CN111849256A - Preparation method of slow-release microcapsule antifouling material - Google Patents
Preparation method of slow-release microcapsule antifouling material Download PDFInfo
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- CN111849256A CN111849256A CN202010466584.7A CN202010466584A CN111849256A CN 111849256 A CN111849256 A CN 111849256A CN 202010466584 A CN202010466584 A CN 202010466584A CN 111849256 A CN111849256 A CN 111849256A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D107/02—Latex
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B01J13/14—Polymerisation; cross-linking
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
- C09D5/1612—Non-macromolecular compounds
- C09D5/1625—Non-macromolecular compounds organic
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to a preparation method of a slow-release microcapsule antifouling material, belonging to the technical field of environment-friendly materials. The invention adopts a complex coacervation method to prepare a slow-release microcapsule antifouling material, the complex coacervation method utilizes two wall materials with different charges in solution to cross-link with each other through electrostatic interaction between ions to obtain a microcapsule of a composite wall material, the action principle is that a positively charged wall material solution is mixed with another negatively charged wall material solution, coacervate is formed by the interaction of positive and negative charges to separate and deposit around a core material, and the core material is coated to obtain the microcapsule.
Description
Technical Field
The invention relates to a preparation method of a slow-release microcapsule antifouling material, belonging to the technical field of environment-friendly materials.
Background
Marine vessels, submarine industrial equipment, submarines and the like can cause the enrichment growth of marine microorganisms, algae and mollusks after being exposed in seawater for a certain time. The marine organism pollution can increase the navigation resistance of the marine ship and the submarine in the seawater, shorten the service life of the ship body and increase the fuel consumption. Antifouling coatings are currently the most effective way to inhibit fouling of marine equipment by marine organisms. The efficient, environment-friendly and green antifouling technology needs to have the following characteristics: is non-toxic to non-target fishes and mammals; can not be gathered in the food chain, can be degraded in the environment, and has low cost and long action effect.
In recent years, people have been engaged in research and development of marine resources due to the scarcity of land resources. Ships and equipment exposed in the marine environment are easily polluted by algae and mollusks in a humid environment, the advancing resistance is greatly increased, and the oil consumption is further increased. Meanwhile, the cleaning work of marine microbial pollution is very difficult. On the other hand, the adhesion of organisms has a great influence on the life of the ship itself. Therefore, we must adopt some method to slow down the attachment of the organism.
Exposure to seawater of materials without any toxicity can cause the attachment and colonization of many marine organisms. Marine biofouling generally consists of three steps: the first step is as follows: organic molecules such as protein, polysaccharide and the like in seawater are firstly adsorbed on the surface of a material by a physical adsorption mode to form a conditioned film. Then, planktonic bacteria accumulate and grow on the surface of the material. Bacteria form a reversible adhesion on the surface of materials through weak covalent bond forces (electrostatic attraction, van der waals forces). After the biological membrane is mature, the transportation of nutritive salt can be started, and under proper condition, the nutrient salt can be developed into macroscopic bacterial colony, and the second step: after the formation of the basal biofilm, multicellular microorganisms begin to grow attached to the biofilm. These multicellular microorganisms secrete more mucus protein to grow and expand; the third step: macroalgae, barnacles, mollusk bryozoans and sponges are beginning to grow continuously, causing large scale irreversible biofouling.
People began to paint antifouling paints containing heavy metals (copper, lead, mercury, arsenic, etc.) on the surface of marine equipment in the late 19 th century, which can effectively block the adhesion of marine microorganisms on the surface, but the heavy metal antifouling paints gradually began to exit the stage as the heavy metals began to endanger other non-target organisms in the sea and even began to enter the food chain of human beings. In the 20 th century and the fifties, organic tin compounds (triphenyl hydroxide, butyl tin compound, triphenyl tin compound and the like) are researched, the antifouling efficiency is high, the cost is low, and the organic tin compounds become the most efficient antifouling agents in the market once. However, the organotin compounds can cause the distortion of shellfish and other mollusks, and bring great harm to the ecological environment. In 2008, the use of organotin antifouling paints on ships was completely prohibited by the international maritime organization belonging to the united nations. Researchers have been working on make internal disorder or usurp for efficient and environmentally friendly antifouling coatings in recent years. Experts at home and abroad synthesize a series of paints which can be used as marine equipment surface antifouling paint, such as capsaicins, alkaloids, DCOIT, TCPM, marine organism extracts and the like. The antifouling agents are easy to degrade in marine environment, harmless to environment and good in antifouling effect. The coating with the antifouling effect can effectively inhibit the attachment growth of marine microorganisms, interfere the nerve conduction of soft-shelled animals and the like, play a certain role in avoiding and do no harm to marine environment and human beings. At present, most of antifouling agents are prepared into coatings to be coated on the bottom of a ship body, but the coatings are easy to fall off and can be replaced after a period of time, and slow release cannot be achieved.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that most of the prior antifouling agents are prepared into coatings which are smeared at the bottom of a ship body and easily fall off, and the coatings are possibly replaced after a period of time and cannot be slowly released, the preparation method of the slow-release microcapsule antifouling material is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
(1) adding the antifouling microcapsules and deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, and stirring at the rotation speed of 10000-12000 r/min for 20-30 min at normal temperature to obtain mixed latex;
(2) adding rosin emulsion, casein powder, glycerol, sodium stearate and an antioxidant 1010 into the mixed latex, placing the mixed latex into a high-shear emulsifying machine, and carrying out high-speed shearing at a rotating speed of 20000-24000 r/min for 40-60 min under the condition of a water bath at the temperature of 30-40 ℃ to obtain a mixed material;
(3) placing the mixture in an ultrasonic dispersion machine, and ultrasonically dispersing for 1-2 hours at the temperature of 30-40 ℃ to obtain a mixed dispersing material;
(4) drying the mixed dispersed material in an oven at the temperature of 120-140 ℃ for 2-4 h to obtain a mixture;
(5) and (3) placing the mixture into a mold, placing the mixture into a hot press for hot pressing for 8-10 min, cooling at normal temperature, and demolding to obtain the slow-release microcapsule antifouling material.
The weight parts of the antifouling microcapsule, the natural latex, the rosin emulsion, the casein powder, the glycerol, the sodium stearate, the antioxidant 1010 and the deionized water are 20-30 parts of the antifouling microcapsule, 40-60 parts of the natural latex, 16-24 parts of the rosin emulsion, 12-18 parts of the casein powder, 8-12 parts of the glycerol, 4-6 parts of the sodium stearate, 0.4-0.6 part of the antioxidant 1010 and 20-30 parts of the deionized water.
And (4) the power of ultrasonic dispersion in the step (3) is 500-600W.
The specification of the die in the step (5) is 550mm multiplied by 300mm, and the hot pressing treatment conditions are that the temperature is 140-160 ℃ and the pressure is 6-8 MPa.
The specific preparation steps of the antifouling microcapsule in the step (1) are as follows:
(1) adding gelatin into 1/2 deionized water, and stirring for 10-12 min at a rotating speed of 160-180 r/min under a water bath condition of 50-60 ℃ to obtain a gelatin solution;
(2) adding capsaicin powder into a gelatin solution, stirring at the normal temperature at the rotating speed of 300-350 r/min for 20-30 min, and placing in an ultrasonic dispersion machine for ultrasonic dispersion for 30-40 min to obtain dispersion liquid;
(3) adding chitosan into the residual 1/2 deionized water, adding an acetic acid solution, stirring for 15-20 min at a rotating speed of 250-300 r/min under a water bath condition of 40-50 ℃, and preserving heat to obtain a chitosan acetic acid solution;
(4) Slowly adding the dispersion into a chitosan acetic acid solution, placing the chitosan acetic acid solution into a high-shear emulsifying machine, and stirring the chitosan acetic acid solution for 15-20 min at the rotating speed of 8000-10000 r/min under the water bath condition of 40-50 ℃ to obtain a mixed solution;
(5) keeping the temperature of the mixed solution at 0-5 ℃ for 40-60 min, adjusting the pH value to 4-5, adding glutaraldehyde, heating to 60-70 ℃, stirring at the rotating speed of 240-280 r/min for 30-40 min, standing and curing for 2-4 h, cooling at normal temperature, and drying to obtain the antifouling microcapsule;
the weight parts of the capsaicin powder, the gelatin, the chitosan, the acetic acid solution and the deionized water are 20-30 parts of the capsaicin powder, 30-40 parts of the gelatin, 30-40 parts of the chitosan, 10-15 parts of the acetic acid solution with the mass fraction of 10% and 200-300 parts of the deionized water.
And (3) the power of the ultrasonic dispersion in the step (2) is 400-500W.
And (4) adding the dispersion liquid in the step (4) at a rate of 60-80 mL/min.
The pH adjustment in the step (5) adopts 10 percent by mass of acetic acid solution.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention adopts gelatin and chitosan as wall materials to prepare a sustained-release microcapsule antifouling material, the gelatin is a protein mixture, can not be dissolved in cold water and can not be dissolved in organic solvents, the gelatin has low price, wide source, safety, no toxicity and good water solubility, simultaneously has good film forming property, biodegradability and biocompatibility, and is suitable for being used as the wall material of microcapsules, the chitosan is a product obtained by deacetylating chitin, the chitosan is widely existed in the nature, the shells of a plurality of fishes, shrimps and crabs and the cell walls of microorganisms contain abundant chitosan, the annual output is high, the price is low, the chitosan is the only natural alkaline polysaccharide discovered so far, the pure chitin and the chitosan are white flaky or powdery solids and can stably exist at normal temperature, the molecular chain of the chitosan contains amino and carboxyl, the adsorption and the chelating ability of the chitosan in acidic solution are strong, the chitosan molecule is easy to carry out chemical modification, intramolecular and intermolecular hydrogen bonds formed by some groups are also arranged on the chitosan molecule, so that the chitosan molecule is easy to crystallize, the chitosan molecule has high crystallinity, the physical and chemical properties of the chitosan determine that the chitosan has good bioabsorption, biodegradability, biocompatibility, film forming property, fiber forming property, moisture retention and the like, and the chitosan has the functions of slow release and targeting due to the unique functional properties of the chitosan, so the slow release antifouling microcapsule prepared by taking the chitosan as a wall material is safe and nontoxic and can be effectively bonded with a base material;
(2) The invention adopts a complex coacervation method to prepare a slow-release microcapsule antifouling material, the complex coacervation method utilizes two wall materials with different charges in solution to cross-link with each other through electrostatic interaction between ions to obtain a microcapsule of a composite wall material, the action principle is that a positively charged wall material solution is mixed with another negatively charged wall material solution, coacervate is formed by the interaction of positive and negative charges to separate and deposit around a core material, the core material is coated to obtain the microcapsule, when the positive and negative charges of the two substances are equal, the yield of the microcapsule is the largest, the method can avoid using an organic solvent and a chemical cross-linking agent, simultaneously, the complex coacervation method can microencapsulate solid microcapsules, the yield is higher, the microcapsule preparation by the complex coacervation method needs three stages of wall film formation, deposition and cross-linking curing, the embedding rate of the core material is very high, the formed wall film has high compactness and good slow release effect, and can effectively prevent the anti-fouling agent from falling off.
Detailed Description
Respectively weighing 20-30 parts by weight of capsaicin powder, 30-40 parts by weight of gelatin, 30-40 parts by weight of chitosan, 10-15 parts by weight of 10% acetic acid solution and 200-300 parts by weight of deionized water, adding the gelatin into 1/2 parts by weight of deionized water, stirring for 10-12 min at a rotating speed of 160-180 r/min under a water bath condition of 50-60 ℃ to obtain a gelatin solution, adding the capsaicin powder into the gelatin solution, stirring for 20-30 min at a rotating speed of 300-350 r/min at normal temperature, ultrasonically dispersing for 30-40 min in an ultrasonic dispersion machine at a power of 400-500W to obtain a dispersion liquid, adding the chitosan into the rest 1/2 parts by weight of deionized water, adding the acetic acid solution, stirring for 15-20 min at a rotating speed of 250-300 r/min under a water bath condition of 40-50 ℃, preserving heat to obtain a chitosan acetic acid solution, slowly adding the dispersion liquid into the chitosan acetic acid solution at a speed of 60-80 mL/min, placing the mixture into a high-shear emulsifying machine, stirring for 15-20 min at a rotating speed of 8000-10000 r/min under a water bath condition of 40-50 ℃ to obtain a mixed solution, placing the mixed solution into a water bath condition of 0-5 ℃ for heat preservation for 40-60 min, dropwise adding 1% by mass of sodium carbonate to adjust the pH value to 4-5, adding glutaraldehyde, heating to 60-70 ℃, stirring for 30-40 min at a rotating speed of 240-280 r/min, standing and curing for 2-4 h, cooling at normal temperature, and drying to obtain an antifouling microcapsule; respectively weighing 20-30 parts of antifouling microcapsules, 40-60 parts of natural latex, 16-24 parts of rosin emulsion, 12-18 parts of casein powder, 8-12 parts of glycerol, 4-6 parts of sodium stearate, 0.4-0.6 part of antioxidant 1010 and 20-30 parts of deionized water according to parts by weight, adding the antifouling microcapsules and the deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, stirring at the normal temperature at the rotating speed of 10000-12000 r/min for 20-30 min to obtain mixed latex, adding the rosin emulsion, the casein powder, the glycerol, the sodium stearate and the antioxidant 1010 into the mixed latex, placing the mixed latex in the high-shear emulsifying machine, shearing at the high speed of 20000-24000 r/min for 40-60 min under the condition of water bath at the temperature of 30-40 ℃ to obtain a mixed material, placing the mixed material in an ultrasonic dispersion machine, ultrasonically dispersing the mixed material at the power of 500-600W for 1-2 h under the condition of 30-40 ℃, and (3) obtaining a mixed dispersing material, placing the mixed dispersing material in an oven at the temperature of 120-140 ℃ for drying for 2-4 hours to obtain a mixture, placing the mixture in a mould with the specification of 550mm multiplied by 300mm, placing the mould in a hot press, carrying out hot pressing treatment for 8-10 min at the temperature of 140-160 ℃ and under the pressure of 6-8 MPa, cooling at normal temperature, and demoulding to obtain the slow-release microcapsule antifouling material.
Example 1
Respectively weighing 20 parts of capsaicin powder, 30 parts of gelatin, 30 parts of chitosan, 10 parts of 10% acetic acid solution by mass fraction and 200-300 parts of deionized water according to parts by weight, adding the gelatin into 1/2 deionized water, stirring for 10min at a rotating speed of 160r/min under a water bath condition of 50 ℃ to obtain a gelatin solution, adding the capsaicin powder into the gelatin solution, stirring for 20min at a rotating speed of 300r/min at normal temperature, ultrasonically dispersing for 30min in an ultrasonic dispersion machine at a power of 400W to obtain a dispersion liquid, adding the chitosan into the rest 1/2 deionized water, adding the acetic acid solution, stirring for 15min at a rotating speed of 250r/min under a water bath condition of 40 ℃ and preserving heat to obtain a chitosan acetic acid solution, slowly adding the dispersion liquid into the chitosan acetic acid solution at a speed of 60mL/min, placing the chitosan acetic acid solution into a high-shear emulsion machine, stirring for 15min at a rotating speed of 8000r/min under a water bath condition of 40 ℃, obtaining a mixed solution, keeping the temperature of the mixed solution at 0 ℃ for 40min, dropwise adding sodium carbonate with the mass fraction of 1% to adjust the pH value to 4, adding glutaraldehyde, heating to 60 ℃, stirring at the rotating speed of 240r/min for 30min, standing and curing for 2h, cooling at normal temperature, and drying to obtain the antifouling microcapsule; respectively weighing 20 parts of antifouling microcapsules, 40 parts of natural latex, 16 parts of rosin emulsion, 12 parts of casein powder, 8 parts of glycerol, 4 parts of sodium stearate, 0.4 part of antioxidant 1010 and 20 parts of deionized water according to parts by weight, adding the antifouling microcapsules and the deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, stirring at the normal temperature for 20min at the rotating speed of 100000r/min to obtain mixed latex, adding the rosin emulsion, the casein powder, the glycerol, the sodium stearate and the antioxidant 1010 into the mixed latex, placing the mixed latex in the high-shear emulsifying machine, shearing at the high speed of 20000r/min for 40min under the water bath condition of 30 ℃ to obtain a mixed material, placing the mixed material in an ultrasonic dispersion machine, ultrasonically dispersing for 1h under the condition of 30 ℃ and the power of 500W to obtain a mixed dispersed material, placing the mixed dispersed material in an oven of 120 ℃ for drying for 2h to obtain a mixture, placing the mixture in a mould with the specification of 550mm × 550mm × 300mm, placing in a hot press, carrying out hot pressing treatment for 8min at the temperature of 140 ℃ and under the pressure of 6MPa, cooling at normal temperature, and demoulding to obtain the slow-release microcapsule antifouling material.
Example 2
Respectively weighing 25 parts of capsaicin powder, 35 parts of gelatin, 35 parts of chitosan, 13 parts of 10 mass percent acetic acid solution and 250 parts of deionized water according to parts by weight, adding the gelatin into 1/2 parts of deionized water, stirring for 11min at the rotating speed of 170r/min under the water bath condition of 55 ℃ to obtain gelatin solution, adding the capsaicin powder into the gelatin solution, stirring for 25min at the rotating speed of 325r/min at normal temperature, ultrasonically dispersing for 35min in an ultrasonic dispersion machine at the power of 450W to obtain dispersion liquid, adding the chitosan into the rest 1/2 parts of deionized water, adding the acetic acid solution, stirring for 17min at the rotating speed of 275r/min under the water bath condition of 45 ℃, preserving heat to obtain chitosan acetic acid solution, slowly adding the dispersion liquid into the chitosan acetic acid solution at the speed of 70mL/min, placing the chitosan acetic acid solution into a high-shear emulsion machine, stirring for 17min at the rotating speed of 9000r/min under the water bath condition of 45 ℃, obtaining a mixed solution, keeping the temperature of the mixed solution at 3 ℃ for 50min, dropwise adding sodium carbonate with the mass fraction of 1% to adjust the pH value to 4.5, adding glutaraldehyde, heating to 65 ℃, stirring at the rotating speed of 260r/min for 35min, standing and curing for 3h, cooling at normal temperature, and drying to obtain the antifouling microcapsule; respectively weighing 25 parts of antifouling microcapsules, 50 parts of natural latex, 20 parts of rosin emulsion, 15 parts of casein powder, 10 parts of glycerol, 5 parts of sodium stearate, 0.5 part of antioxidant 1010 and 25 parts of deionized water according to parts by weight, adding the antifouling microcapsules and the deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, stirring at the normal temperature at the rotating speed of 11000r/min for 25min to obtain mixed latex, adding the rosin emulsion, the casein powder, the glycerol, the sodium stearate and the antioxidant 1010 into the mixed latex, placing the mixed latex in the high-shear emulsifying machine, shearing at the high speed of 22000r/min for 50min under the water bath condition of 35 ℃ to obtain a mixed material, placing the mixed material in an ultrasonic dispersion machine, ultrasonically dispersing at the power of 550W for 1.5h under the condition of 35 ℃ to obtain a mixed dispersed material, placing the mixed dispersed material in an oven at the temperature of 130 ℃ for drying for 3h to obtain a mixture, placing the mixture in a mould with the specification of 550mm × 550mm × 300mm, placing in a hot press, performing hot pressing treatment for 9min at the temperature of 150 ℃ and under the pressure of 7MPa, cooling at normal temperature, and demolding to obtain the slow-release microcapsule antifouling material.
Example 3
Respectively weighing 30 parts of capsaicin powder, 40 parts of gelatin, 40 parts of chitosan, 15 parts of 10 mass percent acetic acid solution and 300 parts of deionized water according to parts by weight, adding the gelatin into 1/2 parts of deionized water, stirring for 12min at a rotating speed of 180r/min under a water bath condition of 60 ℃ to obtain a gelatin solution, adding the capsaicin powder into the gelatin solution, stirring for 30min at a rotating speed of 350r/min at normal temperature, ultrasonically dispersing for 40min in an ultrasonic dispersion machine at a power of 500W to obtain a dispersion liquid, adding the chitosan into the rest 1/2 parts of deionized water, adding the acetic acid solution, stirring for 20min at a rotating speed of 300r/min under a water bath condition of 50 ℃, preserving heat to obtain a chitosan acetic acid solution, slowly adding the dispersion liquid into the chitosan acetic acid solution at a speed of 80mL/min, placing in a high-shear emulsion machine, stirring for 20min at a rotating speed of 10000r/min under a water bath condition of 50 ℃, obtaining a mixed solution, keeping the temperature of the mixed solution at 5 ℃ for 60min, dropwise adding sodium carbonate with the mass fraction of 1% to adjust the pH value to 5, adding glutaraldehyde, heating to 70 ℃, stirring at the rotating speed of 280r/min for 40min, standing and solidifying for 4h, cooling at normal temperature, and drying to obtain the antifouling microcapsule; respectively weighing 30 parts of antifouling microcapsules, 60 parts of natural latex, 24 parts of rosin emulsion, 18 parts of casein powder, 12 parts of glycerol, 6 parts of sodium stearate, 0.6 part of antioxidant 1010 and 30 parts of deionized water according to parts by weight, adding the antifouling microcapsules and the deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, stirring at the normal temperature at the rotating speed of 12000r/min for 30min to obtain mixed latex, adding the rosin emulsion, the casein powder, the glycerol, the sodium stearate and the antioxidant 1010 into the mixed latex, placing the mixed latex in the high-shear emulsifying machine, shearing at the high speed of 24000r/min for 60min under the water bath condition of 40 ℃ to obtain a mixed material, placing the mixed material in an ultrasonic dispersion machine, ultrasonically dispersing at the power of 600W for 2h under the condition of 40 ℃ to obtain a mixed dispersed material, placing the mixed dispersed material in an oven of 140 ℃ for drying for 4h to obtain a mixture, placing the mixture in a mould with the specification of 550mm × 550mm × 300mm, placing in a hot press, performing hot pressing treatment for 10min at the temperature of 160 ℃ and under the pressure of 8MPa, cooling at normal temperature, and demolding to obtain the slow-release microcapsule antifouling material.
The slow release microcapsule antifouling material prepared by the invention is subjected to performance detection, and specific detection results are shown in the following table 1.
TABLE 1 characterization of Slow-Release microcapsule antifouling Material Properties
As shown in Table 1, the slow-release microcapsule antifouling material prepared by the invention can slow down the release of the antifouling agent and achieve the slow-release effect.
Claims (9)
1. A preparation method of a slow-release microcapsule antifouling material is characterized by comprising the following specific preparation steps:
(1) adding the antifouling microcapsules and deionized water into the natural latex, placing the natural latex in a high-shear emulsifying machine, and stirring at the rotation speed of 10000-12000 r/min for 20-30 min at normal temperature to obtain mixed latex;
(2) adding rosin emulsion, casein powder, glycerol, sodium stearate and an antioxidant 1010 into the mixed latex, placing the mixed latex into a high-shear emulsifying machine, and carrying out high-speed shearing at a rotating speed of 20000-24000 r/min for 40-60 min under the condition of a water bath at the temperature of 30-40 ℃ to obtain a mixed material;
(3) placing the mixture in an ultrasonic dispersion machine, and ultrasonically dispersing for 1-2 hours at the temperature of 30-40 ℃ to obtain a mixed dispersing material;
(4) drying the mixed dispersed material in an oven at the temperature of 120-140 ℃ for 2-4 h to obtain a mixture;
(5) and (3) placing the mixture into a mold, placing the mixture into a hot press for hot pressing for 8-10 min, cooling at normal temperature, and demolding to obtain the slow-release microcapsule antifouling material.
2. The preparation method of the slow-release microcapsule antifouling material as claimed in claim 1, wherein the weight parts of the antifouling microcapsule, the natural latex, the rosin emulsion, the casein powder, the glycerol, the sodium stearate, the antioxidant 1010 and the deionized water are 20-30 parts of the antifouling microcapsule, 40-60 parts of the natural latex, 16-24 parts of the rosin emulsion, 12-18 parts of the casein powder, 8-12 parts of the glycerol, 4-6 parts of the sodium stearate, 0.4-0.6 part of the antioxidant 1010 and 20-30 parts of the deionized water.
3. The preparation method of the slow-release microcapsule antifouling material as claimed in claim 1, wherein the ultrasonic dispersion power in step (3) is 500-600W.
4. The method for preparing a sustained-release microcapsule antifouling material according to claim 1, wherein the specification of the mold in the step (5) is 550mm x 300mm, and the hot-pressing treatment is performed at a temperature of 140 to 160 ℃ and a pressure of 6 to 8 MPa.
5. The method for preparing the slow-release microcapsule antifouling material as claimed in claim 1, wherein the specific preparation steps of the antifouling microcapsule in step (1) are as follows:
(1) adding gelatin into 1/2 deionized water, and stirring for 10-12 min at a rotating speed of 160-180 r/min under a water bath condition of 50-60 ℃ to obtain a gelatin solution;
(2) Adding capsaicin powder into a gelatin solution, stirring at the normal temperature at the rotating speed of 300-350 r/min for 20-30 min, and placing in an ultrasonic dispersion machine for ultrasonic dispersion for 30-40 min to obtain dispersion liquid;
(3) adding chitosan into the residual 1/2 deionized water, adding an acetic acid solution, stirring for 15-20 min at a rotating speed of 250-300 r/min under a water bath condition of 40-50 ℃, and preserving heat to obtain a chitosan acetic acid solution;
(4) slowly adding the dispersion into a chitosan acetic acid solution, placing the chitosan acetic acid solution into a high-shear emulsifying machine, and stirring the chitosan acetic acid solution for 15-20 min at the rotating speed of 8000-10000 r/min under the water bath condition of 40-50 ℃ to obtain a mixed solution;
(5) and (3) keeping the temperature of the mixed solution at 0-5 ℃ for 40-60 min, adjusting the pH value to 4-5, adding glutaraldehyde, heating to 60-70 ℃, stirring at the rotating speed of 240-280 r/min for 30-40 min, standing and curing for 2-4 h, cooling at normal temperature, and drying to obtain the antifouling microcapsule.
6. The preparation method of a slow-release microcapsule antifouling material as claimed in claim 5, wherein the weight parts of the capsaicin powder, the gelatin, the chitosan, the acetic acid solution and the deionized water are 20-30 parts of the capsaicin powder, 30-40 parts of the gelatin, 30-40 parts of the chitosan, 10-15 parts of the 10% acetic acid solution by mass and 200-300 parts of the deionized water.
7. The preparation method of the slow-release microcapsule antifouling material as claimed in claim 5, wherein the ultrasonic dispersion power in the step (2) is 400-500W.
8. The preparation method of a slow-release microcapsule antifouling material as claimed in claim 5, wherein the addition rate of the dispersion liquid in the step (4) is 60-80 mL/min.
9. The method for preparing sustained-release microcapsule antifouling material according to claim 5, wherein the pH adjustment in step (5) is performed using a 10% by mass acetic acid solution.
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