KR100649114B1 - A method for manufacturing high purity magnesium hydroxide having excellent dispersibility - Google Patents
A method for manufacturing high purity magnesium hydroxide having excellent dispersibility Download PDFInfo
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- KR100649114B1 KR100649114B1 KR1020050034035A KR20050034035A KR100649114B1 KR 100649114 B1 KR100649114 B1 KR 100649114B1 KR 1020050034035 A KR1020050034035 A KR 1020050034035A KR 20050034035 A KR20050034035 A KR 20050034035A KR 100649114 B1 KR100649114 B1 KR 100649114B1
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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
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/16—Magnesium hydroxide by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
Abstract
본 발명은 고무 및 플라스틱 등의 첨가제로 사용되는 수산화마그네슘의 제조방법에 관한 것이다.The present invention relates to a method for producing magnesium hydroxide used as an additive such as rubber and plastics.
본 발명은 해수로부터 제조된 마그네시아를 0.044mm 이하의 입경을 갖는 입자가 80% 이상이 되도록 분쇄하는 단계; 상기 분쇄된 마그네시아를 물에 수화하여 수산화마그네슘을 제조하는 단계; 상기 제조된 수산화마그네슘을 순도가 99% 이상이 되도록 산처리하는 단계; 및 상기 산처리된 수산화마그네슘을 세척한 다음 건조 및 분쇄하는 단계;를 포함하는 수산화마그네슘의 제조방법에 관한 것이다.The present invention comprises the steps of grinding the magnesia prepared from seawater so that the particles having a particle size of less than 0.044mm to 80% or more; Hydrating the pulverized magnesia in water to produce magnesium hydroxide; Acid-treating the prepared magnesium hydroxide to have a purity of 99% or more; And washing and drying and pulverizing the acid-treated magnesium hydroxide.
본 발명은 낮은 제조비용으로 분산성이 우수한 고순도 수산화마그네슘을 제공할 수 있다.The present invention can provide high purity magnesium hydroxide having excellent dispersibility at low manufacturing cost.
마그네시아, 수산화마그네슘, 고순도, 분산성, 수화, 산처리 Magnesia, Magnesium Hydroxide, High Purity, Dispersibility, Hydration, Acid Treatment
Description
본 발명은 고무 및 플라스틱 등의 첨가제로 사용되는 수산화마그네슘의 제조방법에 관한 것으로, 보다 상세하게는 제조비용이 저렴할 뿐만 아니라 고분산성 및 고순도를 갖는 수산화마그네슘의 제조방법에 관한 것이다.The present invention relates to a method for producing magnesium hydroxide used as an additive such as rubber and plastics, and more particularly, to a method for producing magnesium hydroxide having a low manufacturing cost and high dispersibility and high purity.
일반적으로 수산화마그네슘(Mg(OH)2)은 염기성 내화재료인 마그네시아(MgO)의 원료로 사용되며, 최근에는 고무 및 플라스틱 등에 첨가하여 고무 및 플라스틱 등이 잘 타지 않도록 하는 난연제로의 사용이 증대되고 있다. 상기와 같이 수산화마그네슘이 난연제로 사용되기 위해서는 고순도이어야 할 뿐만 아니라 원재료인 고무나 플라스틱 및 다른 첨가물들과의 분산성이 우수하여야 한다.In general, magnesium hydroxide (Mg (OH) 2 ) is used as a raw material of magnesia (MgO), a basic refractory material, and recently added to rubber and plastics to increase the use of flame retardants to prevent the burning of rubber and plastics well. have. As described above, in order for magnesium hydroxide to be used as a flame retardant, it must be not only high purity but also excellent in dispersibility with rubber, plastic and other additives as raw materials.
수산화마그네슘의 제조방법은 브루사이트나 천연산 마그네사이트를 이용하는 방법, 해수나 간수를 이용하는 방법, 그리고 염화마그네슘을 이용하는 방법 등이 있다. 상기 제조방법중 브루사이트나 천연산 마그네사이트를 이용하는 방법은 브루사이트를 정제하거나 천연산 마그네사이트를 소성 및 수화하여 제조하는 방법이다. 그러나, 이러한 제조방법에 따르면 고순도의 수산화마그네슘을 얻을 수 없는 문제점이 있다. 또한, 상기 제조방법중 해수나 간수를 이용하는 방법은 해수나 간수를 알칼리와 반응시켜 수산화마그네슘을 제조하게 된다. 그러나, 이러한 제조방법에 따르면 고순도의 수산화마그네슘을 얻는 것은 가능하나, 생성된 입자의 형상이 원형상으로 응집되어 분산이 어려운 문제점이 있다. 또한, 상기 제조방법중 염화마그네슘을 이용하는 방법은 염화마그네슘을 알칼리와 반응시켜 수산화마그네슘을 제조하게 된다. 그러나, 이러한 제조방법에 따르면 고순도 및 육각판상의 결정형태를 지닌 수산화마그네슘을 제조하는 것은 가능하나, 제조비용이 너무 상승하여 경제성이 떨어지는 문제점이 있다.Magnesium hydroxide may be prepared by using brucite or natural magnesite, using seawater or brine, and using magnesium chloride. Among the production methods, a method of using brucite or natural magnesite is a method of purifying brucite or calcining and hydrating the natural magnesite. However, according to this manufacturing method, there is a problem in that high purity magnesium hydroxide cannot be obtained. In addition, the method of using seawater or brine among the above production method is to produce magnesium hydroxide by reacting seawater or brine with alkali. However, according to such a manufacturing method, it is possible to obtain high purity magnesium hydroxide, but there is a problem in that the shape of the particles produced is aggregated in a circular shape, making it difficult to disperse. In addition, the method using magnesium chloride in the production method is to produce magnesium hydroxide by reacting magnesium chloride with alkali. However, according to such a manufacturing method, it is possible to produce magnesium hydroxide having a high purity and a hexagonal crystal form, but there is a problem in that the manufacturing cost is so high that economic efficiency is low.
수산화마그네슘을 제조하는 대표적인 종래기술로는 일본 공개특허공보 평5-238725호 및 2000-233924호가 있다. 상기 종래기술들중 일본 공개특허공보 평5-238725호는 B2O3 흡착수지를 이용하여 MgO 99.3% 이상의 고순도 수산화마그네슘을 제조하고 있으나, 이러한 수산화마그네슘은 해수에서 추출된 마그네슘 이온이 석회유와 반응하여 형성된 것으로서 응집성을 가지기 때문에 분산을 요하는 첨가제용으로는 이용이 불가능하다. 또한, 상기 종래기술들중 일본 공개특허공보 2000-233924호는 염화마그네슘과 알칼리 및 산화마그네슘의 수열처리 등에 의하여 수산화마그네슘을 제조하고 있어 고순도 및 고분산성의 수산화마그네슘의 제조가 가능하기는 하나, 제조비용이 너무 고가여서 경제성이 없는 문제점이 있다.Representative prior arts for producing magnesium hydroxide include Japanese Patent Application Laid-Open Nos. Hei 5-238725 and 2000-233924. Japanese Patent Application Laid-Open No. 5-238725 manufactures high-purity magnesium hydroxide of MgO 99.3% or more using B 2 O 3 adsorption resin, but such magnesium hydroxide reacts with magnesium oil extracted from seawater with lime oil. Because it is formed by cohesiveness and cannot be used for additives requiring dispersion. In addition, Japanese Unexamined Patent Publication No. 2000-233924 of the prior art manufactures magnesium hydroxide by hydrothermal treatment of magnesium chloride, alkali, and magnesium oxide, but it is possible to manufacture magnesium hydroxide of high purity and high dispersibility. There is a problem that the cost is too expensive and economical.
본 발명은 상기 종래기술들의 문제점을 해결하기 위한 것으로, 해수로부터 제조된 마그네시아를 원료로 이용함으로써 제조비용을 낮추고 해수로부터 제조된 마그네시아를 적절하게 처리함에 의하여 분산성을 향상시킨 고순도 수산화마그네슘의 제조방법을 제공하는데, 그 목적이 있다.The present invention is to solve the problems of the prior art, the manufacturing method of high purity magnesium hydroxide to improve the dispersibility by lowering the manufacturing cost by using magnesia prepared from seawater as a raw material and appropriately treating the magnesia prepared from seawater To provide, for that purpose.
상기 목적을 달성하기 위한 본 발명은, 해수로부터 제조된 마그네시아를 0.044mm 이하의 입경을 갖는 입자가 80% 이상이 되도록 분쇄하는 단계;The present invention for achieving the above object, the step of grinding the magnesia produced from seawater so that the particles having a particle diameter of 0.044mm or less to 80% or more;
상기 분쇄된 마그네시아를 물에 수화하여 수산화마그네슘을 제조하는 단계;Hydrating the pulverized magnesia in water to produce magnesium hydroxide;
상기 제조된 수산화마그네슘을 순도가 99% 이상이 되도록 산처리하는 단계; 및 Acid-treating the prepared magnesium hydroxide to have a purity of 99% or more; And
상기 산처리된 수산화마그네슘을 세척한 다음 건조 및 분쇄하는 단계;를 포함하는 분산성이 우수한 고순도 수산화마그네슘의 제조방법에 관한 것이다.It relates to a method for producing high purity magnesium hydroxide having excellent dispersibility, including; washing the acid-treated magnesium hydroxide, followed by drying and pulverizing.
이하, 본 발명을 상세하게 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에서는 해수로부터 제조된 마그네시아를 원료로 이용하게 되며, 해수로부터 제조된 마그네시아를 이용하지 않는 경우 수산화마그네슘의 순도 및 결정상등이 본 발명과 부합되지 않거나, 또는 제조비용이 고가로 되는 등의 문제점이 있다. 해수로부터 마그네시아를 제조하는 통상적인 방법은 탈탄산 처리된 해수를 석 회유와 반응시켜 수산화마그네슘을 제조하고, 이어 상기 수산화마그네슘을 세척, 건조, 소성함으로써 제조된다.In the present invention, the magnesia prepared from seawater is used as a raw material, and when the magnesia prepared from seawater is not used, the purity and crystal phase of magnesium hydroxide are not compatible with the present invention, or the manufacturing cost becomes expensive. There is this. Conventional methods for producing magnesia from seawater are prepared by reacting decarbonized seawater with lime oil to produce magnesium hydroxide, followed by washing, drying and calcining the magnesium hydroxide.
먼저, 본 발명에서는 상기와 같이 해수로부터 제조된 마그네시아를 0.044mm 이하의 입경을 갖는 입자가 80% 이상이 되도록 분쇄한다. 상기 입자크기보다 큰 입자를 사용하는 경우에는 이후의 수화처리시 생산성이 저하될 뿐만 아니라 우수한 분산성을 확보할 수 없게 된다.First, in the present invention, the magnesia prepared from the sea water as described above is pulverized so that the particles having a particle diameter of 0.044 mm or less are 80% or more. In the case of using particles larger than the particle size, not only productivity is lowered during the subsequent hydration treatment but also excellent dispersibility cannot be obtained.
이때, 상기 해수로부터 제조된 마그네시아로 해수로부터 마그네시아를 제조하는 공정중에 부산물로 발생되는 1mm 이하의 마그네시아 미분을 이용하면 보다 저렴하게 수산화마그네슘을 제조하는 것이 가능하므로 보다 바람직하다.At this time, the use of magnesia fine powder of 1 mm or less generated as a by-product during the process of producing magnesia from seawater with magnesia prepared from the seawater is more preferable because it is possible to produce magnesium hydroxide at a lower cost.
또한, 상기 해수로부터 제조된 마그네시아는 95~98중량%의 MgO를 함유하는 것을 이용하는 것이 바람직한데, 그 이유는 상기 MgO함량이 95중량% 미만이면 이후 산처리 및 수세하더라도 99중량% 이상의 MgO 함량을 얻기가 어렵고, 98중량%를 초과하면 제조비용이 상승하는 문제점이 있기 때문이다.In addition, the magnesia prepared from the seawater is preferably used containing 95 to 98% by weight of MgO, the reason is that if the MgO content is less than 95% by weight, even after acid treatment and washing with water content of 99% by weight or more It is because it is difficult to obtain, and if it exceeds 98% by weight, there is a problem that the manufacturing cost increases.
이어 상기 분쇄된 마그네시아를 물에 수화하여 수산화마그네슘을 제조하게 되며, 이후 상기 제조된 수산화마그네슘을 산처리한다.Subsequently, the pulverized magnesia is hydrated in water to prepare magnesium hydroxide, which is then acid-treated with the prepared magnesium hydroxide.
상기 산처리시 순도가 99% 이상이 되도록 산처리하는 것이 바람직하며, 순도가 99% 미만일 경우 나머지 성분들이 불순물로 작용하게 되어 최종제품의 열안정성을 현저하게 저하시키게 된다.The acid treatment is preferably an acid treatment so that the purity is more than 99%, if the purity is less than 99%, the remaining components act as an impurity to significantly lower the thermal stability of the final product.
이후, 상기 산처리된 수산화마그네슘을 통상의 방법을 이용하여 세척한 다음, 건조하고 분쇄하게 된다.Thereafter, the acid treated magnesium hydroxide is washed using a conventional method, and then dried and pulverized.
이때 상기 분쇄후 수산화마그네슘의 비표면적은 10㎡/g 이하로 제한하는 것이 바람직한데, 그 이유는 상기 비표면적이 10㎡/g을 초과하면 고무나 수지 등에 첨가될 경우 분산성이 불충분할 뿐만 아니라 기계적 강도가 저하되고 백화현상 등의 문제점이 발생될 수 있다.At this time, the specific surface area of magnesium hydroxide after pulverization is preferably limited to 10 m 2 / g or less. The reason is that when the specific surface area exceeds 10 m 2 / g, dispersibility is insufficient when added to rubber or resin. Mechanical strength may be lowered and problems such as bleaching may occur.
또한, 상기와 같이 제조된 수산화마그네슘의 결정상은 육각판상인 것이 바람직하며, 이는 결정상이 육각판상일 때 분산성 및 기타특성이 가장 우수하기 때문이다.In addition, the crystal phase of magnesium hydroxide prepared as described above is preferably in the hexagonal plate shape, because the dispersibility and other properties are the best when the crystal phase is a hexagonal plate shape.
이하, 실시예를 통하여 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[실시예]EXAMPLE
(발명예)(Invention example)
탈탄산 해수와 정제된 석회와의 반응에 의해 생성된 수산화마그네슘을 탈수, 건조, 소성하여 MgO함량 97.4중량%의 마그네시아 제조하였으며, 상기 공정중에 발생된 1mm 이하의 미분을 채취하여 이를 0.044mm 이하의 입경을 갖는 입자가 85%가 되도록 미분쇄하였다. 이후 상기 미분쇄된 마그네시아를 물에 수화하고, 99% 이상의 순도를 갖도록 마그네시아 1kg당 0.3M의 염산을 이용하여 산처리하였다. 이후, 통상의 방법으로 세척 및 건조한 수산화마그네슘에 대하여 MgO 순도, 결정상, 분산성 및 제조비용지수를 평가하였으며, 그 결과는 하기 표 1과 같다.Magnesium hydroxide produced by the reaction of decarbonated seawater with purified lime was dehydrated, dried and calcined to produce magnesia with 97.4% by weight of MgO. It was pulverized so that the particles having a particle diameter became 85%. Thereafter, the pulverized magnesia was hydrated in water and acid treated with 0.3 M hydrochloric acid per kg of magnesia to have a purity of 99% or more. Then, MgO purity, crystal phase, dispersibility and manufacturing cost index for the washed and dried magnesium hydroxide in a conventional manner, the results are shown in Table 1 below.
(비교예)(Comparative Example)
비교예1은 탈탄산 해수와 정제된 석회와의 반응에 의해 생성된 수산화마그네슘, 비교예2는 천연 마그네사이트를 소성한 마그네시아를 상기 발명예의 제조조건을 이용하여 처리한 수산화마그네슘, 비교예3은 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 이용하였다. 상기 비교예1, 비교예2 및 비교예3의 MgO 순도, 결정상, 분산성 및 제조비용지수를 평가하였으며, 그 결과는 하기 표 1과 같다.Comparative Example 1 is magnesium hydroxide produced by the reaction of decarbonated seawater with purified lime, Comparative Example 2 is magnesium hydroxide obtained by treating magnesia calcined with natural magnesite using the preparation conditions of the present invention, Comparative Example 3 is chloride Magnesium hydroxide produced by reacting magnesium with caustic soda was used. The MgO purity, crystal phase, dispersibility and manufacturing cost index of Comparative Example 1, Comparative Example 2 and Comparative Example 3 were evaluated, and the results are shown in Table 1 below.
상기 표 1에 나타난 바와 같이, 본 발명의 범위를 만족하는 발명예의 경우 99중량% 이상의 고순도이면서 분산성이 양호할 뿐만 아니라 제조비용도 상대적으로 저렴한 수산화마그네슘을 제조할 수 있었다.As shown in Table 1, in the case of the invention examples satisfying the scope of the present invention was not only high purity and good dispersibility of 99% by weight or more, it was possible to manufacture magnesium hydroxide with a relatively low manufacturing cost.
그러나, 탈탄산 해수와 정제된 석회와의 반응에 의해 생성된 수산화마그네슘을 직접 이용한 비교예1의 경우, 제조비용은 저렴하였으나, 순도가 낮았을 뿐만 아니라 분산성도 불량한 문제점이 있었다.However, in Comparative Example 1 using direct magnesium hydroxide produced by the reaction of decarbonated seawater with purified lime, the manufacturing cost was low, but there was a problem that the purity was low and the dispersibility was poor.
또한, 천연 마그네사이트를 소성하여 제조된 마그네시아를 본 발명의 방법을 이용하여 처리한 비교예2의 경우, 순도와 분산성이 매우 열악하였다.In addition, in Comparative Example 2 in which magnesia produced by calcining natural magnesite was treated using the method of the present invention, purity and dispersibility were very poor.
또한, 염화마그네슘과 가성소다를 반응시켜 생성된 수산화마그네슘을 이용한 비교예3의 경우, 순도, 분산성이 우수하기는 하였으나, 제조비용이 현저하게 높아 실생산에 적용되기 어려웠다.In addition, in the case of Comparative Example 3 using magnesium hydroxide produced by reacting magnesium chloride with caustic soda, although purity and dispersibility were excellent, manufacturing cost was remarkably high and it was difficult to apply to actual production.
상술한 바와 같이, 본 발명에 따르면 낮은 제조비용으로 분산성이 우수한 고순도 수산화마그네슘을 제공할 수 있으며, 이와 같이 제조된 수산화마그네슘은 고무 및 플라스틱 등에 난연제로 이용하는 것이 가능하다.As described above, according to the present invention, it is possible to provide high purity magnesium hydroxide having excellent dispersibility at a low manufacturing cost, and the magnesium hydroxide thus prepared can be used as a flame retardant in rubber and plastics.
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| EP0599085A1 (en) | 1992-10-29 | 1994-06-01 | Daicel Abosisangyo Co., Ltd. | Method for the production of active magnesium hydroxide |
| US5461101A (en) | 1992-04-23 | 1995-10-24 | Defped Limited | Particulate magnesium hydroxide |
| KR20020088786A (en) * | 2001-05-21 | 2002-11-29 | 주식회사 액티마그 | Manufacturing method for high concentration slurry of magnesium hydroxide |
| KR20030054393A (en) * | 2001-12-24 | 2003-07-02 | 주식회사 포스코 | Slurry comprising magnesium hydroxide produced from seawater with high concentration |
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| US5461101A (en) | 1992-04-23 | 1995-10-24 | Defped Limited | Particulate magnesium hydroxide |
| EP0599085A1 (en) | 1992-10-29 | 1994-06-01 | Daicel Abosisangyo Co., Ltd. | Method for the production of active magnesium hydroxide |
| KR20020088786A (en) * | 2001-05-21 | 2002-11-29 | 주식회사 액티마그 | Manufacturing method for high concentration slurry of magnesium hydroxide |
| KR20030054393A (en) * | 2001-12-24 | 2003-07-02 | 주식회사 포스코 | Slurry comprising magnesium hydroxide produced from seawater with high concentration |
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