KR101770227B1 - Method for preparing coating composition having antifouling-antimoist barrier nature and Method for preparing film having antifouling-antimoist barrier nature using the same - Google Patents
Method for preparing coating composition having antifouling-antimoist barrier nature and Method for preparing film having antifouling-antimoist barrier nature using the same Download PDFInfo
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- KR101770227B1 KR101770227B1 KR1020150124281A KR20150124281A KR101770227B1 KR 101770227 B1 KR101770227 B1 KR 101770227B1 KR 1020150124281 A KR1020150124281 A KR 1020150124281A KR 20150124281 A KR20150124281 A KR 20150124281A KR 101770227 B1 KR101770227 B1 KR 101770227B1
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/02—Polysilicates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- 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
- C09D5/1662—Synthetic film-forming substance
- C09D5/1675—Polyorganosiloxane-containing compositions
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Abstract
According to the present invention, there is provided a process for producing an organic-inorganic hybrid silica sol comprising mixing a metal alkoxide silane sol, an organosilane coupling agent, a co-solvent containing distilled water and an alcohol, and an acidic or alkaline catalyst, step; Preparing an antifouling-damp-proof barrier mixture by mixing and stirring the gel-balance preventing additive, the organic polymer that imparts antifouling-moisture barrier properties, and distilled water; And a step of mixing and aging the organic-inorganic hybrid silica sol in the antifouling-damp-proofing barrier mixture to aging the mixture to synthesize a coating composition, and a method for preparing the composition for antifouling- A moisture-impermeable barrier film is provided. According to the present invention, the process of coating the surface of the polymer film is convenient, and it has an advantage that an antifouling-moisture barrier film having various properties can be easily produced.
Description
The present invention relates to a method for producing a coating composition having excellent antifouling-moisture barrier properties and a method for producing an antifouling-damp-proof barrier film using the same. More particularly, To a method for preparing a composition for hybrid coating and coating the same on a polymer film to produce an antifouling-moisture barrier film.
In general, the function of protecting and preserving the contents of the package is important in the field of food packaging. Therefore, the anti-fouling-barrier property (barrier property) of each species is an important property that determines the preservation property of the contents, and the necessity thereof is further increased by the packaging method, the distribution form, and the contents diversification.
Particularly, the oxygen barrier material is very important for a means for effectively blocking oxygen and for controlling the deterioration of food such as gas filling and vacuum packaging. In addition to oxygen, it has a barrier function such as various gases, organic solvent vapor, aroma and the like and can be used for prevention of rust prevention, deodorization and sublimation, and can be used in fields of confectionery bag, retort, carbonated beverage container and the like.
The anti-fouling-moisture barrier properties as described above are required not only for food packaging but also for various fields such as optical, electric, electronic, and solar cell thin films in order to improve the chemical and physical properties of advanced materials.
In order to meet the above requirements, there is a difficulty in applying a relatively high-dimensional technique when fabricating an anti-fouling-moisture barrier film using a polymer film. In addition, it is difficult to prepare a coating solution for producing an antifouling-moisture barrier film, but coating a film with a coating solution requires a high level of skill. Moreover, the equipment used for coating is expensive, and there are many difficulties in the process of continuously producing the film in connection with the coating process at the production site.
On the other hand, a polymer can manifest its functionality by its flexibility and precise processability. However, since the polymer is a material which is produced by repeatedly repeating crystallization and non-crystallization, the gas permeability of a portion having non-crystallinity is high. Therefore, the technique of shielding the amorphous portion and preventing the gas from permeating is important.
Accordingly, in order to improve the anti-fouling property of the polymer film, it is possible to modify the chemical structure of the polymer or to add a molecular level additive in order to compensate the disadvantage of the non-crystallinity of the polymer. However, this method suffers from the problem that the manufacturing method is difficult and the manufacturing cost is increased.
In order to solve the above problem, a method of laminating a film layer having good antifouling-moisture barrier property with polypropylene, polyester, polyamide film or the like is taken. As the lamination method, a solution coating method, a melt lamination method, an extrusion lamination method and the like are used in the case of a polymer material depending on a laminated material, and a vapor deposition method or a sputtering method in the case of a metal or a metal oxide.
A film layer having good anti-fouling-moisture barrier properties may be laminated with a film layer such as an aluminum metal film or a metal oxide film. However, the metal film has disadvantages of transparency and can not be used in applications requiring transparency. And the metal oxide film is good in transparency, but has insufficient flexibility, and has a disadvantage in that the cost for the deposition equipment and the processing equipment is high.
In addition, they may be coated by using a material having a high sintering synthesis such as polyvinyl alcohol, ethylene vinyl alcohol copolymer, polyacrylonitrile, cellulose, polyvinylidene chloride and the like. However, there is an environmental problem of dioxin generation when polyvinylidene chloride is coated, and there is a disadvantage that when the ethylene vinyl alcohol copolymer is pneumatically shipped, it is unreleased, and there is a limit to use thereof, and in particular, There is a drawback that the function is very poor.
On the other hand, as prior art data of the present invention, Korean Patent Laid-Open Publication No. 2014-0079803 (2014.06.27) and Korean Patent Laid-open Publication No. 2014-0010113 (Apr.
Accordingly, an object of the present invention is to provide a method for producing a composition for an antifouling-damp-proof barrier coating which is convenient in the process of coating the surface of a polymer film, and a method for producing an antifouling- In order to solve the problem.
According to an aspect of the present invention, there is provided a method for producing a metal alkoxide, which comprises mixing a metal alkoxide silane sol, an organosilane coupling agent, a co-solvent containing distilled water and an alcohol, and an acidic or alkaline catalyst, Synthesizing an organic-inorganic hybrid silica sol; Preparing an antifouling-damp-proof barrier mixture by mixing and stirring the gel-balance preventing additive, the organic polymer that imparts antifouling-moisture barrier properties, and distilled water; And mixing the organic-inorganic hybrid silica sol with the antifouling-damp-proofing barrier mixture, agitating the mixture, and aging the mixture to synthesize a coating composition.
In this step, the step of synthesizing the organic-inorganic hybrid silica sol is preferably carried out at a temperature of 20 to 40 캜 for 4 to 8 hours so that sufficient hydrolysis and condensation reaction can take place.
The silane sol may be prepared by adding one or two or more silanes selected from the group consisting of tetraethoxysilane, vinyltriethoxysilane and methyltriethoxysilane to a co-solvent in which the alcohol and water are mixed at a concentration of 0.1 to 3.5 mol .
The organosilane coupling agent is preferably one or two or more selected from the group consisting of 3-glycidoxypropyltrimethoxysilane, 3-aminopropyltriethoxysilane and urnyltriethoxysilane.
The alcohols of the cosolvent are preferably one or more selected from the group consisting of methyl alcohol, ethyl alcohol, isopropyl alcohol, propyl alcohol and butyl alcohol.
The acidic catalyst is preferably one or more selected from the group consisting of hydrochloric acid, sulfuric acid, acetic acid, and nitric acid.
On the other hand, the organic polymer is preferably included in an amount of 1 to 20 parts by weight based on 100 parts by weight of the coating composition.
The gel-balance preventing additive may be selected from the group consisting of formamide, dimethylformamide, dioxane, acetylacetone, and triethanolamine.
The organic polymer is preferably one or more selected from the group consisting of polyacrylic acid, polyvinylamine, polyvinylpyridine, chitosan, and polyvinyl alcohol.
When the organic polymer has an anionic property in the step of making the antifouling-damp-proof barrier mixture, the pH is adjusted to 4.5 by adding an acid while stirring the organic polymer, .
Also, the step of stirring the anti-fouling-damping barrier mixture and the organic-inorganic hybrid silica sol is preferably carried out at a temperature of 20 to 40 ° C for 20 to 30 hours. Here, it is preferable that aging is carried out for 40 to 60 hours in the stationary state after stirring the above-mentioned antifouling-moisture barrier mixture mixture and the organic-inorganic hybrid silica sol.
According to another aspect of the present invention, there is provided an antifouling-damp-proof barrier film comprising a polymer film coated with a composition for an antifouling-damp-proof barrier coating produced by the above-described method.
Here, the composition for an antifouling-moisture barrier coating which is coated on the polymer film is preferably hot-air dried at a temperature of 70 to 120 ° C.
The coating of the composition for the anti-fouling-moisture barrier coating may be carried out by chemical vapor deposition (CVD), physical vapor deposition (PVD), sputtering, gravure roll coating, May be used.
According to the present invention, a composition for an anti-fouling-moisture barrier coating which is prepared by using the organic-inorganic hybrid principle of a sol-gel process is prepared by controlling in a solution state, so that a process of coating the surface of the polymer film is convenient, It can be used in various ways. In terms of the physical properties of the coating composition, it is possible to easily control the molecular structure of the material. Furthermore, since the specificity of the organic substance can be introduced into the network structure of the inorganic net, thereby manifesting the functionality, diversity can be obtained.
Also, the composition for an antifouling-damp-proof barrier coating according to the present invention can be applied to an antifouling-moisture barrier film having various properties such as anti-fogging, plastic abrasion resistance, metal corrosion resistance, antistatic property, gas barrier property and the like.
1 is a flowchart illustrating a method of preparing a composition for an anti-fouling-moisture barrier coating according to an embodiment of the present invention and a method for producing an anti-fouling-moisture barrier film using the same.
The inventors of the present invention have developed a composition for an antifouling-damping barrier coating which can be prepared in a solution state by using the organic-inorganic hybrid principle of the sol-gel process while researching and developing a functional new material composite material, The present invention has been accomplished by developing an anti-fouling-moisture barrier film which can be conveniently applied on the surface of a substrate.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the present invention is not limited by these examples.
1 is a flowchart illustrating a method of preparing a composition for an anti-fouling-moisture barrier coating according to an embodiment of the present invention and a method for producing an anti-fouling-moisture barrier film using the same.
Referring to the drawings, a method (S10) for preparing a composition for an antifouling-damping barrier coating according to an embodiment of the present invention comprises the steps of synthesizing an organic-inorganic hybrid silica sol (S110) (S120), and synthesizing a coating composition (S130).
In the step (S110) of synthesizing the organic-inorganic hybrid silica sol, the organic-inorganic hybrid silica sol comprises a metal alkoxide silane sol which is a silane precursor, an organosilane coupling agent, The co-solvent and the acidic or alkaline catalyst are mixed and stirred to synthesize.
In order to more stably form the above-mentioned organic-inorganic hybrid silica sol, a method of synthesizing a sol-gel is used. In this case, the silane used is a silica-based hybrid silica sol in which silica, titanium, alumina, zirconia, The metal alkoxide silane sol is used for the hydrolysis and the condensation reaction. At this time, the characteristics of the coating composition vary depending on the silane sol selected as the precursor.
Wherein the metal alkoxide silane sol is at least one selected from the group consisting of a co-solvent in which alcohol and water are mixed at a concentration of 0.1 to 3.5 moles of one or two or more silanes selected from the group consisting of tetraethoxysilane, vinyltriethoxysilane and methyltriethoxysilane It is preferable to add them.
Since the organosilane coupling agent has an organic functional group, the molecular structure of the organic-inorganic functional network formed using the precursor becomes a well-formed molecular structure, and the size of the pores can be well imparted, so that the functional material can be effectively produced. Such an organosilane coupling agent is preferably one or two or more selected from the group consisting of 3-glycidoxypropyltrimethoxysilane, 3-aminopropyltriethoxysilane and urnyltriethoxysilane, and 0.08 to 0.2 mol Do.
The alcohols of the co-solvent are preferably selected from the group consisting of methyl alcohol, ethyl alcohol, isopropyl alcohol, propyl alcohol and butyl alcohol, and one or more of them is used in an amount of 2.5 to 4 moles. It is also preferable to mix 20 to 45 mol of distilled water. Here, the molar ratio of the metal alkoxide silane sol (silane precursor) to the co-solvent is important for producing a hybrid solution in a homogeneous state. It is also an important parameter for determining whether or not a solution can be densely coated and whether or not it can be stored for a long period of time.
The catalyst may be an acidic catalyst. As the acidic catalyst, it is preferable to mix one or more selected from the group consisting of hydrochloric acid, sulfuric acid, acetic acid, and nitric acid and 0.05 to 0.3 mol.
In the embodiment of the present invention as described above, the organic-inorganic hybrid silica sol is prepared by mixing a metal alkoxide silane sol, an organosilane coupling agent, a co-solvent and a catalyst, For 8 hours with stirring.
In the step (S120) of preparing the antifouling-damp-proof barrier mixture, the antifouling-damp-proof barrier mixture is prepared by mixing a gel anti-imbalance additive, an organic polymer imparting anti- .
It is preferable that the gel-balance preventing additive is selected from the group consisting of formamide, dimethylformamide, dioxane, acetylacetone, and triethanolamine, and 0.05 to 0.4 mol is mixed therein. These anti-gel additives are needed to prevent cracking during coating and drying and to obtain a dense film structure.
The organic polymer is introduced into the organic-inorganic hybrid silica sol to further increase the flexibility of a solid gel-gel mix, and to form a dense membrane structure to enhance gas-barrier performance. As the organic polymer, one or more selected from the group consisting of polyacrylic acid, polyvinylamine, polyvinylpyridine, chitosan, and polyvinyl alcohol may be selected and mixed, and 100 parts by weight of total 100 parts by weight of the coating composition To 20 parts by weight.
On the other hand, since the organic-inorganic hybrid silica sol prepared firstly has cations or neutrality, organic polymers having cationic or neutral properties should be added. If an anionic organic polymer is added, anion must be added to prevent it from being ionized. For example, when the organic polymer to be added has an anionic property such as polyacrylic acid, an acid (hydrochloric acid, sulfuric acid, etc.) is added while stirring to a hydrogen ion concentration (pH) of 4.5. Thereafter, it is preferable to maintain the hydrogen ion concentration (pH) at 4.5, and if it is less than 4.5, the solution becomes opaque.
In the step of synthesizing the coating composition (S130), the organic-inorganic hybrid silica sol is mixed with the antifouling-moisture barrier mixture mixture, stirred, and aged to synthesize a coating composition.
The above-mentioned antifouling-moisture barrier mixture mixture and the organic-inorganic hybrid silica sol are preferably stirred at a temperature of 20 to 40 ° C for 20 to 30 hours. Thereafter, it is preferable to aged at 40 to 60 hours in a static state.
As described above, the composition for an antifouling-damping barrier coating, which is prepared by using the organic-inorganic hybrid principle of the sol-gel process, is prepared by controlling in a solution state, so that the process of coating the surface of the polymer film is convenient, It can be used in various ways.
In terms of the physical properties of the coating composition, it is possible to easily control the molecular structure of the material.
Furthermore, since the specificity of the organic substance can be introduced into the network structure of the inorganic net, thereby manifesting the functionality, diversity can be obtained.
Hereinafter, a method for producing an antifouling-moisture barrier film using the composition for an antifouling-moisture barrier coating of the present invention produced by the above-described method will be described.
1, the antifouling-damp proof barrier film of the present invention is prepared by coating a
As the
The anti-fouling-moisture barrier film produced by the above method may have various properties such as anti-fogging property, plastic abrasion resistance, metal corrosion resistance, antistatic property, gas barrier property and the like depending on the characteristics of the coating composition.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.
≪ Example 1 >
In this example, 1.4 moles of tetraethoxysilane, 1.1 moles of vinyltrimethoxysilane, 0.3 moles of 3-glycidoxypropyltrimethoxysilane, 33 moles of isopropyl alcohol, 37 moles of distilled water and 0.08 moles of hydrochloric acid were mixed , And stirred at 30 DEG C for 6 hours to synthesize a hybrid silica sol.
Next, 0.1 mol of hydrochloric acid was added while stirring 15 wt% of polyacrylic acid, 10 wt% of polyvinyl alcohol (polymerization degree of 500), 0.3 mol of dimethylformamide, and 30 mol of distilled water, and the pH of the solution was adjusted to 4.5 or less. Thereafter, the mixture was stirred for about 2 hours to prepare an antifouling-moisture barrier mixture.
Next, the above-mentioned antifouling-moisture barrier mixture was put into the synthesized hybrid silica sol, and then stirred at 30 DEG C for 24 hours or longer. Thereafter, the composition for an antifouling-moisture barrier coating was finally synthesized by aging in a static state for 48 hours.
Finally, the composition for a synthetic anti-fouling-moisture barrier coating was coated on a polyethylene terephthalate (PET) film by gravure coating. In order to dry the coating solution, hot air was blown at 70 to 80 ° C to dry the coating solution to prepare an antifouling-moisture barrier film.
≪ Example 2 >
In this example, 1.4 mol of tetraethoxysilane, 1.1 mol of vinyltrimethoxysilane, 0.3 mol of 3-glycidoxypropyltrimethoxysilane, 33 mol of isopropyl alcohol, 40 mol of distilled water and 0.2 mol of hydrochloric acid were mixed , And stirred at 30 DEG C for 6 hours to synthesize a hybrid silica sol.
Next, 0.1 mol of hydrochloric acid was added while stirring 15 wt% of polyacrylic acid, 10 wt% of polyvinyl alcohol (polymerization degree of 500), 0.3 mol of dimethylformamide and 37 mol of distilled water, and the pH of the solution was adjusted to 4.5 or less. Thereafter, the mixture was stirred for about 2 hours to prepare an antifouling-moisture barrier mixture.
Next, the above-mentioned antifouling-moisture barrier mixture was put into the synthesized hybrid silica sol, and then stirred at 30 DEG C for 24 hours or longer. Thereafter, the composition for an antifouling-moisture barrier coating was finally synthesized by aging at a static state for 48 hours.
Finally, the composition for a synthetic anti-fouling-moisture barrier coating was coated on a polyethylene terephthalate (PET) film by gravure coating. In order to dry the coating solution, hot air was blown at 70 to 80 ° C to dry the coating solution to prepare an antifouling-moisture barrier film.
≪ Experimental Example 1 > Evaluation of moisture barrier property
Using the films prepared in Examples 1 and 2, the moisture barrier properties were evaluated as shown in Table 1 below. The results are shown in Table 2.
(g / m 2 · day)
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. It will be understood that various modifications and changes may be made without departing from the scope of the appended claims.
Claims (15)
0.05 to 0.4 moles of one of the gel balance inhibiting additives selected from the group consisting of formamide, dimethylformamide, dioxane, acetylacetone and triethanolamine, and one or more additives selected from the group consisting of polyacrylic acid, polyvinylamine, polyvinylpyridine, and chitosan Preparing an antifouling-moisture barrier mixture mixture by mixing and stirring one or more organic polymers selected from the group consisting of an organic polymer which imparts antifouling-barrier properties and distilled water; And
Mixing the organic-inorganic hybrid silica sol with the antifouling-damping barrier mixture mixture, stirring the mixture, and aging to synthesize a coating composition,
The organic polymer is contained in an amount of 1 to 20 parts by weight based on 100 parts by weight of the total amount of the coating composition,
In the step of making the antifouling-moisture barrier mixture mixture,
Wherein when the organic polymer has an anionic property, an acid is added thereto while stirring to adjust the hydrogen ion concentration (pH) to 4.5, and then the hydrogen ion concentration (pH) is maintained at 4.5. ≪ / RTI >
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| CN110643278B (en) * | 2019-09-10 | 2020-09-22 | 华南理工大学 | Water-based low-surface-energy antifouling paint and preparation method and application thereof |
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| JP2009275111A (en) | 2008-05-14 | 2009-11-26 | Dainippon Printing Co Ltd | Method for producing gas barrier composition and gas barrier laminated film |
| KR101183544B1 (en) * | 2012-01-31 | 2012-09-20 | (주)케이피텍 | Preparation method of gas barrier coating liquid |
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| JP2009275111A (en) | 2008-05-14 | 2009-11-26 | Dainippon Printing Co Ltd | Method for producing gas barrier composition and gas barrier laminated film |
| KR101183544B1 (en) * | 2012-01-31 | 2012-09-20 | (주)케이피텍 | Preparation method of gas barrier coating liquid |
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