KR20140057898A - Product method of magnesium sulfate and calcium chloride - Google Patents
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- KR20140057898A KR20140057898A KR1020120124229A KR20120124229A KR20140057898A KR 20140057898 A KR20140057898 A KR 20140057898A KR 1020120124229 A KR1020120124229 A KR 1020120124229A KR 20120124229 A KR20120124229 A KR 20120124229A KR 20140057898 A KR20140057898 A KR 20140057898A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
Description
본발명은 황산마그네슘 및 염화칼슘 제조방법에 관한 것으로, 보다 상세하게는 마그네슘 및 칼슘을 포함하는 돌로마이트를 이용하여 황산마그네슘과 염화칼슘을 제조하는 황산마그네슘 및 염화칼슘 제조방법에 관한 것이다.The present invention relates to a method for producing magnesium sulfate and calcium chloride, and more particularly, to a method for producing magnesium sulfate and calcium chloride using magnesium and calcium-containing dolomite to produce magnesium sulfate and calcium chloride.
일반적으로 황산마그네슘 수용액은 유화공장등에서 ABS수지제조시 염석제 등으로 사용하고 있다. 그리고 상기 황산마그네슘을 제조하는 방법으로서 종래기술로서 특허등록번호 10-0509658호의 황산마그네슘 제조방법이 있으며, 그 기술적 요지는, 괴상의 은백색인 100% 순수마그네슘 광석이나 입자를 분쇄하여 분말화한 다음, 상기 순수마그네슘 분말에, 관용되고 있는 금속광물질과의 반응이 가능한 묽은 황산수용액이 되도록 황산과 물의 양을 조절하면서 번갈아 첨가하되, 황산과 물이 혼합시에 발생되는 자체 반응열에 의하여 황산과 마그네슘이 작용하여 별도로 열을 가하지 않고도 무색결정의 황산마그네슘이 발생되면서 은백색의 순수마그네슘은 없어질때까지 황산과 물의 첨가를 계속한 후, 공지의 방법으로 여과하여 미반응의 황산수용액을 제거한 다음, 잔류 고형물인 무색결정의 황산마그네슘만을 대기중에 방치하여 자연 건조시켜 완제품인 황산마그네슘 결정을 얻음을 특징으로 하는 황산마그네슘의 제조방법이다.Generally, the magnesium sulfate aqueous solution is used as a salting agent in the production of ABS resin in an oil painting factory or the like. As a conventional method for producing magnesium sulfate, there is a magnesium sulfate manufacturing method of Patent Registration No. 10-0509658 as a prior art. The technical point of this method is to pulverize 100% pure magnesium ore or particles which are massive silver white, The pure magnesium powder is added to the magnesium powder in an alternating manner to adjust the amount of sulfuric acid and water to be a dilute sulfuric acid aqueous solution capable of reacting with the commonly used metal mineral substances. In addition, sulfuric acid and magnesium act And the addition of sulfuric acid and water was continued until the silver-white pure magnesium disappears while the magnesium sulfate of the colorless crystals was generated without applying any heat. Then, the unreacted sulfuric acid aqueous solution was removed by a known method, Only the crystalline magnesium sulfate was allowed to stand in the air to dry naturally. A method for manufacturing a magnesium characterized by obtaining the magnesium sulfate crystals.
또한, 다른 종래기술로서 등록번호 10-0270086호에는 황산마그네슘 수용액의 제조방법이 기재되어 있고, 그 기술적 요지는, 마그네사이트, 백운석, 마그네시아계 폐연와로 부터 선택된 1종 또는 2종이상의 원료물질를 250메쉬이하의 분말로 분쇄하는 단계; 상기 분말을 농도가 10-35%인황산과 혼합하여 반응시키는 단계; 상기 반응용액에 NaOH 또는 Mg(OH)2용액을 상기 반응용액대비 10vol%이하 첨가하여 pH를 7-8로 조정하는 단계; 및 상기 반응용액에 KMnO4수용액을 철성분의 당량비에 맞춰 투입하는 단계를 프함하여 구성되는 것을 특징으로하는 황산마그네슘 수용액의 제조방법이다.As another prior art, Registration No. 10-0270086 discloses a method for producing an aqueous solution of magnesium sulfate. The technical point is that one or two or more raw materials selected from magnesite, dolomite and magnesia- By weight of powder; Mixing the powder with sulfuric acid having a concentration of 10-35% and reacting; Adjusting the pH to 7-8 by adding NaOH or Mg (OH) 2 solution to the reaction solution in an amount of 10 vol% or less relative to the reaction solution; And adding the KMnO 4 aqueous solution to the reaction solution in an amount corresponding to an equivalence ratio of the iron component to the aqueous solution of magnesium sulfate.
그러나 상기와 같은 종래기술과 같이 황산마그네슘을 생산하게 되는 경우, 마그네슘의 주요 생산 원료인 산화마그네슘 및 수산화마그네슘의 부존자원이 점차 감소하면서 가격의 상승과 원료의 고갈로 황산마그네슘 생산에 어려움이 발생하고 있는 실정이다. However, when magnesium sulfate is produced as in the prior art as described above, magnesium oxide and magnesium hydroxide, which are major raw materials for producing magnesium, are gradually reduced in resources, resulting in increase in price and depletion of raw materials, In fact.
따라서 본발명은 상기와 같은 문제점을 해결하고자 안출된 것으로서, 저품질의 마그네슘 및 칼슘 원료인 돌로마이트를 이용하여 불순물을 정제하여 고품질의 황산마그네슘과 부산물인 염화칼슘을 생산함으로써 작업이 간단하며 효율적이고 경제성이 높은 황산마그네슘 및 염화칼슘 제조방법을 제공하고자 하는 것이다.SUMMARY OF THE INVENTION Accordingly, the present invention has been made to solve the above-mentioned problems, and it is an object of the present invention to solve the above problems and to provide a high- Magnesium sulfate, and calcium chloride.
본발명은 황산마그네슘 및 칼슘 제조방법에 관한 것으로, 돌로마이트를 물에 습윤시켜 슬러리를 제조하는 슬러리 제조단계; 상기 슬러리에 황산을 투입하여 마그네슘을 용해시키는 마그네슘 용해단계; 상기 마그네슘이 용해된 황산용액에 산화제를 투입하여 용해성 철분 및 불순물을 제거하는 불순물 제거 단계; 상기 철분 및 불순물이 제거된 용액에 탄산나트륨을 첨가하여 칼슘이온을 탄산칼슘으로 변화하는 탄산칼슘 변화단계; 용액에서 탄산칼슘 슬러지를 제거하는 필터링 단계;를 거쳐서 황산마그네슘을 제조하며, 또한 상기 필터링 단계;를 거쳐서 필터링된 탄산칼슘 슬러지에 염산을 첨가하여 상기 탄산칼슘을 용해하고, 산화제를 투입하여 용해성 철분 및 불순물을 제거하여, 염화칼슘을 제조하는 것을 특징으로 한다.The present invention relates to a method for producing magnesium sulfate and calcium, comprising: a slurry producing step of preparing a slurry by wetting a dolomite with water; A magnesium dissolution step of dissolving magnesium by adding sulfuric acid to the slurry; An impurity removing step of adding an oxidizing agent to the sulfuric acid solution in which the magnesium is dissolved to remove soluble iron and impurities; A calcium carbonate changing step of adding sodium carbonate to the solution from which the iron powder and impurities have been removed to convert calcium ions into calcium carbonate; Magnesium sulfate is produced through a filtering step of removing calcium carbonate sludge from the solution, and hydrochloric acid is added to the calcium carbonate sludge filtered through the filtering step to dissolve the calcium carbonate, And impurities are removed to produce calcium chloride.
본발명은 저품질의 마그네슘 및 칼슘 원료인 돌로마이트를 이용하여 불순물을 정제하여 고품질의 황산마그네슘과 부산물인 염화칼슘을 생산함으로써 작업이 간단하며 효율적이고 경제성이 높은 현저한 효과가 있다.The present invention has a remarkable effect of simple, efficient, and economical operation by purifying impurities using dolomite as a raw material of low-quality magnesium and calcium and producing high-quality magnesium sulfate and calcium chloride as a by-product.
도 1은 본발명의 주요 공정도1 is a schematic view of a main process of the present invention
본발명은 황산마그네슘 및 염화칼슘 제조방법에 관한 것으로, 돌로마이트를 물에 습윤시켜 슬러리를 제조하는 슬러리 제조단계; 상기 슬러리에 황산을 투입하여 마그네슘을 용해시키는 마그네슘 용해단계; 상기 마그네슘이 용해된 황산용액에 산화제를 투입하여 용해성 철분 및 불순물을 제거하는 불순물 제거 단계; 상기 철분 및 불순물이 제거된 용액에 탄산나트륨을 첨가하여 칼슘이온을 탄산칼슘으로 변화하는 탄산칼슘 변화단계; 용액에서 탄산칼슘 슬러지를 제거하는 필터링 단계;를 거쳐서 황산마그네슘을 제조하며, 또한 상기 필터링 단계;를 거쳐서 필터링된 탄산칼슘 슬러지에 염산을 첨가하여 상기 탄산칼슘을 용해하고, 산화제를 투입하여 용해성 철분 및 불순물을 제거하여, 염화칼슘을 제조하는 것을 특징으로 한다.The present invention relates to a method for producing magnesium sulfate and calcium chloride, comprising: a slurry producing step of preparing a slurry by wetting a dolomite with water; A magnesium dissolution step of dissolving magnesium by adding sulfuric acid to the slurry; An impurity removing step of adding an oxidizing agent to the sulfuric acid solution in which the magnesium is dissolved to remove soluble iron and impurities; A calcium carbonate changing step of adding sodium carbonate to the solution from which the iron powder and impurities have been removed to convert calcium ions into calcium carbonate; Magnesium sulfate is produced through a filtering step of removing calcium carbonate sludge from the solution, and hydrochloric acid is added to the calcium carbonate sludge filtered through the filtering step to dissolve the calcium carbonate, And impurities are removed to produce calcium chloride.
또한, 상기 돌로마이트는 마그네슘과 칼슘을 포함하는 것으로, 마그네슘과 칼슘의 비율이 마그네슘 40 ~60중량부에 대하여, 칼슘 40 ~60중량부인 것을 특징으로 한다. The dolomite includes magnesium and calcium. The dolomite is characterized in that the ratio of magnesium to calcium is 40 to 60 parts by weight of calcium relative to 40 to 60 parts by weight of magnesium.
또한, 상기 불순물 제거단계에서 사용되는 산화제는 과망간칼륨 또는 과산화수소인 것을 특징으로 한다. The oxidizing agent used in the impurity removing step may be potassium permanganate or hydrogen peroxide.
본발명을 첨부도면에 의해 구체적으로 설명하면 다음과 같다. 도 1은 본발명의 주요 공정도이다. 먼저 마그네슘과 칼슘의 비율이 마그네슘 40 ~ 60중량부에 대하여, 칼슘 40 ~ 60중량부 정도의 혼합비를 가지는 저품위 원료인 돌로마이트를 물에 습윤시켜 슬러리를 제조하고, 1차로 황산을 투입하여 마그네슘을 용해시킨다. 여기에 돌로마이트 원료 내에 불순물로 첨가되어 있는 용해성 철분 및 기타의 불순물을 제거하기 위해 산화제(과망간칼륨 및 과산화수소 등)를 투입하여 제거하고 탄산나트륨을 첨가하여 용존하고 있는 칼슘이온을 탄산칼슘으로 변화하여 필터를 하여 순도가 높은 황산마그네슘 용액을 제조한다. 반응식은 하기와 같다.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail with reference to the accompanying drawings. 1 is a main process diagram of the present invention. First, a dolomite, which is a low-quality raw material having a mixing ratio of magnesium to calcium of 40 to 60 parts by weight, is mixed with 40 to 60 parts by weight of magnesium to prepare a slurry to prepare a slurry. Then, sulfuric acid is firstly added to dissolve the magnesium . In order to remove soluble iron and other impurities added as impurities in the dolomite raw material, an oxidizing agent (such as potassium permanganate and hydrogen peroxide) is added and removed, and sodium carbonate is added to change the dissolved calcium ions to calcium carbonate, To prepare a high purity magnesium sulfate solution. The reaction formula is as follows.
<반응식 1 >용해성 철분 및 기타의 불순물을 제거과정≪ Reaction Scheme 1 > Process of removing soluble iron and other impurities
3Fe2 + + MnO4 - + 7H2O → 3Fe(OH)3(S) + MnO2(S) + 5H+
3Fe 2 + + MnO 4 - + 7H 2 O? 3Fe (OH) 3 (S) + MnO 2 (S) + 5H +
<반응식 2 > 탄산칼슘 변화과정(칼슘이온제거과정)<Reaction formula 2> Calcium carbonate change process (calcium ion removal process)
Ca2 + + Na2Co3 → CaCo3 + Na2 +
Ca 2 + + Na 2 Co 3 → CaCo 3 + Na 2 +
그리고 탄산칼슘은 각종 건조제의 배합용, 제설용, 의료용, 전자재료용, 콘크리트와 혼합하여 빙결방지, 탈색탄(脫色炭)의 제조, 용제류의 탈수용, 제설용, 식품첨가제 등으로 사용되는 염화칼슘을 제조하는 원료로 이용된다. And calcium carbonate is used for mixing of various desiccants, for snow removal, for medical use, for electronic materials, for preventing icing by mixing with concrete, for producing decolorized charcoal, for dehydrating solvents, for snow removal, for food additives It is used as a raw material for producing calcium chloride.
염화칼슘을 제조하는 공정은 상기 황산마그네슘 제조공정에서 탄산칼슘 필터링 단계;를 거쳐서 필터링된 탄산칼슘 슬러지에 염산을 첨가하여 칼슘을 용해하고, 과망간칼륨 및 과산화수소 등의 산화제를 투입하여 재차 용해성 철분 및 불순물을 제거하여, 염화칼슘 용액을 제조하는 것이다. In the process for producing calcium chloride, calcium chloride is added to the calcium carbonate sludge filtered through the calcium carbonate filtering step in the magnesium sulfate manufacturing step, calcium is dissolved, and an oxidizing agent such as potassium and hydrogen peroxide is introduced into the calcium carbonate sludge to dissolve the soluble iron and impurities To prepare a calcium chloride solution.
따라서 본발명은 저품질의 마그네슘 및 칼슘 원료인 돌로마이트를 이용하여 불순물을 정제하여 고품질의 황산마그네슘과 부산물인 염화칼슘을 생산함으로써 작업이 간단하며 효율적이고 경제성이 높다. Accordingly, the present invention produces refined impurities using dolomite, which is a low-quality magnesium and calcium raw material, and produces high-quality magnesium sulfate and calcium chloride, which is a by-product, so that the operation is simple, efficient, and economical.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112607782A (en) * | 2020-12-18 | 2021-04-06 | 中信大锰矿业有限责任公司 | Method for preparing battery-grade high-purity manganese sulfate by using metal manganese anode slime |
| CN112795773A (en) * | 2020-12-18 | 2021-05-14 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for removing Ca and Mg in electrolytic manganese metal anode mud |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112607782A (en) * | 2020-12-18 | 2021-04-06 | 中信大锰矿业有限责任公司 | Method for preparing battery-grade high-purity manganese sulfate by using metal manganese anode slime |
| CN112795773A (en) * | 2020-12-18 | 2021-05-14 | 中信大锰矿业有限责任公司大新锰矿分公司 | Method for removing Ca and Mg in electrolytic manganese metal anode mud |
| CN112795773B (en) * | 2020-12-18 | 2022-10-14 | 南方锰业集团有限责任公司大新锰矿分公司 | Method for removing Ca and Mg in electrolytic manganese metal anode mud |
| CN112607782B (en) * | 2020-12-18 | 2022-10-14 | 南方锰业集团有限责任公司 | Method for preparing battery-grade high-purity manganese sulfate by using metal manganese anode slime |
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