KR102130041B1 - High Performance Antirust Admixture Composition - Google Patents

High Performance Antirust Admixture Composition Download PDF

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KR102130041B1
KR102130041B1 KR1020190110149A KR20190110149A KR102130041B1 KR 102130041 B1 KR102130041 B1 KR 102130041B1 KR 1020190110149 A KR1020190110149 A KR 1020190110149A KR 20190110149 A KR20190110149 A KR 20190110149A KR 102130041 B1 KR102130041 B1 KR 102130041B1
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concrete
composition
rust
present
weight
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이재남
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주식회사 에스엔투
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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
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/121—Amines, polyamines
    • 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
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/085—Acids or salts thereof containing nitrogen in the anion, e.g. nitrites
    • 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
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/16—Acids or salts thereof containing phosphorus in the anion, e.g. phosphates
    • C04B22/165—Acids
    • 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
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/60—Agents for protection against chemical, physical or biological attack
    • C04B2103/61—Corrosion inhibitors

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

The present invention relates to a high-performance anti-rust admixture composition comprising an amino compound and phosphoric acid.

Description

고성능 방청 혼화제 조성물{High Performance Antirust Admixture Composition}High Performance Antirust Admixture Composition

본 발명은 방청 혼화제의 주원료로 사용되어오던 아질산칼슘의 사용규제와 사용상의 안전성 문제를 극복할 수 있으며, 소량으로도 안정적인 방청성능이 발현되는 것은 물론 배합에 의해 경화 전 및 후의 콘크리트 성능을 향상시킬 수 있는 고성능 방청 혼화제 조성물에 관한 것이다.The present invention can overcome the use of calcium nitrite, which has been used as a main material for the rust preventive admixture, and safety problems in use. In addition, stable antirust performance is exhibited in a small amount as well as improving the concrete performance before and after curing by mixing. It relates to a high-performance anti-corrosive admixture composition.

기존의 범용화 된 방청방법으로는 콘크리트 제조 시 소정의 방청 혼화제를 사용하고 있으며, 철근 콘크리트용 방청제의 종류에는 유기계, 무기계 및 유.무기 복합계가 있다. Existing generalized anti-corrosion methods use certain anti-corrosive admixtures for the production of concrete, and the types of anti-corrosive agents for reinforced concrete include organic, inorganic and organic/inorganic composites.

또한, 방청 매커니즘에는 애노드형 및 캐소드형이 있다. 특히, 기존 방청 혼화제에 주로 사용되어지는 원료인 아질산칼슘의 경우 양극억제제인 애노드형 이며, 애노드형 화합물의 방청성능은 용액 중에 칼슘이 존재하지 않아도 방청효과가 우수하나, 사용량이 적거나 함량이 줄어들 경우 애노드로 작용하는 금속 표면을 완전히 덮어주지 못하게 되면 철근의 전면 부식을 일으키는 문제점이 있었다. 따라서 현장에서 비용 절감을 위해 배합설계 시 애노드형 방청제의 사용량을 충분한 량으로 설계하지 않을 경우 철근부식에 의한 구조물 하자의 원인이 된다.In addition, there are an anode type and a cathode type in the antirust mechanism. In particular, in the case of calcium nitrite, which is a raw material mainly used for the existing rust preventive admixture, it is an anode type, which is an anode inhibitor, and the rust prevention performance of the anode type compound is excellent in rust prevention effect even if calcium is not present in the solution, but the amount is less or the content is reduced. In the case of failing to completely cover the surface of the metal acting as the anode, there was a problem that causes the entire corrosion of the rebar. Therefore, in order to reduce the cost in the field, if the amount of anode type rust preventive agent is not designed in sufficient amount during the formulation design, it may cause a structure defect due to corrosion of the rebar.

한편 더욱 심각한 문제는 아질산칼슘이 2018년 3월 환경부에서 고시한 화학물질관리법에 따라 유독물질로 분류됨에 따라 그 성분을 25% 이상 첨가할 수 없어 사용이 제한적이며, 철근콘크리트용 방청 혼화제로 제조하여 사용 시 혼화제 사용량이 충분하지 않을 경우 방청성능을 충분히 발휘할 수 없는 문제점이 있다. On the other hand, the more serious problem is that calcium nitrite is classified as a toxic substance according to the Chemical Management Act announced by the Ministry of Environment in March 2018, so its use cannot be added more than 25%, so its use is limited, and it is manufactured as a rust preventive admixture for reinforced concrete. When the amount of the admixture used is not sufficient, there is a problem that the rust prevention performance cannot be sufficiently exhibited.

또한, 아질산칼슘 분말의 경우 용해도가 물 0℃, 77g/100mL로 온도변화에 따라 석출되는 문제점이 있으며, 인화점이 110℃로 운반, 보관 및 제조 시 화재 및 폭발의 위험성이 있다. 특히, 아질산칼슘 수용액 25%에 기타 질산염계 물질 혼합 시 일부 유효성분이 석출되어 방청제의 성능의 변동을 일으키는 문제점이 있다.In addition, in the case of calcium nitrite powder, there is a problem that the solubility is precipitated according to the temperature change to 0 ℃, 77g/100mL of water, and there is a risk of fire and explosion during transport, storage and manufacturing at a flash point of 110 ℃. In particular, when mixing other nitrate-based substances in 25% of calcium nitrite aqueous solution, some active ingredients are precipitated, which causes a problem in the performance of the rust inhibitor.

이러한 문제점을 해결하기 위해 사용이 제한적이지 않아 고농축 제조가 가능하고, 사용량 변화에 따른 안정적 방청성능을 확보하며, 이를 유통, 생산 그리고 사용하는 과정에서 안전성 등이 확보된 철근콘크리트용 방청 혼화제 개발의 필요성이 있다.In order to solve this problem, the use is not limited, it is possible to manufacture highly concentrated, secure stable anti-rust performance according to the change in usage, and the need for the development of anti-rust admixtures for reinforced concrete that secures safety in the process of distribution, production and use. There is this.

대한민국 특허등록 제1235641호Republic of Korea Patent Registration No. 1235641

본 발명은 앞에서 설명한 바와 같은 종래 기술의 문제점을 해결하기 위하여 발명된 것으로서, 아질산칼슘 베이스의 종래 방청 혼화제 보다 고농축 제조가 가능하고 제조자 및 사용자의 안전성을 확보하며, 소량으로도 안정적인 방청성능의 확보가 가능하고, 배합시 콘크리트 경화 전 및 후의 물성을 향상시킬 수 있는 고성능 방청 혼화제 조성물을 제공하고자 함이다.The present invention was invented to solve the problems of the prior art as described above, it is possible to produce a higher concentration than the conventional anti-corrosive admixture based on calcium nitrite, secure the safety of manufacturers and users, and secure a stable anti-rust performance even in a small amount It is possible to provide a high-performance anti-corrosive admixture composition capable of improving physical properties before and after curing of concrete when compounding.

상기와 같은 목적을 달성하기 위한 본 발명에 따른 고성능 방청 혼화제 조성물(이하 "본 발명의 조성물"이라함)은 아미노화합물, 인산, 아질산염을 포함하는 것을 특징으로 한다. The high-performance anti-rust admixture composition according to the present invention (hereinafter referred to as "the composition of the present invention") according to the present invention for achieving the above object is characterized by comprising an amino compound, phosphoric acid, nitrite.

하나의 예로 아미노화합물 100중량부에 대해 인산 30 내지 60중량부, 아질산염 5 내지 15중량부를 포함하는 것을 특징으로 한다. As an example, it is characterized in that it contains 30 to 60 parts by weight of phosphoric acid and 5 to 15 parts by weight of nitrite based on 100 parts by weight of the amino compound.

하나의 예로 아미노화합물 100중량부에 대해 에틸렌디아민테트라아세트산나트륨 30 내지 60중량부가 더 포함되는 것을 특징으로 한다.As an example, 30 to 60 parts by weight of sodium ethylenediaminetetraacetic acid is further included with respect to 100 parts by weight of the amino compound.

앞서 설명한 바와 같이, 본 발명의 조성물은 아질산칼슘과 동일한 성능 대비 유효성분 함량을 약 50% 수준으로 낮출 수 있으며, 약 3 내지 4배 정도의 고농축 제조가 가능하여 적은 사용량에서도 우수한 방식성능을 발현시킬 수 있고, 고농축으로 제조하더라고 발화에 대한 안전성이 확보되는 장점이 있다. As described above, the composition of the present invention can lower the content of the active ingredient compared to the same performance as calcium nitrite to a level of about 50%, and it is possible to produce a high concentration of about 3 to 4 times, so that it can express excellent anticorrosive performance even at a small amount. It has the advantage of ensuring safety against ignition even when manufactured with high concentration.

또한, 안정적인 방청성능이 발현되는 것은 물론 배합시 콘크리트의 경화 전 및 후의 물성도 향상시킬 수 있는 장점이 있다.In addition, it has the advantage of being able to improve the physical properties of the concrete before and after curing of the concrete as well as stable anti-rust performance.

도 1은 혼화제 사용량에 따른 방청률을 나타내는 그래프.
도 2는 콘크리트중의 철근부식 촉진시험에 사용되는 공시체의 규격을 나타내는 도면.1 is a graph showing the rust prevention rate according to the amount of admixture used.
Figure 2 is a view showing the specifications of the specimen used in the reinforcement corrosion test in concrete.

아래에서는 본 발명에 따른 양호한 실시 예를 상세히 설명한다.Hereinafter, a preferred embodiment according to the present invention will be described in detail.

본 발명의 조성물은 아미노화합물(Amino Compound), 인산(Phosphoric Acid)을 포함하며, 아질산염(Nitrite)이 소량으로 더 포함될 수 있는 것을 특징으로 한다. 바람직하게는 아미노화합물 100중량부에 대해 인산 30 내지 60중량부, 아질산염 5 내지 15중량부를 포함하는 것을 특징으로 한다. The composition of the present invention is characterized in that it contains an amino compound (Amino Compound), phosphoric acid (Phosphoric Acid), nitrite (Nitrite) can be further included in a small amount. Preferably it is characterized in that it contains 30 to 60 parts by weight of phosphoric acid and 5 to 15 parts by weight of nitrite relative to 100 parts by weight of the amino compound.

본 발명의 조성물은 3개의 1차 알코올이 포함된 아미노화합물 및 인산을 포함하고, 물에 용해 시 알칼리 자유이온을 만드는 아질산염이 포함되도록 하는 것이다. The composition of the present invention is to include an amino compound and phosphoric acid containing three primary alcohols, and to include nitrite, which, when dissolved in water, produces alkali free ions.

이에 더하여 본 발명의 조성물에는 아미노화합물 100중량부에 대해 에틸렌디아민테트라아세트산나트륨 30 내지 60중량부가 더 포함되는 예가 제시된다. 에틸렌디아민테트라아세트산나트륨은 2가 및 3가의 금속이온과 안정한 수용성 킬레이트를 형성하는 안정화제로서 기능을 하는 것이다. In addition to this, the composition of the present invention is presented an example in which 30 to 60 parts by weight of sodium ethylenediaminetetraacetic acid is further included with respect to 100 parts by weight of the amino compound. Sodium ethylenediaminetetraacetate functions as a stabilizer to form stable water-soluble chelates with divalent and trivalent metal ions.

본 발명의 조성물에 의한 염화물 이온의 고정 메커니즘은 아미노화합물 및 인산 유도체 말단의 알콜기인 OH-와 Cl-이 만나 R-NH-Cl 또는 R-PO-CL을 형성하게 되고 외부로 OH-이온을 방출하는 특성을 나타내어 부식부의 장벽 역할을 하여 부동태피막을 유지한다. The mechanism of fixation of chloride ions by the composition of the present invention is that the OH - and Cl - alcohol groups at the ends of amino compounds and phosphoric acid derivatives meet to form R-NH-Cl or R-PO-CL and release OH - ions to the outside. It exhibits the characteristics of the film, and acts as a barrier for the corrosion part to maintain the passivation film.

또한, 시멘트 내 C3A가 초기에 염화물을 흡착하였다가 탄산화가 진행되면서 해리상태가 되나 아미노화합물 유도체는 Cl-의 이온 친화력에 의해 고정화 되어 안정된 상태이다. In addition, C 3 A in cement initially adsorbs chloride and then dissociates as carbonation proceeds, but the amino compound derivative is immobilized by the ionic affinity of Cl - and is stable.

특히, 에틸렌디아민테트라아세트산나트륨은 2가 및 3가의 금속이온과 안정한 수용성 킬레이트를 형성하고, 킬레이트성 방청피막을 형성시킴으로써 콘크리트 및 보수 모르타르 내 철근의 부식 또는 녹의 용출을 막아주는 역할을 한다. In particular, sodium ethylenediaminetetraacetic acid forms a stable water-soluble chelate with divalent and trivalent metal ions, and forms a chelating rust-preventive film to prevent corrosion of steel bars or elution of rust in concrete and repair mortar.

이에 더하여 에틸렌디아민테트라아세트산나트륨에 있어 양이온(NA+)의 정전기적 반발력으로 콘크리트의 경화 전 물성(작업성)을 개선시키는 작용을 하게 되는 것이며, 아질산염이 물에 용해 시 알칼리 자유이온을 형성함에 의해 시멘트 중 C3A 및 C2S 물질의 수화에 기여함에 따라 콘크리트의 경화 후 물성(압축강도)를 개선시키는 작용을 하게 되는 것이다. In addition, in sodium ethylenediaminetetraacetic acid, the electrostatic repulsion of cations (NA + ) acts to improve the properties (workability) before curing of concrete, and when nitrite is dissolved in water, alkali free ions are formed. As it contributes to hydration of C 3 A and C 2 S materials in cement, it will act to improve physical properties (compressive strength) after curing of concrete.

즉 본 발명의 조성물에 의해 부동태피막의 유지 및 염소이온의 고정화가 이루어지고 킬레이트성 방청피막이 더 형성되도록 하여 방청성을 배가시키도록 함과 동시에 경화전 및 후의 콘크리트의 물성도 향상시킬 수 있게 되는 것이다. That is, by maintaining the passivation film and immobilization of chlorine ions and further forming a chelating anti-corrosion film by the composition of the present invention, it is possible to double the anti-corrosion property and at the same time improve the physical properties of the concrete before and after curing.

이하에서는 실험 예에 의해 본 발명에 대해 설명한다.Hereinafter, the present invention will be described by experimental examples.

<철근의 염수침지시험><Brine immersion test of rebar>

먼저 하기 표 1에서 보는 바와 같이 KS F 2561 철근 콘크리트용 방청제 규격에 따른 염분의 조성으로 1L의 수용액이 되도록 염분 용액을 제조하였다.First, as shown in Table 1 below, a salt solution was prepared to be an aqueous solution of 1 L with the composition of salt according to the specification of KS F 2561 anti-corrosive agent for reinforced concrete.

Figure 112019091626918-pat00001
Figure 112019091626918-pat00001

그리고 시험용 염수는 측정용 용기를 사용하여 처음에 물 250mL를 넣고, 상기 제조된 염분 용액 203mL를 가한 후에 수산화칼슘 3g을 가해 교반하였으며, 여기에 기존 방청제 원료(A)인 아질산칼슘 25% 수용액과 본 발명의 조성물(B) 25% 수용액을 500중량%를 기준으로 각각 0.5중량%, 1.0중량%, 1.5중량%, 2.0중량%, 2.5 중량% 및 3.0중량%를 첨가하고, 교반하면서 다시 물을 가하여 전량이 500mL가 되도록 시험용 용액을 각각 6수준, 2배치로 조제 하였다.And for the test saline, 250 mL of water was initially added using a measuring vessel, and after adding 203 mL of the prepared saline solution, 3 g of calcium hydroxide was added and stirred. Here, a 25% aqueous solution of calcium nitrite, which is an existing rust inhibitor raw material (A), and the present invention The composition (B) of a 25% aqueous solution was added 0.5 wt%, 1.0 wt%, 1.5 wt%, 2.0 wt%, 2.5 wt% and 3.0 wt%, respectively, based on 500 wt%. The test solution was prepared in 6 levels and 2 batches, respectively, to make this 500 mL.

각각 시험용 염수용액에 기준 철근을 침지하여 방청율을 측정 및 산출 하였으며, 사용된 기준철근은 KS D 3526의 SGD3에 규정하는 재질을 가지고 KS D 3561에 규정하는 것을 사용하였다.The rust resistance was measured and calculated by immersing the standard rebar in each test brine solution, and the standard rebar used was KS D 3561 with the material specified in SGD3 of KS D 3526.

침지조건은 시험용 용기를 밀봉한 상태에서 7일간 30℃의 조건으로 진행하였으며, 결과의 계산은 철근면적에 대한 표면 부식면적의 백분율로 산출하여 정리하였다.The immersion conditions were conducted under conditions of 30°C for 7 days while the test container was sealed, and the calculation of the results was summarized by calculating the percentage of surface corrosion area to rebar area.

각각의 시료에 대한 실험결과가 도 1 및 하기 표 2에 도시되고 있는 바, 도 1 및 표 2에서 보는 바와 같이 사용량 증가에 따라 안정적 부식억제 효과가 향상되는 것을 알 수 있으며, 특히 본 발명의 조성물의 경우가 동일한 농도 대비 우수한 방식성을 확보하는 것으로 확인 되었다. As the experimental results for each sample are shown in FIGS. 1 and 2, it can be seen that, as shown in FIGS. 1 and 2, the stable corrosion inhibitory effect is improved according to the increase in usage, and in particular, the composition of the present invention It was confirmed that the case secures excellent anticorrosiveness compared to the same concentration.

이는 상기에서 언급한 바와 같이 아미노화합물과 인산의 유ㆍ무기 복합에 따른 애노드 및 캐소드의 복합작용과 에틸렌디아민테트라아세트산나트륨의 킬레이트성 방청피막의 형성에 의해 사용량 변화에 따른 안정적 방식성능을 확보하며, 기존 방청제(비교예)에 비해 적은 사용량에도 방식성능에 대한 유리한 효과가 발현되는 것이다.This ensures stable anticorrosive performance according to the amount of use by the complex action of the anode and cathode according to the organic/inorganic complex of the amino compound and phosphoric acid and the formation of a chelating rust preventive film of ethylenediaminetetraacetic acid, as mentioned above. Advantageous effect on the anticorrosive performance is expressed even in a small amount of use compared to the existing rust inhibitor (comparative example).

특히, 본 발명의 조성물(B)은 아질산칼슘 25% 수용액 보다 동일한 사용량에서 최소 2배 이상의 방청성능을 보이고 있어 2배 이상의 고농축 제조가 가능한 것이 확인 되었으며, 필요에 따라 농축 수준을 달리 적용하여 상용 할 수 있는 장점이 확인 되었다.In particular, the composition (B) of the present invention has been confirmed to be capable of producing at least two times higher concentration than the 25% aqueous solution of calcium nitrite at the same amount of use, thus making it possible to produce two times higher concentrations and to apply commercially different concentration levels as needed. An advantage that could be identified.

Figure 112019091626918-pat00002
Figure 112019091626918-pat00002

<콘크리트중의 철근부식 촉진시험><Reinforcement test for reinforced corrosion in concrete>

하기 표 3에서 보는 바와 같이 KS F 2561 철근콘크리트용 방청제 규격에 따라 공시체를 제작하였다. 물은 상수돗물을 사용하였으며, 염분용액은 상기 표 1에서 보는 바와 같이 KS F 2561 철근 콘크리트용 방청제 규격에 따른 염분의 조성으로 1L의 수용액이 되도록 염분 용액을 제조하였다.As shown in Table 3 below, a specimen was prepared according to the specification of KS F 2561 anti-corrosive agent for reinforced concrete. Water was used as tap water, and the salt solution was prepared to be an aqueous solution of 1 L with the composition of salt according to the KS F 2561 rust inhibitor specification for reinforced concrete as shown in Table 1 above.

Figure 112019091626918-pat00003
Figure 112019091626918-pat00003

도 2에서 보는 바와 같이 공시체는 직경 100mm, 높이 200mm의 원주형 몰드를 사용하고, 철근은 KS D 3526의 SGD3에 규정하는 재질을 가지고 KS D 3561에 규정하는 것을 사용하였다.As shown in Figure 2, the specimen is a cylindrical mold having a diameter of 100 mm and a height of 200 mm, and the reinforcing bar has a material specified in SGD3 of KS D 3526 and is specified in KS D 3561.

하기 표 4에서 보는 바와 같이 KS F 2561 철근콘크리트용 방청제 규격에 따라 콘크리트중의 철근부식 촉진시험을 위한 콘크리트 배합을 실시하였다. 또한, 기존 아질산 칼슘계 방청제의 범용화 된 사용량인 3.9kg/m3을 고려하여 본 발명의 조성물(B)의 유효성분은 15%로 낮게 제조하여 적용하였다.As shown in Table 4 below, concrete formulations for the reinforcement corrosion test in concrete were carried out according to the KS F 2561 anti-corrosive agent specification for reinforced concrete. In addition, considering the generalized use amount of the conventional calcium nitrite-based rust inhibitor 3.9kg/m 3 , the active ingredient of the composition (B) of the present invention was manufactured and applied as low as 15%.

Figure 112019091626918-pat00004
Figure 112019091626918-pat00004

상기 방법으로 시험편을 제작하고, 20±3 ℃의 조건으로 7일간 표준양생을 실시 한 후 KS F 2561 철근콘크리트용 방청제 규격에 따라 하기의 방법으로 실험을 진행 하였다.The test piece was prepared by the above method, and standard curing was performed for 7 days under the condition of 20±3° C., and then the experiment was conducted according to the KS F 2561 anti-corrosive agent specification for reinforced concrete.

a) 양생이 종료된 시험체를 오토클레이브 장치에 넣고 밀폐하여 3시간~4시간에 온도 약 180℃ 또는 압력이 약 1.0MPa 까지 상승시킨 후, 그 상태를 5시간 유지한다.a) The cured specimen is placed in an autoclave, sealed, and then raised to a temperature of about 180° C. or a pressure of about 1.0 MPa in 3 to 4 hours, and the state is maintained for 5 hours.

b) a)의 조작을 한 후 자연 방랭한다.b) After the operation of a), let it cool naturally.

c) 오토클레이브 개시부터 약 24기산 경과 후 그 상태를 유지한다.c) It remains in the state after about 24 calculations have elapsed since the start of the autoclave.

d) 다시 a) 및 b)의 조작을 하고, 제 2회 오토클레이브 개시 약 24시간 경과 후에 공시체를 꺼낸다.d) The operations of a) and b) are performed again, and the specimen is taken out after about 24 hours after the start of the second autoclave.

e) 공시체를 갈라서 철근을 떼어낸다.e) Remove the rebar by splitting the specimen.

f) 철근의 부식 면적은 철근의 표면에 투명한 시트를 대고 부식한 부분을 찍어 그 면적(mm2)을 적당한 방법으로 구한다.f) The corrosion area of the reinforcing bar is determined by placing the transparent sheet on the surface of the reinforcing bar and taking the corroded area to find the area (mm2) in a suitable way.

g) 방청율은 이하의 수학식1에 의하여 산출한다.g) The rust prevention rate is calculated by the following equation (1).

Figure 112019091626918-pat00005
Figure 112019091626918-pat00005

여기에서,From here,

I : 방청율(%)I: Anti-corrosion rate (%)

ΣP0.2 : P0.2의 철근 6개의 합계 부식면적(mm2)ΣP0.2: Total corrosion area of 6 reinforcing bars of P0.2 (mm2)

ΣI0.2 : I0.2의 철근 6개의 합계 부식면적(mm2)ΣI0.2: Total corrosion area of 6 reinforcing bars of I0.2 (mm2)

하기 표 5에 콘크리트중의 철근부식 촉신시험에 따른 방청율 실험결과를 개시하고 있는 바, 본 발명의 조성물(B)은 KS F 2561에 따른 방청율 규정인 95% 이상을 만족하는 것으로 나타났으며, 본 발명의 조성물(B)은 유효성분 15%의 조성에도 기존 아질산 칼슘계 방청제의 범용화 된 사용량인 3.9kg/m3 보다 적은 사용량인 3.0kg/m3의 사용량으로도 95.1%의 방청율이 발현되는 것으로 나타났다. The results of the anti-corrosion test according to the reinforcing corrosion test in concrete in Table 5 are disclosed, and the composition (B) of the present invention was found to satisfy the anti-corrosion rate regulation of 95% or more according to KS F 2561. , The composition (B) of the present invention has a rust prevention rate of 95.1% even with a usage of 3.0kg/m 3 , which is less than the generalized usage of 3.9kg/m 3, which is a generalized usage of the existing calcium nitrite-based rust inhibitor even in the composition of 15% of the active ingredient. Appeared to be expressed.

이 실험을 통하여 본 발명의 조성물(B)의 낮은 사용량에 대한 성능안정성이 확인 되었으며, 필요에 따라 농축수준을 달리 적용하여 상용할 수 있는 장점이 확인 되었다.Through this experiment, the performance stability for the low amount of the composition (B) of the present invention was confirmed, and the advantage of being able to be used by applying different concentration levels was confirmed.

Figure 112019091626918-pat00006
Figure 112019091626918-pat00006

<콘크리트 경화 전 물성 및 경화 후 압축강도시험><Physical properties before concrete curing and compressive strength test after curing>

하기 표 6에서 보는 바와 같이 각 KS F 2561 : 철근 콘크리트용 방청제 규격에 따라 콘크리트를 제조하여 경화 전 물성 및 압축강도시험을 진행 하였다. 본 발명의 조성물(B)은 유효성분 15%의 것을 사용하였다.As shown in Table 6 below, each KS F 2561: concrete was prepared according to the anti-corrosive agent specification for reinforced concrete, and properties and compressive strength tests were conducted before curing. As the composition (B) of the present invention, an active ingredient of 15% was used.

Figure 112019091626918-pat00007
Figure 112019091626918-pat00007

콘크리트 배출 직 후의 물성 평가는 KS F 2402 : 콘크리트의 슬럼프 시험 규격에 따라 수행하였으며, 경화 후 압축강도 평가는 KS F 2405 : 콘크리트 압축강도 시험방법 규격에 따라 수행 하였다. Evaluation of the physical properties immediately after the discharge of concrete was performed according to the specification of KS F 2402: Concrete slump test, and evaluation of compressive strength after curing was performed according to the standard of KS F 2405: Concrete compression strength test method.

시험 재령 및 결과의 산출은 재령 7일 및 28일에 압축강도를 측정하여 기준 콘크리트의 압축강도에 대한 시험 콘크리트 압축강도의 백분율로 압축강도비를 산출하여 비교 및 정리하였다. The test age and results were calculated and compared by arranging the compressive strength ratio as a percentage of the test concrete compressive strength to the compressive strength of the reference concrete by measuring the compressive strength on the 7th and 28th day.

하기 표 7에 슬럼프 및 압축강도비 실험결과를 개시하고 있는 바, 본 발명의 조성물 즉 방청제 원료를 사용하지 않은 기준 콘크리트 보다 방청제 원료를 사용한 시험 콘크리트가 콘크리트 배출 직 후의 물성에 유리한 효과가 발현되는 것을 알 수 있다. 이는 본 발명의 조성물 중 에틸렌디아민테트라아세트산나트륨의 말단에 있는 Na+ 이온의 정전기적 반발력으로 콘크리트의 경화 전 물성을 개선시키는 작용에 따른 결과이다. The slump and compressive strength ratio test results are disclosed in Table 7 below, indicating that the composition of the present invention, that is, the test concrete using the rust-preventing material rather than the reference concrete without using the rust-preventing material, exhibits a favorable effect on physical properties immediately after the concrete is discharged. Able to know. This is a result of the action of improving the properties of the concrete before curing by the electrostatic repulsion of Na+ ions at the end of sodium ethylenediaminetetraacetic acid in the composition of the present invention.

또한, 본 발명의 조성물을 사용하지 않은 기준 콘크리트 보다 본 발명의 조성물을 사용한 시험 콘크리트가 압축강도 면에서 유리한 효과가 발현되는 것을 알 수 있다. 이는 방청제 원료 중 일부가 배합수에서 자유 알칼리 이온으로 존재하므로 시멘트 중 C3A 및 C2S 물질의 수화에 기여한 것으로 방청제 원료를 첨가하지 않은 경우보다 압축강도 면에서 유리한 효과가 발현되는 것으로 판단된다.In addition, it can be seen that the test concrete using the composition of the present invention exhibits an advantageous effect in terms of compressive strength than the reference concrete without using the composition of the present invention. This contributes to the hydration of C 3 A and C 2 S substances in cement because some of the rust preventive raw materials exist as free alkali ions in the blended water, and it is judged that a beneficial effect is expressed in terms of compressive strength than when no rust preventive raw materials are added. .

Figure 112019091626918-pat00008
Figure 112019091626918-pat00008

이상과 같이 본 발명은 비록 한정된 실시예와 도면에 의해 설명되었으나, 본 발명은 상기 실시예에 한정되지 않음은 물론이며, 본 발명이 속하는 분야에서 통상의 기술적 지식을 가진 자에 의해 상기 기재된 내용으로부터 다양한 수정 및 변형이 가능할 수 있음은 물론이다.As described above, although the present invention has been described with limited embodiments and drawings, the present invention is not limited to the above embodiments, and the contents described above by those skilled in the art to which the present invention pertains Of course, various modifications and variations may be possible.

Claims (4)

아미노화합물 100중량부에 대해 인산 30 내지 60중량부, 아질산염 5 내지 15중량부를 포함하되, 킬레이트성 방청피막을 형성함과 동시에 콘크리트의 경화전 작업성을 개선시키기 위해 에틸렌디아민테트라아세트산나트륨 30 내지 60중량부가 더 포함되는 것을 특징으로 하는 고성능 방청 혼화제 조성물.Containing 30 to 60 parts by weight of phosphoric acid and 5 to 15 parts by weight of nitrite relative to 100 parts by weight of the amino compound, 30 to 60 ethylenediaminetetraacetic acid sodium to form a chelating rust-preventive film and improve workability before curing of concrete High performance rust preventive admixture composition, characterized in that it further comprises parts by weight. 삭제delete 삭제delete 삭제delete
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