Method for preparing fertilizer by extracting minerals from valine fermentation liquor

Abstract

The invention discloses a method for preparing a fertilizer by extracting minerals from valine fermentation broth, and relates to the technical field of fertilizer preparation, the method comprises the following steps: pretreatment of valine fermentation broth, mineral extraction and purification, nutrition blending and biological excitation, and the biological excitation comprises low-temperature fermentation precipitation and magnetic stirring. The method has the advantages that the impurities in the valine fermentation liquor are removed through the steps of pretreatment and biological excitation on the impurities in the valine fermentation liquor, meanwhile, a foundation is laid for the subsequent extraction and purification steps, energy consumption is reduced, and through magnetic stirring and ventilation operation, the purity of the impurities in the valine fermentation liquor is improved. The method can ensure uniform distribution of substances in the supernatant, promote natural growth of microorganisms, monitor the change of chemical components after stirring, make the whole extraction process more scientific and accurate, and can effectively separate mineral ions from the fermentation broth by using ion exchange resin and an adsorption material in the mineral extraction and purification stage.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a method for preparing fertilizer by extracting minerals from valine fermentation liquid. Background Art

[0002] In modern agricultural production, efficient and environmentally friendly fertilizers are crucial to improving crop yields and quality. With the continuous advancement of science and technology, people have higher and higher requirements for fertilizers. They not only require them to have rich nutrients, but also expect them to have greener and more sustainable sources.

[0003] As an important amino acid, valine produces a large amount of fermentation liquid during the fermentation production process. In addition to organic components such as valine, these valine fermentation liquids also contain rich mineral resources. However, the current treatment of valine fermentation liquids often focuses on the extraction and recovery of valine, while ignoring the potential value of the minerals therein. On the one hand, the production of traditional fertilizers usually relies on limited mineral resources, which not only faces the problem of gradual resource depletion, but also may cause great damage to the environment during mining and processing. On the other hand, with the growing demand for sustainable agricultural development, finding new fertilizer resources and production methods has become a top priority. In this context, it is urgent to develop a method for extracting minerals from valine fermentation broth to prepare fertilizers, which has important practical significance. Through a series of operations such as pretreatment of valine fermentation broth, mineral extraction and purification, nutrient formulation and biostimulation, the valine fermentation broth that might have been wasted can be converted into a new type of fertilizer rich in various nutrients. This method can not only realize the reuse of resources and reduce dependence on traditional mineral resources, but also reduce the pollution of valine fermentation broth to the environment, providing a greener and more sustainable source of fertilizer for agricultural production. To this end, we propose a method for extracting minerals from valine fermentation broth to prepare fertilizers. Summary of the invention

[0004] The object of the present invention is to provide a method for preparing fertilizer by extracting minerals from valine fermentation broth.

[0005] In order to solve the problems raised in the above background technology, the present invention provides the following technical solutions: a method for extracting minerals from valine fermentation broth to prepare fertilizer, comprising pretreatment of valine fermentation broth, mineral extraction and purification, nutrient preparation and biostimulation, wherein the biostimulation includes low-temperature fermentation precipitation and magnetic stirring, and the specific operation steps of extracting minerals from valine fermentation broth to prepare fertilizer are as follows:

[0006] Step 1, transferring the crude valine fermentation broth into a low-temperature fermentation sedimentation tank, adding microbial flora and stirring, wherein the amount of microbial flora added is determined according to the volume of the fermentation broth, taking the supernatant after the valine fermentation broth is precipitated, and transferring it into a corrosion-resistant container in a sterile environment for standby use;

[0007] Step 2: transferring the supernatant of the valine fermentation liquid into a magnetic stirring tank, using magnetic stirring and ventilation to ensure that the substances in the supernatant are evenly distributed, waiting for the microorganisms to grow naturally, and monitoring the growth state of the microorganisms and the changes in the chemical composition of the supernatant. After the treatment is completed, the valine fermentation liquid is obtained;

[0008] Step 3: transferring the treated valine fermentation liquid into an extraction tank, and using ion exchange resin and adsorption material to adsorb mineral ions in the valine fermentation liquid;

[0009] Step 4: placing the adsorbent material with mineral ions into an eluent, and after the minerals are eluted, transferring it to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution;

[0010] Step 5: Add nitrogen, phosphorus, potassium and trace elements to the mineral solution, stir and mix, evaporate and concentrate, add adhesive to the concentrate, use a granulator to make it into fertilizer granules, extract part of the fertilizer for quality monitoring, and bag it for use after passing the quality control.

[0011] As a further solution of the present invention: in the step 1, the crude valine fermentation broth is transferred to a low-temperature fermentation sedimentation tank at 2°C-10°C, the screened microbial flora is added, and the broth is stirred at a stirring rate of 120r / min-140r / min for 30min-60min. After the stirring is completed, the broth is allowed to stand at a temperature of 5°C-10°C for 24h-48h.

[0012] As a further solution of the present invention: in the step 1, after the precipitation is completed, the supernatant in the crude valine fermentation broth is taken out and transferred into a corrosion-resistant container for light protection. The amount of microbial flora added is determined according to the total volume of the crude valine fermentation broth, and each 1L of fermentation broth contains 0.1g-0.5g of microbial flora.

[0013] As a further solution of the present invention: in step 2, the treated supernatant is transferred to a magnetic stirring tank, the stirring speed is set to 90r / min-120r / min, the temperature is controlled between 25°C-30°C, and the magnetic stirring tank is ventilated, and the ventilation volume is 0.1m per liter of valine fermentation liquid. 3 / min-0.5m 3 / min, and monitor the changes in the chemical composition of the supernatant during fermentation, including organic matter content, pH and mineral concentration. The natural growth time of microorganisms is 18h-24h.

[0014] As a further scheme of the present invention: in the step three, the treated valine fermentation broth is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected according to the volume of the fermentation broth and the content of minerals to adsorb the mineral ions in the valine fermentation broth. During the adsorption process, the valine fermentation broth is slowly stirred, the adsorption time is 2h-4h, and the mass of the adsorption material is 10g / L-50g / L, and the specific mass needs to be adjusted according to the performance of the adsorption material and the characteristics of the valine fermentation broth.

[0015] As a further solution of the present invention: in the step four, the adsorption material that has adsorbed mineral ions is placed in an eluent to elute the mineral ions from the adsorption material while avoiding damage to the adsorption material. After the mineral ions are eluted, they are transferred to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution.

[0016] As a further solution of the present invention: in the step 4, the eluent includes a dilute acid solution and a salt solution, wherein the concentration of the dilute acid solution is 0.1 mol / L-0.5 mol / L, and the concentration of the salt solution is 0.2 mol / L-1 mol / L.

[0017] As a further scheme of the present invention: in the step five, nitrogen, phosphorus, potassium and trace elements are added to the high-purity mineral solution, the ratio of nitrogen, phosphorus and potassium is 15:15:15, and the trace elements include calcium, magnesium, iron, zinc and other salt compounds. After adding nitrogen, phosphorus, potassium and trace elements according to the ratio, stirring and mixing are carried out for evaporation and concentration, and the concentration temperature is controlled at 50°C-80°C. During the concentration, a binder is added, and the amount of the binder added is 2%-4% of the total amount of the high-purity mineral solution.

[0018] As a further solution of the present invention: in the step five, after the evaporation and concentration is completed, a granulator is used to make fertilizer granules with a particle size of 2mm-4mm. After the granulation is completed, the fertilizer granules are extracted for quality inspection, including nutrient component analysis, particle strength test and solubility test. After passing the inspection, the granules are bagged and put into use.

[0019] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are:

[0020] 1. The present invention not only removes impurities in the crude valine fermentation broth by pretreating the impurities in the valine fermentation broth and performing the biostimulation step, but also lays a foundation for the subsequent extraction and purification steps and reduces energy consumption. Through magnetic stirring and ventilation operations, it can ensure that the substances in the supernatant are evenly distributed, promote the natural growth of microorganisms, and monitor the changes in its chemical composition after stirring, so that the entire extraction process is more scientific and accurate. In the mineral extraction and purification stage, by using ion exchange resins and adsorption materials, mineral ions can be effectively separated from the fermentation broth, thereby improving the utilization rate of resources. Residual organic matter and impurities are removed by a membrane filtration device to obtain a high-purity mineral solution, which not only reduces the demand for the exploitation of traditional mineral resources, but also can prepare high-purity fertilizers and reduce environmental pollution problems caused by mineral exploitation and processing;

[0021] 2. The present invention adds nitrogen, phosphorus, potassium and trace elements in scientific proportions so that the fertilizer can meet the different needs of crop growth. The use of a membrane filtration device further removes residual organic matter and impurities, ensuring the high purity of the mineral solution. By accurately selecting adsorption materials such as ion exchange resins, zeolites and activated carbon according to the volume of the fermentation liquid and the content of minerals, and controlling the quality and adsorption time of the adsorption materials, the adsorption process of mineral ions is made more efficient and accurate, ensuring the purity and quality of the extracted minerals. Through evaporation concentration and the addition of a binder for granulation, the prepared fertilizer particles have a moderate size, good solubility and stability, are easy to apply and be absorbed and utilized by crops, and high-quality fertilizers can increase the yield and quality of crops, reduce the use of chemical fertilizers, reduce agricultural production costs, and also reduce pollution to the soil and the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic diagram of a specific process of preparing fertilizer from minerals in an embodiment of the present invention;

[0023] Figure 2 Schematic diagram for comparing fertilizer properties of five groups of embodiments in the present invention. DETAILED DESCRIPTION

[0024] The specific embodiments of the present invention are 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. 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.

[0025] The present invention discloses a method for extracting minerals from valine fermentation broth to prepare fertilizer, comprising pretreatment of the valine fermentation broth, mineral extraction and purification, nutrient preparation and biostimulation, wherein the biostimulation comprises low-temperature fermentation precipitation and magnetic stirring, and the specific operation steps of extracting minerals from the valine fermentation broth to prepare fertilizer are as follows:

[0026] Step 1, transferring the crude valine fermentation broth into a low-temperature fermentation sedimentation tank, adding microbial flora and stirring, wherein the amount of microbial flora added is determined according to the volume of the fermentation broth, taking the supernatant after the valine fermentation broth is precipitated, and transferring it into a corrosion-resistant container in a sterile environment for standby use;

[0027] Step 2: transferring the supernatant of the valine fermentation liquid into a magnetic stirring tank, using magnetic stirring and ventilation to ensure that the substances in the supernatant are evenly distributed, waiting for the microorganisms to grow naturally, and monitoring the growth state of the microorganisms and the changes in the chemical composition of the supernatant. After the treatment is completed, the valine fermentation liquid is obtained;

[0028] Step 3: transferring the treated valine fermentation liquid into an extraction tank, and using ion exchange resin and adsorption material to adsorb mineral ions in the valine fermentation liquid;

[0029] Step 4: placing the adsorbent material with mineral ions into an eluent, and after the minerals are eluted, transferring it to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution;

[0030] Step 5: Add nitrogen, phosphorus, potassium and trace elements to the mineral solution, stir and mix, evaporate and concentrate, add adhesive to the concentrate, use a granulator to make it into fertilizer granules, extract part of the fertilizer for quality monitoring, and bag it for use after passing the quality control.

[0031] In one embodiment of the present invention: in step 1, the crude valine fermentation broth is transferred to a low-temperature fermentation sedimentation tank at 2°C-10°C, the screened microbial flora is added, and the broth is stirred at a stirring rate of 120r / min-140r / min for 30min-60min. After the stirring is completed, it is allowed to stand at a temperature of 5°C-10°C for 24h-48h.

[0032] In one embodiment of the present invention: in step 1, after precipitation is completed, the supernatant in the crude valine fermentation broth is taken out and transferred to a corrosion-resistant container for light protection. The amount of microbial flora added is determined according to the total volume of the crude valine fermentation broth, and each 1L of fermentation broth contains 0.1g-0.5g of microbial flora.

[0033] In one embodiment of the present invention, in step 2, the treated supernatant is transferred to a magnetic stirring tank, the stirring speed is set at 90 r / min-120 r / min, the temperature is controlled between 25°C and 30°C, and the magnetic stirring tank is ventilated at a ventilation rate of 0.1 m / L of valine fermentation liquid. 3 / min-0.5m 3 / min, and monitor the changes in the chemical composition of the supernatant during fermentation, including organic matter content, pH and mineral concentration. The natural growth time of microorganisms is 18h-24h.

[0034] In one embodiment of the present invention: in step three, the treated valine fermentation broth is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected according to the volume of the fermentation broth and the content of minerals to adsorb the mineral ions in the valine fermentation broth. During the adsorption process, the valine fermentation broth is slowly stirred, the adsorption time is 2h-4h, and the mass of the adsorption material is 10g / L-50g / L. The specific mass needs to be adjusted according to the performance of the adsorption material and the characteristics of the valine fermentation broth.

[0035] In one embodiment of the present invention: in step four, the adsorption material that has adsorbed mineral ions is placed in an eluent to elute the mineral ions from the adsorption material while avoiding damage to the adsorption material. After the mineral ions are eluted, they are transferred to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution.

[0036] In one embodiment of the present invention: in step 4, the eluent includes a dilute acid solution and a salt solution, wherein the concentration of the dilute acid solution is 0.1 mol / L-0.5 mol / L, and the concentration of the salt solution is 0.2 mol / L-1 mol / L.

[0037] In one embodiment of the present invention: in step five, nitrogen, phosphorus, potassium and trace elements are added to the high-purity mineral solution, the ratio of nitrogen, phosphorus and potassium is 15:15:15, the trace elements include calcium, magnesium, iron, zinc and other salt compounds, after adding nitrogen, phosphorus, potassium and trace elements according to the ratio, stirring and mixing are carried out for evaporation and concentration, the concentration temperature is controlled at 50°C-80°C, and a binder is added during concentration, and the amount of the binder added is 2%-4% of the total amount of the high-purity mineral solution.

[0038] In one embodiment of the present invention: in step five, after evaporation and concentration are completed, a granulator is used to make fertilizer granules with a particle size of 2mm-4mm. After granulation is completed, the fertilizer granules are extracted for quality inspection, including nutrient analysis, particle strength test and solubility test. After passing the inspection, they are bagged and put into use.

[0039] In one embodiment of the present invention, when adding the microbial flora to the low-temperature fermentation sedimentation tank of the valine fermentation broth, two operation modes of multiple small-scale addition and premixed addition can be used. The multiple small-scale addition is to divide the microbial flora into multiple small groups, add them to the fermentation broth in batches, and slowly stir them while adding to make the microbial flora initially dispersed, and then add the next portion of the microbial flora. The premixed addition is to first premix the microbial flora with a small amount of valine fermentation broth in a separate container, stir it evenly, and then pour it into the fermentation broth in the low-temperature fermentation sedimentation tank to avoid the local focusing phenomenon that may occur when the microbial flora is directly added to the valine fermentation broth.

[0040] In one embodiment of the present invention: the concentrated valine fermentation liquid fertilizer can be made into powder fertilizer and liquid fertilizer. The powder fertilizer is made by spray drying the concentrated valine fermentation liquid into powder. During the spray drying process, it is necessary to control the air inlet temperature, air outlet temperature and spray speed to ensure the quality of the powder fertilizer. The liquid fertilizer is made by directly canning the concentrated fertilizer solution. During the canning process, the cleanliness and sealing of the container must be ensured to prevent the fertilizer from deteriorating and leaking.

[0041] In one embodiment of the present invention: the dilute acid solution is a dilute hydrochloric acid solution, the salt solution is a sodium chloride solution, and the adhesive is ordinary starch. The sodium chloride solution has a small effect on the adsorption material and is not likely to cause a significant change in the result of the adsorption material. The starch can be decomposed by microorganisms in the soil and will not cause pollution to the soil.

[0042] In one embodiment of the present invention: when detecting the organic matter content, pH value and mineral concentration of the supernatant, the organic matter content in the supernatant is detected by potassium dichromate method, the pH value in the supernatant is directly detected by pH meter, and the mineral concentration in the supernatant is detected by inductively coupled plasma optical emission spectrometry (ICP-OES).

[0043] Embodiment 1

[0044] First, 10L of crude valine fermentation broth was prepared, and it was transferred to a low-temperature fermentation sedimentation tank at 5°C. Microbial flora was added in a small amount and multiple additions, and 0.3g of microbial flora was added to each 1L of fermentation broth. A portion of the microbial flora was first added to the fermentation broth, and stirred at a stirring rate of 130r / min for a period of time to make the microbial flora initially dispersed, and then the next portion of the microbial flora was added. The total stirring time was 45min. After the stirring was completed, it was allowed to stand at a temperature of 8°C for 36h. After the precipitation was completed, the supernatant in the crude valine fermentation broth was taken out and transferred to a corrosion-resistant container for light protection;

[0045] Next, the supernatant was transferred to a magnetic stirring tank, the stirring speed was set at 100 r / min, the temperature was controlled at 28°C, and the magnetic stirring tank was ventilated at a ventilation rate of 0.3 m3 / min per liter of valine fermentation liquid. The microorganisms were allowed to grow naturally, and the chemical composition changes of the supernatant, including the organic matter content, pH value and mineral concentration, were monitored. The organic matter content in the supernatant was detected by the potassium dichromate method, the pH value in the supernatant was directly detected by a pH meter, and the mineral concentration in the supernatant was detected by inductively coupled plasma optical emission spectrometry (ICP-OES). The natural growth time of the microorganisms was 20 h.

[0046] Afterwards, the treated valine fermentation liquid is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected to adsorb mineral ions in the valine fermentation liquid according to the volume of the fermentation liquid and the content of minerals. During the adsorption process, the valine fermentation liquid is slowly stirred, the mass of the adsorption material is 30 g / L, and the adsorption time is 3 hours;

[0047] Then, the adsorbent material that has adsorbed the mineral ions is placed in an eluent consisting of a 0.3 mol / L dilute hydrochloric acid solution and a 0.6 mol / L sodium chloride solution to elute the mineral ions from the adsorbent material while avoiding damage to the adsorbent material. After the mineral ions are eluted, they are transferred to a membrane filtration device. After elution, the volume of the mineral solution is 5 L, and the total amount of adsorbed mineral ions is 50 g. Residual organic matter and impurities are removed to obtain a high-purity mineral solution.

[0048] Finally, nitrogen, phosphorus, potassium and trace elements including calcium, magnesium, iron and zinc are added to the high-purity mineral solution in a ratio of 15:15:15. The mixture is stirred and concentrated by evaporation at 70°C. Ordinary starch accounting for 3% of the total amount of the high-purity mineral solution is added as a binder. A granulator is used to make it into fertilizer granules with a particle size of 3 mm. Part of the fertilizer is extracted for quality monitoring, including nutrient analysis, particle strength test and solubility test. After passing the test, it is bagged and put into use.

[0049] The volume of the fermentation liquid is 10L, and 0.3g of microbial flora is added per liter, and the total amount = 10L × 0.3g / L = 3g;

[0050] The volume of the mineral solution after elution was 5 L, and the total amount of adsorbed mineral ions was 50 g;

[0051] Mineral solution concentration = 50g ÷ 5L = 10g / L.

[0052] Embodiment 2

[0053] First, 8L of crude valine fermentation broth was prepared, and it was transferred to a low-temperature fermentation sedimentation tank at 5°C. Microbial flora was added in a small amount and multiple additions, and 0.3g of microbial flora was added to every 1L of fermentation broth. A portion of the microbial flora was first added to the fermentation broth, and stirred at a stirring rate of 130r / min for a period of time to make the microbial flora initially dispersed, and then the next portion of the microbial flora was added. The total stirring time was 45min. After the stirring was completed, it was allowed to stand at a temperature of 7°C for 40h. After the precipitation was completed, the supernatant in the crude valine fermentation broth was taken out and transferred to a corrosion-resistant container for light protection;

[0054] Next, the supernatant was transferred to a magnetic stirring tank, the stirring speed was set at 95 r / min, the temperature was controlled at 27°C, and the magnetic stirring tank was ventilated at a ventilation rate of 0.25 m3 / min per liter of valine fermentation liquid. The microorganisms were allowed to grow naturally, and the chemical composition changes of the supernatant, including the organic matter content, pH value and mineral concentration, were monitored. The organic matter content in the supernatant was detected by the potassium dichromate method, the pH value in the supernatant was directly detected by a pH meter, and the mineral concentration in the supernatant was detected by inductively coupled plasma emission spectrometry. The natural growth time of the microorganisms was 20 h.

[0055] Afterwards, the treated valine fermentation liquid was transferred to an extraction tank. According to the volume of the fermentation liquid and the content of minerals, ion exchange resin, zeolite and activated carbon were selected to adsorb the mineral ions in the valine fermentation liquid. During the adsorption process, the valine fermentation liquid was slowly stirred. The mass of the adsorption material was 25 g / L and the adsorption time was 2.5 h.

[0056] Then, the adsorbent material that has adsorbed the mineral ions is placed in an eluent consisting of a 0.2 mol / L dilute hydrochloric acid solution and a 0.5 mol / L sodium chloride solution to elute the mineral ions from the adsorbent material while avoiding damage to the adsorbent material. After the mineral ions are eluted, they are transferred to a membrane filtration device with a solution volume of 4 L and a total amount of 40 g of adsorbed mineral ions. Residual organic matter and impurities are removed to obtain a high-purity mineral solution.

[0057] Finally, nitrogen, phosphorus, potassium and trace elements including calcium, magnesium, iron and zinc are added to the high-purity mineral solution in a ratio of 15:15:15. The mixture is stirred and concentrated by evaporation at 70°C. Ordinary starch accounting for 3% of the total amount of the high-purity mineral solution is added as a binder. A granulator is used to make it into fertilizer granules with a particle size of 3 mm. Part of the fertilizer is extracted for quality monitoring, including nutrient analysis, particle strength test and solubility test. After passing the test, it is bagged and put into use.

[0058] 8L fermentation liquid, add 0.3g per liter, total amount = 8L × 0.3g / L = 2.4g;

[0059] The volume of the solution is 4L, and the total amount of mineral ions adsorbed is 40g;

[0060] Mineral solution concentration = 40g ÷ 4L = 10g / L.

[0061] Embodiment 3

[0062] First, prepare 12L crude valine fermentation broth, transfer it to a low-temperature fermentation sedimentation tank at 8°C, add microbial flora in a small amount and multiple additions, add 0.4g of microbial flora to every 1L of fermentation broth, first add a portion of the microbial flora to the fermentation broth, stir at a stirring rate of 135r / min for a period of time to make the microbial flora initially dispersed, and then add the next portion of the microbial flora. The total stirring time is 50min. After the stirring is completed, let it stand at a temperature of 9°C for 42h to precipitate. After the precipitation is completed, take out the supernatant in the crude valine fermentation broth and transfer it to a corrosion-resistant container for light protection;

[0063] Next, the supernatant was transferred to a magnetic stirring tank, the stirring speed was set at 110 r / min, the temperature was controlled at 28°C, and the magnetic stirring tank was ventilated at a ventilation rate of 0.4 m3 / min per liter of valine fermentation liquid. The microorganisms were allowed to grow naturally, and the chemical composition changes of the supernatant, including organic matter content, pH value and mineral concentration, were monitored. The organic matter content in the supernatant was detected by potassium dichromate method, the pH value in the supernatant was directly detected by pH meter, and the mineral concentration in the supernatant was detected by inductively coupled plasma emission spectrometry. The natural growth time of the microorganisms was 22 h.

[0064] Afterwards, the treated valine fermentation liquid is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected to adsorb mineral ions in the valine fermentation liquid according to the volume of the fermentation liquid and the content of minerals. During the adsorption process, the valine fermentation liquid is slowly stirred, the mass of the adsorption material is 35 g / L, and the adsorption time is 3 hours;

[0065] Then, the adsorbent material that has adsorbed the mineral ions is placed in an eluent consisting of a 0.4 mol / L dilute hydrochloric acid solution and a 0.8 mol / L sodium chloride solution to elute the mineral ions from the adsorbent material while avoiding damage to the adsorbent material. After the mineral ions are eluted, they are transferred to a membrane filtration device. After elution, the volume of the mineral solution is 6 L, and the total amount of adsorbed mineral ions is 60 g. Residual organic matter and impurities are removed to obtain a high-purity mineral solution.

[0066] Finally, nitrogen, phosphorus, potassium and trace elements including calcium, magnesium, iron and zinc are added to the high-purity mineral solution in a ratio of 15:15:15. The mixture is stirred and concentrated by evaporation at 75°C. Ordinary starch accounting for 3% of the total amount of the high-purity mineral solution is added as a binder. A granulator is used to make it into fertilizer granules with a particle size of 3 mm. Part of the fertilizer is extracted for quality monitoring, including nutrient analysis, particle strength test and solubility test. After passing the test, it is bagged and put into use.

[0067] 12L fermentation liquid, add 0.4g per liter, total amount = 12L × 0.4g / L = 4.8g;

[0068] The volume of the mineral solution after elution was 6 L, and the total amount of adsorbed mineral ions was 60 g;

[0069] Mineral solution concentration = 60g ÷ 6L = 10g / L.

[0070] Embodiment 4:

[0071] First, 9L of crude valine fermentation broth was prepared, and it was transferred to a low-temperature fermentation sedimentation tank at 6°C. Microbial flora was added in a small amount and multiple additions. 0.25g of microbial flora was added to every 1L of fermentation broth. A portion of the microbial flora was first added to the fermentation broth, and stirred at a stirring rate of 110r / min for a period of time to make the microbial flora initially dispersed, and then the next portion of the microbial flora was added. The total stirring time was 45min. After the stirring was completed, it was allowed to stand at a temperature of 8°C for 38h. After the precipitation was completed, the supernatant in the crude valine fermentation broth was taken out and transferred to a corrosion-resistant container for light protection;

[0072] Next, the supernatant was transferred to a magnetic stirring tank, the stirring speed was set at 100 r / min, the temperature was controlled at 26°C, and the magnetic stirring tank was ventilated at a ventilation rate of 0.35 m3 / min per liter of valine fermentation liquid. The microorganisms were allowed to grow naturally, and the chemical composition changes of the supernatant, including organic matter content, pH value and mineral concentration, were monitored. The organic matter content in the supernatant was detected by potassium dichromate method, the pH value in the supernatant was directly detected by pH meter, and the mineral concentration in the supernatant was detected by inductively coupled plasma emission spectrometry. The natural growth time of the microorganisms was 21 h.

[0073] Afterwards, the treated valine fermentation liquid is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected to adsorb mineral ions in the valine fermentation liquid according to the volume of the fermentation liquid and the content of minerals. During the adsorption process, the valine fermentation liquid is slowly stirred, the mass of the adsorption material is 30 g / L, and the adsorption time is 3 hours;

[0074] Then, the adsorbent material that has adsorbed the mineral ions is placed in an eluent consisting of a 0.3 mol / L dilute hydrochloric acid solution and a 0.7 mol / L sodium chloride solution to elute the mineral ions from the adsorbent material while avoiding damage to the adsorbent material. After the mineral ions are eluted, the volume of the eluted mineral solution is 4.5 L, and the total amount of adsorbed mineral ions is 45 g. The solution is transferred to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution.

[0075] Finally, nitrogen, phosphorus, potassium and trace elements including calcium, magnesium, iron and zinc are added to the high-purity mineral solution in a ratio of 15:15:15. The mixture is stirred and concentrated by evaporation at 70°C. Ordinary starch accounting for 3% of the total amount of the high-purity mineral solution is added as a binder. A granulator is used to make it into fertilizer granules with a particle size of 3 mm. Part of the fertilizer is extracted for quality monitoring, including nutrient analysis, particle strength test and solubility test. After passing the test, it is bagged and put into use.

[0076] 9L fermentation liquid, add 0.25g per liter, total amount = 9L × 0.25g / L = 2.25g;

[0077] The volume of the mineral solution after elution was 4.5 L, and the total amount of adsorbed mineral ions was 45 g;

[0078] Mineral solution concentration = 45g ÷ 4.5L = 10g / L.

[0079] Embodiment 5

[0080] First, 15L of crude valine fermentation broth was prepared, and it was transferred to a low-temperature fermentation sedimentation tank at 7°C. Microbial flora was added in a small amount and multiple additions. 0.45g of microbial flora was added to every 1L of fermentation broth. A portion of the microbial flora was first added to the fermentation broth, and stirred at a stirring rate of 115r / min for a period of time to make the microbial flora initially dispersed, and then the next portion of the microbial flora was added. The total stirring time was 55min. After the stirring was completed, it was allowed to stand at a temperature of 8°C for 45h. After the precipitation was completed, the supernatant in the crude valine fermentation broth was taken out and transferred to a corrosion-resistant container for light protection.

[0081] Next, the supernatant was transferred to a magnetic stirring tank, the stirring speed was set at 110 r / min, the temperature was controlled at 28°C, and the magnetic stirring tank was ventilated at a ventilation rate of 0.3 m3 / min per liter of valine fermentation liquid. The microorganisms were allowed to grow naturally, and the chemical composition changes of the supernatant, including the organic matter content, pH value and mineral concentration, were monitored. The organic matter content in the supernatant was detected by the potassium dichromate method, the pH value in the supernatant was directly detected by a pH meter, and the mineral concentration in the supernatant was detected by inductively coupled plasma emission spectrometry. The natural growth time of the microorganisms was 20 h.

[0082] Afterwards, the treated valine fermentation liquid was transferred to an extraction tank. According to the volume of the fermentation liquid and the content of minerals, ion exchange resin, zeolite and activated carbon were selected to adsorb the mineral ions in the valine fermentation liquid. During the adsorption process, the valine fermentation liquid was slowly stirred. The mass of the adsorption material was 40 g / L and the adsorption time was 3.5 h.

[0083] Then, the adsorbent material that has adsorbed the mineral ions is placed in an eluent consisting of a 0.4 mol / L dilute hydrochloric acid solution and a 0.9 mol / L sodium chloride solution to elute the mineral ions from the adsorbent material while avoiding damage to the adsorbent material. After the mineral ions are eluted, they are transferred to a membrane filtration device. After elution, the volume of the mineral solution is 7.5 L, and the total amount of adsorbed mineral ions is 75 g. Residual organic matter and impurities are removed to obtain a high-purity mineral solution.

[0084] Finally, nitrogen, phosphorus, potassium and trace elements including calcium, magnesium, iron and zinc are added to the high-purity mineral solution in a ratio of 15:15:15. The mixture is stirred and concentrated by evaporation at 75°C. Ordinary starch accounting for 3.5% of the total amount of the high-purity mineral solution is added as a binder. A granulator is used to make it into fertilizer granules with a particle size of 3 mm. Part of the fertilizer is extracted for quality monitoring, including nutrient analysis, particle strength test and solubility test. After passing the test, it is bagged and put into use.

[0085] 15L fermentation liquid, add 0.45g per liter, total amount = 15L × 0.45g / L = 6.75g;

[0086] The volume of the mineral solution after elution was 7.5 L, and the total amount of adsorbed mineral ions was 75 g;

[0087] Mineral solution concentration = 75g ÷ 7.5L = 10g / L.

[0088] Fertilizer finished product quality inspection,

[0089] Nutritional analysis:

[0090] Methods: Chemical analysis and atomic absorption spectrometry were used to determine the content of trace elements;

[0091] Nitrogen content was determined by Kjeldahl method;

[0092] Phosphorus and potassium contents were determined by spectrophotometry.

[0093] It was detected that the ratio of nitrogen, phosphorus and potassium in the finished fertilizers prepared in the above five groups of embodiments was in accordance with 15:15:15, and the contents of trace elements such as calcium, magnesium, iron and zinc were within a certain range.

[0094] Particle strength test:

[0095] Method: Use a particle strength tester to apply pressure to a certain number of fertilizer particles until the particles break, and record the pressure value when they break.

[0096] Solubility test:

[0097] Method: Take a certain amount of fertilizer particles and put them into water, stir them at 27℃ for 30 minutes, then determine the content of nutrients in the solution and calculate the solubility.

[0098] The particle strength calculation results are as follows:

[0099] Embodiment 1

[0100] 100 fertilizer particles were tested, and the total pressure value was 500N;

[0101] Average particle strength = 500N / 100 = 5N.

[0102] Embodiment 2

[0103] The total pressure value is 450N;

[0104] Average particle strength = 450N / 100 = 4.5N.

[0105] Embodiment 3

[0106] The total pressure value is 550N;

[0107] Average particle strength = 550N / 100 = 5.5N.

[0108] Embodiment 4:

[0109] The total pressure value is 480N;

[0110] Average particle strength = 480N / 100 = 4.8N.

[0111] Embodiment 5

[0112] The total pressure value is 600N;

[0113] Average particle strength = 600N / 100 = 6N.

[0114] The solubility test results are as follows:

[0115] Embodiment 1

[0116] Take 100g of fertilizer granules and put them into water, and stir them at 27℃ for 30min;

[0117] Determine the content of nutrients in the solution, the total amount of dissolved nutrients is 30g;

[0118] Solubility = 30g / 100g x 100% = 30%.

[0119] Embodiment 2

[0120] Take 90g of fertilizer granules and test them under the same conditions. The total amount of dissolved nutrients is 27g;

[0121] Solubility = 27g / 90g x 100% = 30%.

[0122] Embodiment 3

[0123] Take 110g of fertilizer granules, the total amount of dissolved nutrients is 33g;

[0124] Solubility = 33g / 110g x 100% = 30%.

[0125] Embodiment 4:

[0126] Take 95g of fertilizer granules, the total amount of dissolved nutrients is 28.5g;

[0127] Solubility = 28.5 g / 95 g x 100% = 30%.

[0128] Embodiment 5

[0129] Take 120g of fertilizer granules, the total amount of dissolved nutrients is 36g;

[0130] Solubility = 36 g / 120 g x 100% = 30%.

[0131] In summary, the feasibility and effectiveness of extracting minerals from valine fermentation broth to prepare fertilizers in the five embodiments of the present invention have important practical significance and application value.

[0132] The embodiments of the present invention are described in detail above with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. For those skilled in the art, various changes, modifications, substitutions and variations of these embodiments are made without departing from the principles and spirit of the present invention, and still fall within the scope of protection of the present invention.

[0133] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0134] The above contents are merely examples and explanations of the present invention. Various modifications or additions to the specific embodiments described or replacements in similar ways by technicians in the technical field shall fall within the protection scope of the present invention as long as they do not deviate from the invention or exceed the scope defined by the claims.

[0135] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for extracting minerals from valine fermentation broth to prepare fertilizer, comprising pretreatment of the valine fermentation broth, mineral extraction and purification, nutrient preparation and biostimulation, wherein the biostimulation comprises low-temperature fermentation precipitation and magnetic stirring, and is characterized in that: The specific operation steps of extracting minerals from the valine fermentation liquid to prepare fertilizer are as follows: Step 1: transfer the crude valine fermentation broth into a low-temperature fermentation sedimentation tank, add microbial flora and stir, take the supernatant after precipitation, and transfer it into a corrosion-resistant container for standby use; Step 2: transferring the supernatant of the valine fermentation broth into a magnetic stirring tank, using magnetic stirring and ventilation, waiting for the natural growth of microorganisms, and monitoring the growth state of the microorganisms and the changes in the chemical composition of the supernatant to obtain the valine fermentation broth; Step 3: transferring the treated valine fermentation liquid into an extraction tank, and using ion exchange resin and adsorption material to adsorb mineral ions in the valine fermentation liquid; Step 4: placing the adsorbent material with mineral ions into an eluent, and after the minerals are eluted, transferring it to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution; Step 5: Add nitrogen, phosphorus, potassium and trace elements to the mineral solution, stir and mix, evaporate and concentrate, add adhesive to the concentrate, use a granulator to make it into fertilizer granules, extract part of the fertilizer for quality monitoring, and bag it for use after passing the quality control.

2. A method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 1, the crude valine fermentation broth is transferred to a low-temperature fermentation sedimentation tank at 2°C-10°C, the screened microbial flora is added, and the broth is stirred at a stirring rate of 120r / min-140r / min for 30min-60min. After the stirring is completed, the broth is allowed to stand at a temperature of 5°C-10°C for 24h-48h.

3. A method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 1, after the precipitation is completed, the supernatant in the crude valine fermentation broth is taken out and transferred into a corrosion-resistant container for light protection. The amount of microbial flora added is determined according to the total volume of the crude valine fermentation broth, and each 1L of fermentation broth contains 0.1g-0.5g of microbial flora.

4. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In step 2, the treated supernatant is transferred to a magnetic stirring tank, the stirring speed is set to 90 r / min-120 r / min, the temperature is controlled between 25°C and 30°C, and the magnetic stirring tank is ventilated at a ventilation rate of 0.1 m / L of valine fermentation liquid. 3 / min-0.5m 3 / min, and monitor the changes in the chemical composition of the supernatant during fermentation, including organic matter content, pH and mineral concentration. The natural growth time of microorganisms is 18h-24h.

5. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step three, the treated valine fermentation broth is transferred to an extraction tank, and ion exchange resin, zeolite and activated carbon are selected according to the volume of the fermentation broth and the content of minerals to adsorb the mineral ions in the valine fermentation broth. During the adsorption process, the valine fermentation broth is slowly stirred, the adsorption time is 2h-4h, and the mass of the adsorption material is 10g / L-50g / L, and the specific mass needs to be adjusted according to the performance of the adsorption material and the characteristics of the valine fermentation broth.

6. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 4, the adsorption material that has adsorbed mineral ions is placed in an eluent to elute the mineral ions from the adsorption material while avoiding damage to the adsorption material. After the mineral ions are eluted, they are transferred to a membrane filtration device to remove residual organic matter and impurities to obtain a high-purity mineral solution.

7. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 4, the eluent includes a dilute acid solution and a salt solution, wherein the concentration of the dilute acid solution is 0.1 mol / L-0.5 mol / L, and the concentration of the salt solution is 0.2 mol / L-1 mol / L.

8. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 5, nitrogen, phosphorus, potassium and trace elements are added to the high-purity mineral solution, the ratio of nitrogen, phosphorus and potassium is 15:15:15, and the trace elements include calcium, magnesium, iron, zinc and other salt compounds. After adding nitrogen, phosphorus, potassium and trace elements according to the ratio, stirring and mixing are carried out for evaporation and concentration. The concentration temperature is controlled at 50° C.-80° C., and a binder is added during concentration. The amount of the binder added is 2%-4% of the total amount of the high-purity mineral solution.

9. The method for extracting minerals from valine fermentation liquid to prepare fertilizer according to claim 1, characterized in that: In the step 5, after the evaporation and concentration is completed, a granulator is used to make fertilizer granules with a particle size of 2mm-4mm. After the granulation is completed, the fertilizer granules are extracted for quality inspection, including nutrient analysis, particle strength test and solubility test. After passing the inspection, they are bagged and put into use.

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