KR100661638B1 - Method for preparing catalyst carrier by extrusion molding - Google Patents
Method for preparing catalyst carrier by extrusion molding Download PDFInfo
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- KR100661638B1 KR100661638B1 KR1020050076037A KR20050076037A KR100661638B1 KR 100661638 B1 KR100661638 B1 KR 100661638B1 KR 1020050076037 A KR1020050076037 A KR 1020050076037A KR 20050076037 A KR20050076037 A KR 20050076037A KR 100661638 B1 KR100661638 B1 KR 100661638B1
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- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000001125 extrusion Methods 0.000 title claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 239000007787 solid Substances 0.000 claims abstract description 15
- 239000008247 solid mixture Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 22
- 239000011230 binding agent Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 4
- 239000004927 clay Substances 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 4
- 239000010457 zeolite Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 3
- 229920000609 methyl cellulose Polymers 0.000 claims description 3
- 239000001923 methylcellulose Substances 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 239000000969 carrier Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 125000000914 phenoxymethylpenicillanyl group Chemical group CC1(S[C@H]2N([C@H]1C(=O)*)C([C@H]2NC(COC2=CC=CC=C2)=O)=O)C 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
본 발명은 압출성형에 의한 촉매담체의 제조 방법에 관한 것으로서, 특정 조건하에서 고체 성분 혼합과 액체 성분 혼합을 별도로 수행한 후 고체 혼합물에 액체 혼합물을 첨가하는 방식으로 균질한 조성의 촉매담체 조성물을 수득한 후, 이를 압출성형, 건조 및 열처리시키는 본 발명에 따르면, 균일한 외관을 갖는 촉매담체 압출성형품을 제조할 수 있다.The present invention relates to a method for preparing a catalyst carrier by extrusion molding, wherein the catalyst carrier composition having a homogeneous composition is obtained by separately performing the solid component mixing and the liquid component mixing under specific conditions and then adding the liquid mixture to the solid mixture. Then, according to the present invention by extrusion molding, drying and heat treatment, it is possible to produce a catalyst carrier extruded article having a uniform appearance.
Description
도 1은 본 발명에 따른 촉매담체의 제조 방법에 있어서 원료 조성물의 혼합 공정의 일예를 나타낸 것이고,Figure 1 shows an example of the mixing process of the raw material composition in the method for producing a catalyst carrier according to the present invention,
도 2a 및 2b는 본 발명의 공정에 사용되는 혼합기들의 예를 나타낸 것이며,2A and 2B show examples of mixers used in the process of the present invention,
도 3a 및 3b는 각각 본 발명의 실시예 1 및 비교예 1에 따라 제조된 촉매담체의 외관 사진을 나타낸 것이다.Figure 3a and 3b shows an external photograph of the catalyst carrier prepared according to Example 1 and Comparative Example 1 of the present invention, respectively.
본 발명은 촉매담체의 제조방법에 관한 것으로서, 구체적으로는 원료 조성물을 균일하게 혼합시킴으로써 고품질의 압출성형품을 제조하기 위한 방법에 관한 것이다.The present invention relates to a method for producing a catalyst carrier, and more particularly, to a method for producing a high quality extruded article by uniformly mixing the raw material composition.
제올라이트 허니컴 구조체 등과 같은 촉매담체 압출성형품은 통상적으로 촉매, 무기 또는 유기 결합제 및 기타 첨가제의 혼합, 혼련, 압출성형, 건조 및 열처 리의 단계들을 거쳐 제조되고 있으며, 최종 생성물의 물성을 제어하기 위한 기술 중 하나는 사용되는 물질들의 혼합 공정을 개선하는 것이다.Catalyst carrier extruded articles, such as zeolite honeycomb structures and the like, are typically manufactured through the steps of mixing, kneading, extruding, drying, and heat treating a catalyst, an inorganic or organic binder, and other additives. One is to improve the mixing process of the materials used.
압출성형품을 제조하기 위한 원료의 혼합방식으로는 자연적 혼합방식과 강제적 혼합방식이 있는데, 전자의 경우 혼합시간의 장기화 및 혼합성이 불충분한 문제점이 있으므로 주로 특정의 수단을 이용하는 강제적 혼합방식이 이용되고 있다.The mixing method of the raw materials for producing the extruded article is a natural mixing method and a compulsory mixing method. In the former case, the forced mixing method using a specific means is mainly used because of the problem of prolonged mixing time and insufficient mixing. have.
예를 들어, 한국 특허출원공고 제1993-6206호에서는 사용 물질들을 압출성형기에 공급하여 혼합한 다음, 탈기 후 다이를 통해 압출성형하여 세라믹 성형품을 제조하는 방법이 개시되어 있다.For example, Korean Patent Application Publication No. 1993-6206 discloses a method of manufacturing a ceramic molded article by supplying and mixing materials to be used in an extruder and then extruding through a die after degassing.
그러나, 원료들을 동시에 압출성형기에 공급하여 혼합을 수행하는 경우에는 미처 혼합되지 않은 원료가 성형기 내부에서 잔존하였다가 그대로 다이로 이송됨에 따라 원활하지 못한 배토(원료 조성물)의 흐름을 유도하여 최종 성형물의 외형 불량을 초래하기 쉽다.However, in the case where mixing is carried out by simultaneously supplying the raw materials to the extruder, the unmixed raw material remains inside the molding machine and is transferred to the die, thereby inducing a flow of unsoiled soil (raw material composition), resulting in the final molding. It is easy to cause appearance defects.
또한, 한국 특허출원공고 제1995-1384호 및 1995-4143호에 개시된 물질 혼합 방법을 이용하는 경우에도 원료 성분들의 입경 및 비중차에 의해 재분리 현상이 일어났으며, 원료의 혼합 과정중에 발생하는 원심력, 전단력 등 혼합 물질에 가해지는 기계적 외력에 의해 최종 물성이 저해되어 만족할만한 품질의 성형물을 얻지 못했을 뿐만 아니라 혼합시간 또한 길었다.In addition, in the case of using the material mixing method disclosed in Korean Patent Application Publication Nos. 1995-1384 and 1995-4143, re-separation phenomenon occurred due to particle size and specific gravity difference of raw material components, and centrifugal force generated during mixing of raw materials. The final physical properties were impaired by the mechanical external force applied to the mixed materials such as the shear force and shear force, which resulted in not only satisfactory moldings but also a long mixing time.
이에, 본 발명자들은 원료 성분들의 입경 및 비중차를 근본적으로 극복하여 원료들의 혼합도를 개선할 수 있는 방법을 예의 연구한 결과, 원료 중의 고체 성분들과 액체 성분들을 분리하여 각각을 먼저 혼합한 후 얻어진 각 혼합물을 합쳐 다 시 혼합하는 경우, 한번에 모든 성분들을 혼합했을 때 보다 단시간에 혼합공정을 수행하여 최종 성형물의 외형 불량을 현저히 감소시킬 수 있음을 발견하고 본 발명을 완성하게 되었다.Therefore, the present inventors have diligently studied how to improve the mixing of the raw materials by fundamentally overcoming the particle size and specific gravity difference of the raw material components, after separating the solid components and liquid components in the raw materials and mixing each first When the obtained mixtures were combined and mixed again, the present invention was found to be able to significantly reduce the appearance defect of the final molding by performing the mixing process in a shorter time than when all the components were mixed at once.
본 발명의 목적은 압출성형에 의한 촉매담체의 제조에 있어서 원료의 혼합도를 개선시킴으로써 최종 제품의 품질을 향상시키기 위한 방법을 제공하는 것이다.It is an object of the present invention to provide a method for improving the quality of the final product by improving the mixing of raw materials in the production of catalyst carriers by extrusion molding.
상기의 목적을 달성하기 위해, 본 발명에서는 In order to achieve the above object, in the present invention
(1) 0.1 내지 10㎛ 범위의 평균 입경을 갖는 촉매 물질 및 10 내지 100㎛ 범위의 평균 입경을 갖는 고상의 무기 또는 유기 결합제를 포함하는 고체 원료 성분들을 혼합하여 고체 혼합물을 제조하고,(1) preparing a solid mixture by mixing solid raw materials comprising a catalyst material having an average particle diameter in the range of 0.1 to 10 μm and a solid inorganic or organic binder having an average particle diameter in the range of 10 to 100 μm,
(2) 용매, 액상의 무기 또는 유기 결합제 및 나머지 액상 첨가제를 포함하는 액체 원료 성분들을 혼합하여 액체 혼합물을 제조하고,(2) preparing a liquid mixture by mixing a liquid raw material component comprising a solvent, a liquid inorganic or organic binder, and the remaining liquid additive,
(3) 상기 고체 혼합물에 상기 액체 혼합물을 투입 혼합하여 촉매담체 조성물을 수득한 후, 이를 압출성형, 건조 및 열처리시키는 것을 포함하는, 촉매담체의 제조방법을 제공한다.(3) After the liquid mixture is added and mixed to the solid mixture to obtain a catalyst carrier composition, the present invention provides a method for preparing a catalyst carrier, which comprises extrusion molding, drying and heat treatment.
이하, 본 발명을 첨부된 도면을 참조로 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail with reference to the accompanying drawings.
촉매담체 조성물은 통상 주원료인 촉매 성분과 부원료인 무기 결합제를 주성 분으로 하여, 기타 첨가제로서 결합력을 향상시키기 위한 유기 결합제, 윤활성과 성형성을 부여하기 위한 가소제, 윤활제, 용매로서의 증류수 등을 첨가함으로써 제조될 수 있다. The catalyst carrier composition usually contains a catalyst component as a main raw material and an inorganic binder as a subsidiary ingredient, and by adding an organic binder for improving binding strength as another additive, a plasticizer for imparting lubricity and formability, a lubricant, distilled water as a solvent, and the like. Can be prepared.
본 발명은 이러한 촉매담체 조성물을 제조하는데 있어서, 도 1에 개략적으로 나타낸 바와 같이, 원료들을 고체 성분과 액체 성분으로 분리하여 미리 별도로 혼합한 후 이들을 합쳐 다시 혼합하여 원료 조성물인 배토를 수득하는 것을 특징으로 한다.In the present invention, in the preparation of such a catalyst carrier composition, as shown schematically in FIG. 1, raw materials are separated into solid and liquid components, previously mixed separately, and then combined and mixed again to obtain clay, which is a raw material composition. It is done.
구체적으로, 본 발명에서는 먼저 일정 크기의 분말 상태로 제어된 고체 성분, 즉 0.5 내지 10㎛ 범위의 평균 입경을 갖는 촉매 물질 및 10 내지 100㎛ 범위의 평균 입경을 갖는 무기 또는 유기 결합제를, 도 2a에 도시된 바와 같이 로터와 팬이 구비된 혼합기에 넣고 혼합한다. 이때, 상기 로터 및 팬의 회전속도는 특별히 제한되는 것은 아니지만, 로터의 회전 속도는 100 내지 500 rpm, 바람직하게는 150 내지 400 rpm, 팬의 회전 속도는 50 내지 200rpm, 바람직하게는 100 내지 150 rpm으로 설정하되, 회전 방향을 반대로 하여 1 내지 5분, 바람직하게는 2 내지 3분동안 혼합을 수행할 수 있다. 본 발명에서, 상기와 같은 크기로 제어된 고체 성분을 사용하는 이유는 최밀충전 상태의 입도분포를 조성하여 비표면적을 증대시킴으로써 성형성 및 강도를 향상시키기 위함이다.Specifically, in the present invention, first, a solid component controlled in a powder state of a predetermined size, that is, a catalyst material having an average particle diameter in the range of 0.5 to 10 μm and an inorganic or organic binder having an average particle diameter in the range of 10 to 100 μm, is illustrated in FIG. 2A. As shown in the rotor and a pan equipped with a mixer and mix. At this time, the rotational speed of the rotor and fan is not particularly limited, the rotational speed of the rotor is 100 to 500 rpm, preferably 150 to 400 rpm, the rotational speed of the fan is 50 to 200 rpm, preferably 100 to 150 rpm It is set to, but mixing can be performed for 1 to 5 minutes, preferably 2 to 3 minutes in the reverse direction of rotation. In the present invention, the reason for using the solid component controlled to the above size is to improve the moldability and strength by forming a particle size distribution in the state of closest filling to increase the specific surface area.
한편, 조성물을 구성하는 액체 성분인 액상의 무기 또는 유기 결합제, 용매(예: 증류수), 가소제, 윤활제, 및 임의의 기타 액상 첨가제는, 도 2b에 도시된 바와 같이 회전 모터 및 임펠라가 구비되어 액체에 회전력을 전달하여 균일한 혼합을 유도하는 혼합기에서 30 내지 150rpm, 바람직하게는 50 내지 100 rpm의 속도로 1 내지 5분, 바람직하게는 2 내지 3분 동안 혼합할 수 있다.On the other hand, liquid inorganic or organic binders, solvents (e.g., distilled water), plasticizers, lubricants, and any other liquid additives, which are the liquid components constituting the composition, are equipped with a rotary motor and an impeller as shown in FIG. Mixing may be performed for 1 to 5 minutes, preferably 2 to 3 minutes at a speed of 30 to 150 rpm, preferably 50 to 100 rpm in a mixer that transmits rotational force to induce uniform mixing.
다음, 분말상의 고체 혼합물에 별도로 제조한 액체 혼합물을 0.5 내지 3ℓ/분의 유량으로 투입하여 습식 혼합을 수행함으로써 촉매담체 조성물을 수득한다. 이때, 혼합기의 로터 회전속도는 200 내지 500rpm, 바람직하게는 300 내지 400 rpm, 팬의 회전 속도는 로터 회전방향과 반대방향으로 50 내지 200 rpm, 바람직하게는 100 내지 150 rpm으로 설정하여 1 내지 5분, 바람직하게는 3 내지 5분 동안 혼합을 수행할 수 있다. Next, a separately prepared liquid mixture is added to a powdery solid mixture at a flow rate of 0.5 to 3 l / min to perform wet mixing to obtain a catalyst carrier composition. At this time, the rotor rotation speed of the mixer is 200 to 500rpm, preferably 300 to 400 rpm, the rotation speed of the fan is set to 50 to 200 rpm, preferably 100 to 150 rpm in the opposite direction to the rotor rotation direction 1 to 5 Mixing can be carried out for minutes, preferably for 3 to 5 minutes.
한편, 상기 액체 혼합물의 유량이 0.5ℓ/분 미만인 경우에는 혼합시간이 길어져 성분들의 재분리 현상이 발생할 수 있으며, 3ℓ/분을 초과하는 경우에는 액상의 과다투입으로 인해 고체 혼합물과 액체 혼합물이 혼합되기 전에 국부적인 뭉침현상이 발생하여 혼합도에 불리한 영향을 미친다.On the other hand, when the flow rate of the liquid mixture is less than 0.5l / min, the mixing time is long, re-separation of the components may occur, and when the liquid mixture exceeds 3l / min due to the over-injection of the liquid mixture of the solid mixture and the liquid mixture Local agglomeration occurs before this can adversely affect mixing.
이어서, 수득된 촉매담체 조성물을 통상적인 방법으로 압출기를 이용한 압출성형, 건조 및 열처리시킴으로써 촉매담체를 제조한다. 이때, 건조는 25 내지 100℃에서 100시간 동안 수행될 수 있으며, 열처리는 400 내지 700℃에서 5시간 동안 수행될 수 있다.The catalyst carrier is then prepared by extrusion molding, drying and heat treatment using an extruder in a conventional manner. At this time, drying may be performed at 25 to 100 ° C. for 100 hours, and heat treatment may be performed at 400 to 700 ° C. for 5 hours.
이와 같이, 원료의 고상 혼합과 액상 혼합을 별도로 수행하여 촉매담체 조성물을 제조하는 경우, 고체 성분 및 액체 성분 각각의 혼합도를 일차적으로 증가시킴으로써 각각의 혼합물을 추후 합치더라도 성분들의 입경 및 비중차에 따른 분리현상이 감소됨에 따라, 약 10분 내외의 짧은 원료 혼합시간에도 불구하고 균질한 상태의 조성물을 제조할 수 있으며, 이러한 균질 조성물을 압출성형하게 되면 기존의 압출성형기를 이용한 혼합 방식에서 미처 혼합되지 못한 원료가 압출성형기내에 잔존함에 따라 발생되는 최종 성형물의 불량 원인들을 해소할 수 있다.As such, in the case of preparing the catalyst carrier composition by separately performing solid phase mixing and liquid phase mixing of raw materials, the mixing ratios of the solid and liquid components are increased first, so that even if the respective mixtures are later combined, As the separation phenomenon is reduced, the composition can be prepared in a homogeneous state despite a short raw material mixing time of about 10 minutes, and when the homogeneous composition is extruded, it is mixed in a conventional mixing method using an extruder. It is possible to solve the causes of failure of the final molding caused by the raw material remaining in the extrusion machine.
본 발명에서, 촉매 물질로는 다양한 분야에서 촉매담체로 사용되는 여러 가지 세라믹 물질이 사용될 수 있으며, 그 중에서도 제올라이트 및 이산화티탄이 본 발명의 방법에 적합하다.In the present invention, as the catalyst material, various ceramic materials used as catalyst carriers in various fields may be used, among which zeolite and titanium dioxide are suitable for the method of the present invention.
고상 무기 결합제로는 세라믹계 촉매담체 조성물에 통상적으로 사용되는 점토, 벤토나이트 등이 촉매 물질 100 중량％를 기준으로 20 내지 40 중량％의 함량으로 사용될 수 있으며, 고상 유기 결합제로는 메틸셀룰로오스와 같은 셀룰로오스계 화합물, 폴리비닐알콜, 전분 등이 촉매 물질 100 중량％를 기준으로 1 내지 5 중량％의 함량으로 사용될 수 있다.As the solid inorganic binder, clay, bentonite, and the like, which are commonly used in ceramic catalyst carrier compositions, may be used in an amount of 20 to 40 wt% based on 100 wt% of the catalyst material, and as the solid organic binder, cellulose such as methyl cellulose may be used. System compounds, polyvinyl alcohol, starch and the like can be used in an amount of 1 to 5% by weight based on 100% by weight of the catalyst material.
액상의 무기 결합제로는 실리카 졸, 알루미나 졸 등을, 액상의 유기 결합제로는 에틸렌글리콜, 트리에틸렌글리콜 등이 촉매 물질 100 중량％를 기준으로 2 내지 4 중량％의 함량으로 사용될 수 있다.As a liquid inorganic binder, silica sol, alumina sol, and the like, and as a liquid organic binder, ethylene glycol, triethylene glycol, and the like may be used in an amount of 2 to 4 wt% based on 100 wt% of the catalyst material.
용매로서 사용되는 증류수는 다른 성분들의 균일한 혼련을 위한 것으로서, 촉매 물질 100 중량％를 기준으로 15 내지 20 중량％의 함량으로 사용될 수 있다.Distilled water used as the solvent is for uniform kneading of the other components, it may be used in an amount of 15 to 20% by weight based on 100% by weight of the catalyst material.
또한, 본 발명에서 가소제로는 글리세린, 에틸렌글리콜 등을, 윤활제로는 스테아린산, 왁스에멀젼, 폴리에틸렌글리콜 등을 사용할 수 있으며, 이외에도 압출성형용 조성물에 통상적으로 첨가되는 기타 첨가제들이 사용될 수 있다.In addition, glycerin, ethylene glycol, and the like may be used as the plasticizer in the present invention, and stearic acid, wax emulsion, polyethylene glycol, etc. may be used as the lubricant, and other additives commonly added to the composition for extrusion molding may be used.
이하에서는 본 발명의 실시예들을 통하여 본 발명을 보다 구체적으로 설명하 나, 본 발명이 이에 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail through embodiments of the present invention, but the present invention is not limited thereto.
압출성형용 촉매담체 조성물의 제조Preparation of Extrusion Molding Catalyst Carrier Composition
실시예 1Example 1
도 2에 도시된 바와 같이 로터와 팬이 반대로 회전하는 혼합기에서, 평균 입경 약 5 ㎛의 천연 제올라이트, 평균 입경 약 50 ㎛의 점토 및 평균 입경 약 50 ㎛의 메틸셀룰로오스를 100:32:3의 중량비로 넣은 후, 혼합기의 로터 회전속도를 300 rpm, 팬의 회전 속도를 120 rpm으로 설정하여 약 2분 동안 혼합기를 작동시켜 고상 혼합물을 수득하였다.As shown in FIG. 2, in a mixer in which the rotor and the fan rotate in opposite directions, a natural zeolite having an average particle diameter of about 5 μm, clay having an average particle diameter of about 50 μm, and methylcellulose having an average particle diameter of about 50 μm are weight ratios of 100: 32: 3. After mixing, the mixer was operated for about 2 minutes with the rotor rotation speed of 300 rpm and the fan rotation speed of 120 rpm to obtain a solid phase mixture.
별도로, 회전 모터 및 임펠라가 구비된 혼합기에, 증류수, 실리카 졸, 액상의 PVA, 글리세린, 스테아린산을 넣고, 70 rpm의 회전 속도를 설정하여 약 2분 동안 혼합기를 작동시켜 액상 혼합물을 수득하였다.Separately, distilled water, silica sol, liquid PVA, glycerin, stearic acid were added to a mixer equipped with a rotary motor and an impeller, and the mixer was operated for about 2 minutes by setting a rotation speed of 70 rpm to obtain a liquid mixture.
다음, 앞서 수득한 고상 혼합물에 별도로 수득한 액상 혼합물을 1ℓ/분의 유량으로 투입한 후, 혼합기의 로터 회전속도를 350 rpm, 팬의 회전 속도를 120 rpm으로 설정하여 혼합기를 약 4분 동안 작동시켜 습식 혼합을 수행함으로써 촉매담체 조성물을 수득하였다.Next, the separately obtained liquid mixture was added to the solid mixture obtained at a flow rate of 1 l / min, and the mixer was operated for about 4 minutes by setting the rotor rotation speed of the mixer to 350 rpm and the fan rotation speed to 120 rpm. To carry out wet mixing to obtain a catalyst carrier composition.
이어서, 1축 스크류를 구비한 압출기 및 200 CPSI (cells per square inch) 이하의 밀도를 갖는 성형 다이를 이용하여, 상기에서 수득된 조성물을 압출성형한 후 통상적인 건조 및 열처리 공정을 수행하여 촉매담체를 제조하였다.Subsequently, using the extruder with a single screw and a molding die having a density of 200 cells per square inch (CPSI) or less, the obtained composition is extruded and then subjected to a conventional drying and heat treatment process to carry out a catalyst carrier. Was prepared.
비교예 1Comparative Example 1
도 2에 도시된 바와 같이 로터와 팬이 반대로 회전하는 혼합기에, 상기 실시예 1에서 사용된 모든 성분을 동시에 넣은 후 혼합기의 로터 회전속도를 350 rpm, 팬의 회전 속도를 120 rpm으로 설정하여 약 10분 동안 혼합기를 작동시켜 촉매담체 조성물을 수득하였으며, 수득된 조성물의 압출성형, 건조 및 열처리 공정은 실시예 1과 동일한 방법으로 수행하여 촉매담체를 제조하였다.As shown in FIG. 2, the rotor and the fan are rotated in opposite directions, and all the components used in Example 1 are simultaneously added, and the rotor rotation speed of the mixer is set to 350 rpm and the fan rotation speed is set to 120 rpm. The mixer was operated for 10 minutes to obtain a catalyst carrier composition, and the extrusion, drying and heat treatment processes of the obtained composition were carried out in the same manner as in Example 1 to prepare a catalyst carrier.
상기 실시예 1 및 비교예 1로부터 제조된 압출성형 촉매담체의 외관 사진을 각각 도 3a 및 3b에 도시하였으며, 이들로부터 본 발명의 실시예 1에 따라 제조된 촉매담체가 비교예 1의 촉매담체보다 균일한 외관을 가짐을 확인할 수 있다. 3A and 3B show external photographs of the extruded catalyst carriers prepared from Example 1 and Comparative Example 1, respectively, from which the catalyst carriers prepared according to Example 1 of the present invention are better than those of Comparative Example 1 It can be confirmed that it has a uniform appearance.
본 발명에 따르면, 촉매담체 조성물의 혼합방식을 개선함으로써 고품질의 촉매담체 압출성형품을 제조할 수 있다.According to the present invention, a high quality catalyst carrier extruded article can be produced by improving the mixing method of the catalyst carrier composition.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101073344B1 (en) | 2009-09-23 | 2011-10-14 | 두산중공업 주식회사 | Extrusion method of internal reforming catalyst for Molten Carbonate Fuel Cell |
| WO2011081341A3 (en) * | 2009-12-30 | 2011-11-24 | 한국항공우주연구원 | Catalyst carrier for a spacecraft thruster and method for preparing same |
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| JPH06172057A (en) * | 1992-07-24 | 1994-06-21 | Tech Sep | Monolithic ceramic support for tangent filtration film |
| KR20000010218A (en) * | 1998-07-31 | 2000-02-15 | 유철진 | Ceramic carrier and preparation method thereof |
| KR20020007021A (en) * | 2000-07-14 | 2002-01-26 | 신동우 | Fabricating Method for Ceramic Catalyst Supporter |
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2005
- 2005-08-19 KR KR1020050076037A patent/KR100661638B1/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06172057A (en) * | 1992-07-24 | 1994-06-21 | Tech Sep | Monolithic ceramic support for tangent filtration film |
| KR20000010218A (en) * | 1998-07-31 | 2000-02-15 | 유철진 | Ceramic carrier and preparation method thereof |
| KR20020007021A (en) * | 2000-07-14 | 2002-01-26 | 신동우 | Fabricating Method for Ceramic Catalyst Supporter |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101073344B1 (en) | 2009-09-23 | 2011-10-14 | 두산중공업 주식회사 | Extrusion method of internal reforming catalyst for Molten Carbonate Fuel Cell |
| WO2011081341A3 (en) * | 2009-12-30 | 2011-11-24 | 한국항공우주연구원 | Catalyst carrier for a spacecraft thruster and method for preparing same |
| US9480970B2 (en) | 2009-12-30 | 2016-11-01 | Korea Aerospace Research Institute | Catalyst carrier for a spacecraft thruster and method for preparing same |
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