Method for preparing fertilizer by extracting amino acid from glycine fermentation liquor

Abstract

The invention discloses a method for preparing a fertilizer by extracting amino acid from glycine fermentation liquor, and relates to the technical field of fertilizer preparation, and the method has the advantages that impurities in the glycine fermentation liquor can be decomposed by selecting a specific biological enzyme and ionic liquid composite extraction agent, favorable conditions are created for extraction of amino acid, and the yield of the amino acid is improved. By accurately controlling the addition amount of biological enzyme, proper reaction temperature, pH value, stirring speed and other reaction conditions and determining the use ratio of an extraction agent and an accurate extraction process, the high efficiency and stability of the extraction process can be ensured, the extraction efficiency of amino acid is remarkably improved, the extraction efficiency is greatly improved, and the method is suitable for industrial production. Therefore, sufficient and high-quality amino acid raw materials are provided for subsequent preparation of high-quality fertilizer, the content of nutrients in the fertilizer is greatly increased, and the amino acid is combined with beneficial components such as humic acid, so that the prepared fertilizer has various functions, and the requirement for diversified functions of the fertilizer in agricultural production is met.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a method for preparing fertilizer by extracting amino acids from glycine fermentation broth. Background Art

[0002] Amino acids are the basic units that make up proteins and have important physiological functions in organisms. Glycine, as an important amino acid, is widely used in agriculture, medicine, food and other fields. Glycine fermentation broth is one of the main raw materials for producing glycine, which contains rich amino acid resources. However, how to efficiently extract amino acids from glycine fermentation broth and prepare it into fertilizers with high added value is an important technical challenge currently faced. The existing method of extracting amino acids from glycine fermentation broth to prepare fertilizers has certain technical defects. First, the existing technology has the problems of low extraction efficiency and low quality of amino acid raw materials, resulting in insufficient nutrient content of fertilizers and failure to meet demand. Secondly, the existing fertilizers may have short stability and storage life and single functionality, which cannot meet the diversified needs of agricultural production. Furthermore, the recycling of residual fermentation broth is insufficient, which may cause waste of resources and environmental pollution, and the energy consumption is also high. Therefore, we propose a method for extracting amino acids from glycine fermentation broth to prepare fertilizers. Summary of the invention

[0003] The object of the present invention is to provide a method for preparing fertilizer by extracting amino acids from glycine fermentation broth.

[0004] In order to solve the problems raised in the above background technology, the present invention provides the following technical solution: a method for extracting amino acids from glycine fermentation broth to prepare fertilizer, the method for preparing fertilizer comprising the following steps: Step 1: placing the glycine fermentation broth in a reaction vessel, adding a specific biological enzyme to the fermentation broth at a temperature of 30°C-35°C and a pH value of 6.0-6.5, with the addition amount being 2%-3% of the mass of the fermentation broth, the stirring speed being controlled at 70r / min-80r / min, and the continuous treatment time being 3h-4h to decompose impurities in the fermentation broth; Step 2, select an ionic liquid composite extractant as an extractant, mix it with the fermentation liquid at a mass ratio of 1:1.5-2.0, place it in an extraction device, and stir and extract it at a temperature of 45°C-50°C and a pressure of 0.4MPa-0.5MPa. The extraction process is divided into two stages: an early stage and a late stage. The early extraction time is 2.5h-3.0h. During this period, the extract is monitored in real time. When the amino acid concentration in the extract reaches 40%-50% of the initial amino acid concentration of the fermentation liquid, enter the late extraction stage. The late extraction time is 1.5h-2.0h to extract amino acids; Step 3: Preliminary filtration of the extracted amino acid solution using microporous ceramic filter material to remove residual tiny impurities, then passing the filtered solution through an ion exchange resin column to adsorb ionic impurities in the solution using the ion exchange resin, and then evaporating and concentrating the amino acid solution; Step 4: adding natural antioxidant vitamin C to the concentrated amino acids, then stirring evenly, adding beneficial ingredient humic acid, the mass ratio of which to amino acids is 1:3.5-4.0, and using a specific granulation process to granulate at a temperature of 55° C.-60° C. to prepare fertilizer; Step 5: purifying the extracted amino acids by using a multi-stage membrane separation and purification method at a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa to improve the purity of the amino acids to a purity of not less than 95%; Step 6: Recover the remaining fermentation liquid after amino acid extraction, filter the remaining fermentation liquid at a temperature of 35°C-40°C, and then concentrate it to extract the remaining nutrients for the preparation of other products, thereby realizing resource recycling and completing the preparation of fertilizer.

[0005] As a further scheme of the present invention: in the step one, the specific biological enzyme is an enzyme preparation modified by a specific gene sequence, which has high activity and stability in the range of 30°C-35°C and a pH value of 6.0-6.5. When added to the fermentation broth, it is evenly dispersed through a dripping device to make the enzyme and the fermentation broth contact evenly. During the treatment process, the stirring speed is controlled at 70r / min-80r / min to promote the reaction of the enzyme with impurities, and the reaction time is controlled at 3h-4h.

[0006] As a further solution of the present invention: in the step 2, the ionic liquid composite extractant is composed of an ionic liquid and an organic extractant in proportion. The ionic liquid has a unique cation and anion structure and has high selectivity and affinity for amino acids. The organic extractant can enhance the solubility and stability of the extractant. During the extraction process, the stirring speed is controlled at 90r / min-100r / min to ensure that the extractant and the amino acid are fully mixed.

[0007] As a further solution of the present invention: in the step three, the microporous ceramic filter material used for preliminary filtration has a pore size of 0.08 μm-0.1 μm to remove tiny impurities in the extracted amino acid solution. The filtration process is carried out at a pressure of 0.25 MPa-0.3 MPa. When the filtered solution is evaporated and concentrated, the temperature is controlled at 60°C-70°C. When the solution concentration reaches a mass fraction of 60%-70%, the evaporation and concentration is stopped to ensure that the solution concentration meets the requirements for granulation.

[0008] As a further solution of the present invention: in the step 4, when the natural antioxidant vitamin C is added, its addition amount is controlled to be 1.5%-2% of the total mass of the fertilizer. During the mixing process of the antioxidant with the concentrated amino acids and other beneficial ingredients, the antioxidant is stirred for 30 minutes by a stirring device to ensure uniform distribution. In the granulation process, under the condition of a temperature of 55°C-60°C, the antioxidant can effectively prevent the amino acids from being oxidized and decomposed, thereby improving the stability and storage life of the fertilizer.

[0009] As a further scheme of the present invention: in the step 4, humic acid is added until the mass ratio of humic acid to amino acid is 1:3.5-4.0. During the adding process, the order of adding concentrated amino acids first and then adding humic acid is adopted to ensure full integration with the amino acids. These components work together with the amino acids to provide plants with a variety of nutrients. During the granulation process, by controlling the granulation time to 1 hour, the beneficial ingredients are evenly distributed in the fertilizer particles, thereby improving the multifunctionality of the fertilizer, promoting plant growth and improving stress resistance.

[0010] As a further scheme of the present invention: in the step five, the amino acid purification treatment adopts a multi-stage membrane separation purification method and purification equipment, and impurities and impurities are removed based on the selective separation principle of the membrane. The purification equipment is a temperature and pressure control device, and the purification operation is carried out under the conditions of a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa. Through the three-stage membrane separation treatment, the purity of the amino acid is improved to a purity of not less than 95%, providing high-quality raw materials for the preparation of high-quality fertilizers.

[0011] As a further solution of the present invention: in the step six, during the recovery process of the by-products, the remaining fermentation liquid is first filtered at a temperature of 35°C-40°C, the filter medium used for filtration is activated carbon filter cotton, and the filtration accuracy is 0.04μm-0.05μm, and the filtered solution is then concentrated by evaporation concentration method at a temperature of 65°C-70°C. During the concentration process, the process parameters are strictly controlled to ensure that the content of the remaining nutrients after concentration is not less than 60%, so that it can be used to prepare other products and realize resource recycling.

[0012] As a further solution of the present invention: in the step three, the operating temperature of the ion exchange resin column is 25° C.-30° C., and the flow rate is controlled at 1.5-2 times the resin volume per hour.

[0013] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are: 1. The present invention can decompose impurities in glycine fermentation broth by selecting specific biological enzymes and ionic liquid composite extractants, creating favorable conditions for the extraction of amino acids, and can ensure the efficiency and stability of the extraction process by accurately controlling the amount of biological enzymes added, suitable reaction temperature, pH value, stirring speed and other reaction conditions, while clarifying the use ratio of the extractant and the precise extraction process, so that the extraction efficiency of amino acids is significantly improved, and the extraction efficiency is greatly improved, thereby providing sufficient and high-quality amino acid raw materials for the subsequent preparation of high-quality fertilizers, and greatly improving the nutrient content in the fertilizer.

[0014] 2. The present invention can prevent the oxidative decomposition of amino acids by adding natural antioxidant vitamin C in the fertilizer preparation process, so that the stability and storage period of the fertilizer can be extended, and the prepared fertilizer has multiple functions by combining amino acids with beneficial components such as humic acid. It can not only improve soil structure, but also promote plant growth and improve its stress resistance, thus meeting the demand for diversified fertilizer functions in agricultural production; 3. The present invention recovers the remaining fermentation liquid after extracting amino acids, and extracts the remaining nutrients for preparing other products through filtration at a specific temperature, precise filtration medium and concentration treatment, thereby maximizing resource utilization and reducing resource waste. At the same time, compared with traditional extractants, the ionic liquid composite extractant has lower volatility and toxicity, reducing pollution to the environment. These measures reduce energy consumption and waste emissions, and greatly reduce pollution to the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] 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

[0016] 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.

[0017] 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.

[0018] Please see attached Figure 1 -Attached Figure 2 The present invention provides a method for preparing fertilizer by extracting amino acids from glycine fermentation broth. The method for preparing fertilizer comprises the following steps: Step 1: placing the glycine fermentation broth in a reaction vessel, adding a specific biological enzyme to the fermentation broth at a temperature of 30°C-35°C and a pH value of 6.0-6.5, with the addition amount being 2%-3% of the mass of the fermentation broth, the stirring speed being controlled at 70r / min-80r / min, and the continuous treatment time being 3h-4h to decompose impurities in the fermentation broth; Step 2, select an ionic liquid composite extractant as an extractant, mix it with the fermentation liquid at a mass ratio of 1:1.5-2.0, place it in an extraction device, and stir and extract it at a temperature of 45°C-50°C and a pressure of 0.4MPa-0.5MPa. The extraction process is divided into two stages: an early stage and a late stage. The early extraction time is 2.5h-3.0h. During this period, the extract is monitored in real time. When the amino acid concentration in the extract reaches 40%-50% of the initial amino acid concentration of the fermentation liquid, enter the late extraction stage. The late extraction time is 1.5h-2.0h to extract amino acids; Step 3: Preliminary filtration of the extracted amino acid solution using microporous ceramic filter material to remove residual tiny impurities, then passing the filtered solution through an ion exchange resin column to adsorb ionic impurities in the solution using the ion exchange resin, and then evaporating and concentrating the amino acid solution; Step 4: adding natural antioxidant vitamin C to the concentrated amino acids, then stirring evenly, adding beneficial ingredient humic acid, the mass ratio of which to amino acids is 1:3.5-4.0, and using a specific granulation process to granulate at a temperature of 55° C.-60° C. to prepare fertilizer; Step 5: purifying the extracted amino acids by using a multi-stage membrane separation and purification method at a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa to improve the purity of the amino acids to a purity of not less than 95%; Step 6: Recover the remaining fermentation liquid after amino acid extraction, filter the remaining fermentation liquid at a temperature of 35°C-40°C, and then concentrate it to extract the remaining nutrients for the preparation of other products, thereby realizing resource recycling and completing the preparation of fertilizer.

[0019] In one embodiment of the present invention: in step one, the specific biological enzyme is an enzyme preparation modified by a specific gene sequence, which is highly active and stable in the range of 30°C-35°C and a pH value of 6.0-6.5. When added to the fermentation broth, it is evenly dispersed through a dripping device to make the enzyme and the fermentation broth contact evenly. During the treatment process, the stirring speed is controlled at 70r / min-80r / min to promote the reaction of the enzyme with impurities, and the reaction time is controlled at 3h-4h.

[0020] In one embodiment of the present invention: in step 2, the ionic liquid composite extractant is composed of an ionic liquid and an organic extractant in proportion. The ionic liquid has a unique cation and anion structure and has high selectivity and affinity for amino acids. The organic extractant can enhance the solubility and stability of the extractant. During the extraction process, the stirring speed is controlled at 90r / min-100r / min to ensure that the extractant and the amino acid are fully mixed.

[0021] In one embodiment of the present invention: in step three, the microporous ceramic filter material used for preliminary filtration has a pore size of 0.08 μm-0.1 μm to remove tiny impurities in the extracted amino acid solution. The filtration process is carried out at a pressure of 0.25 MPa-0.3 MPa. When the filtered solution is evaporated and concentrated, the temperature is controlled at 60°C-70°C. When the solution concentration reaches a mass fraction of 60%-70%, the evaporation and concentration is stopped to ensure that the solution concentration meets the requirements for granulation.

[0022] In one embodiment of the present invention: in step 4, when adding natural antioxidant vitamin C, its addition amount is controlled to be 1.5%-2% of the total mass of the fertilizer. During the mixing process of the antioxidant with the concentrated amino acids and other beneficial ingredients, the antioxidant is stirred for 30 minutes by a stirring device to ensure uniform distribution. In the granulation process, under the condition of a temperature of 55°C-60°C, the antioxidant can effectively prevent the amino acids from being oxidized and decomposed, thereby improving the stability and storage life of the fertilizer.

[0023] In one embodiment of the present invention: in step 4, humic acid is added until the mass ratio of humic acid to amino acid is 1:3.5-4.0. During the addition process, the order of adding concentrated amino acids first and then adding humic acid is adopted to ensure full integration with the amino acids. These components work together with the amino acids to provide plants with a variety of nutrients. During the granulation process, by controlling the granulation time to 1 hour, the beneficial ingredients are evenly distributed in the fertilizer particles, thereby improving the versatility of the fertilizer, promoting plant growth and improving stress resistance.

[0024] In one embodiment of the present invention: In step five, the amino acid purification treatment adopts a multi-stage membrane separation purification method and purification equipment, and impurities and impurities are removed based on the selective separation principle of the membrane. The purification equipment is a temperature and pressure control device, and the purification operation is performed under the conditions of a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa. The purity of the amino acid is improved by three-stage membrane separation treatment, so that its purity is not less than 95%, providing high-quality raw materials for the preparation of high-quality fertilizers.

[0025] In one embodiment of the present invention: In step six, during the recovery process of the by-products, the remaining fermentation liquid is first filtered at a temperature of 35°C-40°C, the filter medium used for filtration is activated carbon filter cotton, and the filtration accuracy is 0.04μm-0.05μm, and the filtered solution is then concentrated by evaporation concentration method at a temperature of 65°C-70°C. During the concentration process, the process parameters are strictly controlled to ensure that the content of the remaining nutrients after concentration is not less than 60%, so that it can be used to prepare other products and realize resource recycling.

[0026] In one embodiment of the present invention: in step 3, the operating temperature of the ion exchange resin column is 25° C.-30° C., and the flow rate is controlled at 1.5-2 times the resin volume per hour.

[0027] Example 1, please refer to the attached Figure 1 -Attached Figure 2First, the glycine fermentation liquid was placed in a reaction vessel. Under the conditions of a temperature of 35°C and a pH value of 6.0, a specific biological enzyme was added to the fermentation liquid in an amount of 3% of the mass of the fermentation liquid. The enzyme was evenly dispersed through a dripping device so that the enzyme was evenly in contact with the fermentation liquid. The stirring speed was controlled at 80r / min and the treatment was continued for 4 hours to decompose the impurities in the fermentation liquid. Then, an ionic liquid composite extractant was selected as the extractant. After being mixed with the fermentation liquid at a mass ratio of 1:2.0, the extractant was placed in an extraction device and stirred and extracted at a temperature of 50°C and a pressure of 0.5MPa. The extraction process was divided into two stages: the early stage and the late stage. The initial extraction time is 3.0h, during which the extract is monitored in real time. When the amino acid concentration in the extract reaches 50% of the initial amino acid concentration in the fermentation broth, the late extraction stage begins. The late extraction time is 2.0h, and the amino acids are fully extracted. Then, the extracted amino acid solution is preliminarily filtered. The filtration adopts a microporous ceramic filter material with a pore size of 0.08μm. The filtration is carried out at a pressure of 0.25MPa to remove the remaining tiny impurities. Then, the filtered solution is passed through an ion exchange resin column. The operating temperature of the ion exchange resin column is 25℃, and the flow rate is controlled at 2 times the resin volume per hour. The ion impurities in the solution are removed by the ion exchange resin. The amino acid solution is then evaporated and concentrated, the temperature is controlled at 60°C, and the evaporation and concentration is stopped when the solution concentration reaches 60% by mass. After that, natural antioxidant vitamin C is added to the concentrated amino acid, and its addition amount is controlled to be 1.5% of the total mass of the fertilizer, followed by stirring evenly, and then the beneficial ingredient humic acid is added, and the mass ratio of humic acid to amino acid is 1:4. A specific granulation process is used to granulate at a temperature of 55°C to prepare fertilizer, and the granulation time is 1h. The extracted amino acids are then purified by a multi-stage membrane separation and purification method and purification equipment. Impurities and impurities are removed based on the selective separation principle of the membrane, and the purification is carried out. The equipment is a temperature and pressure control device, which performs purification operations at a temperature of 40°C and a pressure of 0.35MPa. Through three-stage membrane separation treatment, the purity of amino acids is improved to no less than 95%, providing high-quality raw materials for the preparation of high-quality fertilizers. Finally, the remaining fermentation liquid after the amino acids are extracted is recovered and filtered at a temperature of 40°C. The filter medium used for filtration is activated carbon filter cotton with a filtration accuracy of 0.04μm. It is then concentrated by evaporation concentration method at a temperature of 70°C to extract the remaining nutrients for the preparation of other products, thereby realizing resource recycling.

[0028] Example 2, please refer to the attached Figure 1 -Attached Figure 2First, the glycine fermentation liquid is placed in a reaction container, and under the conditions of a temperature of 32°C and a pH value of 6.2, a specific biological enzyme is added to the fermentation liquid in an amount of 2.5% of the mass of the fermentation liquid. The enzyme is evenly dispersed through a dripping device so that the enzyme is evenly in contact with the fermentation liquid. The stirring speed is controlled at 75r / min and the treatment is continued for 3.5h to decompose impurities in the fermentation liquid. Then, an inorganic salt extractant is selected as an extractant, and after mixing with the fermentation liquid at a mass ratio of 1:1.8, the extractant is placed in an extraction device and stirred and extracted at a temperature of 48°C and a pressure of 0.45MPa. The extraction process is divided into two stages: the early stage and the late stage. The early stage extraction time is 2.8 hours. During this period, the extract is monitored in real time. When the amino acid concentration in the extract reaches 45% of the initial amino acid concentration of the fermentation broth, the late stage of extraction begins. The late extraction time is 1.8 hours. The amino acids are fully extracted. Then, the extracted amino acid solution is preliminarily filtered. The filtration adopts ordinary filter paper with a pore size of 0.08μm. The filtration is carried out under a pressure of 0.2MPa to remove the residual tiny impurities. Then, the filtered solution is passed through an ion exchange resin column. The operating temperature of the ion exchange resin column is 28℃ and the flow rate is controlled at 100 μm per hour. The volume of the resin was 1.8 times that of the resin, and the ion impurities in the solution were adsorbed by the ion exchange resin. Then, the amino acid solution was evaporated and concentrated, and the temperature was controlled at 65°C. When the solution concentration reached 65% by mass, the evaporation and concentration were stopped. After that, the natural antioxidant vitamin C was added to the concentrated amino acid, and its addition amount was controlled to be 1.8% of the total mass of the fertilizer. Then, it was stirred evenly, and the beneficial ingredient humic acid was added, and the mass ratio of humic acid to amino acid was 1:3.8. A specific granulation process was used, and granulation was carried out at a temperature of 58°C to prepare the fertilizer. The granulation time was 1 hour, and then the extracted amino acids were purified. , a two-stage membrane separation and purification method and purification equipment are used to perform purification operations at a temperature of 38°C and a pressure of 0.4MPa. The purity of amino acids is improved through three-stage membrane separation treatment to a purity of not less than 90%. Finally, the remaining fermentation liquid after the amino acids are extracted is recovered and filtered at a temperature of 38°C. The filter medium used for filtration is ordinary filter cotton with a filtration accuracy of 0.05μm. It is then concentrated using an evaporation concentration method at a temperature of 68°C to extract the remaining nutrients for the preparation of other products, thereby realizing resource recycling.

[0029] Example 3, please refer to the attached Figure 1 -Attached Figure 2First, the glycine fermentation broth was placed in a reaction vessel, and trypsin was added to the fermentation broth at a temperature of 30°C and a pH value of 6.5, with the addition amount of 2% of the mass of the fermentation broth being uniformly dispersed through a dripping device so that the enzyme was in uniform contact with the fermentation broth, and the stirring speed was controlled at 70r / min, and the treatment was continued for 3 hours to decompose the impurities in the fermentation broth. Then, an organic solvent extractant was selected as an extractant, and after mixing with the fermentation broth at a mass ratio of 1:1.5, the extractant was placed in an extraction device, and stirred and extracted at a temperature of 45°C and a pressure of 0.4MPa. The process is divided into two stages: the early stage and the late stage. The early stage extraction time is 2.5 hours. During this period, the extract is monitored in real time. When the amino acid concentration in the extract reaches 40% of the initial amino acid concentration of the fermentation broth, the late stage of extraction begins. The late extraction time is 1.5 hours to fully extract the amino acids. Then, the extracted amino acid solution is preliminarily filtered using gauze filter material with a pore size of 0.5 μm. The filtration is performed at a pressure of 0.1 MPa to remove residual tiny impurities. The filtered solution is then passed through an ion exchange resin column. The operating temperature of the ion exchange resin column is 25°C and the flow rate is controlled at 100 μm per liter. The volume of the resin was increased by 1.5 times per hour, and the ion impurities in the solution were adsorbed by the ion exchange resin. Then, the amino acid solution was evaporated and concentrated. The temperature was controlled at 60°C. When the solution concentration reached 60% by mass, the evaporation and concentration were stopped. After that, an artificial synthetic antioxidant was added to the concentrated amino acid. The amount of the antioxidant was controlled to be 1% of the total mass of the fertilizer. Then, the fertilizer was stirred evenly. Then, the beneficial ingredient humic acid was added. The mass ratio of humic acid to amino acid was 1:3.5. The conventional granulation process was used. The fertilizer was prepared at a temperature of 55°C. The granulation time was 0.5h. Then, the extracted amino acids were subjected to a granulation. The method and equipment for purifying by using a membrane separation method are as follows: the purification operation is carried out at a temperature of 40°C and a pressure of 0.3MPa; the purity of amino acids is improved by using a membrane separation treatment to a value not less than 85%; finally, the remaining fermentation liquid after the amino acids are extracted is recovered and filtered at a temperature of 35°C; the filtration medium used is ordinary filter cotton with a filtration accuracy of 0.1μm; and then the filtration liquid is concentrated by using an evaporation concentration method at a temperature of 65°C to extract the remaining nutrients for preparing other products, thereby realizing resource recycling.

[0030] Material testing: Experimental equipment: reaction vessel, extraction equipment, filtration device, evaporation concentration equipment, granulation equipment, purification equipment, amino acid analyzer, element analyzer, stability testing equipment, chemical oxygen demand tester; Experimental steps: Three groups of experiments were set up, namely, Example 1, Example 2 and Example 3; Take an equal amount of 1000 ml of the fertilizer prepared by the glycine fermentation broth in Example 1, Example 2 and Example 3 and the corresponding 200 ml of the waste liquid remaining from the fertilizer preparation; In each example, the following data were recorded: Amino acid extraction efficiency: The concentration of amino acids in the amino acid solution obtained after the extraction and purification steps was measured by an amino acid analyzer. The extraction efficiency was calculated as follows: extraction efficiency (%) = (mass of amino acids after purification / initial mass of amino acids in the fermentation broth) × 100%; Nutrient content of fertilizer: Use an element analyzer to analyze the content of nitrogen, phosphorus and potassium in the prepared fertilizer. Nutrient content (%) = (mass of elements in fertilizer / total mass of fertilizer) × 100%; Fertilizer stability: Store the prepared fertilizer under certain conditions and regularly test the changes in the content of the active ingredients in the fertilizer. The fertilizer stability (active ingredient retention rate) is calculated as follows: Stability (%) = (mass of active ingredients in the fertilizer after storage / mass of active ingredients in the fertilizer before storage) × 100%; Shelf life: record the time from the preparation of the fertilizer to the time when the stability drops to a certain level (such as the retention rate of active ingredients is lower than a certain threshold), in months; Resource utilization rate: measure the amount of residual nutrients extracted from the remaining fermentation liquid. The resource utilization rate is calculated as follows: Resource utilization rate (%) = (mass of the remaining nutrients extracted / mass of the initial nutrients in the remaining fermentation liquid) × 100%. For the small amount of waste liquid that may still exist after evaporation concentration and subsequent treatment, component analysis is also performed; Environmental pollution indicators: Use a chemical oxygen demand meter to detect the discharge of wastewater and waste residue during the experiment. Take chemical oxygen demand (COD) as an example, the unit is mg / L; As attached Figure 2 As shown, the present application shows excellent results in terms of amino acid extraction efficiency, fertilizer nutrient content, stability and storage life, resource utilization, and environmental protection; The amino acid extraction efficiency of Example 1 reaches 90.50%, which can effectively extract amino acids from glycine fermentation broth, providing sufficient and high-quality amino acid raw materials for the subsequent preparation of high-quality fertilizers; The nitrogen nutrient content of the fertilizer in Example 1 is 20.30%, which shows that the fertilizer prepared by this method has rich nutrient content, can meet the needs of plant growth, and greatly improves the nutritional value of the fertilizer; The fertilizer of Example 1 has the best stability performance, with an effective ingredient retention rate of 95.20% and a storage period of 18 months, which means that the fertilizer can maintain good stability during storage, the effective ingredients are not easily lost, and the service life of the fertilizer is extended; The resource utilization rate of Example 1 reached 92.30%, indicating that the remaining nutrients can be fully extracted for preparing other products, achieving maximum utilization of resources and reducing resource waste; The environmental pollution index (COD) of Example 1 is 51 mg / L, which is lower than 70.3 mg / L of Example 2 and 90.5 mg / L of Example 3. Compared with traditional extractants, the ionic liquid composite extractant has lower volatility and toxicity, which reduces pollution to the environment. At the same time, through the reasonable treatment of the remaining fermentation liquid, energy consumption and waste emissions are reduced, which greatly reduces pollution to the environment.

[0031] 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 method for extracting amino acids from glycine fermentation broth to prepare fertilizer, characterized in that: The method for preparing the fertilizer comprises the following steps: Step 1: placing the glycine fermentation broth in a reaction vessel, adding a specific biological enzyme to the fermentation broth at a temperature of 30°C-35°C and a pH value of 6.0-6.5, with the addition amount being 2%-3% of the mass of the fermentation broth, the stirring speed being controlled at 70r / min-80r / min, and the continuous treatment time being 3h-4h to decompose impurities in the fermentation broth; Step 2, select an ionic liquid composite extractant as an extractant, mix it with the fermentation liquid at a mass ratio of 1:1.5-2.0, place it in an extraction device, and stir and extract it at a temperature of 45°C-50°C and a pressure of 0.4MPa-0.5MPa. The extraction process is divided into two stages: an early stage and a late stage. The early extraction time is 2.5h-3.0h. During this period, the extract is monitored in real time. When the amino acid concentration in the extract reaches 40%-50% of the initial amino acid concentration of the fermentation liquid, enter the late extraction stage. The late extraction time is 1.5h-2.0h to extract amino acids; Step 3: Preliminary filtration of the extracted amino acid solution using microporous ceramic filter material to remove residual tiny impurities, then passing the filtered solution through an ion exchange resin column to adsorb ionic impurities in the solution using the ion exchange resin, and then evaporating and concentrating the amino acid solution; Step 4: adding natural antioxidant vitamin C to the concentrated amino acids, then stirring evenly, adding beneficial ingredient humic acid, the mass ratio of which to amino acids is 1:3.5-4.0, and using a specific granulation process to granulate at a temperature of 55° C.-60° C. to prepare fertilizer; Step 5: purifying the extracted amino acids by using a multi-stage membrane separation and purification method at a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa to improve the purity of the amino acids to a purity of not less than 95%; Step 6: Recover the remaining fermentation liquid after extracting amino acids, filter the remaining fermentation liquid at a temperature of 35°C-40°C, and then concentrate it to extract the remaining nutrients for preparing other products, thereby realizing resource recycling and completing the final preparation of the fertilizer.

2. A method for extracting amino acids from glycine fermentation broth to prepare fertilizer according to claim 1, characterized in that: In the step 1, the specific biological enzyme is an enzyme preparation modified by gene sequence, which has high activity and stability in the range of 30°C-35°C and pH value of 6.0-6.

5. When added to the fermentation broth, it is evenly dispersed through a dripping device so that the enzyme is evenly in contact with the fermentation broth. During the treatment process, the stirring speed is controlled at 70r / min-80r / min to promote the reaction of the enzyme with impurities, and the reaction time is controlled at 3h-4h.

3. A method for extracting amino acids from glycine fermentation broth to prepare fertilizer according to claim 1, characterized in that: In the step 2, the ionic liquid composite extractant is compounded by the ionic liquid and the organic extractant in proportion. During the extraction process, the stirring speed is controlled at 90r / min-100r / min.

4. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step three, the microporous ceramic filter material used for preliminary filtration has a pore size of 0.08 μm-0.1 μm to remove tiny impurities in the extracted amino acid solution. The filtration process is carried out at a pressure of 0.25 MPa-0.3 MPa. When the filtered solution is evaporated and concentrated, the temperature is controlled at 60°C-70°C. When the solution concentration reaches a mass fraction of 60%-70%, the evaporation and concentration is stopped.

5. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step 4, when adding the natural antioxidant vitamin C, its addition amount is controlled to be 1.5%-2% of the total mass of the fertilizer. During the mixing process of the antioxidant with the concentrated amino acids and other beneficial ingredients, the mixture is stirred for 30 minutes by a stirring device.

6. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step 4, humic acid is added until the mass ratio of humic acid to amino acid is 1:3.5-4.

0. During the addition process, the order of adding concentrated amino acids first and then humic acid is adopted. During the granulation process, the granulation time is controlled to be 1 hour.

7. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step 5, the amino acid purification treatment adopts a multi-stage membrane separation purification method and purification equipment to remove impurities and impurities based on the selective separation principle of the membrane. The purification equipment is a temperature and pressure control device, and the purification operation is carried out under the conditions of a temperature of 40°C-45°C and a pressure of 0.35MPa-0.4MPa. The purity of the amino acid is improved by three-stage membrane separation treatment, so that its purity is not less than 95%.

8. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step six, during the recovery process of the by-products, the remaining fermentation liquid is first filtered at a temperature of 35°C-40°C, the filter medium used for filtration is activated carbon filter cotton, and the filtration accuracy is 0.04μm-0.05μm. The filtered solution is then concentrated by evaporation concentration method at a temperature of 65°C-70°C. During the concentration process, the process parameters are strictly controlled to ensure that the remaining nutrient content after concentration is not less than 60%.

9. The method for preparing fertilizer by extracting amino acids from glycine fermentation broth according to claim 1, characterized in that: In the step 3, the operating temperature of the ion exchange resin column is 25° C.-30° C., and the flow rate is controlled at 1.5-2 times the resin volume per hour.

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