Insect-expelling and weight-gaining microcapsule and preparation method thereof

Abstract

The invention discloses an insect-expelling and weight-gaining microcapsule and a preparation method thereof. The insect-expelling and weight-increasing microcapsule comprises a shell material and a core material, the shell material comprises urea resin / nano tourmaline, and the core material comprises one or more of an insecticide and a plant extract; a metal chelate is loaded on the surface of the shell material. The insect-expelling and weight-increasing microcapsule disclosed by the invention not only can efficiently and lastingly expel insects around potted plants and kill possible eggs, but also can slowly release nutrient substances required by growth of crops, thereby providing a brand new thought for development of slow-release fertilizers.

Description

Technical Field

[0001] This invention belongs to the field of soil remediation, specifically relating to an insect-repellent and fertilizer-enhancing microcapsule and its preparation method. Background Technology

[0002] Scientific research shows that green plants play an irreplaceable role in improving indoor and outdoor air quality, regulating humidity, and reducing noise pollution. However, in actual flower cultivation, while traditional self-watering basins simplify the watering process to some extent, they also expose many problems, such as mosquito breeding caused by high soil moisture and plant growth problems caused by nutrient loss.

[0003] CN117247301A discloses a gel fertilizer suitable for potted plant cultivation. This fertilizer consists of a hydrogel encapsulating soluble fertilizer, fragrance, insect repellent, etc., forming a cross-linked film on the hydrogel surface through secondary cross-linking, giving the fertilizer a slow-release effect. However, this product still has limitations such as unsatisfactory slow-release effect, the need for frequent re-fertilization, and poor mosquito repellent effect. Therefore, it is necessary to develop a more advanced and comprehensive potted plant fertilizer. Summary of the Invention

[0004] To address the problems existing in the prior art, this invention provides an insect-repelling and fertilizer-enhancing microcapsule and its preparation method. The insect-repelling and fertilizer-enhancing microcapsule of this invention can not only efficiently and persistently repel insects around potted plants and kill any potential insect eggs, but also slowly release nutrients needed for crop growth, providing a novel approach to the development of slow-release fertilizers.

[0005] The first aspect of the present invention provides an insect repellent and weight gain microcapsule, the insect repellent and weight gain microcapsule comprising a shell material and a core material, the shell material comprising urea-formaldehyde resin (UF) / nano-tourmaline, the core material comprising one or more of an insecticide and a plant extract; the surface of the shell material is loaded with a metal chelate.

[0006] Furthermore, the diameter of the insect-repelling and fattening microcapsules is 3-20 μm.

[0007] Furthermore, the mass ratio of the shell material to the core material of the insect-repelling and fattening microcapsule is 1:(0.5-2.5).

[0008] Furthermore, the core material preferably comprises both an insecticide and a plant extract. The mass ratio of the insecticide to the plant extract is 1:(0.5-4).

[0009] Furthermore, the insecticide is one or more of the following: neonicotinoid insecticides, pyrethroid insecticides, and insect growth regulator insecticides.

[0010] Furthermore, the number of carbon atoms in the neonicotinoid insecticide is >6; preferably, it is one or more of imidacloprid, acetamiprid, flonicamid, dinotefuran, chlorthiazoline, and thiamethoxam.

[0011] Furthermore, the pyrethroid insecticide has >21 carbon atoms; preferably, it is one or more of cypermethrin, bifenthrin, deltamethrin, cypermethrin, ethionyl cyanide, and deltamethrin.

[0012] Furthermore, the insect growth regulator insecticide has >20 carbon atoms; preferably, it is one or more of chlorfenapyr, tebufenozide, methoxyfenozide, and cyclotebufenozide.

[0013] Furthermore, the boiling point of the plant extract is >160℃; preferably, it is one or more of lemon essential oil, camphor essential oil, and peppermint essential oil.

[0014] Furthermore, in the shell material, the mass ratio of urea-formaldehyde resin to nano-tourmaline is (2-10):1.

[0015] Furthermore, the shell material surface is loaded with a metal chelate, wherein the metal is preferably one or more of iron, manganese, zinc, copper, calcium, and nickel.

[0016] Furthermore, the shell material surface is loaded with metal chelates, and the metal loading accounts for 0.1wt%-2wt% of the total mass of the insect-repellent and fattening microcapsules.

[0017] A second aspect of the present invention provides a method for preparing insect-repellent and weight-enhancing microcapsules, comprising:

[0018] S1: Mix nano-tourmaline powder, surfactant and solvent, modify under stirring, wash after modification, freeze dry to obtain modified nano-tourmaline powder;

[0019] S2: Mix one or more of the insecticide and plant extract to obtain the core material mixture;

[0020] S3: Add the modified nano-tourmaline powder obtained in step S1 and the core material mixture obtained in step S2 to the urea aqueous solution and stir.

[0021] S4: Add formaldehyde solution to the reaction system of step S3, and carry out the reaction under stirring. After the reaction is completed, the mixture is aged, washed, filtered, and freeze-dried to obtain the insect-repellent and fattening microcapsule matrix.

[0022] S5: Disperse the insect-repellent and fattening microcapsule matrix obtained in step S4 in methanol, then add a coupling agent methanol solution, adjust the pH value, process under stirring, then filter, wash, and freeze dry.

[0023] S6: Disperse the solid powder obtained after freeze-drying in step S5 in a buffer solution, add a chelating agent, process under stirring, filter, wash, and freeze-dry.

[0024] S7: Disperse the solid powder obtained after freeze-drying in step S6 in a metal ion salt - N,N-dimethylformamide (DMF) solution, and process it with stirring. After the reaction is complete, filter, wash, and freeze-dry to obtain insect-repellent and fattening microcapsules.

[0025] Furthermore, in step S1, the particle size of the nano-tourmaline powder is 10-100 nm.

[0026] Further, in step S1, the surfactant is an anionic surfactant, preferably at least one of sodium dodecylbenzenesulfonate (SDBS), sodium dodecyl sulfate (SDS), and 2-morpholine ethanesulfonic acid, and more preferably sodium dodecylbenzenesulfonate.

[0027] Further, in step S1, the solvent is an aprotic solvent with a boiling point >100℃, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide, and more preferably formamide.

[0028] Further, in step S1, the mass ratio of the nano-tourmaline powder to the surfactant is (1-10):1, and the mass ratio of the solvent to the surfactant is (20-40):1.

[0029] Further, in step S1, the stirring speed is 400-600 rpm; the modification temperature is 100-200℃; and the modification time is 4-8 hours.

[0030] Furthermore, in step S1, the freeze-drying conditions are: vacuum drying for 4-8 hours at a temperature of -40°C to -20°C.

[0031] Further, in step S2, the mixing is carried out under stirring, the stirring speed is 300-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 3-10 minutes.

[0032] Further, in step S3, the mass ratio of urea to water in the aqueous solution of urea is 1:(5-50).

[0033] Furthermore, in step S3, the pH of the urea aqueous solution is adjusted to 2.5-5.5 before use. The pH can be adjusted using organic acids, such as one or more of citric acid, formic acid, and acetic acid.

[0034] Further, in step S3, the mass ratio of the core material mixture to the modified nano-tourmaline powder is 1:(0.1-0.5); the mass ratio of the core material mixture to urea is 1:(0.2-1).

[0035] Furthermore, in step S3, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 1-2 hours.

[0036] Further, in step S4, the formaldehyde solution is an aqueous solution of formaldehyde with a mass concentration of 35%-40%. The amount of formaldehyde solution added satisfies the molar ratio of formaldehyde to urea in the reaction system of step S3 as (1.5-2.5):1.

[0037] Furthermore, in step S4, the stirring speed is 400-600 rpm, the stirring temperature is 50-80℃, and the reaction time under stirring is 4-6 hours.

[0038] Further, in step S4, the aging conditions are: standing at 50-80℃ for 1-12 hours. The freeze-drying conditions are: vacuum drying at -40--20℃ for 4-8 hours.

[0039] Furthermore, in step S5, the insect-repellent and fattening microcapsule matrix is ​​dispersed in methanol, which can be achieved by ultrasonic dispersion.

[0040] Further, in step S5, the coupling agent methanol solution is prepared by mixing the coupling agent and methanol, and the mass ratio of methanol to coupling agent is (1-15):1.

[0041] Further, in step S5, the coupling agent is a silane coupling agent, preferably at least one of 3-chloropropyltrimethylsilane, (dichloromethyl)trimethylsilane, (trichloromethyl)trimethylsilane, and (chlorodifluoromethyl)trimethylsilane, and more preferably 3-chloropropyltrimethylsilane.

[0042] Further, in step S5, the mass ratio of methanol to the insect-repellent and fattening microcapsule matrix is ​​(1-20):1. The mass ratio of the coupling agent methanol solution to the insect-repellent and fattening microcapsule matrix is ​​(0.1-10):1.

[0043] Furthermore, in step S5, the pH can be adjusted using an alkaline solution, such as ammonia.

[0044] Furthermore, in step S5, the stirring speed is 200-450 rpm; the processing temperature is 40-60℃; and the processing time is 4-6 hours.

[0045] Furthermore, in step S5, the treatment is carried out under the protection of nitrogen or an inert gas.

[0046] Furthermore, in step S5, the freeze-drying conditions are: vacuum drying at -40°C to -20°C for 4-8 hours.

[0047] Furthermore, in step S6, the dispersion can be carried out by ultrasonic dispersion.

[0048] Furthermore, the buffer solution mentioned in step S6 is preferably one or more of phosphate buffer and carbonate buffer, and more preferably carbonate buffer.

[0049] Further, in step S6, the pH value of the buffer solution is 9-12.

[0050] Further, in step S6, the mass ratio of the buffer solution to the solid powder obtained after lyophilization in step S5 is (5-50):1.

[0051] Further, in step S6, the chelating agent has a ligand tooth number >2, preferably iminodiacetic acid, triethylenediamine, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, aminotriacetic acid, hydroxyethylethylenediaminetriacetic acid, dihydroxyethylglycine, and more preferably ethylenediaminetetraacetic acid.

[0052] Furthermore, in step S6, the stirring speed is 200-450 rpm, the processing temperature is 40-60℃, and the processing time is 2-5 hours.

[0053] Furthermore, in step S6, the freeze-drying conditions are: vacuum drying at -40°C to -20°C for 4-8 hours.

[0054] Furthermore, in step S7, the solid powder obtained after drying in step S6 is dispersed in a metal ion salt-DMF (N,N-dimethylformamide) solution, which can be done by ultrasonic dispersion.

[0055] Further, in step S7, the metal ion salt is preferably one or more of iron ion salt, manganese ion salt, zinc ion salt, copper ion salt, calcium ion salt, and nickel ion salt, and more preferably one or more of ferric chloride, manganese chloride, zinc chloride, copper chloride, calcium chloride, and nickel chloride.

[0056] Further, in step S7, the molar ratio of the metal ion salt to DMF in the metal ion salt-DMF solution is (0.1-2):1.

[0057] Further, in step S7, the mass ratio of the metal ion salt-DMF solution to the solid powder obtained after drying in step S6 is (10-30):1.

[0058] Furthermore, in step S7, the stirring speed is 200-450 rpm, the processing temperature is 100-150℃, and the processing time is 2-5 hours.

[0059] Furthermore, in step S7, the freeze-drying conditions are: vacuum drying at -40°C to -20°C for 4-8 hours.

[0060] Compared with the prior art, the present invention has the following advantages:

[0061] (1) The insect-repellent and fertilizer-enhancing microcapsules of the present invention have a shell material comprising a composite shell material of urea-formaldehyde resin / nano-tourmaline. In the preparation process of the insect-repellent and fertilizer-enhancing microcapsules, nano-tourmaline powder can replace the template agent in the synthesis of microcapsules to maintain the stability of the microcapsule core material droplets. In addition, in the process of modifying the shell material with metal ions, the negative ion field released by tourmaline can adsorb metal ions onto the surface of the microcapsules, effectively increasing the loading of trace metal ions on the shell material of the microcapsules. Furthermore, after being sprinkled on the soil surface, the nano-tourmaline powder contained inside the shell material of the insect-repellent and fertilizer-enhancing microcapsules will release a negative ion field, which has the effects of purifying the air, promoting crop metabolism, enhancing crop enzyme activity, and promoting crop photosynthesis, thereby achieving the purpose of promoting plant growth.

[0062] (2) The insect-repellent and fattening microcapsules of the present invention have a non-toxic and harmless urea-formaldehyde resin shell material that can be degraded in the soil by the combined action of microorganisms and water, continuously releasing nitrogen and various trace metal elements immobilized on its surface, thereby achieving the purpose of long-term fattening.

[0063] (3) The insect-repellent and fattening microcapsules of the present invention encapsulate various insecticides and volatile essential oils in a urea-formaldehyde resin / nano-tourmaline composite shell. The volatile essential oils and insecticides can be released slowly together to kill insect eggs, keep insects away from the planting area, avoid the impact of insects on plants and people, and have a long-lasting insect-repellent effect. Attached Figure Description

[0064] Figure 1 The image shown is a scanning electron microscope (SEM) image of the insect-repelling and fattening microcapsules obtained in Example 1. Detailed Implementation

[0065] To further illustrate the relevant features and technical means of the present invention, the present invention will be clearly and thoroughly described below in conjunction with embodiments.

[0066] The morphology of the insect-repellent and fattening microcapsules of this invention was tested using a ZEISS Supra 55 scanning electron microscope with an accelerating voltage of 20kV. Since the microcapsule wall material is non-conductive, the samples need to be sputtered with gold before testing.

[0067] The insect-repellent and fattening microcapsules of the present invention were subjected to surface elemental testing using an X-ray energy dispersive spectroscopy (EDS) instrument to confirm that metal ions were successfully modified onto the surface of the microcapsules.

[0068] In this invention, the weight gain effect is evaluated using the following method:

[0069] The insect-repellent and fertilizer-enhancing microcapsules were mixed with air-dried soil using a mixing machine at a mass ratio of 1:100. The soil was then placed in self-watering potted planters (30cm in diameter and 15cm in height, with a water-filled inner pot at the bottom to slowly supply water to the upper soil) and wheatgrass was planted. The planters were then moved to a planting area for a potted plant experiment, and the growth height of the wheatgrass was monitored after 28 days.

[0070] In this invention, the insect-repelling effect is evaluated using the following method:

[0071] A low-powered light source of the same size was placed on top of the potted planters. On the nights of the 7th and 28th days (6 p.m. to 7 a.m. the next day), the number of insects above the planters was monitored and recorded using a camera to examine the insect repellent effect.

[0072] Example 1

[0073] S1: Add tourmaline powder with a particle size of 80nm, sodium dodecylbenzenesulfonate and formamide to the first container. The mass ratio of tourmaline powder, sodium dodecylbenzenesulfonate and formamide is 3:1:30. Stir at 400 rpm for 5 hours at 140℃ to modify the surface of the nano tourmaline powder. After modification, wash the modified nano tourmaline with ethanol several times and vacuum dry at -30℃ for 5 hours for later use.

[0074] S2: Add fipronil, cypermethrin, tebufenozide and lemon essential oil in a mass ratio of 1:1:1:6 to the second container, and stir at 400 rpm for 5 minutes at 50°C to obtain the core material mixture.

[0075] S3: Add urea and deionized water in a mass ratio of 1:10 to the third container, stir at 400 rpm for 1 hour at 50°C, and then adjust the pH of the system to 4 using acetic acid.

[0076] Then add the modified nano tourmaline powder and core material mixture, with a mass ratio of core material mixture, urea and modified nano tourmaline powder of 4:2:1, and continue stirring at 400 rpm for 1 hour at 50°C.

[0077] S4: Add 37wt% formaldehyde solution, with a molar ratio of urea to formaldehyde of 1:2, raise the reaction temperature to 65℃, stir the reaction for 6 hours, keep the reaction temperature constant after stirring, age for 2 hours, filter and wash the solid in the reaction system after aging, and vacuum dry at -30℃ for 5 hours to obtain the insect-repellent and fattening microcapsule matrix.

[0078] S5: The insect-repellent and fattening microcapsule matrix was dispersed in methanol by ultrasonic dispersion, and then 20 wt% 3-chloropropyltrimethylsilane methanol solution was added dropwise. The pH value was adjusted to 11 with ammonia water. The mixture was stirred for 5 hours at 400 rpm and 60°C. The mass ratio of methanol, insect-repellent and fattening microcapsule matrix and 3-chloropropyltrimethylsilane methanol solution was 5:1:1. The reaction was carried out under nitrogen protection throughout. After stirring, the solid powder was filtered, washed, and vacuum dried at -30°C for 5 hours.

[0079] S6: The solid powder obtained in step S5 is ultrasonically dispersed in a carbonate buffer solution with pH=11, and then ethylenediaminetetraacetic acid is added. The mass ratio of carbonate buffer solution, solid powder and ethylenediaminetetraacetic acid is 200:15:1. The mixture is stirred for 5 hours at 400 rpm and 50°C. After stirring, the solid powder is filtered, washed and vacuum dried at -30°C for 5 hours.

[0080] S7: The solid powder obtained in step S6 is ultrasonically dispersed in a metal ion salt-DMF solution. The molar ratio of metal ions to DMF is 0.5:1. The metal ion salts are copper chloride, zinc chloride, manganese chloride, and calcium chloride in the same molar ratio. The mass ratio of solid powder to metal ion salt-DMF solution is 1:20. The mixture is stirred at 400 rpm and 140°C for 5 hours. After stirring, the solid powder is filtered, washed, and vacuum dried at -30°C for 5 hours to obtain the insect-repellent and fattening microcapsules. The electron micrograph is shown below. Figure 1 .

[0081] Example 2

[0082] Except for step S2, in which chlorothiazoline, deltamethrin, cypermethrin, and peppermint oil are added to the second container in a mass ratio of 1:1:1:6, the rest is the same as in Example 1.

[0083] Example 3

[0084] Except for step S2, in which fipronil, cypermethrin, tebufenozide, and lemon essential oil are added to the second container in a mass ratio of 1:1:1:2, the rest is the same as in Example 1.

[0085] Example 4

[0086] Except for step S3, where the mass ratio of the core material mixture, urea, and modified nano-tourmaline powder is 4:4:1, the rest is the same as in Example 1.

[0087] Example 5

[0088] Except for step S5, where the silane coupling agent is (dichloromethyl)trimethylsilane, the rest is the same as in Example 1.

[0089] Example 6

[0090] Except for the chelating agent being iminodiacetic acid in step S6, the rest is the same as in Example 1.

[0091] Example 7

[0092] Except for step S7, where the metal ion salts are manganese chloride, calcium chloride, nickel chloride, and ferric chloride in the same molar ratio, the rest is the same as in Example 1.

[0093] Comparative Example 1

[0094] A comparative planting experiment was conducted by spreading air-dried soil without insect-repellent and fertilizer-enhancing microcapsules in self-watering potted plants.

[0095] Comparative Example 2

[0096] A mixture of fipronil, cypermethrin, tebufenozide, and lemon essential oil in a mass ratio of 1:1:1:6 was sprayed onto the surface of air-dried soil. The mass ratio of air-dried soil to the mixture was 100:1. The soil was then thoroughly turned over, and the air-dried soil was further placed in a self-watering pot for a planting experiment.

[0097] Comparative Example 3

[0098] S1: Add tourmaline powder with a particle size of 80nm, sodium dodecylbenzenesulfonate and formamide to the first container. The mass ratio of tourmaline powder, sodium dodecylbenzenesulfonate and formamide is 3:1:30. Stir at 400 rpm for 5 hours at 140℃ to modify the surface of the nano tourmaline powder. After modification, wash the modified nano tourmaline with ethanol several times and vacuum dry at -30℃ for 5 hours for later use.

[0099] S2: Add fipronil, cypermethrin, tebufenozide and lemon essential oil in a mass ratio of 1:1:1:6 to the second container, and stir at 400 rpm for 5 minutes at 50°C to obtain the core material mixture.

[0100] S3: Add urea and deionized water in a mass ratio of 1:10 to the third container, stir at 400 rpm for 1 hour at 50°C, and then adjust the pH of the system to 4 using acetic acid.

[0101] Then add the modified nano tourmaline powder and core material mixture, with a mass ratio of core material mixture, urea and modified nano tourmaline powder of 4:2:1, and continue stirring at 400 rpm for 1 hour at 50°C.

[0102] S4: Add 37wt% formaldehyde solution, with a molar ratio of urea to formaldehyde of 1:2, raise the reaction temperature to 65℃, stir the reaction for 6 hours, keep the reaction temperature constant after stirring, age for 2 hours, filter and wash the solid in the reaction system after aging, and vacuum dry at -30℃ for 5 hours to obtain insect-repellent and fattening microcapsules.

[0103] Comparative Example 4

[0104] S1: Add urea and deionized water in a mass ratio of 1:10 to the container, stir at 400 rpm for 1 hour at 50°C, and then adjust the pH of the system to 4 using acetic acid.

[0105] S2: Add 37wt% formaldehyde solution, with a molar ratio of urea to formaldehyde of 1:2, raise the reaction temperature to 65℃, stir the reaction for 6 hours, keep the reaction temperature constant after stirring, age for 2 hours, filter and wash the solid in the reaction system after aging, and vacuum dry at -30℃ for 5 hours to obtain the fertilizer matrix.

[0106] S3: The fertilizer matrix was dispersed in methanol by ultrasonic dispersion, and then 20 wt% 3-chloropropyltrimethylsilane methanol solution was added dropwise. The pH was adjusted to 11 with ammonia. The mixture was stirred for 5 hours at 400 rpm and 60°C. The mass ratio of methanol, fertilizer matrix and 3-chloropropyltrimethylsilane methanol solution was 5:1:1. The reaction was carried out under nitrogen protection throughout. After stirring, the solid powder was filtered, washed and vacuum dried at -30°C for 5 hours.

[0107] S4: The solid powder obtained in step S3 is ultrasonically dispersed in a carbonate buffer solution with pH=11, and then ethylenediaminetetraacetic acid is added. The mass ratio of carbonate buffer solution, solid powder and ethylenediaminetetraacetic acid is 200:15:1. The mixture is stirred for 5 hours at 400 rpm and 50°C. After stirring, the solid powder is filtered, washed and vacuum dried at -30°C for 5 hours.

[0108] S5: The solid powder obtained in step S4 is ultrasonically dispersed in a metal ion salt-DMF solution. The molar ratio of metal ion salt to DMF is 0.5:1. The metal ion salts are copper chloride, zinc chloride, manganese chloride, and calcium chloride with the same molar ratio. The mass ratio of solid powder to metal ion salt-DMF solution is 1:20. The mixture is stirred at 400 rpm and 140°C for 5 hours. After stirring, the solid powder is filtered, washed, and vacuum dried at -30°C for 5 hours to obtain the fertilizer granules.

[0109] Comparative Example 5

[0110] S1: Add fipronil, cypermethrin, tebufenozide and lemon essential oil in a mass ratio of 1:1:1:6 to the first container, and stir at 400 rpm for 5 minutes at 50°C to obtain the core material mixture.

[0111] S2: Add urea and deionized water in a mass ratio of 1:10 to the second container, stir at 400 rpm for 1 hour at 50°C, and then adjust the pH of the system to 4 using acetic acid.

[0112] Then add sodium dodecylbenzenesulfonate and core material mixture, with a mass ratio of core material mixture, urea and sodium dodecylbenzenesulfonate of 4:2:0.5, and continue stirring at 400 rpm for 1 hour at 50°C.

[0113] S3: Add 37wt% formaldehyde solution, with a molar ratio of urea to formaldehyde of 1:2, raise the reaction temperature to 65℃, stir the reaction for 6 hours, keep the reaction temperature constant after stirring, age for 2 hours, filter and wash the solid in the reaction system after aging, and vacuum dry at -30℃ for 5 hours to obtain the insect-repellent and fattening microcapsule matrix.

[0114] S4: The insect-repellent and fattening microcapsule matrix was dispersed in methanol by ultrasonic dispersion, and then 20 wt% 3-chloropropyltrimethylsilane methanol solution was added dropwise. The pH value was adjusted to 11 with ammonia water. The mixture was stirred for 5 hours at 400 rpm and 60°C. The mass ratio of methanol, insect-repellent and fattening microcapsule matrix and 3-chloropropyltrimethylsilane methanol solution was 5:1:1. The reaction was carried out under nitrogen protection throughout. After stirring, the solid powder was filtered, washed, and vacuum dried at -30°C for 5 hours.

[0115] S5: The solid powder obtained in step S4 is ultrasonically dispersed in a carbonate buffer solution with pH=11, and then ethylenediaminetetraacetic acid is added. The mass ratio of carbonate buffer solution, solid powder and ethylenediaminetetraacetic acid is 200:15:1. The mixture is stirred for 5 hours at 400 rpm and 50°C. After stirring, the solid powder is filtered, washed and vacuum dried at -30°C for 5 hours.

[0116] S6: The solid powder obtained in step S5 is ultrasonically dispersed in a metal ion salt-DMF solution. The molar ratio of metal ion salt to DMF is 0.5:1. The metal ion salts are copper chloride, zinc chloride, manganese chloride, and calcium chloride with the same molar ratio. The mass ratio of solid powder to metal ion salt-DMF solution is 1:20. The mixture is stirred at 400 rpm and 140°C for 5 hours. After stirring, the solid powder is filtered, washed, and vacuum dried at -30°C for 5 hours to obtain insect-repellent and fattening microcapsules.

[0117] Table 1 Results of weight gain and deworming tests for each case.

[0118]

[0119]

[0120] It should be emphasized that the above-mentioned content is only a specific embodiment of the present invention and should not be construed as limiting the present invention to the above description in specific implementation. For researchers and those skilled in the art to which this invention pertains, any simple deductions and improvements made without departing from the spirit and principles of the present invention should be considered within the scope of protection of the present invention.

Claims

1. A type of insect-repelling and weight-gaining microcapsule, characterized in that, The insect-repellent and fattening microcapsule comprises a shell material and a core material. The shell material comprises urea-formaldehyde resin / nano-tourmaline, and the core material comprises one or more of insecticides and plant extracts. The surface of the shell material is loaded with metal chelates.

2. The insect-repelling and weight-enhancing microcapsule according to claim 1, characterized in that, The diameter of the insect-repelling and fattening microcapsules is 3-20 μm; And / or, the mass ratio of the shell material to the core material of the insect-repellent and fattening microcapsule is 1:(0.5-2.5).

3. The insect-repelling and weight-enhancing microcapsule according to claim 1, characterized in that, The core material includes both insecticide and plant extract; the mass ratio of the insecticide to the plant extract is 1:(0.5-4).

4. The insect-repelling and weight-gaining microcapsule according to claim 1 or 3, characterized in that, The insecticide is one or more of the following: neonicotinoid insecticides, pyrethroid insecticides, and insect growth regulator insecticides. Preferably, the neonicotinoid insecticide has >6 carbon atoms; preferably, it is one or more of imidacloprid, acetamiprid, flonicamid, dinotefuran, chlorpyrifos, and thiamethoxam. And / or, the pyrethroid insecticide has >21 carbon atoms; preferably, it is one or more of cypermethrin, bifenthrin, deltamethrin, cypermethrin, ethionyl cyanide, and deltamethrin. And / or, the number of carbon atoms in the insect growth regulator insecticide is >20; preferably, it is one or more of chlorfenapyr, tebufenozide, methoxyfenozide, and cyclotebufenozide; And / or, the boiling point of the plant extract is >160°C; preferably one or more of lemon essential oil, camphor essential oil, and peppermint essential oil.

5. The insect-repelling and weight-enhancing microcapsule according to claim 1, characterized in that, In the shell material, the mass ratio of urea-formaldehyde resin to nano-tourmaline is (2-10):

1.

6. The insect-repelling and weight-enhancing microcapsule according to claim 1, characterized in that, The shell material surface is loaded with a metal chelate, wherein the metal is preferably one or more of iron, manganese, zinc, copper, calcium, and nickel; And / or, the metal loading accounts for 0.1wt%-2wt% of the total mass of the insect-repellent and fattening microcapsules.

7. The method for preparing the anthelmintic and fattening microcapsules according to any one of claims 1-6, comprising: S1: Mix nano-tourmaline powder, surfactant and solvent, modify under stirring, wash after modification, freeze dry to obtain modified nano-tourmaline powder; S2: Mix one or more of the insecticide and plant extract to obtain the core material mixture; S3: Add the modified nano-tourmaline powder obtained in step S1 and the core material mixture obtained in step S2 to the urea aqueous solution and stir. S4: Add formaldehyde solution to the reaction system of step S3, and carry out the reaction under stirring. After the reaction is completed, the mixture is aged, washed, filtered, and freeze-dried to obtain the insect-repellent and fattening microcapsule matrix. S5: Disperse the insect-repellent and fattening microcapsule matrix obtained in step S4 in methanol, then add a coupling agent methanol solution, adjust the pH value, process under stirring, then filter, wash, and freeze dry. S6: Disperse the solid powder obtained after freeze-drying in step S5 in a buffer solution, add a chelating agent, process under stirring, filter, wash, and freeze-dry. S7: Disperse the solid powder obtained after freeze-drying in step S6 in a metal ion salt - N,N-dimethylformamide solution, and process it with stirring. After the reaction is complete, filter, wash, and freeze-dry to obtain insect-repellent and fattening microcapsules.

8. The method according to claim 7, characterized in that, In step S1, the particle size of the nano-tourmaline powder is 10-100 nm; And / or, the surfactant is an anionic surfactant, preferably at least one of sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, and 2-morpholine ethanesulfonic acid; And / or, the solvent is an aprotic solvent with a boiling point >100°C, preferably at least one of formamide, N,N-dimethylformamide, dimethylacetamide, and dimethylphosphoramide; And / or, the mass ratio of the nano-tourmaline powder to the surfactant is (1-10):1, and the mass ratio of the solvent to the surfactant is (20-40):

1.

9. The method according to claim 7, characterized in that, In step S1, the stirring speed is 400-600 rpm; the modification temperature is 100-200℃; and the modification time is 4-8 hours.

10. The method according to claim 7, characterized in that, In step S2, the mixing is carried out under stirring, the stirring speed is 300-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 3-10 minutes.

11. The method according to claim 7, characterized in that, In step S3, the mass ratio of urea to water in the urea aqueous solution is 1:(5-50); the pH of the urea aqueous solution is adjusted to 2.5-5.5 before use. And / or, the mass ratio of the core material mixture to the modified nano-tourmaline powder is 1:(0.1-0.5); the mass ratio of the core material mixture to urea is 1:(0.2-1).

12. The method according to claim 7, characterized in that, In step S3, the stirring speed is 400-600 rpm, the stirring temperature is 40-60℃, and the stirring time is 1-2 hours.

13. The method according to claim 7, characterized in that, In step S4, the formaldehyde solution is an aqueous solution of formaldehyde with a mass concentration of 35%-40%; the amount of formaldehyde solution added satisfies the molar ratio of formaldehyde to urea in the reaction system of step S3 as (1.5-2.5):

1.

14. The method according to claim 7, characterized in that, In step S4, the stirring speed is 400-600 rpm, the stirring temperature is 50-80℃, and the reaction time under stirring is 4-6 hours.

15. The method according to claim 7, characterized in that, In step S5, the coupling agent methanol solution is prepared by coupling agent and methanol, and the mass ratio of methanol to coupling agent is (1-15):1; And / or, the coupling agent is a silane coupling agent, preferably at least one of 3-chloropropyltrimethylsilane, (dichloromethyl)trimethylsilane, (trichloromethyl)trimethylsilane, and (chlorodifluoromethyl)trimethylsilane; And / or, the mass ratio of methanol to the insect repellent and fattening microcapsule matrix is ​​(1-20):1, and the mass ratio of the coupling agent methanol solution to the insect repellent and fattening microcapsule matrix is ​​(0.1-10):

1.

16. The method according to claim 7, characterized in that, In step S5, the stirring speed is 200-450 rpm; the processing temperature is 40-60℃; and the processing time is 4-6 hours.

17. The method according to claim 7, characterized in that, The buffer solution mentioned in step S6 is one or more of phosphate buffer and carbonate buffer; the pH value of the buffer solution is 9-12; And / or, the mass ratio of the buffer solution to the solid powder obtained after lyophilization in step S5 is (5-50):

1.

18. The method according to claim 7, characterized in that, In step S6, the stirring speed is 200-450 rpm, the processing temperature is 40-60℃, and the processing time is 2-5 hours.

19. The method according to claim 7, characterized in that, In step S7, the mass ratio of the metal ion salt-DMF solution to the solid powder obtained after drying in step S6 is (10-30):

1. And / or, the stirring speed is 200-450 rpm, the processing temperature is 100-150℃, and the processing time is 2-5 hours.

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