KR100732536B1 - Process of producing non-alkaline accelerators admixtures for concrete complex - Google Patents
Process of producing non-alkaline accelerators admixtures for concrete complex Download PDFInfo
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- KR100732536B1 KR100732536B1 KR1020040067060A KR20040067060A KR100732536B1 KR 100732536 B1 KR100732536 B1 KR 100732536B1 KR 1020040067060 A KR1020040067060 A KR 1020040067060A KR 20040067060 A KR20040067060 A KR 20040067060A KR 100732536 B1 KR100732536 B1 KR 100732536B1
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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
- 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
- C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
- C04B22/142—Sulfates
- C04B22/148—Aluminium-sulfate
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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
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/06—Oxides, Hydroxides
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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
- C04B24/122—Hydroxy amines
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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Abstract
본 발명은 기존의 강알칼리성의 소디움실리게이트, 소디움알루미네이트 급결제 대체용으로 비알칼리성이며, 장기강도 발현성이 우수한 새로운 개념의 콘크리트 혼화용 비알칼리성 급결제 제조방법에 관한 것으로 수용성의 알루미늄 설페이트와 알루미늄 하이드록사이드를 주성분으로 하고, 최소한 하나이상의 아민류 및 안정제, 폼억제제 및 급결조제 그리고 pH 조절제등을 첨가한 환경친화성이 우수하고, 장기강도 발현특성이 개선된 비알칼리성 급결제에 관한 것이다. The present invention relates to a non-alkaline, non-alkaline fastener for producing a new concept of concrete admixture, which is non-alkaline, and has excellent long-term strength expression, as an alternative to the existing strong alkali sodium silicate and sodium aluminate quickener. The present invention relates to a non-alkaline quickener having aluminum hydroxide as a main component, and having excellent environmental friendliness with at least one or more amines and stabilizers, foam inhibitors and fastening aids, and pH adjusting agents.
Description
제1도는 본 발명의 콘크리트 혼화용 비알칼리성 급결제 제조방법의 공정도이다.1 is a process chart of the non-alkaline quickener manufacturing method for concrete admixture of the present invention.
제2도는 본 발명의 실시예와 비교예의 12시간 수화물의 XRD 패턴 그래프이다.2 is an XRD pattern graph of the 12-hour hydrate of Examples and Comparative Examples of the present invention.
제3도는 본 발명의 실시예와 비교예의 7시간 수화물의 XRD 패턴 그래프이다. 3 is an XRD pattern graph of a seven-hour hydrate of Examples and Comparative Examples of the present invention.
본 발명은 시멘트 급결제에 관한 것으로서, 기존의 강알칼리성의 소디움실리게이트, 소디움알루미네이트 급결제 대체용으로 비알칼리성이며, 장기강도 발현성이 우수한 새로운 개념의 급결제에 관한 것이다.The present invention relates to a cement fastener, and relates to a new concept fastener which is non-alkaline and has excellent long-term strength expression as a substitute for the existing strong alkali sodium silicate and sodium aluminate quickener.
현재 국내에서 일반적으로 사용되고 있는 급결제로는 크게 3가지로 분류된다. 첫째, 소디움실리케이트 및 포타시움실리케이트가 주성분인 무기염계 급결제이 다. 이는 액상타입으로 반응성 및 혼합성이 우수하나 장기적인 내구성이 취약하고, 또한 강알칼리성이기 때문에 주변토양오염 및 작업환경이 나쁘다는 치명적인 단점을 가지고 있다. 두번째로는 급경성 광물성급결제가 있는데, 주성분으로는 하소한 명반석으로 수산화칼슘과 반응하여 칼슘알루미네이트 수화물, 에트링가이트(ettringite)등을 생성시켜 시멘트를 급결시킨다. 그러나 이 급결제 자체로는 자경성이 없기 때문에 특성이 나쁘다는 단점이 있다. 마지막으로 시멘트계 급결제로써 칼슘알루미네이트 및 칼슘설포알루미네이트계가 있다. 이는 장기강도가 다른 두 종류보다 우수하다는 장점은 있으나, 리바운드율이 높고 또한 알칼리성이기 때문에 작업환경이 나쁘다는 단점이 있다.Currently, three types of quick payments are generally used in Korea. First, sodium silicate and potassium silicate are inorganic salt quickeners. It is a liquid type, which has excellent reactivity and mixing properties, but has a long-term durability, and strong alkalinity has a fatal disadvantage that the surrounding soil pollution and work environment is bad. Secondly, there is a rapid mineral starch settlement. The main component is calcined alum, which reacts with calcium hydroxide to form calcium aluminate hydrate, etringite, etc. to quench cement. However, this quick payment agent itself has a disadvantage in that its properties are bad because it is not hard. Finally, the cement-based fasteners include calcium aluminate and calcium sulfoaluminate. This has the advantage that the long-term strength is superior to the other two types, but the disadvantage is that the work environment is bad because of the high rebound rate and alkaline.
이와 같이 기존의 급결제는 강알칼리성이기 때문에 폐쇄공간에서 작업하는 작업자의 건강뿐만 아니라 주변 토양의 오염등에 심각한 악영향을 미친다. 그리고 리바운율이 20% 이상으로 시공성이 떨어져 경제적인 손실이 큰 단점이 있다. 특히 일반 콘크리트에 비해 숏크리트(shotcrete)용 콘크리트의 경우 초기강도 증진은 우수하나 장기강도 발현성이 나빠 내구성에 떨어진다는 문제점을 가지고 있다. 그러므로 기존의 급결제는 강알칼리성이고, 장기강도가 약하다는 단점 때문에 그 이용범위가 제한적이었다. As such, the existing fasteners are strongly alkaline, which seriously affects not only the health of the workers working in the closed space but also the pollution of the surrounding soil. In addition, the rebounce rate is more than 20%, the construction is poor, there is a big economic loss. In particular, in the case of shotcrete concrete, compared with general concrete, the initial strength is improved, but the long-term strength is poor, and the durability is poor. Therefore, the existing fasteners are strongly alkaline, and their use range is limited because of their weak long-term strength.
따라서 본 발명은 상기한 바와 같은 선행기술의 제반 문제점을 해소할 수 있는 급결제로서 상기 기존의 급결제의 단점을 보완할 수 있는 알칼리가 없고 장기강 도도 일반 콘크리트랑 대등하거나 그 이상의 강도를 갖는 새로운 재료를 개발함으로서 보수·보강, 절개면·사면정리등 각종 토목, 건축공사의 급결성이 요구되는 부분에 응용할 수 있는 비알칼리성 급결제를 제공하는 것을 그 목적으로 한다.Therefore, the present invention is a new fastener which can solve all the problems of the prior art as described above, which has no alkali, which can compensate for the shortcomings of the existing fastener, and has a strength equal to or greater than that of general concrete. By developing materials, it aims to provide non-alkaline quickeners that can be applied to various civil works such as repair, reinforcement, incision surface, slope trimming, and the like.
상기한 과제를 해결하기 위하여 본 발명자는 알루미늄 설페이트, 알루미늄 하이드록사이드, 디에탄올아민, 트리에탄올아민, 산 , 글리세롤 및 AE감수제를 본 발명의 바람직한 혼합비에 의해 혼합하면 알칼리가 없고, 초기급결 특성 및 장기강도의 발현이 우수하고, 리바운드율이 적을 뿐 아니라 주변토양의 오염등을 줄일 수 있는 친환경적인 시공에 적합한 콘크리트 혼화용 비알칼리성 급결제를 제공할 수 있다는 것을 알게 되어 본 발명을 완성하게 된 것이다.
In order to solve the above problems, the present inventors are free of alkalis by mixing aluminum sulfate, aluminum hydroxide, diethanolamine, triethanolamine, acid, glycerol and an AE reducing agent by a preferred mixing ratio of the present invention, and the initial quenching characteristics and long term The present invention has been completed by knowing that it is possible to provide a non-alkaline quickener for admixture of concrete, which is suitable for environmentally friendly construction, which is excellent in expression of strength, has low rebound rate, and reduces pollution of surrounding soil.
그러므로 본 발명에 의하면 콘크리트 혼화용 급결제의 제조방법에 있어서, (a)알루미늄 설페이트 35∼40중량%, 알루미늄 하이드록사이드 10∼15중량% 및 물 45∼55 중량%를 혼합한 후 교반하는 공정, (b)상기 혼합물 100 중량부에 대해 디에탄올아민 2.0∼5.0 중량부 및 트리에탄올아민 2.0∼5.0 중량부를 첨가하여 교반하는 공정, (c)상기 (b)공정의 혼합물에 유기산 1.0∼3.0중량부를 첨가하여 교반하는 공정, (d)상기 (c)공정의 혼합물에 글리세롤 2.0∼5.0 중량부를 첨가하여 교반하는 공정 및 (e)상기 (d)공정의 혼합물에 AE감수제 1.0∼2.0 중량부를 첨가하고 교반하는 공정을 포함하고 전 공정을 10∼40℃에서 행하는 것을 특징으로 하는 콘크리트 혼화용 비알칼리성 급결제의 제조방법이 제공된다.Therefore, according to the present invention, in the method for producing a concrete mixing fastener, (a) 35 to 40% by weight of aluminum sulfate, 10 to 15% by weight of aluminum hydroxide and 45 to 55% by weight of water, followed by stirring (b) adding 2.0 to 5.0 parts by weight of diethanolamine and 2.0 to 5.0 parts by weight of triethanolamine with respect to 100 parts by weight of the mixture, and stirring (c) 1.0 to 3.0 parts by weight of organic acid to the mixture of step (b). Adding and stirring, (d) adding 2.0 to 5.0 parts by weight of glycerol to the mixture of step (c) and stirring, and (e) adding 1.0 to 2.0 parts by weight of AE reducing agent to the mixture of step (d) and stirring The manufacturing method of the non-alkaline quickening agent for concrete admixtures including the process to carry out, and performing all processes at 10-40 degreeC is provided.
이하 도면을 참고하여 본 발명을 보다 상세히 설명하기로 한다.Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings.
본 발명의 급결제는 10∼40℃에서 알루미늄 설페이트 35∼40중량%, 알루미늄 하이드록사이드 10∼15중량% 및 물 45∼55 중량%를 혼합한 후 교반하는 공정, 상기 혼합물 100중량부에 대해 디에탄올아민 2.0∼5.0 중량부 및 트리에탄올아민 2.0∼5.0 중량부를 첨가하여 교반하는 공정, 유기산 1.0∼3.0 중량부를 첨가하여 교반하는 공정, 글리세롤 2.0∼5.0 중량부를 첨가하여 교반하는 공정 및 AE감수제 1.0∼2.0중량부를 첨가하고 교반하는 공정을 통해 제공될 수 있는데, 본 발명의 급결제는 후에 시멘트 조성물(페이스트, 몰탈, 콘크리트 등)에 대해 혼합될 때 응결 및 경화 작용을 위해 3∼15중량% 첨가되어 사용될 수 있다.The fastener of the present invention is a step of mixing 35-40% by weight of aluminum sulfate, 10-15% by weight of aluminum hydroxide, and 45-55% by weight of water at 10 to 40 ° C, followed by stirring, with respect to 100 parts by weight of the mixture. Adding 2.0 to 5.0 parts by weight of diethanolamine and 2.0 to 5.0 parts by weight of triethanolamine and stirring, adding and stirring 1.0 to 3.0 parts by weight of organic acid, stirring to add 2.0 to 5.0 parts by weight of glycerol and 1.0 to AE water reducing agent. It can be provided through a process of adding and stirring 2.0 parts by weight, the fastener of the present invention is added to 3 to 15% by weight for the condensation and curing action when mixed with the cement composition (paste, mortar, concrete, etc.) Can be used.
본 발명에서 급결제의 혼합은 10∼40℃에서 시행되며 먼저 물 45∼55 중량%에 알루미늄 설페이트 35∼40중량%, 알루미늄 하이드록사이드 10∼15중량%를 첨가한 후 미세한 알갱이가 보이지 않을 때까지 교반한다. 대략 6시간 이후 더 이상의 침전물이 발견되지 않을 때 상기 혼합물 100중량부에 대해 디에탄올아민 2.0∼5.0 중량부, 트리에탄올아민 2.0∼5.0 중량부를 첨가하는데 이때 미세한 부유물들이 사라지게 된다. 그 후로 유기산 1.0∼3.0 중량부, 글리세롤 2.0∼5.0 중량부 및 AE감수제 1.0∼2.0 중량부의 순서로 첨가하여 교반하는 공정을 각각 행하여 급결제를 제조한다. In the present invention, the mixing of the fastener is performed at 10 to 40 ° C., and when fine particles are not seen after first adding 35 to 40 wt% of aluminum sulfate and 10 to 15 wt% of aluminum hydroxide to 45 to 55 wt% of water. Stir until. When no more precipitate is found after about 6 hours, 2.0 to 5.0 parts by weight of diethanolamine and 2.0 to 5.0 parts by weight of triethanolamine are added to 100 parts by weight of the mixture, whereby fine suspensions disappear. Thereafter, 1.0 to 3.0 parts by weight of an organic acid, 2.0 to 5.0 parts by weight of glycerol, and 1.0 to 2.0 parts by weight of an AE reducing agent are added and stirred, respectively, to prepare a fastener.
본 발명에서 알루미늄 설페이트 35∼40중량%, 알루미늄 하이드록사이드 10∼15중량%를 물에 용해하는 이유는 강도증진 및 초기급결의 작용을 부여하기 위함이다.In the present invention, the reason for dissolving 35 to 40% by weight of aluminum sulfate and 10 to 15% by weight of aluminum hydroxide in water is to give the action of increasing strength and initial quenching.
상기 혼합성분 중 디에탄올아민, 트리에탄올아민 및 유기산을 상기 범위 미만을 첨가하는 경우에는 응결 및 경화 시간이 증가하는 경우가 있고, 상기 범위를 초과하는 경우에는 장기 강도에도 악영향을 끼치게 된다. 상기 유기산은 아크릴산, 말레산 및 구연산으로 이루어진 군으로부터 선택되는 어느 하나인 것을 사용할 수 있다.When the diethanolamine, triethanolamine and organic acid in the above mixed components are added below the above ranges, the condensation and curing time may increase, and when the above ranges are exceeded, the long-term strength is adversely affected. The organic acid may be any one selected from the group consisting of acrylic acid, maleic acid and citric acid.
글리세롤 2.0∼5.0중량부 및 AE감수제 1.0∼2.0 중량부를 첨가하는 이유는 응결시간단축 및 작업성 개선의 작용을 부여하기 위함이다. 본 발명에서는 상기와 같은 순서로 배합을 하지 않으면 각각의 구성물질이 완전히 용해하지를 않고 침전물이 발생하게 되므로 상기 순서를 따르는 것이 바람직하다.The reason for adding 2.0 to 5.0 parts by weight of glycerol and 1.0 to 2.0 parts by weight of AE reducing agent is to impart the action of shortening the setting time and improving workability. In the present invention, if the compound is not mixed in the above-described order, it is preferable to follow the above-described order because each component is not completely dissolved and precipitates are generated.
또한, 본 발명에서는 상기 콘크리트 혼화용 비알칼리성 급결제 100중량부에 대해 Li2CO3, Li2SO4 또는 그 혼합물을 0.5∼10 중량부 더 첨가하여 교반하는데, 이는 급결제의 미세한 응결시간 및 pH를 조절하여 급결효과의 증대 및 작업의 안정성의 효과를 부여하기 위함이다.In addition, in the present invention, 0.5 to 10 parts by weight of Li 2 CO 3, Li 2 SO 4 or a mixture thereof is further added to 100 parts by weight of the non-alkaline fastener for concrete mixing, which is a fine setting time and This is to adjust the pH to increase the quickening effect and to give the effect of stability of work.
본 발명에서는 상기 콘크리트 혼화용 비알칼리성 급결제 100중량부에 대해 시멘트 0.5∼15중량부를 더 첨가할 수도 있으며, 메타카올린 분말을 0.5∼15중량부를 더 첨가하여 장기강도 증진, 점성증가로 인한 리바운드율 감소를 도모할 수도 있다.In the present invention, 0.5 to 15 parts by weight of cement may be further added to 100 parts by weight of the non-alkaline quickener for concrete mixing, and 0.5 to 15 parts by weight of metakaolin powder is added to increase the long-term strength and increase the rebound due to viscosity. It can also reduce.
이상 설명한 바와 같은 본 발명의 콘크리트 혼화용 비알칼리성 급결제의 제조방법은 후술하는 실시예로부터 보다 명백하게 될 것이다. 단, 본 발명이 하기 실시예로 제한되지는 않는다. The manufacturing method of the non-alkaline quickener for concrete admixture of this invention as demonstrated above will become clear from the Example mentioned later. However, the present invention is not limited to the following examples.
[실시예 1]Example 1
알루미늄 설페이트 35중량%, 알루미늄 하이드록사이드 10중량% 및 물 55중량%를 혼합한 후 교반하고, 상기 혼합물 100중량부에 대해 디에탄올아민 3.0중량부 및 트리에탄올아민 2.0중량부를 첨가하여 교반한 후, 유기산 1.0중량부를 첨가하여 교반하고, 글리세롤 5.0중량부를 첨가하여 교반하고, AE감수제 2.0 중량부를 첨가하고 교반하여 콘크리트 혼화용 비알칼리성 급결제를 제조하였다, 상기 전 공정은 35℃에서 행하였다. 상기 급결제를 1종 포틀랜드 시멘트의 몰탈에 중량비로 5% 혼합하여 수화물을 제조하였다. After mixing 35% by weight of aluminum sulfate, 10% by weight of aluminum hydroxide and 55% by weight of water, the mixture was stirred, and 3.0 parts by weight of diethanolamine and 2.0 parts by weight of triethanolamine were added to 100 parts by weight of the mixture, followed by stirring. 1.0 weight part of organic acid was added, it stirred, 5.0 weight part of glycerol was added, it stirred, 2.0 weight part of AE reducing agents were added, and it stirred, and the non-alkaline quickening agent for concrete mixing was prepared, and the said whole process was performed at 35 degreeC. The fastener was mixed with 5% by weight of mortar of one Portland cement to prepare a hydrate.
[실시예 2]Example 2
상기 실시예 1의 급결제 100중량부에 대해 Li2CO3를 3 중량부 첨가하고 상기 급결제를 1종 포틀랜드 시멘트의 몰탈에 중량비로 5% 혼합하여 수화물을 제조하였다A hydrate was prepared by adding 3 parts by weight of Li 2 CO 3 to 100 parts by weight of the fastener of Example 1 and mixing the fastener with 5% by weight of mortar of one Portland cement.
[비교예 1]Comparative Example 1
1종 포틀랜드 시멘트, 물 및 골재를 혼합하여 몰탈을 제조하였다. 상기 실시예와 비교예의 길모어침에 의한 페이스트 응결시간 및 몰탈 압축강도를 비교하여 아래 표1 및 표2에 나타내었다. 급결제를 첨가하였을 경우 응결 시간이 단축되고 각 재령의 강도 값이 증가함을 알 수 있었다. 도 2∼3에 의해 급결제가 첨가된 경우의 수화물을 비교하면 급결제 첨가시 에트링가이트(ettringite)의 생성이 빨라져 초기 수화가 빨라져 초기 강도가 높아지고 재령7일에선 Ca(OH)2생성이 많아져 중·장기 강도 발현에 진입했음을 알 수 있었다.Mortar was prepared by mixing one Portland cement, water and aggregate. Paste condensation time and mortar compressive strength of the examples and the comparative examples by Gil Gam are shown in Table 1 and Table 2 below. It was found that the addition of the rapid binder shortened the setting time and increased the strength value of each age. Comparing the hydrates when the fastener is added according to FIGS. 2 to 3, the formation of ettringite is faster when the fastener is added, the initial hydration is faster, and the initial strength is higher, and Ca (OH) 2 production is observed on day 7 It was found that they entered the mid- and long-term intensity.
상기 실시예 2와 비교예의 응결시간변화를 pH 값으로 표 3에 나타내었다. Li2CO3를 첨가하지 않은 것에 비교해서 응결시간 단축이 이루어졌으며 또한 pH가 증가를 하였다. pH값은 알루미늄 설페이트 및 알루미늄 하이드록사이드의 비율 및 Li염의 첨가량에 따라 조절할 수 있다.The change in the setting time of Example 2 and Comparative Example is shown in Table 3 as the pH value. Compared with no addition of Li 2 CO 3 , the setting time was shortened and the pH was increased. pH value can be adjusted with the ratio of aluminum sulfate and aluminum hydroxide, and the addition amount of Li salt.
이상 설명한 바와 같이 본 발명에 의하면 기존의 알루미네이트계 및 실리케 이트계 급결제에 비해 장기 강도저하가 없고 낮은 pH를 나타내어 콘크리트시공 및 시멘트계 혼합물에 첨가 될 때 높은 장기 강도와 내구성, 친환경적 사용, 적은 인체유해성 등의 좋은 특성을 나타낼 수 있다. 또한 시멘트에 메타카올린을 첨가함으로서 응결시간 단축과 장기강도의 증진을 이룰 수 있는 장점을 가진다.As described above, according to the present invention, there is no long-term strength deterioration and low pH compared to conventional aluminate- and silicate-based fasteners. It can exhibit good properties such as human harm. In addition, by adding metakaolin to the cement has the advantage that it can shorten the setting time and increase the long-term strength.
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