was used to measure the particle size of the raw material. If the particle size was not within the range of 0.1 mm to 0.3 mm, the raw material was screened, and the glutamine particles within the particle size range were retained, and particles that did not meet the requirements were removed. Then, the moisture content of the raw material was determined by the drying loss method. When the moisture content exceeded 0.5%, the raw material was dried until the moisture content reached the requirement. Then, acetic acid, manganese chloride and urea were weighed in a ratio of 3:2:1 and the three substances were mixed. The glutamine and activator combination needs to be stirred in a stirring device at a temperature of 50°C, the stirring speed of the stirring device is controlled at 120r / min, the stirring time is 3h, and the mixture is stirred at a uniform speed to be evenly mixed to prepare an activator combination. After that, the high-purity glutamine and the activator combination are placed in a stirring device for contact. During the contact process, a stirring device is used for stirring to mix the activator and glutamine evenly. The temperature and stirring state are monitored during the mixed contact process to ensure that the process parameters are stable. Subsequently, the activator combination is prepared. Prepare a solvent and pretreat the solvent. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. In the solvent pretreatment, the ratio of deionized water, propylene glycol and the organic chelating agent is 5:2:1. Heat the deionized water to 40°C and oscillate for 30 minutes with an oscillation frequency of 30 kHz. Then, perform the first stage dissolution of the activated glutamine and the pretreated solvent. Place the mixed system in a dissolution container and use a stirring device to continuously stir at a speed of 100 r / min to ensure that glutamine is uniformly dissolved in the solvent to form a preliminary solution system.

[0031] Experimental design: Take an equal amount of the liquid fertilizer base solution prepared in Example 1, Example 2, Example 3, and Example 4, wheat of the same variety and similar growth conditions, plant 10 trees in each pot, soil (select fertile, loose, well-drained black soil with a soil organic matter content of 2.5% and a pH value of 7.0), planting containers (each container is the same size, with a diameter of 30 cm), conventional fertilizers, etc.; Experimental steps: Prepare 4 identical planting containers and fill them with soil.

[0032] Wheat seedlings of the same variety and similar growth conditions were planted in individual planting containers, with 10 plants planted in each pot; The planting containers were randomly divided into four groups, which were marked as Group A, Group B, Group C, and Group D according to Example 1, Example 2, Example 3, and Example 4, respectively; Groups B, C, and D were further processed using the liquid fertilizer base solutions prepared in Example 1, Example 2, Example 3, and Example 4, respectively, and fertilized after being made into finished liquid fertilizers. The dosage of fertilizer was 50 ml per pot, and fertilizer was applied once a week. Wheat seedlings were cultivated under the same environmental conditions (light, temperature, humidity, etc. remained the same), and the growth of wheat was observed and recorded every 4 days, including growth rate (plant height was measured every week, unit: cm), plant height (measured at harvest, unit: cm), leaf color (assessed by colorimetric card, the value range is 1-10, the larger the value, the darker the green), fruit yield (weighed at harvest, unit: g), etc. The measurement cycle was to measure the growth rate once a week for a total of 8 weeks, and the plant height and fruit yield were measured at harvest; At the same time, the stability of the liquid fertilizer of each experimental group was tested regularly to observe whether there was any stratification or precipitation, and the glutamine content in the fertilizer was measured (unit: mg / L). The stability of the liquid fertilizer was tested once a week for a total of 8 weeks, and the glutamine content was measured at the end of the experiment; Experimental data calculation formula: Glutamine bioactivity (glutamine content) (mg / L): The glutamine content measured at the end of the experiment was recorded directly; Crop yield (fruit yield) (g / tree): total weight of fruit yield (weight of all fruits at harvest) / tree planted; Crop quality (leaf color evaluation value) (1-10): leaf color was evaluated multiple times and the average value was taken; Record the experimental data, as shown in the attached Figure 2As shown, Example 1 performs well in all aspects, and its glutamine biological activity is the highest, which shows that the preparation process of Example 1 can effectively improve the biological activity of glutamine. At the same time, the crop yield of Example 1 is higher than that of other examples, indicating that it has a significant effect on improving crop yield. In addition, the leaf color evaluation value of Example 1 is relatively high, reflecting its positive effect on improving crop quality. In terms of liquid fertilizer stability, the liquid fertilizer of Example 1 did not show stratification and precipitation during the entire experimental process, while Example 2 and Example 4 began to show stratification and precipitation from the 6th week and the 5th week respectively. Although Example 3 did not show stratification and precipitation, the overall effect was still not as good as Example 1. In summary, the table data fully proves that the preparation process of Example 1 has obvious advantages in improving glutamine biological activity, crop yield and quality, and ensuring liquid fertilizer stability, and has the best effect.

[0033] Although the present invention is disclosed as above in terms of preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art may make possible changes and modifications without departing from the spirit and scope of the present invention. Therefore, any modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention shall fall within the scope of protection defined by the claims of the present invention.

Claims

1. A pretreatment process for preparing liquid fertilizer using high-purity glutamine, characterized in that: The pretreatment process comprises the following steps: Step 1, screening and testing high-purity glutamine raw materials, using high performance liquid chromatography to test the purity of glutamine, when the purity of glutamine does not reach 99.5%, it is purified until the concentration reaches more than 99.5%, and at the same time, the particle size of the raw material is measured using a particle size analyzer. When the particle size is not within 0.1mm-0.3mm, the raw material is screened, and glutamine particles with a particle size within the range of 0.1mm-0.3mm are retained, and particles that do not meet the requirements are removed. The water content of the raw material is determined by the drying loss method. When the water content exceeds 0.5%, the raw material is dried until the water content meets the requirements; Step 2: Weigh citric acid, ferrous sulfate and cellulase respectively, transfer the three substances into a mixing container, and stir them at a constant speed to mix them evenly to prepare an activator combination; Step 3, placing the high-purity glutamine and the activator in a stirring device for contact, and using a stirring device to stir during the contact process to make the activator and glutamine evenly mixed, and monitoring the temperature and stirring state during the mixing and contact process to ensure that the process parameters are stable; Step 4: preparing a solvent and pretreating the solvent. The solvent is composed of deionized water, propylene glycol and an organic chelating agent. First, the deionized water is heated, and then propylene glycol and the organic chelating agent are added in proportion. After stirring evenly, the mixed solvent is subjected to ultrasonic treatment. Step 5: dissolving the activated glutamine and the pretreated solvent in the first stage, placing the mixed system in a dissolution container, and using a stirring device to continuously stir at a speed of 100r / min-110r / min to ensure that the glutamine is uniformly dissolved in the solvent to form a preliminary solution system; Step 6: Perform the first stage activation treatment, using ultrasonic assisted activation, an ultrasonic device with a frequency of 40kHz-50kHz and a power of 1000W, and place the solution in an ultrasonic environment; Step seven, carry out the second stage of dissolution, adjust the temperature to 42°C-44°C, the stirring speed to 120r / min-130r / min, and the stirring time to 1.0h-1.5h, so that the glutamine activated in the first stage can be better dissolved in the solvent to form a liquid fertilizer base solution.

2. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 1, for the purification of glutamine, a recrystallization method is used, glutamine is dissolved in a mixed solvent of ethanol and water at a temperature of 55°C-60°C, wherein the volume ratio of ethanol to water is 3:2, and then the temperature is slowly lowered to 10°C-15°C to allow glutamine to crystallize and precipitate, and high-purity glutamine is obtained after filtration and drying, the screening and filtration adopts a microporous filter membrane, and the drying is carried out at a temperature of 50°C-60°C and a vacuum degree of -0.08MPa to -0.1MPa, and the drying time is 4h-5h.

3. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 1, for the particle size screening of glutamine, a vibration screening machine is used with a vibration frequency of 50 Hz-60 Hz and a mesh size of 0.1 mm and 0.3 mm, so that the retained glutamine particle size is within the range of 0.1 mm-0.3 mm.

4. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 1, the glutamine is dried by hot air drying at a temperature of 70° C.-80° C. and a wind speed of 3 m / s-5 m / s for 3 h-4 h, so that the water content of the glutamine does not exceed 0.5%.

5. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 2, citric acid, ferrous sulfate and cellulase are added in a ratio of 2:3:

1.

6. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 3, the combination of glutamine and the activator needs to be stirred in a stirring device at a temperature of 40° C.-50° C., the stirring speed of the stirring device is controlled at 80 r / min-120 r / min, and the stirring time is 2 h-3 h.

7. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 4, in the solvent pretreatment, the ratio of deionized water, propylene glycol and organic chelating agent is 8:1:1, the deionized water is heated to 40°C-50°C, and then propylene glycol and organic chelating agent are added, stirred evenly, and ultrasonic treatment is performed for 30min-40min, and the ultrasonic frequency is 30kHz-33kHz, which can effectively change the properties of the solvent, making it more conducive to the dissolution of glutamine and the improvement of the performance of liquid fertilizer.

8. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In the step 5, during the first stage of dissolution, the temperature is controlled at 38° C.-40° C., and the stirring speed is 100 r / min-110 r / min for 1.5 h-2 h.

9. The pretreatment process for preparing liquid fertilizer using high-purity glutamine according to claim 1, characterized in that: In step six, the first stage activation treatment adopts ultrasonic assisted activation, and the activation treatment is carried out at a temperature of 48° C.-50° C. and a time of 1.0 h-1.5 h.

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