KR20170025782A

KR20170025782A - Manufacturing method of controlled release micropowder with nanoporosity

Info

Publication number: KR20170025782A
Application number: KR1020150122729A
Authority: KR
Inventors: 배진성; 유지훈; 김태국; 박은수
Original assignee: 주식회사 티케이케미칼; 배진성; 주식회사 피비알케미칼
Priority date: 2015-08-31
Filing date: 2015-08-31
Publication date: 2017-03-08
Also published as: KR101779846B1

Abstract

The present invention relates to a sustained-release fine powder having nano-porosity and a method for producing the same.
A polymer aqueous dispersion producing step of producing a milky white homogeneous polymer resin aqueous dispersion; A core material-containing coarse particle producing step of producing a coarse material-containing coarse particle-shaped water dispersion; A water-dispersed polymer nanocomposite producing aqueous dispersion in which water-dispersed polymer nanocomposite particles containing a core material are formed; A curing agent injecting step of injecting a curing agent; A nanoporous fine powder forming step of forming a sustained-release fine powder having spherical nanoporosity; A particle sorting step of sorting by size; A method for producing a sustained-release fine powder having nano-porosity capable of effectively controlling a release rate of a deep-seated fine powder, comprising an airtight packing step of compressing and packing with an aluminum laminate film, A sustained release fine powder having nanoporous structure composed of a resin, 1 to 10 parts by weight of an organic amine, 10 to 50 parts by weight of a functional core material, 0.1 to 5 parts by weight of a particle stabilizer, 10 to 80 parts by weight of a nanofiller and 0.1 to 5 parts by weight of a curing agent .

Description

TECHNICAL FIELD The present invention relates to a sustained-release fine powder having nanoporosity and a method of manufacturing the same,

The present invention relates to a method for producing a controlled release micropowder having nanoporosity and, more particularly, to a method for producing a controlled release micropowder comprising a core material, A sustained-release fine powder having nanoporous property capable of controlling the release rate of core material by adjusting pore size at a mixing ratio between an eater dispersion and a nanofiller, and a preparation thereof &Lt; / RTI >

Chemical additives are used in the processing or polymerization process to facilitate the processing of plastic or synthetic resin and to improve the performance of the final product. These additives supplement the plastic's vulnerability And plays a role of saving characteristics.

The purpose of using plastic additives is to improve the quality of plastics, to improve the processability of molded products, to improve the physical properties and to maintain long-term stability. Plasticizers, heat stabilizers, antioxidants, ultraviolet stabilizers UV stabilizers, flame retardants, antistatic agents, lubricants, etc. It is an essential component for the production of plastic products depending on the function and use of the product.

As an example, light and oxygen cause decomposition reaction in the polymer, which is not only visually confirmed by discoloration, but also causes deterioration of mechanical and physical properties. Ultraviolet rays in the wavelength range of 290 to 400 nm in the sunlight break down the chemical bonds of the polymer to form free radicals which cause chain cutting or crosslinking and ultimately cause discoloration, And deterioration of mechanical properties. Therefore, UV stabilizers and antioxidants should be added to the outdoor products.

UV stabilizers are absorbers, quenchers and hindered amine light stabilizers (HALS), depending on the mechanism of action.

Among the polymer additives, UV stabilizers are one of the fastest growth areas in comparison with other high additives. However, most of them are low molecular weight and have low compatibility with polymers. In order to overcome the disadvantages such as migration of components to the surface of finished products, , And studies have been made in the direction of high molecular weight bivalent. Antioxidants are used to minimize the occurrence of decomposition, crosslinking, and coloring of polymers by blocking radicals generated during polymerization, processing, storage and use of finished products or by preventing radical initiation reaction. Thus, phenolic antioxidants are the main species and almost all thermoplastic It is an additive that is essential to thermoplastic.

A microcapsule is a microcapsule that is surrounded by a polymer, a ceramic or an organic composite material, a core material of an active ingredient which is unstable or weak in stability or is unstable to very small particles or films which are invisible only in diameter of a few microns to several hundreds of microns , And coating technology.

It can be designed so that it can be easily destroyed only by external stimuli or the contents can be gradually released during actual use, especially during the manufacturing process or during normal use. In particular, it can be designed to respond only to certain external conditions such as pressure, pH, It is manufacturable.

Microencapsulation was established in the drug delivery system in the 1940s, but the first successful commercialization was through pressure sensitive papers developed by the National Cash Register Co. in the 1950s .

Decompression copy paper is a copy paper that prints when the pressure is applied and the ink contained in the capsule bursts out. Typical examples are copy paper used for credit card receipts.

National Cash Register Corp. introduced microcapsule technology to protect the oil particles that originally dissolved the coloring agent, but found that the release of the dye was controlled by external pressure, resulting in the creation of a pressure-sensitive copy. Although there have been attempts to apply microcapsules to various daily necessities, they have not been commercialized.

In the 1980s, Japan succeeded in commercialization of functional fiber materials using microcapsules containing various functional materials such as direction, deodorant, antibacterial and the like.

Polymer microcapsules penetrate functional molecules such as medicines, enzymes, perfumes, pesticides and insecticides into the inside to maintain the effect for a long time. As a related technology, it has been difficult to maintain the effect by being broken easily during use.

In Korea, a new technology to fabricate synthetic polymer peptide microcapsules with very uniform size and shape using a microfluidic system has been developed, and a nano cavity, which can be easily opened and closed according to external conditions such as hydrogen ion concentration and temperature, Generation drug delivery system that is not destroyed even in harsh environments. Using this technology, Korean researchers succeeded in stabilizing coenzyme Q10, which is unstable to oxidation through contact with air. When the microcapsule contains moisture or air-unstable functional ingredients, it is usually kept in a stable state in the capsule, and when it is applied to the skin, it is destroyed by the friction to release the functional ingredient.

In recent years, development of a self healing system through the release of active chemical substances encapsulated in microcapsules within a material is underway. This technology has been actively researched and developed as an effective countermeasure when unexpected damage is applied to orbit like a spacecraft in a practical aspect.

Also, for the infrastructure of bridges and other social infrastructures, the microcapsule-based self-repair is investing a lot of research funds as a means to greatly improve the safety and life of the structure.

A chitosan nanocontainer has been proposed that can control UV emission and release. The chitosan nanospheres capable of absorbing this ultraviolet light can perform better than photo filters and control the release of the encapsulated active material.

Other studies have developed self-exploding microcapsules that release exactly one day's drug and vaccine into the body for several weeks or months when injected into the body. Such a drug delivery system can be a very useful solution when it is necessary to dispense several times or continuously with time lag. The system is expected to change the way in which several vaccines are injected and is expected to drastically reduce the number of drug doses.

In the United States, next-generation microcapsule technology for use in carbon-free copying has been reported. The technology is expected to be applied to home, personal care, and medicine fields as microcapsules that emit light when they receive light.

In the case of liquid-filled capsules, self-healing plastic is used. In this case, the monomer and catalyst are mixed in the capsule, so that the capsule is broken and the contents are mixed and discharged, . The microcapsule thus developed is composed of nylon having a size of a grain of sand, and a compound and a carbon nanotube are mixed in the inside, and when the laser light is irradiated, the carbon nanotube is heated and the nylon The capsule breaks and the contents are released to the outside.

Using these techniques, doctors will be able to inject capsules containing anticancer drugs around the cancer cells, so that they can be used to deliver the anticancer drug to the desired site in a timely manner.

Thus, there has been a continuing need in the industry for a method to effectively control the rate of release of deep-seated fine powder.

The prior art and the patent literature developed until now to improve these characteristics will be described as follows.

Korean Patent No. 100532038 discloses a method for producing sustained release microcapsules using silica. According to the present invention, when silica coated with an acid or a base is used as an adsorbent for a functional core material, the total release amount and release rate of the functional core material embedded in the microcapsule can be easily and effectively controlled, It can be advantageously used in medicine field, fragrance field and agricultural field where control is required. Korean Patent No. 100431360 discloses a sustained-release resin composition containing a fragrant powder containing a directional component in a separate carrier and a microcapsule-oriented microcapsule powder. The sustained-release resin composition of the above-mentioned patent is characterized in that the aromatic component maintains the heat resistance that can withstand high temperatures during processing of the polymer and the initial high strength of the fragrance due to the simultaneous application of the sustained-release technology and the smell intensity even when it is used for a long period of time. Korean Patent Publication No. 1020090107795 discloses a method of controlling the mixing ratio of the hydrophobic biodegradable polymer, poly 竜 -caprolactone and the hydrophilic biodegradable polymer, and adding the functional core material, the organic solvent and the additive to the biodegradable polymer at a predetermined ratio Discloses a method for producing sustained release microcapsules which can easily control the release rate and release amount of functional core materials and a method for producing the microcapsules prepared thereby. The microcapsule according to the present invention can be usefully applied in the fields of medicine, pesticide, food, and cosmetics where a control and release system for functional core materials is required. Korean Patent No. 100537952 discloses a hollow-type hydrophobic polymer microcapsule made of a hydrophobic polymer and having an internal structure hollowed in order to improve the stability thereof in order to contain a large amount of water-soluble active ingredients used in cosmetics, a method for producing the same, Or a pharmaceutically acceptable salt thereof. The hollow microcapsule using the hydrophobic polymer of the present invention can contain a large amount of a water-soluble active ingredient and can stably maintain it, so that the function of the active ingredient can be effectively exerted. In Korean Patent No. 100524820, a precursor which imparts hydrophilic or lipophilic properties is prepared by adding tetraethyl orthosilicate (TEOS) to an aqueous solution containing a hydrolysis catalyst to adjust the degree of hydrolysis, And an aminopropyltrialkoxy silane serving as an internal gelling agent are mixed and dissolved in a predetermined amount, and this solution is emulsified and dispersed in a solution having a polarity opposite to that of the core material to form a core The present invention relates to a method for microencapsulating a substance to be surrounded by a silica film, which is less polluted by environmental pollution than an existing method using an alkali such as ammonia water as a gelling agent. In selecting the core material, hydrophilic or hydrophobic, Preparation of Applicable Silica Microcapsules The present law. Korean Patent No. 100774613 discloses a crystalline nuclear material; An active ingredient layer formed on the outer surface of the crystalline nuclear material and comprising a pharmacologically active ingredient and a water-insoluble polymer; And a sustained-release layer formed on the outer surface of the active ingredient layer and including a sustained-release film-forming substance. Korean Patent Registration No. 100574213 discloses a sustained-release preparation comprising a drug-containing core material and a multilayer coating layer covering the core material, wherein adjacent layers in the multilayer coating layer contain a hydrophobic organic compound-water-soluble polymer mixture different from each other, And a drug-containing core material by spray coating a solution containing a mixture of a hydrophobic organic compound and a water-soluble polymer, continuously spray-coating a solution containing different hydrophobic organic compound-water-soluble polymer mixture on the obtained coating layer, Wherein the hydrophilic organic compound-water-soluble polymer mixture is a hydrophilic organic compound-water-soluble polymer mixture. WO 2010024615 A2 discloses a process for the preparation of sustained-release microspheres which is capable of continuously controlling drug release. More specifically, in the preparation of microparticles encapsulating a drug in a carrier made of a biodegradable polymer, a solvent exchange evaporation method using a co-solvent is used to suppress the initial excessive release of the physiologically active substance Whereby the sustained release microparticles can be efficiently produced so that the physiologically active substance can be continuously and uniformly released from the body. U.S. Pat. No. 5,366,734 discloses a method for preparing an agent that mixes drugs in a biodegradable polymer, solidifies it into an implant form, and coating the exterior to lower initial overdischarge. However, since such an implant is too large in size, The size of the needle of the syringe must be enlarged in order to make the patient feel panic, and local anesthesia must be performed due to the pain. In Korean Patent Laid-Open Nos. 2001-110244 and 2002-59395, microcapsule walls are made porous or soft so as to control the release rate of functional core materials of microcapsules, To be controlled by diffusion through the hole in the capsule wall. In addition, it has been disclosed that chitosan is used as a wall material of microcapsules to prepare microcapsules by changing the molecular weight and concentration of chitosan, thereby controlling the release rate of the core material Korean Patent No. 0409413 discloses a method for producing microspheres by an underwater drying method and then heating and drying at a temperature higher than the glass transition temperature of the biodegradable polymer to significantly suppress initial overdischarge and minimize organic solvent, Such a manufacturing method is disadvantageous in that the physiologically active substance can be denatured by heat.

In recent years, as interest in health has increased, the development of high-function and high-value-added products using natural functional substances has become common in various industrial fields. Typically, microcapsules are being spotlighted as means for releasing functional materials to the outside or protecting them from the outside environment by imparting functional materials capable of exhibiting desired functions to various products in various ways. Such microcapsules have been actively applied and studied throughout the fields of medicine, herbicides, extinction agents, fungicides, agricultural chemicals applied as fungicides, foods, and cosmetics.

In general, the microcapsule can control the release rate of the functional core material depending on the chemical structure of the wall of the microcapsule made of a thin synthetic or natural polymer film, the thickness and the particle size of the microcapsule.

A known method for controlling the release rate of the microcapsules is to control the release rate of the functional core material by adjusting the wall thickness of the microcapsule or the thickness of the natural polymer.

However, this method is not suitable for the production of microcapsules by controlling the hydrophilic property of the microcapsule wall, or in the case of containing volatile functional core materials, the synthesis of the walls of the microcapsules or the release of core materials It becomes difficult to adjust the speed.

Accordingly, an object of the present invention is to provide a method for producing a sustained-release fine powder having nano-porosity that can effectively control the release rate of the deep-seated fine powder.

Another object of the present invention is to provide a process for preparing a sustained-release fine powder having a nano-porosity capable of controlling the discharge speed of a core material by controlling a pore size at a mixing ratio between a polymer resin aqueous dispersion and a nanofiller, Method.

It is still another object of the present invention to provide a sustained-release fine powder having nanoporous porosity produced by the above production method.

In order to accomplish the above object, the present invention provides a method for producing an ethylene-methyl acrylate-maleic anhydride terpolymer of 40 to 80 parts by weight in a reactor equipped with a stirrer, a temperature controller and a condenser, (ethylene-methyl acrylate-maleic anhydride terpolymer), ethylene-ethyl acrylate-maleic anhydride terpolymer, ethylene-methyl methacrylate-ethylene-maleic anhydride terpolymer methacrylate-maleic anhydride terpolymer, ethylene-ethyl methacrylate-maleic anhydride terpolymer, and 20 to 40 parts by weight of cyclohexanone, or tetrahydrofuran tetrahydrofuran, dioxane, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether (ethy) lethylene glycol monopropyl ether and ethylene glycol monobutyl ether and ethylene glycol n-butyl ether, an organic solvent such as 1 to 10 parts by weight of N-methyl N, N-diethanolamine, triethylamine, aminoethanolamine, diethylamine, N, N-dimethylethanolamine ( N, N-dimethylethanolamine) and 150-300 parts by weight of distilled water. The mixture is stirred for 5 to 30 minutes at a rotation speed of 100 to 500 rpm, And the mixture is further stirred for 10 to 20 minutes and then the reactor temperature is lowered to 20 to 30 DEG C while stirring the mixture continuously at a rotation speed of 100 to 500 rpm and the mixture is heated to a temperature of from 0.1 to & Under a pressure of 0.4 MPa, the flat weave has a filament diameter of 0.001 to 0.05 mm A step of preparing a polymer aqueous dispersion which is obtained by filtration through a metal filter such as stainless steel to produce a milky white homogeneous polymer resin aqueous dispersion;

211 to 430 parts by weight of the polymer aqueous dispersion prepared in the above step of preparing the polymer aqueous dispersion were added to a reactor equipped with a stirrer, a temperature controller and a condenser, and while stirring at a rotation speed of 100 to 500 rpm, 2,6-di- 2,6-di-tert-butyl-4-methyl phenol, poly (1,2-dihydro-2,2,4-trimethylquinoline) , 2,4-trimethyl quinoline), tetrakis [methylene (3,5-di-tert-butyl-4-hydroxy-hydrosinamate) 4-hydroxy-hydrocinnamate) methane] and tris (2,4-di-tert-butyl-phenyl) phosphite], phytoncide such as phytoncide, polyethyleneimine, anthraquinone, hydroquinone, naphthaquinone, benzoquinone, zinc ricinoleate, zinc abetate, and the like. Deodorant, Methyl 2-benzimidazole cabamate, pentachlorophenol, p-hydroxybenzoic acid, 2,4-dihydroxybenzoic acid (referred to as " 2,4-dihydroxybenzoic acid and ciprofloxacin or fragrances such as aroma components, fruit extracting oils and herbal extracts, zinc stearates, magnesium stearates, magnesium stearates, 0.1 to 5 parts by weight of a particle stabilizer is added to 10 to 50 parts by weight of a functional core material such as an activator such as starch or calcium stearate or a hardening agent and then agitated for 20 to 60 minutes, A core material-containing coarse particle-forming step of producing a water-dispersed particle-shaped dispersion;

10 to 80 parts by weight of titanium dioxide, tin oxide, aluminum oxide, zinc oxide (ZnO), indium oxide ( aqueous dispersion polymer nanocomposite particles containing a core material are prepared by stirring the mixture with stirring at a stirring speed of 500 to 2000 rpm for 20 to 40 minutes to prepare an aqueous dispersion of water-dispersed polymer nanocomposite ;

To the aqueous dispersion prepared in the step of producing the water-dispersed polymer nanocomposite, 0.1 to 5 parts by weight of an isocyanate compound, a melamine compound, an oxazoline compound, an epoxy compound, a zirconium compound, A curing agent injecting step of injecting a curing agent such as a zirconium salt compound and a silane coupling agent;

In the step of adding the curing agent, the water dispersion containing the curing agent is heated at a temperature of 50 to 120 ° C. while stirring at a rate of 500 to 2000 rpm to form the aqueous dispersion liquid for 20 to 60 minutes. A nanoporous fine powder forming step of curing the water-dispersed polymer nanocomposite coarse particles containing a core material to form a sustained-release fine powder having spherical nanoporosity;

A particle sorting step of filtering, washing, drying and classifying the sustained-release nano-porous fine powder having spherical shape prepared in the step of forming nanoporous fine powder;

Through a hermetic packaging step of compressing and packing a sustained-release fine powder having nanoporosity classified by size in a sorting step into a final aluminum laminate film;

The composition is composed of 40 to 80 parts by weight of a polymer resin, 1 to 10 parts by weight of an organic amine, 10 to 50 parts by weight of a functional core material, 0.1 to 5 parts by weight of a particle stabilizer, 10 to 80 parts by weight of a nanofiller and 0.1 to 5 parts by weight of a curing agent A sustained-release fine powder having nano porosity can be easily produced.

As described above, according to the present invention, it is possible to easily manufacture a sustained-release fine powder capable of controlling the discharge speed of the core material by controlling the pore size at the blending ratio between the polymer resin aqueous dispersion and the nanofiller, .

1 is a process flow diagram illustrating an embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS The above and other objects, features and advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings, in which:

According to the process flow chart of Fig. 1

The polymer resin in the step of preparing the polymer aqueous dispersion is used in an amount of 40 to 80 parts by weight, and the ethylene-methyl acrylate-maleic anhydride terpolymer, the ethylene-ethyl acrylate-maleic anhydride terpolymer ethylene-acrylate-maleic anhydride terpolymers such as ethylene-ethyl acrylate-maleic anhydride terpolymer and ethylene-methyl methacrylate-maleic anhydride terpolymers. maleic anhydride terpolymer, an ethylene-alkyl methacrylate-maleic anhydride terpolymer such as ethylene-ethyl methacrylate-maleic anhydride terpolymer, ), But also polyvinyl acetate, ethylene- Ethylene-vinyl acetate copolymer, polyvinyl chloride, polyvinylidene chloride, ethylene- (meth) acrylic acid copolymer, polyester (polyvinyl chloride) Polyester resin, modified nylon resin, urethane resin, phenol resin, silicone resin and epoxy resin may be used alone or in combination. The present invention is not limited thereto.

When the amount of the polymer resin used is less than 40 parts by weight, no fine powder is formed. When the amount of the polymer resin is more than 80 parts by weight, no water dispersion is formed.

The organic amine in the preparation of the polymer aqueous dispersion may be prepared by reacting ethylamine, isopropylamine, N-methyl-N, N-diethanolamine, diethanolamine, triethylamine, N, N-dimethyl ethanolamine, aminoethanolamine, and diethylamine. However, the present invention is not limited thereto. It is not.

When the amount of the organic amine used is less than 1 part by weight, a polymer aqueous dispersion is not formed. When the amount of the organic amine is more than 10 parts by weight, the solubility of the fine powder is lowered.

The organic solvent in the step of preparing the polymer aqueous dispersion is 20 to 40 parts by weight as a solvent of the polymer resin and is selected from the group consisting of ethanol, n-propanol, isopropanol, n-butanol, Methyl ethyl ketone, cyclohexanone, tetrahydrofuran, dioxane, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, And ethylene glycol monobutyl ether may be used alone or in combination, but the present invention is not limited thereto.

When the amount of the organic solvent used is less than 20 parts by weight, polymeric water dispersions are not formed. When the amount of the organic solvent is more than 40 parts by weight, the shape of the fine powder becomes irregular.

A water-soluble polymer such as polyvinyl alcohol, polyvinyl pyrrolidone, gelatin or starch is used as the particle stabilizer in the core material-containing coarse particle forming step, and 0.1 to 5 wt. Is preferably used.

If the content of the particle stabilizer is less than 0.1 part by weight, the resulting particles tend to clog the particles. If the content of the particle stabilizer is more than 5 parts by weight, the purity of the obtained fine powder is low.

10 to 50 parts by weight of the functional core material of the core material-containing coarse particles is used, and 2,6-di-tert-butyl-4-methyl phenol is used. , Poly (1,2-dihydro-2,2,4-trimethyl quinoline), tetrakis [methylene (3,5-di- Butyl-4-hydroxy-hydrocinnamate)] methane] or tris (2,4-di-tert-butyl Antioxidants such as tris (2,4-di-tert-butyl-phenyl) phosphite, phytoncide, polyethyleneimine, anthraquinone, hydroquinone, Deodorants such as naphthaquinone, benzoquinone, zinc ricinoleate and zinc abetate, methyl 2-benzimidazole cabamate, pentachlorophenol ( pentachlorophenol), p-hyd Antimicrobial agents such as p-hydroxybenzoic acid, 2,4-dihydroxybenzoic acid, ciprofloxacin, aromatic aroma components, fruit extracting oils , Lubricants such as herbal extract oil, lubricants such as zinc stearate, magnesium stearate, and calcium stearate, and hardening agents may be used, but the present invention is not limited thereto.

If the content of the functional core material used is less than 10 parts by weight, the efficacy of the sustained release is deteriorated. If the content is more than 50 parts by weight, economical efficiency is deteriorated.

10 to 80 parts by weight of the nanofiller used in the water-dispersed polymer nanocomposite production step is used. The particle size of the nanofiber is 10 to 100 nm, and is selected from the group consisting of titanium dioxide, tin oxide, aluminum oxide, zinc oxide ZnO and indium oxide are preferable, but chopped carbon fiber, graphene oxide, carbon black, clay and the like can be used. It is not.

When the amount of the nanofiller used is less than 10 parts by weight, nano-porosity is not formed in the fine powder. When the amount is more than 80 parts by weight, no fine powder is formed.

0.1 to 5 parts by weight of a cross-linking agent in the curing agent-introducing step is used, and hexamethylene diisocyanate, 2,4-toluene diisocyanate, isophorone diisocyanate isophorone diisocyanate, hexakis (methoxymethyl) melamine, hexamethylmethoxymethyl melamine, and other melamine compounds such as 2,2 < RTI ID = 0.0 > 2-oxazoline), 2- (1,1-bis (hydroxymethyl) ethyl) -2-oxazoline (2- (1-oxazoline) Bis (hydroxymethyl) ethyl) -2-oxazoline, 2- (1,1-bis (hydroxymethyl) 2-oxazoline, oxazoline compounds such as bisphenol A diglycidyl ether, and epoxides such as bisphenol A diglycidyl ether. z compond, zirconium salt compounds such as zirconium alpha-hydroxycarboxylic acid salt, vinyltrimethoxysilane, acryloxy 3-methacryloxy Acryloxy 3-methacryloxypropyl-trimethoxysilane, ß- (3,4 epoxycyclohexyl) -ethyl tri trimethoxysilane (ß- (3,4 epoxycyclohexyl) -ethyltrimethoxysilane), r-glycidoxypropyl A silane coupling agent such as r-glycidoxypropyl-trimethoxysilane or 3-aminopropyl-triethoxysilane is preferable.

When the amount of the curing agent used is less than 0.1 part by weight, curing does not proceed. When the amount of the curing agent is more than 5 parts by weight, the purity of the produced fine powder is decreased.

The method for producing a sustained-release fine powder having nano porosity according to the present invention will now be described in more detail, and its embodiments will be described as follows.

Hereinafter, the present invention will be described in more detail with reference to examples.

However, the scope of the present invention is not limited to the illustrated embodiments.

The components listed in Table 1 were mixed in the following manner using a reactor at respective mixing ratios to produce a sustained-release fine powder having nanoporosity.

Preparation of polymer aqueous dispersion of Example 1-4 A 2 L reactor was charged with 60 parts by weight of an acrylate-maleic anhydride terpolymer, 30 parts by weight of ethylene glycol-n-butyl ether, 4 parts by weight of N, N-dimethylethanolamine and 210 parts by weight Distilled water were sequentially added thereto, and the mixture was stirred for 10 minutes at a rotation speed of 300 rpm, and then the temperature of the reactor was increased to 140 ° C and stirred for an additional 20 minutes. While the mixture was stirred at 300 rpm, the reactor temperature was lowered to 25 캜, and the mixture was filtered through a 0.03 mm diameter SUS filter under a pressure of 0.2 MPa to prepare a water component.

Example 1

304 parts by weight of the polymer aqueous dispersion prepared in the 2 L reactor, 20 parts by weight of 2,6-di-tert-butyl-4-methylphenol and 0.5 part by weight of polyvinyl alcohol were sequentially added and stirred at 300 rpm for 30 minutes. (Methoxymethyl) melamine was added thereto, and the mixture was stirred at 1000 rpm while the temperature of the reactor was raised to 80 DEG C, followed by curing for 30 minutes. Then, the mixture was stirred for 30 minutes at a stirring rate of 500 rpm and mixed with 1 part by weight of hexakis The produced fine powder is filtered, washed and dried to prepare a sustained-release fine powder having nano-porosity containing an antioxidant as a core material.

Example 2

304 parts by weight of a polymer aqueous dispersion prepared in a 2 L reactor, 20 parts by weight of polyethyleneimine and 0.5 part by weight of polyvinyl alcohol were successively added, and the mixture was stirred at 300 rpm for 30 minutes, followed by the addition of 30 parts by weight of titanium dioxide. The mixture was stirred for 30 minutes, and 1 part by weight of hexakis (methoxymethyl) melamine was added thereto. The temperature of the reactor was raised to 80 DEG C while stirring at a speed of 1000 rpm, and the mixture was cured for 30 minutes. The resulting fine powder was filtered, washed, A sustained-release fine powder having nanoporosity containing a deodorant is prepared.

Example 3

304 parts by weight of the polymer aqueous dispersion prepared in the 2 L reactor, 20 parts by weight of methyl 2-benzimidazole carbamate and 0.5 part by weight of polyvinyl alcohol were sequentially added, stirred at 300 rpm for 30 minutes, and then 30 parts by weight of titanium dioxide The mixture was stirred for 30 minutes at a stirring speed of 500 rpm, and 1 part by weight of hexakis (methoxymethyl) melamine was added thereto. The mixture was stirred at 1000 rpm at elevated temperature to 80 DEG C for 30 minutes, Washed and dried to prepare a sustained-release fine powder having nanoporosity containing an antimicrobial agent as a core material.

Example 4

304 parts by weight of a polymer aqueous dispersion prepared in a 2 L reactor, 20 parts by weight of lavender herbal extract oil, and 0.5 part by weight of polyvinyl alcohol were sequentially added and stirred at 300 rpm for 30 minutes, followed by 30 parts by weight of titanium dioxide, The mixture was stirred for 30 minutes at a speed of 500 rpm, and 1 part by weight of hexakis (methoxymethyl) melamine was added thereto. The mixture was stirred at 1000 rpm and the temperature of the reactor was raised to 80 DEG C for 30 minutes. And dried to produce a sustained-release fine powder having a nano-porosity containing a fragrance as a core material.

Table 1 shows the release rates of the deep-seated fine powders by the thermogravimetric analyzer (TG) and the difference in the volatilization amounts of the refractory materials with temperature and time.

As shown in Table 1, the sustained release fine powder having nanoporous properties according to the present invention has a pore size of 45 to 70 nm, and it is confirmed that the release rate of the deep release fine powder is effectively controlled.

The method of producing sustained-release fine powder having nano-porosity according to the present invention can be applied not only to the field of polymer additives requiring a control and release system of deep seawater but also to the fields of medicine, spices and fragrance as well as herbicide, extinction agent, fungicide, And the value of its use will be tremendous.

Claims

A polymer resin, an organic solvent, an organic amine, and distilled water are sequentially added to a reactor equipped with a stirrer, a temperature controller and a condenser The mixture was stirred for 5 to 30 minutes at a rotation speed of 100 to 500 rpm and then maintained at a temperature of 60 to 220 ° C for an additional 10 to 20 minutes and then the mixture was stirred at a rotating speed of 100 to 500 rpm While the stirring was continued, the temperature of the reactor was lowered to 20 to 30 占 폚 and the mixture was filtered with a metal filter such as stainless steel having a filament diameter of 0.001 to 0.05 mm in a flat weave under a pressure of 0.1 to 0.4 MPa, A polymer aqueous dispersion producing step of producing a homogeneous polymer resin aqueous dispersion;
The polymer aqueous dispersion prepared in the step of preparing the polymer aqueous dispersion was added to a reactor equipped with a stirrer, a temperature controller and a condenser, and stirred at a rotating speed of 100 to 500 rpm to prepare an antioxidant, a deodorant, an antimicrobial agent, A core material-containing coarse particle-forming step of preparing a coarse particle-containing coarse particle-containing water dispersion by adding a particle stabilizer to a functional coarse material as a hardening agent, and then stirring for 20 to 60 minutes;
The nano-filler was added to the aqueous dispersion prepared in the step of producing the core material-containing coarse particles, stirred at a stirring speed of 500 to 2000 rpm for 20 to 40 minutes to prepare an aqueous dispersion A water-dispersed polymer nanocomposite producing step of preparing a water-dispersed polymer nanocomposite;
A curing agent injecting step of injecting a curing agent into the aqueous dispersion prepared in the step of producing the water-dispersed polymer nanocomposite;
In the step of adding the curing agent, the water dispersion containing the curing agent is heated at a temperature of 50 to 120 ° C. while stirring at a rate of 500 to 2000 rpm to form the aqueous dispersion liquid for 20 to 60 minutes. A nanoporous fine powder forming step of curing the water-dispersed polymer nanocomposite coarse particles containing a core material to form a sustained-release fine powder having spherical nanoporosity;
A particle sorting step of filtering, washing, drying and classifying the sustained-release nano-porous fine powder having spherical shape prepared in the step of forming nanoporous fine powder;
Wherein the step of compressing and packing the sustained-release fine powder having nanoporosity classified by size in the sorting step into a final aluminum laminate film is carried out in an airtight packaging step.

The method according to claim 1,
40 to 80 parts by weight of a polymer resin, 20 to 40 parts by weight of an organic solvent, 1 to 10 parts by weight of an organic amine and 150 to 300 parts by weight of distilled water are sequentially added in the step of preparing the polymer aqueous dispersion In the core material-containing coarse particle producing step of producing the water dispersion containing the core material-containing coarse particles, 211 to 430 parts by weight of the polymer water dispersion prepared in the step of producing the polymer water dispersion is administered, and the functional core material 10 To 50 parts by weight of a water-dispersible polymer nanocomposite, and 0.1 to 5 parts by weight of a particle stabilizer, wherein 10 to 80 parts by weight of a nanofiller is added And 0.1 to 5 parts by weight of a curing agent is added in the step of injecting the curing agent.

A polymer aqueous dispersion producing step of producing a milky white homogeneous polymer resin aqueous dispersion; A core material-containing coarse particle producing step of producing a coarse material-containing coarse particle-shaped water dispersion; A water-dispersed polymer nanocomposite producing aqueous dispersion in which water-dispersed polymer nanocomposite particles containing a core material are formed; A curing agent injecting step of injecting a curing agent; A nanoporous fine powder forming step of forming a sustained-release fine powder having spherical nanoporosity; A particle sorting step of sorting by size; (1) to 10 parts by weight of an organic amine, (2) 10 to 50 parts by weight of a functional core material, (3) 0.1 to 5 parts by weight of a particle stabilizer, 10 to 80 parts by weight of a nanofiller and 0.1 to 5 parts by weight of a curing agent.