KR101347725B1 - Binder Compositions Of Hybrid Modified Silicates And Method For Preparing The Same - Google Patents
Binder Compositions Of Hybrid Modified Silicates And Method For Preparing The Same Download PDFInfo
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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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
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
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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
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
본 발명은 도료 및 마감재에 사용하기 위한 하이브리드 변성 실리케이트 바인더 조성물에 관한 것으로, 보다 상세하게는 통기성, 불연성, 강도가 우수한 알칼리금속 실리케이트 수용액에 실란 커플링제와 메틸 트리메톡시 실란을 가수분해 및 중합시켜 내수성과 내구성을 향상시킨 하이브리드 변성 실리케이트 바인더 조성물에 관한 것이다.
본 발명의 구성성분은, 조성물 총 100 중량부를 기준으로, 규산칼륨 수용액 50~80 중량부, 규산리튬 수용액 5~20 중량부, 실란커플링제 1~10 중량부, MTMS 1~10 중량부, 아크릴 에멀젼 수용액 1~5 중량부 및 물을 포함하는 하이브리드 변성 실리케이트계 바인더 조성물을 제공한다.The present invention relates to a hybrid modified silicate binder composition for use in paints and finishes, and more particularly, by hydrolyzing and polymerizing a silane coupling agent and methyl trimethoxy silane in an aqueous alkali metal silicate solution having excellent breathability, nonflammability, and strength. The present invention relates to a hybrid modified silicate binder composition having improved water resistance and durability.
The components of the present invention, based on 100 parts by weight of the total composition, 50 to 80 parts by weight of an aqueous potassium silicate solution, 5 to 20 parts by weight of an aqueous lithium silicate solution, 1 to 10 parts by weight of a silane coupling agent, 1 to 10 parts by weight of MTMS, acrylic It provides a hybrid modified silicate-based binder composition comprising 1 to 5 parts by weight of an aqueous emulsion solution and water.
Description
본 발명은 도료 및 마감재에 사용하기 위한 하이브리드 변성 실리케이트 바인더 조성물 및 그의 제조방법에 관한 것으로, 보다 상세하게는 통기성, 불연성, 강도가 우수한 알칼리금속 실리케이트 수용액에 실란 커플링제와 메틸 트리메톡시 실란(methyl trimethoxy silane)을 첨가하여 가수분해 및 중합시켜 내수성과 내구성을 향상시킨 하이브리드 변성 실리케이트 바인더 조성물 및 그의 제조방법에 관한 것이다.
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to hybrid modified silicate binder compositions for use in paints and finishes, and more particularly, to silane coupling agents and methyl trimethoxy silanes in aqueous alkali metal silicate solutions having excellent breathability, nonflammability, and strength. The present invention relates to a hybrid modified silicate binder composition which is hydrolyzed and polymerized by adding trimethoxy silane) to improve water resistance and durability, and a method of preparing the same.
알칼리금속 실리케이트는 화학식 M2OxSiO2 (여기서 M은 Na, K, Li 등의 알칼리 금속임)로 나타낼 수 있으며, 규산나트륨, 규산칼륨 및 규산리튬으로 구분할 수 있다. 이들 알칼리금속 실리케이트 수용액은 상온에서 건조에 의해 경화되어 통기성, 불연성 및 강도가 우수한 바인더 역할을 하게 된다. 특히, 유기계 바인더에 비해 도막 강도가 우수하고, 시멘트, 콘크리트 등에 대한 부착력이 우수하고, 통기성을 보유하고 있으며, 친환경성 재료라는 측면에서 알칼리금속 실리케이트는 바인더로 널리 사용되고 있다.
Alkali metal silicates can be represented by the formula M 2 O x SiO 2 (where M is an alkali metal such as Na, K, Li, etc.) and can be classified into sodium silicate, potassium silicate and lithium silicate. These alkali metal silicate aqueous solution is cured by drying at room temperature to serve as a binder excellent in breathability, nonflammability and strength. In particular, alkali metal silicates are widely used as binders in terms of excellent coating film strength, excellent adhesion to cement, concrete, etc., breathability, and environmentally friendly materials compared to organic binders.
그러나 알칼리 금속 실리케이트는 공기 중의 수분이나 물과 쉽게 반응하여 알칼리금속이 용해되어 강도가 저하되고 백화가 발생되기 때문에 바인더로서의 역할을 하지 못하는 내수성이 매우 취약한 단점을 갖고 있다. 이에 따라서 내수성을 개선하기 위해서 다양한 기술개발이 이루어지고 있는 실정이다.However, alkali metal silicates are easily reacted with water or water in the air, so that the alkali metal is dissolved, the strength is lowered, and whitening is generated. Accordingly, various technical developments are being made to improve water resistance.
이와 관련된 기술개발과 관련하여, 알칼리금속 실리케이트 수용액에 있어서 M2O에 대한 SiO2의 몰비를 증가시키는 방법, 혹은 아세트산, 인산 등의 산을 첨가하는 방법, 2가 금속염 등을 첨가하는 방법 및 유기 고분자 에멀젼을 첨가하는 방법 등이 제시되고 있다. In connection with the related technology development, a method of increasing the molar ratio of SiO 2 to M 2 O in an aqueous alkali metal silicate solution, or adding an acid such as acetic acid or phosphoric acid, adding a divalent metal salt, etc. and organic A method of adding a polymer emulsion and the like have been proposed.
그러나, 상기에서 M2O에 대한 SiO2의 몰비를 증가시키는 방법은 결합강도가 감소되어 바인더 기능이 저하되는 단점이 있고, 산을 첨가하는 방법 및 2가 금속염 등을 첨가하는 방법은 반응속도가 너무 빠르기 때문에 저장안정성이 짧은 단점이 있다. 한편 유기고분자 에멀젼을 첨가하는 방법은 알칼리금속 실리케이트와 유기고분자 에멀젼의 균일한 혼합이 힘들고, 장기간 보관시 유기고분자 에멀젼이 파괴되어 최종적으로 바인더의 결합력이 감소되는 단점이 있다.
However, the method of increasing the molar ratio of SiO 2 to M 2 O has a disadvantage in that the binder strength decreases due to a decrease in the bond strength, and the method of adding an acid and a method of adding a divalent metal salt have a reaction rate. It is too fast and has a short storage stability. On the other hand, the method of adding an organic polymer emulsion has a disadvantage in that it is difficult to uniformly mix the alkali metal silicate and the organic polymer emulsion, and the organic polymer emulsion is destroyed during long-term storage and finally the binding strength of the binder is reduced.
본 발명자들은 이러한 문제점들을 해결하고자 연구를 거듭한 결과, 알칼리금속 실리케이트 중에서 도막 형성능이 우수하며, 백화가 발생되지 않는 규산칼륨 및 규산리튬 수용액에 실란커플링제와 메틸 트리메톡시 실란(methyl trimethoxy silane, MTMS)을 첨가하여 가수분해 및 부분 중합시켜 변성 실리케이트를 제조하고 여기에 아크릴 에멀젼을 첨가함으로써 장기간 보관이 가능하고, 결합강도가 우수한 하이브리드 변성 실리케이트계 바인더조성물을 제공할 수 있다는 사실을 알아내고 본 발명을 완성하기에 이르렀다.The present inventors have conducted research to solve these problems, and as a result, the silane coupling agent and the methyl trimethoxy silane in the aqueous solution of potassium silicate and lithium silicate are excellent in the film-forming ability among alkali metal silicates, and whitening does not occur. MTMS) was added to prepare a modified silicate by hydrolysis and partial polymerization, and it was found that the present invention can provide a hybrid modified silicate binder composition which can be stored for a long time by adding an acrylic emulsion and having excellent bonding strength. Came to complete.
따라서, 본 발명의 목적은 내수성, 부착강도, 불연성이 우수한 하이브리드 변성 실리케이트계 바인더 조성물 및 그의 제조방법을 제공하는 데 있다.
Accordingly, it is an object of the present invention to provide a hybrid modified silicate-based binder composition excellent in water resistance, adhesion strength, and incombustibility, and a method for producing the same.
이와 같이 본 발명에 의한 하이브리드 변성 실리케이트계 바인더 조성물은 공기 중의 수분이나 물과 반응하여 알칼리금속 성분이 용해되지 않아 내수성이 개선됨으로써 바인더로서 역할을 할 수 있다. 또한 무기계 성분의 함량이 높기 때문에 통기성, 불연성, 강도 등이 매우 높은 특징을 갖고 있다. 따라서 도료 및 바름재 성분의 바인더로 사용될 수 있다.
As described above, the hybrid modified silicate-based binder composition according to the present invention does not dissolve an alkali metal component due to reaction with moisture or water in the air and thus may serve as a binder by improving water resistance. In addition, because of the high content of inorganic components, it has very high characteristics such as breathability, incombustibility, strength. Therefore, it can be used as a binder of paint and varnish components.
이하, 본 발명을 더욱 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
본 발명은, 조성물 총 100 중량부를 기준으로, 다음 성분과 조성비를 갖는 하이브리드 변성 실리케이트계 바인더 조성물을 제공한다: The present invention provides a hybrid modified silicate-based binder composition having the following components and composition ratios based on 100 parts by weight of the total composition:
- 규산칼륨 수용액 50∼80 중량부, 50 to 80 parts by weight of aqueous potassium silicate solution,
- 규산리튬 수용액 5∼20 중량부, 5-20 parts by weight of an aqueous lithium silicate solution,
- 실란커플링제 1∼10 중량부, 1 to 10 parts by weight of the silane coupling agent,
- 메틸트리메톡시 실란 1∼10 중량부, 1 to 10 parts by weight of methyltrimethoxy silane,
- 아크릴 에멀젼 수용액 1∼5 중량부 및 1 to 5 parts by weight of an acrylic emulsion aqueous solution and
- 물(100 중량%까지 보충).Water (up to 100% by weight).
본 발명에서 사용되는 규산칼륨 수용액은 K2O와 SiO2의 몰비가 1 : 3.1∼3.4인 조성을 갖고, 고형분 함량이 40∼45 중량%이며, 그 사용량은 조성물 총 100 중량부를 기준으로 50∼80 중량부, 바람직하기로는 60∼75 중량부이다. 규산칼륨 수용액의 사용량이 50 중량부 미만인 경우에는 주 바인더 역할을 하는 규산칼륨 성분이 너무 낮기 때문에 결합 강도가 저하되어 바인더로서 사용하기 힘든 문제점이 있다. 반면에 80 중량부를 초과하면 수분에 취약한 규산칼륨 성분의 함량이 너무 높기 때문에 내수성을 개선하는데 한계가 있다. The potassium silicate aqueous solution used in the present invention has a composition in which the molar ratio of K 2 O and SiO 2 is 1: 3.1 to 3.4, and the solid content is 40 to 45% by weight, and the amount thereof is 50 to 80 based on 100 parts by weight of the total composition. Parts by weight, preferably 60 to 75 parts by weight. If the amount of the aqueous potassium silicate solution is less than 50 parts by weight, since the potassium silicate component serving as the main binder is too low, there is a problem in that the bonding strength is lowered and it is difficult to use as a binder. On the other hand, if it exceeds 80 parts by weight, the content of potassium silicate component vulnerable to moisture is too high, there is a limit to improve the water resistance.
본 발명에서 사용되는 규산리튬 수용액은, Li2O와 SiO2의 몰비가 1 : 4.5∼5.0인 조성을 갖고, 고형분 함량이 20∼25 중량%이며, 그 사용량은 조성물 총 100 중량부를 기준으로 5∼20 중량부, 바람직하기로는 7∼15 중량부이다. The lithium silicate aqueous solution used in the present invention has a composition in which the molar ratio of Li 2 O and SiO 2 is 1: 4.5 to 5.0, the solid content is 20 to 25% by weight, and the amount of the lithium silicate solution is 5 to 5 parts by weight based on 100 parts by weight of the total composition. 20 parts by weight, preferably 7 to 15 parts by weight.
본 발명에서 규산리튬 수용액은 상기 규산칼륨 바인더의 강도를 향상시키기 위해서 첨가하며, 그 사용량이 5 중량부 미만인 경우에는 강도향상 효과가 미비하다. 반면에 사용량이 20 중량부를 초과하더라도 더 이상 강도가 향상되지 않는다. In the present invention, the lithium silicate aqueous solution is added to improve the strength of the potassium silicate binder, and when the amount thereof is less than 5 parts by weight, the effect of improving strength is insufficient. On the other hand, even if the amount exceeds 20 parts by weight, the strength no longer improves.
본 발명에서 사용되는 실란커플링제는 규산칼륨 성분과 아크릴 에멀젼의 상용성을 개선하기 위해서 첨가하게 되며, 아미노에틸 아미노프로필 트리메톡시실란(Aminoethyl aminopropyl trimethoxysilane, AEAPTMS), 아미노프로필 트리메톡시실란(Aminopropyl trimethoxy silane, APTMS), 글리시드 옥시프로필 트리메톡시실란(Glycid oxypropyl trimethoxy silane, GPTMS), 메타크릴 옥시프로필 트리메톡시 실란(Metacryl oxypropyl trimethoxy silane, MPTMS) 및 이들의 혼합물로 이루어진 군에서 1 종 또는 그 이상이 선택되며, 그 사용량은 조성물 총 100 중량부를 기준으로 1∼10 중량부, 바람직하게는 1∼8 중량부이다. 실란커플링제의 사용량이 1 중량부 미만인 경우에는 아크릴 에멀젼과 상용성 개선 효과가 거의 없고, 10 중량부 이상인 경우에는 겔화가 발생되는 문제점이 있다. The silane coupling agent used in the present invention is added to improve the compatibility of the potassium silicate component and the acrylic emulsion, aminoethyl aminopropyl trimethoxysilane (AEAPTMS), aminopropyl trimethoxysilane (Aminopropyl trimethoxy silane (APTMS), glycid oxypropyl trimethoxy silane (GPTMS), methacryl oxypropyl trimethoxy silane (MPTMS) and mixtures thereof More than one is selected and the amount used is 1 to 10 parts by weight, preferably 1 to 8 parts by weight, based on 100 parts by weight of the total composition. When the amount of the silane coupling agent is less than 1 part by weight, there is little effect of improving the compatibility with the acrylic emulsion, and when it is 10 parts by weight or more, there is a problem that gelation occurs.
상기 실란커플링제는 하기 화학식(1)을 갖는다:The silane coupling agent has the formula (1)
상기 식에서, Where
R1은 R 1 is
R2는 CH3 혹은 C2H5이다.R 2 is CH 3 or C 2 H 5 .
상기 화학식(1)의 실란커플링제를 규산칼륨 수용액 중의 수분과 반응하는 가수분해 반응식(I)은 다음과 같다:The hydrolysis reaction formula (I) wherein the silane coupling agent of formula (1) is reacted with water in an aqueous potassium silicate solution is as follows:
반응식 (I)Scheme (I)
상기 반응식에서, R1및 R2는 상기 화학식(1)에서 정의한 바와 같다.In the above scheme, R 1 and R 2 are as defined in formula (1).
본 발명에서 사용되는 메틸트리메톡시 실란(methyl trimethoxy silane, MTMS)은 하이브리드 변성 실리케이트계 바인더에 발수성을 부여하기 위해 첨가하게 되며, 그 사용량은 조성물 총 100 중량부를 기준으로 1∼10 중량부, 바람직하게는 1∼6 중량부이다. MTMS의 사용량이 1 중량부 미만이면 발수성 효과가 없고, 10 중량부를 초과하면 겔화가 발생되는 문제점이 있다. Methyl trimethoxy silane (MTMS) used in the present invention is added in order to impart water repellency to the hybrid modified silicate-based binder, the amount used is 1 to 10 parts by weight, based on 100 parts by weight of the total composition, preferably Preferably it is 1-6 weight part. If the amount of MTMS is less than 1 part by weight, there is no water repellency effect, and if it exceeds 10 parts by weight, there is a problem that gelation occurs.
본 발명에서 사용되는 메틸트리메톡시 실란은 하기 화학식(2)을 갖는다:Methyltrimethoxy silane used in the present invention has the formula (2)
상기 화학식 (2)의 메틸트리메톡시 실란은 규산칼륨 수용액 중의 수분과 반응하여 하기 반응식 (II)과 같이 가수분해된다:The methyltrimethoxy silane of formula (2) is reacted with water in an aqueous potassium silicate solution to hydrolyze as shown in Scheme (II):
반응식 (II)Reaction formula (II)
반응식 (I) 및 반응식 (II)에서 생성된 각각의 실란올기(Si-OH)는 하기 반응식 (III)과 같이 부분적으로 중합반응이 진행된다:Each silanol group (Si-OH) produced in Schemes (I) and (II) is partially polymerized as in Scheme (III):
반응식 (III)Scheme (III)
상기 반응식 (III)에서 생성된 부분중합체는 규산칼륨 수용액에 존재하는 규산이온 주변에 위치하여 규산이온을 안정화시키는 작용을 한다.The partial polymer produced in Scheme (III) is located around the silicate ions present in the aqueous potassium silicate solution to stabilize the silicate ions.
본 발명에서 사용되는 아크릴 에멀젼 수용액(고형분 함량이 40중량%)은 규산칼륨 성분이 수분에 노출되었을 때 규산칼륨이 용해되지 않도록 내수성을 개선하기 위해서 첨가되며, 그 사용량은 조성물 총 100 중량부를 기준으로 1∼5 중량부, 바람직하게는 2∼5 중량부이다. 아크릴 에멀젼의 사용량이 조성물 총 100 중량부를 기준으로 1 중량부 미만이면 내수성의 개선 효과가 미비하고, 5 중량부를 초과하여도 내수성 개선효과가 더 이상 증가하지 않는다. 또한 아크릴 에멀젼의 고형분 함량이 40중량% 미만인 경우에 상기 중량부를 만족하여도 내수성을 개선하는 효과가 미비하다.The aqueous acrylic emulsion solution (solid content of 40% by weight) used in the present invention is added to improve the water resistance so that potassium silicate does not dissolve when the potassium silicate component is exposed to water, and the amount thereof is used based on 100 parts by weight of the total composition. 1 to 5 parts by weight, preferably 2 to 5 parts by weight. If the amount of the acrylic emulsion is less than 1 part by weight based on 100 parts by weight of the total composition, the effect of improving water resistance is inadequate, and even if it exceeds 5 parts by weight, the effect of improving water resistance is no longer increased. In addition, in the case where the solid content of the acrylic emulsion is less than 40% by weight, the effect of improving the water resistance is insufficient even if the weight part is satisfied.
아크릴 에멀젼 수용액의 pH는 8 이상이어야 한다. pH가 8 미만인 경우에는 규산칼륨 수용액의 겔화가 발생될 수 있다.The pH of the aqueous acrylic emulsion solution should be at least 8. If the pH is less than 8, gelation of the aqueous potassium silicate solution may occur.
본 발명은 또한 규산칼륨 수용액을 상온에서 100 rpm으로 교반하면서 규산리튬 수용액을 첨가하여 1 시간 동안 균일하게 혼합한 후, 상기 혼합물에 실란커플링제와 MTMS를 넣고 상온에서 200 rpm으로 2 시간 동안 가수분해시켜 안정한 변성 실리케이트 수용액을 얻은 다음, 아크릴 에멀전 수용액과 물을 첨가하여 100 rpm으로 2 시간 동안 교반함으로써 하이브리드 변성 실리케이트계 바인더 조성물을 제조하는 방법을 제공한다.The present invention also adds a lithium silicate aqueous solution while stirring the aqueous potassium silicate solution at room temperature at 100 rpm and uniformly mixed for 1 hour, and then adds a silane coupling agent and MTMS to the mixture and hydrolyzes at room temperature at 200 rpm for 2 hours. By providing a stable modified silicate aqueous solution, and then adding an acrylic emulsion aqueous solution and water and stirring for 2 hours at 100 rpm to provide a method for producing a hybrid modified silicate-based binder composition.
이하에서는, 실시예를 통하여 본 발명을 더욱 상세하게 설명하지만, 실시예가 본 발명을 한정하는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the Examples do not limit the present invention.
<< 실시예Example >>
실시예Example 1 One
교반기가 구비된 5 리터 용기에 45% 규산칼륨 수용액(상품명 PS-C200 영일화성 제품) 70g 을 넣고 상온에서 100 rpm으로 교반하면서 25% 규산리튬 수용액(상품명 LS-L100, 영일화성 제품) 5g 을 첨가하여 1 시간 동안 균일하게 혼합한 후, 상기 혼합물에 실란커플링제로 APAETMS(상품명 Z-6020, 다우코팅 제품) 10g과 MTMS(상품명 6070, 다우코팅 제품) 5g을 넣고 상온에서 200 rpm으로 2 시간 동안 가수분해시켜 안정한 변성 실리케이트 수용액을 얻은 다음, 40% 아크릴 에멀젼 수용액 “AP-6243” (아팩사 제품) 5g 과 물 10g을 첨가하여 100 rpm으로 2 시간 동안 교반함으로써 하이브리드 변성 실리케이트계 바인더 조성물 100g을 얻었다. In a 5-liter container equipped with a stirrer, 70 g of 45% aqueous potassium silicate solution (trade name: PS-C200 Youngil Chemical) and 5g of 25% aqueous lithium silicate (trade name LS-L100, Youngilsung) were stirred at 100 rpm at room temperature. After uniformly mixing for 1 hour, 10 g of APAETMS (trade name Z-6020, Dow coating product) and 5 g MTMS (trade name 6070, Dow coating product) were added to the mixture as a silane coupling agent at room temperature for 200 hours at 200 rpm. After hydrolysis to obtain a stable modified silicate aqueous solution, 5 g of 40% acrylic emulsion aqueous solution “AP-6243” (manufactured by Afax) and 10 g of water were added thereto, followed by stirring at 100 rpm for 2 hours to obtain 100 g of a hybrid modified silicate binder composition. .
실시예Example 2 내지 4 2 to 4
하기 표 2에 나타낸 성분과 조성비를 사용한 것을 제외하고는 실시예 1에서와 동일한 방법으로 실시하여 본 발명에 따른 하이브리드 변성 실리케이트계 바인더 조성물을 제조하였다. 여기에서 APTMS로서는 “Z-6011”(다우코닝사 제품), GPTMS로서는 “Z-6040”(다우코닝사 제품) 및 MPTMS로서는 “Z-6030(다우코닝사 제품)을 각각 사용하였다.A hybrid modified silicate-based binder composition according to the present invention was prepared in the same manner as in Example 1 except that the components and composition ratios shown in Table 2 were used. Here, "Z-6011" (manufactured by Dow Corning Corporation) as APTMS, "Z-6040" (manufactured by Dow Corning Corporation) as GPTMS, and "Z-6030 (manufactured by Dow Corning Corporation) as MPTMS were used, respectively.
비교예Comparative Example
본 발명의 조성물과 기존 제품의 성능을 비교하기 위하여 시중에서 구입한 규산칼륨 수용액(상품명 PS-C200 영일화성 제품) 80g 과 규산리튬 수용액(상품명 LS-L100, 영일화성 제품) 20g을 혼합하였다.In order to compare the performance of the composition of the present invention and the existing product, 80 g of a commercially available potassium silicate aqueous solution (trade name PS-C200 Youngil Chemical) and 20g of lithium silicate aqueous solution (trade name LS-L100, Youngil Chemical) were mixed.
1Example
One
2Example
2
3Example
3
4Example
4
5Example
5
에멀젼acryl
emulsion
<< 실험예Experimental Example >>
상기 실시예 1 내지 5에서 제조된 본 발명의 조성물을 이용하여 내수성, 몰탈 표면에서의 부착강도, 내수성 평가 후 부착강도를 평가하여 성능시험을 수행하였다.Using the composition of the present invention prepared in Examples 1 to 5, the performance test was performed by evaluating the adhesion strength after the water resistance, the adhesion strength on the mortar surface, and the water resistance evaluation.
(시편의 제조)(Production of specimen)
실시예 1∼5에서 제조된 바인더 조성물 및 비교예의 바인더를 20cm x 20cm 크기의 시멘트 보드에 0.1kg/㎡의 양으로 균일하게 도포하여 7일간 상온에서 경화시켜 시편을 제작하였다.The binder composition prepared in Examples 1 to 5 and the binder of Comparative Example were uniformly applied in an amount of 0.1 kg / m 2 on a 20 cm x 20 cm cement board, and cured at room temperature for 7 days to prepare a specimen.
실험예 1 (내수성 평가) Experimental Example 1 (water resistance evaluation)
7일간 경화된 시편을 수조에 2시간 동안 담가 도막의 상태를 육안으로 평가하여 다음과 같이 등급을 매겨 평가하였다.The specimens cured for 7 days were immersed in a water bath for 2 hours and evaluated by visual evaluation of the state of the coating film as follows.
○: 도막의 표면에 이상이 없는 경우.(Circle): When there is no abnormality in the surface of a coating film.
△: 도막 면적의 10% 이하가 파괴된 경우.(Triangle | delta): When 10% or less of a coating film area is destroyed.
X: 도막 면적의 10% 이상이 파괴된 경우. X: 10% or more of the coating film area is destroyed.
하기 표 2에 나타난 바와 같이, 하이브리드 변성 실리케이트계 바인더의 경우 내수성이 모두 우수하게 나타난 반면에 비교예는 내수성이 전혀 없는 것으로 나타났다.As shown in Table 2 below, the hybrid modified silicate-based binder showed excellent water resistance while the comparative example showed no water resistance at all.
실험예 2 (부착강도 평가) Experimental Example 2 (Adhesive Strength Evaluation)
7일간 경화된 시편을 KS F 4936 “콘크리트 보호용 도막재”의 시험방법에 의거하여 부착강도를 평가하였다.The adhesive strength of the specimen cured for 7 days was evaluated according to the test method of KS F 4936 "Concrete protective coating material".
하기 표 2에 나타낸 바와 같이, 부착강도는 본 발명에 따른 실시예 1 내지 5의 하이브리드 변성 실리케이트계 바인더의 경우 2.0 이상을 나타낸 반면에 비교예의 경우 1.4를 나타내고 있다. 따라서 부착강도가 매우 향상되었음을 알 수 있다. As shown in Table 2 below, the adhesion strength of the hybrid modified silicate-based binders of Examples 1 to 5 according to the present invention is 2.0 or more, whereas 1.4 is shown for the comparative example. Therefore, it can be seen that the adhesion strength is greatly improved.
실험예 3 (내수성 평가 후 부착강도 평가) Experimental Example 3 (Adhesion strength evaluation after water resistance evaluation)
내수성 평가후 부착강도는 내구성을 평가하기 위해 진행하였으며, 일반적으로 실리케이트계 바인더는 공기 중의 수분을 흡착하거나, 물의 침투로 도막의 강도가 약해지기 때문에 장기간 사용하기 힘든 문제점이 있다. 따라서 실험예 1에서 육안으로 내수성을 평가한 시편의 표면에 존재하는 수분을 제거한 후에 KS F 4936 “콘크리트 보호용 도막재”의 시험방법에 의거하여 부착강도를 평가하였다.After the water resistance evaluation, the adhesion strength was progressed to evaluate the durability, and in general, the silicate-based binder has a problem that it is difficult to use for a long time because the strength of the coating film becomes weak due to adsorption of water in the air or penetration of water. Therefore, after removing the moisture present on the surface of the specimen that was visually evaluated the water resistance in Experiment 1, the adhesion strength was evaluated based on the test method of KS F 4936 "concrete protective coating material".
하기 표 2에 나타낸 배와 같이, 내수성 평가후 부착강도는 하이브리드 변성 실리케이트계 바인더의 경우 다소 감소되더라도 1.8N/㎟ 이상의 높은 부착강도를 유지하는 반면에, 내수성이 취약한 비교예의 경우 0.8 N/㎟ 이하로 나타났다.As shown in Table 2 below, after the water resistance evaluation, the adhesive strength is maintained at a high adhesion strength of 1.8 N / mm 2 or more even if the hybrid modified silicate-based binder is slightly reduced, whereas 0.8 N / mm 2 or less in the comparative example where the water resistance is weak. Appeared.
(N/㎟)Bond strength
(N / mm < 2 &
부착강도(N/㎟)After evaluation of water resistance
Bond strength (N / mm2)
이상의 설명은 본 발명의 기술사상을 예시적으로 설명한 것에 불과하며, 본 발명이 속하는 기술분야의 당업자라면 본 발명의 본질적인 특성에서 벗어나지 않는 범위에서 다양한 수정 및 변형을 할 수 있을 것이다.The above description is merely illustrative of the technical spirit of the present invention, and those skilled in the art to which the present invention pertains may make various modifications and changes without departing from the essential characteristics of the present invention.
또한, 본 명세서에 기재된 실시예는 본 발명의 기술사상을 한정하기 위한 것이 아니라 설명하기 위한 것이고, 이러한 실시예에 의하여 본 발명의 기술사상의 범위가 한정되는 것은 아니다.In addition, the Example described in this specification is for describing rather than limiting the technical thought of this invention, and the range of the technical thought of this invention is not limited by these Examples.
그러므로 본 발명의 보호범위는 하기 청구범위에 의하여 해석되어야 하며, 그와 동등한 범위 내에 있는 모든 기술사상은 본 발명의 권리범위에 포함되는 것으로 해석되어야 할 것이다.
Therefore, the protection scope of the present invention should be interpreted by the following claims, and all technical ideas within the equivalent scope will be construed as being included in the scope of the present invention.
Claims (5)
규산칼륨 수용액에서 K2O와 SiO2의 몰비가 1 : 3.1∼3.4이고, 고형분 함량이 40∼45 중량%이며; 규산리튬 수용액에서 Li2O와 SiO2의 몰비가 1 : 4.5∼5.0이고, 고형분 함량이 20∼25 중량%이며; 아크릴 에멀젼 수용액에서 고형분 함량이 40 중량%이고, pH가 8 이상인 것을 특징으로 하는 하이브리드 변성 실리케이트계 바인더 조성물.
50 to 80 parts by weight of an aqueous potassium silicate solution, 5 to 20 parts by weight of an aqueous lithium silicate solution, 1 to 10 parts by weight of a silane coupling agent, 1 to 10 parts by weight of methyltrimethoxy silane, and an aqueous solution of an acrylic emulsion based on 100 parts by weight of the total composition. In the hybrid modified silicate-based binder composition comprising ~ 5 parts by weight and water (replenishing up to 100 parts by weight),
The molar ratio of K 2 O and SiO 2 in an aqueous potassium silicate solution is from 3.1 to 3.4 and the solid content is from 40 to 45% by weight; The molar ratio of Li 2 O and SiO 2 in an aqueous lithium silicate solution is 1: 4.5 to 5.0, and the solid content is 20 to 25% by weight; Hybrid modified silicate-based binder composition, characterized in that the solid content is 40% by weight in the acrylic emulsion aqueous solution, the pH is 8 or more.
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| KR20010089978A (en) * | 2000-04-07 | 2001-10-17 | 김성수 | Coating Material Comprising Aqueous Silicate Solution and a Coating Method Using The Same |
| KR20110006477A (en) * | 2009-07-14 | 2011-01-20 | (주) 캐어콘 | Waterproofing method of concrete structure |
| KR100982229B1 (en) | 2010-05-13 | 2010-09-14 | (주)디오 | High permeable amphiprotic agent for surface treatment of concrete and process for the preparation thereof |
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| KR20130106644A (en) | 2013-09-30 |
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