KR20110055134A - Method for manufacturing subsidence calcium carbonate using drop method and subsidence calcium carbonate manufactured with this - Google Patents

Method for manufacturing subsidence calcium carbonate using drop method and subsidence calcium carbonate manufactured with this Download PDF

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KR20110055134A
KR20110055134A KR1020090112029A KR20090112029A KR20110055134A KR 20110055134 A KR20110055134 A KR 20110055134A KR 1020090112029 A KR1020090112029 A KR 1020090112029A KR 20090112029 A KR20090112029 A KR 20090112029A KR 20110055134 A KR20110055134 A KR 20110055134A
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calcium carbonate
mixture
precipitated calcium
drop
manufacturing
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KR1020090112029A
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Korean (ko)
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김형석
안지환
한기천
유광석
한춘
임미희
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한국지질자원연구원
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/38—Particle morphology extending in three dimensions cube-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

PURPOSE: A method for manufacturing precipitated calcium carbonate using a drop method and the precipitated calcium carbonate are provided to improve the uniformity of manufacturing processes by continuously supplying milk of lime. CONSTITUTION: Carbon dioxide is dissolved in distilled water to obtain a first mixture. The first mixture and milk of lime are prepared. The milk of lime is supplied to the first mixture by drops to obtain a second mixture. Carbon dioxide with constant flow rate is injected into the second mixture to induce carbonation reaction. Precipitated calcium carbonate is cleaned and filtered. The cleaned and filtered calcium carbonated is dried.

Description

드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘{METHOD FOR MANUFACTURING SUBSIDENCE CALCIUM CARBONATE USING DROP METHOD AND SUBSIDENCE CALCIUM CARBONATE MANUFACTURED WITH THIS}METHODS FOR MANUFACTURING SUBSIDENCE CALCIUM CARBONATE USING DROP METHOD AND SUBSIDENCE CALCIUM CARBONATE MANUFACTURED WITH THIS}

본 발명은 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘에 관한 것으로서, 보다 구체적으로는 회분식 반응이 아닌 석회유의 연속적 공급을 통해 균일한 형상의 침강성 탄산칼슘을 제조할 수 있는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘에 관한 것이다.The present invention relates to a method for preparing precipitated calcium carbonate and precipitated calcium carbonate produced by the same, and more specifically, to a drop method method for producing precipitated calcium carbonate having a uniform shape through continuous supply of lime oil rather than a batch reaction. It relates to a precipitated calcium carbonate production method utilized and a precipitated calcium carbonate produced thereby.

탄산칼슘 분말은 가격이 낮으면서도 고백색도, 불활성, 불연성 등의 우수한 특성을 가지고 있는 소재로서 고무, 플라스틱, 제지, 도료, 접착제 등의 무기 충진제로 널리 사용되고 있다. 현재 제지공업에서 많이 이용되고 있는 카올리나이트의 경우 미세한 육각판상으로서 종이 표면에 평행하게 배열하여 광택도, 평활도, 인쇄성이 뛰어난 데 비해 백색도가 떨어지는 단점이 있다. 그러나 침강성 탄산칼슘은 백색도가 카올리나이트보다 뛰어나고 제조방법에 따라 입자의 형상과 크기를 제어 할 수 있기 때문에 다양한 용도의 제지충진제로 사용되고 있다. Calcium carbonate powder is a material having a low price and excellent characteristics such as high whiteness, inertness, and incombustibility, and is widely used as an inorganic filler such as rubber, plastic, paper, paint, and adhesive. Kaolinite, which is widely used in the papermaking industry, is arranged in parallel with the surface of paper as a fine hexagonal plate and has a disadvantage in that whiteness is inferior to that of gloss, smoothness, and printability. However, precipitated calcium carbonate is used as a papermaking filler for various purposes because its whiteness is superior to kaolinite and the particle shape and size can be controlled according to the manufacturing method.

침강성 탄산칼슘을 합성하는 방법은 석회석을 출발물질로 하여 소성 및 수화공정을 거쳐 석회유를 만든 다음 탄산화시키는 방법에 따라 탄산가스 화합법, 석회-소다법, 소다법 등으로 구분된다.   The method of synthesizing precipitated calcium carbonate is divided into carbon dioxide gas mixing method, lime-soda method, and soda method according to the method of making lime oil through calcining and hydration process using limestone as starting material and then carbonizing.

탄산가스 화합법은 석회유에 석회석 소성시 발생된 탄산가스를 정화시킨 후 주입하여 탄산칼슘을 재합성하는 방법이다. 석회-소다법은 석회유나 수산화칼슘을 탄산소다와 반응시켜 탄산칼슘을 부산물로 제조하지만 주 제품은 가성소다이며, 합성된 침강성 탄산칼슘은 입도가 크고 안료특성이 떨어지는 등의 문제점이 있다. 또한 소다법은 가용성염을 이용한 방법으로 소다공업의 부산물을 이용하기 위해 미국에서 개발되었으며 염화칼슘과 탄산소다를 반응시켜 침강성 탄산칼슘을 얻을 수 있다. 이상과 같이 석회-소다법 및 소다법은 가용성염인 탄산소다 및 염화암모니움 등을 사용하기 때문에 합성된 탄산칼??의 회수에 충분한 세척을 하여야 하며, 입자의 크기 및 결정 입자의 형태조절이 용이하지 않아 최근에는 거의 사용되지 않고 있다. 이에 반하여 탄산가스 화합법은 석회석의 소성시 발생하는 탄산가스를 활용하고 합성시 원료가 탄산칼슘의 조성성분만으로 이루어져 있어서 공정이 비교적 단순하면서도 입자의 크기나 모양을 합성조건에 따라 조절이 가능하여 현재에는 거의 이 방법으로 침강성 탄산칼슘을 제조하고 있다.   Carbon dioxide gas compounding is a method of resynthesizing calcium carbonate by purifying and injecting carbon dioxide gas generated during limestone firing into lime oil. The lime-soda method produces calcium carbonate as a by-product by reacting lime oil or calcium hydroxide with sodium carbonate, but the main product is caustic soda, and the precipitated calcium carbonate synthesized has problems such as large particle size and poor pigment characteristics. In addition, the soda method was developed in the United States to utilize by-products of soda industry by using a soluble salt, and precipitated calcium carbonate can be obtained by reacting calcium chloride with sodium carbonate. As mentioned above, the lime-soda method and the soda method use soluble salts such as sodium carbonate and ammonium chloride, so they have to be sufficiently washed to recover the synthesized calcium carbonate. It is rarely used recently. On the contrary, the carbon dioxide gas compounding method utilizes carbon dioxide gas generated during calcining of limestone, and the raw material is composed only of calcium carbonate in synthesis. Precipitated calcium carbonate is produced by this method.

그러나 탄산가스 화합법의 경우 발열반응으로 반응속도를 아주 빠르게 유지시키지 않으면 통상 방추형의 침강성 탄산칼슘이 합성된다. 이와 같은 방법으로 고농도의 석회유에 저농도의 탄산가스를 접촉시키면 대부분 방추형의 침강성 탄산칼 슘이 합성된다.  However, in the case of carbon dioxide gas compounding method, fusiform precipitated calcium carbonate is usually synthesized unless the reaction rate is kept very fast by exothermic reaction. In this way, when a high concentration of lime oil is brought into contact with a low concentration of carbon dioxide, most of the fusiform precipitated calcium carbonate is synthesized.

국내 석회석의 경우 대부분이 회분식 반응기에 의해 방추형의 칼사이트가 생산되지만 입도 조절이 잘 이루어지지 않는 단점이 있기 때문에 이를 해결하기 위한 기술 개발이 요구된다.   Most domestic limestone is produced in the form of fusiform calcit by a batch reactor, but there is a disadvantage in that the particle size control is not made well, it is required to develop a technology to solve this problem.

본 발명은 상기한 종래 기술의 문제점을 해결하기 위해 안출된 것으로서, 회분식 반응기에 의한 침강성 탄산칼슘 제조 방법을 보완하여 드랍 메소드(Drop Method)를 이용하여 석회유의 연속공급을 통한 균일한 침강성탄산칼슘 제조를 가능하게 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘을 제공하는데 그 목적이 있다.The present invention has been made to solve the above-mentioned problems of the prior art, the production of uniform precipitated calcium carbonate through the continuous supply of lime oil using a drop method to complement the method of producing precipitated calcium carbonate by a batch reactor It is an object of the present invention to provide a method for preparing precipitated calcium carbonate using the drop method method for enabling the precipitated calcium carbonate prepared by the method.

상기 목적을 달성하기 위하여, 본 발명은, 증류수에 CO2를 용해시킨 제1 혼합물과 석회유를 마련하는 제1 단계와; 상기 제1 혼합물에 석회유를 방울단위로 일정속도로 공급함으로써 제2 혼합물을 제조하는 제2 단계와; 상기 제2 혼합물에 일정유량의 탄산가스를 주입하여 탄산화반응을 유도하는 제3 단계;로 이루어지는 것을 특징으로 한다.In order to achieve the above object, the present invention, the first step of preparing a first mixture and lime oil dissolved CO 2 in distilled water; A second step of preparing a second mixture by supplying lime oil to the first mixture at a constant speed in a drop unit; And a third step of inducing a carbonation reaction by injecting a predetermined amount of carbonic acid gas into the second mixture.

여기서 상기 제3 단계에서 침전된 탄산칼슘을 세척 및 여과하는 제4 단계와, 상기 제4 단계에서 세척 및 여과된 탄산칼슘을 건조시키는 제5 단계를 더 포함하는 것을 특징으로 한다.The method may further include a fourth step of washing and filtering the calcium carbonate precipitated in the third step, and a fifth step of drying the calcium carbonate washed and filtered in the fourth step.

또한 상기 제1 단계에서 석회유에 첨가되는 Ca(OH)2 양은 1~2wt%이고, 상기 제3 단계에서 탄산가스 주입률은 100~400mL/min이며, 상기 제2 단계에서 석회유 공급속도는 60~120 drops/min인 것을 특징으로 한다.In addition, the amount of Ca (OH) 2 added to the lime oil in the first step is 1 ~ 2wt%, the carbon dioxide gas injection rate in the third step is 100 ~ 400mL / min, the lime oil supply rate in the second step is 60 ~ And 120 drops / min.

상술된 바와 같이, 본 발명에 따른 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘은 비교적 제조하기 어려운 균일한 입도와 형상의 침강성 탄산칼슘을 회분식 반응기에 의한 종래의 침강성 탄산칼슘 제조방법이 아닌 드랍 메소드(Drop Method)를 이용하여 석회유의 연속공급을 통해 균일한 침강성 탄산칼슘을 제조할 수 있음에 따라 제지, 도료 등 미세하고 균일한 탄산칼슘 입자가 요구되는 산업 분야에 상당한 파급효과를 기대할 수 있다.As described above, the method of producing precipitated calcium carbonate using the drop method method according to the present invention and the precipitated calcium carbonate prepared by the present invention, the precipitated calcium carbonate having a uniform particle size and shape, which is relatively difficult to prepare, has been conventionally precipitated by a batch reactor. As it is possible to manufacture uniform precipitated calcium carbonate through continuous supply of lime oil using the drop method rather than the calcium carbonate manufacturing method, it is necessary for industrial fields that require fine and uniform calcium carbonate particles such as paper and paint. Significant ripple effects can be expected.

이하, 도면을 참조로 하여 본 발명에 따른 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법 및 이에 의해 제조된 침강성 탄산칼슘을 설명하기로 한다.Hereinafter, with reference to the drawings will be described a precipitated calcium carbonate manufacturing method using the drop method method and the precipitated calcium carbonate produced thereby.

본 발명에 따른 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법은 기본적으로 증류수에 CO2를 용해시킨 제1 혼합물과, 석회유를 마련하는 제1 단계와, 제1 혼합물에 석회유를 방울단위로 일정속도로 공급함으로써 제2 혼합물을 제조하는 제2 단계와, 제2 혼합물에 일정유량의 탄산가스를 주입하여 탄산화반응을 유도하는 제3 단계로 이루어지며, 산업적으로 활용하기 위해 제3 단계에서 침전된 탄산칼슘을 세척 및 여과하는 제4 단계와, 제4 단계에서 세척 및 여과된 탄산칼슘을 건조시키는 제5 단계를 더 포함한다.Precipitated calcium carbonate manufacturing method using the drop method method according to the present invention is basically a first step of dissolving CO 2 in distilled water, a first step of preparing lime oil, and a constant rate of lime oil in the first mixture in drops And a third step of preparing a second mixture by injecting a second mixture, and a third step of inducing a carbonation reaction by injecting a certain amount of carbon dioxide gas into the second mixture, and the carbonic acid precipitated in the third step for industrial use. A fourth step of washing and filtering the calcium, and a fifth step of drying the calcium carbonate washed and filtered in the fourth step.

여기서 제1 단계에서 석회유에 첨가되는 Ca(OH)2 양은 1~2wt%이고, 제3 단계에서 탄산가스 주입률은 100~400mL/min인 한편, 제2 단계에서 석회유 공급속도는 60~120 drops/min이다.Here, the amount of Ca (OH) 2 added to the lime oil in the first stage is 1 to 2 wt%, the carbon dioxide gas injection rate is 100 to 400 mL / min in the third stage, and the lime oil supply rate is 60 to 120 drops in the second stage. / min.

이하에서는 본 발명에 따른 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법을 실시예를 통해 살펴보기로 한다.Hereinafter, a method for preparing precipitated calcium carbonate using a drop method method according to the present invention will be described.

<실시예><Examples>

상기 제1 단계에서 첨가되는 Ca(OH)2는 순도 95%이고, 제3 단계에서의 탄산가스(CO2가스)는 순도가 99.9%인 것을 사용하였다. Ca (OH) 2 added in the first step was 95% purity, and the carbon dioxide gas (CO 2 gas) in the third step was used having a purity of 99.9%.

우선적으로 증류수 150ml에 CO2를 용해시킨 제1 혼합물과 석회유를 마련한 다음, 그 석회유를 용량 250ml이고 액체를 방울단위로 드랍할 수 있는 종래의 석회유 공급장치를 사용하여 그 제1 혼합물에 일정한 속도로 떨어뜨리면서 탄산화 반응을 유도하여 제2 혼합물을 제조하였으며, 이 과정에서 사용된 석회유에 첨가된 Ca(OH)2의 농도는 1∼2wt%로 하였다.First, prepare a first mixture and lime oil dissolved in CO 2 in 150ml of distilled water, and then use the conventional lime oil feeder capable of dropping the liquid 250ml and dropping the liquid dropwise, at a constant rate to the first mixture. A second mixture was prepared by inducing a carbonation reaction while dropping, and the concentration of Ca (OH) 2 added to the lime oil used in the process was 1 to 2 wt%.

그 후에 제2 혼합물에 탄산가스(CO2)를 100∼400ml/min의 속도로 주입하여 탄산화 반응을 유도하였으며, 제2 및 제3 단계에 걸쳐 드랍되는 석회유 공급속도는 60 및 120drops/min로 실험하였다.Thereafter, carbon dioxide (CO 2 ) was injected into the second mixture at a rate of 100 to 400 ml / min to induce a carbonation reaction, and the lime oil drop rates dropped through the second and third stages were tested at 60 and 120 drops / min. It was.

이렇게 제조된 침강성 탄산칼슘 분말을 세척 및 여과시킨 후에 60℃의 진공오븐(vacumn oven)에서 24시간 건조하였다.The precipitated calcium carbonate powder thus prepared was washed and filtered and then dried in a vacuum oven at 60 ° C. for 24 hours.

도 1a 내지 도 1d는 본 발명의 실시예에 따라 제조된 침강성 탄산칼슘을 나타낸 것으로, 25~40℃에서 Ca(OH)2가 2wt% 농도로 첨가된 석회유의 공급 속도를 60 drops/min으로 했을 때, 100∼400ml/min 범위 내에서 CO2 주입 속도 변화에 따라 생성된 침전물의 주사 현미경 사진이다.1A to 1D show precipitated calcium carbonate prepared according to an embodiment of the present invention, and the feed rate of lime oil added with Ca (OH) 2 at a concentration of 2wt% at 25 to 40 ° C. was 60 drops / min. When, the scanning micrograph of the precipitate produced according to the CO 2 injection rate change in the range of 100-400 ml / min.

생성된 탄산칼슘은 입자크기가 0.5∼1μm인 입방형을 나타내고 있으며, 탄산가스의 공급속도가 증가함에 따라 입자크기가 다소 감소하는 경향을 나타내었다.The resulting calcium carbonate exhibited a cubic shape with a particle size of 0.5 to 1 μm, and the particle size tended to decrease slightly as the supply rate of carbon dioxide gas increased.

석회유에 포함된 Ca(OH)2 농도, 석회유 공급속도 및 탄산가스 주입률을 이전에 기술된 바와 같은 범위 내에서 변경시킴에 따라 효율적으로 균일한 입도와 형상을 갖는 침강성 탄산칼슘의 제조가 가능하다는 것을 확인하였다.By varying the Ca (OH) 2 concentration, lime oil feed rate and carbon dioxide injection rate within the range as previously described, it is possible to efficiently produce precipitated calcium carbonate having a uniform particle size and shape. It was confirmed.

도 1은 본 발명에 따라 제조된 침강성 탄산칼슘을 나타낸 주사 현미경 사진.1 is a scanning micrograph showing precipitated calcium carbonate prepared according to the present invention.

Claims (6)

증류수에 CO2를 용해시킨 제1 혼합물과 석회유를 마련하는 제1 단계와;A first step of preparing a first mixture and lime oil in which CO 2 is dissolved in distilled water; 상기 제1 혼합물에 석회유를 방울단위로 일정속도로 공급함으로써 제2 혼합물을 제조하는 제2 단계와;A second step of preparing a second mixture by supplying lime oil to the first mixture at a constant speed in a drop unit; 상기 제2 혼합물에 일정유량의 탄산가스를 주입하여 탄산화반응을 유도하는 제3 단계;로 이루어지는 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법. A third step of inducing a carbonation reaction by injecting a predetermined amount of carbon dioxide gas into the second mixture; Method of producing precipitated calcium carbonate using a drop method method comprising the. 청구항 1에 있어서,The method according to claim 1, 상기 제3 단계에서 침전된 탄산칼슘을 세척 및 여과하는 제4 단계를 더 포함하는 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법. Method for producing precipitated calcium carbonate using a drop method method characterized in that it further comprises a fourth step of washing and filtering the calcium carbonate precipitated in the third step. 청구항 2에 있어서,The method according to claim 2, 상기 제4 단계에서 세척 및 여과된 탄산칼슘을 건조시키는 제5 단계가 더 포함하는 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법. And a fifth step of drying the washed and filtered calcium carbonate in the fourth step, the precipitated calcium carbonate manufacturing method using the drop method method. 청구항 1에 있어서,The method according to claim 1, 상기 제1 단계에서 석회유에 첨가되는 Ca(OH)2 양은 1~2wt%이고, 상기 제3 단 계에서 탄산가스 주입률은 100~400mL/min인 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법. The amount of Ca (OH) 2 added to the lime oil in the first step is 1 ~ 2wt%, and the carbon dioxide gas injection rate in the third step is 100 ~ 400mL / min precipitated carbonic acid using the drop method method Calcium manufacturing method. 청구항 1에 있어서,The method according to claim 1, 상기 제2 단계에서 석회유 공급속도는 60~120 drops/min인 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘 제조방법. In the second step, the lime oil supply rate is 60 ~ 120 drops / min precipitated calcium carbonate manufacturing method using a drop method method characterized in that. 청구항 1 내지 청구항 5 중 어느 한 항에 따라 제조되는 것을 특징으로 하는 드랍 메소드 방식을 활용한 침강성 탄산칼슘. Precipitated calcium carbonate using a drop method method, characterized in that prepared according to any one of claims 1 to 5.
KR1020090112029A 2009-11-19 2009-11-19 Method for manufacturing subsidence calcium carbonate using drop method and subsidence calcium carbonate manufactured with this KR20110055134A (en)

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CN104098928A (en) * 2014-03-17 2014-10-15 福建省万旗非金属材料有限公司 Preparation method and thixotropy test method of nano calcium carbonate with negative thixotropy

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104098928A (en) * 2014-03-17 2014-10-15 福建省万旗非金属材料有限公司 Preparation method and thixotropy test method of nano calcium carbonate with negative thixotropy
CN104098928B (en) * 2014-03-17 2016-08-17 福建省万旗非金属材料有限公司 The preparation method of a kind of nano-calcium carbonate with negative thixotroping and thixotropy method of testing thereof

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