KR101351468B1 - Manufacturing method of diesel particulate filter and diesel particulate filter manufactured by the method - Google Patents
Manufacturing method of diesel particulate filter and diesel particulate filter manufactured by the method Download PDFInfo
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- KR101351468B1 KR101351468B1 KR1020120036723A KR20120036723A KR101351468B1 KR 101351468 B1 KR101351468 B1 KR 101351468B1 KR 1020120036723 A KR1020120036723 A KR 1020120036723A KR 20120036723 A KR20120036723 A KR 20120036723A KR 101351468 B1 KR101351468 B1 KR 101351468B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2068—Other inorganic materials, e.g. ceramics
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
Abstract
본 발명은 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터에 관한 것으로, 더욱 상세하게는 코디어라이트, 월넛, 흑연, 바인더, 폴리비닐알코올, 트리에틸렌글리콜 및 윤활오일을 혼합하는 혼합물제조단계, 상기 혼합물제조단계에서 혼합된 혼합물을 성형하는 성형단계, 상기 성형단계를 통해 제조된 성형물을 가열하는 가열단계 및 상기 가열단계를 거친 성형물을 소성하는 소성단계로 이루어진다.
상기의 과정으로 이루어지는 디젤 입자 필터의 제조방법은 소성단계가 이산화탄소 또는 질소 분위기에서 진행되어 열 팽창 계수가 매우 낮은 디젤 입자 필터를 제공한다.The present invention relates to a method for producing a diesel particle filter and a diesel particle filter prepared by the method, and more particularly to mixing cordierite, walnut, graphite, binder, polyvinyl alcohol, triethylene glycol and lubricating oil. Mixture manufacturing step, the molding step of molding the mixture mixed in the mixture manufacturing step, the heating step of heating the molded product produced by the molding step and the firing step of firing the molding after the heating step.
In the method for producing a diesel particle filter comprising the above process, the firing step is performed in a carbon dioxide or nitrogen atmosphere to provide a diesel particle filter having a very low coefficient of thermal expansion.
Description
본 발명은 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터에 관한 것으로, 더욱 상세하게는 이산화탄소 또는 질소 분위기에서 소성단계가 진행되어 열 팽창 계수가 매우 낮은 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터에 관한 것이다.
The present invention relates to a method for producing a diesel particle filter and a diesel particle filter prepared by the method, and more particularly, a method for producing a diesel particle filter having a very low thermal expansion coefficient due to a sintering step in a carbon dioxide or nitrogen atmosphere. It relates to a diesel particle filter produced by the production method.
본 발명은 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터에 관한 것으로, 더욱 상세하게는 이산화탄소 또는 질소 분위기에서 소성단계가 진행되어 열 팽창 계수가 매우 낮은 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터에 관한 것이다.The present invention relates to a method for producing a diesel particle filter and a diesel particle filter prepared by the method, and more particularly, a method for producing a diesel particle filter having a very low thermal expansion coefficient due to a sintering step in a carbon dioxide or nitrogen atmosphere. It relates to a diesel particle filter produced by the production method.
자동차의 배출가스 중에 함유되는 디젤 입자(Diesel Particulate)는 탄소를 주성분으로 하는 미립자로, 자동차의 엔진이 고속회전될 경우에는 배출되는 배기가스가 비교적 고온이므로 디젤 입자가 자연적으로 연소되지만, 자동차의 엔진이 저속으로 회전할 경우에는 디젤 입자의 연소가 잘 이루어지지 않고, 배기가스와 함께 대기중으로 방출되어 대기를 오염시키게 된다.Diesel particles contained in the exhaust gas of automobiles are carbon-based particulates. When the engine of a vehicle is rotated at high speed, the exhaust gas is relatively high and diesel particles are naturally burned. When the engine rotates at a low speed, combustion of diesel particles is not performed well, and it is released into the atmosphere together with the exhaust gas to pollute the atmosphere.
상기와 같이 디젤 입자로 인한 대기의 오염을 방지하기 위해 배출가스가 배출되는 배기기관에 세라믹 재질로 이루어진 디젤 입자 필터가 장착되어 디젤입자의 대기 방출을 억제하고 있다.As described above, a diesel particle filter made of a ceramic material is installed in an exhaust pipe through which exhaust gas is discharged in order to prevent air pollution due to diesel particles, thereby suppressing the emission of diesel particles into the air.
그러나, 종래에 디젤 입자 필터는 열팽창계수가 높아 고온의 배기가스를 오랜 기간 여과하는 과정에서, 필터에 균열 등과 같은 기계적 물성의 저하가 발생하는 문제점이 있었다.However, the conventional diesel particle filter has a high thermal expansion coefficient, there is a problem that the mechanical properties such as cracks in the filter occurs in the process of filtering the high-temperature exhaust gas for a long time.
또한, 종래에 디젤 입자 필터는 필터에 형성된 기공의 크기 및 기공의 분포가 고르지 못하고, 기공 연결도가 낮은 문제점이 있었다.
In addition, the conventional diesel particle filter has a problem that the size of the pores formed in the filter and the distribution of the pores are uneven, and the pore connection degree is low.
본 발명의 목적은 열팽창계수가 낮아 오랜 기간 고온의 배기가스를 여과하더라도, 균열 등과 같은 기계적 물성의 저하가 발생하지 않는 필터를 제공하는 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터를 제공하는 것이다.SUMMARY OF THE INVENTION An object of the present invention is a method for producing a diesel particle filter, and a diesel particle filter manufactured by the method, which provide a filter having a low coefficient of thermal expansion and which does not cause deterioration of mechanical properties such as cracking even when filtering a high temperature exhaust gas for a long time. To provide.
본 발명의 다른 목적은 기공의 크기 및 기공의 분포가 고르며, 기공 연결도가 높은 필터를 제공하는 디젤 입자 필터의 제조방법 및 그 제조방법으로 제조된 디젤 입자 필터를 제공하는 것이다.
It is another object of the present invention to provide a method for producing a diesel particle filter which provides a filter having a uniform pore size and pore distribution, and high porosity connection, and a diesel particle filter manufactured by the method.
본 발명의 목적은 코디어라이트, 월넛, 흑연, 바인더, 폴리비닐알코올, 트리에틸렌글리콜 및 윤활오일을 혼합하는 혼합물제조단계, 상기 혼합물제조단계를 통해 혼합된 혼합물을 성형하는 성형단계, 상기 성형단계를 통해 제조된 성형물을 가열하는 가열단계 및 상기 가열단계를 거친 성형물을 소성하는 소성단계로 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법을 제공함에 의해 달성된다.An object of the present invention is to produce a mixture of mixing cordierite, walnut, graphite, binder, polyvinyl alcohol, triethylene glycol and lubricating oil, the molding step of molding the mixture through the mixture manufacturing step, the molding step It is achieved by providing a method for producing a diesel particle filter, characterized in that consisting of a heating step of heating the molded product produced through and a firing step of firing the molded product after the heating step.
본 발명의 바람직한 특징에 따르면, 상기 혼합물제조단계는 코디어라이트 100 중량부, 월넛 10 내지 20 중량부, 흑연 1 내지 2 중량부, 바인더 4 내지 6 중량부, 폴리비닐알코올 1 내지 2 중량부, 트리에틸렌글리콜 0.1 내지 1 중량부 및 윤활오일 0.1 내지 1 중량부를 혼합하여 이루어지는 것으로 한다.According to a preferred feature of the invention, the mixture manufacturing step is 100 parts by weight of cordierite, 10 to 20 parts by weight of walnut, 1 to 2 parts by weight of graphite, 4 to 6 parts by weight of binder, 1 to 2 parts by weight of polyvinyl alcohol, It is assumed that 0.1 to 1 part by weight of triethylene glycol and 0.1 to 1 part by weight of lubricating oil are mixed.
본 발명의 더 바람직한 특징에 따르면, 상기 성형단계는 상기 혼합물제조단계를 통해 혼합된 혼합물을 허니컴구조로 성형하여 이루어지는 것으로 한다.According to a more preferred feature of the invention, the molding step is to be made by molding the mixture mixed through the mixture manufacturing step in a honeycomb structure.
본 발명의 더욱 바람직한 특징에 따르면, 상기 가열단계는 상기 성형단계를 통해 제조된 성형물을 0.87 내지 3℃/min의 승온속도로 1350℃까지 가열하여 이루어지는 것으로 한다.According to a more preferred feature of the invention, the heating step is to be made by heating the molded product produced through the molding step to 1350 ℃ at a temperature increase rate of 0.87 to 3 ℃ / min.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 소성단계는 상기 가열단계를 거친 성형물을 1350 내지 1410℃의 온도로 14 내지 18시간 동안 소성하여 이루어지는 것으로 한다.According to a still more preferable feature of the present invention, the firing step is to be made by firing the molded product after the heating step for 14 to 18 hours at a temperature of 1350 to 1410 ℃.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 소성단계는 이산화탄소 또는 질소를 10L/min으로 주입하여 이루어지는 것으로 한다.
According to a further preferred feature of the invention, the firing step is to be made by injecting carbon dioxide or nitrogen at 10L / min.
또한, 본 발명의 목적은 디젤 입자 필터의 제조방법으로 제조되는 것을 특징으로 하는 디젤 입자 필터를 제공함에 의해서도 달성될 수 있다.
In addition, the object of the present invention can also be achieved by providing a diesel particle filter, characterized in that the manufacturing method of the diesel particle filter.
본 발명에 따른 디젤 입자 필터의 제조방법은 열팽창계수가 낮아 오랜 기간 고온의 배기가스를 여과하더라도, 균열 등과 같은 기계적 물성의 저하가 발생하지 않는 디젤 입자 필터를 제공하는 탁월한 효과를 나타낸다.The method for producing a diesel particulate filter according to the present invention exhibits an excellent effect of providing a diesel particulate filter having a low coefficient of thermal expansion and filtering of high temperature exhaust gas for a long time without deterioration of mechanical properties such as cracking.
또한, 기공의 크기 및 기공의 분포가 고르며, 기공 연결도가 높은 디젤 입자 필터를 제공하는 탁월한 효과를 나타낸다.
In addition, the pore size and pore distribution are uniform, and exhibits an excellent effect of providing a diesel particle filter having a high porosity connection.
도 1은 본 발명에 따른 디젤 입자 필터의 제조방법을 나타낸 순서도이다.
도 2는 본 발명의 실시예 1 및 비교예 1을 통해 제조된 디젤 입자 필터의 열팽창계수를 측정하여 나타낸 그래프이다.
도 3은 본 발명의 실시예 1 및 비교예 1을 통해 제조된 디젤 입자 필터의 표면을 SEM으로 촬영하여 나타낸 사진이다.
도 4는 본 발명의 실시예 1 내지 3을 통해 제조된 디젤 입자 필터의 표면을 SEM으로 촬영하여 나타낸 사진이다.1 is a flow chart illustrating a method of manufacturing a diesel particle filter according to the present invention.
Figure 2 is a graph showing the thermal expansion coefficient of the diesel particle filter manufactured in Example 1 and Comparative Example 1 of the present invention measured.
Figure 3 is a photograph taken by SEM the surface of the diesel particle filter prepared in Example 1 and Comparative Example 1 of the present invention.
Figure 4 is a photograph showing the SEM photograph of the surface of the diesel particle filter prepared in Examples 1 to 3 of the present invention.
이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.
Hereinafter, preferred embodiments of the present invention and physical properties of the respective components will be described in detail with reference to the accompanying drawings. However, the present invention is not limited thereto, And this does not mean that the technical idea and scope of the present invention are limited.
본 발명에 따른 디젤 입자 필터의 제조방법은 코디어라이트, 월넛, 흑연, 바인더, 폴리비닐알코올, 트리에틸렌글리콜 및 윤활오일을 혼합하는 혼합물제조단계(S101), 상기 혼합물제조단계(S101)를 통해 혼합된 혼합물을 성형하는 성형단계(S103), 상기 성형단계(S103)를 통해 제조된 성형물을 가열하는 가열단계(S105) 및 상기 가열단계(S105)를 거친 성형물을 소성하는 소성단계(S107)로 이루어진다.
Method for producing a diesel particle filter according to the present invention is through a mixture preparation step (S101), the mixture production step (S101) for mixing cordierite, walnut, graphite, binder, polyvinyl alcohol, triethylene glycol and lubricating oil Molding step (S103) for molding the mixed mixture, the heating step (S105) for heating the molded product produced through the molding step (S103) and the firing step (S107) for firing the molded product through the heating step (S105) Is done.
상기 혼합물제조단계(S101)는 코디어라이트, 월넛, 흑연, 바인더, 폴리비닐알코올, 트리에틸렌글리콜 및 윤활오일을 혼합하여 혼합물을 제조하는 단계로, 코디어라이트 100 중량부, 월넛 10 내지 20 중량부, 흑연 1 내지 2 중량부, 바인더 4 내지 6 중량부, 폴리비닐알코올 1 내지 2 중량부, 트리에틸렌글리콜 0.1 내지 1 중량부 및 윤활오일 0.1 내지 1 중량부를 혼합하여 이루어지는 것이 바람직하다.The mixture production step (S101) is a step of preparing a mixture by mixing cordierite, walnut, graphite, binder, polyvinyl alcohol, triethylene glycol and lubricating oil, 100 parts by weight of cordierite, 10 to 20 weight of walnut It is preferably made by mixing 1 to 2 parts by weight of graphite, 4 to 6 parts by weight of binder, 1 to 2 parts by weight of polyvinyl alcohol, 0.1 to 1 parts by weight of triethylene glycol and 0.1 to 1 parts by weight of lubricating oil.
상기 코디어라이트는 본 발명에 따른 디젤 입자 필터의 주재료로, 코디어라이트 재질의 디젤 입자 필터는 다른 재료로 이루어진 디젤 입자 필터에 비해 배압이 높기 때문에, 코디어라이트로 이루어진 디젤 입자 필터는 기공의 크기 및 분포를 고르게 하기 위해 배압을 낮출 필요성이 있다.The cordierite is the main material of the diesel particle filter according to the present invention, since the cordierite diesel particle filter has a higher back pressure than the diesel particle filter made of other materials, the diesel particle filter made of cordierite There is a need to lower the back pressure to even out the size and distribution.
일반적으로, 코디어라이트로 이루어진 디젤 입자 필터는 내부에 존재하는 기공은 5 내지 50㎛의 직경을 나타내며, 기공 연결도 낮기 때문에 배압특성이 우수하지 못한 문제점이 있다.In general, the diesel particle filter made of cordierite has a pore present within the diameter of 5 to 50㎛, because the pore connection is low, there is a problem that the back pressure characteristics are not excellent.
따라서, 상기의 문제점을 해결하기 위해, 상기 가열단계(S105)에서는 승온 속도를 0.87 내지 3℃/min로 조절하여 혼합물제조단계에서 혼합된 원료에 의하여 생성된 미세 기공과 기공형성제인 월넛 및 흑연에 의하여 형성된 거대기공을 균일화한다.Therefore, in order to solve the above problems, in the heating step (S105) by adjusting the temperature increase rate to 0.87 to 3 ℃ / min in the walnut and graphite which is a fine pore and pore-forming agent produced by the raw material mixed in the mixture manufacturing step To homogenize the formed macropores.
이때, 상기 바인더 성분은 물, 알코올, 아크릴 및 메틸셀룰로오스로 이루어진 그룹으로부터 선택된 하나로 이루어질 수 있으며, 메틸셀룰로오스로 이루어지는 것이 가장 바람직하다.At this time, the binder component may be made of one selected from the group consisting of water, alcohol, acryl and methyl cellulose, and most preferably made of methyl cellulose.
또한, 상기 혼합물은 혼합물 입경이 소결체의 밀도, 기계적 특성 등에 영향을 미치므로 이를 고려하여 분쇄공정을 통해 분말형태로 분쇄되는 분쇄공정을 거치는데, 분쇄공정은 볼 밀링(ball milling) 공정을 이용할 수 있는데, 볼 밀링 공정을 이용할 경우, 혼합분말을 볼 밀링기(ball milling machine)에 장입하고 일정 속도로 회전시켜 혼합분말을 기계적으로 분쇄하여 이루어진다.In addition, since the mixture particle diameter affects the density, mechanical properties, and the like of the sintered compact, the mixture undergoes a pulverization process in which it is pulverized into a powder form through a pulverization process. The pulverization process may use a ball milling process. In the case of using a ball milling process, the mixed powder is charged into a ball milling machine and rotated at a constant speed to mechanically crush the mixed powder.
볼 밀링에 사용되는 볼은 불순물의 생성을 억제하기 위하여 알루미나로 이루어진 세라믹 재질의 볼을 사용하는 것이 바람직하며, 볼은 모두 같은 크기의 것일 수도 있고 2가지 이상의 크기를 갖는 볼을 함께 사용할 수도 있다. 볼의 크기, 밀링 시간, 볼 밀링기의 분당 회전속도 등을 조절하여 목표하는 입자의 크기로 분쇄한다. In order to suppress the generation of impurities, the balls used for ball milling are preferably made of ceramic balls made of alumina, and the balls may be all of the same size or may have balls of two or more sizes. The size of the balls, the milling time, and the rotation speed per minute of the ball miller are adjusted so as to be crushed to the target particle size.
바람직하게는 분쇄되는 혼합물의 입자 크기를 고려하여 볼의 크기는 20 내지60밀리미터 정도의 범위로 설정하고, 볼 밀링기의 회전속도는 10 내지 300rpm의 범위로 설정할 수 있다. 볼 밀링 시간은 목표로 하는 입자의 크기 등을 고려하여 1 내지 24시간 동안 실시된다.Preferably, in consideration of the particle size of the mixture to be ground, the size of the ball may be set in the range of about 20 to 60 millimeters, and the rotational speed of the ball mill may be set in the range of 10 to 300 rpm. The ball milling time is carried out for 1 to 24 hours in consideration of the target particle size and the like.
볼 밀링에 의해 혼합분말은 미세한 크기의 입자로 분쇄되고, 균일한 입자 크기 분포를 갖게 된다.
By ball milling, the mixed powder is pulverized into fine-sized particles and has a uniform particle size distribution.
상기 성형단계(S103)는 상기 혼합물제조단계(S101)를 통해 혼합된 혼합물을 성형하는 단계로, 상기 혼합물제조단계(S101)를 통해 혼합된 혼합물을 허니컴구조로 성형하여 이루어지데, 이때, 허니컴구조로 성형된 성형물에 형성된 관통홀의 단면은 삼각형, 정사각형, 육각형 및 원형 등으로 이루어질 수 있다.The molding step (S103) is a step of molding the mixture mixed through the mixture manufacturing step (S101), and is made by molding the mixture mixed through the mixture manufacturing step (S101) into a honeycomb structure, in this case, the honeycomb structure The cross section of the through-hole formed in the molded article may be made of a triangle, a square, a hexagon and a circle.
이러한, 성형단계(S103)에서 상기 혼합물제조단계(S101)를 통해 혼합된 혼합물을 허니컴 구조로 성형하는 과정은, 특별히 한정된 성형방법이나 성형장치가 사용되는 것이 아니라, 공지된 성형방법 및 성형장치를 사용할 수 있으며, 허니컴 구조를 갖는 성형물의 내벽 두께는 디젤입자필터를 정화하기에 가장 적합한 100 내지 400 밀리미터를 갖도록 성형되는 것이 바람직하다.
In the molding step (S103), the process of molding the mixture mixed through the mixture manufacturing step (S101) into a honeycomb structure is not a specially limited molding method or a molding apparatus, but a known molding method and a molding apparatus. It is possible to use, and the inner wall thickness of the molding having a honeycomb structure is preferably molded to have a 100 to 400 millimeters most suitable for purifying the diesel particle filter.
상기 가열단계(S105)는 상기 성형단계(S103)를 통해 제조된 성형물을 가열하는 단계로, 상기 성형단계(S103)를 통해 제조된 성형물을 0.87 내지 3℃/min의 승온 속도로 1350℃까지 가열하여 이루어지데, 이러한 가열단계(S105)를 통해 성형물의 표면에 형성된 거대 기공이 미세하고, 일정한 범위의 직경을 갖는 기공으로 균일화된다.The heating step (S105) is a step of heating the molded product produced by the molding step (S103), heating the molded product produced by the molding step (S103) to 1350 ℃ at an elevated temperature rate of 0.87 to 3 ℃ / min It is made, through the heating step (S105) through the large pores formed on the surface of the molding is fine, uniform to the pores having a certain range of diameter.
상기 가열단계(S105)는 전기로, 벽돌로 및 가스로로 이루어진 그룹으로부터 선택된 하나의 로에서 이루어지는 것이 바람직하며, 승온 온도가 0.87℃/min인 가스로에서 이루어지는 것이 가장 바람직하다.
The heating step (S105) is preferably made in one furnace selected from the group consisting of an electric furnace, a brick furnace and a gas furnace, most preferably in a gas furnace having a temperature rising temperature of 0.87 ° C / min.
상기 소성단계(S107)는 상기 가열단계(S105)를 거친 성형물을 소성하는 단계로, 상기 가열단계(S105)를 거친 성형물을 1350 내지 1410℃의 온도에서 14 내지 18시간 동안 소성하여 이루어지데, 이때, 소성단계는 공기(Air) 분위기가 아니라, 이산화탄소 또는 질소를 10L/min으로 주입하여 로 내에 산소의 농도가 낮아진 이산화탄소 또는 질소분위기에서 이루어진다.The firing step (S107) is a step of firing the molded product through the heating step (S105), it is made by firing the molded product through the heating step (S105) for 14 to 18 hours at a temperature of 1350 to 1410 ℃, wherein , The firing step is performed in a carbon dioxide or nitrogen atmosphere in which the concentration of oxygen in the furnace is lowered by injecting carbon dioxide or nitrogen at 10 L / min, not an air atmosphere.
산소의 농도가 낮아진 이산화탄소 또는 질소분위기에서 소성된 디젤 입자 필터는 열팽창 계수가 매우 낮은 특성을 나타낸다.
Diesel particle filters fired in a carbon dioxide or nitrogen atmosphere with low oxygen concentrations exhibit very low thermal expansion coefficients.
상기의 혼합물제조단계(S101), 성형단계(S103), 가열단계(S105) 및 소성단계(S107)를 거치면, 열팽창계수가 낮아 오랜 기간 고온의 배기가스를 여과하더라도, 균열 등과 같은 기계적 물성의 저하가 발생하지 않고, 기공의 크기 및 기공의 분포가 고르며, 기공 연결도가 높은 디젤 입자 필터가 제조된다.
When the mixture preparation step (S101), forming step (S103), heating step (S105) and firing step (S107) of the mixture, the thermal expansion coefficient is low, even if the high-temperature exhaust gas is filtered for a long time, mechanical properties such as cracks, etc. Does not occur, the pore size and pore distribution is uniform, and a diesel particle filter having a high porosity is produced.
이하에서는, 본 발명에 따른 디젤 입자 필터의 제조방법 및 그 제조방법을 통해 제조된 디젤 입자 필터의 물성을 실시예를 들어 설명한다.
Hereinafter, the physical properties of the diesel particle filter prepared by the method and the method for producing the diesel particle filter according to the present invention will be described with reference to Examples.
<실시예 1>≪ Example 1 >
코디어라이트 100 중량부, 월넛 15 중량부, 흑연 1.5 중량부, 메틸셀룰로오스 5 중량부, 폴리비닐알코올 1.5 중량부, 트리에틸렌글리콜 0.6 중량부 및 윤활오일 0.6 중량부를 혼합하여 혼합물을 제조하고, 제조된 혼합물을 허니컴구조를 갖는 성형물로 성형하고, 허니컴구조로 성형된 성형물을 전기로에 투입하여 3℃/min의 승온 속도로 1350℃까지 가열하고, 1350℃로 가열된 성형물이 투입된 전기로에 질소를 10L/min으로 주입하면서 성형물을 1410℃의 온도로 16시간 동안 소성하여 디젤 입자 필터(Φ10.5인치/200셀, 두께 100밀리미터)를 제조하였다.
A mixture was prepared by mixing 100 parts by weight of cordierite, 15 parts by weight of walnut, 1.5 parts by weight of graphite, 5 parts by weight of methyl cellulose, 1.5 parts by weight of polyvinyl alcohol, 0.6 parts by weight of triethylene glycol, and 0.6 parts by weight of lubricating oil. The formed mixture into a molded article having a honeycomb structure, and a molded article formed into a honeycomb structure was put into an electric furnace, heated to 1350 ° C. at a heating rate of 3 ° C./min, and 10 L of nitrogen was added to the electric furnace into which the molded product heated to 1350 ° C. was put. The molding was fired at a temperature of 1410 ° C. for 16 hours while injecting at / min to prepare a diesel particle filter (Φ10.5 inch / 200 cells, thickness 100 millimeters).
<실시예 2><Example 2>
상기 실시예 1과 동일하게 진행하되, 전기로 대신 승온속도가 1.8℃/min인 벽돌로를 사용하여 디젤 입자 필터(Φ10.5인치/200셀, 두께 100밀리미터)를 제조하였다.
Proceed in the same manner as in Example 1, using a brick furnace having a heating rate of 1.8 ℃ / min instead of an electric furnace to prepare a diesel particle filter (Φ 10.5 inches / 200 cells, thickness 100mm).
<실시예 3><Example 3>
상기 실시예 1과 동일하게 진행하되, 전기로 대신 승온속도가 0.87℃/min인 가스로를 사용하여 디젤 입자 필터(Φ10.5인치/200셀, 두께 100밀리미터)를 제조하였다.
Proceed in the same manner as in Example 1, a diesel particle filter (Φ 10.5 inches / 200 cells, thickness 100mm) using a gas furnace having a temperature rising rate of 0.87 ℃ / min instead of an electric furnace.
<비교예 1>≪ Comparative Example 1 &
상기 실시예 1과 동일하게 진행하되, 질소를 주입하지 않고, 공기 분위기에서 소성과정을 진행하여 디젤 입자 필터(Φ10.5인치/200셀, 두께 100밀리미터)를 제조하였다.
Proceed in the same manner as in Example 1, without the injection of nitrogen, the firing process in the air atmosphere to prepare a diesel particle filter (Φ 10.5 inches / 200 cells, thickness 100mm).
상기 실시예 1 및 비교예 1을 통해 제조된 디젤 입자 필터의 밀도, 기공율, 흡수율, 열팽창계수 및 연화점을 측정하여 아래 표 1 및 도 2에 나타내었다.The density, porosity, water absorption, coefficient of thermal expansion, and softening point of the diesel particulate filter prepared through Example 1 and Comparative Example 1 were measured and shown in Table 1 and FIG. 2 below.
{단, 밀도와 흡수율은 아르키메데스법을 이용하여 측정하였으며, 기공율은 수은압입법(Mercury Porosimeter)으로 측정하였으며, 열팽창계수와 연화점은 열팽창계수측정기(Dilatometer)를 사용하여 측정하였다.}
{However, the density and the water absorption were measured using the Archimedes method, the porosity was measured by the Mercury Porosimeter, and the coefficient of thermal expansion and softening point were measured using a Dilatometer.}
<표 1>TABLE 1
위에 표 1 및 아래 도 2에 나타낸 것처럼 본 발명의 실시예 1을 통해 제조된 디젤 입자 필터는 열팽창계수가 비교예 1을 통해 제조된 디젤 입자 필터에 비해 월등하게 낮아진 것을 알 수 있다.As shown in Table 1 above and Figure 2 below, it can be seen that the diesel particle filter manufactured through Example 1 of the present invention is significantly lower than the diesel particle filter prepared through Comparative Example 1.
또한, 기공율과 흡수율은 소성시에 산소 농도와는 무관한 것을 알 수 있다.In addition, it can be seen that the porosity and the water absorption rate are independent of the oxygen concentration at the time of firing.
또한, 실시예 1 및 비교예 1을 통해 제조된 디젤 입자 필터의 표면을 SEM으로 촬영하여 아래 도 3에 나타내었다.In addition, the surface of the diesel particle filter prepared in Example 1 and Comparative Example 1 was taken by SEM and shown in Figure 3 below.
아래 도 3에 나타낸 것처럼 SEM을 통해 기공의 미세구조를 촬영한 결과 소성시의 산소 농도와 미세구조는 무관한 것을 알 수 있다.
As shown in FIG. 3 below, when the microstructure of the pores was photographed through the SEM, it can be seen that the oxygen concentration and the microstructure during firing are irrelevant.
또한, 상기 실시예 1 내지 3을 통해 제조된 디젤 입자 필터의 표면을 SEM으로 촬영하여 아래 도 4에 나타내었다.In addition, the surface of the diesel particle filter prepared in Examples 1 to 3 was taken in SEM is shown in Figure 4 below.
아래 도 4에 나타낸 것처럼 가열단계에서 승온 조건에 따라 기공의 미세구조가 변하는 것을 알 수 있으며, 승온 온도가 가장 낮은 가스로를 사용하였을 때, 가장 미세하고 고른 미세기공이 형성되는 것을 알 수 있다.
As shown in FIG. 4, it can be seen that the microstructure of the pores is changed depending on the temperature raising conditions in the heating step, and when the gas furnace having the lowest temperature is used, the finest and evenest micropores are formed.
S101 ; 혼합물제조단계
S103 ; 성형단계
S105 ; 가열단계
S107 ; 소성단계S101; Mixture manufacturing step
S103; Molding step
S105; Heating step
S107; Firing step
Claims (7)
상기 혼합물제조단계에서 혼합된 혼합물을 성형하는 성형단계;
상기 성형단계를 통해 제조된 성형물을 가열하는 가열단계; 및
상기 가열단계를 거친 성형물을 소성하는 소성단계;로 이루어지며,
상기 소성단계의 소성은 이산화탄소 또는 질소를 주입하여 이산화탄소 또는 질소분위기하에서 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법.
100 parts by weight of cordierite, 10 to 20 parts by weight of walnut, 1 to 2 parts by weight of graphite, 4 to 6 parts by weight of binder, 1 to 2 parts by weight of polyvinyl alcohol, 0.1 to 1 parts by weight of triethylene glycol, and 0.1 to 1 part by weight of lubricating oil. Mixing step of mixing 1 part by weight;
A molding step of molding the mixture mixed in the mixture manufacturing step;
A heating step of heating the molded product manufactured through the molding step; And
It consists of a firing step of firing the molded product after the heating step,
The firing of the firing step is a method for producing a diesel particle filter, characterized in that the injection of carbon dioxide or nitrogen is made under a carbon dioxide or nitrogen atmosphere.
상기 성형단계는 상기 혼합물제조단계를 통해 혼합된 혼합물을 허니컴구조로 성형하여 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법.
The method according to claim 1,
The molding step is a method for producing a diesel particle filter, characterized in that formed by the honeycomb structure of the mixture mixed through the mixture manufacturing step.
상기 가열단계는 상기 성형단계를 통해 제조된 성형물을 0.87 내지 3℃/min의 승온속도로 1350℃까지 가열하여 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법.
The method according to claim 1,
The heating step is a method for producing a diesel particle filter, characterized in that by heating the molded product produced through the forming step to 1350 ℃ at a temperature increase rate of 0.87 to 3 ℃ / min.
상기 소성단계는 상기 가열단계를 거친 성형물을 1350 내지 1410℃의 온도로 14 내지 18시간 동안 소성하여 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법.
The method according to claim 1,
The firing step is a method for producing a diesel particle filter, characterized in that by firing the molded product after the heating step for 14 to 18 hours at a temperature of 1350 to 1410 ℃.
상기 이산화탄소 또는 질소 주입은 10L/min으로 주입하여 이루어지는 것을 특징으로 하는 디젤 입자 필터의 제조방법.
The method according to claim 1,
The carbon dioxide or nitrogen injection is a method for producing a diesel particle filter, characterized in that the injection is made at 10L / min.
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| KR1020120036723A KR101351468B1 (en) | 2012-04-09 | 2012-04-09 | Manufacturing method of diesel particulate filter and diesel particulate filter manufactured by the method |
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| KR1020120036723A KR101351468B1 (en) | 2012-04-09 | 2012-04-09 | Manufacturing method of diesel particulate filter and diesel particulate filter manufactured by the method |
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| KR20130114400A KR20130114400A (en) | 2013-10-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200057462A (en) * | 2018-11-16 | 2020-05-26 | (주) 세라컴 | Manufacturing method of diesel particulate filter with an improved thermal expansion coefficient and diesel particulate filter manufactured by the method |
| KR20210054404A (en) | 2019-11-05 | 2021-05-13 | (주) 세라컴 | Resin composition for diesel particulate filter having excellent extrusion property and shape retention and diesel particulate filter comprising the same |
| KR102325976B1 (en) | 2020-10-16 | 2021-11-15 | (주) 세라컴 | Filter coating composition for fine dust reduction, fine dust reduction filter and manufacturing method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102024115B1 (en) * | 2018-02-06 | 2019-09-23 | (주) 세라컴 | Method for making diesel particulate filter having low thermal expansion coefficient and diesel particulate filter comprising the same |
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| KR20020082211A (en) * | 2000-11-24 | 2002-10-30 | 니뽄 가이시 가부시키가이샤 | Porous honeycomb filter and method for manufacture thereof |
| WO2007102561A1 (en) | 2006-03-07 | 2007-09-13 | Ngk Insulators, Ltd. | Ceramic structure and process for producing the same |
| KR20110048506A (en) * | 2008-07-28 | 2011-05-11 | 히타치 긴조쿠 가부시키가이샤 | Ceramic honeycomb structure and its manufacturing method |
| JP2011194346A (en) | 2010-03-23 | 2011-10-06 | Ngk Insulators Ltd | Filter and method for manufacturing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020082211A (en) * | 2000-11-24 | 2002-10-30 | 니뽄 가이시 가부시키가이샤 | Porous honeycomb filter and method for manufacture thereof |
| WO2007102561A1 (en) | 2006-03-07 | 2007-09-13 | Ngk Insulators, Ltd. | Ceramic structure and process for producing the same |
| KR20110048506A (en) * | 2008-07-28 | 2011-05-11 | 히타치 긴조쿠 가부시키가이샤 | Ceramic honeycomb structure and its manufacturing method |
| JP2011194346A (en) | 2010-03-23 | 2011-10-06 | Ngk Insulators Ltd | Filter and method for manufacturing the same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200057462A (en) * | 2018-11-16 | 2020-05-26 | (주) 세라컴 | Manufacturing method of diesel particulate filter with an improved thermal expansion coefficient and diesel particulate filter manufactured by the method |
| KR102199010B1 (en) * | 2018-11-16 | 2021-01-07 | (주) 세라컴 | Manufacturing method of diesel particulate filter with an improved thermal expansion coefficient and diesel particulate filter manufactured by the method |
| KR20210054404A (en) | 2019-11-05 | 2021-05-13 | (주) 세라컴 | Resin composition for diesel particulate filter having excellent extrusion property and shape retention and diesel particulate filter comprising the same |
| KR102325976B1 (en) | 2020-10-16 | 2021-11-15 | (주) 세라컴 | Filter coating composition for fine dust reduction, fine dust reduction filter and manufacturing method thereof |
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| KR20130114400A (en) | 2013-10-17 |
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