KR100839457B1 - Manufacturing inorganic panel using waste titanium dioxide - Google Patents
Manufacturing inorganic panel using waste titanium dioxide Download PDFInfo
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- KR100839457B1 KR100839457B1 KR1020060120589A KR20060120589A KR100839457B1 KR 100839457 B1 KR100839457 B1 KR 100839457B1 KR 1020060120589 A KR1020060120589 A KR 1020060120589A KR 20060120589 A KR20060120589 A KR 20060120589A KR 100839457 B1 KR100839457 B1 KR 100839457B1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B33/00—Clay-wares
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
본 발명은 폐 이산화티탄 슬러지를 이용하여 색상이 아름답고 경량화 된 무기패널의 제조방법에 관한 것으로, 폐 이산화티탄 20-60중량%, 유리 부산물 10-30중량%, 점토질 원료 10-70중량%로 구성되는 조성물 100중량부에 대하여 수분을 5-30중량부 추가한 다음, 혼합분쇄하고, 성형, 건조 및 소성하는 과정을 포함하며, 폐자원을 활용하는 장점과 폐 이산화티탄에 포함된 유기 물질로 인해 얻어진 패널은 경량화가 가능하고, 이산화티탄의 발색으로 무기패널의 색을 조절할 수 있다.The present invention relates to a method for producing an inorganic panel with beautiful color and light weight using waste titanium dioxide sludge, comprising 20-60 wt% of waste titanium dioxide, 10-30 wt% of glass by-product, and 10-70 wt% of clay raw material. 5-30 parts by weight of water is added to 100 parts by weight of the composition, and then mixed, pulverized, molded, dried, and fired, and the advantages of utilizing waste resources and organic materials contained in waste titanium dioxide The obtained panel can be reduced in weight, and the color of the inorganic panel can be adjusted by the color development of titanium dioxide.
폐 이산화티탄, 유리 부산물, 점토질 원료, 무기패널, 압출, 프레스 Waste Titanium Dioxide, Glass By-Products, Clay Material, Inorganic Panel, Extrusion, Press
Description
도 1은 무기패널 소지 조성인 점토-유리 부산물-장석의 조성 성분을 점토-장석-규석으로 전환한 삼성분계이고,1 is a Samsung system that converts the composition of clay-glass by-products-feldspar, which is the composition of the inorganic panel, to clay-feldspar-gyuseok,
도 2는 사용된 소지의 점토-장석-규석의 삼성분계이고, 2 is the Samsung demarcation of the clay-feldspar-gyuseok of the body used,
도 3은 소지 조성 변화에 따른 소결체의 미세구조 변화를 나타낸 사진이고, 3 is a photograph showing a microstructure change of the sintered body according to the change in the composition of the body,
도 4는 본 발명의 제조공정도이다.4 is a manufacturing process diagram of the present invention.
본 발명은 폐 이산화티탄 슬러지를 이용하여 색상이 아름답고 경량화 된 무기패널의 제조방법에 관한 것이다.The present invention relates to a method for producing an inorganic panel having a beautiful color and light weight using waste titanium dioxide sludge.
이산화티탄 슬러지는 황산법에 의한 이산화티탄 제조시 중화 처리하여 발생되는 부산물로 CaSO4 , TiO2, Fe2O3등이 부산물로 존재하는 무기산화물이다. 이 부산물은 국내에서 월 10,000톤 이상 발생되고 있으며 주로 단순 매립에 의해 폐기되고 있는 실정으로 금속성분의 유출에 의한 2차 오염을 방지하여야 할 실정이다. Titanium dioxide sludge is a by-product produced by neutralization in the production of titanium dioxide by the sulfuric acid method and is an inorganic oxide in which CaSO 4 , TiO 2, Fe 2 O 3, etc. are present as by-products. This by-product is generated more than 10,000 tons per month in Korea, and is mainly disposed of by landfilling.
따라서 이 슬러지에 함유된 TiO2 성분 등 유리한 금속산화물의 특성(색상, 강도)을 활용한 복합 산화물을 형성을 통하여 무기패널 제조에 응용할 경우 폐기물을 자원화 하여 공해방지 및 경제적인 환경 친화적 제품 개발이 가능할 것으로 기대된다.Therefore, it is possible to prevent waste and develop eco-friendly products by recycling wastes when applying to inorganic panel production by forming composite oxides utilizing the characteristics (color, strength) of advantageous metal oxides such as TiO 2 contained in this sludge. It is expected to be.
현재까지 이산화티탄 슬러지를 활용한 무기패널에의 응용연구에 대한 사례는 보고되지 않고 있다. 유사한 연구로서 유리 부산물, 폐 연마슬러지, 폐석고, 점토광물, 발포제 등을 혼합하여 고강도 경량타일을 제조(대한민국 특허 등록번호 10-0400634)하거나 산업현장이나 광산 등에서 쉽게 구입할 수 있는 폐석고 등을 이용해 건축용 석고 판넬을 제조(대한민국 특허 공개번호 특1998-0009181)한 예가 거의 전부이다. 위의 기술들은 본 발명의 이산화티탄 슬러지 활용과는 거리가 있다. 본 발명에서 활용하는 폐 이산화티탄 슬러지는 이산화티탄 등 광촉매 기능 및 고유의 색상을 갖는 금속산화물이 포함되어 있어 패널 등에 응용시 아름다운 색상과 광촉매, 자정기능을 갖는 패널제품이 가능하다.To date, there have been no reports of applied research on inorganic panels utilizing titanium dioxide sludge. In a similar study, gypsum for construction is produced by mixing glass by-products, waste abrasive sludge, waste gypsum, clay minerals, foaming agents, etc. Almost all examples of manufacturing the panel (Korean Patent Publication No. 1998-0009181). The above techniques are far from utilizing the titanium dioxide sludge of the present invention. The waste titanium dioxide sludge used in the present invention includes a metal oxide having a photocatalytic function and a unique color such as titanium dioxide, and thus a panel product having a beautiful color, a photocatalyst and a self-cleaning function when applied to a panel is possible.
본 발명은 이산화티탄 제조공정 중에 발생되는 페기물인 폐 이산화티탄 슬러지를 재활용하는 것을 목적으로 한다. 본 발명의 다른 목적은 경량성과 질감이 우수한 무기패널을 제공하는 것이다. 본 발명의 또 다른 목적은 자정기능을 가지는 무기패널을 제공하는 것이다.An object of the present invention is to recycle waste titanium dioxide sludge, which is a waste product generated during the production of titanium dioxide. Another object of the present invention is to provide an inorganic panel having excellent light weight and texture. Still another object of the present invention is to provide an inorganic panel having a self-cleaning function.
본 발명은 폐 이산화티탄 슬러지 20-60중량%, 유리 부산물 10-30중량%, 점토질 원료 10-70중량%로 구성되는 조성물 100중량부에 수분을 5-30 중량부 가하고 볼밀을 이용하여 분쇄 및 혼합한 다음, 가압 성형하고 건조 및 소성하는 것으로 구성된다.The present invention is added 5-30 parts by weight of water to 100 parts by weight of the composition consisting of 20-60% by weight of waste titanium dioxide sludge, 10-30% by weight of glass by-products, 10-70% by weight of clay raw material, and pulverized using a ball mill. Mixing, then press forming, drying and firing.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명에서 사용되는 이산화티탄 슬러지, 유리 부산물, 점토의 조성은 점토-장석-규석의 삼성분계로 도1과 같다.The composition of the titanium dioxide sludge, glass by-products, and clays used in the present invention are as shown in FIG. 1 as the Samsung system of clay-feldspar-gyuseok.
각 원료의 특성은 다음과 같다. The characteristics of each raw material are as follows.
이산화티탄 슬러지는 칼슘, 철, 티타늄이 주성분인 화합물로 이루어져 있고 통상 이산화티탄이 약 20~30%를 차지하고 있다. 본 발명에서는 폐 이산화티탄 슬러지에 이산화티탄이 10%이상 함유된 것이면 적용이 가능하다. 유리 부산물은 실리카의 함량이 65~75%, 칼슘 산화물이 3~10% 이상, 기타 알칼리 성분이 10~15%를 차지하고 있다. 점토질 원료는 실리카, 알루미나, 칼슘 산화물이 전체 조성의 80% 이상을 차지하고 있다. Titanium dioxide sludge is composed of compounds mainly composed of calcium, iron, and titanium, and usually titanium dioxide accounts for about 20-30%. In the present invention, it is applicable if the waste titanium dioxide sludge contains 10% or more of titanium dioxide. Glass by-products comprise 65-75% of silica, 3-10% or more of calcium oxide, and 10-15% of other alkali components. In clay materials, silica, alumina, and calcium oxide account for more than 80% of the total composition.
폐 이산화티탄 슬러지 20-60중량%, 유리 부산물 10-30중량%, 점토질 원료 10-70중량%로 구성되는 조성물 100중량부를 혼합한 다음, 물을 5-30중량부 가하고 볼밀을 이용하여 혼합 분쇄한다. 100 parts by weight of a composition consisting of 20-60% by weight of waste titanium dioxide sludge, 10-30% by weight of glass by-products and 10-70% by weight of clay raw materials are mixed, and then 5-30 parts by weight of water is added and mixed and ground using a ball mill. do.
혼합 분쇄된 상기 조성물은 프레스나 압출기를 이용하여 성형한다.The mixed and ground composition is molded by using a press or an extruder.
성형물은 통상의 건자재의 제조방법과 같이 건조과정을 거친 후 소성과정을 거치게 된다. 본 발명에서의 소성온도는 950-1150℃의 범위가 적절하다.The molded product is subjected to a firing process after drying, as in the manufacturing method of a conventional building material. The firing temperature in the present invention is preferably in the range of 950-1150 占 폚.
본 발명의 실시예는 아래와 같다.An embodiment of the present invention is as follows.
아래 실시예들은 조성식에 따라 준비된 세 가지 원료를 혼합한 후 원형 몰드(내경 36 x 높이 60 mm)에 10g 의 원료들을 넣어 88kgf/mm2의 힘으로 상하 가압하여 성형하였다. 가압 유지 시간은 1분으로 하였다. 성형된 시편은 전기로를 이용하여 소성하였다. 소성은 산화, 중성, 환원 분위기(일산화탄소, 질소, 공기)에서 실시하였다. 소결시 로(furnace)의 온도를 400℃까지 승온 시킨 후 가스를 주입하였다. 일정온도에서 1시간 동안 유지시킨 후 가스 주입을 차단하고 자연적으로 냉각하였다. 소결 온도는 950-1150℃ 범위에서 실시하였다. The following examples were molded by mixing the three raw materials prepared according to the composition formula and then pressurized up and down with a force of 88kgf / mm 2 put 10g of raw materials in a circular mold (inner diameter 36 x height 60 mm). Pressurized holding time was 1 minute. The molded specimen was fired using an electric furnace. Firing was carried out in an oxidation, neutral, and reducing atmosphere (carbon monoxide, nitrogen, air). During sintering, the furnace was heated up to 400 ° C and gas was injected. After maintaining for 1 hour at a constant temperature, the gas injection was blocked and naturally cooled. Sintering temperature was carried out in the range of 950-1150 ℃.
소결 시편의 흡수율과 밀도는 KS규격 (KS L-4008)에 의하여 측정하였다. 증류수가 담긴 용기 속에 소결시편을 넣고 5시간동안 끓인 다음 냉각하였다. 포화된 시료를 물속 상태에서 각 시료의 무게를 0.01g까지 정확히 측정하여 수중 무게 w2로 표시하였다. 증류수로 포화된 시료를 꺼내 젖은 천으로 표면을 가볍게 닦고 0.01g까지 정확하게 무게를 달아 포수 무게 w3으로 표기하였다. 포수된 시료는 110℃의 오븐에서 항량이 될 때까지 건조하고 데시케이터 속에서 냉각시킨 다음 0.01g까지 측정할 수 있는 저울로 정확히 무게를 달아 w1로 하였다. 밀도의 계산은 건조된 시료의 무게를 포수무게와 수중무게의 차로 나누어 값으로 계산되어진다.Absorption rate and density of the sintered specimens were measured by KS standard (KS L-4008). The sintered specimen was placed in a container containing distilled water, boiled for 5 hours, and cooled. Saturated samples were accurately weighed to 0.01 g in water and expressed in water weight w 2 . A sample saturated with distilled water was taken out, and the surface was lightly wiped with a damp cloth, weighed accurately to 0.01 g, and labeled as catcher weight w 3 . The catcher was dried in an oven at 110 ° C. until weighed, cooled in a desiccator, and weighed exactly to a weight of 1 g with a weighing scale of 0.01 g. The density is calculated by dividing the weight of the dried sample by the difference between the catcher's weight and the underwater weight.
<실시예 1><Example 1>
TiO2 슬러지 40-60%, 유리 부산물 10-30%, 점토질 원료 30-50% 범위에서 볼밀을 이용하여 배합한 후 가압 성형하여 무기패널을 제조하였다. 소지의 조성은 도2와 같이 점토-장석-규석의 삼성분계로 나타내었다. 제조한 시편은 산화분위기하에서 1050oC에서 1시간동안 소성하였다. 실시예에 사용된 시편을 폐기물공정시험법으로 중금속 용출실험을 진행한 결과 납, 카드뮴, 크롬, 수은은 불검출 되었고, 구리(0.02 ppm)만 극소량 검출되어 관련기준을 충족시키는 물성을 갖고 있음을 확인 하였다. 무기패널의 흡수율은 15.4-23.5%, 밀도는 1.6-2.1g/ml를 나타냈고 표면은 황색 또는 황갈색을 띠었다.Inorganic panels were prepared by blending 40-60% of TiO 2 sludge, 10-30% of glass by-products, and 30-50% of clay raw materials using a ball mill. The composition of the body is represented by the Samsung demarcation of clay-feldspar-gyuseok as shown in FIG. The prepared specimens were calcined at 1050 ° C. for 1 hour under an oxidizing atmosphere. As a result of the heavy metal dissolution test using the waste process test method for the sample used in the example, lead, cadmium, chromium, and mercury were not detected, and only a small amount of copper (0.02 ppm) was detected to have properties satisfying the relevant standards. It was. The absorption rate of the inorganic panel was 15.4-23.5%, the density was 1.6-2.1g / ml, and the surface was yellow or yellowish brown.
도 3은 소지 조성 변화에 따른 소결체의 미세구조를 정리한 것이다. 소지 조성중 장석양을 고정하고 (a,b,c) 규석의 양을 증가시킬 경우 (점토량은 감소) 미세구조에서 기공의 크기와 기공률이 증가하는 것을 알 수 있다. 그러나 일정한 규석 량에서(a,d,e) 장석량을 증가시킬 경우 시편의 미세구조로는 뚜렷한 차이를 판단할 수 없었다. Figure 3 summarizes the microstructure of the sintered body according to the change in the base composition. When the amount of feldspar is fixed and the amount of (a, b, c) silica is increased (reduced clay amount), it can be seen that the pore size and porosity increase in the microstructure. However, when the amount of feldspar was increased at a certain amount of silica (a, d, e), the microstructure of the specimen could not determine the difference.
<실시예 2> <Example 2>
실시예 2에서는 TiO2 슬러지 40-60%, 유리 부산물 10-20%, 점토질 원료 40-50%의 조성으로 볼밀을 이용하여 배합한 후 가압 성형하여 무기패널을 제조하였다. 소지의 조성은 그림 2와 같이 점토-장석-규석의 삼성분계로 나타내었다. 제조한 시편은 환원(일산화탄소 4% 이상)분위기하에서 1050 oC에서 1시간동안 실시하였다. 환원분위기에서 흡수율은 12.4-13.5%, 밀도는 2.3g/ml을 나타냈다. In Example 2, an inorganic panel was prepared by mixing with a ball mill in a composition of 40-60% of TiO 2 sludge, 10-20% of glass by-products, and 40-50% of clay raw materials. The composition of the body is represented by the Samsung demarcation of clay-feldspar-gyuseok, as shown in Figure 2. The prepared specimens were run at 1050 ° C. for 1 hour under a reducing (at least 4% carbon monoxide) atmosphere. Absorption was 12.4-13.5% and density was 2.3g / ml in the reducing atmosphere.
<실시예 3><Example 3>
실시예 3에서는 TiO2 슬러지 40%, 유리 부산물 20%, 점토질 원료 40%의 조성으로 볼밀을 이용하여 배합한 후 가압 성형하여 무기패널을 제조하였다. 소지의 조성은 그림 2와 같이 점토-장석-규석의 삼성분계로 나타내었다. 제조한 시편은 950-1150oC 범위에서 산화 분위기하에서 1시간동안 소성하였다. 소성온도 950oC에서 높은 흡수율(28.2%)과 낮은 밀도(1.5g/ml)를 나타내고 있지만 강도는 낮았다. 반면 1050oC에서 고강도 경량의 무기패널을 제조할 수 있었다. In Example 3, an inorganic panel was prepared by blending a ball mill using a composition of 40% TiO 2 sludge, 20% glass byproduct, and 40% clay material. The composition of the body is represented by the Samsung demarcation of clay-feldspar-gyuseok, as shown in Figure 2. The prepared specimen was calcined for 1 hour in an oxidizing atmosphere in the range of 950-1150 o C. The high absorption rate (28.2%) and low density (1.5g / ml) were obtained at the firing temperature of 950 ° C, but the strength was low. On the other hand, high-strength lightweight inorganic panels could be manufactured at 1050 o C.
<비교예 1>Comparative Example 1
TiO2 슬러지 40-60%, 유리 부산물 30-50%, 점토질 원료 10-30% 범위에서 실 시예 1과 동일한 조건에서 가압 성형하여 무기패널을 제조하였다. 제조한 시편은 산화분위기하에서 1050oC에서 1시간동안 소성하였다. 무기패널은 끓음 현상으로 시편표면이 매우 불규칙하였고, 형상도 변형되어 패널을 만드는데 적절치 않았다. Inorganic panels were manufactured by pressing under the same conditions as in Example 1 in the range of 40-60% of TiO 2 sludge, 30-50% of glass by-products, and 10-30% of clay raw materials. The prepared specimens were calcined at 1050 ° C. for 1 hour under an oxidizing atmosphere. Inorganic panels were boiled, and the specimen surface was very irregular, and the shape was also deformed, making them unsuitable for making panels.
<비교예 2>Comparative Example 2
비교예 2에서는 실시예 3과 동일조성으로 볼밀을 이용하여 배합한 후 가압 성형하여 무기패널을 제조하였다. 제조한 시편은 900oC와 1200oC에서 각각 산화 분위기하에서 1시간동안 소성하였다. 900oC에서 소성된 시편은 높은 흡수율을 보였지만 소결이 이루어지지 않아 약간의 압력만으로 시편이 부서졌고, 1200oC에서 소성한 시편은 지나치게 수축이 많이 일어나 형상변형이 심했다. In Comparative Example 2, an inorganic panel was prepared by blending using a ball mill in the same composition as in Example 3 and then pressing. The prepared specimens were calcined at 900 o C and 1200 o C for 1 hour in an oxidizing atmosphere, respectively. The specimens fired at 900 o C showed high absorption, but the specimens were broken by only a little pressure due to no sintering, and the specimens fired at 1200 o C suffered from excessive shrinkage, resulting in severe deformation.
본 발명에서는 광촉매 및 페인트 첨가제로 주로 이용되는 이산화티탄 제조공정 중 발생하는 폐기물인 이산화티탄 슬러지와 유리 부산물, 점토질 원료를 활용하여 무기패널을 제조한다. 구체적으로 폐 이산화티탄과 점토질 원료, 유리부산물을 혼합분쇄(볼밀 또는 롤크러셔)하고, 수분을 조정한 후 무기패널을 프레스 또는 압출하여 제조하였다. 제조된 무기패널은 폐자원을 활용하는 장점과 폐 이산화티탄에 포함된 유기 물질로 인해 경량화가 가능하고, 이산화티탄의 발색으로 무기패널의 색을 조절할 수 있다. 사용된 유리부산물은 알카리 금속이 다량 함유되어 있어 소성시 저온에서 치밀화되어 무기패널을 제조하는데 적은 에너지로 소성이 가능하다. In the present invention, an inorganic panel is manufactured by using titanium dioxide sludge, glass by-products, and clay raw materials, which are wastes generated during a titanium dioxide manufacturing process mainly used as a photocatalyst and a paint additive. Specifically, waste titanium dioxide, clay material, and glass by-products were mixed and ground (ball mill or roll crusher), and after adjusting moisture, an inorganic panel was prepared by pressing or extruding. The manufactured inorganic panel can be lightened due to the advantages of utilizing waste resources and organic materials contained in waste titanium dioxide, and the color of the inorganic panel can be adjusted by the color of titanium dioxide. The glass by-product used contains a large amount of alkali metal, so it is densified at low temperature during firing, and thus it can be fired with little energy to prepare an inorganic panel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR0148343B1 (en) * | 1988-07-26 | 1998-11-02 | 알프레드 페르나트 | Sintered high titanium aglomerates |
| US5830251A (en) | 1996-04-10 | 1998-11-03 | Vortec Corporation | Manufacture of ceramic tiles from industrial waste |
| US5989331A (en) | 1996-05-28 | 1999-11-23 | Southern Clay Products, Inc. | TiO2 slurry stabilization |
| KR100501214B1 (en) | 2003-01-17 | 2005-07-18 | 주식회사 성현퍼라이트 | A method for producing lightweight material based on perite powder and yellow earth |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR0148343B1 (en) * | 1988-07-26 | 1998-11-02 | 알프레드 페르나트 | Sintered high titanium aglomerates |
| US5830251A (en) | 1996-04-10 | 1998-11-03 | Vortec Corporation | Manufacture of ceramic tiles from industrial waste |
| US5989331A (en) | 1996-05-28 | 1999-11-23 | Southern Clay Products, Inc. | TiO2 slurry stabilization |
| KR100501214B1 (en) | 2003-01-17 | 2005-07-18 | 주식회사 성현퍼라이트 | A method for producing lightweight material based on perite powder and yellow earth |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101379541B1 (en) | 2013-10-23 | 2014-03-28 | 고광식 | Preparation method of construct materials using wasted water sludge |
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