KR20100089450A - Method of manufacting magnetite by using dust of electronic furnance and iron sulfate - Google Patents
Method of manufacting magnetite by using dust of electronic furnance and iron sulfate Download PDFInfo
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- KR20100089450A KR20100089450A KR1020090008701A KR20090008701A KR20100089450A KR 20100089450 A KR20100089450 A KR 20100089450A KR 1020090008701 A KR1020090008701 A KR 1020090008701A KR 20090008701 A KR20090008701 A KR 20090008701A KR 20100089450 A KR20100089450 A KR 20100089450A
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- magnetite
- alkali metal
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- iron sulfate
- magnetite particles
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910000358 iron sulfate Inorganic materials 0.000 title claims abstract description 22
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000000428 dust Substances 0.000 title claims description 22
- 239000002245 particle Substances 0.000 claims abstract description 42
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 35
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001339 alkali metal compounds Chemical class 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000011575 calcium Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000002440 industrial waste Substances 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000003337 fertilizer Substances 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910000616 Ferromanganese Inorganic materials 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
Description
본 발명은 전기로 분진과 황산철을 이용한 마그네타이트의 제조방법에 관한 것이다.The present invention relates to a method for producing magnetite using an electric dust and iron sulfate.
보다 구체적으로 본 발명은 상기 전기로 분진에 포함된 알칼리금속을 이용하여 마그네타이트를 제조함과 동시에 부수적으로 비료원료 등에 사용되는 알칼리금속화합물을 제조하는 방법에 관한 것이다.More specifically, the present invention relates to a method for producing an alkali metal compound used for fertilizer raw materials and the like, while simultaneously producing magnetite using the alkali metal contained in the dust.
종래에는 전기로 분진에 포함된 금속들을 회수하는 것이 상업적으로 불가능하여 상기 전기로 분진을 산업 폐기물로 폐기처리하여 왔다.Conventionally, it has not been commercially possible to recover the metals contained in the dust of an electric furnace, so that the dust of the electric furnace has been disposed of as industrial waste.
전기로 분진을 그대로 건축자재나 아스팔트 재료로 사용하는 경우에는 유해한 금속물질이 많이 포함되어 환경공해를 유발하기 때문에 사실상 사용이 불가능 하였다.In the case of using electric dust as a building material or asphalt material, it was practically impossible to use because it contains many harmful metals and causes environmental pollution.
상기와 같이 종래에는 전기로 분진에 포함된 망간 함유 화합물 및 기타 금속 을 상업적으로 회수할 수 없어서 경제적으로 불리하고, 전기로 분진을 산업 폐기물로 폐기처리하는 비용도 부담해야 하는 문제점이 있었다.As described above, conventionally, manganese-containing compounds and other metals included in the electric furnace dust cannot be recovered commercially, which is economically disadvantageous, and there is a problem in that the electric furnace dust has to be disposed of as industrial waste.
대한민국 공개특허 제2003-0028006호에서는 농황산 43~45중량%, 페로망간 합금철 전기로더스트 60~70중량% 및 페로망간 6~7중량%로 혼합하여 95℃로 5시간 가열하여 반응시킨 후 여과한 다음, 금속아연분말 3~4%를 넣어 중금속을 제거한 후 농축, 건조하여 황산망간을 제조하는 방법을 게재하고 있으나, 상기 종래기술은 농황산을 95℃로 장시간 가열하기 때문에 환경유해가 심각하고 에너지 낭비가 많아 상업적인 실시가 불가능한 문제가 있었다.In Korean Patent Laid-Open Publication No. 2003-0028006, 43 to 45% by weight of concentrated sulfuric acid, 60 to 70% by weight of ferro-manganese ferroalloy electric furnace, and 6 to 7% by weight of ferro-manganese were mixed, heated to 95 ° C for 5 hours, and then filtered. Next, a method of preparing manganese sulfate by removing heavy metals by adding 3-4% of metal zinc powder and then drying it is disclosed. However, the prior art heats concentrated sulfuric acid to 95 ° C. for a long time and seriously wastes energy. There were many problems that commercial implementation is impossible.
본 발명의 과제는 전기로 분진으로부터 알칼리금속을 회수하여 마그네타이트를 제조하는 방법을 제공하는 것이다.An object of the present invention is to provide a method for producing magnetite by recovering alkali metal from dust in an electric furnace.
또 다른 본 발명의 과제는 전기로 분진으로부터 알칼리금속을 회수하여 마그네타이트를 제조함과 동시에 비료원료 등에 사용되는 알칼리금속화합물들로 부수적으로 회수하는 방법을 제공하는 것이다.Still another object of the present invention is to provide a method for recovering alkali metal from dust in an electric furnace and producing a magnetite, and at the same time, additionally recovering alkali metal compounds used in fertilizer raw materials.
이와 같은 과제를 달성하기 위해서 본 발명에서는 알칼리금속을 함유하는 전기로 분진을 물로 세척후 여과하여 알칼리금속이 용해된 용액(A)을 제조한 다음, 황산철 및 황산철이 용해된 용액(B)중에서 선택된 1종을 상기 알칼리금속이 용해된 용액(A)에 첨가한 후 가열, 교반 및 산화반응시켜 마그네타이트 입자를 생성함으로서 마그네타이트 입자가 생성된 용액(C)을 제조한 다음, 상기 마그네타이트 입자가 생성된 용액(C)을 여과하여 마그네타이트 입자와 여과용액(D)을 제조한 다음, 여과된 마그네타이트 입자를 세척, 건조 및 분쇄하여 마그네타이트를 제조한다.In order to achieve the above object, in the present invention, an electric dust containing an alkali metal is washed with water and filtered to prepare a solution (A) in which the alkali metal is dissolved, and then in a solution (B) in which the iron sulfate and iron sulfate are dissolved. The selected solution is added to the solution (A) in which the alkali metal is dissolved, and then heated, stirred, and oxidized to produce magnetite particles, thereby preparing a solution (C) in which the magnetite particles are produced, and then producing the magnetite particles. The solution (C) is filtered to produce magnetite particles and a filtrate (D), and then the filtered magnetite particles are washed, dried and pulverized to produce magnetite.
또한, 본 발명에서는 상기 여과용액(D)을 건조하여 알칼리금속화합물을 회수한다.In the present invention, the filtration solution (D) is dried to recover the alkali metal compound.
본 발명은 전기로 분진 내에 함유된 알칼리금속을 회수하여 마그네타이트제조 등에 사용하고, 비료원료로 사용될 수 있는 알칼리금속화합물도 부수적으로 회수할 수 있다.The present invention is used to recover the alkali metal contained in the dust in the electric furnace used in the production of magnetite, etc., it is also possible to additionally recover the alkali metal compound that can be used as a fertilizer raw material.
이하, 첨부한, 도면을 통하여 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
본 발명은 (ⅰ) 알칼리금속을 함유하는 전기로 분진을 물로 세척후 여과하여 알칼리금속이 용해된 용액(A)을 제조하는 공정;The present invention (i) a step of preparing a solution (A) in which alkali metal is dissolved by filtration after washing the dust with an electric water containing alkali metal;
(ⅱ) 황산철 및 황산철이 용해된 용액(B)중에서 선택된 1종을 상기 알칼리금속이 용해된 용액(A)에 첨가한 후 가열, 교반 및 산화반응시켜 마그네타이트 입자를 생성함으로서 마그네타이트 입자가 생성된 용액(C)을 제조하는 공정;(Ii) magnetite particles are produced by adding one selected from the solution (B) in which iron sulfate and iron sulfate are dissolved, to the solution (A) in which the alkali metal is dissolved, and then heating, stirring and oxidizing to produce magnetite particles. Preparing a solution (C);
(ⅲ) 상기 마그네타이트 입자가 생성된 용액(C)을 여과하여 마그네타이트 입자와 여과용액(D)을 제조하는 공정; 및 (Iii) filtering the solution (C) in which the magnetite particles are produced to produce the magnetite particles and the filtrate (D); And
(ⅳ) 여과된 마그네타이트 입자를 세척, 건조 및 분쇄하여 마그네타이트를 제조하는 공정;들을 포함하는 것을 특징으로 한다.(Iii) washing, drying and pulverizing the filtered magnetite particles to produce magnetite.
도 1은 본 발명의 공정순서를 나타내는 플로우 차트(Flow Chart)이다.1 is a flowchart illustrating a process sequence of the present invention.
먼저, 본 발명은 알칼리금속을 함유하는 전기로 분진을 물로 세척후 여과하여 알칼리금속이 용해된 용액(A)을 제조한다.First, in the present invention, a solution (A) in which an alkali metal is dissolved is prepared by washing the dust with an electric water containing an alkali metal with water and filtration.
상기 전기로 분진에 포함된 알칼리금속은 칼륨(K), 나트륨(Na), 칼슘(Ca), 리튬(Li) 또는 이들의 혼합물 등이다.Alkali metals contained in the electric dust are potassium (K), sodium (Na), calcium (Ca), lithium (Li), or a mixture thereof.
상기 전기로 분진내 알칼리금속의 함량은 5중량%, 보다 바람직하기로는 10중량% 이상인 것이 좋다.The content of the alkali metal in the electric dust is preferably 5% by weight, more preferably 10% by weight or more.
다음으로는, 황산철 및 황산철이 용해된 용액(B)중에서 선택된 1종을 상기 알칼리금속이 용해된 용액(A)에 첨가한 후 가열, 교반 및 산화반응시켜 마그네타이트 입자를 생성함으로서 마그네타이트 입자가 생성된 용액(C)을 제조한다.Next, magnetite particles are formed by adding one selected from the solution (B) in which iron sulfate and iron sulfate are dissolved, to the solution (A) in which the alkali metal is dissolved, and then heating, stirring and oxidizing to produce magnetite particles. Prepared solution (C).
상기 산화반응은 60~120℃에서 4~12시간 동안, 보다 바람직하기로는 80~100℃에서 6~10시간 동안 실시하는 것이 바람직하다.The oxidation reaction is preferably carried out at 60 to 120 ° C. for 4 to 12 hours, more preferably at 80 to 100 ° C. for 6 to 10 hours.
다음으로, 상기 마그네타이트 입자가 생성된 용액(C)을 여과하여 마그네타이트 입자와 여과용액(D)을 제조한 후, 여과된 마그네타이트 입자를 세척, 건조 및 분쇄하여 마그네타이트를 제조한다.Next, after filtering the solution (C) in which the magnetite particles are produced to produce the magnetite particles and the filtrate (D), the filtered magnetite particles are washed, dried and pulverized to produce magnetite.
이때, 여과된 마그네타이트 입자를 50~500℃에서 5~15시간 동안, 보다 바람 직하기로는 60~150℃에서 6~12시간 동안 실시하는 것이 바람직하다.At this time, the filtered magnetite particles are preferably performed at 50 to 500 ° C. for 5 to 15 hours, more preferably at 60 to 150 ° C. for 6 to 12 hours.
또한, 상기 여과용액(D)을 건조하여 알칼리금속화합물을 회수하고, 마그네타이트 입자를 분쇄장치로 분쇄할때 분쇄장치내에 마그네타이트 입자와 함께 용매 및 분산제를 투입하는 것이 바람직하다.In addition, it is preferable to dry the filtrate (D) to recover the alkali metal compound, and to add a solvent and a dispersant together with the magnetite particles in the grinding device when the magnetite particles are ground by the grinding device.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
그러나, 본 발명은 하기 실시예에 의해서 권리범위가 한정되는 것은 아니다.However, the present invention is not limited by the following examples.
실시예 1Example 1
알칼리금속을 15중량% 포함하는 전기로 분진을 증류수에 투입하여 2시간 교반시켜 세척한 다음, 이를 여과하여 알칼리금속인 나트륨(Na), 칼륨(K), 칼슘(Ca) 등이 용해된 여과용액(A)을 제조하였다.Electric dust containing 15% by weight of alkali metals was added to distilled water, followed by stirring for 2 hours, followed by filtration. The filtrate was dissolved in sodium (Na), potassium (K) and calcium (Ca) alkali metals. (A) was prepared.
다음으로는, 황산철을 증류수에 용해시킨 용액(B)을 알칼리금속이 용해된 상기 용액(A)에 첨가하여 100℃에서 6시간 동안 가열, 교반 및 산화반응을 시켜 마그네타이트 입자를 생성시켜 마그네타이트 입자가 생성된 용액(C)을 제조하였다.Next, a solution (B) in which iron sulfate was dissolved in distilled water was added to the solution (A) in which the alkali metal was dissolved, and heated, stirred, and oxidized at 100 ° C. for 6 hours to produce magnetite particles, thereby producing magnetite particles. Prepared solution (C).
이때, 황산철:알칼리금속의 몰비를 1:2로 조절하였다.At this time, the molar ratio of iron sulfate: alkali metal was adjusted to 1: 2.
다음으로는, 상기 공정에서 얻어진 마그네타이트 입자가 생성된 용액(C)을 여과하여 마그네타이트 입자와 여과용액(D)을 분리하였다.Next, the solution (C) in which the magnetite particles obtained in the above step were produced was filtered to separate the magnetite particles and the filtrate (D).
다음으로는, 여과된 마그네타이트 입자를 세척한 후 60℃에서 12시간 동안 건조하고, 건조된 마그네타이트 입자를 볼밀을 이용하여 분쇄하여 마그네타이트를 제조하였다.Next, the filtered magnetite particles were washed and dried at 60 ° C. for 12 hours, and the dried magnetite particles were pulverized using a ball mill to prepare magnetite.
또한, 알칼리금속이 용해된 여과용액(A)을 건조하여 비료원료로 사용되어질 수 있는 알칼리금속화합물을 회수하였다.In addition, the filtered solution (A) in which the alkali metal is dissolved was dried to recover an alkali metal compound that can be used as a fertilizer.
실시예 2Example 2
알칼리금속을 20중량% 포함하는 전기로 분진을 증류수에 투입하여 2시간 교반시켜 세척한 다음, 이를 여과하여 알칼리금속인 나트륨(Na), 칼륨(K), 칼슘(Ca) 등이 용해된 여과용액(A)을 제조하였다.Electric dust containing 20% by weight of alkali metals was added to distilled water, followed by stirring for 2 hours, followed by filtration. The filtrate was dissolved in alkali metals such as sodium (Na), potassium (K), and calcium (Ca). (A) was prepared.
다음으로는, 황산철을 증류수에 용해시킨 용액(B)을 알칼리금속이 용해된 상기 용액(A)에 첨가하여 80℃에서 10시간 동안 가열, 교반 및 산화반응을 시켜 마그네타이트 입자를 생성시켜 마그네타이트 입자가 생성된 용액(C)을 제조하였다.Next, a solution (B) in which iron sulfate was dissolved in distilled water was added to the solution (A) in which the alkali metal was dissolved, followed by heating, stirring, and oxidation reaction at 80 ° C. for 10 hours to produce magnetite particles. Prepared solution (C).
이때, 황산철:알칼리금속의 몰비를 1:2로 조절하였다.At this time, the molar ratio of iron sulfate: alkali metal was adjusted to 1: 2.
다음으로는, 상기 공정에서 얻어진 마그네타이트 입자가 생성된 용액(C)을 여과하여 마그네타이트 입자와 여과용액(D)을 분리하였다.Next, the solution (C) in which the magnetite particles obtained in the above step were produced was filtered to separate the magnetite particles and the filtrate (D).
다음으로는, 여과된 마그네타이트 입자를 세척한 후 100℃에서 8시간 동안 건조하고, 건조된 마그네타이트 입자를 볼밀을 이용하여 분쇄하여 마그네타이트를 제조하였다.Next, the filtered magnetite particles were washed, dried at 100 ° C. for 8 hours, and the dried magnetite particles were pulverized using a ball mill to prepare magnetite.
또한, 알칼리금속이 용해된 여과용액(A)을 건조하여 비료원료로 사용되어질 수 있는 알칼리금속화합물을 회수하였다.In addition, the filtered solution (A) in which the alkali metal is dissolved was dried to recover an alkali metal compound that can be used as a fertilizer.
도 1은 본 발명에 따라 마그네타이트와 알칼리금속화합물을 제조하는 플로우 차트(Flow chart).1 is a flow chart for producing a magnetite and an alkali metal compound according to the present invention (Flow chart).
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| KR101251860B1 (en) * | 2012-04-24 | 2013-04-10 | 조굉래 | A method for recovering k and mn from dust of electric furnace, and a method for preparing ferrous oxide and potassium sulfate from k from dust of electric furnace and ferrous sulfate scrap |
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