Liquid fertilizer formula formed by compounding tylosin finished product liquid and other components

Abstract

The invention discloses a liquid fertilizer formula prepared by compounding a tylosin finished product liquid and other components, and relates to the technical field of fertilizer preparation, and the liquid fertilizer formula comprises the steps of special pretreatment of tylosin, auxiliary compounding, nutrient substance addition and quality detection post-treatment. Certain carbon-carbon bonds, carbon-hydrogen bonds and other chemical bonds in tylosin molecules and byproducts thereof can be broken and recombined under bombardment of active particles, more functional groups with high activity are generated, the biological activity of the finished tylosin liquid can be enhanced, the finished tylosin liquid can be more easily compounded with other components in the subsequent process, and the stability of the finished tylosin liquid is improved. A stable compound with better synergy is formed by means of chemical bonding, hydrogen bonding and the like, ultrasonic waves are uniformly spread in a supercritical carbon dioxide medium, generated high-frequency vibration, cavitation effect and the like act on all the components, and the agglomeration phenomenon possibly existing among the components is further broken.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a liquid fertilizer formula in which tylosin finished product liquid is compounded with other components. Background Art

[0002] In the development process of modern agriculture, improving the yield and quality of crops has always been one of the core goals. As a key input to ensure the growth of crops, the performance and efficacy of fertilizers play a vital role in the benefits of agricultural production. Traditional fertilizers can only provide basic nitrogen, phosphorus, potassium and other macroelements. Although they can meet some of the nutrient needs of crop growth, with the changes in the planting environment, the diversification of soil fertility and the increase in people's demand for high-quality agricultural products, conventional fertilizers alone can no longer meet the comprehensive needs of crops for multiple nutrients and functional substances at different growth stages. For example, in some lands with poor soil or where a single crop is planted for consecutive years, crops are prone to slow growth and weak resistance to diseases and pests. There is an urgent need for more targeted fertilizer products with more comprehensive nutrients and other beneficial functions to improve growth conditions and increase yield and quality. Tylosin is a commonly used veterinary antibiotic, which is mainly produced by microbial fermentation. The finished liquid obtained in its production process contains not only tylosin itself, but also a variety of by-products produced by fermentation metabolism and residual nutrient matrix components. In the past, the treatment of tylosin finished liquid has focused on its subsequent processing in the pharmaceutical field or environmental treatment of waste. However, studies have found that some components in these finished liquids have the potential to be developed and applied in the field of agricultural fertilizers. For example, some organic small molecules, trace elements and some unknown factors with biostimulatory effects produced in the process of microbial metabolism may be used to promote plant growth, It plays a positive role in enhancing the ability of plants to resist diseases and pests, etc. However, in the existing technology, in the utilization of tylosin finished liquid, the previous application cognition was mostly limited to the fields of medicine and environmental protection, and its potential value in liquid fertilizer was not fully explored, resulting in waste of resources. In addition, the analysis of the mechanism of action of its components on plant growth is not comprehensive and in-depth, which is not conducive to formula development, and the compounding technology faces challenges. There are compatibility problems between different ingredients, and it is difficult to formulate a stable and effective product. At the same time, there is a lack of scientific and reasonable compounding ratio basis for each ingredient, which is easy to have adverse effects on plant growth and soil environment. For this reason, we propose a liquid fertilizer formula of tylosin finished liquid compounded with other ingredients. Summary of the invention

[0003] The purpose of the present invention is to provide a liquid fertilizer formula in which tylosin finished liquid is compounded with other ingredients.

[0004] In order to solve the problems raised in the above background technology, the present invention provides the following technical solutions: a liquid fertilizer formula of tylosin finished liquid compounded with other ingredients, including special pretreatment of tylosin, auxiliary compounding, nutrient addition and quality inspection post-processing, and the specific steps of preparing the liquid fertilizer formula of tylosin finished liquid compounded with other ingredients are as follows: Step 1, collecting the tylosin finished product liquid into a vacuum filtration device, performing vacuum filtration through a filter membrane, and transferring it into a plasma activation reaction chamber for activation treatment to obtain a tylosin activated liquid; Step 2: Select an amino acid concentrate and add it to the wall material solution. After the mixing is completed, add a cross-linking agent and mix and stir to obtain an amino acid concentrate. At the same time, prepare a magnetized microbial agent suspension for standby use. Step 3: Add tylosin activation solution, amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer into a high-pressure reactor in a supercritical carbon dioxide environment, subject it to ultrasonic oscillation operation, and obtain a composite mixed solution after completion; Step 4: adding the microbial agent suspension to the compound mixed solution and stirring to mix, and then adding the plant growth regulator thereto, stirring and mixing to obtain a liquid fertilizer product; Step 5: Conduct quality inspection on the finished liquid fertilizer and adjust it according to the actual pH value. If it passes the inspection, it will be packaged and stored.

[0005] As a further solution of the present invention: in the step 1, the tylosin finished liquid produced from the tylosin production link and preliminarily removed from impurities is collected, and the tylosin content in the tylosin finished liquid needs to be between 5% and 8%. After the collection is completed, it is transported to a vacuum filtration device, and the filtration membrane is a polyethersulfone filter membrane with a pore size of 0.5um. Before filtration, the vacuum degree of the vacuum filtration device is adjusted to -0.08MPa--0.1MPa, and the vacuum filtration device is turned on to control the filtration speed to 1L / min-2L / min. After the filtration is completed, the preliminarily filtered tylosin finished liquid is obtained, and it is stored in a corrosion-resistant container for standby use.

[0006] As a further solution of the present invention: in the step 1, the tylosin finished liquid after preliminary filtration is slowly transported to the plasma activation reaction chamber through a sterile pipeline, and argon gas with a purity of 99.999% is introduced into the reaction chamber at a flow rate of 25 cm 3 / min-30cm 3 / min, and at the same time, the vacuum degree in the chamber was adjusted to maintain at 15Pa, the radio frequency plasma generator was started, the operating frequency was set to 14MHz-16MHz, and the treatment time was set to 12min-15min. After the treatment was completed, tylosin activation solution was obtained.

[0007] As a further scheme of the present invention: in the step 2, an amino acid concentrate prepared by hydrolyzing plant-based protein is selected, and the degree of hydrolysis is required to reach more than 80%. The composition of the amino acid concentrate is configured according to the ratio of glutamic acid: lysine: arginine = 4:3:2. The amino acid concentrate is added to a stirring container and stirred at an initial stirring speed of 300r / min to prepare a wall material solution. The wall material solution is a mixture of sodium carboxymethyl cellulose and gelatin in a mass ratio of 3:2, and then deionized water at 50°C-60°C is added thereto, and the stirring speed is controlled to 400r / min-500r / min. Deionized water is added while stirring, and after sufficient dissolution, it is configured to a concentration of 6%-8%. The wall material solution is prepared, and glutaraldehyde-phosphate crosslinker is prepared at the same time. It is diluted with water to a concentration of 12%-15% and set aside. The stirring device of the glass container is turned on, and the amino acid concentrate is slowly added dropwise to the stirring wall material solution. The stirring speed is controlled to 500r / min, and the dropping speed is controlled to 10mL / min-15L / min. At the same time, a peristaltic pump is used to slowly drop glutaraldehyde-phosphate crosslinker at a flow rate of 5mL / min-8mL / min. The addition amount is 50%-65% of the total volume of the amino acid concentrate. The temperature is maintained at 40℃-45℃ during the dropping process. After continuous stirring and reaction for 60min-90min, a microencapsulated amino acid concentrate is obtained.

[0008] As a further solution of the present invention: In the step 2, a microbial agent prepared by mixing Bacillus, Trichoderma and Bacillus amyloliquefaciens in a viable count ratio of 2:1:2 is selected, placed in a sterile and clean glass beaker, sterile water is added for mixing, and stirred at room temperature using a magnetic stirrer at a stirring speed of 200r / min-300r / min for 30min-45min, and the viable count is configured to be 1×10 8 The bacterial suspension of CFU / mL is set aside, the prepared microbial inoculant bacterial suspension is transferred to the magnetic field generating device, the magnetic field strength is controlled to 0.6T-0.8T, the treatment environment temperature is controlled between 18℃-20℃, the treatment time is 25min-30min, during which a sterile glass rod is used to stir at a stirring speed of 60r / min-80r / min every 8min-10min. After the treatment is completed, it is transferred to a sterile, sealed and light-proof container and placed in a low temperature environment of 4℃-8℃ for standby use.

[0009] As a further scheme of the present invention: in the step 3, tylosin activation solution, microencapsulated amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer are added to a special reactor under a supercritical carbon dioxide environment, the equipment temperature is adjusted to 35° C., and the pressure in the equipment is increased to 7.5 MPa, the ultrasonic oscillation device built into the reactor is started, the power is set to 400 W, and the frequency is adjusted to 25 kHz. During the ultrasonic oscillation operation, the magnetic stirring device at the bottom of the reactor is turned on at the same time, and the stirring speed is set to 80 r / min-100 r / min. The operation lasts for 70 min-80 min, and the temperature and pressure parameters in the reactor are continuously monitored during the period to ensure the stability of the supercritical carbon dioxide environment and the smooth progress of the compounding process.

[0010] As a further solution of the present invention: in the step three, after completing the ultrasonic oscillation operation, slowly adjust the pressure release valve of the supercritical fluid equipment, reduce the pressure at a rate of 0.5 MPa / min, gradually reduce the pressure in the reactor to normal pressure, and gradually gasify and discharge the supercritical carbon dioxide. After the carbon dioxide is completely discharged, open the reactor, and transfer the obtained compound mixed liquid to a sterile, sealed storage container with a light-shielding function. The storage container is sterilized in advance and the temperature is maintained at 10°C-15°C.

[0011] As a further scheme of the present invention: in the step 4, the magnetized microbial agent suspension is taken out and placed in an environment of 20°C-25°C for 10min-15min, the microbial agent suspension is gently shaken during the standing process, natural plant-derived auxin is selected as a plant growth regulator, and the microbial agent suspension is slowly added to the compound mixed liquid in a reactor with a stirring device in a sterile manner. During the addition process, the stirring speed is set to 120r / min-150r / min, and the microbial agent suspension is evenly dispersed in the compound mixed liquid. After the addition is completed, the stirring is continued for 30min-40min. During the stirring process, the plant growth regulator solution is slowly dripped into the compound solution containing microorganisms using sterile drip irrigation, and the dripping speed is controlled between 2mL / min-5mL / min. After the dripping is completed, the mixing and stirring are performed for 20min-30min, and the plant growth regulator and the components in the liquid fertilizer system are fully mixed to prepare a stable liquid fertilizer product.

[0012] As a further solution of the present invention: in the step five, the quality inspection content specifically includes pH value inspection, component content inspection and microbial viable bacteria count inspection. The pH value standard range of the liquid fertilizer product is 6.5-7.2, and adjustments are made according to the actual pH value.

[0013] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are: 1. The present invention uses plasma activation operation to break and reorganize some carbon-carbon bonds, carbon-hydrogen bonds and other chemical bonds in tylosin molecules and their byproducts under the bombardment of active particles, generating more highly active functional groups, which can enhance the biological activity of the tylosin finished liquid itself, and make it easier to form a stable and more synergistic composite through chemical bonding, hydrogen bonding and other methods when it is subsequently compounded with other ingredients. Ultrasonic waves are evenly propagated in a supercritical carbon dioxide medium, and the high-frequency vibration and cavitation effect generated act on each component, further breaking the possible bonds between the components. Agglomeration phenomenon promotes more complete and uniform mixing and chemical reaction between the components under the coordination of nano-scale composite catalysts to form a stable compound system. By using the amino acid concentrate for microencapsulation and magnetization, the permeability of the cell membrane of the microbial agent will be appropriately adjusted, and the gene expression related to nutrient metabolism and environmental adaptation in the cell will change. When the microorganisms are subsequently compounded into liquid fertilizers and applied to the soil, they can more efficiently play their functions of promoting soil nutrient conversion, inhibiting harmful pathogens, and interacting with plant roots, thereby better helping plant growth; 2. The present invention performs compounding operation under supercritical carbon dioxide environment. The high diffusivity and low surface tension characteristics of supercritical carbon dioxide are combined with the high-frequency vibration and cavitation effect of ultrasound and the uniform mixing effect of magnetic stirring. The problems of uneven mixing and poor compatibility caused by differences in the properties of the components in the conventional compounding process are overcome. The components can be more evenly and fully mixed in this special environment, promoting physical and chemical interactions between each other to form a stable compounding system. At the same time, after completing the ultrasonic oscillation operation, the pressure is slowly reduced to discharge supercritical carbon dioxide, which not only ensures that the compounding mixture can be obtained smoothly, but also can recycle and reuse the discharged carbon dioxide, which meets environmental protection requirements. By selecting natural plant-derived auxin as a plant growth regulator, and slowly dripping it with a sterile dropper, it is evenly mixed into the compound solution containing microorganisms, which can synergize with other components, more effectively regulate plant growth, promote physiological processes such as root development and flower bud differentiation, and improve the absorption and utilization efficiency of nutrients by plants, thereby improving the yield and quality of crops. Moreover, the full integration of the plant growth regulator with the entire liquid fertilizer system ensures that it can play a stable role during use and continuously assist the various growth stages of plants. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 The figure is a schematic diagram of the process of preparing liquid fertilizer from tylosin finished liquid in an embodiment of the present invention. DETAILED DESCRIPTION

[0015] 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.

[0016] The invention discloses a liquid fertilizer formula of tylosin finished liquid compounded with other ingredients, comprising special tylosin pretreatment, auxiliary compounding, nutrient addition and quality inspection post-processing. The specific steps of preparing the liquid fertilizer formula of tylosin finished liquid compounded with other ingredients are as follows: Step 1, collecting the tylosin finished product liquid into a vacuum filtration device, performing vacuum filtration through a filter membrane, and transferring it into a plasma activation reaction chamber for activation treatment to obtain a tylosin activated liquid; Step 2: Select an amino acid concentrate and add it to the wall material solution. After the mixing is completed, add a cross-linking agent and mix and stir to obtain an amino acid concentrate. At the same time, prepare a magnetized microbial agent suspension for standby use. Step 3: Add tylosin activation solution, amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer into a high-pressure reactor in a supercritical carbon dioxide environment, subject it to ultrasonic oscillation operation, and obtain a composite mixed solution after completion; Step 4: adding the microbial agent suspension to the compound mixed solution and stirring to mix, and then adding the plant growth regulator thereto, stirring and mixing to obtain a liquid fertilizer product; Step 5: Conduct quality inspection on the finished liquid fertilizer and adjust it according to the actual pH value. If it passes the inspection, it will be packaged and stored.

[0017] In one embodiment of the present invention: in step 1, the tylosin finished liquid produced from the tylosin production link and preliminarily removed from impurities is collected, and the tylosin content in the tylosin finished liquid needs to be between 5% and 8%. After the collection is completed, it is transported to a vacuum filtration device, and the filtration membrane is a polyethersulfone filter membrane with a pore size of 0.5um. Before filtration, the vacuum degree of the vacuum filtration device is adjusted to -0.08MPa--0.1MPa, and the vacuum filtration device is turned on to control the filtration speed to 1L / min-2L / min. After the filtration is completed, the preliminarily filtered tylosin finished liquid is obtained, which is stored in a corrosion-resistant container for standby use.

[0018] In one embodiment of the present invention, in step 1, the tylosin finished liquid after preliminary filtration is slowly transported to the plasma activation reaction chamber through a sterile pipeline, and argon gas with a purity of 99.999% is introduced into the reaction chamber at a flow rate of 25 cm 3 / min-30cm 3 / min, and at the same time, the vacuum degree in the chamber was adjusted to maintain at 15Pa, the radio frequency plasma generator was started, the operating frequency was set to 14MHz-16MHz, and the treatment time was set to 12min-15min. After the treatment was completed, tylosin activation solution was obtained.

[0019] In one embodiment of the present invention: in step 2, an amino acid concentrate prepared by hydrolyzing plant-based protein is selected, and the degree of hydrolysis is required to reach more than 80%. The composition of the amino acid concentrate is configured according to the ratio of glutamic acid: lysine: arginine = 4:3:2. The amino acid concentrate is added to a stirring container and stirred at an initial stirring speed of 300r / min to prepare a wall material solution. The wall material solution is a mixture of sodium carboxymethyl cellulose and gelatin in a mass ratio of 3:2, and then deionized water at 50°C-60°C is added thereto, and the stirring speed is controlled to 400r / min-500r / min. Deionized water is added while stirring, and after sufficient dissolution, it is configured to a concentration of 6%-8%. The wall material solution is prepared, and glutaraldehyde-phosphate crosslinker is prepared at the same time. It is diluted with water to a concentration of 12%-15% and set aside. The stirring device of the glass container is turned on, and the amino acid concentrate is slowly added dropwise to the stirring wall material solution. The stirring speed is controlled to 500r / min, and the dropping speed is controlled to 10mL / min-15L / min. At the same time, a peristaltic pump is used to slowly drop glutaraldehyde-phosphate crosslinker at a flow rate of 5mL / min-8mL / min. The addition amount is 50%-65% of the total volume of the amino acid concentrate. The temperature is maintained at 40℃-45℃ during the dropping process. After continuous stirring and reaction for 60min-90min, a microencapsulated amino acid concentrate is obtained.

[0020] In one embodiment of the present invention, in step 2, a microbial agent prepared by mixing Bacillus, Trichoderma and Bacillus amyloliquefaciens in a viable count ratio of 2:1:2 is selected, placed in a sterile and clean glass beaker, sterile water is added for mixing, and stirred at room temperature using a magnetic stirrer at a stirring speed of 200 r / min-300 r / min for 30 min-45 min to prepare a viable count of 1×10 8 The bacterial suspension of CFU / mL is set aside, the prepared microbial inoculant bacterial suspension is transferred to the magnetic field generating device, the magnetic field strength is controlled to 0.6T-0.8T, the treatment environment temperature is controlled between 18℃-20℃, the treatment time is 25min-30min, during which a sterile glass rod is used to stir at a stirring speed of 60r / min-80r / min every 8min-10min. After the treatment is completed, it is transferred to a sterile, sealed and light-proof container and placed in a low temperature environment of 4℃-8℃ for standby use.

[0021] In one embodiment of the present invention: in step three, tylosin activation solution, microencapsulated amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer are added to a special reactor under a supercritical carbon dioxide environment, the equipment temperature is adjusted to 35°C, and the pressure in the equipment is increased to 7.5MPa, the ultrasonic oscillation device built into the reactor is started, the power is set to 400W, and the frequency is adjusted to 25kHz. During the ultrasonic oscillation operation, the magnetic stirring device at the bottom of the reactor is turned on at the same time, and the stirring speed is set to 80r / min-100r / min. The operation lasts for 70min-80min, and the temperature and pressure parameters in the reactor are continuously monitored during the period to ensure the stability of the supercritical carbon dioxide environment and the smooth progress of the compounding process.

[0022] In one embodiment of the present invention: in step three, after completing the ultrasonic oscillation operation, slowly adjust the pressure release valve of the supercritical fluid equipment, reduce the pressure at a rate of 0.5MPa / min, gradually reduce the pressure in the reactor to normal pressure, and gradually gasify and discharge the supercritical carbon dioxide. After the carbon dioxide is completely discharged, open the reactor, and transfer the obtained compound mixed liquid to a sterile, sealed storage container with a light-shielding function. The storage container is sterilized in advance and the temperature is maintained at 10°C-15°C.

[0023] In one embodiment of the present invention: in step 4, the magnetized microbial agent suspension is taken out and placed in an environment of 20°C-25°C for 10min-15min, the microbial agent suspension is gently shaken during the standing process, natural plant-derived auxin is selected as a plant growth regulator, and the microbial agent suspension is slowly added to the compound mixed liquid in a reactor with a stirring device in a sterile manner. During the addition process, the stirring speed is set to 120r / min-150r / min, and the microbial agent suspension is evenly dispersed in the compound mixed liquid. After the addition is completed, stirring is continued for 30min-40min. During the stirring process, the plant growth regulator solution is slowly dripped into the compound solution containing microorganisms using sterile drip irrigation, and the dripping speed is controlled between 2mL / min-5mL / min. After the dripping is completed, the mixing and stirring are performed for 20min-30min, and the plant growth regulator and the components in the liquid fertilizer system are fully mixed to prepare a stable liquid fertilizer product.

[0024] In one embodiment of the present invention: in step five, the quality inspection content specifically includes pH value inspection, component content inspection and microbial viable count inspection. The pH value standard range of the liquid fertilizer product is 6.5-7.2, and adjustments are made according to the actual pH value.

[0025] In one embodiment of the present invention: In step 1, during the plasma activation process, high-energy electrons, ions, free radicals and other active ions in the plasma undergo complex physical and chemical reactions with various organic components, residual nutrient matrix components and the like in the tylosin finished product liquid. For some carbon-carbon bonds and carbon-hydrogen bonds in the tylosin molecules and their byproducts, the chemical bonds break and reorganize under the bombardment of active particles, generating more highly active functional groups, including hydroxyl, carboxyl and amino groups. When the tylosin finished product liquid after the plasma activation treatment becomes slightly lighter in color and slightly more transparent in appearance, the tylosin activated liquid is obtained.

[0026] In one embodiment of the present invention: in step five, if the pH value is low, an appropriate amount of a potassium hydroxide solution regulator with a concentration of 1mol / L-2mol / L can be slowly added, and the pH value change is monitored in real time until it reaches the qualified range. If the pH value is high, an appropriate amount of a phosphoric acid solution regulator with a concentration of 0.5mol / L-1mol / L is added, and the adjustment is also performed under stirring to ensure the accuracy and stability of the pH value adjustment, and to avoid adverse effects on the activity and stability of the components in the liquid fertilizer due to excessive fluctuations in the pH value. The amount of the regulator added each time is estimated according to the degree of deviation of the pH value and the total volume of the liquid fertilizer. After adding, it is necessary to fully stir and test the pH value again, and repeat the operation until the pH value meets the requirements.

[0027] Example The tylosin finished product liquid was collected and its tylosin content was tested to be 6.5%. The total collection volume was 80L. A sterile stainless steel collection bucket was used during the collection process to ensure a clean environment and prevent impurities from mixing in. An amino acid concentrate prepared by hydrolysis of soy protein was selected, with a hydrolysis degree of 83%. It was accurately weighed and prepared according to the ratio of glutamic acid: lysine: arginine = 4:3:2. The total volume after preparation was 15L and placed in a glass stirring container with a polytetrafluoroethylene stirring paddle. The initial stirring speed was set to 300r / min. 9kg of sodium carboxymethyl cellulose and 6kg of gelatin were weighed and mixed, and placed in a stainless steel container with heating and stirring functions. Deionized water at a temperature of 55°C was added, and stirring was performed at a stirring speed of 450r / min until The mixture was fully dissolved to prepare a wall material solution with a concentration of about 7% and a total volume of 35 L. An appropriate amount of glutaraldehyde-phosphate crosslinker was taken and diluted to a concentration of 13% with a phosphate buffer with a pH value of 7.5. The total volume was 10 L. A microbial inoculant prepared by mixing Bacillus, Trichoderma and Bacillus amyloliquefaciens in a viable count ratio of 2:1:2 was selected and placed in a sterile and clean 10 L glass beaker. Sterile water was added and stirred at a stirring speed of 250 r / min for 40 min using a magnetic stirrer at room temperature to prepare a viable count of 1×10 8CFU / mL of bacterial suspension is reserved, a specific variety of brown algae is selected, and after the cell wall is broken by low-temperature ultrasound, seaweed polysaccharides are extracted by composite enzymatic hydrolysis, and the extraction rate reaches 28%. The average molecular weight of the extracted seaweed polysaccharides is about 8kDa, and the preparation amount is 12L. Trace elements such as iron, zinc, manganese, boron, and molybdenum are chelated with a specific amino acid chelator at a molar ratio of 1:1.2, wherein the iron element exists in the form of EDTA-Fe, the zinc element exists in the form of DTPA-Zn, the manganese element exists in the form of EDTA-Mn, the boron element exists in the form of sugar alcohol boron, and the molybdenum element exists in the form of ammonium molybdate. The preparation amount is 5L, sodium citrate and potassium dihydrogen phosphate are accurately weighed in a mass ratio of 1:1, and mixed to form a 3L buffer solution, and a natural plant-derived auxin analogue extracted from leguminous plant seeds and purified by multiple column chromatography is selected, and the active ingredient content reaches 92%, and 100g is weighed for standby; The collected 80L tylosin finished liquid was transported to a vacuum filtration device through a sterile pipeline. The device was equipped with a polyethersulfone filter membrane with a pore size of 0.5um. Before filtration, the vacuum degree of the vacuum filtration device was adjusted to -0.09MPa, the filtration pump was turned on, and the filtration speed was controlled to 1.5L / min, so that the tylosin finished liquid slowly passed through the filter membrane. The entire filtration process lasted for about 53min, during which impurity particles larger than 0.5um were observed to be trapped on the surface of the filter membrane. After the filtration was completed, about 78L of the tylosin finished liquid after preliminary filtration was collected and transferred to a pre-sterilized 100L corrosion-resistant (316 stainless steel) storage container for standby use. The tylosin after preliminary filtration was transferred to a sterile pipeline. The finished product liquid is slowly transported to the plasma activation reaction chamber, and argon gas with a purity of 99.999% is introduced into the reaction chamber. The gas flow rate is adjusted to 28cm³ / min, and the vacuum degree in the chamber is adjusted to maintain at 15Pa. The radio frequency plasma generator is started, and its operating frequency is set to 15MHz. The processing time is set to 13min. During the activation process, a faint luminescence phenomenon can be observed in the reaction chamber, which is a manifestation of plasma generation. After the treatment is completed, the obtained tylosin activation liquid has a slightly lighter color and a slightly increased transparency, which is in line with the expected phenomenon. Then it is transferred to another 80L storage container that has been sterilized and protected from light, ready for subsequent compounding and use; The stirring device of the glass stirring container was turned on, and 15 L of the amino acid concentrate was slowly added dropwise at a dropping speed of 12 mL / min to the 35 L wall material solution being stirred at 500 r / min. At the same time, 10 L of glutaraldehyde-phosphate crosslinking agent (the added amount was about 60% of the total volume of the amino acid concentrate) was slowly added dropwise at a flow rate of 6 mL / min using a peristaltic pump. The temperature was maintained at 42° C. during the dropping process, and the stirring reaction was continued for 75 minutes. After the reaction was completed, microcapsules with a particle size mostly between 20 μm and 40 μm, spherical shape and relatively uniform dispersion were observed through a microscope, that is, microcapsules were prepared. The encapsulated amino acid concentrate is transferred to a sterile, sealed 50L storage container with a refrigeration function (maintained at 6°C) for standby use. The prepared 10L microbial inoculant suspension is transferred to a special magnetic field generator, and the magnetic field strength is controlled to 0.7T. The treatment environment temperature is controlled at 19°C. The treatment time is 28min. During this period, a sterile glass rod is used to gently stir once at a stirring speed of 70r / min every 9min to make the microorganisms evenly magnetized. After the treatment is completed, the magnetized microbial inoculant suspension is transferred to a sterile, sealed and light-proof 10L container and placed in a low temperature environment of 6°C for standby use. Using professional supercritical fluid equipment, the equipment temperature was adjusted to 35°C, and the pressure was slowly increased to 7.5MPa through the pressure regulating device to make the carbon dioxide reach a supercritical state. Then, 80L of tylosin activation solution, 50L of microencapsulated amino acid concentrate, 12L of seaweed polysaccharide extract, 5L of trace element chelate and 3L of buffer were slowly added to the special high-pressure reactor (volume of 200L) under the supercritical carbon dioxide environment through the sterile and high-pressure resistant feeding pipeline. During the feeding process, the liquid level sensor of the reactor was closely monitored to ensure that each component was accurately added in proportion, and the error was controlled within ±0.5%. The built-in ultrasonic oscillation device of the reactor was started, and its power was set to 400W and the frequency was adjusted to 25kHz. At the same time, the magnetic stirring device at the bottom of the reactor was turned on and the stirring speed was set to 90r / min to make each component fully mixed in the supercritical carbon dioxide environment. The reaction was continued for 75 minutes. During this period, the temperature and pressure sensors configured on the reactor were used to continuously monitor parameter changes to ensure that the supercritical carbon dioxide environment was stable. The actual monitoring temperature fluctuation range was 35°C ± 0.2°C, and the pressure fluctuation range was 7.5MPa ± 0.03MPa to ensure that the compounding process was carried out smoothly. After the ultrasonic oscillation operation was completed, the pressure release valve of the supercritical fluid equipment was slowly adjusted to reduce the pressure at a rate of 0.5MPa / min. After about 15 minutes, the pressure in the reactor was gradually reduced to normal pressure. During this period, it was observed that the supercritical carbon dioxide was gradually gasified and discharged. The discharged carbon dioxide was collected by a recovery device. After the carbon dioxide was completely discharged, the reactor was opened and the prepared compound mixture was transferred to a sterile, sealed 150L storage container with a light-shielding function. The storage container was sterilized in advance and kept at a temperature of 12°C. The magnetized microbial agent suspension was taken out from the low-temperature environment, and allowed to stand at 22°C for 12 minutes. During this period, the container containing the suspension was gently shaken every 2 minutes to make it evenly dispersed. Then, a sterile silicone tube with a flow rate control valve was used to slowly add 10L of the microbial agent suspension to a 150L reactor equipped with a stirring device and filled with the compound mixture at a flow rate of 12mL / min. During the addition process, the stirring device of the reactor was turned on and the stirring speed was set to 130r / min. After the addition was completed, stirring was continued for 35 minutes to make the microbial agent evenly dispersed in the compound mixture, fully contact and interact with each component to form a preliminary liquid fertilizer system. 100g of plant growth regulator was weighed and added to the reactor. The agent is placed in a clean, sterile agate mortar with a grinding function, 200g of sterile distilled water is added, and the plant growth regulator is gently ground with a grinding rod for 8min to fully dissolve the plant growth regulator and form a uniform paste. Then an appropriate amount of sterile distilled water is added to make the volume 1L to prepare a plant growth regulator solution. The plant growth regulator solution is slowly added to the compound solution containing microorganisms at a dropping rate of 3mL / min using a sterile dropper. After the addition is completed, stirring and mixing is continued for 25min to fully mix the plant growth regulator and the components in the liquid fertilizer system. Finally, a stable liquid fertilizer product is made. At this time, the total volume of the liquid fertilizer product is about 160L, which is transferred to a storage tank with shading and temperature control functions (the temperature is maintained at 12°C) for standby use.

[0028] Quality inspection of liquid fertilizer products. pH value detection: Use a calibrated high-precision acidity meter to take samples from different locations of the storage tank (upper, middle and lower layers, 3 points in each layer) to detect the pH value of the finished liquid fertilizer. After testing, the average pH value of the samples taken was 6.8, which is within the standard range of 6.5-7.2 and meets the requirements; Detection of the content of each component: The content of the main components such as tylosin, amino acids, seaweed polysaccharides, and trace element chelates in the liquid fertilizer product was analyzed using a high performance liquid chromatography (HPLC). According to the chemical properties and polarity differences of the components, a C18 reverse phase column was selected as the chromatographic column, and methanol-water (volume ratio of 40:60) was used as the mobile phase. The flow rate was set to 1.0 mL / min, the column temperature was set to 35°C, and the detection wavelength corresponding to each component (the detection wavelength of tylosin was 280 nm, etc.) was set. By comparing the retention time and peak area with those of the standard, the actual content of each component in the liquid fertilizer product was calculated. The test results showed that the content of each component met the requirements of the formula design, and the error was within ±3%; Microbial viable count detection: The plate count method combined with a plate counter is used for detection. First, the liquid fertilizer sample is diluted to 10 -5 , 10 -6 , 10 -7Three dilution multiples), and then 0.1mL of the diluted sample solution was evenly spread on the corresponding microbial culture medium plate (Bacillus used nutrient agar medium and cultured at 37℃ for 36h, Trichoderma used potato dextrose agar medium and cultured at 26℃ for 112h, and Bacillus amyloliquefaciens also used nutrient agar medium and cultured at 37℃ for 48h). Four replicate plates were set for each dilution. After the colonies grew, the colonies on the plate were counted and counted using a plate counter to convert the number of live microorganisms in the original liquid fertilizer sample. The results showed that the number of live bacteria of Bacillus was about 1.2×10 8 CFU / mL, the number of viable bacteria of Trichoderma is about 6×10 7 CFU / mL, the number of viable Bacillus amyloliquefaciens is about 1.1×10 8 CFU / mL, all meet the corresponding standards set in the formula, which can ensure that it can effectively play the role of regulating soil microecology in liquid fertilizer.

[0029] By implementing the above-provided liquid fertilizer formula of tylosin finished liquid compounded with other ingredients and detailed preparation steps, a liquid fertilizer product was successfully prepared, indicating the feasibility of using tylosin finished liquid compounded with other ingredients to prepare a liquid fertilizer product.

[0030] 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.

[0031] 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.

[0032] 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.

[0033] 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 liquid fertilizer formula of tylosin finished liquid and other ingredients, including special pretreatment of tylosin, auxiliary compounding, nutrient addition and quality inspection post-processing, characterized in that: The specific steps of preparing the liquid fertilizer formula of the tylosin finished liquid and other ingredients are as follows: Step 1, collecting the tylosin finished product liquid into a vacuum filtration device, performing vacuum filtration through a filter membrane, and transferring it into a plasma activation reaction chamber for activation treatment to obtain a tylosin activated liquid; Step 2: Select an amino acid concentrate and add it to the wall material solution, and add a cross-linking agent to mix and stir to obtain an amino acid concentrate, and prepare a magnetized microbial agent suspension for standby use; Step 3: Add tylosin activation solution, amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer into a high-pressure reactor in a supercritical carbon dioxide environment, subject it to ultrasonic oscillation operation, and obtain a composite mixed solution after completion; Step 4: adding the microbial agent suspension to the compound mixed solution and stirring to mix, and then adding the plant growth regulator thereto, stirring and mixing to obtain a liquid fertilizer product; Step 5: Conduct quality inspection on the finished liquid fertilizer and adjust it according to the actual pH value. If it passes the inspection, it will be packaged and stored.

2. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step 1, the tylosin finished liquid produced from the tylosin production link and preliminarily removed from impurities is collected, and the tylosin content in the tylosin finished liquid needs to be between 5% and 8%. After the collection is completed, it is transported to a vacuum filtration device, and the filtration membrane is a polyethersulfone filter membrane with a pore size of 0.5um. Before filtration, the vacuum degree of the vacuum filtration device is adjusted to -0.08MPa--0.1MPa, and the vacuum filtration device is turned on to control the filtration speed to 1L / min-2L / min. After the filtration is completed, the preliminarily filtered tylosin finished liquid is obtained, and it is stored in a corrosion-resistant container for standby use.

3. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step 1, the tylosin finished product liquid after preliminary filtration is slowly transported to the plasma activation reaction chamber through a sterile pipeline, and argon gas with a purity of 99.999% is introduced into the reaction chamber at a flow rate of 25 cm 3 / min-30cm 3 / min, and at the same time, the vacuum degree in the chamber was adjusted to maintain at 15Pa, the radio frequency plasma generator was started, the operating frequency was set to 14MHz-16MHz, and the treatment time was set to 12min-15min. After the treatment was completed, tylosin activation solution was obtained.

4. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step 2, an amino acid concentrate prepared by hydrolyzing plant-based protein is selected, and the degree of hydrolysis is required to reach more than 80%. The composition of the amino acid concentrate is configured according to the ratio of glutamic acid: lysine: arginine = 4:3:

2. The amino acid concentrate is added to a stirring container and stirred at an initial stirring speed of 300r / min to prepare a wall material solution. The wall material solution is mixed with sodium carboxymethyl cellulose and gelatin in a mass ratio of 3:2, and then deionized water at 50°C-60°C is added thereto, and the stirring speed is controlled to 400r / min-500r / min. Deionized water is added while stirring, and after sufficient dissolution, it is configured into a wall material solution with a concentration of 6%-8%, and the same Prepare glutaraldehyde-phosphate crosslinking agent, dilute it with water to a concentration of 12%-15% and set it aside, turn on the stirring device of the glass container, slowly drop the amino acid concentrate into the stirring wall material solution, control the stirring speed to 500r / min, and the dropping speed to 10mL / min-15L / min. At the same time, use a peristaltic pump to slowly drop the glutaraldehyde-phosphate crosslinking agent at a flow rate of 5mL / min-8mL / min, and the added amount is 50%-65% of the total volume of the amino acid concentrate. Keep the temperature at 40°C-45°C during the dropping process, and continue stirring the reaction for 60min-90min to obtain a microencapsulated amino acid concentrate.

5. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step 2, a microbial agent prepared by mixing Bacillus, Trichoderma and Bacillus amyloliquefaciens in a ratio of 2:1:2 in terms of viable bacteria count was selected, placed in a sterile and clean glass beaker, and sterile water was added for mixing and stirring. A magnetic stirrer was used at room temperature and stirred at a stirring speed of 200 r / min-300 r / min for 30 min-45 min to prepare a viable bacteria count of 1×10 8 The bacterial suspension of CFU / mL is set aside, the prepared microbial inoculant bacterial suspension is transferred to the magnetic field generating device, the magnetic field strength is controlled to 0.6T-0.8T, the treatment environment temperature is controlled between 18℃-20℃, the treatment time is 25min-30min, during which a sterile glass rod is used to stir at a stirring speed of 60r / min-80r / min every 8min-10min. After the treatment is completed, it is transferred to a sterile, sealed and light-proof container and placed in a low temperature environment of 4℃-8℃ for standby use.

6. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step three, tylosin activation solution, microencapsulated amino acid concentrate, seaweed polysaccharide extract, trace element chelate and buffer are added to a special reactor under a supercritical carbon dioxide environment, the equipment temperature is adjusted to 35° C., and the pressure in the equipment is increased to 7.5 MPa. The ultrasonic oscillation device built into the reactor is started, and its power is set to 400 W, and the frequency is adjusted to 25 kHz. During the ultrasonic oscillation operation, the magnetic stirring device at the bottom of the reactor is turned on at the same time, and the stirring speed is set to 80 r / min-100 r / min. The operation lasts for 70 min-80 min, and the temperature and pressure parameters in the reactor are continuously monitored during the period to ensure the stability of the supercritical carbon dioxide environment and the smooth progress of the compounding process.

7. A liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step three, after completing the ultrasonic oscillation operation, slowly adjust the pressure release valve of the supercritical fluid equipment, reduce the pressure at a rate of 0.5 MPa / min, gradually reduce the pressure in the reactor to normal pressure, and gradually gasify and discharge the supercritical carbon dioxide. After the carbon dioxide is completely discharged, open the reactor, and transfer the obtained compound mixed liquid to a sterile, sealed storage container with a light-shielding function. The storage container is sterilized in advance and the temperature is maintained at 10°C-15°C.

8. The liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In the step 4, the magnetized microbial agent suspension is taken out and placed in an environment of 20°C-25°C for 10min-15min, the microbial agent suspension is gently shaken during the standing process, natural plant-derived auxin is selected as a plant growth regulator, and the microbial agent suspension is slowly added to the composite mixed liquid in a reactor with a stirring device in a sterile manner. During the addition process, the stirring speed is set to 120r / min-150r / min, and the microbial agent suspension is evenly dispersed in the composite mixed liquid. After the addition is completed, the stirring is continued for 30min-40min. During the stirring process, the plant growth regulator solution is slowly dripped into the composite solution containing the microorganisms using sterile drip irrigation, and the dripping speed is controlled between 2mL / min-5mL / min. After the dripping is completed, the mixing and stirring are performed for 20min-30min, and the plant growth regulator and the components in the liquid fertilizer system are fully mixed to prepare a stable liquid fertilizer product.

9. The liquid fertilizer formula of a tylosin finished liquid compounded with other ingredients according to claim 1, characterized in that: In step five, the quality inspection content specifically includes pH value inspection, component content inspection and microbial viable bacteria count inspection. The pH value standard range of the liquid fertilizer product is 6.5-7.2, and adjustments are made based on the actual pH value.

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