KR101062476B1 - Magnesium-based hydrogen generating powder and preparation method thereof - Google Patents
Magnesium-based hydrogen generating powder and preparation method thereof Download PDFInfo
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Abstract
본 발명은 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)로 이루어진 마그네슘계 수소발생용 분말 및 이의 제조방법에 관한 것이다.The present invention relates to a magnesium-based hydrogen generating powder consisting of magnesium hydride powder (MgH 2 ) and magnesium oxide powder (MgO) and a method for producing the same.
본 발명에 의한 마그네슘계 수소발생용 분말은, 마그네슘수소화물분말(MgH2) 90 내지 95중량%와, 마그네슘산화물분말(MgO) 5 내지 10중량%를 포함하여 구성됨을 특징으로 한다. 또한 본 발명에 의한 마그네슘계 수소발생용 분말의 제조방법은, 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 준비하는 분말준비단계(S100)와, 상기 마그네슘수소화물분말(MgH2) 90 내지 95중량%와 상기 마그네슘산화물분말(MgO) 5 내지 10중량%를 혼합하는 분말혼합단계(S200)로 이루어진다. 이와 같은 본 발명에 의하면, 저렴한 제조 비용으로 보다 많은 수소를 발생시킬 수 있으며, 수소 발생시 부산물로서 마그네슘이 주성분인 마그네슘산화물이나 마그네슘수화물을 얻을 수 있는 이점이 있다. Magnesium-based hydrogen generating powder according to the present invention is characterized in that it comprises 90 to 95% by weight of magnesium hydride powder (MgH 2 ), and 5 to 10% by weight of magnesium oxide powder (MgO). In addition, the method for producing a magnesium-based hydrogen generating powder according to the present invention, a powder preparation step (S100) for preparing a magnesium hydride powder (MgH 2 ) and magnesium oxide powder (MgO), and the magnesium hydride powder (MgH 2 A powder mixing step (S200) of mixing 90 to 95% by weight and 5 to 10% by weight of the magnesium oxide powder (MgO). According to the present invention, it is possible to generate more hydrogen at a low production cost, there is an advantage that can obtain a magnesium oxide or magnesium hydrate of magnesium as a main component by-product when hydrogen is generated.
수소발생용 분말, 마그네슘, 마그네슘산화물분말, 마그네슘수소화물분말 Hydrogen generating powder, magnesium, magnesium oxide powder, magnesium hydride powder
Description
도 1 은 본 발명에 의한 마그네슘계 수소발생용분말의 제조방법을 나타낸 공정 순서도.1 is a process flow chart showing a method for producing magnesium-based hydrogen generating powder according to the present invention.
도 2 는 본 발명에 의한 마그네슘계 수소발생용분말의 실시예와 비교예에서 물과 반응시간이 증가함에 따른 기체(수소)방출량 및 반응생성부산물 종류를 나타낸 표.Figure 2 is a table showing the gas (hydrogen) emission amount and the reaction product by-product type with increasing reaction time with water in the Examples and Comparative Examples of magnesium-based hydrogen generation powder according to the present invention.
도 3 은 본 발명에 의한 마그네슘계 수소발생용분말의 실시예와 비교예에서 분당 방출된 기체무게를 환산하여 비교한 표.Figure 3 is a table comparing the gas weight released per minute in the Example and Comparative Example of the magnesium-based hydrogen generation powder according to the present invention.
* 도면의 주요 부분에 대한 부호의 설명 *Explanation of symbols on the main parts of the drawings
S100. 분말준비단계 S200. 분말혼합단계S100. Powder preparation step S200. Powder Mixing Step
본 발명은 마그네슘계 수소발생용 분말 및 이의 제조방법에 관한 것으로, 보다 상세하게는, 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 포함하여 구성되어 저렴한 제조 비용으로 보다 많은 수소를 발생시킬 수 있으며, 수소 발생시 부산물로서 마그네슘을 얻을 수 있도록 한 마그네슘계 수소발생용 분말 및 이의 제조방법에 관한 것이다.The present invention relates to a magnesium-based hydrogen-generating powder and a method for producing the same, and more specifically, it comprises a magnesium hydride powder (MgH 2 ) and magnesium oxide powder (MgO) to produce more hydrogen at a lower manufacturing cost It can be generated, and relates to a magnesium-based hydrogen-generating powder and a method for producing the same to obtain magnesium as a by-product when hydrogen is generated.
수소의 저장 방법으로는 압축기체저장법, 액체수소저장법 및 수소저장합금을 이용한 저장법 등이 있다. Hydrogen storage methods include a compressed gas storage method, a liquid hydrogen storage method, and a storage method using a hydrogen storage alloy.
압축기체저장법은 상대적으로 체적당 저장밀도가 낮고 고압의 가스용기를 사용하여야 하는 위험이 있으며, 액체수소저장법의 경우 체적당 저장밀도는 압축기체저장법보다 크지만 수소의 액화점인 영하 235℃ 이하로 유지해야 하기 때문에 특수 단열 시스템이 요구되고 장시간의 저장에 부적합하다. Compressor storage method has a relatively low storage density per volume and there is a risk of using a high pressure gas container.In the case of liquid hydrogen storage method, the storage density per volume is larger than the compressor storage method, but is below the liquefaction point of hydrogen below minus 235 ℃. Special insulation systems are required because of the need to maintain and are unsuitable for long term storage.
이에 비해 수소저장합금을 이용하는 저장법은 체적당 저장밀도가 크고 장시간 저장이 용이하며 고압 저장이 필요하지 않아 안전한 저장법이라는 장점들을 가지고 있다. 수소저장합금은 FeTi, LaNi, V-Ti-Cr계, 마그네슘계 등이 있으나 이론적 수소저장용량이 마그네슘계가 제일 높고 가볍고 원료가 풍부한 장점이 있다. On the other hand, the storage method using the hydrogen storage alloy has the advantages of high storage density per volume, easy storage for a long time, and high pressure storage, which is a safe storage method. Hydrogen storage alloys include FeTi, LaNi, V-Ti-Cr, magnesium, etc., but the theoretical hydrogen storage capacity is the highest magnesium-based, light and rich raw materials.
일반적으로 이러한 수소저장합금은 수소분위기에서 가압하여 수소를 저장하고 방출시는 수소 압력이 낮은 상태에서 방출하여 수소를 원료로 하는 연료전지에 공급하게 된다. Generally, such hydrogen storage alloys are pressurized in a hydrogen atmosphere to store hydrogen, and when released, the hydrogen storage alloy is released at a low hydrogen pressure to be supplied to a fuel cell using hydrogen as a raw material.
한편, 수소발생방법으로서 알루미늄이나 알루미늄 합금, 마그네슘이나 마그네슘합금 등을 이용하여 물과 반응하여 수소를 발생시키는 연구가 진행되어 왔다.On the other hand, as a method of generating hydrogen, research has been conducted to generate hydrogen by reacting with water using aluminum, an aluminum alloy, magnesium, magnesium alloy, or the like.
그러나, 알루미늄은 물과 반응하여 수소를 발생시키기 위해서는 산을 첨가해야 하며, 수소 발생량이 많지 않은 문제점이 있다.However, aluminum has to add an acid in order to react with water to generate hydrogen, and there is a problem that the amount of hydrogen is not generated.
그리고 대한민국특허청 공개특허 제10-2007-0032955호에는 알루미늄, 마그네슘 및 그들의 합금으로 이루어지는 군으로부터 선택되는 1이상의 금속재료를 포함하고, 이러한 금속재료는 60㎛ 이하의 입경을 가지는 입자가 80 중량% 이상의 비율로 포함되어 있으서, 물과 반응시에 수소를 발생시킬 수 있도록 한 "수소발생재료"가 게시되어 있다. And Korean Patent Application Laid-Open No. 10-2007-0032955 includes at least one metal material selected from the group consisting of aluminum, magnesium, and alloys thereof, wherein the metal material contains 80 wt% or more of particles having a particle diameter of 60 μm or less. The "hydrogen generating material" which is contained in the ratio and made it possible to generate | occur | produce hydrogen in reaction with water is published.
마그네슘이나 마그네슘합금 등을 이용하여 물과 반응하여 반응식 Mg + 2H2O Mg(OH)2 + 2H2 의하여 수소(H2)가 발생시키는 경우 반응이 느리고 수소의 발생량이 적은 문제점이 있다.Reaction with water using magnesium or magnesium alloy Mg + 2H 2 O Mg (OH) 2 + 2H 2 When the hydrogen (H 2 ) is generated by the reaction is slow and there is a problem that the amount of hydrogen is generated.
최근에는, 마그네슘 수소화물(MgH2)을 물과 반응하여 MgH2+ 2H2O -> Mg(OH)2 + 2H2 의 반응식에 의하여 수소(H2)를 발생시키는 방법이 개발되어 있다.Recently, a method for generating hydrogen (H 2 ) by reacting magnesium hydride (MgH 2 ) with water has been developed by a reaction formula of MgH 2 + 2H 2 O-> Mg (OH) 2 + 2H 2 .
그러나, 이러한 마그네슘수소화물(MgH2)의 물과 반응을 촉진하기 위하여 니켈이나 마그네슘 염화물을 첨가해야만 한다.However, nickel or magnesium chloride must be added to promote the reaction of the magnesium hydride (MgH 2 ) with water.
또한 마그네슘수소화물(MgH2)에 마그네슘(Mg) 이외의 성분을 가진 니켈(Ni) 등을 첨가하여 물과 반응시킴으로써 수소를 발생하는 방법은, 반응 후 마그네슘(Mg) 이외에 니켈(Ni)을 포함하는 금속성분이나 금속산화물 즉 부산물을 남기게 된다.In addition, a method of generating hydrogen by adding nickel (Ni) having a component other than magnesium (Mg) to magnesium hydride (MgH 2 ) and reacting with water includes nickel (Ni) in addition to magnesium (Mg) after the reaction. To leave metal components or metal oxides or by-products.
이러한 부산물은 매립하게 되더라도 독성을 나타내어 환경오염을 야기할 수 있으며, 내화물 원료나 절연재료용 분말로 재활용하는데에도 용이하지 않은 문제점 이 있다.These by-products, even when buried, may be toxic and cause environmental pollution, and there is a problem that is not easy to recycle into powder for refractory raw materials or insulating materials.
뿐만 아니라, 마그네슘 이외의 금속산화물이나 금속성분 등의 부산물이 섞여 있는 경우 이러한 부산물로부터 순수한 마그네슘 산화물로 분리하는데 어려움이 있다. In addition, when by-products such as metal oxides or metal components other than magnesium are mixed, it is difficult to separate them from pure by-products.
한편, 마그네슘수소화물(MgH2)에 금속염화물 등을 첨가하여 반응시킴으로써 수소를 발생시키는 방법에서는, 염소이온에 의해 반응용기 및 반응기체 유로관을 부식시켜 환경적 관점에서 바람직하지 못하다.On the other hand, in the method of generating hydrogen by adding and reacting metal hydride or the like with magnesium hydride (MgH 2 ), it is not preferable from an environmental point of view by corroding the reaction vessel and the reactor flow channel with chlorine ions.
이 외에 물과 마그네슘수소화물(MgH2)을 반응시에 물에 산을 첨가하여 마그네슘수소화물과 물이 보다 용이하게 반응할 수 있도록 하는 방법도 제시되어 있다.In addition, a method of making the magnesium hydride and water react more easily by adding an acid to the water at the time of reacting the water with magnesium hydride (MgH 2 ).
그러나, 이러한 기술은 반응속도는 높일 수 있으나 인체에 유독하고 반응용기 및 유로관 등을 부식시키게 되는 문제점이 있다.However, such a technique can increase the reaction speed, but there is a problem in that it is toxic to the human body and corrodes the reaction vessel and the flow passage.
본 발명의 목적은 상기한 문제점을 해결하기 위하여 안출된 것으로, 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 소정의 중량 비율로 혼합하는 과정만으로 제조 완료함으로써 제조 비용을 절감할 수 있고, 물과 반응시에 보다 많은 수소를 발생시킬 수 있도록 한 마그네슘계 수소발생용 분말의 제조방법을 제공하는 것에 있다.An object of the present invention is to solve the above problems, it is possible to reduce the manufacturing cost by completing the manufacturing process only by mixing a magnesium hydride powder (MgH 2 ) and magnesium oxide powder (MgO) in a predetermined weight ratio. In addition, the present invention provides a method for producing a magnesium-based hydrogen-generating powder capable of generating more hydrogen upon reaction with water.
본 발명의 다른 목적은, 물과 반응하여 수소 발생시 부산물로서 마그네슘산화물(MgO)이나 마그네슘수화물(Mg(OH2))을 얻을 수 있도록 한 마그네슘계 수소발생 용 분말을 제공하는 것에 있다.Another object of the present invention is to provide a magnesium-based hydrogen-generating powder which can react with water to obtain magnesium oxide (MgO) or magnesium hydrate (Mg (OH 2 )) as a by-product when hydrogen is generated.
상기한 목적을 달성하기 위한 마그네슘계 수소발생용 분말은, 마그네슘수소화물분말(MgH2) 90 내지 95중량%와, 마그네슘산화물분말(MgO) 5 내지 10중량%를 포함하여 구성됨을 특징으로 한다.Magnesium-based hydrogen generation powder for achieving the above object is characterized in that it comprises 90 to 95% by weight magnesium hydride powder (MgH 2 ), and 5 to 10% by weight of magnesium oxide powder (MgO).
상기 마그네슘계 수소발생용 분말은, 물과 반응시에 마그네슘산화물(MgO)과 마그네슘수화물(Mg(OH2)) 중 하나 이상의 부산물과 수소(H2)를 생성하는 것을 특징으로 한다.The magnesium-based hydrogen generating powder is characterized in that when reacting with water to produce at least one by-product and hydrogen (H 2 ) of magnesium oxide (MgO) and magnesium hydrate (Mg (OH 2 )).
본 발명에 의한 마그네슘계 수소발생용 분말의 제조방법은, 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 준비하는 분말준비단계와, 상기 마그네슘수소화물분말(MgH2) 90 내지 95중량%와 상기 마그네슘산화물분말(MgO) 5 내지 10중량%를 혼합하는 분말혼합단계로 이루어지는 것을 특징으로 한다.The method for preparing magnesium-based hydrogen generating powder according to the present invention includes preparing a powder for preparing magnesium hydride powder (MgH 2 ) and magnesium oxide powder (MgO), and the magnesium hydride powder (MgH 2 ) 90 to 95 It is characterized by consisting of a powder mixing step of mixing 5% by weight to 10% by weight of the magnesium oxide powder (MgO).
상기 분말혼합단계는, 상기 마그네슘수소화물분말과 마그네슘산화물분말을 2시간 동안 볼밀링하는 과정임을 특징으로 한다.The powder mixing step is characterized in that the ball milling the magnesium hydride powder and magnesium oxide powder for 2 hours.
상기 분말혼합단계에서 유성볼밀링이 적용되는 것을 특징으로 한다.In the powder mixing step, planetary ball milling is applied.
이상 본 발명에 의한 마그네슘계 수소발생용 분말의 구성을 설명한다.The constitution of the magnesium-based hydrogen generating powder according to the present invention is described above.
마그네슘계 수소발생용 분말은 물과 반응시에 수소를 발생시키기 위한 것으로, 마그네슘수소화물분말과 마그네슘산화물분말을 포함하여 구성된다.Magnesium-based hydrogen generating powder is for generating hydrogen upon reaction with water, and comprises a magnesium hydride powder and magnesium oxide powder.
그리고, 상기 마그네슘계 수소발생용 분말은 물과 반응시 마그네슘산화 물(MgO)과 마그네슘수화물(Mg(OH2)) 중 어느 하나 이상의 부산물을 생성하게 된다.The magnesium-based hydrogen generating powder generates by-products of any one or more of magnesium oxide (MgO) and magnesium hydrate (Mg (OH 2 )) when reacted with water.
보다 상세하게는 상기 마그네슘계 수소발생용 분말은, 마그네슘수소화물분말(MgH2) 90 내지 95중량%와, 마그네슘산화물분말(MgO) 5 내지 10중량%를 포함하여 구성되며, 유성 볼밀링에 의해 혼합되어 물과 반응시에 마그네슘 이외의 다른 금속성분이 전혀 포함되지 않은 마그네슘산화물(MgO)과 마그네슘수화물(Mg(OH2)) 중 어느 하나 이상의 부산물을 생성하게 된다.More specifically, the magnesium-based hydrogen generating powder is composed of 90 to 95% by weight of magnesium hydride powder (MgH 2 ) and 5 to 10% by weight of magnesium oxide powder (MgO), by planetary ball milling. When mixed with water, by-products of at least one of magnesium oxide (MgO) and magnesium hydrate (Mg (OH 2 )) containing no metal other than magnesium are produced.
그리고, 상기 마그네슘계 수소발생용 분말은 3분 내지 60분간 0.01 내지 0.2329 g/분의 수소방출량을 나타낸다. 이러한 결과는 아래 실험을 통해 확인하기로 한다.In addition, the magnesium-based hydrogen generating powder exhibits a hydrogen emission amount of 0.01 to 0.2329 g / min for 3 to 60 minutes. These results will be confirmed through the following experiment.
이하 상기 마그네슘계 수소발생용 분말의 제조방법을 첨부된 도 1을 참조하여 설명한다.Hereinafter, a method of preparing the magnesium-based hydrogen generating powder will be described with reference to FIG. 1.
도 1에는 본 발명에 의한 마그네슘계 수소발생용분말의 제조방법을 나타낸 공정 순서도가 도시되어 있다.1 is a process flowchart showing a method for producing a magnesium-based hydrogen generating powder according to the present invention.
도면과 같이, 본 발명에 의한 마그네슘계 수소발생용 분말의 제조방법은, 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 준비하는 분말준비단계(S100)와, 상기 마그네슘수소화물분말(MgH2) 90 내지 95중량%와 상기 마그네슘산화물분말(MgO) 5 내지 10중량%를 혼합하는 분말혼합단계(S200)로 이루어진다.As shown in the drawing, the method for preparing magnesium-based hydrogen generating powder according to the present invention includes preparing a powder of magnesium hydride (MgH 2 ) and magnesium oxide powder (MgO) (S100) and the magnesium hydride powder (MgH 2 ) It consists of a powder mixing step (S200) of mixing 90 to 95% by weight and 5 to 10% by weight of the magnesium oxide powder (MgO).
우선, 90 중량% 내지 95 중량%의 마그네슘수소화물분말(MgH2)과 5중량% 내지 10중량%의 마그네슘산화물분말(MgO)을 분말준비단계(S100)에서 준비한 다음, 준비된 마그네슘수소화물분말(MgH2)과 마그네슘산화물분말(MgO)을 볼밀링하여 혼합하게 된다(분말혼합단계:S200).First, 90% to 95% by weight of magnesium hydride powder (MgH 2 ) and 5% to 10% by weight of magnesium oxide powder (MgO) are prepared in a powder preparation step (S100), and then prepared magnesium hydride powder ( MgH 2 ) and magnesium oxide powder (MgO) are ball milled and mixed (powder mixing step: S200).
상기한 두 단계만으로 본 발명에 의한 마그네슘계 수소발생용 분말의 제조는 완료되며, 상기 마그네슘수소화물분말과 마그네슘산화물분말의 중량비에 대한 수치 한정 이유는 아래에서 실시예 및 비교예를 통해 보다 상세히 설명한다.The production of magnesium-based hydrogen generating powder according to the present invention is completed only by the above two steps, and the reason for limiting the numerical value of the weight ratio of the magnesium hydride powder and the magnesium oxide powder will be described in more detail with reference to Examples and Comparative Examples below. do.
그리고, 상기 분말혼합단계(S200)에서 마그네슘계 수소발생용 분말을 볼밀링 하는 이유는 마그네슘수소화물분말과 마그네슘산화물분말이 미세하게 분쇄되고 잘 혼합이 되어서 물과 반응시에 반응속도를 높이기 위함이다.The reason for the ball milling of the magnesium-based hydrogen generating powder in the powder mixing step (S200) is to increase the reaction rate when the magnesium hydride powder and the magnesium oxide powder are finely ground and mixed well to react with water. .
즉, 볼밀링을 실시하지 않은 마그네슘계 수소발생용 분말은 물과의 반응이 너무 느려서 수소 발생에 어려움이 있기 때문이다.That is, the magnesium-based hydrogen generating powder without ball milling is difficult to generate hydrogen because the reaction with water is too slow.
그리고, 상기 마그네슘수소화물분말은 물과 반응하는 주성분이며, 혼합된 마그네슘계 수소발생용 분말 전체 중량에 대하여 90중량% 내지 95중량%의 마그네슘수소화물분말이 요구된다. 그리고, 마그네슘산화물분말은 마그네슘계 수소발생용 분말의 전체 중량에 대하여 5중량% 내지 10중량%이 포함되어야 한다.The magnesium hydride powder is a main component that reacts with water, and requires 90 to 95 wt% magnesium hydride powder based on the total weight of the mixed magnesium-based hydrogen generating powder. In addition, the magnesium oxide powder should contain 5% by weight to 10% by weight relative to the total weight of the magnesium-based hydrogen generating powder.
이러한 이유는 상기 마그네슘산화물분말의 중량%가 5.0 미만이면 마그네슘수소화물분말의 분쇄가 용이하지 않을 뿐 아니라, 마그네슘계 수소발생용 분말과 물의 반응시 촉매 효과가 적어 반응이 잘 일어나지 않게 된다.The reason for this is that when the weight percentage of the magnesium oxide powder is less than 5.0, the hydride of magnesium hydride powder is not easy to be pulverized, and the reaction of the magnesium-based hydrogen-generating powder and water is less effective, resulting in less reaction.
또한, 상기 마그네슘계 수소발생용 분말의 전체 중량에 대하여 마그네슘산화 물분말의 중량%가 10.0을 초과하게 되면, 물과 반응하는 주성분인 마그네슘수소화물분말의 양이 상대적으로 적어 수소발생량이 줄어들게 되는 문제점을 야기하게 된다.In addition, when the weight percentage of the magnesium oxide powder exceeds 10.0 with respect to the total weight of the magnesium-based hydrogen-generating powder, the amount of magnesium hydride powder, which is a main component reacting with water is relatively small, the hydrogen generation amount is reduced Will cause.
따라서, 물과 반응시 수소발생량을 증가시키고 반응성도 높이기 위해서 상기 마그네슘계 수소발생용 분말은, 마그네슘수소화물분말(MgH2) 90 내지 95중량%와 상기 마그네슘산화물분말(MgO) 5 내지 10중량%를 포함하여 구성됨이 바람직하다.Therefore, the magnesium-based hydrogen generating powder is 90 to 95% by weight of magnesium hydride powder (MgH 2 ) and 5 to 10% by weight of magnesium oxide powder (MgO) in order to increase the amount of hydrogen generated when reacting with water and to increase the reactivity. It is preferably configured to include.
이하 첨부된 도 2 및 도 3을 참조하여 본 발명의 실시예와 비교예를 서로 비교하여 설명하기로 한다.Hereinafter, embodiments and comparative examples of the present invention will be described with reference to FIGS. 2 and 3.
도 2에는 본 발명에 의한 마그네슘계 수소발생용분말의 실시예와 비교예에서 물과 반응시간이 증가함에 따른 기체(수소)방출량 및 반응생성부산물 종류를 나타낸 표가 도시되어 있고, 도 3에는 본 발명에 의한 마그네슘계 수소발생용분말의 실시예와 비교예에서 분당 방출된 기체무게를 환산하여 비교한 표가 도시되어 있다.2 is a table showing the gas (hydrogen) emission amount and the reaction product by-product type with increasing reaction time with water in the examples and comparative examples of magnesium-based hydrogen generation powder according to the present invention, Figure 3 Tables comparing the gas weights released per minute in the examples and comparative examples of the magnesium-based hydrogen generation powder according to the invention are shown.
[비교예1][Comparative Example 1]
순수한 물 2.08g을 상온에서 유지시에 시간 변화에 따른 무게 감소량을 측정하였다. 60분간 무게 감소량을 측정하였으나, 감소된 물의 양은 매우 작았으며 감소된 물은 수분의 중발에 기인한다. 2.08 g of pure water at room temperature was measured for weight loss with time. The weight loss was measured for 60 minutes, but the amount of reduced water was very small and the reduced water was due to the water buildup.
[비교예2]Comparative Example 2
볼밀링하지 않은 알루미늄(Al)분말 0.7572g에 물 2.08g을 첨가하여 시간 경 과에 따른 물과 알루미늄(Al)분말 혼합물의 무게 변화량을 측정하였다.2.08 g of water was added to 0.7572 g of aluminum (Al) powder without ball milling, and the weight change of the water and aluminum (Al) powder mixture was measured over time.
즉, 측정 시간동안 물과 알루미늄분말이 반응하여 수소가 발생하게 되면, 수소 발생량은 감소된 무게와 비례하게 되므로 물 및 알루미늄분말의 감소량을 60분동안 측정하였으나 감소량은 매우 적었다.That is, when water and aluminum powder reacted during the measurement time to generate hydrogen, the amount of hydrogen generated was proportional to the reduced weight, so the decrease of water and aluminum powder was measured for 60 minutes, but the decrease was very small.
[비교예3][Comparative Example 3]
볼밀링하지 않는 TiH2분말 0.7572g을 물 2.08g에 첨가하여 시간 경과에 따른 물과 TiH2분말 혼합물의 무게변화를 측정하였다. 0.7572 g of TiH 2 powder without ball milling was added to 2.08 g of water to measure the weight change of the water and TiH 2 powder mixtures over time.
즉, 반응 시간이 증가함에 따라 수소 발생량이 증가하게 되면 결국 반응전 물과 TiH2분말의 무게가 비례하여 감소하게 되므로 60분 동안 물과 TiH2분말의 감소량을 측정하였다.In other words, if the amount of hydrogen generated increases with increasing reaction time, the weight of water and TiH 2 powder before reaction is reduced proportionally, and thus the amount of reduction of water and TiH 2 powder was measured for 60 minutes.
그러나, 물과 TiH2분말의 감소량은 극히 적었다.However, the decrease in water and TiH 2 powder was extremely small.
[비교예4][Comparative Example 4]
볼밀링하지 않은 마그네슘 분말 0.7572g을 물 2.08g과 혼합하여 시간 변화에 따른 물과 마그네슘분말 혼합물의 무게 변화를 측정하였다.0.7572 g of non-ball milled magnesium powder was mixed with 2.08 g of water to measure the weight change of the water and magnesium powder mixture over time.
그 결과, 60분동안 감소된 물 및 마그네슘 분말의 무게는 극히 작은 것으로 나타났다.As a result, the weight of water and magnesium powder reduced for 60 minutes was found to be extremely small.
[비교예5][Comparative Example 5]
볼밀링된 마그네슘분말 0.7572g을 물 2.08g과 혼합하여 시간 경과에 따른 물과 마그네슘분말 혼합물의 무게 변화를 60분 동안 측정하였다.0.7572 g of the ball milled magnesium powder was mixed with 2.08 g of water, and the weight change of the water and magnesium powder mixture over time was measured for 60 minutes.
그 결과, 물과 마그네슘분말의 무게 감소량은 극히 작아서 수소 발생량을 측정하는데 어려움이 있었다. 이것은 물과 마그네슘분말의 반응성이 낮은 것을 증명하는 것으로 볼 수 있다.As a result, the weight loss of water and magnesium powder was extremely small, which made it difficult to measure the amount of hydrogen generated. This can be seen as evidence of low reactivity of water and magnesium powder.
[비교예6]Comparative Example 6
볼밀링을 하지 않는 마그네슘수소화물(MgH2)분말 0.7572g을 물 2.08g에 첨가하여 시간 경과에 따른 물과 마그네슘수소화물분말 혼합물의 무게 감소량을 60분간 측정하였다.0.7572 g of magnesium hydride (MgH 2) powder without ball milling was added to 2.08 g of water, and the weight loss of water and magnesium hydride powder mixtures over time was measured for 60 minutes.
그 결과, 전술한 [비교예1] 내지 [비교예5]보다는 수소발생량이 증가하였으나, 만족할만한 수소 발생량을 얻지 못했다. As a result, although the amount of hydrogen generation increased from [Comparative Example 1] to [Comparative Example 5] described above, a satisfactory amount of hydrogen generation was not obtained.
[비교예7]Comparative Example 7
볼밀링 한 마그네슘수소화물(MgH2)분말 0.7572g을 물 2.08g을 첨가하여 시간경과에 따른 물과 마그네슘수소화물(MgH2)분말 혼합물의 무게 감소량을 60분간 측정하였다.0.7572 g of ball milled magnesium hydride (MgH 2) powder was added with 2.08 g of water, and the weight loss amount of the water and magnesium hydride (MgH 2) powder mixture over time was measured for 60 minutes.
그 결과 [비교예6]보다는 수소발생량이 증가하긴 했으나, 만족할만한 수소발생량을 얻지는 못했다.As a result, although the amount of hydrogen generation increased than [Comparative Example 6], satisfactory hydrogen generation amount was not obtained.
[비교예8]Comparative Example 8
마그네슘수소화물(MgH2)분말 97.5 중량%와 마그네슘산화물분말(MgO) 2.5중량%를 유성볼밀을 이용하여 2시간 동안 혼합하였다.97.5 wt% of magnesium hydride (MgH2) powder and 2.5 wt% of magnesium oxide powder (MgO) were mixed for 2 hours using a planetary ball mill.
이렇게 얻어진 혼합분말 0.7572g을 물 2.08g과 섞어 시간 경과에 따른 혼합물의 무게 감소 변화량을 측정하였다.0.7572 g of the mixed powder thus obtained was mixed with 2.08 g of water to measure the change in weight loss of the mixture over time.
1시간 동안 무게 감소 변화량을 측정한 결과 감소된 무게가 크지 않아 수소 발생량은 극히 적은 것으로 볼 수 있다.As a result of measuring the weight loss change for 1 hour, the reduced weight is not so large that hydrogen generation is extremely small.
[비교예9]Comparative Example 9
마그네슘수소화물(MgH2)분말 85 중량%와 마그네슘산화물분말(MgO) 15중량%를 혼합한 후 유성볼밀을 이용하여 2시간 동안 혼합하였다.85 wt% of magnesium hydride (MgH2) powder and 15 wt% of magnesium oxide powder (MgO) were mixed and mixed for 2 hours using a planetary ball mill.
이때 얻어진 혼합분말 0.7572g과 물 2.08g을 섞어 시간 변화에 따른 혼합물의 무게 감소량을 측정하였다.0.7572 g of the mixed powder obtained and 2.08 g of water were mixed to measure the weight loss of the mixture with time.
그 결과, 수소발생량은 극히 작게 나타났다.As a result, the hydrogen generation amount was extremely small.
[비교예10]Comparative Example 10
마그네슘수소화물(MgH2)분말 75중량%와 마그네슘산화물분말(MgO) 25중량%를 유성 볼밀을 이용하여 2시간 동안 혼합하였다.75 wt% of magnesium hydride (MgH2) powder and 25 wt% of magnesium oxide powder (MgO) were mixed for 2 hours using an oily ball mill.
이렇게 얻어진 혼합분말 0.7572g을 물 2.08g에 첨가하여 시간 경과에 따른 혼합분말의 무게 감소를 측정함으로써 수소 발생량을 환산하였다.0.7572 g of the mixed powder thus obtained was added to 2.08 g of water, and the amount of hydrogen generated was converted by measuring the weight loss of the mixed powder over time.
비교예10에서도 역시 수소 발생량은 낮았다.In Comparative Example 10, the hydrogen generation amount was also low.
[비교예11]Comparative Example 11
볼밀링하지 않은 마그네슘수소화물(MgH2)분말 95중량%와 마그네슘산화분말(MgO) 5중량%를 스푼을 이용하여 2시간동안 교반하여 혼합하였다.95% by weight of the non-ball milled magnesium hydride (MgH 2) powder and 5% by weight of magnesium oxide powder (MgO) were stirred and mixed for 2 hours using a spoon.
이렇게 얻어진 혼합분말 0.7572g을 물 2.08g에 첨가하여 이러한 혼합분말의 무게 감소를 60분 동안 측정하였다.0.7572 g of the mixed powder thus obtained was added to 2.08 g of water to measure the weight loss of the mixed powder for 60 minutes.
그 결과 볼밀링 과정이 생략됨에 따른 반응성 저하로 인해 수소 발생량이 낮게 나타났다.As a result, the hydrogen generation was low due to the decrease in reactivity as the ball milling process was omitted.
[실시예1]Example 1
마그네슘수소화물(MgH2)분말 95 중량%, 마그네슘산화물분말(MgO) 5중량%를 혼합한 후 유성볼밀을 이용하여 2시간 동안 교반 및 분쇄하였다.Magnesium hydride (MgH 2 )
이렇게 얻어진 혼합분말 0.7572g을 물 2.08g에 첨가하여 시간 경과에 따른 혼합분말의 무게 감소량을 측정하였다.0.7572 g of the mixed powder thus obtained was added to 2.08 g of water to measure the weight loss of the mixed powder over time.
측정 결과, 비교예1 내지 비교예11보다 높은 수소무게를 나타내었다.As a result of the measurement, the hydrogen weight was higher than that of Comparative Examples 1 to 11.
즉, 본 발명의 실시예1에서는 3분간 반응시간을 주었을 때 0.2329g/분의 기체발생무게를 나타내었으며, 시간이 경과함에 따라 수소발생중량은 증가하였다.That is, in Example 1 of the present invention, when the reaction time was given for 3 minutes, the gas generation weight was 0.2329 g / min, and the hydrogen generation weight increased with time.
[실시예2]Example 2
마그네슘수소화물(MgH2)분말 90중량%, 마그네슘산화물분말(MgO) 10중량%를 혼합한 후 유성볼밀을 이용하여 2시간 동안 교반 및 분쇄하였다.Magnesium hydride (MgH 2 )
이렇게 제조된 마그네슘계 수소발생용분말은 실시예1보다는 수소발생무게에 있어서 증가하였다.The magnesium-based hydrogen generating powder thus prepared was increased in weight of hydrogen generation than in Example 1.
상기와 같은 비교예들과 실시예들을 단위 시간(분)당 수소발생량을 측정해본 결과 도 3과 같이, 0.01 내지 0.2329 g/분으로서 비교예와 대비할 때 본 발명의 실시예에 따라 제조된 마그네슘계 수소발생용 분말은 수소 발생량이 현저히 증가한 것을 알 수 있다.As a result of measuring the hydrogen generation amount per unit time (minutes) of the comparative examples and examples as described above, as compared to the comparative example as 0.01 to 0.2329 g / min as prepared in accordance with the embodiment of the present invention Hydrogen generation powder can be seen that the hydrogen generation amount increased significantly.
이러한 본 발명의 범위는 상기에서 예시한 실시 예에 한정하지 않고, 상기와 같은 기술범위 안에서 당업계의 통상의 기술자에게 있어서는 본 발명을 기초로 하는 다른 많은 변형이 가능할 것이다.The scope of the present invention is not limited to the above-exemplified embodiments, and many other modifications based on the present invention may be made by those skilled in the art within the above technical scope.
상기와 같은 구성을 가지는 본 발명에 의한 마그네슘계 수소발생용 분말의 제조방법에서는, 소정의 비율로 마그네슘계 수소발생용 분말, 마그네슘계산화분말을 볼밀링 하는 과정만으로 마그네슘계 수소발생용 분말이 제조 가능하도록 구성하였다.In the method for producing magnesium-based hydrogen-generating powder according to the present invention having the above structure, magnesium-based hydrogen-generating powder is produced only by the process of ball milling magnesium-based hydrogen-generating powder and magnesium-based oxidation powder at a predetermined ratio. It was configured to be possible.
따라서, 제조 공정이 간소하여 생산성이 향상되고 불량률이 감소하게 되며, 물과 반응시에 보다 많은 수소를 발생시킬 수 있는 이점이 있다.Therefore, the manufacturing process is simple, the productivity is improved, the defect rate is reduced, there is an advantage that can generate more hydrogen when reacting with water.
또한, 본 발명에 따른 마그네슘계 수소발생용 분말은, 물과 반응시에 부산물로서 순수한 마그네슘산화물이나 마그네슘수화물을 얻을 수 있게 되며, 마그네슘 이외에는 어떠한 금속 성분도 포함되지 않게 된다.In addition, the magnesium-based hydrogen-generating powder according to the present invention can obtain pure magnesium oxide or magnesium hydrate as a by-product when reacted with water, and does not contain any metal components other than magnesium.
따라서, 물과 반응시에 수소를 발생시킬 뿐만 아니라, 마그네슘산화물(MgO)과 마그네슘수화물(Mg(OH2)) 중 하나 이상의 부산물을 동시에 생산할 수 있는 이점이 있다.Therefore, in addition to generating hydrogen when reacting with water, there is an advantage that can simultaneously produce one or more by-products of magnesium oxide (MgO) and magnesium hydrate (Mg (OH 2 )).
뿐만 아니라, 마그네슘 이외에 다른 금속 성분이 전혀 포함되지 않은 부산물을 생성하게 되므로, 종래의 매립 등으로 인한 환경 오염을 미연에 차단할 수 있는 이점이 있다.In addition, since by-products do not contain any other metal components other than magnesium, there is an advantage that can prevent the environmental pollution due to the conventional landfill, etc. in advance.
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| KR100567426B1 (en) | 1997-10-22 | 2006-04-04 | 하이드로-퀘벡 | Nanocomposites with activated interfaces prepared by mechanical grinding of magnesium hydrides and process for preparing the same |
| KR100811116B1 (en) | 2006-11-14 | 2008-03-06 | 한국과학기술연구원 | Fabrication method of magnesium based hydrogen storage metarial |
| JP2008266781A (en) | 2007-03-24 | 2008-11-06 | Tokai Univ | METHOD FOR MANUFACTURING Mg-Al BASED HYDROGEN STORAGE ALLOY POWDER AND Mg-Al BASED HYDROGEN STORAGE ALLOY POWDER OBTAINED BY THE MANUFACTURING METHOD |
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| JP2004204309A (en) | 2002-12-26 | 2004-07-22 | National Institute Of Advanced Industrial & Technology | Hydrogen storage material, and production method therefor |
| KR100811116B1 (en) | 2006-11-14 | 2008-03-06 | 한국과학기술연구원 | Fabrication method of magnesium based hydrogen storage metarial |
| JP2008266781A (en) | 2007-03-24 | 2008-11-06 | Tokai Univ | METHOD FOR MANUFACTURING Mg-Al BASED HYDROGEN STORAGE ALLOY POWDER AND Mg-Al BASED HYDROGEN STORAGE ALLOY POWDER OBTAINED BY THE MANUFACTURING METHOD |
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