WO2019027138A1 - Composition de résine pour pierre artificielle et pierre artificielle constituée de ladite composition de résine - Google Patents
Composition de résine pour pierre artificielle et pierre artificielle constituée de ladite composition de résine Download PDFInfo
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- WO2019027138A1 WO2019027138A1 PCT/KR2018/006676 KR2018006676W WO2019027138A1 WO 2019027138 A1 WO2019027138 A1 WO 2019027138A1 KR 2018006676 W KR2018006676 W KR 2018006676W WO 2019027138 A1 WO2019027138 A1 WO 2019027138A1
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- WIPO (PCT)
- Prior art keywords
- resin composition
- resin
- engineered
- engineered stone
- inorganic aggregate
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/30—Oxides other than silica
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/18—Polyesters; Polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/017—Antistatic agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
Definitions
- the present invention relates to an engineered stone resin composition and engineered stone formed therefrom. More specifically, the present invention relates to a resin composition for engineered stones excellent in weatherability, antibacterial properties, and engineering stones formed therefrom.
- Natural stones such as granite and marble have been used as decorative materials since ancient times because of their beautiful surface patterns. Natural stone is a material showing high-quality texture, and its demand has been greatly increased in the fields of flooring, wall, and sink top plate. However, since expensive natural stone can not meet the demand, various kinds of artificial stones are being developed.
- engineered stone is a resin composition obtained by mixing a natural mineral and a binder resin under compression or vibration or under vacuum / vibration conditions, thereby showing the texture of natural stone.
- Engineered stones may be prepared to have a multicolor tone by being produced in a single color, or by blending a resin mixture with each of the pigments of different colors added thereto in a mixer, or using a chip to have a natural stone texture.
- engineered stones can be manufactured to exhibit various colors and textures according to mixed natural minerals, kinds of binder resins, color of pigment, stirring process, etc., and natural stone is used as a main material, , And hardness.
- An object of the present invention is to provide a resin composition for engineered stones excellent in weatherability, antibacterial properties and the like.
- Another object of the present invention is to provide an engineered stone formed from the resin composition for engineering stone.
- the resin composition comprises a matrix resin; Inorganic aggregate; (B / A) of the peak A in the region of 370 to 390 nm and the peak B in the region of 450 to 600 nm is about 0.01 to about 3 mu m, and the average particle size is about 0.8 to about 3 mu m.
- ≪ / RTI > to about < RTI ID 0.0 > 1.0. ≪ / RTI >
- the resin composition comprises about 5 to about 20 weight percent of the matrix resin; About 40 to about 94 wt% of said inorganic aggregate; And from about 0.1 to about 10 weight percent of the zinc oxide.
- the weight ratio of the matrix resin and the inorganic aggregate may be from about 1: about 5 to about 1: about 18.
- the weight ratio of the zinc oxide and the inorganic aggregate may be from about 1: about 30 to about 1: about 500.
- the matrix resin may include at least one of a polyester resin, an acrylic resin, an epoxy resin, and a polyurethane resin.
- the matrix resin may be an unsaturated polyester resin.
- the inorganic aggregate may be a silica-based natural mineral.
- the inorganic aggregate may include at least one of a silica sand, a quartz chip, and a silica powder.
- the inorganic aggregate may comprise about 20 to about 75 weight percent silica sand, about 0.1 to about 40 weight percent quartz chip, and about 20 to about 40 weight percent silica powder.
- the resin composition may further include at least one of a curing agent, a curing accelerator, a silane coupling agent, and a pigment.
- the resin composition is prepared by measuring the initial color (L 0 * , a 0 * , b 0 * ) using a colorimeter for a 50 mm ⁇ 90 mm ⁇ 3 mm size injection sample, (L 1 * , a 1 * , b 1 * ) after the test was measured using a colorimeter, and then the color change ( ⁇ E ) Can be from about 2 to about 7:
- ⁇ L * is a difference (L 1 * -L 0 *) in the L * values before and after the test
- ⁇ a * is the difference between (a 1 * - a 0 * ) of the a * values before and after the test
- ⁇ b * Is the difference (b 1 * - b 0 * ) between the values of b * before and after the test.
- Another aspect of the present invention relates to engineered stones formed from the resin composition for Engineered Stone.
- the present invention has the effect of providing an engineered stone resin composition excellent in weatherability, antibacterial properties and the like and engineered stone formed therefrom.
- the resin composition for engineered stone according to the present invention comprises (A) a matrix resin; (B) inorganic aggregate; And (C) zinc oxide.
- a matrix resin used for engineering stone (resin-reinforced natural stone) known in the art can be used without limitation.
- an (unsaturated) polyester resin, an acrylic resin, an epoxy resin, a polyurethane resin, a combination thereof, or the like can be used.
- an unsaturated polyester resin or an acrylic resin can be used.
- the (unsaturated) polyester resin may be prepared by condensation reaction of an alpha, beta -unsaturated dibasic acid or a mixture of the dibasic acid and a saturated dibasic acid with a polyhydric alcohol.
- Examples of the?,? - unsaturated dibasic acids and saturated dibasic acids include maleic anhydride, citraconic acid, fumaric acid, itaconic acid, phthalic acid, , Phthalic anhydride, isophthalic acid, terephthalic acid, succinic acid, aipic acid, sebacic acid, tetrahydrophthalic acid, and combinations thereof.
- polyhydric alcohols such as ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, dipropylene glycol, tripropylene glycol, polypropylene glycol, 1,3-butylene glycol, hydrogenated bisphenol-A, neopentyl glycol, 2,2,4-trimethyl-1,3-pentanediol, glycerin, combinations of these, and the like.
- the polyester resin may be a monobasic acid such as acrylic acid, propionic acid or benzoic acid; Or a polybasic acid such as trimellitic acid, tetracarboxylic acid of benzol, and the like.
- the polyester-based resin may have a weight average molecular weight, as measured by gel permeation chromatography (GPC), of from about 1,000 to about 10,000 g / mol, such as from about 1,500 to about 4,000 g / mol.
- GPC gel permeation chromatography
- the acrylic resin is a polymer of a (meth) acrylic monomer such as methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl But are not limited to, polymers of monomers (blends), including but not limited to, benzyl (meth) acrylate, glycidyl (meth) acrylate, combinations thereof and the like.
- a (meth) acrylic monomer such as methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, 2-ethylhexyl
- monomers including but not limited to, benzyl (meth) acrylate, glycidyl (meth) acrylate, combinations thereof and the like.
- the acrylic resin may have a weight average molecular weight, as measured by gel permeation chromatography (GPC), of from about 10,000 to about 150,000 g / mol, such as from about 30,000 to about 100,000 g / mol.
- GPC gel permeation chromatography
- epoxy resin a bisphenol-A type epoxy resin, a bisphenol-S type epoxy resin, a tetraphenyl ethane epoxy resin, a phenol novolak type epoxy resin, a mixture thereof and the like can be used, but the present invention is not limited thereto.
- the matrix resin may comprise from about 5 to about 20 weight percent, such as from about 6 to about 13 weight percent, specifically from about 7 to about 10 weight percent, of 100 weight percent of the total resin composition.
- the engineered stone resin composition can be excellent in fluidity and the like, and an engineered stone excellent in workability, appearance (color, etc.) can be obtained.
- the inorganic aggregate according to one embodiment of the present invention is capable of exhibiting the appearance and texture of natural stone, and inorganic aggregate used in known engineering stone (resin-reinforced natural stone) can be used without limitation.
- the inorganic aggregate may include silica-based natural minerals such as silica sand, quartz chip, silica powder, combinations thereof, and the like.
- the inorganic aggregate comprises about 20% to about 75% by weight of the silica sand, such as about 30% to about 55% by weight of the silica sand, about 0.1% to about 40% by weight of the quartz chip, About 7 to about 20 weight percent of the silica powder and about 20 to about 40 weight percent of the silica powder, such as about 20 to about 28 weight percent. It is possible to obtain a resin composition for engineered stone capable of realizing the appearance and texture closer to natural stone in the above range.
- the silica sand may have an average particle size as measured by a sieving method (apparatus) of about 0.1 to about 1.5 mm, such as about 0.1 to about 1.2 mm, and the quartz chip has an average particle size From about 0.5 to about 10 mm, such as from about 1.3 to about 9 mm, and the silica powder may have an average particle size of from about 5 to about 50 microns, for example from about 10 to about 45 microns. It is possible to obtain a resin composition for engineered stone which can be easily mixed with the matrix resin in the above range, can prevent the occurrence of pores when mixed with the matrix resin, and can realize appearance and texture close to natural stone.
- the inorganic aggregate may have a Mohs hardness of greater than about 3 to about 9, such as from about 6 to about 8. Within the above range, the surface hardness, workability, crack resistance and the like of engineered stone can be excellent.
- the inorganic aggregate may comprise from about 40 to about 94 weight percent, such as from about 75 to about 90 weight percent, specifically from about 80 to about 90 weight percent, of 100 weight percent of the total resin composition.
- the engineered stone resin composition can be excellent in fluidity and the like, and an engineered stone excellent in workability, appearance (color, etc.) can be obtained.
- the weight ratio (A) :( B) of the matrix resin (A) and the inorganic aggregate (B) is about 1: about 5 to about 1: about 18, About 1: about 15, specifically about 1: about 7 to about 1: about 14. It is possible to obtain an engineered stone having better processability, appearance characteristics and the like in the above range.
- the size ratio (B / A) of the peak A and the peak B of the zinc oxide is less than about 0.01, the antibacterial property of the resin composition may be deteriorated. If the ratio B / A is more than about 1.0, There is a concern.
- the zinc oxide may have a specific surface area BET of less than or equal to about 10 m 2 / g, such as from about 1 to about 7 m 2 / g, and a purity of greater than or equal to about 99%. Within the above range, the mechanical properties and discoloration resistance of the resin composition may be excellent. In addition, when zinc oxide having a BET surface area of more than about 10 m 2 / g is applied, the intended weatherability of the present invention can not be secured.
- the zinc oxide has a peak position 2 ⁇ value in the range of 35 to 37 ° in X-ray diffraction (XRD) analysis, and the measured FWHM value (Full of diffraction peak the crystallite size value calculated by applying Scherrer's equation (equation 2) based on the width at half maximum may be about 1,000 to about 2,000 A, for example, about 1,200 to about 1,800 A.
- the resin composition may be excellent in initial color, weather resistance (discoloration resistance), antimicrobial property, mechanical property balance thereof and the like.
- K is a shape factor,? Is an X-ray wavelength,? Is an FWHM value (degree) of an X-ray diffraction peak,? Is a peak position value (peak position degree).
- the zinc oxide may be prepared by melting zinc in the form of a metal and then heating to about 850 to about 1000 ⁇ , such as about 900 to about 950 ⁇ , And then heating at about 400 to about 900 DEG C, for example, about 500 to about 800 DEG C for about 30 to about 150 minutes, for example, about 60 to about 120 minutes.
- the zinc oxide may comprise from about 0.1 to about 10 weight percent, for example, from about 0.3 to about 5 weight percent, specifically from about 0.5 to about 2 weight percent, of 100 weight percent of the total resin composition. In the above range, the weatherability and antimicrobial property for engineering stone can be excellent.
- the weight ratio (C) :( B) of the zinc oxide (C) and the inorganic aggregate (B) is about 1: about 30 to about 1: about 500, About 1: about 300, specifically about 1: about 40 to about 1: about 200. It is possible to obtain engineered stones having better weatherability, antibacterial properties, processability, appearance, balance of physical properties, and the like in the above range.
- the resin composition for engineered stones according to one embodiment of the present invention may further include additives including a curing agent, a curing accelerator, a silane coupling agent, a pigment, a mineral, and combinations thereof.
- the curing agent may be t-butyl peroxy benzoate (TBPB), methyl ethyl ketone peroxide (MEKPO) or a combination thereof.
- TBPB t-butyl peroxy benzoate
- MEKPO methyl ethyl ketone peroxide
- a reddish brown pigment such as iron oxide, a yellow pigment such as iron hydroxide, a green pigment such as chromium oxide, an azure blue pigment such as sodium aluminosilicate, a white pigment such as titanium oxide, Pigments, black pigments such as carbon black, azo pigments, phthalocyanine pigments, etc., and pearl can be further added and used, but the present invention is not limited thereto.
- the mineral may be talc (talc), gypsum, calcite, combinations thereof and the like, preferably talc, which can improve the crack resistance of engineered stones.
- the mineral has a Mohs hardness of from about 1 to about 3 and an average particle size as measured by a particle size analyzer of from about 1 to about 50 microns, such as from about 5 to about 45 microns. In the above range, the surface hardness and crack resistance of engineered stone can be excellent.
- the additive when used, it is not particularly limited as long as it does not deteriorate the physical properties of the present invention.
- about 0.1 to about 30 parts by weight may be included per 100 parts by weight of the matrix resin.
- the initial color (L 0 * , a 0 * , b 0 * ) is measured using a colorimeter for a 50 mm ⁇ 90 mm ⁇ 3 mm size injection sample ,
- the injection specimen was subjected to weather resistance test for 3,000 hours in accordance with SAE J 1960 and the color (L 1 * , a 1 * , b 1 * ) after the test was measured using a colorimeter,
- the calculated color change ([Delta] E) may be from about 2 to about 7, for example from about 2 to about 5.
- the weatherability of engineered stone can be excellent in the above range.
- ⁇ L * is a difference (L 1 * -L 0 *) in the L * values before and after the test
- ⁇ a * is the difference between (a 1 * - a 0 * ) of the a * values before and after the test
- ⁇ b * Is the difference (b 1 * - b 0 * ) between the values of b * before and after the test.
- the engineered stone according to the present invention is formed from the resin composition for engineered stone.
- the resin composition may be prepared (molded) according to a known engineering stone manufacturing method using the resin composition. Specifically, the respective components of the resin composition may be mixed (agitated), compression molded and cured under vibration or vacuum / vibration conditions, and then, if necessary, surface polished. Since such a process is well known, a detailed description thereof will be omitted.
- An unsaturated polyester resin having a weight average molecular weight of 2,500 g / mol (manufacturer: Aekyung Chemical Co., Ltd., product name: ATM100) was used.
- the ratio of the peak A in the region of 370 to 390 nm and the peak B of the region of 450 to 600 nm in the range of 370 to 390 nm in the measurement of the average particle size, the BET surface area, the purity, and the photo luminescence of the zinc oxide (C1, B / A) and the crystallite size were measured and are shown in Table 1 below.
- Average particle size (unit: ⁇ ⁇ ): The average particle size (volume average) was measured using a particle size analyzer (Beckman Coulter Laser Diffraction Particle Size Analyzer LS I3 320 instrument).
- BET surface area (unit: m 2 / g): The BET surface area was measured with a BET analyzer (Micromeritics Surface Area and Porosity Analyzer ASAP 2020 instrument) using a nitrogen gas adsorption method.
- Purity (unit:%): Purity was measured using TGA thermal analysis at a temperature of 800 ° C.
- B / A Spectra emitted from a He-Cd laser (KIMMON company, 30 mW) at a wavelength of 325 nm at room temperature was irradiated to the sample according to a photoluminescence , And the temperature of the CCD detector was maintained at -70 ° C. (B / A) of the peak A in the 370 to 390 nm region and the peak B in the 450 to 600 nm region was measured.
- the injection specimen was subjected to PL analysis by injecting a laser into the specimen without any additional treatment.
- the zinc oxide powder was placed in a pelletizer having a diameter of 6 mm and pressed to form a flat specimen. Respectively.
- K is a shape factor,? Is an X-ray wavelength,? Is an FWHM value (degree) of an X-ray diffraction peak,? Is a peak position value (peak position degree).
- (A) a matrix resin, (B) an inorganic aggregate and (C) zinc oxide were mixed according to the composition and content of the following Table 2, and 100 parts by weight of a curing agent (t-butylperoxybenzoate 1 part by weight of a silane coupling agent (trade name: Gudam, product name: WD-70) and 2 parts by weight of a curing accelerator (TBPB manufactured by Centaial Inc.), 0.2 parts by weight of a curing accelerator (6% cobalt-octoate, And 5 parts by weight of a pigment (TiO 2 , manufactured by WASIN PIGMENT, product name: HUNTSMAN TR92) were added and mixed to obtain a resin composition for Engineered Stone.
- a curing agent t-butylperoxybenzoate 1 part by weight of a silane coupling agent (trade name: Gudam, product name: WD-70) and 2 parts by weight of a curing accelerator (TBPB manufactured by Centaial Inc.), 0.2 parts by weight of
- the resin composition was put into a mold having a size of 300 mm x 300 mm x 100 mm, and the mold was vibrated for 2 minutes by up-and-down vibration at a motor speed of 3,600 rpm, and a pressure of 2 to 3 bar, , And the resin was cured at 90 DEG C for 1 hour to prepare an engineered stone.
- the weatherability and antimicrobial activity of the engineered stone thus produced were evaluated and are shown in Table 2 below.
- ⁇ L * is a difference (L 1 * -L 0 *) in the L * values before and after the test
- ⁇ a * is the difference between (a 1 * - a 0 * ) of the a * values before and after the test
- ⁇ b * Is the difference (b 1 * - b 0 * ) between the values of b * before and after the test.
- Antibacterial activity value Staphylococcus aureus and E. coli were inoculated on a 5 cm x 5 cm specimen according to JIS Z 2801 antibacterial evaluation method, and cultured at 35 ° C and RH 90% for 24 hours. Respectively.
- Antibacterial activity log (M1 / M2)
- M1 is the number of bacteria after 24 hours of incubation for the blank specimen
- M2 is the number of bacteria after 24 hours of incubation for the resin composition specimen.
- the engineered stone resin composition and engineered stone of the present invention are excellent in weather resistance, antibacterial property, flexural strength, scratch resistance and the like.
- Comparative Example 1 in which zinc oxide (C2) having a size ratio (B / A) of peaks A and B of greater than 1.0 (9.8) was measured during photoluminescence measurement of zinc oxide, weatherability, And in Comparative Example 2 using zinc oxide (C3) having a size ratio (B / A) of less than 0.01 (0.0016), the weather resistance, scratch resistance and the like are reduced. Further, in Comparative Example 3 in which zinc oxide was not used, it was found that the weather resistance and antibacterial property were lowered.
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Abstract
La présente invention concerne une composition de résine pour pierre artificielle caractérisée en ce qu'elle comprend : une résine de matrice ; un agrégat inorganique ; et de l'oxyde de zinc qui présente une taille moyenne des particules d'approximativement 0,8 à approximativement 3 µm, et dans lequel le rapport des tailles (B/A) entre un pic de région B de 450 à 600 nm et un pic de région A de 370 à 390 nm tels que mesurés par photoluminescence est d'approximativement 0,01 à approximativement 1,0. La composition de résine pour pierre artificielle présente d'excellentes propriétés antibactériennes et de résistance aux intempéries.
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US16/627,415 US20200123057A1 (en) | 2017-07-31 | 2018-06-12 | Resin Composition for Engineered Stone and Engineered Stone Formed Therefrom |
CN201880048166.7A CN110944959A (zh) | 2017-07-31 | 2018-06-12 | 用于工程石材的树脂组合物和由其形成的工程石材 |
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KR1020180037197A KR102200627B1 (ko) | 2017-07-31 | 2018-03-30 | 엔지니어드 스톤용 수지 조성물 및 이로부터 형성된 엔지니어드 스톤 |
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