KR960002620B1 - Elevating method of utility value of kaoline using waste fluoric acid - Google Patents
Elevating method of utility value of kaoline using waste fluoric acid Download PDFInfo
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- KR960002620B1 KR960002620B1 KR1019920020684A KR920020684A KR960002620B1 KR 960002620 B1 KR960002620 B1 KR 960002620B1 KR 1019920020684 A KR1019920020684 A KR 1019920020684A KR 920020684 A KR920020684 A KR 920020684A KR 960002620 B1 KR960002620 B1 KR 960002620B1
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- kaolin
- hydrofluoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- Processing Of Solid Wastes (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
제1도는 본 발명에서 사용한 내산성 교반반응조의 개략도를 도시한 것이고,FIG. 1 shows a schematic diagram of an acid resistant stirring reactor used in the present invention.
제2도는 카올린의 폐불산 처리시간에 따른 X-선 회절 분석결과를 그래프로 도시한 것으로서 (a)는 4시간 (b)8시간 (c)12시간 및 (d)16시간을 불산처리한 것이며,(● : AlF3·3H2O, ∇ : Al2Si2O5(OH)4, ○ : SiO2)Figure 2 shows the results of X-ray diffraction analysis according to the hydrofluoric acid treatment time of kaolin, (a) is hydrofluoricated for 4 hours (b) 8 hours (c) 12 hours and (d) 16 hours , (●: AlF 3 · 3H 2 O, ∇: Al 2 Si 2 O 5 (OH) 4 , ○: SiO 2 )
제3도는 불산처리 후 열처리가 완료된 상태에서 뮬라이트(m)생성을 그래프로 도시한 것으로서 (a)는 12시간 불산처리 후 열처리를 한 것이고, (b)는 16시간 불산처리 후 열처리를 한 것이다.3 is a graph showing the mullite (m) generation in a state in which the heat treatment after the hydrofluoric acid treatment is completed, (a) is a heat treatment after hydrofluoric acid treatment for 12 hours, (b) is a heat treatment after hydrofluoric acid treatment for 16 hours.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : PVC 반응기 2 : 패킹 워터(packing water)1: PVC reactor 2: packing water
3 : 카올린와 폐불산의 혼합물3: mixture of kaolin and waste hydrofluoric acid
본 발명은 폐불산을 이용한 카올린의 부가가치 향상방법에 관한 것으로, 좀 더 구체적으로는 폐불산으로 카올린을 처리, 건조 및 하소하므로서 카올린에서 SiO2및 불순물을 제거하여 뮬라이트(mullite)나 고알루미나 원료를 제조하는 카올린의 부가가치 향상방법에 관한 것이다.The present invention relates to a method for improving the added value of kaolin using waste hydrofluoric acid, and more specifically, to remove mullite or high alumina raw material by removing SiO 2 and impurities from kaolin by treating, drying and calcining kaolin with waste hydrofluoric acid. It relates to a method for improving the added value of kaolin to be produced.
일반적으로 유리, 제철 공업 등에서 세척제등으로 불산을 다량 사용하기 때문에 이로인한 폐불산 처리를 위해 많은 경비를 들여 폐기물 처리시설을 가동시키고 있는 실정이다. 이에 본 발명자는 폐불산을 유용하게 활용할 수 있는 방법을 연구한 결과 카올린에서 SiO2및 불순물을 제거시키므로서 상당한 부가가치를 도출시킬 수 있게 되었다.In general, since the glass, steel industry, etc. use a large amount of hydrofluoric acid as a cleaning agent, the waste treatment facility is operated at a high cost for waste hydrofluoric acid treatment. Accordingly, the present inventors have studied a method of utilizing waste hydrofluoric acid, and as a result, it is possible to derive considerable added value by removing SiO 2 and impurities from kaolin.
따라서 본 발명의 목적은 폐불산을 카올린의 정제에 사용하므로서 폐기물 처리시설에 드는 비용을 감소시키면서 고순도의 뮬라이트를 얻을 수 있는 방법을 제공하는데 그 목적이 있다.Accordingly, an object of the present invention is to provide a method for obtaining high purity mullite while reducing the cost of waste treatment facilities by using waste hydrofluoric acid for the purification of kaolin.
상술한 목적을 달성하기 위하여 내산성 반응용기에서 카올린과 폐불산을 반응시킨 뒤 건조시키고 하소하므로서 Al2O3함량을 뮬라이트 조성 이상으로 높일 수 있었다.In order to achieve the above object, by reacting kaolin and waste hydrofluoric acid in an acid resistant reactor, drying and calcining, the Al 2 O 3 content could be increased beyond the mullite composition.
본 발명을 좀 더 상세히 설명하면 다음과 같다.The present invention is described in more detail as follows.
카올린을 불산으로 처리하게 되면 카올린의 결정구조가 완전히 와해되어 주로 AIF3·3H2O와 SiF4가 생기게 된다.Treatment of kaolin with hydrofluoric acid completely disrupts the crystal structure of kaolin, resulting in AIF 3 · 3H 2 O and SiF 4 .
먼저 200메쉬를 통과시킨 카올린 분말(그 분석치는 하기 표1에 기재)과 그 함량의 2~4배에 해당하는 약 10% 농도의 폐불산 수용액을 내산성 교반반응조에 넣고 150~300rpm으로 12~24시간 반응시킨다.First, the kaolin powder which passed 200 mesh (the analysis value is shown in Table 1 below) and the waste hydrofluoric acid solution of about 10% concentration corresponding to 2 to 4 times its content were put into the acid resistant stirring reactor and it was 12 to 24 at 150 to 300 rpm. React time.
[표 1]TABLE 1
상기 반응시킨 침전 생성물은 플라스틱 여과장치내의 여과지를 통과, 걸러서 분리시켜서 120℃로 유지시킨 건조기내에서 24시간 건조시켰다.The reacted precipitated product was passed through a filter paper in a plastic filtration device, separated by filtration, and dried in a drier maintained at 120 ° C for 24 hours.
상기 건조분말은 0.5㎏/㎠의 낮은 압력에서 지름 10㎜, 높이 약 5㎜의 디스크형 성형체를 만들어 칸탈(kanthal) 발열체를 사용한 전기로에서 700~800℃에서 1.5~3시간 동안 하소하였다. 이때 상기 하소시간이 700℃ 미만이면 미반응물이 남아 있는 문제가 있고 800℃를 초과하면 비경제적인 문제가 있다.The dry powder was made into a disk shaped body having a diameter of 10 mm and a height of about 5 mm at a low pressure of 0.5 kg / cm 2 and calcined for 1.5 to 3 hours at 700 to 800 ° C. in an electric furnace using a kanthal heating element. At this time, if the calcination time is less than 700 ℃ there is a problem that remains unreacted, if it exceeds 800 ℃ there is an uneconomic problem.
하기의 실시예 및 비교예는 본 발명의 효능, 효과를 좀 더 구체적으로 설명하는 것이지, 본 발명의 범주를 한정하는 것은 아니다.The following examples and comparative examples will be described in more detail the efficacy, effect of the present invention, but not to limit the scope of the present invention.
[실시예 1]Example 1
먼저 경남 서부지역의 하동산 도색 카올린을 200메쉬(74㎛)체를 통과시킨 후 건조시킨 분말 1㎏과 6.3wt%의 불산 수용액 약 1㎏을 내산성 교반반응조에 넣고 200rpm의 회전속도로 12시간 동안 처리하였다.First, 1 kg of dried powder and 1 kg of 6.3 wt% hydrofluoric acid aqueous solution were put into an acid resistant stirring reactor after passing 200 mesh (74㎛) sieve of Hadongsan-painted kaolin in western Gyeongnam Province for 12 hours at a rotational speed of 200 rpm. Treated.
반응시킨 침전 생성물은 플라스틱 여과장치내의 여과지를 통과, 걸러서 분리시켜서 120℃로 유지시킨 건조기내에서 약 24시간 건조시켰다.The reacted precipitated product was passed through a filter paper in a plastic filtration device, separated by filtration, and dried in a drier maintained at 120 ° C for about 24 hours.
상기 생성물을 X-회절 분석기로 30kV-l5mA, 스켄 스피드 2θ/min, 2000 CPS의 조건하에서 분말 X-선 회절 분석을 행하여 그 결과를 제2도에 도시하였다.(제2c도)The product was subjected to powder X-ray diffraction analysis with an X-diffraction analyzer under conditions of 30 kV-1 5 mA, scan speed 2θ / min, 2000 CPS, and the result is shown in FIG. 2 (FIG. 2C).
불산처리한 카올린의 건조분말은 0.5㎏/㎠의 낮은 압력에서 지름 10㎜, 높이 약 5㎜의 디스크형 성형체를 만들어 칸탈(kanthal) 발열체를 사용한 전기로에서 800℃의 온도에서 2시간 동안 하소하였다.The dry powder of hydrofluoric acid treated kaolin was made into a disk shaped body having a diameter of 10 mm and a height of about 5 mm at a low pressure of 0.5 kg / cm 2 and calcined at 800 ° C. for 2 hours in an electric furnace using a kanthal heating element.
그 결과 뮬라이트의 생성을 X-회절 분석기로 분석하여 제3a도에 도시하였다.As a result, the production of mullite was analyzed by X-diffraction analyzer and shown in FIG. 3a.
[실시예 2]Example 2
카올린을 폐불산으로 처리하는 시간을 16시간으로 한 것을 제외하고는 상기 실시예 1과 동일하게 불산처리하고 건조시킨 생성물을 X-선 회절 분석을 행하여 그 결과를 제2도에 도시하였다. (제2d도)X-ray diffraction analysis was performed on the product of hydrofluoric acid treated and dried in the same manner as in Example 1 except that the time for treating kaolin with waste hydrofluoric acid was 16 hours, and the result is shown in FIG. (Figure 2d)
그 후에 상기 실시예 1과 동일하게 열처리하여 뮬라이트의 생성을 X-회절 분석기로 분석하여 제3b도에 도시하였다.Thereafter, heat treatment was performed in the same manner as in Example 1, and the production of mullite was analyzed by an X-diffraction analyzer, and is shown in FIG. 3b.
[비교예 1]Comparative Example 1
카올린을 폐불산으로 처리하는 시간을 4시간으로 한 것을 제외하고는 상기 실시예1과 동일하게 실시하였다.The same procedure as in Example 1 was carried out except that the time for treating kaolin with waste hydrofluoric acid was 4 hours.
상기 생성물을 X-선 회절 분석을 행하여 그 결과를 제2도에 도시하였다. (제2a도) 상기 생성물은 열처리하여도 수율이 나쁘므로 열처리할 필요가 없다.The product was subjected to X-ray diffraction analysis and the results are shown in FIG. (FIG. 2A) The product is poor in yield even when heat treated, and thus does not need to be heat treated.
[비교예 2]Comparative Example 2
카올린을 폐불산으로 처리하는 시간을 8시간으로 한 것을 제외하고는 상기 실시예 1과 동일하게 실시하였다.The same procedure as in Example 1 was carried out except that the time for treating kaolin with waste hydrofluoric acid was 8 hours.
상기 생성물을 X-선 회절 분석을 행하여 그 결과를 제2도에 도시하였다. (제1b도) 상기 생성물도 비교예 1과 같은 이유로 열처리하지 않았다.The product was subjected to X-ray diffraction analysis and the results are shown in FIG. (Fig. 1b) The product was not heat treated for the same reason as in Comparative Example 1.
본발명에 의하여 카올린을 폐불산을 이용하여 효과적으로 처리하여 고순도에 뮬라이트를 얻을 수 있었다.According to the present invention, kaolin was effectively treated with waste hydrofluoric acid to obtain mullite at high purity.
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| KR1019920020684A KR960002620B1 (en) | 1992-11-05 | 1992-11-05 | Elevating method of utility value of kaoline using waste fluoric acid |
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| KR1019920020684A KR960002620B1 (en) | 1992-11-05 | 1992-11-05 | Elevating method of utility value of kaoline using waste fluoric acid |
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| KR960002620B1 true KR960002620B1 (en) | 1996-02-24 |
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