KR20050025534A - The manufacturing method of ceramic body having good adiabatic capacity - Google Patents

The manufacturing method of ceramic body having good adiabatic capacity Download PDF

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KR20050025534A
KR20050025534A KR1020030069407A KR20030069407A KR20050025534A KR 20050025534 A KR20050025534 A KR 20050025534A KR 1020030069407 A KR1020030069407 A KR 1020030069407A KR 20030069407 A KR20030069407 A KR 20030069407A KR 20050025534 A KR20050025534 A KR 20050025534A
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inorganic adhesive
porous ceramic
sponge
polymer sponge
thermal insulation
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KR1020030069407A
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Korean (ko)
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KR100588421B1 (en
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유기홍
이홍재
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주식회사 경동세라텍
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Priority to EP04773948A priority Critical patent/EP1685080A4/en
Priority to CNB2004800293539A priority patent/CN100450973C/en
Priority to US10/574,718 priority patent/US20070072761A1/en
Priority to JP2006532066A priority patent/JP4511541B2/en
Priority to PCT/KR2004/001446 priority patent/WO2005033042A1/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303Inorganic additives
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
    • C04B38/0058Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607Thermal properties, e.g. thermal expansion coefficient

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Porous Artificial Stone Or Porous Ceramic Products (AREA)

Abstract

A method for manufacturing porous ceramic preform is provided, which offers excellent heat insulation and a large-sized ceramic preform without cracking and bending by impregnating polymeric sponge with inorganic binders and dry-hardening. The porous ceramic preform is manufactured by the following steps of: (i) impregnating a polymeric sponge, forming a network structure, with liquid inorganic binders such as sodium silicate, potassium silicate, silica sol, alumina sol and aluminum phosphate; (ii) dehydrating binder-impregnated sponge to keep the amount of binder properly; (iii) drying the polymer sponge at 100-180deg.C to harden inorganic binders. The inorganic binders are optionally mixed with hardening agent, surfactant, silane coupling agent(or organic binder), and sodium silicofluoride(or magnesium sulfate). Also, Al(OH)3, Mg(OH)2, Sb compound, phosphate, phosphorous/halogen flame retarding agents, and thermal hardening agent are optionally added to the inorganic binders. The resultant ceramic preform is manufactured by repeating the steps like impregnating, dehydrating and drying.

Description

단열성이 우수한 다공질의 세라믹 성형체 제조방법{THE MANUFACTURING METHOD OF CERAMIC BODY HAVING GOOD ADIABATIC CAPACITY} Method for manufacturing porous ceramic molded article with excellent insulation {THE MANUFACTURING METHOD OF CERAMIC BODY HAVING GOOD ADIABATIC CAPACITY}

본 발명은 단열성이 우수한 다공질의 세라믹 성형체 제조방법에 관한 것이다. The present invention relates to a method for producing a porous ceramic formed body having excellent thermal insulation.

일반적으로 다공질의 세라믹 성형체는 분말형태의 세라믹 원료를 사용하여 제조되며, 대표적인 제조방법으로는 입자충전법, 발포법, 스펀지법이 있다. In general, the porous ceramic formed body is manufactured using a ceramic raw material in powder form, and typical manufacturing methods include a particle filling method, a foaming method, and a sponge method.

입자충전법은 한국요업학회지, 36(6),pp.662~670. 1999에 기재(무가압 분말 충전법에 의한 다공질 세락믹스의 제조 및 특성)된 바와 같이 구형입자를 벌크(bulk)상으로 충전하게 될 때 충전형태에 따라 형성되는 간극을 기공으로 이용하여 고온에서 소결함으로써 다공체를 제조하는 방법이다. The Korean Journal of Ceramic Industry, 36 (6), pp.662 ~ 670. As described in 1999 (Preparation and Characterization of Porous Ceramic Mix by Pressureless Powder Filling Method) When Spherical Particles are Filled into Bulk, Sintering at High Temperature Using Pores Formed by Filling Forms as Pores This is a method for producing a porous body.

따라서, 입자충전법은 공정이 비교적 단순하지만 기공의 크기 및 기공율 조절이 어렵고, 기공율이 다른 제조방법에 비하여 절반 정도밖에 되지 않는다. Therefore, the particle filling method is relatively simple but difficult to control the pore size and porosity, and the porosity is only about half that of other manufacturing methods.

또, 발포법은 한국 특허출원 제10-1999-0058380호(포말법에 의한 다공질 세라믹스의 제조방법) 및 한국 특허출원 제10-2001-0076036호(계면활성제를 이용한 다공성 세라믹스의 제조기술) 등에 제시된 바와 같이 원료인 세라믹분말의 혼합, 슬러리(Slurry)제조, 발포, 성형, 건조, 소성 공정을 통해 제조하는 방법이다. In addition, the foaming method is disclosed in Korean Patent Application No. 10-1999-0058380 (Method for Producing Porous Ceramics by Foam Method) and Korean Patent Application No. 10-2001-0076036 (Technology for Producing Porous Ceramics Using Surfactant) As described above, the method is manufactured by mixing ceramic powder as a raw material, preparing a slurry, foaming, molding, drying, and baking.

상기 발포법에 의한 제조공정 중 발포공정은 계면활성제를 이용하여 발포하는 방법과 원료혼합물과 반응하여 기체를 발생하는 발포성 물질을 첨가하여 발포시키는 방법이 있는데, 두 가지 방법 모두가 성형체의 기공율 및 기공크기의 조절이 곤란하다. The foaming step of the manufacturing process by the foaming method is a method of foaming using a surfactant and a method of foaming by adding a foaming material that generates a gas by reacting with the raw material mixture, both methods are the porosity and porosity of the molded body Difficult to control the size

또, 상기의 제조방법 중에서 스펀지법은 미국특허 3090094호(method of making porous ceramic articles) 및 한국 특허출원 제10-1999-0057840호(강도가 우수한 고순도 세라믹 폼의 제조방법)와 한국 특허출원 제10-2001-0029138호(경질의 다공성 세라믹 흡음재 및 그 제조방법)와 같이 원료인 세라믹분말의 혼합, 슬러리(Slurry)제조, 슬러리를 스펀지에 함침, 잉여 슬러리의 제거, 건조, 소성 공정을 통하여 형틀에 해당하는 스펀지와 동일한 기공구조의 세라믹 다공체를 제조하는 방법이다. In addition, the sponge method of the above manufacturing method is US Patent 3090094 (method of making porous ceramic articles) and Korean Patent Application No. 10-1999-0057840 (method of manufacturing high purity ceramic foam with excellent strength) and Korean Patent Application No. 10 Like -2001-0029138 (hard porous ceramic sound-absorbing material and its manufacturing method), mixing the ceramic powder as raw material, manufacturing slurry, impregnating the slurry into sponge, removing excess slurry, drying and firing It is a method for producing a ceramic porous body having the same pore structure as the corresponding sponge.

상기와 같은 세 가지 제조방법은 모두 소성공정을 통하여 세라믹 분말을 고온으로 열융착시킴으로써 다공질의 세라믹 구조체를 형성하는 방법이다. All three manufacturing methods as described above are methods for forming a porous ceramic structure by thermally fusion ceramic powder at high temperature through a firing process.

따라서, 단열성이 우수한 저밀도의 성형체를 얻기 위하여 다공질 격막의 두께를 얇게 할 경우에는 소성공정 과정에서 격막이 용융되어 다공질 구조가 붕괴되는 현상이 발생되고, 이로 인하여 온전한 성형체를 얻기가 곤란하였다. Therefore, when the thickness of the porous diaphragm is made thin in order to obtain a low density molded article having excellent thermal insulation property, the membrane is melted in the firing process to collapse the porous structure, which makes it difficult to obtain an intact molded article.

또, 대형의 다공질 세라믹 구조체를 제조할 때는 열에 의해 마이크로 크랙 및 휨 현상이 발생하는 문제점도 있었다. Moreover, when manufacturing a large sized porous ceramic structure, there also existed a problem that a micro crack and a bending phenomenon generate | occur | produce by heat.

또한, 소성공정은 원료에 따라 조금씩 차이가 있기는 하지만 일반적으로 1000∼2000℃ 의 고온을 필요로 하는 공정으로써 적지 않은 비용이 소요됨에도 불구하고 그 제조물인 다공질 세라믹 구조체의 단열성 및 경제성이 일반적인 단열재료에 비해 매우 낮아 촉매담체 또는 소형필터 등 극히 제한적인 분야에만 사용되었다. In addition, although the firing process varies slightly depending on the raw materials, it is generally a process requiring a high temperature of 1000 to 2000 ° C., although it requires a considerable amount of cost, the thermal insulation and economical efficiency of the porous ceramic structure as a manufactured product It is very low compared to other materials and is used only in extremely limited fields such as catalyst carriers or small filters.

이러한 문제점을 해소하기 위하여 본원출원의 발명자에 의하여 삼차원 망목상의 다공질 구조를 형성하고 있는 폴리머스펀지에 무기질접착제를 함침시키고 탈수시킨 후 건조시켜 경화되도록 하는 "단열성이 우수한 다공질의 세라믹 성형체 제조방법"(한국 특허출원 제10-2003-0062778호, 2003. 09. 08.출원)이 안출되었다. In order to solve this problem, the inventors of the present application impregnated and dehydrated the inorganic adhesive to the polymer sponge forming the porous porous structure of the three-dimensional network, and then dried and cured. Patent Application No. 10-2003-0062778, filed Sep. 08, 2003).

그러나, 상기 방법에서는 무기질접착제가 건조되어 생성된 피막이 수분흡수에 의하여 단열성능이 저하되는 단점 및 무기질접착제의 종류에 따라 백화현상이 발생되는 단점을 갖는데 이를 해소하기 위한 방법들이 제시되지 못하였다. However, the above method has a disadvantage in that the heat-insulating performance of the film produced by drying the inorganic adhesive has a disadvantage of deterioration due to water absorption and a disadvantage in that bleaching occurs according to the type of the inorganic adhesive.

본 발명은 다공질 구조를 형성하고 있는 폴리머스펀지에 액상의 무기질접착제가 적정량 함침되도록 한 후 고비용이 소요되는 소성공정이 없이 건조공정을 통해 무기질접착제를 경화시킴으로써 저렴한 비용으로 단열성이 우수한 다공질의 세라믹 성형체를 얻으려는데 목적이 있다. The present invention provides a porous ceramic molded article having excellent thermal insulation at low cost by curing an inorganic adhesive through a drying process without impregnating an appropriate amount of a liquid inorganic adhesive onto a polymer sponge forming a porous structure without a costly firing process. The purpose is to gain.

또, 무기질접착제를 폴리머스펀지에 함침, 탈수, 경화시키는 공정을 통해 세라믹 성형체를 제조하더라도 수분흡수에 의한 단열성의 저하현상 등이 발생되지 않도록 하려는 목적도 있다. In addition, even if the ceramic molded body is manufactured through the process of impregnating, dehydrating and curing the inorganic adhesive into the polymer sponge, there is also an object to prevent the deterioration of thermal insulation due to water absorption.

또, 마이크로 크랙 및 휨 현상이 발생되지 않은 대형의 다공질 세라믹 성형체를 안정적으로 생산할 수 있도록 하려는 목적도 있다. In addition, there is also an object to be able to stably produce a large-scale porous ceramic molded body free of micro cracks and warpage.

본 발명은 단열성이 우수한 다공질의 세라믹 성형체 제조방법에 관한 것이다. The present invention relates to a method for producing a porous ceramic formed body having excellent thermal insulation.

본 발명에서는 개방셀(open cell)로서 삼차원 망목상의 다공질 구조를 형성하고 있는 폴리머스펀지를 액상의 무기질접착제에 잠기도록 하여 무기질접착제가 폴리머스펀지의 내부까지 완전히 침투되도록 한 후 폴리머스펀지에 함침된 무기질접착제를 일부 제거하여 밀도에 따른 적정량의 무기질접착제만을 갖도록 한 후 경화시킴으로써 단열성이 우수한 다공질의 세라믹 성형체를 얻는다. In the present invention, the polymer sponge that forms the porous porous structure of the three-dimensional network as an open cell is immersed in the liquid inorganic adhesive so that the inorganic adhesive penetrates completely to the inside of the polymer sponge, and then the inorganic adhesive impregnated in the polymer sponge. Particularly, the porous ceramic molded body having excellent thermal insulation property is obtained by removing some of it to have only an appropriate amount of inorganic adhesive according to the density.

따라서, 본 발명의 다공질 세라믹 성형체 제조방법은, Therefore, the porous ceramic molded body manufacturing method of the present invention,

개방셀(open cell)로서 삼차원 망목상의 다공질 구조를 형성하고 있는 폴리머스펀지를 액상의 무기질접착제에 잠기도록 하여 무기질접착제가 폴리머스펀지의 내부까지 완전히 침투되도록 하는 함침공정과;  An impregnation step of allowing the inorganic sponge to completely penetrate into the inside of the polymer sponge by immersing the polymer sponge, which is a three-dimensional network-like porous structure as an open cell, in the liquid inorganic adhesive;

무기질접착제가 함침된 폴리머스펀지로부터 무기질접착제를 일부 제거하여 얻으려는 성형체의 밀도에 따른 적정량의 무기질접착제만을 갖도록 하는 탈수공정과; A dehydration step of having an inorganic adhesive of an appropriate amount according to the density of the molded product to be obtained by partially removing the inorganic adhesive from the polymer sponge impregnated with the inorganic adhesive;

탈수공정을 거친 폴리머스펀지를 건조시켜 무기질접착제가 경화되도록 하는 건조공정;을 갖는다. It has a drying step of drying the polymer sponge after the dehydration step to cure the inorganic adhesive.

탈수공정에서 폴리머스펀지로부터 무기질접착제를 일부 제거하기 위한 방법에는 다양한 방법이 있다. There are various methods for removing some of the inorganic adhesive from the polymer sponge in the dehydration process.

보다 구체적으로 설명하면, 폴리머스펀지가 연질인 경우에는 롤러(roller)를 사용한 방법 및 폴리머스펀지에 압축공기를 분사하는 방법을 통해 무기질접착제를 제거할 수 있다. In more detail, when the polymer sponge is soft, the inorganic adhesive may be removed by using a roller and spraying compressed air on the polymer sponge.

폴리머스펀지가 경질인 경우에는 롤러를 사용하여 탈수하는 것이 불가능하므로 폴리머스펀지 표면에 압축공기를 분사하는 방법을 통해 함침된 무기질접착제를 제거한다. If the polymer sponge is hard, it is impossible to dehydrate it using a roller. Thus, the impregnated inorganic adhesive is removed by spraying compressed air on the surface of the polymer sponge.

그러나, 폴리머스펀지가 연질인 경우에도 흡음성능을 강화하기 위하여 기공과 기공이 모두 연결되는 연속개방기공을 얻으려 할 때에는 폴리머스펀지에 압축공기를 분사하여 무기질접착제를 제거한다. However, even when the polymer sponge is soft, in order to obtain continuous open pores in which both pores and pores are connected to enhance sound absorption performance, the compressed air is blown onto the polymer sponge to remove the inorganic adhesive.

본 발명의 건조공정에서의 건조온도는 100 ~ 180℃ 정도가 바람직하다. As for the drying temperature in the drying process of this invention, about 100-180 degreeC is preferable.

또, 폴리머스펀지의 완전한 건조(완제품의 중량감소가 거의 일어나지 않는 상태)가 이루어지지 못하면 완제품인 다공질의 세라믹 성형체가 200℃ 정도의 비교적 저온 상태에 놓일 경우 무기질접착제에 의한 부풀음 현상이 발생하므로 완전한 건조가 이루어질 때까지 건조시킨다. In addition, if the polymer sponge is not completely dried (a state in which the weight loss of the finished product hardly occurs), when the porous ceramic molded body, which is a finished product, is placed at a relatively low temperature of about 200 ° C, swelling phenomenon occurs due to the inorganic adhesive. Dry until done.

탈수공정 직후 폴리머스펀지에 잔존하는 무기질접착제는 액상이기 때문에 밑으로 흘러내리는 현상에 의한 밀도의 편재 현상이 발생될 수 있다. Since the inorganic adhesive remaining in the polymer sponge immediately after the dehydration process is a liquid phase, a density phenomenon may occur due to the phenomenon of flowing down.

그러므로 탈수공정 직후에 건조를 실시할 경우에는 폴리머스펀지를 자주 뒤집어주어 밀도의 편재현상을 방지하는 것이 바람직하다. Therefore, in the case of drying immediately after the dehydration step, it is desirable to frequently turn the polymer sponge over to prevent ubiquitous density.

그러나, 상기와 같이 밀도의 편재현상을 방지하기 위하여 폴리머스펀지를 자주 뒤집어주는 작업이 추가되면 제조비용이 상승될 뿐만 아니라 편재현상을 완전히 방지할 수는 없어 단열성도 다소 저하될 수밖에 없다. However, in order to prevent the ubiquitous density, the polymer sponge is often inverted to increase the manufacturing cost, and the phenomena cannot be prevented completely.

이를 해소하기 위하여, 본 발명의 제조공정에는 폴리머스펀지가 빠르게 경화되도록 하는 경화공정을 추가할 수 있다. In order to solve this problem, the curing process of the polymer sponge may be added to the manufacturing process of the present invention.

경화방법으로는 탈수공정을 거친 폴리머스펀지의 공극에 이산화탄소와 같은 기체경화제가 들어가도록 하여 경화시키는 방법이 있다. As a curing method, there is a method in which a gas hardening agent such as carbon dioxide enters into the pores of a polymer sponge that has been dehydrated to be cured.

이와 같이 폴리머스펀지에 이산화탄소가 들어가도록 하는 경우 급속한 경화를 위하여 폴리머스펀지에 압력을 가해 불어넣는 것이 바람직하다. As such, when carbon dioxide enters the polymer sponge, it is preferable to apply pressure to the polymer sponge and blow it in for rapid curing.

경화의 또 다른 방법으로는 탈수공정을 거친 폴리머스펀지의 공극에 압축공기를 사용하여 시멘트와 같은 고체를 불어넣는 방법이 있다. Another method of curing is to use a compressed air to blow solids such as cement into the pores of the polymer sponge after the dehydration process.

또, 원료를 준비하는 단계에서 무기질접착제에 상기의 고체경화제 또는 알루민산나트륨과 같은 액체 경화제를 혼합하되 탈수공정까지 소요되는 시간을 고려하여 적정량의 경화제를 혼합시킨 후 작업함으로써 경화시키는 방법이 있다. In addition, there is a method of curing by mixing the appropriate amount of the curing agent in consideration of the time required until the dehydration process, while mixing the liquid curing agent such as the above-mentioned solid curing agent or sodium aluminate to the inorganic adhesive in the step of preparing the raw material.

즉, 경화제의 투입량에 따라서 무기질접착제의 경화속도가 결정되므로 이 액체경화제의 투입량을 통해 탈수공정이 끝나는 시점에서 무기질접착제의 편재가 일어나지 않을 정도로 경화가 진행된 상태가 되도록 하는 것이다. That is, since the curing rate of the inorganic adhesive is determined according to the amount of the curing agent, the amount of the curing agent is set so that the curing process is in such a state that ubiquity of the inorganic adhesive does not occur at the end of the dehydration process.

상기와 같은 경화방법들은 다공질의 세라믹 성형체의 용도 및 제조공정상의 편의성을 감안하여 선택적으로 실시할 수 있다. Such curing methods may be selectively performed in consideration of the use of the porous ceramic molded body and the convenience of the manufacturing process.

또한, 본 발명에서는 일정한 상태로 경화된 성형체에 무기질접착제를 다시 함침시키고 탈수시킨 후 경화시키는 공정을 반복적으로 실시하여 강도가 높은 다공질의 세라믹 성형체를 제조할 수도 있다. In addition, in the present invention, a porous ceramic molded article having high strength may be produced by repeatedly impregnating the inorganic adhesive into the molded article cured in a constant state, dehydrating, and curing.

즉, 함침공정과 탈수공정과 건조공정을 여러 번 반복 실시하거나, 함침공정과 경화공정을 여러 번 반복 실시하는 것이다. That is, the impregnation process, the dehydration process, and the drying process may be repeated several times, or the impregnation process and the curing process may be repeated several times.

본 발명의 무기질접착제로는 규산나트륨, 규산칼륨, 규산리튬 등의 규산염 및 변성규산염계와, 실리카졸, 알루미나졸 등의 졸(sol)계 화합물, 인산알루미늄(Mono Aluminium Phosphate, Al2O3. 3(P2O5). 6(H2O)), 변성인산알루미늄 등의 인산염계 접착제을 사용할 수 있는데 밀도 조절이 용이하도록 적정량의 물로 희석하여 사용한다. Examples of the inorganic adhesive of the present invention include silicates and modified silicates such as sodium silicate, potassium silicate and lithium silicate, sol compounds such as silica sol and alumina sol, and mono aluminum phosphate (Al2O3.3 (P2O5). 6 (H2O)) and modified phosphate adhesives such as modified aluminum phosphate can be used. Dilute with an appropriate amount of water for easy density control.

또, 본 발명의 효과를 보다 증진시키기 위하여 발수제, 백화방지제, 접착보조제나 내열성증진제 등의 다양한 첨가제를 추가로 무기질접착제에 혼합하여 사용할 수 있다.In addition, in order to further enhance the effect of the present invention, various additives such as water repellent, anti-whitening agent, adhesion aid or heat resistance enhancer may be further mixed and used in the inorganic adhesive.

구체적으로 설명하면 무기질접착제가 건조되어 생성된 피막은 수분흡수에 의하여 단열성능이 저하되는 단점을 가지고 있다. 이러한 단점을 보완하기 위하여 실리콘계 또는 파라핀계의 발수제를 무기질접착제에 혼합하여 사용할 수 있다. Specifically, the coating film formed by drying the inorganic adhesive has a disadvantage in that the thermal insulation performance is reduced by water absorption. In order to compensate for these disadvantages, a silicone-based or paraffin-based water repellent may be mixed with the inorganic adhesive.

그리고 무기질접착제 중에서 규산나트륨과 같은 것은 함유되어 있는 나트륨이온이 대기중의 이산화 탄소와 반응할 경우 백색결정이 생성되는 백화현상이 발생되는데, 규불화소다 및 황산마그네슘을 무기질접착제에 혼합하여 사용하면 백화현상의 요인인 나트륨이온과 결합하여 불용성 염을 생성시키므로 백화현상을 방지할 뿐만 아니라 내구성이 향상된다. In the inorganic adhesives, such as sodium silicate, whitening occurs when sodium ions are reacted with carbon dioxide in the air, and whitening occurs when sodium silicate and magnesium sulfate are mixed with the inorganic adhesive. It combines with sodium ions, which causes the phenomenon, to form insoluble salts, which not only prevents bleaching but also improves durability.

또한, 액상의 무기질접착제가 고상의 유기질 스폰지에 균일하게 코팅될 수 있도록 하고, 건조된 후에 무기질 피막이 폴리머스펀지에 보다 견고하게 부착될 수 있도록 접착보조제를 무기질 접착제에 혼합하여 사용할 수 있다.In addition, a liquid inorganic adhesive may be uniformly coated on a solid organic sponge, and after drying, an adhesive aid may be mixed with an inorganic adhesive so that the inorganic coating can be more firmly attached to the polymer sponge.

상기 접착보조제로는 다양한 것들이 있으며, 계면활성제를 접착보조제로 사용하면 액상의 무기질접착제가 고상의 유기질 스폰지에 보다 균일하게 코팅되도록 할 수 있고, 실란커플링제나 폴리비닐알콜, 메칠셀룰 로우스계, 염화비닐수지, 아크릴수지, EVA(Ethylene Vinyl Acetate) 등 유기접착제를 혼합, 사용하면 건조된 후에 무기질 피막이 스펀지에 보다 견고하게 부착된 결과물을 얻을 수 있다. The adhesion assistant may be various, and when the surfactant is used as the adhesion assistant, the liquid inorganic adhesive may be more uniformly coated on the solid organic sponge, and the silane coupling agent, polyvinyl alcohol, methyl cellulose, chloride When organic adhesives such as vinyl resin, acrylic resin, and EVA (Ethylene Vinyl Acetate) are mixed and used, the result is that the inorganic film is more firmly attached to the sponge after drying.

또, 본 발명에 수산화알루미늄, 수산화마그네슘, 안티몬화합물, 붕산 및 붕사, 인산 및 인산염, 인계 및 할로겐계 난연제와 멜라민, 에폭시, 페놀 등 열경화성수지 등의 내열성증진제를 추가로 혼합하여 사용할 수도 있다. In addition, the present invention may further be used by adding a mixture of heat resistance enhancers such as aluminum hydroxide, magnesium hydroxide, antimony compounds, boric acid and borax, phosphoric acid and phosphates, phosphorus and halogen flame retardants and thermosetting resins such as melamine, epoxy and phenol.

상기와 같은 내열성 증진제는 유기질인 스폰지의 난연성을 부여하거나, 탄화시에 많은 차르(char)를 형성시키므로 열에 의한 형태의 변형을 막아주는 역할을 한다.Such heat resistance enhancers impart flame retardancy of an organic sponge or form a large amount of char during carbonization, thereby preventing deformation of the form due to heat.

본 발명에 사용되는 폴리머스펀지는 결과물인 다공질의 세라믹 성형체의 용도에 따라서 연질이나 반경질 또는 경질의 것을 사용할 수 있다. The polymer sponge used in the present invention may be soft, semi-hard or hard, depending on the use of the resulting porous ceramic formed body.

또, 폴리머스펀지가 갖는 기공의 크기도 용도에 따라 선택하여 사용할 수 있는데 본 발명의 제조공정을 거치면 기공의 크기가 작아질 수 있으므로 이를 감안하여 기공의 크기가 조금 큰 것을 사용하는 것이 바람직하다. In addition, the size of the pores of the polymer sponge can be selected and used according to the use, but the size of the pores may be reduced through the manufacturing process of the present invention, it is preferable to use a slightly larger pore size in view of this.

본 발명을 실시 예를 통하여 보다 구체적으로 설명하면 다음과 같다. The present invention will be described in more detail with reference to the following Examples.

그러나, 실시 예는 본 발명을 보다 구체적으로 설명하기 위한 것이므로 본 발명의 기술적 사상이 실시 예에 한정되는 것은 아니다. However, since the embodiments are intended to describe the present invention in more detail, the technical spirit of the present invention is not limited to the embodiments.

[실시예 1]Example 1

무기질접착제인 40보메의 규산나트륨 용액이 들어있는 수조를 준비하였다. A water bath containing 40 bome sodium silicate solution, which is an inorganic adhesive, was prepared.

크기가 300㎜ ×300㎜ ×50㎜이고 셀의 크기가 약 10 PPI(pores per linear inch)인 폴리우레탄 스펀지를 준비하였다. Polyurethane sponges having a size of 300 mm x 300 mm x 50 mm and a cell size of about 10 pores per linear inch (PPI) were prepared.

상기 수조에 준비한 폴리우레탄 스펀지를 넣어 규산나트륨 용액에 잠기도록 한 상태에서 폴리우레탄 스펀지를 5회 반복 압축하여 규산나트륨 용액이 내부까지 완전히 침투되도록 하는 함침공정을 실시하였다. The impregnation process was carried out so as to completely penetrate the sodium silicate solution by repeatedly compressing the polyurethane sponge five times in a state in which the prepared polyurethane sponge was immersed in the sodium silicate solution.

상기 함침공정 후 폴리우레탄 스펀지를 수조에서 꺼내어 밀도가 100㎏/㎥가 되는 다공질의 세라믹 성형체를 얻기 위해 잉여의 규산나트륨 용액을 탈수하는 탈수공정을 실시하였다. After the impregnation step, the polyurethane sponge was taken out of the water bath, and a dehydration step of dehydrating the excess sodium silicate solution was performed to obtain a porous ceramic molded body having a density of 100 kg / m 3.

상기 탈수공정을 거친 폴리우레탄 스펀지의 공극에 이산화탄소가 들어가도록 하는 경화공정을 실시하였다. A curing process was performed to allow carbon dioxide to enter the pores of the polyurethane sponge which had been subjected to the dehydration process.

상기 경화공정을 거친 폴리우레탄 스펀지를 105℃ 가 유지되는 건조실에서 24시간 건조시켜서 다공질의 세라믹 성형체를 제조하였다. The polyurethane sponge, which had undergone the curing process, was dried in a drying chamber maintained at 105 ° C. for 24 hours to prepare a porous ceramic formed body.

[실시예 2]Example 2

실시예 1과 같은 방법으로 다공질의 세라믹 성형체를 제조하되, 탈수공정에서 밀도가 대략 60㎏/㎥가 되는 다공질의 세라믹 성형체를 얻기 위한 규산나트륨 용액의 탈수를 실시하였다. A porous ceramic compact was prepared in the same manner as in Example 1, but in the dehydration process, the sodium silicate solution was dehydrated to obtain a porous ceramic compact having a density of approximately 60 kg / m 3.

[실시예 3]Example 3

실시예 1과 같은 방법으로 다공질의 세라믹 성형체를 제조하되, 탈수공정에서 밀도가 대략 150㎏/㎥가 되는 다공질의 세라믹 성형체를 얻기 위한 규산나트륨 용액의 탈수를 실시하였다. A porous ceramic compact was prepared in the same manner as in Example 1, but in the dehydration process, the sodium silicate solution was dehydrated to obtain a porous ceramic compact having a density of approximately 150 kg / m 3.

[실시예 4]Example 4

실시예 1과 같은 방법으로 다공질의 세라믹 성형체를 제조하되, 함침공정에서 무기질접착제로 사용된 규산나트륨을 인산알루미늄(Mono Aluminium Phosphate, Al2O3. 3(P2O5). 6(H2O))으로 대체하고, 탈수공정을 거친 후 건조공정을 실시하였다. A porous ceramic molded body was prepared in the same manner as in Example 1, except that sodium silicate used as an inorganic adhesive in the impregnation process was replaced with mono aluminum phosphate, Al 2 O 3 (P 2 O 5) 6 (H 2 O), and dehydration. After the step was carried out a drying step.

건조공정에서는 건조온도를 140℃ 로 유지하면서 24시간 건조시켰다. In a drying process, it dried for 24 hours, maintaining a drying temperature at 140 degreeC.

[실시예 5]Example 5

실시예 4와 같은 방법으로 다공질의 세라믹 성형체를 제조하되, 함침공정에서 무기질접착제로 사용된 규산나트륨을 실리카졸로 대체하였다. A porous ceramic compact was prepared in the same manner as in Example 4, except that sodium silicate used as an inorganic adhesive in the impregnation process was replaced with silica sol.

[실시예 6]Example 6

실시예 1과 같은 방법으로 다공질의 세라믹 성형체를 제조하되, 함침공정에서 무기질접착제로 사용되는 규산나트륨 용액에 실란커플링제를 혼합한 후 폴리우레탄 수지에 무기질접착제가 함침되도록 하였다. A porous ceramic molded body was prepared in the same manner as in Example 1, but the silane coupling agent was mixed with the sodium silicate solution used as the inorganic adhesive in the impregnation process, so that the inorganic adhesive was impregnated into the polyurethane resin.

실시예 1 ∼ 6에 의해 제조된 시편을 대한민국 품질규격 KS F 4714 방법에 의하여 밀도와 KS L 9016 방법에 의하여 열전도율을 측정하고, 이를 시중에서 일반적으로 사용되는 무기질단열재인 발수성 펄라이트 보온재(KS F 4714)와 규산칼슘 보온재(KS L 9101)의 KS 규격상 열전도율과 비교하여 [표 1]에 나타내었다. The specimens prepared according to Examples 1 to 6 were measured for density and thermal conductivity by KS L 9016 method according to Korean Quality Standard KS F 4714 method, and the water-repellent pearlite insulating material which is an inorganic insulating material generally used in the market (KS F 4714). ) And calcium silicate insulation (KS L 9101) are shown in [Table 1] in comparison with the thermal conductivity according to the KS standard.

<표 1> 열전도율 비교<Table 1> Thermal Conductivity Comparison

시험구 Test 실시예1 Example 1 실시예2 Example 2 실시예3 Example 3 실시예4 Example 4 실시예5 Example 5 실시예6 Example 6 발수성퍼라이트보온재Water repellent perlite insulation 규산칼슘보온재 Calcium silicate insulation 밀도(㎏/㎤) Density (kg / cm 3) 99 99 70 70 144 144 137 137 106 106 110 110 155이하 155 and below 170이하 Less than 170 전도율(㎉/mh℃) Conductivity (㎉ / mh ℃) 0.0418 0.0418 0.0371 0.0371 0.0474 0.0474 0.0465 0.0465 0.420 0.420 0.0421 0.0421 0.047이하 Less than 0.047 0.047이하 Less than 0.047

상기 실험결과를 통해 알 수 있듯이 본 발명의 제조방법에 의해 제조된 다공질의 세라믹 성형체는 종래의 세라믹 성형체나 시중에서 일반적으로 단열재료로 사용되는 무기질단열재인 발수성 펄라이트 보온재(KS F 4714)와 규산칼슘 보온재(KS L9101)에 비하여 단열성이 우수함을 확인할 수 있었다. As can be seen from the experimental results, the porous ceramic molded body manufactured by the manufacturing method of the present invention is a conventional ceramic molded body or a water-repellent pearlite insulating material (KS F 4714) and calcium silicate, which are inorganic insulating materials generally used as insulating materials in the market. It was confirmed that the thermal insulation is superior to the heat insulating material (KS L9101).

또, 관능시험을 통하여 확인할 결과 본 발명의 제조방법에 의해 제조된 다공질의 세라믹 성형체는 흡음재로 사용할 수 있을 정도로 흡음성이 우수한 것으로 확인되었다.In addition, as a result of confirming through the sensory test, it was confirmed that the porous ceramic molded body produced by the manufacturing method of the present invention has excellent sound absorption so that it can be used as a sound absorbing material.

본 발명에 의하면, 다공질 구조를 형성하고 있는 폴리머스펀지에 액상의 무기질접착제를 적정량 함침시킨 후 건조공정을 통해 무기질접착제가 단단해지도록 함으로써 단열성이 우수한 다공질의 세라믹 성형체를 얻으므로 다공질의 세라믹 성형체를 얻기 위한 공정이 간단하고 생산비용이 저렴한 특징이 있다. According to the present invention, by impregnating a polymer sponge having a porous structure with an appropriate amount of a liquid inorganic adhesive, the inorganic adhesive is hardened through a drying process to obtain a porous ceramic molded body having excellent thermal insulation, so as to obtain a porous ceramic molded body The process is simple and the production cost is low.

또, 단열성 및 흡음성이 우수하여 일반적인 단열재 또는 흡음재로써 사용할 수 있는 다공질의 세라믹 성형체를 얻을 수 있다. Moreover, the porous ceramic molded object which is excellent in heat insulation and sound absorption property and can be used as a general heat insulation material or a sound absorption material can be obtained.

또한, 마이크로 크랙 및 휨 현상이 발생되지 않은 대형의 다공질 세라믹 성형체를 안정적으로 생산할 수도 있다. In addition, it is also possible to stably produce a large porous ceramic molded body in which micro cracks and warpage are not generated.

도 1은 본 발명의 단열성이 우수한 다공질의 세라믹 성형체 제조방법의 공정도1 is a process chart of a method for producing a porous ceramic formed body having excellent thermal insulation of the present invention

도 2는 경화공정이 추가된 본 발명의 단열성이 우수한 다공질의 세라믹 성형체 제조방법의 공정도Figure 2 is a process diagram of a porous ceramic formed body manufacturing method excellent in thermal insulation of the present invention with the addition of a curing process

Claims (12)

다공질의 세라믹 성형체 제조방법에 있어서, In the method of manufacturing a porous ceramic formed body, 개방셀로서 삼차원 망목상의 다공질 구조를 형성하고 있는 폴리머스펀지를 액상의 무기질접착제에 잠기도록 하여 무기질접착제가 폴리머스펀지의 내부까지 완전히 침투되도록 하는 함침공정과; An impregnation step of allowing the polymer sponge, which has a three-dimensional mesh-like porous structure as an open cell, to be immersed in the liquid inorganic adhesive, so that the inorganic adhesive completely penetrates into the polymer sponge; 상기 함침공정에 의해 무기질접착제가 함침된 폴리머스펀지로부터 무기질접착제를 일부 제거하여 폴리머스펀지가 밀도에 따른 적정량의 무기질접착제만을 갖도록 하는 탈수공정과; A dehydration step of removing some of the inorganic adhesive from the polymer sponge impregnated with the inorganic adhesive by the impregnation process so that the polymer sponge has only an appropriate amount of the inorganic adhesive according to the density; 상기 탈수공정을 거친 폴리머스펀지를 건조시켜 무기질접착제가 경화되도록 하는 건조공정;으로 이루어진, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. And a drying step of drying the polymer sponge after the dehydration step so that the inorganic adhesive is cured. 제 1항에 있어서, The method of claim 1, 상기 탈수공정을 거친 폴리머스펀지의 공극에 기체경화제 또는 고체경화제가 들어가도록 하는 경화공정;을 실시한 후 건조공정을 실시하는 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. And a curing step of allowing a gas hardener or a solid hardener to enter the pores of the polymer sponge which has undergone the dehydration step. The drying process is performed after the porous sponge is formed. 제 1항에 있어서, The method of claim 1, 상기 함침공정은 무기질접착제에 고체경화제나 액체경화제를 혼합한 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation step is characterized in that the polymer sponge is immersed after mixing a solid hardener or a liquid hardener with an inorganic adhesive, a porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제 3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정과 탈수공정과 건조공정을 여러 번 반복 실시한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. A method for producing a porous ceramic formed body having excellent thermal insulation, characterized in that the impregnation step, the dehydration step and the drying step are repeated several times. 제 1항 내지 제 3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 무기질접착제는 규산나트륨, 규산칼륨, 규산리튬 등의 규산염 및 변성규산염계와, 실리카졸, 알루미나졸 등의 졸(sol)계 화합물, 인산알루미늄, 변성인산알루미늄 등의 인산염계 접착제 중에서 선택된 1종 이상인 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The inorganic adhesive is one selected from silicates and modified silicates such as sodium silicate, potassium silicate and lithium silicate, sol-based compounds such as silica sol and alumina sol, and phosphate-based adhesives such as aluminum phosphate and modified aluminum phosphate. The porous ceramic molded product manufacturing method excellent in heat insulation characterized by the above-mentioned. 제 1항 내지 제3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정은 무기질접착제에 계면활성제를 혼합한 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation step is characterized in that the polymer sponge is immersed after mixing the surfactant with the inorganic adhesive, porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정은 무기질접착제에 실란커플링제, 유기접착제 중에서 선택된 1종 이상의 것을 혼합한 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation step is characterized in that the polymer sponge is immersed after mixing at least one selected from the silane coupling agent and the organic adhesive to the inorganic adhesive, porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제 3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정은 무기질접착제에 규불화소다, 황산마그네슘 중에서 선택된 1종 이상의 것을 혼합 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation process is characterized in that the polymer sponge is immersed after mixing at least one selected from sodium silicate and magnesium sulfate in the inorganic adhesive, porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제 3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정은 무기질접착제에 발수제를 혼합 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation step is characterized in that the polymer sponge is immersed after mixing the water-repellent agent to the inorganic adhesive, porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제 3항 중 어느 한 항에 있어서, The method according to any one of claims 1 to 3, 상기 함침공정은 무기질접착제에 수산화알루미늄, 수산화마그네슘, 안티몬화합물, 붕산 및 붕사, 인산 및 인산염, 인계 및 할로겐계 난연제와 열경화성수지 중에서 선택된 1종 이상의 것을 혼합 후 폴리머스펀지가 잠기도록 한 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법. The impregnation process is characterized in that the polymer sponge is immersed after mixing at least one selected from aluminum hydroxide, magnesium hydroxide, antimony compound, boric acid and borax, phosphoric acid and phosphate, phosphorus and halogen flame retardant and thermosetting resin to the inorganic adhesive. , Porous ceramic molded body manufacturing method excellent in heat insulation. 제 2항 내지 제 3항에 있어서, The method according to claim 2, wherein 상기 경화공정을 실시한 후 폴리머스펀지에 무기질접착제가 다시 함침되도록 함침공정과 경화공정을 여러 번 반복하여 실시하는 것을 특징으로 하는, 단열성이 우수한 다공질의 세라믹 성형체 제조방법.After performing the hardening step, the impregnating step and the hardening step are repeated several times so that the inorganic sponge is impregnated again in the polymer sponge, a porous ceramic molded body having excellent thermal insulation. 제 1항 내지 제 3항 중 어느 한 항의 제조방법에 의해 제조된, 단열성이 우수한 다공질의 세라믹 성형체. A porous ceramic formed article having excellent thermal insulation, which is produced by the manufacturing method of any one of claims 1 to 3.
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