Method for promoting flower growth by using acetylisovaleryltylosin tartrate finished product liquid fertilizer

Abstract

The invention discloses a method for promoting flower growth by using an acetylisovaleryltylosin tartrate finished product liquid fertilizer, and relates to the technical field of fertilizer preparation, and the method comprises the following specific steps: step 1, firstly, screening out 1-ethyl-3-methylimidazolium acetate ionic liquid for subsequent treatment, the preparation method has the advantages that the polylactic acid is selected as a microcapsule wrapping material, so that the acetylisovaleryltylosin tartrate can be tightly and stably wrapped, an effective protective barrier is constructed, the influence of external adverse environmental factors on the acetylisovaleryltylosin tartrate is isolated, the activity of the acetylisovaleryltylosin tartrate is powerfully guaranteed to be maintained in the storage and subsequent application process, and the stability of the acetylisovaleryltylosin tartrate is improved. The temperature-sensitive hydrogel prepared from poly (N-isopropylacrylamide) is used as an intelligent response material, the temperature-sensitive characteristic of the temperature-sensitive hydrogel is the key point for realizing intelligent regulation and control, and the hydrogel presents obviously different states at different temperatures, so that the scientificity and accuracy of fertilization are greatly improved, and the application prospect is wide. The flower can obtain proper nutrient supply in different growth stages.

Description

Technical Field

[0001] The invention relates to the technical field of fertilizer preparation, in particular to a method for promoting the growth of flowers by using tyvalocin finished liquid fertilizer. Background Art

[0002] As an antibiotic substance, tyvalosin has been widely used in the field of animal husbandry to prevent and treat livestock and poultry diseases, showing good antibacterial activity. In recent years, studies have found that tyvalosin also has certain application potential in the field of plants. It can regulate the physiological metabolic process of plants, such as promoting the growth and development of plant roots, enhancing plant photosynthesis, etc., thereby playing a positive role in promoting the overall growth of plants. However, the chemical properties of tyvalosin itself make it face some problems when it is actually used in flower planting, such as poor stability, easy to be inactivated by external environmental factors (such as temperature, humidity, light, etc.), and its poor dispersibility in soil or fertilizer system makes it difficult to act evenly on flower plants, resulting in its effect of promoting flower growth not being fully exerted; The existing technology has certain defects. First, there is insufficient research on the stability of Tyvalosin itself. When preparing liquid fertilizer, it is impossible to take effective stabilization treatment measures to protect the activity of Tyvalosin, which makes it easy to change during storage and use, affecting the effect of the fertilizer. Secondly, the initial purity of the existing Tyvalosin finished liquid is low and lacks targeted pretreatment. There is a lack of special and targeted pretreatment processes to improve its purity and remove these potentially harmful impurities. Usually, only some general chemical raw material preliminary treatment methods are used. These methods are not effective for removing impurities from Tyvalosin in flower application scenarios and cannot meet the requirements of flower growth for fertilizer purity. Finally, the existing technology lacks effective means to ensure the stability of Tyvalosin and its coordination with other nutrients. Fertilization lacks precise strategies, which affects flower growth. To this end, we propose a method for promoting flower growth with Tyvalosin finished liquid fertilizer. Summary of the invention

[0003] The object of the present invention is to provide a method for promoting the growth of flowers by using tyvalocin finished liquid fertilizer.

[0004] In order to solve the problems raised in the above background technology, the present invention provides the following technical solution: a method for promoting the growth of flowers with a liquid fertilizer of tyvalocin finished product, the method for promoting the growth of flowers with a liquid fertilizer comprising the following specific steps: Step 1, first screen out 1-ethyl-3-methylimidazolium acetate ionic liquid for subsequent treatment, and the specific preparation process is as follows: first synthesize 1-ethyl-3-methylimidazolium bromide, add 1-methylimidazole and ethyl bromide into a three-necked flask, then add acetonitrile as a solvent, then place the three-necked flask in an oil bath for heating, and turn on a stirring device to react. After the reaction is completed, remove the solvent and unreacted raw materials through a vacuum distillation device until pure 1-ethyl-3-methylimidazolium bromide is obtained; Then, 1-ethyl-3-methylimidazolium acetate is prepared, the synthesized 1-ethyl-3-methylimidazolium bromide is transferred to a clean three-necked flask, and then silver acetate is added to carry out an ion exchange reaction, and dichloromethane is added as a solvent to fully dissolve the reactant, and a stirring device is turned on at room temperature. After the reaction is completed, the generated silver bromide precipitate is filtered out using filter paper, and then the solvent is removed by reduced pressure distillation to obtain 1-ethyl-3-methylimidazolium acetate ionic liquid by distillation; Step 2, transferring the tyvalosin finished liquid to a clean glass container and adjusting the pH value, then filtering with filter paper to complete the pretreatment of the tyvalosin finished liquid, and then mixing the pretreated tyvalosin finished liquid with the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid in a glass extraction container, placing it in a constant temperature water bath for heating and stirring to perform an extraction reaction, after the extraction is completed, transferring the mixed liquid to a membrane separation device for separation, and completing the ionic liquid-membrane separation coupling treatment; Step 3: After membrane separation, the ionic liquid phase containing tyvalosin that passes through the membrane is collected into a clean round-bottom flask, and the tyvalosin is recovered by a back extraction method. n-hexane is selected as an organic solvent, and the ionic liquid phase and n-hexane are mixed in a separatory funnel and shaken, and then allowed to stand for stratification, so that the tyvalosin is transferred to the n-hexane phase, and then the tyvalosin is recovered by distillation through a distillation device, and then the recovered tyvalosin is purified, and the recovered tyvalosin is dissolved in an ethanol solution, and the solution is slowly cooled in a low-temperature thermostatic bath. After the tyvalosin crystals are precipitated, it is filtered through a Buchner funnel with a microporous filter paper to obtain a higher purity tyvalosin; Step 4, preparing microcapsule encapsulation materials and smart response materials, first prepare microcapsule encapsulation materials, select polylactic acid as the material, weigh polylactic acid and dissolve it in dichloromethane, stir and mix with a magnetic stirrer in a well-ventilated environment until the polylactic acid is completely dissolved to form a uniform solution, and at the same time add polysorbate-80 to water to form an aqueous phase, and then slowly add the polylactic acid solution dropwise to the aqueous phase to form an emulsion under high-speed stirring to complete the preparation of microcapsule encapsulation materials, and then prepare smart response materials, mix N-isopropylacrylamide monomer, cross-linking agent N,N'-methylenebisacrylamide, and initiator potassium persulfate in water, put the mixture into a three-necked flask, place it in an oil bath and stir to perform a polymerization reaction to form a thermosensitive hydrogel, and complete the preparation of smart response materials; Step 5, performing microcapsule encapsulation and complex formation of tyvalosin, dissolving the purified tyvalosin in a phosphate buffer solution and adjusting the pH value to a weakly alkaline state, then mixing the prepared emulsion of microcapsule encapsulation material with the tyvalosin solution, and stirring for emulsification-solvent evaporation to form a tyvalosin-microcapsule complex; Step 6, application of the tyvalosin-microcapsule complex, first prepare liquid fertilizer, mix the formed tyvalosin-microcapsule complex with the required nutrient elements (nitrogen, phosphorus, potassium), plant growth regulators (gibberellic acid, auxin) in proportion, then stir evenly to prepare a tyvalosin finished liquid, and then use the prepared tyvalosin finished liquid to fertilize flowers.

[0005] As a further scheme of the present invention: in the step 1, in the process of synthesizing 1-ethyl-3-methylimidazolium bromide, the added amounts of 1-methylimidazole and ethyl bromide are both 0.5 mol-1 mol, the added amount of acetonitrile solvent is 500 mL-700 mL, the oil bath temperature is 60°C-80°C, the stirring speed is 300 r / min-500 r / min, the reaction time is 4h-6h, the reduced pressure distillation pressure after the reaction is completed is 5 kPa-10 kPa, and the temperature is gradually increased to 80°C-100°C.

[0006] As a further scheme of the present invention: in the step 1, in the preparation process of 1-ethyl-3-methylimidazolium acetate, the addition amount of 1-ethyl-3-methylimidazolium bromide is 0.4mol-0.5mol, the addition amount of silver acetate is 0.44mol-0.55mol, the addition amount of dichloromethane solvent is 400mL-500mL, the stirring speed at room temperature is 200r / min-300r / min, the stirring reaction time is 2h-4h, the pore size of the filter paper is 0.4μm-0.5μm, the reduced pressure distillation pressure is 3kPa-8kPa, and the temperature is set to 50℃-70℃.

[0007] As a further solution of the present invention: in the step 2, the tyvalosin finished liquid is transferred to a clean glass container, and then the pH thereof is adjusted to 5.5-7.5 by slowly adding 1 mol / L dilute hydrochloric acid and 1 mol / L sodium hydroxide solution, and then filtered using filter paper with a pore size of 1 μm-4 μm, and then the pretreated tyvalosin finished liquid and the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid are mixed in a glass extraction container at a volume ratio of 1:2.5-3.5, placed in a constant temperature water bath at 40°C-50°C, and subjected to an extraction operation at a stirring speed of 400r / min-500r / min for 1h-2h. After the extraction is completed, the mixed solution is transferred to a membrane separation device using an ultrafiltration membrane with a molecular weight cutoff of 3000Da, and the pressure is set to 0.2MPa-0.3MPa to allow it to pass through the ultrafiltration membrane.

[0008] As a further scheme of the present invention: in the step 4, the polylactic acid weighed is 100g-120g, the dichloromethane is 500mL-600mL, the magnetic stirrer is stirred at 500r / min-600r / min, the temperature is maintained at 25°C-30°C for stirring reaction, the added polysorbate-80 is 10g-15g, the added water content is 1000mL-1100mL, and the polylactic acid solution is slowly added dropwise to the aqueous phase at a dropping speed of 5mL / min-10mL / min, and an emulsion is formed under high-speed stirring at 1500r / min-2000r / min.

[0009] As a further scheme of the present invention: In the step 4, when preparing the smart response material, 50g-55g of N-isopropyl acrylamide monomer, 5g-10g of cross-linking agent N,N'-methylenebisacrylamide, and 1g-3g of initiator potassium persulfate are mixed in 1000mL-1100mL of water, the mixture is put into a three-necked flask, placed in an oil bath at 60℃-70℃, and stirred at 400r / min-500r / min for 3h-4h to form a thermosensitive hydrogel.

[0010] As a further embodiment of the present invention: in the step 5, after adding tyvalosin and dissolving it in the phosphate buffer solution, the pH value needs to be adjusted to 7.2-7.4, and the tyvalosin solution is formed at a ratio of 10 mL-13 mL of buffer solution per gram of tyvalosin, and the emulsification-solvent volatilization process is carried out at a temperature of 20° C.-25° C. and a stirring speed of 100 r / min-200 r / min.

[0011] As a further solution of the present invention: in the step six, the tyvalosin-microcapsule complex is mixed with ammonium nitrate (nitrogen element), potassium dihydrogen phosphate (phosphorus element), potassium chloride (potassium element), gibberellin and auxin in a mass ratio of 20-23:10-12:5-7:8-10:0.1-0.3:0.2-0.5, and the tyvalosin finished liquid is prepared at a temperature of 25°C-30°C and a stirring speed of 300r / min-400r / min.

[0012] As a further solution of the present invention: in the step six, during the rose planting process, the application amount per plant per week is 5mL-10mL in the seedling stage, the dilution multiple is 100 times, the application amount per plant per week in the growth stage is 15mL-20mL, the dilution multiple is 50 times, and the application amount per plant per week before flowering is 20mL-30mL, the dilution multiple is 30 times.

[0013] By adopting the above technical solution, compared with the prior art, the beneficial effects of the present invention are: 1. The present invention selects polylactic acid as the microcapsule encapsulation material, which can tightly and stably encapsulate tyvalosin, build an effective protective barrier, isolate the influence of adverse environmental factors on tyvalosin, and effectively ensure that the activity of tyvalosin is maintained during storage and subsequent applications. The temperature-sensitive hydrogel made of poly (N-isopropylacrylamide) is used as an intelligent response material. Its temperature-sensitive property is the key to realizing intelligent regulation. The hydrogel presents significantly different states at different temperatures. When the temperature is lower than 32°C, it is in a swollen state. At this time, its molecular chain stretches, which can limit the release of tyvalosin to a certain extent. When the temperature is higher than 32°C, the hydrogel shrinks rapidly, and the distance between the molecular chains becomes smaller, so that the tyvalosin encapsulated in the microcapsule can be released more smoothly. After tyvalosin is successfully encapsulated in the microcapsule to form a complex, it is further strengthened. The stability of tyvalosin is improved. This stability enables tyvalosin to maintain a good active state in the face of complex and changeable flower growth, and continue to provide strong support for flower growth. During the vigorous growth period of flowers, the ambient temperature is usually relatively high. At this time, the thermosensitive hydrogel shrinks due to the increase in temperature, and tyvalosin can accelerate the release rate, accurately and timely meeting the strong demand of flowers for the growth-promoting effect of tyvalosin at this critical growth stage. On the contrary, when flowers are in a dormant period or encounter unfavorable environmental conditions such as low temperature, the temperature decreases and causes the hydrogel to swell, and the release rate of tyvalosin slows down accordingly, effectively avoiding the waste of tyvalosin and the adverse effects on flowers such as overnutrition and growth disorders caused by unnecessary release, greatly improving the scientificity and accuracy of fertilization, and ensuring that flowers can obtain just the right nutrient supply at different growth stages; 2. The present invention endows 1-methylimidazole with strong nucleophilicity through the lone pair of electrons on the nitrogen atom in the heterocyclic structure, and ethyl bromide carries an active bromine atom, and the two undergo a nucleophilic substitution reaction to prepare 1-ethyl-3-methylimidazolium bromide. This intermediate product is further subjected to an ion exchange reaction with silver acetate in a dichloromethane solvent to generate a 1-ethyl-3-methylimidazolium acetate ionic liquid, and then the 1-ethyl-3-methylimidazolium acetate ionic liquid is prepared by an ion exchange reaction. The ionic liquid has a special ionic structure, and its cation part has a certain hydrophobicity, and the anion part has a certain hydrophilicity, forming a unique amphiphilic structure. This amphiphilic structure can make tyvalosin better dispersed in the system, which is convenient for extraction and separation operations. The tyvalosin finished liquid is mixed with the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid for extraction operation. In this process, the ionic liquid can fully contact and interact with the effective ingredients in the tyvalosin finished liquid. With the help of its solubility and selectivity, the tyvalosin is effectively extracted and preliminarily separated. The ionic liquid phase containing tyvalosin after membrane separation is mixed with n-hexane in a volume ratio for back extraction operation to achieve the purification of tyvalosin, so that it can play a role in a better state when it is subsequently used as an effective ingredient of liquid fertilizer; 3. In the present invention, the stability of tylvalosin is greatly improved after the composite is formed by microcapsule encapsulation. The microcapsule encapsulation material builds a solid protective barrier for tylvalosin, which can effectively resist the interference of external environmental factors such as temperature, pH value changes and microbial erosion, ensuring that tylvalosin always maintains good activity during storage and use. The tylvalosin-microcapsule composite is used to prepare liquid fertilizer and applied to flower fertilization. When preparing liquid fertilizer, the composite can be integrated with nutrients such as nitrogen, phosphorus, potassium and plant growth regulators to form a fertilizer system with balanced nutrition and good synergy, providing comprehensive and sufficient nutrient supply for flower growth. In the fertilization application link, it is applied to flowers according to the predetermined fertilization time, dosage and method. This precise fertilization strategy plays a vital role. Different growth multiples are diluted according to different flower growth stages, realizing the efficient supply and reasonable utilization of tylvalosin and other nutrients for flower growth, which can improve the quality and yield of flowers. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Schematic diagram of the method steps in an 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 provides a method for promoting the growth of flowers by using a tyvalosin finished liquid fertilizer. The method for promoting the growth of flowers by using a liquid fertilizer comprises the following specific steps: Step 1, first screen out 1-ethyl-3-methylimidazolium acetate ionic liquid for subsequent treatment, and the specific preparation process is as follows: first synthesize 1-ethyl-3-methylimidazolium bromide, add 1-methylimidazole and ethyl bromide into a three-necked flask, then add acetonitrile as a solvent, then place the three-necked flask in an oil bath for heating, and turn on a stirring device to react. After the reaction is completed, remove the solvent and unreacted raw materials through a vacuum distillation device until pure 1-ethyl-3-methylimidazolium bromide is obtained; Then, 1-ethyl-3-methylimidazolium acetate is prepared, the synthesized 1-ethyl-3-methylimidazolium bromide is transferred to a clean three-necked flask, and then silver acetate is added to carry out an ion exchange reaction, and dichloromethane is added as a solvent to fully dissolve the reactant, and a stirring device is turned on at room temperature. After the reaction is completed, the generated silver bromide precipitate is filtered out using filter paper, and then the solvent is removed by reduced pressure distillation to obtain 1-ethyl-3-methylimidazolium acetate ionic liquid by distillation; Step 2, transferring the tyvalosin finished liquid to a clean glass container and adjusting the pH value, then filtering with filter paper to complete the pretreatment of the tyvalosin finished liquid, and then mixing the pretreated tyvalosin finished liquid with the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid in a glass extraction container, placing it in a constant temperature water bath for heating and stirring to perform an extraction reaction, after the extraction is completed, transferring the mixed liquid to a membrane separation device for separation, and completing the ionic liquid-membrane separation coupling treatment; Step 3: After membrane separation, the ionic liquid phase containing tyvalosin that passes through the membrane is collected into a clean round-bottom flask, and the tyvalosin is recovered by a back extraction method. n-hexane is selected as an organic solvent, and the ionic liquid phase and n-hexane are mixed in a separatory funnel and shaken, and then allowed to stand for stratification, so that the tyvalosin is transferred to the n-hexane phase, and then the tyvalosin is recovered by distillation through a distillation device, and then the recovered tyvalosin is purified, and the recovered tyvalosin is dissolved in an ethanol solution, and the solution is slowly cooled in a low-temperature thermostatic bath. After the tyvalosin crystals are precipitated, it is filtered through a Buchner funnel with a microporous filter paper to obtain a higher purity tyvalosin; Step 4, preparing microcapsule encapsulation materials and smart response materials, first prepare microcapsule encapsulation materials, select polylactic acid as the material, weigh polylactic acid and dissolve it in dichloromethane, stir and mix with a magnetic stirrer in a well-ventilated environment until the polylactic acid is completely dissolved to form a uniform solution, and at the same time add polysorbate-80 to water to form an aqueous phase, and then slowly add the polylactic acid solution dropwise to the aqueous phase to form an emulsion under high-speed stirring to complete the preparation of microcapsule encapsulation materials, and then prepare smart response materials, mix N-isopropylacrylamide monomer, cross-linking agent N,N'-methylenebisacrylamide, and initiator potassium persulfate in water, put the mixture into a three-necked flask, place it in an oil bath and stir to perform a polymerization reaction to form a thermosensitive hydrogel, and complete the preparation of smart response materials; Step 5, performing microcapsule encapsulation and complex formation of tyvalosin, dissolving the purified tyvalosin in a phosphate buffer solution and adjusting the pH value to a weakly alkaline state, then mixing the prepared emulsion of microcapsule encapsulation material with the tyvalosin solution, and stirring for emulsification-solvent evaporation to form a tyvalosin-microcapsule complex; Step 6, application of the tyvalosin-microcapsule complex, first prepare liquid fertilizer, mix the formed tyvalosin-microcapsule complex with the required nutrient elements (nitrogen, phosphorus, potassium), plant growth regulators (gibberellic acid, auxin) in proportion, then stir evenly to prepare a tyvalosin finished liquid, and then use the prepared tyvalosin finished liquid to fertilize flowers.

[0018] In one embodiment of the present invention: in step 1, in the process of synthesizing 1-ethyl-3-methylimidazolium bromide, the added amounts of 1-methylimidazole and ethyl bromide are both 0.5 mol-1 mol, the added amount of acetonitrile solvent is 500 mL-700 mL, the oil bath temperature is 60°C-80°C, the stirring speed is 300 r / min-500 r / min, the reaction time is 4h-6h, the reduced pressure distillation pressure after the reaction is completed is 5 kPa-10 kPa, and the temperature is gradually increased to 80°C-100°C.

[0019] In one embodiment of the present invention: in step 1, in the preparation process of 1-ethyl-3-methylimidazolium acetate, the addition amount of 1-ethyl-3-methylimidazolium bromide is 0.4mol-0.5mol, the addition amount of silver acetate is 0.44mol-0.55mol, the addition amount of dichloromethane solvent is 400mL-500mL, the stirring speed at room temperature is 200r / min-300r / min, the stirring reaction time is 2h-4h, the pore size of the filter paper is 0.4μm-0.5μm, the reduced pressure distillation pressure is 3kPa-8kPa, and the temperature is set to 50℃-70℃.

[0020] In one embodiment of the present invention: in step 2, the tyvalosin finished liquid is transferred to a clean glass container, and then the pH is adjusted to 5.5-7.5 by slowly adding 1 mol / L dilute hydrochloric acid and 1 mol / L sodium hydroxide solution. After that, it is filtered using filter paper with a pore size of 1 μm-4 μm, and then the pretreated tyvalosin finished liquid and the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid are mixed in a glass extraction container at a volume ratio of 1:2.5-3.5, placed in a constant temperature water bath at 40°C-50°C, and extracted for 1h-2h at a stirring speed of 400r / min-500r / min. After the extraction is completed, the mixed solution is transferred to a membrane separation device using an ultrafiltration membrane with a molecular weight cutoff of 3000Da, and the pressure is set to 0.2MPa-0.3MPa to allow it to pass through the ultrafiltration membrane.

[0021] In one embodiment of the present invention: in step 4, the weighed polylactic acid is 100g-120g, the dichloromethane is 500mL-600mL, the magnetic stirrer is stirred at 500r / min-600r / min, the temperature is maintained at 25°C-30°C for stirring reaction, the added polysorbate-80 is 10g-15g, the added water content is 1000mL-1100mL, and the polylactic acid solution is slowly added dropwise to the aqueous phase at a dropping speed of 5mL / min-10mL / min, and an emulsion is formed under high-speed stirring at 1500r / min-2000r / min.

[0022] In one embodiment of the present invention: In step 4, when preparing the smart response material, 50g-55g of N-isopropyl acrylamide monomer, 5g-10g of cross-linking agent N,N'-methylenebisacrylamide, and 1g-3g of initiator potassium persulfate are mixed in 1000mL-1100mL of water, and the mixture is put into a three-necked flask, placed in an oil bath at 60℃-70℃, and stirred at 400r / min-500r / min for 3h-4h to form a thermosensitive hydrogel.

[0023] In one embodiment of the present invention: in step 5, after adding tyvalosin and dissolving it in the phosphate buffer solution, the pH value needs to be adjusted to 7.2-7.4, and the tyvalosin solution is formed at a ratio of 10 mL-13 mL of buffer solution per gram of tyvalosin, and the emulsification-solvent volatilization process is carried out at a temperature of 20° C.-25° C. and a stirring speed of 100 r / min-200 r / min.

[0024] In one embodiment of the present invention: in step six, the tyvalosin-microcapsule complex is mixed with ammonium nitrate (nitrogen element), potassium dihydrogen phosphate (phosphorus element), potassium chloride (potassium element), gibberellin and auxin in a mass ratio of 20-23:10-12:5-7:8-10:0.1-0.3:0.2-0.5, and the tyvalosin finished liquid is prepared at a temperature of 25°C-30°C and a stirring speed of 300r / min-400r / min.

[0025] In one embodiment of the present invention: in step six, during the rose flower planting process, the application amount per plant per week in the seedling stage is 5mL-10mL, and the dilution multiple is 100 times; the application amount per plant per week in the growth stage is 15mL-20mL, and the dilution multiple is 50 times; the application amount per plant per week before flowering is 20mL-30mL, and the dilution multiple is 30 times.

[0026] Example 1, please refer to the attached Figure 1First, 1-ethyl-3-methylimidazolium acetate ionic liquid was screened out for subsequent treatment. The specific preparation process was as follows: 1-ethyl-3-methylimidazolium bromide was first synthesized, 1 mol of 1-methylimidazole and 1 mol of ethyl bromide were added to a three-necked flask, and then 700 mL of acetonitrile was added as a solvent. The three-necked flask was then placed in an oil bath pot, the oil bath temperature was set to 80°C, and the stirring device was turned on at the same time. The stirring speed was set to 500r / min, and the reaction was continued for 6 hours. After the reaction was completed, the solvent and unreacted raw materials were removed by a vacuum distillation device. The pressure of the vacuum distillation was set to 10kPa, and the temperature was gradually increased to 100°C until pure 1-ethyl-3-methylimidazolium bromide was obtained, and then 1-ethyl-3-methylimidazolium acetate was prepared by transferring the synthesized 1-ethyl-3-methylimidazolium bromide to a clean three-necked flask, adding 0.5 mol of 1-ethyl-3-methylimidazolium bromide, and then adding 0.55 mol of silver acetate for ion exchange reaction, and adding 500 mL of dichloromethane as a solvent to fully dissolve the reactants, turning on the stirring device at room temperature, the stirring speed was 300 r / min, and the stirring reaction was carried out for 4 hours. After the reaction was completed, the generated silver bromide precipitate was filtered out using a filter paper with a pore size of 0.5 μm, and then the solvent was removed by vacuum distillation. The pressure of the vacuum distillation was 8 kPa, and the temperature was set to 70° C., and 1-ethyl-3-methylimidazolium acetate was obtained by distillation. The tyvalosin finished liquid was then transferred to a clean glass container, and its pH was adjusted to 7.5 by slowly adding 1 mol / L dilute hydrochloric acid and 1 mol / L sodium hydroxide solution. After that, the tyvalosin finished liquid was filtered using a filter paper with a pore size of 4 μm to complete the pretreatment of the tyvalosin finished liquid. The pretreated tyvalosin finished liquid was mixed with the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid in a volume ratio of 1:3.5 in a glass extraction container, placed in a 50°C constant temperature water bath, and extracted for 2 hours at a stirring speed of 500 r / min. After the extraction was completed, the mixed solution was transferred to a membrane separation device using an ultrafiltration membrane with a molecular weight cutoff of 3000 Da, and the pressure was set to 0.3 MPa to make it pass through the ultrafiltration membrane to complete the ionic liquid-membrane separation coupling treatment. After membrane separation, the ionic liquid phase containing tyvalosin that permeates the membrane is collected into a clean round-bottom flask, and the tyvalosin is recovered by the back extraction method. Select n-hexane as the organic solvent, mix the ionic liquid phase with n-hexane in a separating funnel at a volume ratio of 1:2.0, shake for 15 minutes, and then stand for 30 minutes to separate, so that the tyvalosin is transferred to the n-hexane phase, and then distilled and recovered by a distillation device at 80°C, and then the recovered tyvalosin is purified, and it is dissolved in an ethanol solution according to 15mL of ethanol per gram of recovered tyvalosin, and the solution is slowly cooled to -10°C in a low-temperature thermostatic bath. After the tyvalosin crystals are precipitated, the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0, and the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0. After the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0, the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0, and the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0. After the ionic liquid phase is mixed with n-hexane in a separating funnel, the ionic liquid phase is mixed with n-hexane in a separating funnel at a volume ratio of 1:2.0 ...22 μm microporous filter paper was filtered through a Buchner funnel to obtain tyvalocin with higher purity, and then the microcapsule encapsulation material and the intelligent response material were prepared. The microcapsule encapsulation material was prepared first, and polylactic acid was selected as the material. 120 g of polylactic acid was weighed and dissolved in 600 mL of dichloromethane. The solution was stirred at 600 r / min with a magnetic stirrer in a well-ventilated environment, and the temperature was maintained at 30 ° C until the polylactic acid was completely dissolved to form a uniform solution. At the same time, 15 g of polysorbate-80 was added to 1100 mL of water to form an aqueous phase, and the polylactic acid solution was slowly added dropwise to the aqueous phase at a dropping speed of 10 mL / min. 00r / min high-speed stirring to form an emulsion, complete the preparation of microcapsule encapsulation material, and then prepare the smart response material, select poly (N-isopropylacrylamide), according to the ratio of N-isopropylacrylamide monomer 55g, cross-linking agent N, N'-methylenebisacrylamide 10g, initiator potassium persulfate 3g mixed in 1100mL water, the mixture was put into a three-necked flask, placed in a 70℃ oil bath, stirred at 500r / min for 4h polymerization reaction to form a thermosensitive hydrogel, complete the preparation of smart response material, and then carry out microcapsule encapsulation and complex formation of tyvalocin, the purified tyvalocin was dissolved In a phosphate buffer solution, the pH value is then adjusted to 7.4, and a tyvalosin solution is formed according to a ratio of 13 mL of buffer solution per gram of tyvalosin. The prepared emulsion of microcapsule encapsulation material is mixed with the tyvalosin solution, and an emulsification-solvent volatilization process is performed at a temperature of 25° C. and a stirring speed of 200 r / min to form a tyvalosin-microcapsule complex. Finally, the tyvalosin-microcapsule complex is applied by first preparing a liquid fertilizer, and then the formed tyvalosin-microcapsule complex is mixed with the required nutrient elements (nitrogen, phosphorus, potassium) and plant growth regulators (gibberellic acid, auxin) in proportion. The tyvalosin-microcapsule complex is mixed with ammonium nitrate (nitrogen element), potassium dihydrogen phosphate (phosphorus element), potassium chloride (potassium element), gibberellin and auxin in a mass ratio of 23:12:7:10:0.3:0.5, and is prepared into a tyvalosin finished liquid at a temperature of 30°C and a stirring speed of 400r / min, and then applied for fertilization. In the process of rose flower planting, the application amount per plant per week is 10mL in the seedling stage, and the dilution multiple is 100 times; the application amount per plant per week in the growth stage is 20mL, and the dilution multiple is 50 times; the application amount per plant per week before flowering is 30mL, and the dilution multiple is 30 times. .

[0027] Example 2, please refer to the attached Figure 1First, 1-ethyl-3-methylimidazolium acetate ionic liquid was screened out for subsequent treatment. The specific preparation process was as follows: 1-ethyl-3-methylimidazolium bromide was first synthesized, 0.5 mol of 1-methylimidazole and 0.5 mol of ethyl bromide were added to a three-necked flask, and then 500 mL of acetonitrile was added as a solvent. The three-necked flask was then placed in an oil bath pot, the oil bath temperature was set to 60°C, and the stirring device was turned on at the same time. The stirring speed was set to 300 r / min, and the reaction was continued for 4 hours. After the reaction was completed, the solvent and unreacted raw materials were removed by a vacuum distillation device. The pressure of the vacuum distillation was set to 5 kPa, and the temperature was gradually increased to 80°C until pure 1-ethyl-3-methylimidazolium bromide was obtained, and then Then, 1-ethyl-3-methylimidazolium acetate was prepared. The synthesized 1-ethyl-3-methylimidazolium bromide was transferred to a clean three-necked flask. The amount of 1-ethyl-3-methylimidazolium bromide added was 0.4 mol. Then, 0.44 mol of silver acetate was added for ion exchange reaction. At the same time, 400 mL of dichloromethane was added as a solvent to fully dissolve the reactants. The stirring device was turned on at room temperature. The stirring speed was 200 r / min. The reaction was stirred for 2 hours. After the reaction was completed, the generated silver bromide precipitate was filtered out using a filter paper with a pore size of 0.4 μm, and the solvent was removed by vacuum distillation. The pressure of the vacuum distillation was 3 kPa, and the temperature was set to 50° C. 1-ethyl-3-methylimidazolium was obtained by distillation. Acetate ionic liquid, then, the tyvalosin finished liquid was transferred to a clean glass container, and its pH was adjusted to 5.5 by slowly adding 1 mol / L dilute hydrochloric acid and 1 mol / L sodium hydroxide solution. After that, the tyvalosin finished liquid was filtered with a filter paper with a pore size of 1 μm to complete the pretreatment of the tyvalosin finished liquid. Then, the pretreated tyvalosin finished liquid and the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid were mixed in a glass extraction container at a volume ratio of 1:2.5, placed in a 40°C constant temperature water bath, and extracted for 1 hour at a stirring speed of 400 r / min. After the extraction was completed, the mixed solution was transferred to a membrane separation device using an ultrafiltration membrane with a molecular weight cutoff of 3000 Da, and the pressure was set to 0. 2MPa to make it pass through the ultrafiltration membrane to complete the ionic liquid-membrane separation coupling treatment. After membrane separation, the ionic liquid phase containing tyvalosin that permeates the membrane is collected into a clean round-bottom flask, and the tyvalosin is recovered by the back extraction method. Select n-hexane as the organic solvent, mix the ionic liquid phase and n-hexane in a separating funnel at a volume ratio of 1:1.5, shake for 10 minutes, and then stand for 15 minutes to separate, so that the tyvalosin is transferred to the n-hexane phase, and then distilled and recovered at 60°C by a distillation device, and then the recovered tyvalosin is purified, and it is dissolved in an ethanol solution according to 10mL of ethanol per gram of recovered tyvalosin, and the solution is slowly cooled to -5°C in a low-temperature thermostatic bath. After the tyvalosin crystals are precipitated, the 0.The 22 μm microporous filter paper was filtered through a Buchner funnel to obtain tyvalocin with higher purity, and then the microcapsule encapsulation material and the intelligent response material were prepared. The microcapsule encapsulation material was prepared first, and polylactic acid was selected as the material. 100 g of polylactic acid was weighed and dissolved in 500 mL of dichloromethane. The solution was stirred at 500 r / min with a magnetic stirrer in a well-ventilated environment, and the temperature was maintained at 25 ° C until the polylactic acid was completely dissolved to form a uniform solution. At the same time, 10 g of polysorbate-80 was added to 1000 mL of water to form an aqueous phase, and the polylactic acid solution was slowly added dropwise to the aqueous phase at a dropping speed of 5 mL / min. 00r / min high-speed stirring to form an emulsion, complete the preparation of microcapsule encapsulation material, and then prepare the smart response material, select poly (N-isopropylacrylamide), according to the ratio of N-isopropylacrylamide monomer 50g, cross-linking agent N, N'-methylenebisacrylamide 5g, initiator potassium persulfate 1g mixed in 1000mL water, the mixture was put into a three-necked flask, placed in a 60℃ oil bath, stirred at 400r / min for 3h polymerization reaction to form a thermosensitive hydrogel, complete the preparation of smart response material, and then carry out microcapsule encapsulation and complex formation of tyvalocin, the purified tyvalocin was dissolved In a phosphate buffer solution, the pH value is then adjusted to 7.2, and a tyvalosin solution is formed according to a ratio of 10 mL of buffer solution per gram of tyvalosin. The prepared emulsion of microcapsule encapsulation material is mixed with the tyvalosin solution, and an emulsification-solvent volatilization process is performed at a temperature of 20°C and a stirring speed of 100 r / min to form a tyvalosin-microcapsule complex. Finally, the tyvalosin-microcapsule complex is applied by first preparing a liquid fertilizer, and then the formed tyvalosin-microcapsule complex is mixed with the required nutrient elements (nitrogen, phosphorus, potassium) and plant growth regulators (gibberellic acid, auxin) in proportion. , the tyvalosin-microcapsule complex is mixed with ammonium nitrate (nitrogen element), potassium dihydrogen phosphate (phosphorus element), potassium chloride (potassium element), gibberellin and auxin in a mass ratio of 20:10:5:8:0.1:0.2, and prepared into a tyvalosin finished liquid at a temperature of 25°C and a stirring speed of 300r / min, and then applied for fertilization. In the process of rose flower planting, the application amount per plant per week is 5mL in the seedling stage, and the dilution multiple is 100 times; the application amount per plant per week in the growth stage is 15mL, and the dilution multiple is 50 times; the application amount per plant per week before flowering is 20mL, and the dilution multiple is 30 times. .

[0028] According to the above two groups of embodiments, it can be concluded that through a series of rigorous and orderly steps, first, the 1-ethyl-3-methylimidazolium acetate ionic liquid is carefully prepared, then the tylvalosin finished liquid is carefully pretreated, the ionic liquid-membrane separation coupling treatment is carried out, the tylvalosin is recovered and purified, and the microcapsule encapsulation material and the intelligent response material are prepared separately, and then the microcapsule encapsulation and complex formation of tylvalosin are completed, and finally the application of tylvalosin-microcapsule complex in liquid fertilizer and the precise fertilization of rose flowers are realized. This series of processes cooperates and effectively improves the stability and effectiveness of tylvalosin in liquid fertilizer, and with the help of precise control of parameters in each link, efficient mixing and precise ratio between various substances are realized. At the same time, through the purification of tylvalosin and microencapsulation and other treatments, the high-precision output of its effect is guaranteed, which can achieve a good effect of promoting the growth of rose flowers. The method involved in the patent of the present invention has significant technical advantages and broad application prospects.

[0029] Although the present invention is disclosed as above in terms of preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art may make possible changes and modifications without departing from the spirit and scope of the present invention. Therefore, any modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention without departing from the content of the technical solution of the present invention shall fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for promoting flower growth using tyvalocin finished liquid fertilizer, characterized in that: The method for promoting flower growth with liquid fertilizer comprises the following specific steps: Step 1, first screen out 1-ethyl-3-methylimidazolium acetate ionic liquid for subsequent treatment, and the specific preparation process is as follows: first synthesize 1-ethyl-3-methylimidazolium bromide, add 1-methylimidazole and ethyl bromide into a three-necked flask, then add acetonitrile as a solvent, then place the three-necked flask in an oil bath for heating, and turn on a stirring device to react. After the reaction is completed, remove the solvent and unreacted raw materials through a vacuum distillation device until pure 1-ethyl-3-methylimidazolium bromide is obtained; Then, 1-ethyl-3-methylimidazolium acetate is prepared, the synthesized 1-ethyl-3-methylimidazolium bromide is transferred to a clean three-necked flask, and then silver acetate is added to carry out an ion exchange reaction, and dichloromethane is added as a solvent, and a stirring device is turned on at room temperature. After the reaction is completed, the generated silver bromide precipitate is filtered out using filter paper, and then the solvent is removed by reduced pressure distillation to obtain 1-ethyl-3-methylimidazolium acetate ionic liquid; Step 2, transferring the tyvalosin finished liquid to a clean glass container and adjusting the pH value, then filtering with filter paper to complete the pretreatment of the tyvalosin finished liquid, and then mixing the pretreated tyvalosin finished liquid with the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid in a glass extraction container, placing it in a constant temperature water bath for heating and stirring to perform an extraction reaction, after the extraction is completed, transferring the mixed liquid to a membrane separation device for separation, and completing the ionic liquid-membrane separation coupling treatment; Step 3, after membrane separation, collect the ionic liquid phase containing tyvalosin that passes through the membrane into a clean round-bottom flask, use a back extraction method to recover tyvalosin, select n-hexane as an organic solvent, mix the ionic liquid phase and n-hexane in a separatory funnel, shake, and then stand to separate, then distill and recover tyvalosin through a distillation device, then purify the recovered tyvalosin, and dissolve the recovered tyvalosin in an ethanol solution, slowly cool the solution in a low-temperature thermostatic bath, and after tyvalosin crystals are precipitated, filter through a Buchner funnel with a microporous filter paper to obtain tyvalosin with higher purity; Step 4, preparing microcapsule encapsulation materials and smart response materials, first prepare microcapsule encapsulation materials, select polylactic acid as the material, weigh polylactic acid and dissolve it in dichloromethane, stir and mix with a magnetic stirrer in a well-ventilated environment until the polylactic acid is completely dissolved to form a uniform solution, and at the same time add polysorbate-80 to water to form an aqueous phase, and then slowly add the polylactic acid solution dropwise to the aqueous phase to form an emulsion under high-speed stirring to complete the preparation of microcapsule encapsulation materials, and then prepare smart response materials, mix N-isopropylacrylamide monomer, cross-linking agent N,N'-methylenebisacrylamide, and initiator potassium persulfate in water, put the mixture into a three-necked flask, place it in an oil bath and stir to perform a polymerization reaction to form a thermosensitive hydrogel, and complete the preparation of smart response materials; Step 5, performing microcapsule encapsulation and complex formation of tyvalosin, dissolving the purified tyvalosin in a phosphate buffer solution and adjusting the pH value to a weakly alkaline state, then mixing the prepared emulsion of microcapsule encapsulation material with the tyvalosin solution, and stirring for emulsification-solvent evaporation to form a tyvalosin-microcapsule complex; Step 6, application of the tyvalosin-microcapsule complex, first prepare liquid fertilizer, mix the formed tyvalosin-microcapsule complex with the required nutrient elements (nitrogen, phosphorus, potassium), plant growth regulators (gibberellic acid, auxin) in proportion, then stir evenly to prepare a tyvalosin finished liquid, and then use the prepared tyvalosin finished liquid to fertilize flowers.

2. The method for promoting flower growth by using a tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step 1, in the process of synthesizing 1-ethyl-3-methylimidazolium bromide, the added amounts of 1-methylimidazole and ethyl bromide are both 0.5 mol-1 mol, the added amount of acetonitrile solvent is 500 mL-700 mL, the oil bath temperature is 60° C.-80° C., the stirring speed is 300 r / min-500 r / min, the reaction time is 4 h-6 h, the reduced pressure distillation pressure after the reaction is completed is 5 kPa-10 kPa, and the temperature is gradually increased to 80° C.-100° C.

3. The method for promoting flower growth by using a tyvalosin finished liquid fertilizer according to claim 1, characterized in that: In the step 1, in the preparation process of 1-ethyl-3-methylimidazolium acetate, the addition amount of 1-ethyl-3-methylimidazolium bromide is 0.4mol-0.5mol, the addition amount of silver acetate is 0.44mol-0.55mol, the addition amount of dichloromethane solvent is 400mL-500mL, the stirring speed at room temperature is 200r / min-300r / min, the stirring reaction time is 2h-4h, the pore size of the filter paper is 0.4μm-0.5μm, the reduced pressure distillation pressure is 3kPa-8kPa, and the temperature is set to 50℃-70℃.

4. The method for promoting flower growth by using a tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step 2, the tyvalosin finished liquid is transferred to a clean glass container, and then the pH is adjusted to 5.5-7.5 by slowly adding 1 mol / L dilute hydrochloric acid and 1 mol / L sodium hydroxide solution. After that, it is filtered using filter paper with a pore size of 1 μm-4 μm, and then the pretreated tyvalosin finished liquid and the prepared 1-ethyl-3-methylimidazolium acetate ionic liquid are mixed in a glass extraction container at a volume ratio of 1:2.5-3.5, placed in a constant temperature water bath at 40°C-50°C, and extracted for 1h-2h at a stirring speed of 400r / min-500r / min. After the extraction is completed, the mixed solution is transferred to a membrane separation device using an ultrafiltration membrane with a molecular weight cutoff of 3000Da, and the pressure is set to 0.2MPa-0.3MPa to allow it to pass through the ultrafiltration membrane.

5. The method for promoting flower growth by using a tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step 4, 100 g to 120 g of polylactic acid and 500 mL to 600 mL of dichloromethane are weighed, the magnetic stirrer is stirred at 500 r / min to 600 r / min, the temperature is maintained at 25° C. to 30° C. for stirring reaction, 10 g to 15 g of polysorbate 80 is added, the content of water added is 1000 mL to 1100 mL, and the polylactic acid solution is slowly added dropwise to the aqueous phase at a dropping speed of 5 mL / min to 10 mL / min, and an emulsion is formed under high-speed stirring at 1500 r / min to 2000 r / min.

6. The method for promoting flower growth by using a tyvalosin finished liquid fertilizer according to claim 1, characterized in that: In the step 4, when preparing the smart response material, 50g-55g of N-isopropyl acrylamide monomer, 5g-10g of cross-linking agent N,N'-methylenebisacrylamide, and 1g-3g of initiator potassium persulfate are mixed in 1000mL-1100mL of water, the mixture is put into a three-necked flask, placed in an oil bath at 60°C-70°C, and stirred at 400r / min-500r / min for 3h-4h for polymerization reaction to form a thermosensitive hydrogel.

7. The method for promoting flower growth by using tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step 5, after adding tyvalosin and dissolving it in the phosphate buffer solution, the pH value needs to be adjusted to 7.2-7.4, and the tyvalosin solution is formed according to the ratio of 10 mL-13 mL of buffer solution per gram of tyvalosin, and the emulsification-solvent volatilization process is carried out at a temperature of 20° C.-25° C. and a stirring speed of 100 r / min-200 r / min.

8. The method for promoting flower growth by using a tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step six, the tyvalosin-microcapsule complex is mixed with ammonium nitrate (nitrogen element), potassium dihydrogen phosphate (phosphorus element), potassium chloride (potassium element), gibberellin and auxin in a mass ratio of 20-23:10-12:5-7:8-10:0.1-0.3:0.2-0.5, and the tyvalosin finished liquid is prepared at a temperature of 25°C-30°C and a stirring speed of 300r / min-400r / min.

9. The method for promoting flower growth by using a tyvalocin finished liquid fertilizer according to claim 1, characterized in that: In the step six, during the rose planting process, the application amount per plant per week in the seedling stage is 5mL-10mL, the dilution multiple is 100 times, the application amount per plant per week in the growth stage is 15mL-20mL, the dilution multiple is 50 times, and the application amount per plant per week before flowering is 20mL-30mL, the dilution multiple is 30 times.

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