New process for producing high-quality liquid fertilizer from acetylisovaleryltylosin tartrate finished product liquid

Abstract

The invention discloses a novel process for producing a high-quality liquid fertilizer by using an acetylisovaleryltylosin tartrate finished product liquid, and relates to the technical field of fertilizer preparation, and the novel process comprises the following specific steps: step 1, firstly, weighing polyoxyethylene sorbitan fatty acid ester, ethylenediamine tetraacetic acid disodium salt, cellulase and protease, and uniformly stirring; the preparation method has the advantages that the polylactic acid-glycolic acid copolymer serving as a functional high-molecular polymer has good biocompatibility and controlled release performance, and when a solution prepared from the polylactic acid-glycolic acid copolymer is emulsified and mixed with an alginate oligosaccharide solution, a uniform emulsion-like active synergistic carrier solution is formed; the emulsifying and mixing process enables the effective components in the two solutions to be fully and uniformly combined together to form a stable microsphere and micelle structure, so that the continuous and slow release of the acetylisovaleryltylosin tartrate and the synergistic plant growth regulatory factors thereof in the growth cycle of crops can be ensured, the fertilizer effect of the acetylisovaleryltylosin tartrate and the synergistic plant growth regulatory factors thereof can be fully exerted, and the crop quality is improved. Therefore, the problem that the fertilizer efficiency is not obvious in the prior art is effectively solved.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a new process for producing high-quality liquid fertilizer from tyvalocin finished product liquid. Background Art

[0002] Tylvalosin is a veterinary antibiotic widely used in the field of animal husbandry. It is mainly used to prevent and treat various diseases of livestock and poultry. It plays an important role in ensuring the health of livestock and poultry and promoting the development of animal husbandry. Its production process usually produces Tylvalosin finished liquid. However, the main application of Tylvalosin finished liquid is still limited to the veterinary field. With the increasing demand for comprehensive resource utilization and innovative fertilizer research and development in agricultural production, exploring new application methods of Tylvalosin finished liquid in the agricultural field has important practical significance. On the one hand, applying Tylvalosin finished liquid to liquid fertilizer production is expected to achieve resource recycling of this substance originally used in the field of animal husbandry, expand its application scope, and improve the overall utilization efficiency of resources. On the other hand, some characteristics of Tylvalosin itself may, after reasonable process transformation, give liquid fertilizer unique advantages, such as having a positive impact on the growth environment of crops and promoting the activities of beneficial microorganisms in the soil. The existing technology has certain defects. The first is the impurity problem. The industrially produced tyvalocin finished product is often mixed with insoluble impurities, resulting in poor water solubility, affecting the bioavailability of the product, and limiting its application in the large-scale preparation of liquid fertilizers. Secondly, the fertilizer efficiency problem. The existing process of using tyvalocin finished product liquid to produce liquid fertilizer cannot give full play to the fertilizer effect of the effective ingredients in the tyvalocin finished product liquid, resulting in the fertilizer The effect of promoting the growth of crops is not significant enough and cannot meet the demand for high-efficiency fertilizers in agricultural production. The third is the stability problem. The liquid fertilizer produced by the existing technology may have insufficient stability during storage and use, making the effective ingredients easy to decompose, precipitate or deteriorate, thereby affecting the quality and use effect of the fertilizer and reducing its competitiveness in the market. To this end, we propose a new process for producing high-quality liquid fertilizers from tyvalocin finished liquid. Summary of the invention

[0003] The purpose of the present invention is to provide a new process for producing high-quality liquid fertilizer from tyvalocin finished product liquid.

[0004] In order to solve the problems raised in the above background technology, the present invention provides the following technical solutions: a new process for producing high-quality liquid fertilizer from tyvalocin finished liquid, the new process for producing high-quality liquid fertilizer comprising the following specific steps: Step 1, first, weighing polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease, then weighing phosphate buffer according to the content of polyoxyethylene sorbitan fatty acid ester, putting the weighed polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease into the phosphate buffer and stirring to react to prepare a composite reagent, weighing the industrially produced tyvalosin finished liquid and placing it in a stainless steel reaction container, then adding the prepared composite reagent into the reaction container and stirring to react, filtering through a microporous membrane filter after the reaction is completed to obtain a tyvalosin treated liquid with significantly reduced impurity content and good water solubility; Step 2, weighing alginate oligosaccharides, preparing it into alginate oligosaccharide solution, taking polylactic acid-glycolic acid copolymer, preparing it into polylactic acid-glycolic acid copolymer solution, then mixing the alginate oligosaccharide solution with the polylactic acid-glycolic acid copolymer solution, placing it in a high-speed emulsification equipment for emulsification and mixing, forming a uniform emulsion-like active synergistic carrier solution, then weighing the tyvalosin treatment solution, adding the prepared active synergistic carrier solution to the tyvalosin treatment solution for stirring reaction, so that the effective ingredients in the tyvalosin treatment solution are encapsulated in the microsphere and micelle structure to achieve synergistic improvement of fertilizer efficiency, and completing the mixing of the tyvalosin treatment solution and the active synergistic carrier solution; Step 3, weighing silica nanoparticles, dissolving them in an ethanol solution to prepare a nanoparticle dispersion, then stirring and mixing them evenly, weighing polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane to obtain a mixture, and then placing the mixture in an ethanol solution and stirring and mixing to prepare a modification solution; The nanoparticle dispersion liquid and the modification liquid are mixed and stirred evenly, so that the polyethylene glycol segment and the amine group are successfully grafted onto the surface of the silica nanoparticles to form a stable system liquid, and the mixed liquid of the tyvalosin treatment liquid and the active synergistic carrier solution and the stable system liquid are stirred and mixed, so that the effective ingredients of the tyvalosin mixed liquid are specifically combined with the amine groups on the surface of the nanomaterial stable system, and adsorbed on the surface of the silica nanoparticles to improve stability, thereby completing the mixing operation of the tyvalosin mixed liquid and the nanomaterial stable system, and obtaining the tyvalosin-silicon nano composite stable fertilizer liquid precursor; Step 4: Collect the prepared tyvalosin-silicon nanocomposite stable fertilizer liquid precursor, add urea as a nitrogen source, potassium dihydrogen phosphate as a phosphorus source and potassium source, add boric acid, zinc sulfate and iron sulfate as trace elements to the composite stable fertilizer liquid precursor and stir evenly to ensure that all components are fully mixed to obtain liquid fertilizer.

[0005] As a further scheme of the present invention: in the step 1, polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are weighed in a mass ratio of 1:0.5-0.7:0.1-0.3:0.1-0.3, the pH value of the selected phosphate buffer is 7.0-7.4, and the weighed amount of the phosphate buffer is 10mL-16mL per gram of polyoxyethylene sorbitan fatty acid ester. The weighed polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are put into the phosphate buffer and stirred and mixed, the reaction temperature is controlled to 25°C-35°C, and the reaction is stirred at a stirring speed of 120r / min-180r / min for 25min-35min.

[0006] As a further solution of the present invention: in the step 1, the industrially produced tylvalosin finished product placed in the stainless steel reaction container is 10L-13L, the amount of the composite reagent added is 10g-20g per liter of tylvalosin finished product liquid, the reaction temperature is controlled to be 30°C-40°C, the stirring speed is 300r / min-500r / min, the stirring reaction is continued for 2h-3h, and the pore size of the microporous membrane filter for filtration is 0.2μm-0.3μm.

[0007] As a further scheme of the present invention: in the step 2, alginate oligosaccharides are weighed and prepared into an alginate oligosaccharide solution with a concentration of 8%-12%, polylactic acid-glycolic acid copolymer is taken and prepared into a polylactic acid-glycolic acid copolymer solution with a concentration of 8%-12%, the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution are mixed in a volume ratio of 5-7:3-5, the emulsification speed in the emulsification equipment is 800r / min-1200r / min, and the emulsification time is 10min-20min.

[0008] As a further solution of the present invention: in the step 2, the weighed tyvalocin treatment liquid is 10L-13L, the added amount of the active synergistic carrier solution is 200mL-300mL per liter of tyvalocin treatment liquid, and the active synergistic carrier solution is added for stirring reaction at a stirring speed of 120r / min-180r / min in an environment of 35°C-45°C for 1h-2h.

[0009] As a further scheme of the present invention: in the step three, weigh silica nanoparticles, dissolve 0.8g-1.2g of silica nanoparticles in every 100ml of ethanol solution to prepare a nanoparticle dispersion with a concentration of 0.8%-1.2%, stir for 25min-35min in an environment of 35℃-45℃ at a stirring speed of 180r / min-220r / min, the mixture is polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane mixed in a mass ratio of 2-3:1, the weighed amount of ethanol solution is 8mL-12mL per gram of the mixture, and stir at room temperature at a stirring speed of 250r / min-350r / min until completely dissolved to prepare a modification solution.

[0010] As a further solution of the present invention: in the step three, the mixing ratio of the nanoparticle dispersion and the modification solution is 0.7-1.2:1, and the reaction is stirred at 65°C-75°C for 2h-3h at a stirring speed of 350r / min-450r / min.

[0011] As a further solution of the present invention: in the step three, the weighed mixed solution of the tyvalosin treatment solution and the active synergistic carrier solution is 7L-10L, the added amount of the stabilizing system liquid is 60g-100g per liter of the mixed solution, and the reaction is stirred at 25°C-35°C and a stirring speed of 200r / min-300r / min for 1h-2h.

[0012] As a further scheme of the present invention: in the step 4, the amount of urea added as the nitrogen source is 40g-60g, the amount of potassium dihydrogen phosphate added as the phosphorus source and potassium source is 25g-35g, the amount of boric acid added is 4g-6g, the amount of zinc sulfate added is 2g-4g, and the amount of iron sulfate added is 1g-3g. During the addition process, the mixture is stirred evenly at a stirring speed of 180r / min-220r / min at room temperature.

[0013] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are: 1. In the present invention, alginate oligosaccharides are added to the preparation of the tyvalosin active synergistic carrier solution. The alginate oligosaccharides are rich in various plant growth regulatory factors, can promote plant cell division, enhance plant stress resistance, etc. After being prepared into a solution, it lays a foundation for subsequent mixing with the tyvalosin treatment solution, and can synergistically improve the nourishing effect on crops. The polylactic acid-glycolic acid copolymer is a functional high molecular polymer with good biocompatibility and controlled release performance. When the solution prepared by the alginate oligosaccharide solution is emulsified and mixed with the alginate oligosaccharide solution through a high-speed emulsification device, a uniform emulsion-like active synergistic carrier solution is formed. This emulsification mixing process makes the effective The components are fully and evenly combined to form a stable microsphere or micelle structure. When the active synergistic carrier solution is mixed with the tylvalosin treatment solution, on the one hand, the plant growth regulators carried by the alginate oligosaccharide and the effective ingredients in the tylvalosin treatment solution synergize with each other, which can enhance the beneficial effects of tylvalosin on the root microbial community of crops and promote better nutrient absorption by crops. On the other hand, the controlled release performance of PLGA is reflected, which can ensure that tylvalosin and its synergistic plant growth regulators are continuously and slowly released during the growth cycle of crops, giving full play to their fertilizer effect, thereby effectively solving the problem of insignificant fertilizer effect in the existing process. 2. The present invention adds silica nanoparticles as a basic material during the preparation of the tyvalosin-nanomaterial stabilization system. The silica nanoparticles have the characteristics of high specific surface area, good chemical stability and biocompatibility, providing a stable support structure for the entire stabilization system. The polyethylene glycol (PEG) chain segment is grafted onto the surface of the silica nanoparticles through surface modification technology, giving the system excellent hydrophilicity, which enables the entire tyvalosin-nanomaterial stabilization system to maintain good water dispersibility during storage and use, effectively preventing the aggregation or precipitation of the active ingredients caused by uneven water distribution, and ensuring the stability of the system. The amine groups grafted on the surface of the silica nanoparticles can specifically bind to the effective ingredients of the tyvalosin finished liquid mixture. This specific binding allows the effective ingredients of the tyvalosin mixture to be firmly adsorbed on the surface of the silica nanoparticles, thereby enhancing the stability of the effective ingredients in the system. When the tyvalosin-nanomaterial stabilization system is mixed with the tyvalosin mixture, the decomposition, precipitation or deterioration of tyvalosin and other effective ingredients during storage and use can be prevented, which not only greatly improves the stability of the produced liquid fertilizer, but also ensures the long-term effectiveness and reliability of the liquid fertilizer in agricultural production applications. 3. The present invention adopts polyoxyethylene sorbitan fatty acid ester (Tween-80) as a surfactant. With its amphiphilic structure, the insoluble impurities in the tyvalosin finished liquid are emulsified and dispersed, and the impurities originally agglomerated together are changed into tiny particles suspended in the solution, thereby effectively improving the water solubility of the finished liquid and solving the problem of poor water solubility caused by impurities. By using disodium salt of ethylenediaminetetraacetic acid (EDTA) as a chelating agent, it can quickly and accurately form a stable complex with common metal ion impurities in the finished liquid, so that these metal ion impurities are converted from the state that may affect the properties of the solution and subsequent reactions to a complex form soluble in water, further improving the purity of the solution. The two biological enzymes, cellulase and protease, can specifically decompose the organic impurity macromolecules that may exist in the tyvalosin finished liquid, convert them into small molecule soluble substances, significantly reduce the impurity content in the finished liquid, and create excellent conditions for the tyvalosin finished liquid to better participate in the subsequent liquid fertilizer preparation process. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Schematic diagram of the process steps in the embodiment of the present invention. DETAILED DESCRIPTION

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

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

[0017] Please see attached Figure 1 The present invention discloses a new process for producing high-quality liquid fertilizer from tyvalocin finished product liquid, and the new process for producing high-quality liquid fertilizer comprises the following specific steps: Step 1, first, weighing polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease, then weighing phosphate buffer according to the content of polyoxyethylene sorbitan fatty acid ester, putting the weighed polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease into the phosphate buffer and stirring to react to prepare a composite reagent, weighing the industrially produced tyvalosin finished liquid and placing it in a stainless steel reaction container, then adding the prepared composite reagent into the reaction container and stirring to react, filtering through a microporous membrane filter after the reaction is completed to obtain a tyvalosin treated liquid with significantly reduced impurity content and good water solubility; Step 2, weighing alginate oligosaccharides, preparing it into alginate oligosaccharide solution, taking polylactic acid-glycolic acid copolymer, preparing it into polylactic acid-glycolic acid copolymer solution, then mixing the alginate oligosaccharide solution with the polylactic acid-glycolic acid copolymer solution, placing it in a high-speed emulsification equipment for emulsification and mixing, forming a uniform emulsion-like active synergistic carrier solution, then weighing the tyvalosin treatment solution, adding the prepared active synergistic carrier solution to the tyvalosin treatment solution for stirring reaction, so that the effective ingredients in the tyvalosin treatment solution are encapsulated in the microsphere and micelle structure to achieve synergistic improvement of fertilizer efficiency, and completing the mixing of the tyvalosin treatment solution and the active synergistic carrier solution; Step 3, weighing silica nanoparticles, dissolving them in an ethanol solution to prepare a nanoparticle dispersion, then stirring and mixing them evenly, weighing polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane to obtain a mixture, and then placing the mixture in an ethanol solution and stirring and mixing to prepare a modification solution; The nanoparticle dispersion liquid and the modification liquid are mixed and stirred evenly, so that the polyethylene glycol segment and the amine group are successfully grafted onto the surface of the silica nanoparticles to form a stable system liquid, and the mixed liquid of the tyvalosin treatment liquid and the active synergistic carrier solution and the stable system liquid are stirred and mixed, so that the effective ingredients of the tyvalosin mixed liquid are specifically combined with the amine groups on the surface of the nanomaterial stable system, and adsorbed on the surface of the silica nanoparticles to improve stability, thereby completing the mixing operation of the tyvalosin mixed liquid and the nanomaterial stable system, and obtaining the tyvalosin-silicon nano composite stable fertilizer liquid precursor; Step 4: Collect the prepared tyvalosin-silicon nanocomposite stable fertilizer liquid precursor, add urea as a nitrogen source, potassium dihydrogen phosphate as a phosphorus source and potassium source, add boric acid, zinc sulfate and iron sulfate as trace elements to the composite stable fertilizer liquid precursor and stir evenly to ensure that all components are fully mixed to obtain liquid fertilizer.

[0018] In one embodiment of the present invention: in step 1, polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are weighed in a mass ratio of 1:0.5-0.7:0.1-0.3:0.1-0.3, the selected phosphate buffer has a pH value of 7.0-7.4, and the weighed amount of phosphate buffer is 10mL-16mL per gram of polyoxyethylene sorbitan fatty acid ester. The weighed polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are placed in the phosphate buffer and stirred and mixed, the reaction temperature is controlled to 25°C-35°C, and the reaction is stirred at a stirring speed of 120r / min-180r / min for 25min-35min.

[0019] In one embodiment of the present invention: in step 1, the industrially produced tylvalosin finished product placed in a stainless steel reaction container is 10L-13L, the amount of the composite reagent added is 10g-20g per liter of tylvalosin finished product liquid, the reaction temperature is controlled to be 30°C-40°C, the stirring speed is 300r / min-500r / min, the stirring reaction is continued for 2h-3h, and the pore size of the microporous membrane filter for filtration is 0.2μm-0.3μm.

[0020] In one embodiment of the present invention: in step 2, alginate oligosaccharides are weighed and prepared into an alginate oligosaccharide solution with a concentration of 8%-12%, polylactic acid-glycolic acid copolymer is taken and prepared into a polylactic acid-glycolic acid copolymer solution with a concentration of 8%-12%, the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution are mixed in a volume ratio of 5-7:3-5, the emulsification speed in the emulsification equipment is 800r / min-1200r / min, and the emulsification time is 10min-20min.

[0021] In one embodiment of the present invention: in step 2, the weighed tyvalocin treatment liquid is 10L-13L, the added amount of the active synergistic carrier solution is 200mL-300mL per liter of tyvalocin treatment liquid, and the active synergistic carrier solution is added for stirring reaction at a stirring speed of 120r / min-180r / min in an environment of 35°C-45°C for 1h-2h.

[0022] In one embodiment of the present invention: in step three, weigh silica nanoparticles, dissolve 0.8g-1.2g of silica nanoparticles in every 100ml of ethanol solution to prepare a nanoparticle dispersion with a concentration of 0.8%-1.2%, stir for 25min-35min in an environment of 35℃-45℃ at a stirring speed of 180r / min-220r / min, the mixture is polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane in a mass ratio of 2-3:1, the weighed amount of ethanol solution is 8mL-12mL per gram of the mixture, and stir at room temperature at a stirring speed of 250r / min-350r / min until completely dissolved to prepare a modification solution.

[0023] In one embodiment of the present invention: in step three, the mixing ratio of the nanoparticle dispersion and the modification solution is 0.7-1.2:1, and the reaction is stirred at 65°C-75°C at a stirring speed of 350r / min-450r / min for 2h-3h.

[0024] In one embodiment of the present invention: in step three, the weighed mixed solution of the tyvalosin treatment solution and the active synergistic carrier solution is 7L-10L, the added amount of the stabilizing system liquid is 60g-100g per liter of the mixed solution, and the reaction is stirred at 25°C-35°C and a stirring speed of 200r / min-300r / min for 1h-2h.

[0025] In one embodiment of the present invention: in step 4, the amount of urea added as a nitrogen source is 40g-60g, the amount of potassium dihydrogen phosphate added as a phosphorus source and a potassium source is 25g-35g, the amount of boric acid added is 4g-6g, the amount of zinc sulfate added is 2g-4g, and the amount of iron sulfate added is 1g-3g. During the addition process, the mixture is stirred evenly at a stirring speed of 180r / min-220r / min at room temperature.

[0026] In one embodiment of the present invention: in step 1, in the process of adding the weighed polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease into a phosphate buffer for stirring and reacting to prepare a composite reagent, a bioactivity promoter is added, the bioactivity promoter is nano-scale metal oxide particles, and the content thereof is 0.5-1.5 grams of nano-scale metal oxide particles per 100 grams of polyoxyethylene sorbitan fatty acid ester. The nano-scale metal oxide particles can enhance the activity of the enzyme and the synergistic effect between the reagents by changing the microenvironment of the reaction system, so that the removal and solubilization effect of the composite reagent on impurities in the tyvalocin finished liquid is further improved.

[0027] In one embodiment of the present invention: in step 2, when the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution are emulsified and mixed to form a uniform emulsion-like active synergistic carrier solution, a degradable polymer microsphere is introduced into the emulsified mixed system, the particle size of the microsphere is 10μm-50μm, and the addition amount is 5g-10g per 100 ml of the mixed solution. The surface of the degradable polymer microsphere has special functional groups, which can specifically adsorb the effective ingredients in the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution, and promote the effective ingredients to be more tightly combined on the surface of the microsphere during the emulsification process to form a composite microsphere with a "core-shell" structure. When the composite microsphere is subsequently mixed and stirred with the tyvalocin treatment solution, it can achieve a slow release of the effective ingredients and prolong the fertilizer effect time, thereby further improving the nourishing effect on crops.

[0028] In one embodiment of the present invention: in step three, in the process of mixing and stirring the nanoparticle dispersion and the modification liquid to form a stable system liquid, an ultrasonic-assisted processing technology is used, and the frequency of the ultrasonic wave is set to 20kHz-50kHz, and the power is 100W-300W. Under the action of the ultrasonic wave, the polyethylene glycol segments and the amine groups can be grafted onto the surface of the silica nanoparticles more quickly and evenly, thereby reducing the agglomeration phenomenon during the grafting process and improving the uniformity and stability of the stable system liquid.

[0029] In one embodiment of the present invention: In step 4, in the process of adding urea, potassium dihydrogen phosphate, boric acid, zinc sulfate, ferric sulfate and other fertilizer components to the tyvalocin-silicon composite stable fertilizer liquid precursor and stirring evenly, a plant-derived natural moisturizer is added. The plant-derived natural moisturizer is a polysaccharide substance extracted from plants, and the added amount is 5g-10g per liter of the composite stable fertilizer liquid precursor. The plant-derived natural moisturizer can absorb and lock the moisture in the soil after the fertilizer is applied to the soil, forming a local moist microenvironment, which is conducive to the dissolution and diffusion of the fertilizer components and promotes the absorption of nutrients by the roots of crops.

[0030] Example 1, please refer to the attached Figure 1First, polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease were weighed in a mass ratio of 1:0.7:0.3:0.3, 16 mL of phosphate buffer (pH 7.4) was weighed per gram of polyoxyethylene sorbitan fatty acid ester, the weighed substances were placed in the phosphate buffer, the reaction temperature was controlled to be 35°C at a stirring speed of 180 r / min, and the reaction was stirred for 35 minutes to prepare a composite reagent, 13 L of industrially produced tyvalosin finished liquid was weighed and placed in a stainless steel reaction container, and then 20 g of the composite reagent was added per liter of tyvalosin finished liquid The prepared composite reagent was added to the reaction container in an amount of 1000 μg / min, the reaction temperature was controlled to be 40°C and the stirring speed was 500 r / min, and the stirring reaction was continued for 3 h. After the reaction was completed, it was filtered through a microporous membrane filter with a pore size of 0.3 μm to obtain a tyvalocin treatment solution with significantly reduced impurity content and good water solubility. Then, alginate oligosaccharides were weighed and prepared into a 12% alginate oligosaccharide solution, polylactic acid-glycolic acid copolymer was taken and prepared into a 12% polylactic acid-glycolic acid copolymer solution, the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution were mixed in a volume ratio of 7:5, and placed in an emulsifying converter. The mixture was emulsified in a high-speed emulsifying device at a speed of 1200 r / min for 20 min to form a uniform emulsion-like active synergistic carrier solution. Then, 13 L of tyvalosin treatment liquid was weighed, and the prepared active synergistic carrier solution was added to the tyvalosin treatment liquid at an amount of 300 mL of active synergistic carrier solution per liter of tyvalosin treatment liquid. The mixture was stirred at a stirring speed of 180 r / min in an environment of 45° C. for 2 h to encapsulate the active ingredients in the tyvalosin treatment liquid in the microsphere and micelle structure to achieve synergistic improvement of fertilizer efficiency, and the tyvalosin treatment liquid and the active synergistic carrier solution were mixed. Then, the silica nanoparticles were weighed. A nanoparticle dispersion with a concentration of 1.2% was prepared by dissolving 1.2 g of silica nanoparticles in every 100 ml of ethanol solution. The mixture was stirred at a stirring speed of 220 r / min in an environment of 45°C for 35 min to be uniformly stirred. Polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane were weighed and mixed in a mass ratio of 3:1 to obtain a mixture. An ethanol solution was weighed in an amount of 12 mL per gram of the mixture. The mixture was placed in the ethanol solution and stirred at a stirring speed of 350 r / min at room temperature until it was completely dissolved to prepare a modification solution. The nanoparticle dispersion and the modification solution were mixed at a ratio of 1.The mixture was stirred evenly at a mixing ratio of 2:1, and stirred at 75°C for 3 h at a stirring speed of 450 r / min to successfully graft the polyethylene glycol segments and amine groups to the surface of the silica nanoparticles to form a stable system liquid. 10 L of the mixture of the tyvalosin treatment liquid and the active synergistic carrier solution was weighed, and the stabilizing system liquid was added to the mixture at an amount of 100 g per liter of the mixture. The mixture was stirred at 35°C and a stirring speed of 300 r / min for 2 h to allow the active ingredients of the tyvalosin mixture to specifically bind to the amine groups on the surface of the nanomaterial stabilizing system. Combined, adsorbed on the surface of silica nanoparticles to improve stability, so that the mixing operation of the tyvalosin mixed solution and the nanomaterial stabilization system is completed, and the tyvalosin-silicon nanocomposite stable fertilizer liquid precursor is obtained. Finally, the obtained tyvalosin-silicon nanocomposite stable fertilizer liquid precursor is collected, and 60g urea as a nitrogen source, 35g potassium dihydrogen phosphate as a phosphorus source and potassium source, 6g boric acid, 4g zinc sulfate and 3g iron sulfate as trace elements are added thereto, and stirred evenly at room temperature at a stirring speed of 220r / min to ensure that all components are fully mixed to obtain liquid fertilizer. .

[0031] Example 2, please refer to the attached Figure 1First, step 1 is performed, polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are weighed in a mass ratio of 1:0.5:0.1:0.1, 10 mL of phosphate buffer (pH 7.0) is weighed per gram of polyoxyethylene sorbitan fatty acid ester, the weighed substances are placed in the phosphate buffer, the reaction temperature is controlled to be 25°C at a stirring speed of 120 r / min, and the reaction is stirred for 25 minutes to prepare a composite reagent, 10 L of industrially produced tyvalosin finished product liquid is weighed and placed in a stainless steel reaction container, and then 10 L of tyvalosin finished product liquid is added per liter. g of the composite reagent was added to the reaction container as the prepared composite reagent, the reaction temperature was controlled to be 30°C and the stirring speed was 300r / min, and the stirring reaction was continued for 2h. After the reaction was completed, it was filtered through a microporous membrane filter with a pore size of 0.2μm to obtain a tyvalosin treatment solution with significantly reduced impurity content and good water solubility. Then, alginate oligosaccharides were weighed and prepared into an alginate oligosaccharide solution with a concentration of 8%. Polylactic acid-glycolic acid copolymer was taken and prepared into a polylactic acid-glycolic acid copolymer solution with a concentration of 8%. The alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution were mixed at a volume ratio of 5:3 and placed in The emulsification was carried out in a high-speed emulsifying device at an emulsifying speed of 800 r / min for 10 minutes to form a uniform emulsion-like active synergistic carrier solution. Then, 10 L of the tyvalosin treatment liquid was weighed, and the prepared active synergistic carrier solution was added to the tyvalosin treatment liquid at an amount of 200 mL of the active synergistic carrier solution per liter of the tyvalosin treatment liquid. The reaction was stirred at a stirring speed of 120 r / min in an environment of 35° C. for 1 hour, so that the active ingredients in the tyvalosin treatment liquid were encapsulated in the microspheres and micelle structures to achieve synergistic improvement of fertilizer efficiency, and the tyvalosin treatment liquid and the active synergistic carrier solution were mixed. Then, the silica nanoparticles were weighed. 0.8 g of silica nanoparticles were dissolved in 100 ml of ethanol solution to prepare a nanoparticle dispersion with a concentration of 0.8%. The mixture was stirred at a stirring speed of 180 r / min in an environment of 35°C for 25 min to be uniformly stirred. Polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane were weighed and mixed in a mass ratio of 2:1 to obtain a mixture. 8 mL of ethanol solution was weighed per gram of the mixture. The mixture was placed in the ethanol solution and stirred at room temperature at a stirring speed of 250 r / min until it was completely dissolved to prepare a modification solution. The nanoparticle dispersion and the modification solution were mixed at a stirring speed of 0.The mixture was stirred evenly at a mixing ratio of 7:1, and stirred at 65°C for 2 hours at a stirring speed of 350 r / min to successfully graft the polyethylene glycol segments and amine groups to the surface of the silica nanoparticles to form a stable system liquid. 7L of the mixture of the tyvalosin treatment liquid and the active synergistic carrier solution was weighed, and the stable system liquid was added to the mixture at an amount of 60 g per liter of the mixture. The mixture was stirred at 25°C and a stirring speed of 200 r / min for 1 hour to allow the active ingredients of the tyvalosin mixture to specifically bind to the amine groups on the surface of the nanomaterial stable system. , adsorbed on the surface of silica nanoparticles to improve stability, thus completing the mixing operation of the tyvalosin mixed solution and the nanomaterial stabilization system, and obtaining the tyvalosin-silicon nanocomposite stable fertilizer liquid precursor. Finally, the obtained tyvalosin-silicon nanocomposite stable fertilizer liquid precursor was collected, and 40g urea as a nitrogen source, 25g potassium dihydrogen phosphate as a phosphorus source and potassium source, 4g boric acid, 2g zinc sulfate and 1g iron sulfate as trace elements were added thereto, and stirred evenly at room temperature at a stirring speed of 180r / min to ensure that all components were fully mixed to obtain liquid fertilizer. .

[0032] According to the above two groups of embodiments, it can be concluded that, through the impurity treatment link of the tyvalosin finished liquid, a composite reagent is prepared under suitable conditions for reaction and filtration, which significantly reduces the impurity content and improves the water solubility, laying a good foundation for the subsequent steps, and then the tyvalosin treated liquid is mixed with the carefully prepared active synergistic carrier solution, and the emulsified mixing and stirring reaction under specific conditions are carried out to achieve the synergistic improvement of fertilizer efficiency, and then the tyvalosin mixed liquid and the nanomaterial stabilization system are effectively integrated, and the stability is ensured by the synergistic effect of various materials. Finally, various fertilizer components are added and uniformly mixed to obtain liquid fertilizer. This process can achieve the effect of producing high-quality and stable liquid fertilizer through the coordinated operation of various technologies in various links. This method has significant technical innovation and broad application prospects for liquid fertilizer production.

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

Claims

1. A new process for producing high-quality liquid fertilizer from tyvalocin finished liquid, characterized in that: The novel process for producing high-quality liquid fertilizer comprises the following specific steps: Step 1, first, weigh polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease, then weigh phosphate buffer according to the content of polyoxyethylene sorbitan fatty acid ester, put the weighed polyoxyethylene sorbitan fatty acid ester, disodium salt of ethylenediaminetetraacetic acid, cellulase and protease into the phosphate buffer and stir to react to prepare a composite reagent, weigh the industrially produced tyvalosin finished liquid and put it into a stainless steel reaction container, then add the prepared composite reagent into the reaction container and stir to react, and filter through a microporous membrane filter after the reaction to obtain a tyvalosin treated liquid; Step 2, weighing alginate oligosaccharides and preparing them into alginate oligosaccharide solution, taking polylactic acid-glycolic acid copolymer and preparing them into polylactic acid-glycolic acid copolymer solution, then mixing the alginate oligosaccharide solution with the polylactic acid-glycolic acid copolymer solution, placing them in a high-speed emulsification device for emulsification and mixing to form a uniform emulsion-like active synergistic carrier solution, then weighing the tyvalosin treatment solution, adding the prepared active synergistic carrier solution to the tyvalosin treatment solution for stirring reaction, and completing the mixing of the tyvalosin treatment solution and the active synergistic carrier solution; Step 3, weighing silica nanoparticles, dissolving them in an ethanol solution to prepare a nanoparticle dispersion, then stirring and mixing them evenly, weighing polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane to obtain a mixture, and then placing the mixture in an ethanol solution and stirring and mixing to prepare a modification solution; The nanoparticle dispersion liquid and the modified liquid are mixed and stirred evenly to form a stable system liquid, and the mixed liquid of the tyvalosin treatment liquid and the active synergistic carrier solution and the stable system liquid are mixed and stirred to obtain a tyvalosin-silicon nanocomposite stable fertilizer liquid precursor; Step 4: Collect the prepared tyvalosin-silicon nanocomposite stable fertilizer liquid precursor, add urea as a nitrogen source, potassium dihydrogen phosphate as a phosphorus source and potassium source, add boric acid, zinc sulfate and iron sulfate as trace elements to the composite stable fertilizer liquid precursor and stir evenly to obtain liquid fertilizer.

2. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step 1, polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are weighed in a mass ratio of 1:0.5-0.7:0.1-0.3:0.1-0.3, the pH value of the selected phosphate buffer is 7.0-7.4, and the amount of the phosphate buffer is weighed according to 10mL-16mL per gram of polyoxyethylene sorbitan fatty acid ester. The weighed polyoxyethylene sorbitan fatty acid ester, disodium ethylenediaminetetraacetic acid, cellulase and protease are put into the phosphate buffer and stirred and mixed, the reaction temperature is controlled to be 25°C-35°C, and the reaction is stirred at a stirring speed of 120r / min-180r / min for 25min-35min.

3. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step 1, the industrially produced tylvalosin finished product placed in a stainless steel reaction container is 10L-13L, the amount of the composite reagent added is 10g-20g per liter of tylvalosin finished product liquid, the reaction temperature is controlled to be 30°C-40°C, the stirring speed is 300r / min-500r / min, the stirring reaction is continued for 2h-3h, and the pore size of the microporous membrane filter for filtration is 0.2μm-0.3μm.

4. The novel process for producing high-quality liquid fertilizer from a tyvalosin finished liquid according to claim 1, characterized in that: In the step 2, alginate oligosaccharides are weighed and prepared into an alginate oligosaccharide solution with a concentration of 8%-12%, polylactic acid-glycolic acid copolymer is taken and prepared into a polylactic acid-glycolic acid copolymer solution with a concentration of 8%-12%, the alginate oligosaccharide solution and the polylactic acid-glycolic acid copolymer solution are mixed in a volume ratio of 5-7:3-5, the emulsification speed in the emulsification equipment is 800r / min-1200r / min, and the emulsification time is 10min-20min.

5. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step 2, the weighed tyvalocin treatment liquid is 10L-13L, and the added amount of the active synergistic carrier solution is 200mL-300mL per liter of the tyvalocin treatment liquid. The active synergistic carrier solution is added for stirring reaction at a stirring speed of 120r / min-180r / min in an environment of 35°C-45°C for 1h-2h.

6. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step three, weigh silica nanoparticles, dissolve 0.8g-1.2g of silica nanoparticles in every 100ml of ethanol solution to prepare a nanoparticle dispersion with a concentration of 0.8%-1.2%, stir for 25min-35min in an environment of 35°C-45°C at a stirring speed of 180r / min-220r / min, the mixture is polyethylene glycol (PEG) and 3-aminopropyltriethoxysilane mixed in a mass ratio of 2-3:1, the ethanol solution is weighed in an amount of 8mL-12mL per gram of the mixture, and stir at a stirring speed of 250r / min-350r / min at room temperature until completely dissolved to prepare a modification solution.

7. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step 3, the mixing ratio of the nanoparticle dispersion and the modification solution is 0.7-1.2:1, and the reaction is stirred at 65° C.-75° C. for 2 h-3 h at a stirring speed of 350 r / min-450 r / min.

8. The novel process for producing high-quality liquid fertilizer from a tyvalosin finished liquid according to claim 1, characterized in that: In the step 3, the weighed mixed solution of the tyvalosin treatment solution and the active synergistic carrier solution is 7L-10L, the added amount of the stabilizing system liquid is 60g-100g per liter of the mixed solution, and the reaction is stirred at 25°C-35°C and a stirring speed of 200r / min-300r / min for 1h-2h.

9. The novel process for producing high-quality liquid fertilizer from a tyvalocin finished liquid according to claim 1, characterized in that: In the step 4, the amount of urea added as a nitrogen source is 40g-60g, the amount of potassium dihydrogen phosphate added as a phosphorus source and a potassium source is 25g-35g, the amount of boric acid added is 4g-6g, the amount of zinc sulfate added is 2g-4g, and the amount of iron sulfate added is 1g-3g. During the addition process, the mixture is stirred evenly at a stirring speed of 180r / min-220r / min at room temperature.

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