KR101140932B1 - Surface treating composition for corrosion resistance improvement of steel reinforcement - Google Patents
Surface treating composition for corrosion resistance improvement of steel reinforcement Download PDFInfo
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- KR101140932B1 KR101140932B1 KR1020090026383A KR20090026383A KR101140932B1 KR 101140932 B1 KR101140932 B1 KR 101140932B1 KR 1020090026383 A KR1020090026383 A KR 1020090026383A KR 20090026383 A KR20090026383 A KR 20090026383A KR 101140932 B1 KR101140932 B1 KR 101140932B1
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/32—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also pulverulent metals
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/24—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds
- C23C22/26—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing hexavalent chromium compounds containing also organic compounds
- C23C22/28—Macromolecular compounds
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
- C23C22/80—Pretreatment of the material to be coated with solutions containing titanium or zirconium compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C08G2150/00—Compositions for coatings
- C08G2150/90—Compositions for anticorrosive coatings
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
본 발명은 (A) 나노세라믹; (B) 실리카; (C) 알루미나 졸; (D) 수용성 또는 수분산성 수지; (E) 유기 금속 화합물; 및 (F) 물을 포함하여 이루어지는 철근 표면 처리용 용액 조성물에 관한 것으로, 상기 철근 표면 처리용 용액 조성물은 환경 및 인체에 유해한 크롬 등의 중금속을 함유하지 않아 친환경적이고, 염수처리에 대해 우수한 내식성을 나타내며, 철근의 기계적 성질을 저하시키지 않는다.The present invention (A) nanoceramic; (B) silica; (C) alumina sol; (D) water-soluble or water-dispersible resins; (E) organometallic compounds; And (F) a solution composition for rebar surface treatment comprising water, wherein the solution composition for rebar surface treatment does not contain heavy metals such as chromium, which is harmful to the environment and human body, and is environmentally friendly, and has excellent corrosion resistance against salt water treatment. It does not lower the mechanical properties of the rebar.
나노세라믹, 철근, 내식성 Nanoceramic, Rebar, Corrosion Resistance
Description
본 발명은 철근의 부식을 효과적으로 방지하는 표면 처리 용액 조성물에 관한 것이다.The present invention relates to a surface treatment solution composition that effectively prevents corrosion of rebar.
종래, 철근의 부식을 방지하기 위해, 크롬(Cr(VI))을 주성분으로 하는 크로메이트(chromate) 코팅 처리가 일반적으로 실시되었다. 기존의 크로메이트 방청 코팅 처리는 크게 2가지로 분류할 수 있다. 하나는 수지 처리로 수지층의 방식기능을 보완하고 강판에 대한 밀착성을 향상시키기 위한 방법이고, 또 다른 방법은 반응형 크로메이트 처리로서 전해형(Electrolytic reaction type)과 분무형(Spray reaction type) 처리가 있다. 반응형 크로메이트 코팅은 코팅량이 [Cr] 5-80mg/㎡으로 강판의 방청요구 특성에 따라 다양하게 처리하고 있는데 주로 무도장 강판의 내식성을 강화하기 위해서 처리한다.In order to prevent corrosion of reinforcing bars, chromate coating treatment mainly containing chromium (Cr (VI)) has generally been carried out. Conventional chromate rust coating treatment can be classified into two categories. One is to improve the anticorrosive function of the resin layer and to improve the adhesion to the steel sheet by the resin treatment. The other method is the reactive chromate treatment, which is an electrolytic reaction type and a spray reaction type treatment. have. Reactive chromate coating is coated with [Cr] 5-80mg / m2 and variously treated according to the rust-proofing characteristics of the steel sheet, mainly to enhance the corrosion resistance of uncoated steel sheet.
크로메이트는 값이 싸고 내식성이 우수하여 오랫동안 사용되어 왔으나, 오늘날 후두암 등을 일으키는 일급 발암물질로 알려져 있으며, 국제적으로 환경유해 물질로 그 사용을 규제하고 있다. 유럽연합(EU)을 중심으로 한 세계 각국에서는 납(Pb), 카드늄(Cd), 수은(Hg) 등과 함께 크롬(Cr(VI))에 대한 사용을 규제하고 있는데, 이전에는 제조 및 공정배출을 규제하였으나, 최근에는 최종제품에 대해서도 규제하고 있다. 자동차에 관한 폐차조례(ELV; End of Life Cycle)에서는 상기 금속에 대한 전면규제를 시행하고 있으며, 전기 및 전자기기에 관한 RoHS(Restriction of Hazardous Substance) 규정에서는 상기 환경부하 물질이 포함되어 있는 제품의 폐기를 전면 금지하는 규제를 시행하고 있다. 따라서 현재 전세계적으로 건축, 가전 및 자동차용으로 크롬(Cr)을 사용하지 않는 부식 방지제, 즉 방청제의 개발에 부심하고 있다.Chromate has been used for a long time due to its low cost and excellent corrosion resistance. Today, chromate is known as a primary carcinogen causing laryngeal cancer, and is regulated as an environmentally harmful substance internationally. Countries around the world, including the EU, regulate the use of chromium (Cr (VI)) along with lead (Pb), cadmium (Cd), and mercury (Hg). Although recently regulated, the final product is also regulated. In the End of Life Cycle (ELV) for automobiles, the entire regulation of the metal is enforced, and the Restriction of Hazardous Substance (RoHS) regulations for electrical and electronic devices are used to There is a regulation that completely prohibits disposal. Therefore, the world is currently striving to develop corrosion inhibitors that do not use chromium (Cr), that is, rust inhibitors, for construction, home appliances, and automobiles.
크롬을 포함하지 않는 방청제의 개발은 오래전부터 다양한 각도에서 시행되어 왔다. 이러한 방청제의 제조 방법으로는 고분자 수지를 이용하는 방법과 크롬과 동족인 몰리브덴 이용방법, 부동태 피막, 실리카를 이용한 방법, 유기물의 피막에 대한 연구 등이 행해져 왔으며, 최근에는 지르코늄 및 티타늄 화합물 혹은 실란 커플링제를 이용하여 내식성을 보강하기 위한 많은 방청제가 개발되고 있다. 그러나 이들은 크로메이트 피막에 비하여 부착량이 많아야 하고, 보호막(barrier) 특성과 자기수복(self-healing)성이 떨어지며, 내식성도 불충분하기 때문에 크로메이트 대체용으로는 실용화되는데 제약 요인이 많다. 특히 수지를 기본으로 한 유기계 방청제는 코팅층이 부도체인 관계로 전기전도성이 낮으므로 용접성이 좋지 않아 가전 및 자동차 부품용으로 사용에 제한을 받고 있다. 따라서 이러한 문제점을 해결하는 수단으로서 무기계 방청제의 개발이 요구되고 있다. 그러나 종래의 무기계 방청코팅은 내식성과 내화학성이 취약하므로, 이를 해결하는 수단으로서 무기계 방 청성분과 잘 결합하는 고분자 수지를 적정량 첨가한 유-무기계 방청 코팅 조성물을 사용하고 있으나, 경화온도가 높고 전기전도성 및 용액안정성이 떨어지는 단점이 있다.The development of chromium-free rust inhibitors has long been practiced at various angles. As a method of preparing such a rust preventive agent, a method of using a polymer resin, a method of using molybdenum equivalent to chromium, a passivation film, a method using silica, and an organic film have been studied. Recently, a zirconium and titanium compound or a silane coupling agent has been studied. Many anti-corrosive agents have been developed to reinforce corrosion resistance. However, they have a larger amount of adhesion compared to chromate coatings, have poor barrier properties, self-healing properties, and insufficient corrosion resistance. In particular, the organic rust-preventing agent based on resin has a low electrical conductivity because the coating layer is a non-conductor, so the weldability is not good, and thus it is limited to use for home appliances and automobile parts. Therefore, the development of an inorganic rust preventive agent is required as a means to solve this problem. However, since the conventional inorganic anti-corrosive coating is poor in corrosion resistance and chemical resistance, as a means of solving the problem, an organic-inorganic anti-corrosive coating composition containing an appropriate amount of a polymer resin that binds well with an inorganic anti-corrosive component is used. There is a disadvantage of poor conductivity and solution stability.
따라서, 본 발명이 이루고자 하는 기술적 과제는, 국제적으로 사용규제 대상인 크롬(Cr)을 함유하는 공정인 크로메이트 공정처리에 따른 종래의 방식에서 벗어나, 우수한 내식성, 내열성, 용액 안정성을 가지는 철근 부식 방지용 표면 처리 용액 조성물을 제공하는 것이다. Accordingly, the technical problem to be achieved by the present invention is a surface treatment for preventing corrosion of reinforcing bars having excellent corrosion resistance, heat resistance and solution stability, deviating from the conventional method according to chromate processing, which is a process containing chromium (Cr) that is subject to international use restrictions. It is to provide a solution composition.
상기한 목적을 달성하기 위하여, 본 발명은In order to achieve the above object, the present invention
(A) 나노세라믹;(A) nanoceramic;
(B) 실리카;(B) silica;
(C) 알루미나 졸;(C) alumina sol;
(D) 수용성 또는 수분산성 수지;(D) water-soluble or water-dispersible resins;
(E) 유기 금속 화합물; 및(E) organometallic compounds; And
(F) 물 (F) water
을 포함하여 이루어지는 것을 특징으로 하는 철근 부식 방지용 표면 처리 용액 조성물을 제공한다.It provides a surface treatment solution composition for preventing corrosion of the reinforcing bar comprising a.
이하에서 본 발명에 대해 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명은 철근, 특히 스케일층이 얇고 결함을 다수 포함하는 수냉 철근의 부식에 취약한 부분, 특히 스케일층 위, 스케일 박리부, 결함부 등을 포함하는 철 근 표면 전체에 도포, 건조하여 외부의 부식 환경과 철근 표면을 차단시켜 철근의 부식을 효과적으로 방지할 수 있는 철근 부식 방지용 표면 처리 용액 조성물을 제공한다.The present invention is applied to the entire surface of the reinforcing steel bars, including the scale layer, the vulnerable to the corrosion of the water-cooled steel reinforcement containing a large number of defects, in particular on the scale layer, scale peeling, defects, etc. The present invention provides a surface treatment solution composition for preventing corrosion of reinforcing bars that can effectively prevent corrosion of reinforcing bars by blocking the environment and reinforcing bar surfaces.
본 발명의 철근 부식 방지용 표면 처리 용액 조성물은 철근에의 부착력이 우수하고 또한 내식성이 매우 우수하다.The surface treatment solution composition for preventing corrosion of reinforcing bar of the present invention is excellent in adhesion to rebar and very excellent in corrosion resistance.
본 발명은 조성물 총중량에 대하여, The present invention relates to the total weight of the composition,
(A) 나노세라믹 20 내지 30 중량%;(A) 20 to 30% by weight nanoceramic;
(B) 실리카 5 내지 15 중량%;(B) 5 to 15 weight percent silica;
(C) 알루미나 졸 1 내지 5 중량%;(C) 1 to 5% by weight of alumina sol;
(D) 수용성 또는 수분산성 수지 10 내지 20 중량%;(D) 10 to 20% by weight of the water-soluble or water-dispersible resin;
(E) 유기 금속 화합물 5 내지 10 중량%; 및(E) 5 to 10% by weight of the organometallic compound; And
(F) 전체 조성물 총중량인 100 중량%가 되도록 하는 잔량의 물(F) the remaining amount of water to be 100% by weight of the total composition weight
을 포함하여 이루어지는 것을 특징으로 하는 철근 부식 방지용 표면 처리 용액 조성물을 제공한다.It provides a surface treatment solution composition for preventing corrosion of the reinforcing bar comprising a.
이하에서는, 본 발명의 철근 부식 방지용 표면 처리 용액 조성물을 이루는 구성 요소 각각에 대해 설명한다.Hereinafter, each component which comprises the surface treatment solution composition for steel corrosion prevention of this invention is demonstrated.
(A) 나노 세라믹(A) nano ceramic
본 발명의 철근 표면 처리용 용액 조성물에서의 나노세라믹은 내열성 및 내 식성을 부여하기 위하여 필요하다. 상기 나노세라믹은 바람직하게는 Al2O3, SiO2 및 이들의 혼합물로 이루어진 군으로부터 선택되는 하나 이상일 수 있다. Nanoceramic in the solution composition for rebar surface treatment of the present invention is required to impart heat resistance and corrosion resistance. The nanoceramic may be at least one selected from the group consisting of Al 2 O 3 , SiO 2 and mixtures thereof.
본 발명에서 사용가능한 나노 세라믹은 여러 가지를 들 수 있으나, 입자직경이 1~12nm, 바람직하게는 3~10nm인 나노크기 입자의 세라믹이 바람직하다. 입자직경이 15nm 이상인 나노세라믹, 특히 15~50nm인 나노세라믹을 사용할 경우, 용액 조성물을 제조하는 과정에서 용액 조성물의 성상이 불안정하고, 특히 용액 조성물 내에 미세한 입자가 발생하고, 특히 용액이 겔화되는 현상이 발생할 수 있다. 그러나, 입자직경(결정크기)이 3~10nm인 나노세라믹을 이용하는 경우, 용액 안정성이 안정하여 철근의 내식성 향상에 결정적인 역할을 하는 것이다. The nano ceramics that can be used in the present invention may be various, but a nano-sized ceramic having a particle diameter of 1 to 12 nm, preferably 3 to 10 nm is preferable. In the case of using a nanoceramic having a particle diameter of 15 nm or more, particularly a nanoceramic having a diameter of 15 to 50 nm, the properties of the solution composition are unstable in the process of preparing the solution composition, in particular, fine particles are generated in the solution composition, in particular, the solution gelates. This can happen. However, in the case of using a nanoceramic having a particle diameter (crystal size) of 3 to 10 nm, the solution stability is stable and plays a decisive role in improving corrosion resistance of reinforcing bars.
상기 나노세라믹의 함량은 특별히 한정하지 않으나, 바람직하게는 전체 조성물 총 중량에 대하여 20 내지 30 중량% 포함될 수 있다. 상기 나노세라믹이 전체 조성물 총 중량에 대하여 20중량% 미만 포함되는 경우, 양호한 내식성을 확보하기 어렵고, 30 중량%를 초과하여 포함되는 경우, 내식성은 향상되나 저장안정성 및 용액의 성상이 불량해지는, 즉 겔화되는 문제점이 있으므로 바람직하지 않다.The content of the nanoceramic is not particularly limited, but may preferably include 20 to 30% by weight based on the total weight of the total composition. If the nanoceramic is included in less than 20% by weight relative to the total weight of the total composition, it is difficult to ensure good corrosion resistance, when contained in more than 30% by weight, the corrosion resistance is improved, but the storage stability and the appearance of the solution is poor, that is, It is not preferable because there is a problem of gelation.
(B) 실리카 (B) silica
본 발명의 철근 표면 처리용 용액 조성물에서의 실리카는 소지와의 부착성을 향상시키면서 커플링제로의 역할도 수행한다. 본 발명에서 실리카로서 바람직하게 사용될 수 있는 것은 약알칼리계 수분산성 실리카를 들 수 있다. The silica in the solution composition for rebar surface treatment of the present invention also plays a role as a coupling agent while improving adhesion with the base. What can be preferably used as silica in this invention is a weak alkali water-dispersible silica.
상기 실리카의 함량은 특별히 한정하지 않으나, 바람직하게는 전체 조성물 총 중량에 대하여 5 내지 15 중량% 포함될 수 있다. 상기 실리카가 전체 조성물 총 중량에 대하여 5 중량% 미만 포함되는 경우, 양호한 내식성 및 부착성을 확보하기 어렵고, 15 중량%를 초과하여 포함되는 경우, 내식성은 향상되나 저장안정성 및 용액의 성상이 불량해지는, 즉 겔화되는 문제점이 있으므로 바람직하지 않다.The content of the silica is not particularly limited, but may preferably be included in an amount of 5 to 15% by weight based on the total weight of the composition. When the silica is included less than 5% by weight relative to the total weight of the total composition, it is difficult to ensure good corrosion resistance and adhesion, and when included in excess of 15% by weight, the corrosion resistance is improved, but the storage stability and the properties of the solution are poor. That is, it is not preferable because of the problem of gelation.
(C) 알루미나 졸(C) alumina sol
본 발명의 철근 표면 처리 용액 조성물에 포함되는 알루미나 졸은 흰색 반투명 용액, pH 범위는 3.0~3.5, 30~50% 농도 용액으로, 알루미나의 입자직경은 50~300nm인 것이 바람직하고, 입자직경이 50nm인 것이 매우 바람직하다. 본 발명 조성물의 내식성에는 상기 알루미나의 입자직경이 큰 영향을 미치는데, 입자직경의 범위는 처리 용액 조성물의 부착량에 따라 조정하여 사용할 수 있다. 처리 용액 조성물의 부착량이 적을수록 입자직경이 작은 것을 사용하여야 하며 입자직경이 50nm인 알루미나의 사용시 양호한 물성을 나타내는 조성물이 제조된다. 만일 적은 부착량에서 큰 입자직경의 알루미나를 사용할 경우 코팅막이 균일하게 이루어지지 않아 내식성의 증가 효과가 거의 없고 용액의 저장안정성도 불량해진다.The alumina sol contained in the rebar surface treatment solution composition of the present invention is a white translucent solution, pH range is 3.0-3.5, 30-50% concentration solution, the particle diameter of the alumina is preferably 50-300nm, the particle diameter is 50nm Is very preferred. Although the particle diameter of the said alumina has a big influence on the corrosion resistance of the composition of this invention, the range of particle diameter can be adjusted and used according to the adhesion amount of a treatment solution composition. The smaller the adhesion amount of the treatment solution composition, the smaller the particle diameter should be used, and a composition showing good physical properties when using alumina having a particle diameter of 50 nm is prepared. If alumina having a large particle size is used at a small adhesion amount, the coating film is not uniformly formed, and thus the corrosion resistance is hardly increased and the storage stability of the solution is also poor.
상기 알루미나 졸의 함량은 특별히 한정하지 않으나, 바람직하게는 전체 조성물 총 중량에 대하여 1 내지 5 중량% 포함될 수 있다. 상기 알루미나 졸이 전체 조성물 총 중량에 대하여 1 중량% 미만 포함되는 경우, 양호한 내식성을 확보하기 어렵고, 5 중량%를 초과하여 포함되는 경우, 내식성은 향상되나 저장안정성 및 용 액의 성상이 불량해지는 문제점이 있으므로 바람직하지 않다.The content of the alumina sol is not particularly limited, but may be preferably included in an amount of 1 to 5% by weight based on the total weight of the composition. When the alumina sol is included in less than 1% by weight relative to the total weight of the composition, it is difficult to ensure good corrosion resistance, when contained in more than 5% by weight, the corrosion resistance is improved, but the storage stability and the properties of the solution is poor This is not so desirable.
(D) 수용성 또는 수분산성 수지(D) water-soluble or water-dispersible resins
본 발명의 철근 표면 처리 용액 조성물에 포함되는 수용성 또는 수분산성 수지, 즉 수계 수지는 내식성의 향상을 목적으로 배합되는 것이다. 이들 수용성 또는 수분산성 수지로서는 아크릴 수지, 우레탄 수지, 에폭시 수지, 폴리에스테르 수지, 페놀수지, 아세트산 비닐 수지, 염화 비닐리덴 수지 등을 들 수 있으며, 바람직하게는 아크릴 수지, 우레탄 수지 및 에폭시 수지로 이루어지는 군으로부터 선택되는 1종 이상을 사용할 수 있다.The water-soluble or water-dispersible resin, ie, the water-based resin, contained in the rebar surface treatment solution composition of the present invention is blended for the purpose of improving corrosion resistance. Examples of these water-soluble or water-dispersible resins include acrylic resins, urethane resins, epoxy resins, polyester resins, phenol resins, vinyl acetate resins, vinylidene chloride resins, and the like, and preferably consist of acrylic resins, urethane resins and epoxy resins. One or more types selected from the group can be used.
상기 에폭시 수지로서는 특별히 한정하는 것은 아니지만, 비스페놀형 에폭시 수지, 페놀 노볼락형 에폭시 수지, 오르토크레졸 노볼락형 에폭시 수지 등의 아미노화 변성물을 사용하는 것이 바람직하다. Although it does not specifically limit as said epoxy resin, It is preferable to use amino modified compounds, such as a bisphenol-type epoxy resin, a phenol novolak-type epoxy resin, and an ortho cresol novolak-type epoxy resin.
그러나, 수계 에폭시 수지는 무기재와의 상용성과 더불어 고온의 건조 PMT가 필요하고, 수계 우레탄 수지의 사용은 용액으로 제조상에는 문제가 없으나 제조 비용이 높으므로, 제조 비용 및 내식성을 고려하여 제일 제조가 간편하고 효율성이 높은 수용성 또는 수분산성 아크릴 수지를 사용하는 것이 보다 바람직하다. 수용성 또는 수분산성 아크릴 수지를 사용하면, 용액의 안정성과 내식성 및 저장안정성에서도 양호한 물성을 나타낼 수 있다.However, the water-based epoxy resin requires high temperature dry PMT as well as compatibility with the inorganic material, and the use of the water-based urethane resin is a solution, but there is no problem in manufacturing, but the manufacturing cost is high, so it is best to consider the manufacturing cost and corrosion resistance. It is more preferable to use simple and highly efficient water-soluble or water-dispersible acrylic resins. When water-soluble or water-dispersible acrylic resins are used, good physical properties can be exhibited even in solution stability, corrosion resistance and storage stability.
그러나, 모든 수용성 또는 수분산성 아크릴 수지를 사용할 수 있는 것은 아니며, 변성 수용성 아크릴 수지는 제조 후 용액의 안전성이 보장되기 어려우므로 사용하지 않는 것이 바람직하다. However, not all water-soluble or water-dispersible acrylic resins can be used, and the modified water-soluble acrylic resin is not preferably used because it is difficult to ensure the safety of the solution after manufacture.
상기 수용성 또는 수분산성 수지의 함량은 특별히 한정하지 않으나, 바람직하게는 전체 조성물 총 중량에 대하여 10 내지 20 중량% 포함될 수 있다. 상기 수용성 또는 수분산성 수지가 전체 조성물 총 중량에 대하여 10중량% 미만 포함되는 경우, 양호한 내식성을 확보하기 어렵고, 20 중량%를 초과하여 포함되는 경우, 내식성은 향상되나 저장안정성 및 용액의 성상이 불량해지는 문제점이 있으므로 바람직하지 않다.The content of the water-soluble or water-dispersible resin is not particularly limited, but preferably 10 to 20% by weight based on the total weight of the total composition. If the water-soluble or water-dispersible resin is contained less than 10% by weight relative to the total weight of the composition, it is difficult to ensure good corrosion resistance, when contained in more than 20% by weight, the corrosion resistance is improved but storage stability and poor solution properties It is not preferable because there is a problem of degradation.
(E) 유기금속 화합물(E) organometallic compounds
본 발명의 철근 표면 처리 용액 조성물에 포함되는 유기금속 화합물은 철근과 피막과의 밀착성을 향상시키고 결국 내식성을 향상시킨다. 유기금속 화합물로서는 일반적으로 콤플렉스 형상을 하고 있는 금속 착물에 유기물이 결합된 유기 금속화합물이 사용된다. 본 발명에서는 티타네이트 또는 지르코늄계 화합물 또는 실란계 화합물을 사용할 수 있다.The organometallic compound included in the rebar surface treatment solution composition of the present invention improves the adhesion between the reinforcing bar and the coating and, in turn, improves the corrosion resistance. As an organometallic compound, the organometallic compound which organic substance couple | bonded with the metal complex which has a complex shape generally is used. In the present invention, titanate, zirconium compound or silane compound can be used.
상기 티타네이트계 화합물의 구체적인 예로서는 티타늄 스테아레이트 착물, 티타늄 오가노 포스페이트 착물, 티타늄 아세틸아세토네이트, 이소-부톡시 티타늄 에틸아세토아세테이트, 디-이소-프로폭시 티타늄 비스 에틸아세토아세테이트, 테트라이소프로필 티타네이트, 테트라-n-부틸 티타네이트, 테트라-에틸 티타네이트 등을 들 수 있고, 1종 이상을 선택하여 사용할 수 있다. 상기 티타네이트계 화합물은 아주 소량을 첨가하여도 우수한 내식성을 나타내는데, 그 원리는 종래기술에서 언급한 지르코늄 및 티타늄 화합물 혹은 실란 커플링제의 보호막효과(Barrier effect)에 및 자기수복효과(self-healing effect) 때문인 것으로 생각된다. 수용액은 안정한 구조의 킬레이트 화합물을 형성하고, 말단에서는 이소프로폭시드기가 수용액에서 서서히 가수 분해되어 코팅 시 불용성 피막을 형성하는 것으로 보여진다. Specific examples of the titanate-based compound include titanium stearate complex, titanium organophosphate complex, titanium acetylacetonate, iso-butoxy titanium ethyl acetoacetate, di-iso-propoxy titanium bis ethylacetoacetate, tetraisopropyl titanate , Tetra-n-butyl titanate, tetra-ethyl titanate, and the like, and one or more kinds can be selected and used. The titanate-based compound exhibits excellent corrosion resistance even when a very small amount is added. The principle is based on the barrier and self-healing effects of the zirconium and titanium compounds or silane coupling agents mentioned in the prior art. It seems to be). The aqueous solution forms a chelate compound with a stable structure, and at the end, the isopropoxide group is slowly hydrolyzed in the aqueous solution to form an insoluble coating upon coating.
상기 지르코늄계 화합물의 구체적인 예로서는 테트라-n-프로필 지르코네이트, 테트라-n-부틸 지르코네이트, 트리에탄올아민 지르코네이트, 지르코 알루미네이트계인 카르복시 지르코-알루미네이트와 아민기 함유 지르코-알루미네이트 등을 들 수 있고, 1종 이상을 선택하여 사용할 수 있다. 이들 지르코 알루미네이트는 소지와 수지의 부착력, 수지와 사용된 무기재와의 결합력을 상승시켜 도막을 강인하게 하는 역할을 한다. Specific examples of the zirconium-based compound include tetra-n-propyl zirconate, tetra-n-butyl zirconate, triethanolamine zirconate, and zirco aluminate-based carboxy zirco-aluminate and amine group-containing zirco-alumina. Nate etc. can be mentioned and 1 or more types can be selected and used. These zircon aluminates increase the adhesion between the base and the resin, and the bonding force between the resin and the inorganic material used to strengthen the coating film.
상기 실란계 화합물로는 비닐 트리메톡시(에톡시) 실란, 메타 아크릴 옥시프로필 트리메톡시(에톡시) 실란, 3-글리시독시 프로필 트리메톡시(에톡시) 실란, N-(2-아미노에틸)아미노프로필 트리에톡시 실란, 아미노알킬 실란, 감마-글리딜 프로필 트리메톡시(에톡시) 실란 등을 들 수 있고, 1종 이상을 선택하여 사용할 수 있다.As said silane type compound, vinyl trimethoxy (ethoxy) silane, methacrylic oxypropyl trimethoxy (ethoxy) silane, 3-glycidoxy propyl trimethoxy (ethoxy) silane, N- (2-amino Ethyl) aminopropyl triethoxy silane, aminoalkyl silane, gamma- glycidyl propyl trimethoxy (ethoxy) silane, etc. are mentioned, One or more types can be selected and used.
상기 유기금속 화합물의 함량은 특별히 한정하지 않으나, 바람직하게는 전체 조성물 총 중량에 대하여 5 내지 10 중량% 포함될 수 있다. 전체 조성물 총 중량에 대하여 5~10 중량%의 범위로 사용하면, 수지와 강한 결합을 하여 소지에 대한 처리제의 부착력을 증진시키므로 내식성이 우수해져 크롬을 함유한 종래의 처리제 보다 우수한 물성을 갖는 처리제를 얻을 수 있다. 상기 유기금속 화합물이 전체 조성물 총 중량에 대하여 5 중량% 미만 포함되는 경우, 양호한 내식성을 확보하기 어렵고, 10 중량%를 초과하여 포함되는 경우, 용액 제조 비용이 상승하여 제조비용면에서 불리해지는 문제점이 있다. The content of the organometallic compound is not particularly limited, but may preferably be included in an amount of 5 to 10% by weight based on the total weight of the composition. When used in the range of 5 to 10% by weight based on the total weight of the total composition, it has a strong bond with the resin to enhance the adhesion of the treatment agent to the body, so that it has excellent corrosion resistance and has a superior physical property than the conventional treatment agent containing chromium. You can get it. When the organometallic compound is included in less than 5% by weight relative to the total weight of the total composition, it is difficult to ensure good corrosion resistance, and when included in excess of 10% by weight, the solution manufacturing cost increases and disadvantages in terms of manufacturing costs have.
본 발명의 철근 부식 방지용 표면 처리 용액 조성물에 포함되는 물은 특별히 한정되는 것은 아니나, 비저항값이 18M 이상인 탈이온수를 사용하는 것이 바람직하다. 상기 물의 함량은 다른 구성성분의 함량에 따라 조정될 수 있다.Although the water contained in the surface treatment solution composition for steel corrosion protection of this invention is not specifically limited, It is preferable to use deionized water whose specific resistance value is 18 M or more. The content of water can be adjusted according to the content of other components.
본 발명의 철근 부식 방지용 표면 처리 용액 조성물은 상기 언급한 구성 요소 외에 소포제, 증점제, 계면활성제, 표면장력조정제를 추가로 포함할 수 있다. The surface treatment solution composition for preventing corrosion of the present invention may further include an antifoaming agent, a thickener, a surfactant, and a surface tension modifier in addition to the aforementioned components.
본 발명의 철근 부식 방지용 표면 처리 용액 조성물은 상기에서 언급한 화합물을 일정량으로 유리하게 혼합하여 제조될 수 있으며, 혼합 방법은 특별히 제한되지 않으며 여러 가지 공지 방법을 적용할 수 있다. The surface treatment solution composition for preventing corrosion of the present invention may be prepared by advantageously mixing the above-mentioned compounds in a predetermined amount, and the mixing method is not particularly limited and various known methods may be applied.
본 발명의 철근 부식 방지용 표면 처리 용액 조성물은 크로메이트제를 사용하지 않으므로 친환경적이고, 철근에의 부착력이 우수하고 철근의 부식을 효과적으로 방지할 수 있으며 또한 강한 내열성을 가지고 있어 냉각상과 번들링 사이의 공랭시에 철근 표면에 처리가 가능하다. Since the surface treatment solution composition for preventing corrosion of the present invention does not use a chromate agent, it is environmentally friendly, has excellent adhesion to reinforcing bars, effectively prevents corrosion of reinforcing bars, and has strong heat resistance, thereby allowing air cooling between the cold phase and the bundling. On the surface of the rebar can be processed.
이하, 본 발명을 실시예를 통해 더욱 상세히 설명하고자 한다. 그러나 하기 실시예는 본 발명을 예시하는 것일 뿐, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following examples are merely to illustrate the invention, the present invention is not limited by the following examples.
[표면 처리 용액 조성물의 제조] [Production of Surface Treatment Solution Composition]
실시예Example 1 One
표면 처리 용액 조성물 100중량%에 대하여 3~10nm의 나노세라믹 30중량%, 약알칼리계 수분산 실리카 10중량%, 알루미나 졸(50nm) 5중량%, 수분산성 아크릴 수지 20중량%, 티타네이트 화합물 5 중량%, 암모늄 바나데이트 수용액 5중량% 및 잔량의 탈이온수의 혼합액을 혼합하여 표면 처리 용액 조성물을 제조하였다. 30 weight% of nanoceramic of 3-10 nm, 10 weight% of weakly alkaline water-dispersed silica, 5 weight% of alumina sol (50 nm), 20 weight% of water-dispersible acrylic resin, and
실시예 2~6Examples 2-6
상기 실시예 1과 동일한 방법으로 표면 처리 용액 조성물을 제조하되, 그 조성비를 하기 표 1에 도시된 바와 같은 조성으로 변경하여 제조하였다.To prepare a surface treatment solution composition in the same manner as in Example 1, it was prepared by changing the composition ratio to the composition shown in Table 1 below.
비교예 1~8Comparative Examples 1 to 8
상기 실시예 1과 동일한 방법으로 표면 처리 용액 조성물을 제조하되, 그 조성비를 하기 표 1에 도시된 바와 같은 조성으로 변경하여 제조하였다. To prepare a surface treatment solution composition in the same manner as in Example 1, it was prepared by changing the composition ratio to the composition shown in Table 1 below.
상기 표 1에 기재된 실시예 및 비교예의 표면 처리 용액 조성물의 특성을 알아보기 위해 하기 설명된 실험 방법에 따라 시험하였으며, 각 평가 기준에 의거 평가하였다. 또한, 하기 철근은 80~400℃의 표면 온도를 가지는 것을 사용하였다.In order to determine the properties of the surface treatment solution compositions of the Examples and Comparative Examples described in Table 1 above were tested according to the experimental method described below, and evaluated according to each evaluation criteria. In addition, the following rebar was used having a surface temperature of 80 ~ 400 ℃.
<용액 안정성 시험><Solution stability test>
각각의 조성물을 밀봉하여 30일간 보관 후 용액 상태를 측정하여 평가하였다. 실시예 1~6의 표면 처리 용액 조성물은 상태의 변화가 없었으나, 비교예 1~8의 표면 처리 용액 조성물은 층분리가 일어났다.Each composition was sealed and stored for 30 days and then evaluated by measuring the state of the solution. The surface treatment solution compositions of Examples 1 to 6 did not change state, but the surface treatment solution compositions of Comparative Examples 1 to 8 were separated.
<도막 물성 시험><Film Property Test>
* 피막 부착성: 미도포 철근과, 본 발명의 실시예 및 비교예를 도포한 철근 시편의 도막 두께를 투과전자현미경(TEM)으로 측정하고 이를 면적으로 환산하여 부착성을 평가하였다. 실시예 1~6의 표면 처리 용액 조성물은 부착성이 높은데 반해, 비교예 1~8의 표면 처리 용액 조성물은 부착성이 좋지 않았다. * Film adhesion: The thickness of the coating film of the uncoated rebar and the rebar specimens coated with the Examples and Comparative Examples of the present invention was measured by transmission electron microscope (TEM), and the adhesion was evaluated by converting the area. While the surface treatment solution compositions of Examples 1 to 6 had high adhesion, the surface treatment solution compositions of Comparative Examples 1 to 8 did not have good adhesion.
* 외관: 도장된 시편의 외관이 이물질 및 미도장 부위 없이 양호한지 평가하였다. 도장이 양호하게 된 경우, 유백색이 되었다. 본 발명의 실시예 1~6의 표면 처리 용액 조성물이 도장된 시편은 유백색이 되었다. * Appearance: It was evaluated whether the appearance of the coated specimen was good without foreign matter and unpainted area. When coating became favorable, it became milky white. Specimens coated with the surface treatment solution compositions of Examples 1 to 6 of the present invention became milky white.
<염수분무에 대한 내식성>Corrosion resistance to salt spray
미도포 철근과, 본 발명의 실시예 및 비교예를 2 또는 4% 용액으로 희석하여 도포한 철근 시편에, KS D 9502에 의거한 염수 분무 시험 및 combined corrosion tester를 이용하여 녹의 발생을 평가하였다. 일례로서, 실시예 1을 도포한 철근 시편에 염수를 분무하고 2.5시간 경과 후, 비교 시편(미도포철근)에 염수를 분무하고 1시간 경과 후 이들 철근의 표면을 촬영하였으며, 그 결과를 도 1에 나타내었다. 도 1에 나타난 바와 같이, 비교 시편인 표면 무처리 시편은 1시간 만에 철근에 녹이 발생한 반면, 본 발명의 실시예 1의 2% 및 4% 희석액 처리 시편은 2시간 30분 후에도 녹이 훨씬 적게 발생하거나 발생하지 않았다. 상기 시편들의 내부식 특성의 변화를 알아보기 위해, 전기화학적 임피던스 분광법(EIS, Electrochemical Impedance Spectroscopy)을 사용하였다. 1% NaCl 용액 내, 0.01~100 kHz의 주파수에서, AC 10 mV의 전류로 임피던스를 측정하고, 얻어진 임피던스 측정값으로부터 나이퀴스트 플롯(Niquist flot)을 구하여 전하이동저항값(Rct)을 계산할 수 있었으며 이를 도 2에 나타내었다. 상기 도 2에 나타난 바와 같이, 본 발명의 실시예 1의 희석액을 도포한 시편이 부식에 대한 저항성이 높았다.The occurrence of rust was evaluated by using a salt spray test and a combined corrosion tester according to KS D 9502 to uncoated reinforcing bars and reinforcing bar specimens diluted with 2 or 4% solutions of Examples and Comparative Examples of the present invention. As an example, 2.5 hours after the saline was sprayed on the reinforcing bar specimens coated with Example 1, the saline was sprayed on the comparative specimen (uncoated rebar), and the surface of these reinforcing bars was photographed after 1 hour, and the results are shown in FIG. 1. Shown in As shown in FIG. 1, the surface untreated specimen, which is a comparative specimen, was rusted in reinforcing bars in 1 hour, while the 2% and 4% dilution treated specimens of Example 1 of the present invention generated much less rust after 2 hours and 30 minutes. Or did not occur. In order to determine the change in corrosion resistance of the specimens, Electrochemical Impedance Spectroscopy (EIS) was used. In a 1% NaCl solution, the impedance is measured at a current of 10 mV AC at a frequency of 0.01 to 100 kHz, and the Nyquist plot is obtained from the obtained impedance measurement to calculate the charge transfer resistance value (Rct). It was shown in FIG. As shown in FIG. 2, the specimen coated with the diluent of Example 1 of the present invention had high resistance to corrosion.
<기계적 물성> <Mechanical Properties>
한편 상기 시편의 기계적 물성인 인장/항복/연신/굽힘 특성을 관련규격(KS B 0802 및 KS B 0804)에 따라 측정하여, 본 발명의 조성물을 시편에 처리한 후 철근의 기계적 성질이 변화하는지 여부를 도 3에 나타내었다. 도 3에 나타난 바와 같이, 본 발명의 표면 처리 조성물을 철근에 도포하여도 철근의 인장(UTS)/항복(YS)/연신(EL)/굽힘 특성에 변화를 유발하지 않음을 알 수 있었다. On the other hand, by measuring the tensile / yield / elongation / bending properties of the mechanical properties of the specimen in accordance with the relevant standards (KS B 0802 and KS B 0804), whether the mechanical properties of the reinforcing bars after the composition of the present invention treated the specimen Is shown in FIG. 3. As shown in Figure 3, it can be seen that the application of the surface treatment composition of the present invention to the rebar does not cause a change in the tensile (UTS) / yield (YS) / elongation (EL) / bending properties of the rebar.
상기 시험 결과와 같이 본 발명의 철근 표면 처리용 용액 조성물은 용액 안정성이 좋았으며, 철근에 대한 부착성이 뛰어났고, 염수에 대한 철근 부식 방지 능력이 탁월했으며, 이의 도포가 철근의 기계적 성질에 영향을 미치지 않았고, 도포에 의한 외관 또한 양호함을 확인할 수 있었다.As a result of the above test, the solution composition for rebar surface treatment of the present invention had good solution stability, excellent adhesion to reinforcing bars, and excellent anti-corrosion ability for reinforcing salt water, and its application influenced the mechanical properties of reinforcing bars. It was confirmed that the appearance by coating was also good.
도 1은 본 발명의 철근 부식 방지용 표면 처리 용액 조성물을 처리하지 않은 철근 및 2% 및 4% 농도로 희석하여 처리한 철근에 염수분무 테스트를 실시한 결과를 나타낸 사진이다.Figure 1 is a photograph showing the results of the salt spray test on the reinforcing bars treated with dilution to 2% and 4% concentration of unreinforced reinforcing bar surface treatment solution composition of the present invention.
도 2는 본 발명의 철근 부식 방지용 표면 처리 용액 조성물을 처리하지 않은 철근 및 2% 및 4% 농도로 희석하여 처리한 철근에 대해 전기화학적 임피던스 분광법(EIS)으로 전하이동저항을 측정하여 나타낸 그래프이다.FIG. 2 is a graph showing charge transfer resistance measured by electrochemical impedance spectroscopy (EIS) for untreated reinforcing bar and distilled bar in 2% and 4% concentrations. .
도 3은 본 발명의 철근 부식 방지용 표면 처리 용액 조성물을 처리하지 않은 철근 및 2% 및 4% 농도로 희석하여 처리한 철근에 대해 항복/인장/연신/굽힘의 기계적 성질을 측정하여 나타낸 것이다.Figure 3 shows the mechanical properties of yield / tensile / stretching / bending for the non-reinforced reinforcing bar of the surface treatment solution composition for preventing corrosion of the present invention and the reinforcing bar treated at 2% and 4% concentration.
Claims (8)
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| KR100728468B1 (en) * | 2005-12-30 | 2007-06-13 | 동부제강주식회사 | Non-cr inorganic coating materials having a excellent heat resistance and a process to produce steel sheet coated thereof |
| KR100797321B1 (en) * | 2006-12-29 | 2008-01-22 | 주식회사 포스코 | Resin composition for metal surface, method for treating metal surface using the same and metal surface treated thereby |
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| KR100728468B1 (en) * | 2005-12-30 | 2007-06-13 | 동부제강주식회사 | Non-cr inorganic coating materials having a excellent heat resistance and a process to produce steel sheet coated thereof |
| KR100797321B1 (en) * | 2006-12-29 | 2008-01-22 | 주식회사 포스코 | Resin composition for metal surface, method for treating metal surface using the same and metal surface treated thereby |
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