KR20100041183A - Method for leaching magnesium and preparing glass water using sulfuric acid from nickel-slag - Google Patents
Method for leaching magnesium and preparing glass water using sulfuric acid from nickel-slag Download PDFInfo
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- KR20100041183A KR20100041183A KR20080100235A KR20080100235A KR20100041183A KR 20100041183 A KR20100041183 A KR 20100041183A KR 20080100235 A KR20080100235 A KR 20080100235A KR 20080100235 A KR20080100235 A KR 20080100235A KR 20100041183 A KR20100041183 A KR 20100041183A
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- leaching
- magnesium
- sulfuric acid
- silica
- water glass
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- 238000002386 leaching Methods 0.000 title claims abstract description 117
- 239000011777 magnesium Substances 0.000 title claims abstract description 62
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 61
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000002893 slag Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title description 5
- 239000011521 glass Substances 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 96
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 79
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 74
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 42
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 37
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 16
- 239000011707 mineral Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 8
- 229910017625 MgSiO Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052742 iron Inorganic materials 0.000 abstract description 8
- 238000000605 extraction Methods 0.000 abstract description 5
- 239000004575 stone Substances 0.000 abstract description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 29
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 27
- 238000004090 dissolution Methods 0.000 description 19
- 229910004298 SiO 2 Inorganic materials 0.000 description 16
- 230000000694 effects Effects 0.000 description 14
- 239000000395 magnesium oxide Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 235000010755 mineral Nutrition 0.000 description 13
- 239000011734 sodium Substances 0.000 description 13
- 239000012535 impurity Substances 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000007922 dissolution test Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000003337 fertilizer Substances 0.000 description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 3
- 235000019341 magnesium sulphate Nutrition 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000009628 steelmaking Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000009091 Cordyline terminalis Nutrition 0.000 description 1
- 244000289527 Cordyline terminalis Species 0.000 description 1
- 229910002483 Cu Ka Inorganic materials 0.000 description 1
- 241001016380 Reseda luteola Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/04—Alkali metal or ammonium silicate cements ; Alkyl silicate cements; Silica sol cements; Soluble silicate cements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
Description
본 발명은 니켈 슬래그로부터 황산을 이용한 마그네슘의 침출 및 물유리의 제조방법에 관한 것이다.The present invention relates to a leaching of magnesium using sulfuric acid from nickel slag and a method for producing water glass.
슬래그(slag)란 광재(鑛滓)라고도 하는데, 제강(製鋼)에서는 특히 이것을 강재(鋼滓)라고 한다. 광석에서 금속을 빼내는 데는 광석 속에 있는 불필요한 성분을 녹기 쉬운 화합물로 만든 다음 제거하는 방법이 일반적으로 사용된다. 슬래그는 철광석에서 철을 뽑아내고 남는 돌로, 칼슘과 철 함량이 일반 자연 골재보다 높다.Slag is also called slag. In steelmaking, this is called steel. In order to remove metal from the ore, it is common to make unnecessary components in the ore into soluble compounds and then remove them. Slag is a stone that remains after extracting iron from iron ore and has higher calcium and iron content than natural aggregates.
또한, 제강 공정 중 발생하는 슬래그는 일반적으로 실리카로 알려진 이산화규소(SiO2)를 다량 포함하고 있다. 슬래그는 산성이며, 제강 공정의 막바지에 슬래 그의 산화마그네슘 성분이 5% 내지 7%인 것으로 관찰되었다.In addition, the slag generated during the steelmaking process contains a large amount of silicon dioxide (SiO 2 ), commonly known as silica. The slag is acidic, and at the end of the steelmaking process it was observed that its magnesium oxide component is 5% to 7%.
이와 같은 슬래그에는 다량의 마그네슘 성분이 함유되고 있음에도 이로부터 마그네슘을 추출하는 공정은 개발되어 있지 않다.Although such slag contains a large amount of magnesium component, no process for extracting magnesium from it has been developed.
이에, 본 발명자들은 슬래그 중에서 니켈을 함유하는 니켈 슬래그로부터 마그네슘을 추출하는 공정을 개발하고, 아울러, 마그네슘 침출 후의 잔사인 실리카로부터 물유리를 제조하는 방법을 개발함으로써 본 발명을 완성하였다.Therefore, the present inventors have completed the present invention by developing a process for extracting magnesium from nickel slag containing nickel in the slag, and also developing a method for producing water glass from silica which is a residue after magnesium leaching.
본 발명의 목적은 니켈 슬래그로 마그네슘을 추출하고, 침출 후의 잔사인 실리카로부터 물유리를 제조하는 방법을 제공하는 것이다.It is an object of the present invention to provide a method for extracting magnesium with nickel slag and producing water glass from silica which is a residue after leaching.
상기 목적을 달성하기 위하여, 본 발명은 ⅰ) 마그네슘이 함유된 니켈 슬래그(MgSiO3)와 황산을 반응시켜 MgSO4 및 실리카를 제조하는 단계; ⅱ) 상기 MgSO4를 CO2와 반응시켜 MgCO3를 제조하는 단계; 및 ⅲ) 상기 ⅰ) 단계의 실리카를 NaOH와 반응시켜 물유리를 제조하는 단계;를 포함하는 니켈 슬래그로부터 황산을 이용한 마그네슘의 침출 및 물유리의 제조방법을 제공한다.In order to achieve the above object, the present invention comprises the steps of iii) preparing MgSO 4 and silica by reacting magnesium slag (MgSiO 3 ) and sulfuric acid containing magnesium; Ii) reacting the MgSO 4 with CO 2 to produce MgCO 3 ; And iii) reacting the silica of step iii) with NaOH to produce a water glass. The method of claim 1 provides a method for producing magnesium and leaching magnesium using sulfuric acid from nickel slag.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명의 마그네슘의 침출 및 물유리의 제조방법에 있어서, 상기 황산은 1.0 내지 6.0 M인 것이 바람직하고, 상기 ⅰ) 단계의 MgSO4 제조는 50~90℃의 침출온도 10~60분의 침출시간, 50~250 g/ℓ의 광액농도 및 300~4000 rpm의 교반속도에서 이루어지는 것이 바람직하며, 4.0 M 황산, 90℃의 침출온도, 60분의 침출시간, 200 g/ℓ의 광액농도 및 3000 rpm의 교반속도에서 이루어지는 것이 가장 바람직하다.In the leaching of magnesium of the present invention and the method for producing water glass, the sulfuric acid is preferably 1.0 to 6.0 M, the MgSO 4 production of step iii) leaching time of 10 to 60 minutes leaching temperature of 50 ~ 90 ℃, It is preferably made at a mineral liquid concentration of 50-250 g / l and a stirring speed of 300-4000 rpm, and it is preferably 4.0 M sulfuric acid, a leaching temperature of 90 ° C., a leaching time of 60 minutes, a mineral liquid concentration of 200 g / l and a 3000 rpm. Most preferably at a stirring speed.
또한, 본 발명의 마그네슘의 침출 및 물유리의 제조방법에 있어서, 상기 NaOH는 2.5 내지 5.0 M인 것이 바람직하고, 상기 ⅲ) 단계의 물유리 제조는 25~90℃의 반응온도, 5~30분의 반응시간 및 300~700 g/ℓ의 광액농도에서 이루어지는 것이 바람직하다.In addition, in the leaching of magnesium of the present invention and the method for producing water glass, the NaOH is preferably 2.5 to 5.0 M, the water glass production of step iii) the reaction temperature of 25 ~ 90 ℃, reaction of 5 to 30 minutes It is preferable to make it at time and mineral liquid concentration of 300-700 g / L.
본 발명의 마그네슘의 침출 및 물유리의 제조는 마그네슘을 다량함유하는 니켈 슬래그를 황산을 이용하여 MgSiO3를 MgO 및 SiO2로 분해시키고, 아울러, MgO는 환상과 반응하여 MgSO4로 전환된다. 상기 MgSO4는 액상 및 고상의 비료를 제조하는데 사용될 수 있다. 구체적으로, MgSO4는 CO2와 반응시켜 CO2 고정 반응에 의하여 비료원료인 MgCO3를 제조할 수 있다.The leaching of magnesium and the preparation of water glass of the present invention decompose MgSiO 3 to MgO and SiO 2 by using sulfuric acid to decompose a large amount of magnesium slag, and MgO is converted to MgSO 4 by reaction with a ring. The MgSO 4 can be used to prepare liquid and solid fertilizers. Specifically, MgSO 4 may be fixed by the CO 2 reaction is reacted with CO 2 producing a fertilizer raw material it is MgCO 3.
한편, 앞서 분해된 SiO2로부터 실리카를 제조할 수 있는데, 실리카 자체는 단열재, 세라믹 및 비료 원료로 사용될 수 있다. 또한, 실리카는 본 발명과 같이 NaOH와 반응시켜 물유리를 제조하는데 사용될 수 있다.On the other hand, silica can be prepared from the previously decomposed SiO 2 , which can be used as a heat insulating material, a ceramic and a fertilizer raw material. In addition, silica may be used to prepare waterglass by reacting with NaOH as in the present invention.
본 발명은 국내산 니켈슬래그로부터 마그네슘의 산 침출 및 물유리를 제조하는 방법에 관한 것으로, 니켈슬래그의 탄산화에 의한 이산화탄소 격리방법의 실용화를 위하여 마그네슘의 침출의 최적화 및 침출잔사의 활용방안을 제시한다. 구체적으로, 본 발명은 황산을 침출제로 사용하여 황산농도, 침출온도 및 시간, 광액 농도 등이 마그네슘 침출에 미치는 영향을 조사한 결과, 마그네슘의 최적침출 조건은 황산농도; 4.0 M, 침출온도; 90℃, 침출시간; 60분, 광액농도; 200 g/ℓ이었으며, 이때 마그네슘의 침출율은 약 93%였다. 니켈슬래그로부터 마그네슘의 황산침출에 의하여 얻어진 침출잔사는 최대 비표면적이 320 ㎡/g인 다공성으로서 실리카 함량이 약 78%이었으며, 이를 가성소다 용액에 용해하여 물유리를 제조할 수 있었다. 가성소다의 농도, 반응온도 및 시간, 광액농도 등과 같은 실험변수들이 침출잔사의 용해에 미치는 영향을 조사한 결과, 상온에서 SiO2/Na2O 비가 3.85인 물유리를 얻을 수 있었다.The present invention relates to an acid leaching of magnesium from domestic nickel slag and a method for producing water glass, and to optimize the leaching of magnesium and to utilize the leaching residue for the practical use of carbon dioxide sequestration method by carbonation of nickel slag. Specifically, the present invention is to investigate the effect of sulfuric acid concentration, leaching temperature and time, mineral concentration, etc. on the leaching of magnesium using sulfuric acid as a leaching agent, the optimum leaching conditions of magnesium is sulfuric acid concentration; 4.0 M, leaching temperature; 90 ° C., leaching time; 60 minutes, mineral solution concentration; 200 g / l, at which the leaching rate of magnesium was about 93%. The leaching residue obtained by leaching magnesium sulfate from nickel slag was porous with a maximum specific surface area of 320 m 2 / g and had a silica content of about 78%, which was dissolved in a caustic soda solution to prepare a water glass. Results experimental parameters, such as concentration, reaction temperature and time, pulp density of the caustic soda to investigate the effect on dissolution of the leach residue, to obtain a SiO 2 / Na 2 O ratio of 3.85 of water glass at room temperature.
본 발명은 철광석에서 철을 뽑아내고 남는 돌인 슬래그로부터 다량 존재하는 마그네슘을 추출하는 방법 및 추출후 남은 잔사인 실리카로부터 물유리를 제조하는 방법을 제공한다.The present invention provides a method for extracting a large amount of magnesium from the slag, which is the iron that is extracted from iron ore and the remaining stone, and a method for producing water glass from the silica remaining after the extraction.
이하, 본 발명을 하기 실시예 및 비교예에 의거하여 보다 상세하게 설명하고자 한다. 단, 하기 실시예 및 비교예는 본 발명을 예시하기 위한 것일 뿐, 본 발명은 하기 실시예에 의해 한정되는 것이 아니고, 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 치환 및 균등한 타 실시예로 변경할 수 있음은 본 발명이 속 하는 기술분야에서 통상의 지식을 가진 자에게 있어서 명백할 것이다. Hereinafter, the present invention will be described in more detail based on the following Examples and Comparative Examples. However, the following Examples and Comparative Examples are only for illustrating the present invention, the present invention is not limited by the following Examples, and substituted and other equivalent examples within the scope without departing from the technical spirit of the present invention Changes will be apparent to those of ordinary skill in the art.
<실시예 1> 니켈 슬래그의 성분 분석Example 1 Component Analysis of Nickel Slag
본 발명에서 시료로 사용한 니켈 슬래그는 경북 안동지역에서 입수하였다. 니켈 슬래그로부터 불순물을 제거하기 위하여 파쇄, 분쇄, 분급, 습식자력선별 등 일련의 물리적 전처리를 실시한 다음 시료로 사용하였다. 표 1은 니켈 슬래그 원재료 및 전처리된 시료의 화학 조성을 나타낸 것이다. 본 발명에서 시료로 사용한 전처리된 니켈 슬래그의 주요성분은 32 wt% SiO2, 29 wt% MgO, 18 wt% NiO, 3.05 wt% Fe2O3 등이며 강열감량(1000℃)은 8.90 wt%이었다. 그리고 시료 입도는 -45 ㎛(평균입도; 25.7 ㎛, 비표면적; 22 ㎡/g)이었다. 테스트에 사용한 모든 시약은 1급 또는 특급 시약이었다.Nickel slag used as a sample in the present invention was obtained in Andong, Gyeongbuk. In order to remove impurities from nickel slag, a series of physical pretreatments such as crushing, pulverization, classification, and wet magnetic screening were performed, and then used as a sample. Table 1 shows the chemical composition of the nickel slag raw material and the pretreated samples. The main components of the pretreated nickel slag used as samples in the present invention were 32 wt% SiO 2 , 29 wt% MgO, 18 wt% NiO, 3.05 wt% Fe 2 O 3 , and the loss on ignition (1000 ° C.) was 8.90 wt%. . The sample particle size was -45 µm (average particle size; 25.7 µm, specific surface area; 22 m 2 / g). All reagents used in the tests were first-class or premium reagents.
<실시예 2> 마그네슘 침출Example 2 Magnesium Leaching
니켈 슬래그로부터 마그네슘의 침출은 항온조에 설치한 1000 ㎖의 3구 플라스크를 사용하여 수행하였다. 농도가 조절된 500 ㎖의 3구 플라스크를 사용하여 수행하였다. 농도가 조절된 500 ㎖의 황산을 플라스크에 주입한 다음, 정해진 온도에 도달하면 시료를 투입하여 침출을 진행하였다. 일정시간 마다 용액시료를 채취하여 마그네슘의 분석을 행하고 침출율을 계산하였다. 침출 테스트의 조건은 황산농도; 1.0~6.0 M, 침출온도; 50~90℃, 침출시간; 10~60분, 광액농도; 50~250 g/ℓ이었으며, 교반속도는 300~4000 rpm으로 일정하게 하였다. 침출반응의 종료 후 고액분리를 행하고 증류수를 이용하여 잔사를 3차례 세척하였다. 세척한 잔사를 105℃에서 건조하여 수분을 제거한 다음 비표면적 측정과 화학분석을 행하였다.Leaching of magnesium from nickel slag was carried out using a 1000 ml three-necked flask installed in a thermostat. This was done using a 500 ml three-necked flask with controlled concentration. 500 ml of sulfuric acid having a controlled concentration was injected into the flask, and when the temperature was reached, a sample was added to proceed with leaching. Samples were taken at regular intervals to analyze magnesium and the leaching rates were calculated. The conditions of the leaching test were sulfuric acid concentration; 1.0-6.0 M, leaching temperature; 50-90 ° C., leaching time; 10 to 60 minutes, mineral solution concentration; It was 50-250 g / l, and the stirring speed was made constant at 300-4000 rpm. After completion of the leaching reaction, solid-liquid separation was performed and the residue was washed three times with distilled water. The washed residue was dried at 105 ° C. to remove moisture, and then subjected to specific surface area measurement and chemical analysis.
니켈 슬래그로부터 마그네슘을 추출하기 위한 침출제로 황산을 사용하였을 때, 침출반응식은 다음과 같이 나타낼 수 있다.When sulfuric acid is used as a leaching agent for extracting magnesium from nickel slag, the leaching reaction can be expressed as follows.
MgSiO3 ---> MgO + SiO2 (1)MgSiO 3 ---> MgO + SiO 2 (1)
MgO + H2SO4 ---> MgSO4 + H2O (2)MgO + H 2 SO 4 ---> MgSO 4 + H 2 O (2)
침출반응식에서 보는 바와 같이, 니켈 슬래그로부터 마그네슘의 황산침출 시 미용해 실리카가 침출잔사로 얻어졌다. 도 1은 4.0 M H2SO4 용액에 의한 마그네슘의 침출거동을 나타낸 것이다. 침출온도는 90℃로 고정하고 침출시간을 10~60분으로 변화시키면서 침출 테스트를 수행하였으며, 광액농도는 100 g/ℓ이었다. 마그네슘의 침출반응은 급격히 일어나 침출시간이 10분 경과하였을 때 침출율은 약 82%에 도달하였다. 침출시간이 30분을 경과하였을 때, 침출반응은 거의 종료되어 침출율은 더 이상 증가하지 않았다.As shown in the leaching equation, undissolved silica was obtained as leaching residue upon leaching of magnesium from nickel slag. Figure 1 shows the leaching behavior of magnesium by 4.0 MH 2 SO 4 solution. The leaching temperature was fixed at 90 ° C. and the leaching test was performed while changing the leaching time to 10 to 60 minutes, and the concentration of the mineral solution was 100 g / l. Leaching reaction of magnesium occurred rapidly and leaching rate reached about 82% after 10 minutes of leaching time. When the leaching time passed 30 minutes, the leaching reaction was almost finished and the leaching rate did not increase any more.
도 2는 2.0 M H2SO4 용액으로 니켈 슬래그로부터 마그네슘을 60분간 침출하였을 때 침출온도가 침출율에 미치는 영향을 나타낸 그래프이다. 침출온도의 증가에 따라 마그네슘의 침출율은 증가하였다. 침출온도가 50℃일 때 마그네슘의 침출율은 45% 정도였으나, 침출온도가 90℃로 높아짐에 따라 침출율은 90%로 향상되었다.Figure 2 is a graph showing the effect of leaching temperature on leaching rate when leaching magnesium from nickel slag for 2.0 minutes with 2.0 MH 2 SO 4 solution. As leaching temperature increased, leaching rate of magnesium increased. At leaching temperature of 50 ℃, the leaching rate of magnesium was about 45%, but as leaching temperature was increased to 90 ℃, leaching rate was improved to 90%.
황산 농도가 마그네슘의 침출율에 미치는 영향을 조사하여 도 3에 기재하였다. 침출 테스트 조건은 황산 농도; 1.0~6.0 M, 침출온도; 90℃, 침출시간; 60분이었다. 도 3에서 보는 바와 같이, 황산농도가 증가함에 따라 마그네슘의 침출율은 급격히 증가하였으나, 황산농도가 3.0 M 이상에서 마그네슘의 침출율은 약 92%로 일정하였다.The effect of sulfuric acid concentration on the leaching rate of magnesium was investigated and described in FIG. 3. Leaching test conditions include sulfuric acid concentration; 1.0-6.0 M, leaching temperature; 90 ° C., leaching time; It was 60 minutes. As shown in FIG. 3, the leaching rate of magnesium increased rapidly with increasing sulfuric acid concentration, but the leaching rate of magnesium was constant at about 92% when the sulfuric acid concentration was higher than 3.0 M.
니켈 슬래그로부터 마그네슘의 황산침출의 최적화를 위하여 광액농도가 마그네슘의 침출에 미치는 영향을 조사하여 도 4에 나타내었다. 4.0 M H2SO4 용액을 사용하여 90℃에서 60분간 침출을 행하였다. 광액농도가 50~200 g/ℓ 일 때, 마그네슘의 침출율은 약 91~95%이었으며, 광액농도를 증가함에 따라 침출율이 약간씩 감소하였다. 이상과 같이, 니켈 슬래그로부터 마그네슘의 침출 테스트를 통하여 얻어진 최적침출 조건은 황산농도; 4.0 M, 침출온도; 90℃, 침출시간; 60분, 광액농도; 200 g/ℓ이었다.In order to optimize the leaching of magnesium from nickel slag, the effect of mineral concentration on leaching of magnesium is investigated and shown in FIG. 4. The leaching was carried out at 90 ° C. for 60 minutes using a 4.0 MH 2 SO 4 solution. At 50-200 g / l, the leaching rate of magnesium was about 91-95%, and the leaching rate decreased slightly as the mineral solution concentration increased. As described above, the optimum leaching conditions obtained through leaching test of magnesium from nickel slag are sulfuric acid concentration; 4.0 M, leaching temperature; 90 ° C., leaching time; 60 minutes, mineral solution concentration; 200 g / l.
<실시예 3> 물유리 제조Example 3 Preparation of Water Glass
니켈 슬래그로부터 마그네슘의 황산침출 후 얻어진 잔사를 가성소다에 용해하여 물유리를 제조하는 테스트를 행하였다. 침출잔사는 증류수로 여러번 세척하여 잔류 황산을 완전히 제거한 다음 100℃에서 건조하여 실험에 사용하였다. 물유리 제조 테스트에는 250 ㎖ 테플론 비커를 사용하였다. 농도 및 온도가 조절된 100 ㎖의 가성소다 용액을 비커에 주입한 다음 잔사를 장입하여 교반하면서 용해 테스트를 행하였다. 일정시간 경과 후 고/액분리를 하고, 액체와 고체 중의 Si를 분석하여 잔사의 용해율을 계산하였다. 물유리 제조의 실험조건은 가성소다 농도; 2.5~5.0 M NaOH, 반응온도; 25~90℃, 반응시간; 5~30분, 광액농도; 300~700 g/ℓ이었다. 물유리에 함유되어 있는 불순물을 조사하기 위하여 화학분석을 행하였다.The residue obtained after sulfuric acid leaching of magnesium from nickel slag was melt | dissolved in caustic soda, and the test which manufactured water glass was done. The leach residue was washed several times with distilled water to completely remove the residual sulfuric acid and dried at 100 ℃ was used in the experiment. A 250 ml Teflon beaker was used for the water glass preparation test. A 100 ml caustic soda solution with controlled concentration and temperature was injected into the beaker and then the residue was charged and stirred for dissolution test. After a certain time, solid / liquid separation was performed, and the dissolution rate of the residue was calculated by analyzing Si in the liquid and the solid. Experimental conditions for the preparation of water glass include caustic soda concentration; 2.5-5.0 M NaOH, reaction temperature; 25 to 90 ° C., reaction time; 5-30 minutes, mineral solution concentration; 300-700 g / l. A chemical analysis was conducted to investigate the impurities contained in the water glass.
니켈 슬래그와 침출잔사의 상분석에는 X-선 회절기(X-ray Diffractometer, Philips Xpert-MPD coupled with a Cu-Ka radiation tube)를 사용하였으며, 평균입도는 입도측정기(Mastersizer 2000, Malvern Instrument Ltd.)를 사용하여 측정하였다. 원자흡광기(Varian Spectra, Model 400)와 유도결합 플라즈마 원자방출분광기(ICP-AES, Jobin Yvon JY 38plus)를 이용하여 원소분석을 행하였다. 모든 테스트에서 Milli-Q system(Millipore 사)을 이용하여 제조한 증류수(18 ㏁ ㎝)를 사용하였다.Phase analysis of nickel slag and leach residues was carried out using an X-ray diffractometer (Philips Xpert-MPD coupled with a Cu-Ka radiation tube), and the average particle size was measured by a particle size analyzer (Mastersizer 2000, Malvern Instrument Ltd.). ) Was measured. Elemental analysis was performed using an atomic absorber (Varian Spectra, Model 400) and an inductively coupled plasma atomic emission spectrometer (ICP-AES, Jobin Yvon JY 38plus). In all tests, distilled water (18 ㏁cm) prepared using the Milli-Q system (Millipore) was used.
니켈 슬래그로부터 마그네슘의 황산침출 후 얻어진 다공성 실리카 잔사를 가성소다 용액에 용해하여 물유리를 제조하는 테스트를 행하였다. 가성소다 용액에 의한 실리카 용해반응은 다음과 같이 나타낼 수 있다.The porous silica residue obtained after sulfuric acid leaching of magnesium from nickel slag was dissolved in a caustic soda solution to test water glass. Silica dissolution reaction by caustic soda solution can be expressed as follows.
2NaOH + nSiO2 ---> Na2OㆍnSiO2 + H2O (3)2NaOH + nSiO 2 ---> Na 2 O.nSiO 2 + H 2 O (3)
사면체 실리카와 니켈 슬래그로부터 마그네슘 침출시 미용해 실리카 층 사이에 미세한 관이 형성된다. 따라서, 니켈 슬래그로부터 마그네슘의 황산침출시 생성되는 실리카 잔사는 다공성으로 판단된다. 도 5는 여러 침출조건에서 니켈 슬래그부터 마그네슘의 황산 침출 후 얻어진 실리카 잔사의 비표면적을 나타낸 그래프이다. 도 5에 기재된 바와 같이, 니켈 슬래그에 존재하는 MgO의 함량이 낮아질수록, 즉 마그네슘의 침출율이 증가할수록 실리카 잔사의 비표면적은 지속적으로 증가하였다. 실리카 잔사에 남아 있는 MgO의 함량이 약 4.4 wt%일 때 비표면적은 330 ㎡/g로서 최대치를 나타내었다. MgO의 함량이 4.4 wt% 이하로 감소함에 따라 비표적은 조금씩 감소하였는데, 이것은 마그네슘의 침출에 따라 미세기공이 파괴되었기 때문으로 판단된다. Kosuge 등(Kosuge, K. et. al., 1995, Chemistry of Materials, Vol. 7, pp. 2241-2246)의 연구에 의하면 실리카 잔사의 미세기공의 구조의 안정화를 위하여 필요한 MgO의 함량은 약 5 wt%이며, 이때 비표적은 300 ㎡/g 이상이었다.On leaching magnesium from tetrahedral silica and nickel slag a fine tube is formed between the undissolved silica layers. Therefore, the silica residue produced upon leaching of magnesium sulfate from nickel slag is considered to be porous. 5 is a graph showing the specific surface area of silica residue obtained after sulfuric acid leaching of magnesium from nickel slag under various leaching conditions. As shown in FIG. 5, as the content of MgO present in the nickel slag was lowered, that is, as the leaching rate of magnesium increased, the specific surface area of the silica residue increased continuously. When the content of MgO remaining in the silica residue was about 4.4 wt%, the specific surface area reached a maximum value of 330 m 2 / g. As the content of MgO decreased below 4.4 wt%, the specific target decreased little by little, because the micropores were destroyed by leaching of magnesium. According to Kosuge et al. (Kosuge, K. et. Al., 1995, Chemistry of Materials, Vol. 7, pp. 2241-2246), the MgO content required for stabilization of the microporous structure of silica residues is about 5 wt% with a specific target of at least 300 m 2 / g.
물유리 제조 테스트를 위하여 니켈 슬래그로부터 마그네슘의 초적침출 조건인 황산농도; 4.0 M, 침출온도; 90℃, 침출시간; 60분, 광액농도; 200 g/ℓ에서 마그네슘의 침출을 행하여 침출잔사를 얻었다. 물유리 제조 테스트에 사용한 침출잔사의 화학 조성은 표 2에 나타내었다. 침출잔사의 주성분인 실리카의 함량은 약 75 wt%이었으며, 잔존하는 MgO의 양은 4.23 wt%(Mg; 2.46 wt%)이었다. 도 6은 용액온도를 25~90℃로 변화시키면서 5.0 M NaOH 용액으로 침출잔사의 실리카를 30분 동안 용해한 결과를 나타낸 것이다. 도 6에서 보는 바와 같이 실리카의 용해 온도의 영향을 받지 않았으며, 용해율은 약 88%를 유지하였다. 이것은 가성소다 용액에 의한 다공성 침출잔사의 용해반응이 발열반응이므로, 다공성 침출잔사를 가성소다 용액에 투입함에 따라 용액온도가 상승하기 때문이다. 본 테스트 조건에서 25℃의 가성소다 용액에 침출잔사를 투입함에 따라 반응초기에 용액온도가 40~50℃ 정도로 상승하였다(Park, K.Y., et. al., 1997, Industrial & Engineering Chemistry Research, Vol. 36, pp. 2646~2650). 또한, 비표면적인 큰 침출잔사는 반응성이 매우 크므로, 용해온도의 영향을 상당히 감소시키는 것으로 생각된다.Sulfuric acid concentration, which is a super leaching condition of magnesium from nickel slag for water glass manufacturing test; 4.0 M, leaching temperature; 90 ° C., leaching time; 60 minutes, mineral solution concentration; Leaching of magnesium was carried out at 200 g / L to obtain a leaching residue. The chemical composition of the leaching residue used in the water glass manufacturing test is shown in Table 2. The content of silica, the main component of the leaching residue, was about 75 wt%, and the amount of MgO remaining was 4.23 wt% (Mg; 2.46 wt%). Figure 6 shows the result of dissolving the silica of leaching residue with 5.0 M NaOH solution for 30 minutes while changing the solution temperature to 25 ~ 90 ℃. As shown in FIG. 6, the dissolution temperature of silica was not affected, and the dissolution rate was maintained at about 88%. This is because the dissolution reaction of the porous leaching residue by the caustic soda solution is an exothermic reaction, so that the solution temperature increases as the porous leaching residue is added to the caustic soda solution. As the leaching residue was added to the caustic soda solution at 25 ° C under this test condition, the solution temperature rose to about 40-50 ° C at the beginning of the reaction (Park, KY, et. Al., 1997, Industrial & Engineering Chemistry Research, Vol. 36, pp. 2646-2650). It is also believed that the large surface leach residues are very reactive and therefore considerably reduce the effect of dissolution temperature.
도 7은 25℃에서 5.0 M NaOH 용액을 사용하여 침출잔사로부터 실리카를 용해하였을 때 시간에 따른 실리카의 용해율을 나타낸 그래프이다. 용해시간이 5분일 때 75%의 실리카가 용해되었으며, 10분 후 실리카의 용해율이 약 88%로 거의 일정하였다. 따라서, 가성소다 용액에 의한 침출잔사의 용해반응은 실온에서 10분을 경과한 후 완료됨을 알 수 있다.7 is a graph showing the dissolution rate of silica with time when dissolving the silica from the leaching residue using a 5.0 M NaOH solution at 25 ℃. When the dissolution time was 5 minutes, 75% of the silica was dissolved, and after 10 minutes, the dissolution rate of the silica was almost constant, about 88%. Therefore, it can be seen that the dissolution reaction of the leaching residue by the caustic soda solution is completed after 10 minutes at room temperature.
가성소다 용액의 농도를 5.0 M으로 일정하게 하고 침출잔사의 투입량을 변화시키면서 실리카의 용해 테스트를 행하였다. 용해테스트 조건은 용해온도; 25℃, 용해시간; 30분, 광액농도; 300~700 g/ℓ 이었다. 실리카의 용해율과 물유리에서 SiO2/Na2비의 변화를 Na/Si 비의 함수로 도 8에 기재하였다. 도 8에 기재된 바와 같이, Na/Si 비를 0.539~1.259로 변화시켰을 때 실리카의 용해율은 약 87%로 거의 일정한 경향을 나타내었다. 즉, 침출잔사의 광액농도를 300~700 g/ℓ를 변화시키면서 5.0 M NaOH 용액으로 용해하였을 때 용해율은 약 88%로 일정하였다. 이와 같이, 약 10% 정도의 실리카가 용해되지 않는 것은 표 2에 기재된 바와 같이, 침출잔사에 존재하는 다른 원소들과 결합되어 있기 때문으로 판단된다. 니켈 슬래그로부터 마그네슘의 황산침출 후 침출잔사에 단독으로 존재하는 실리카는 다공성이며 비표면적이 크기 때문에 25~90℃에서도 가성소다 용액에 용해되지만, 황산침출 후에도 실리카가 다른 원소들과 복합광물로 존재하면 본 테스트 조건에서 용해되지 않는 것으로 판단된다.The dissolution test of silica was carried out while keeping the concentration of the caustic soda solution at 5.0 M and changing the dosage of the leaching residue. Dissolution test conditions include melting temperature; 25 ° C., dissolution time; 30 minutes, mineral solution concentration; 300-700 g / l. The dissolution rate of silica and the change of SiO 2 / Na 2 ratio in the water glass are described in FIG. 8 as a function of Na / Si ratio. As shown in FIG. 8, when the Na / Si ratio was changed from 0.539 to 1.259, the dissolution rate of silica showed an almost constant tendency of about 87%. That is, the dissolution rate was constant at about 88% when dissolved in a 5.0 M NaOH solution while varying the concentration of the
도 9는 침출잔사의 투입량을 500 g/ℓ으로 일정하게 하고 용액의 농도를 변화시키면서 실리카를 용해한 테스트 결과를 나타낸 도면이다. 용해온도 및 시간은 각각 25℃, 30분이었다. 가성소다의 농도가 3.0~5.0 M일 때, 실리카의 용해율은 85~88%로서 거의 일정하였다. 따라서, 침출잔사로부터 실리카의 용해를 위한 당량비 이상에서는 가성소다의 농도가 실리카의 용해에 미치는 영향은 거의 없으며 이것은 도 8에서 얻어진 결과와 일치한다. 그리고, 3.0 M NaOH 용액으로 500g/ℓ의 침출잔사로부터 실리카를 용해하였을 때 SiO2/Na2비가 4.0 정도인 물유리를 제조하기 위해서는 실리카 광물과 탄산소다(Na2CO3)를 혼합한 뒤 고온에서 용융하여 Na2OㆍxSiO2를 합성하고 이것을 물에 용해하여 제조한다(Weldes, H.H. and Lange, R.K., 1969, Industrial & Engineering Chemistry, Vol. 61, pp. 29-44 ; Minihan, A. 2006, Silicates, in Ullmann's Encyclopedia of Industry Chemistry, 6th Edition, Vol. 32, Wiley-VCH, Germany, pp. 411-417). 따라서, 침출잔사를 이용하여 상온에서 SiO2/Na2O 비가 3.85인 물유리를 제조하였다.9 is a view showing a test result in which silica was dissolved while changing the concentration of the solution to constant the input amount of the leaching residue to 500 g / ℓ. The melting temperature and time were 25 ° C. and 30 minutes, respectively. When the concentration of caustic soda was 3.0 to 5.0 M, the dissolution rate of silica was almost constant as 85 to 88%. Therefore, above the equivalent ratio for the dissolution of silica from the leaching residue, the effect of the concentration of caustic soda on the dissolution of silica is little, which is consistent with the result obtained in FIG. In order to produce a water glass having a SiO 2 / Na 2 ratio of about 4.0 when dissolving silica from a 500 g / L leach residue with a 3.0 M NaOH solution, silica minerals and sodium carbonate (Na 2 CO 3 ) were mixed at a high temperature. It is prepared by melting Na 2 O.xSiO 2 and dissolving it in water (Weldes, HH and Lange, RK, 1969, Industrial & Engineering Chemistry, Vol. 61, pp. 29-44; Minihan, A. 2006, Silicates, in Ullmann's Encyclopedia of Industry Chemistry, 6th Edition, Vol. 32, Wiley-VCH, Germany, pp. 411-417). Accordingly, water glass having a SiO 2 / Na 2 O ratio of 3.85 was prepared at room temperature using a leaching residue.
이상과 같이 다양한 용해조건에서 제조한 물유리에 함유되어 있는 불순물들을 조사하여 표 3에 나타내었다. 표 3에 기재된 바와 같이, 가성소다의 농도가 높을수록 불순물의 함량이 높았다. 물유리에 존재하는 불순물 원소 중에서 침출잔사에 가장 많이 함유되어 있는 마그네슘의 함량이 가장 높았다. 철(Fe)은 물유리에 63~92 ppm 정도 함유되어 있으나, KS 공업규격보다 낮은 농도로서 별도의 정제공정이 필요하지 않다.Table 3 shows the impurities contained in the water glass prepared under various dissolution conditions as described above. As shown in Table 3, the higher the concentration of caustic soda, the higher the content of impurities. Among the impurity elements present in the water glass, the content of magnesium in the leach residue was the highest. Iron (Fe) is contained in 63 ~ 92 ppm in water glass, but it is lower than KS industrial standard and does not need separate purification process.
도 1은 90℃에서 60분 동안 4.0 M H2SO4 용액에 의한 니켈 슬래그로부터 마그네슘의 침출거동을 나타낸 그래프이고, 1 is a graph showing the leaching behavior of magnesium from nickel slag with 4.0 MH 2 SO 4 solution for 60 minutes at 90 ℃,
도 2는 60분 동안 2.0 M H2SO4 용액에 의한 니켈 슬래그로부터 마그네슘의 침출에 있어서 온도의 효과를 나타낸 그래프이고, 2 is a graph showing the effect of temperature on leaching of magnesium from nickel slag with 2.0 MH 2 SO 4 solution for 60 minutes,
도 3은 90℃에서 60분 동안 H2SO4 용액에 의한 니켈 슬래그로부터 마그네슘의 침출시에 H2SO4 용액 농도의 효과를 나타낸 그래프이고, 3 is a graph showing the effect of H 2 SO 4 solution concentration on leaching of magnesium from nickel slag with H 2 SO 4 solution at 90 ° C. for 60 minutes,
도 4는 90℃에서 60분 동안 4.0 M H2SO4 용액에 의한 니켈 슬래그로부터 마그네슘의 침출시에 펄프 밀도의 효과를 나타낸 그래프이고, 4 is a graph showing the effect of pulp density on leaching of magnesium from nickel slag with 4.0 MH 2 SO 4 solution at 90 ° C. for 60 minutes,
도 5는 다양한 조건에서 H2SO4 용액에 의한 마그네슘의 침출후의 잔사의 MgO 함량과 비표면적 간의 상관관계를 나타낸 그래프이고, 5 is a graph showing the correlation between the MgO content and specific surface area of the residue after leaching of magnesium by H 2 SO 4 solution under various conditions,
도 6은 30분 동안 5.0 M NaOH 용액에 의한 침출 잔사로부터 SiO2 분해시에 온도의 효과를 나타낸 그래프이고, 6 is a graph showing the effect of temperature upon SiO 2 decomposition from a leaching residue with 5.0 M NaOH solution for 30 minutes,
도 7은 25℃에서 5.0 M NaOH 용액에 의한 침출 잔사로부터 SiO2 분해시에 시간의 효과를 나타낸 그래프이고, 7 is a graph showing the effect of time upon SiO 2 decomposition from a leaching residue with a 5.0 M NaOH solution at 25 ° C.,
도 8은 30분 동안 25℃에서 5.0 M NaOH 용액에 의한 침출 잔사로부터 SiO2 분해시에 Na/Si 비의 효과를 나타낸 그래프(이때, 펄프 밀도는 300~700 g/ℓ이다) 이고, FIG. 8 is a graph showing the effect of Na / Si ratio on SiO 2 decomposition from a leach residue with 5.0 M NaOH solution at 25 ° C. for 30 minutes, wherein the pulp density is 300-700 g / l,
도 9는 30분 동안 25℃에서 침출 잔사로부터 SiO2 분해시에 NaOH의 효과를 나타낸 그래프(이때, 펄프 밀도는 500 g/ℓ이다)이다. FIG. 9 is a graph showing the effect of NaOH upon SiO 2 decomposition from a leaching residue at 25 ° C. for 30 minutes, wherein the pulp density is 500 g / l.
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