KR100535979B1 - Method for Preparing Carbonaceous Body - Google Patents
Method for Preparing Carbonaceous Body Download PDFInfo
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- KR100535979B1 KR100535979B1 KR10-2003-0096002A KR20030096002A KR100535979B1 KR 100535979 B1 KR100535979 B1 KR 100535979B1 KR 20030096002 A KR20030096002 A KR 20030096002A KR 100535979 B1 KR100535979 B1 KR 100535979B1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6021—Extrusion moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
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Abstract
본 발명은 탄소 성형체의 제조방법에 관한 것으로, 물, 규산염 광물, 흑연 및 탄소분말을 동시에 투입하고 혼합하는 혼합단계; 상기 혼합물을 압출 성형기에 투입하여 상온에서 압출 성형하는 압출성형단계; 및 상기 압출성형단계를 거친 성형체를 상온 내지 100℃이하의 온도에서 건조하고 불활성 분위기 1000℃이상의 온도에서 소성하는 소성단계를 포함하여 이루어지며, 본 발명에 의한 제조방법은 세라믹 결합재를 사용하여 상온에서 압출 성형하여 탄소 성형체를 제조할 수 있는 효과가 있다.The present invention relates to a method for producing a carbon molded body, comprising: a mixing step of simultaneously introducing and mixing water, silicate mineral, graphite and carbon powder; An extrusion molding step of inserting the mixture into an extrusion molding machine and extruding at room temperature; And a firing step of drying the molded article subjected to the extrusion molding step at a temperature of from room temperature to 100 ° C. or below and firing at a temperature of at least 1000 ° C. in an inert atmosphere. The manufacturing method according to the present invention uses a ceramic binder at room temperature. There is an effect that can be produced by extrusion molding a carbon molded body.
Description
본 발명은 탄소계 성형체의 제조방법에 관한 것이다. 더욱 상세하게는 탄소 성형체의 제조에 있어서, 기존의 압출 설비 승온시 결합재 용융에 의한 유동성을 세라믹 결합재의 첨가로 대체하여 상온에서 압출 성형이 가능한 탄소계 성형체의 제조방법에 관한 것이다. The present invention relates to a method for producing a carbon-based molded body. More particularly, the present invention relates to a method for producing a carbon-based molded body which can be extrusion-molded at room temperature by replacing the fluidity of the binder melted with the addition of a ceramic binder when heating the existing extrusion equipment.
기존 탄소계 성형체의 성형은, 결합재 유동성의 향상을 위하여 결합재 수지의 연화점 이상에서 실시해야 했다. 따라서 고온에서 압출성형(일본특허 2003-192438, 2001-342419)하는 문제점이 있었다. Molding of the existing carbon-based molded body had to be performed at or above the softening point of the binder resin in order to improve the binder fluidity. Therefore, there was a problem of extrusion molding at high temperature (Japanese Patent 2003-192438, 2001-342419).
또한, 결합재의 용융에 의해 유동성을 부여하기 위해 의존하여 성형체 제조시 고가의 압출성형 설비가 반드시 구비되어야 하는 단점이 있었다. In addition, there is a disadvantage in that expensive extrusion equipment must be provided when manufacturing a molded body depending on the flowability by melting the binder.
본 발명에서는 결합재의 유동성을 물과의 친화력이 있는 규산염 광물로 대체 부여함으로써, 기존 압출 설비 승온시 결합재 용융에 의해 유동성을 부여하는 기술을 결합재의 대체만으로 크게 개선한 기술이라는데 특징이 있다.In the present invention, by giving the fluidity of the binder replaced by a silicate mineral having affinity with water, it is characterized in that the technology to impart fluidity by melting the binder at the time of heating up the existing extrusion equipment by greatly replacing only the binder.
상기와 같은 문제점을 해결하기 위하여 본 발명은, 세라믹 결합재의 첨가하여 상온에서 압출 성형할 수 있는 탄소계 성형체의 제조방법을 제공하는 것을 목적으로 한다. In order to solve the above problems, an object of the present invention is to provide a method for producing a carbon-based molded article that can be extrusion molded at room temperature by adding a ceramic binder.
본 발명의 상기 목적 및 기타 목적들은 하기 설명되는 본 발명에 의하여 모두 달성될 수 있다. The above and other objects of the present invention can be achieved by the present invention described below.
상기 목적을 달성하기 위하여 본 발명은, The present invention to achieve the above object,
물, 규산염 광물, 흑연 및 탄소분말을 동시에 투입하고 혼합하는 혼합단계; 상기 혼합물을 압출 성형기에 투입하여 상온에서 압출 성형하는 압출성형단계; 및 상기 압출성형단계를 거친 성형체를 상온 내지 100℃이하의 온도에서 건조하고 불활성 분위기 1000℃이상의 온도에서 소성하는 소성단계를 포함하여 이루어지는 것을 특징으로 하는 탄소계 성형체의 제조방법을 제공한다. A mixing step of simultaneously introducing and mixing water, silicate mineral, graphite and carbon powder; An extrusion molding step of inserting the mixture into an extrusion molding machine and extruding at room temperature; And it provides a method for producing a carbon-based molded body comprising the firing step of drying the molded article subjected to the extrusion molding step at a temperature of room temperature to 100 ℃ or less and firing at a temperature of 1000 ℃ or more in an inert atmosphere.
상기 혼합단계는 물과 규산염 광물을 2:1 내지 7:1(중량비)로 혼합하여 슬러리를 제조한 후, 흑연 또는 탄소분말과 상기 슬러리의 비율을 90:10 내지 70:30로 하여 혼합하는 것으로 이루어질 수 있다. The mixing step is to prepare a slurry by mixing water and silicate minerals in a 2: 1 to 7: 1 (weight ratio), and then to mix the graphite or carbon powder and the slurry in a ratio of 90:10 to 70:30. Can be done.
상기 규산염 광물과 동시에 탄소질 결합재를 첨가할 수 있다. A carbonaceous binder may be added simultaneously with the silicate mineral.
이하, 본 발명에 대하여 상세히 설명하면 다음과 같다. Hereinafter, the present invention will be described in detail.
본 발명에 의해 탄소계 성형체를 제조할 경우, 기존의 압출 성형 공정에 의해 제조한 탄소계 성형체에 비해 압출 성형을 상온에서 행할 수 있다는 장점이 있으므로, 비교적 저가의 압출 설비를 이용하여 유사한 성능의 탄소계 성형체를 제조할 수 있다. When manufacturing a carbon-based molded article according to the present invention, there is an advantage that the extrusion molding can be carried out at room temperature, compared to the carbon-based molded article produced by the conventional extrusion molding process, carbon of similar performance using a relatively inexpensive extrusion equipment A system molded object can be manufactured.
본 발명에서는 용매로서 물을 사용하는 것으로 충분하며, 세라믹 결합재로서는 몬모릴로나이트(montmorillonite), 벤토나이트(bentonite)등으로 대표되는 규산염 광물을 일정량 사용함으로써, 탄소질 혹은 흑연질 분말로부터 압출 성형에 의한 성형체의 제조가 가능하다. In the present invention, it is sufficient to use water as a solvent, and by using a predetermined amount of silicate minerals represented by montmorillonite, bentonite, etc. as a ceramic binder, the production of a molded body by extrusion molding from carbonaceous or graphite powder Is possible.
본 발명은 탄소나 흑연 성형체를 제조하는데 있어서, 탄소질 결합재와 더불어 혹은 세라믹 재질만의 결합재를 사용하여, 상온에서 탄소나 흑연분말과 혼합하고, 압출 성형을 통해서 탄소질 성형체를 제조하는 공정과 이때 결합재로서 몬모릴로나이트(montmorillonite), 벤토나이트(bentonite)등 일정량의 규산염 광물을 사용하는 공정으로 구성된다. In the present invention, in the production of carbon or graphite molded body, in addition to the carbonaceous binder or using a ceramic binder alone, mixing with carbon or graphite powder at room temperature, and manufacturing a carbonaceous molded body by extrusion molding It consists of a process using a certain amount of silicate minerals such as montmorillonite, bentonite, etc. as a binder.
(1) 물과 규산염 광물을 혼합하여 슬러리 상태로 만든 결합재를 흑연 혹은 탄소 분말과 균일하게 혼합한다. 이때 탄소질 결합재(핏치, 페놀 등)를 병용할수도 있으며 세라믹 결합재 단독으로 사용할 수도 있다. (1) Mix the water and silicate minerals into a slurry, and uniformly mix the graphite or carbon powder. In this case, carbonaceous binders (pitch, phenol, etc.) may be used in combination, or ceramic binders may be used alone.
(2) 혼합한 배토(흑연 혹은 탄소분말과 결합재)를 압출성형기에 투입, 상온에서 압출성형한다. (2) The mixed clay (graphite or carbon powder and binder) is put into an extruder and extruded at room temperature.
(3) 성형체를 건조하고 소정의 온도에서 열처리하여 최종 탄소 성형체를 얻는다. (3) The molded product is dried and heat treated at a predetermined temperature to obtain a final carbon molded product.
규산염 광물로 구성되어 있는 세라믹 재질 결합재는 흑연 혹은 탄소분말에 물과 함께 투입하여 혼합하여도 관계없으나, 탄소질 분말과의 혼합 이전에 미리 슬러리의 상태로 제조하여 두는 것이 바람직하다. 또한 필요에 따라서 석탄계/석유계 핏치나 페놀과 같은 탄소질 결합재를 병용해서 사용할 수도 있다. The ceramic binder composed of silicate minerals may be mixed with graphite or carbon powder with water, but is preferably prepared in a slurry state before mixing with carbonaceous powder. If necessary, a carbonaceous binder such as coal / petroleum pitch or phenol may be used in combination.
이때 물과 세라믹 재질 결합재의 혼합비율은 물:결합재 = 2:1에서 7:1(중량비)로 하는 것이 바람직하다. 투입하는 물의 양이 그 이하일 때는 결합재의 역할을 할 수 있을 정도의 유동성의 확보가 어려우며, 물의 양이 그 이상이 될 때는 점도가 지나치게 낮아져서 결합재로서의 역할이 불충분해 진다. In this case, the mixing ratio of the water and the ceramic binder is preferably water: binder = 2: 1 to 7: 1 (weight ratio). When the amount of water to be added is less than it is difficult to secure the fluidity enough to act as a binder, when the amount of water is more than that the viscosity is too low, the role as a binder is insufficient.
이와 같은 공정을 통해서 얻은 결합재를 탄소 혹은 흑연 분말과 혼합한다. 이때 결합재의 양은 탄소분말에 대해서 10 내지 30중량비로 혼합한다. 이 이하의 결합재의 양으로는 탄소분말의 유동성 부여가 불가능해서 성형체 제조가 불가능하며, 그 이상의 결합재에서는 성형체의 제조는 가능하지만, 결합재의 양이 지나치게 많아서 열처리(소성)시, 결합재 유래 세라믹과 탄소와의 반응에 기인하여 성형체의 기공율이 증가하여 특성 열화원인으로 작용할 수 있다. The binder obtained through this process is mixed with carbon or graphite powder. At this time, the amount of the binder is mixed in a 10 to 30 weight ratio based on the carbon powder. The amount of the binder below is impossible to impart fluidity of the carbon powder, and thus, it is impossible to manufacture a molded body. In the case of a binder above, the molded body can be manufactured. However, when the amount of the binder is too large, the binder-derived ceramic and carbon Due to the reaction with the porosity of the molded article is increased may act as a cause of deterioration characteristics.
혼합한 배토(흑연 혹은 탄소분말, 결합재)를 압출성형기에 투입하고 압출 성형하여 성형체를 제조한다. The mixed clay (graphite or carbon powder, binder) is put into an extrusion molding machine and extrusion molded to produce a molded body.
압출성형에 의해서 얻은 성형체는 상온 및 100℃부근의 온도에서 건조한 후, 소정의 온도에서 열처리를 행한다. 건조 온도를 100℃이상으로 할 경우, 수분의 증발 속도가 지나치게 빨라서 성형체에 균열이 발생할 수 있다. 건조한 성형체는 불활성 분위기 1000℃이상의 온도에서 소성하여 최종 탄소 혹은 흑연 성형체로 한다. The molded article obtained by extrusion molding is dried at a temperature of around room temperature and 100 캜, and then heat treated at a predetermined temperature. When the drying temperature is 100 ° C. or more, the rate of evaporation of moisture is too high, and cracks may occur in the molded body. The dried molded body is calcined at an inert atmosphere of 1000 ° C. or higher to obtain a final carbon or graphite molded body.
이하 하기의 실시예를 통하여 본 발명을 더욱 상세히 설명하지만, 본 발명의 범위가 실시예에 한정되는 것은 아니다. Hereinafter, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the examples.
[실시예 1] Example 1
규산염 광물인 벤토나이트와 물을 각각 중량비 1:3로 투입하고 교반을 통해서 세라믹 재질 결합재를 제조하였다. 제조한 결합재와 평균입경 10㎛의 흑연을 각각 10:90의 비율로 혼합하고 압출성형에 의해서 탄소 성형체를 제조하였다. Bentonite and water, which are silicate minerals, were added at a weight ratio of 1: 3, respectively, and a ceramic binder was prepared by stirring. The prepared binder and graphite having an average particle diameter of 10 μm were mixed at a ratio of 10:90, respectively, and a carbon molded body was prepared by extrusion molding.
제조한 성형체를 상온에서 48시간, 100℃에서 24시간 건조한후, 1000℃에서 1시간 열처리하였다. 얻어진 탄소 성형체의 밀도는 1.5g/㎤를 나타내었다. The formed article was dried at room temperature for 48 hours, at 100 ° C for 24 hours, and then heat-treated at 1000 ° C for 1 hour. The density of the obtained carbon molded body showed 1.5 g / cm 3.
[실시예 2] Example 2
규산염 광물인 벤토나이트와 물을 각각 중량비 1:6으로 투입하고 교반을 통해서 세라믹 재질 결합재를 제조하였다. 제조한 결합재와 평균입경 10㎛의 흑연을 각각 10:90의 비율로 혼합하고 압출성형에 의해서 탄소 성형체를 제조하였다. Bentonite, which is a silicate mineral, and water were added in a weight ratio of 1: 6, respectively, and a ceramic binder was prepared by stirring. The prepared binder and graphite having an average particle diameter of 10 μm were mixed at a ratio of 10:90, respectively, and a carbon molded body was prepared by extrusion molding.
제조한 성형체를 상온에서 48시간, 100℃에서 24시간 건조한후, 1000℃에서 1시간 열처리하였다. 얻어진 탄소 성형체의 밀도는 1.4g/㎤를 나타내었다. The formed article was dried at room temperature for 48 hours, at 100 ° C for 24 hours, and then heat-treated at 1000 ° C for 1 hour. The density of the obtained carbon molded body showed 1.4 g / cm 3.
[실시예 3] Example 3
규산염 광물인 벤토나이트와 물을 각각 중량비 1:6으로 투입하고 교반을 통해서 세라믹 재질 결합재를 제조하였다. 제조한 결합재와 평균입경 10㎛의 흑연을 각각 10:90의 비율로 투입하고 탄소질 분말 결합재(고상 페놀수지)를 동시에 투입하여 혼합하고 압출성형에 의해서 탄소 성형체를 제조하였다. Bentonite, which is a silicate mineral, and water were added in a weight ratio of 1: 6, respectively, and a ceramic binder was prepared by stirring. The prepared binder and graphite having an average particle diameter of 10 μm were added at a ratio of 10:90, respectively, and a carbonaceous powder binder (solid phenol resin) was added at the same time to mix, and a carbon molded body was prepared by extrusion molding.
제조한 성형체를 상온에서 48시간, 100℃에서 24시간 건조한후, 1000℃에서 1시간 열처리하였다. 얻어진 탄소 성형체의 밀도는 1.5g/㎤를 나타내었다. The formed article was dried at room temperature for 48 hours, at 100 ° C for 24 hours, and then heat-treated at 1000 ° C for 1 hour. The density of the obtained carbon molded body showed 1.5 g / cm 3.
이상에서 설명한 바와 같이 본 발명에 의한 탄소계 성형체의 제조방법은, 기존의 압출 설비 승온시 결합재 용융에 의한 유동성을 세라믹 결합재의 첨가로 대체하여 상온에서 압출 성형이 가능한 탄소계 성형체를 제조하는 효과가 있는 유용한 발명인 것이다. As described above, the method for producing a carbon-based molded article according to the present invention has the effect of manufacturing a carbon-based molded article that can be extruded at room temperature by replacing the fluidity due to the melting of the binder with the addition of a ceramic binder when the existing extrusion equipment is heated. It is a useful invention.
상기에서 본 발명은 기재된 구체예를 중심으로 상세히 설명되었지만, 본 발명의 범주 및 기술사상 범위 내에서 다양한 변형 및 수정이 가능함은 당업자에게 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속하는 것도 당연한 것이다. While the invention has been described in detail above with reference to the described embodiments, it will be apparent to those skilled in the art that various modifications and variations are possible within the scope and spirit of the invention, and such modifications and variations fall within the scope of the appended claims. It is also natural.
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