KR20030026692A - Manufacturing method of ferric sulfates - Google Patents
Manufacturing method of ferric sulfates Download PDFInfo
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- KR20030026692A KR20030026692A KR1020010059780A KR20010059780A KR20030026692A KR 20030026692 A KR20030026692 A KR 20030026692A KR 1020010059780 A KR1020010059780 A KR 1020010059780A KR 20010059780 A KR20010059780 A KR 20010059780A KR 20030026692 A KR20030026692 A KR 20030026692A
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- ferric sulfate
- sulfate
- iron oxide
- ferric
- iron
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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
- C01G49/14—Sulfates
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- 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
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
황산제2철 제품생산은 티타늄(공장)에서 대량생산하고 있다.Ferric sulfate products are mass-produced at titanium (factory).
이제품은(TiO2)산화티타늄제조공정에서 분산물로 생산되는 것으로써 Mn(망간이온)및 질산염, 소다염등의 불순물이 다량존재하는 것으로서 또, Pb,Cd등은 중금속이 규격이상으로 많이 존재함으로서 폐수처리및 동물첨가용 미네랄 제품생산에 큰 장애를 초래하는 결점이 있다.This product is produced as a dispersion in the manufacturing process of (TiO 2 ) Titanium Oxide, which contains a large amount of impurities such as Mn (manganese ions), nitrates, and soda salts, and Pb, Cd, etc. There is a drawback that causes major obstacles to waste water treatment and production of mineral products for animal addition.
이러한 불순물존재는 티타늄광석에서 오염되기도 하고, 황산철에서 산화공정을 거처 황산제2철을 생산하는 공정에서 촉매등의 산화제 오염으로 불순물이 존재한다.Such impurities are sometimes contaminated in titanium ores, and impurities are present due to oxidant contamination such as catalysts in the process of producing ferric sulfate through an oxidation process in iron sulfate.
황산2철은 공장폐수, 염료폐수처리제로서 응집제, 농약, 탈황등의 사용처가 있다.Ferric sulfate is used as a factory wastewater and dye wastewater treatment agent such as flocculant, pesticide, desulfurization.
본 고안에서는 황산철의 원료를 철사공정에서 분산물로 발생하는 산화철 FeO및 산화철 Fe2O3사삼산화철, Fe3O4등의 산화철이 대량발생하는 원료를 사용한다.In the present invention, a raw material in which iron oxides such as iron oxide FeO, iron oxide Fe 2 O 3 tetraoxide, and Fe 3 O 4 are produced in large quantities are used as raw materials of iron sulfate.
이러한 철사제조공정에서 발생하는 산화철은 순도가 높고 품질관리가 양호하여 불순물유입이 적어서 고순도의 황산철제조에 적합한 재료이나 묽은 황산에는 잘 녹지 않는다, 즉, 40∼70% 황산수용액에는 산화철이 용해가 안되는 성질이 있어, 특수용기, 즉, GL탱크등의 용기에 넣고 130℃압력, 5kg/cm2조건에서 용해되는 성질이므로 제질적 한계와 대량생산에 큰 장해요인이 되었다.Iron oxide produced in the wire manufacturing process is high in purity and good in quality control, so that impurities are little insoluble, so it is insoluble in dilute sulfuric acid and materials suitable for manufacturing high-purity iron sulfate, that is, iron oxide is insoluble in 40-70% aqueous sulfuric acid solution. Because of its properties, it is placed in special containers, such as GL tanks, and dissolved at 130 ° C pressure and 5kg / cm 2 , making it a great barrier to material quality and mass production.
기존의 제조공정은 황산제2철생산공정은 황산제1철의 수용액에 70∼80℃온도를 유지하면서 질산염, 아질산염 및 질산등을 사용하여 황산제1철 수용액에 대량공기를 주입하여 황산1철을 2철로 산화전환방법을 사용한다. 이러한 산화공정에서 촉매라는 불순물이 유입되는 결점이 있고 산화공정에서 No2및 No등의 유해성 질소산화물의 배출로 인하여 환경처리시설이 증가하는 결점이 있다.Conventional manufacturing process ferric sulfate production process ferrous sulfate by injecting a large amount of air into ferrous sulfate aqueous solution using nitrate, nitrite and nitrate while maintaining the temperature of 70 ~ 80 ℃ in aqueous solution of ferrous sulfate The oxidation conversion to ferric iron is used. In this oxidation process, there is a defect in that impurities such as a catalyst are introduced therein, and an environmental treatment facility increases due to the emission of harmful nitrogen oxides such as No 2 and No in the oxidation process.
본 발명은 상기의 결점을 해소하여 폐기되는 철사제조공정의 폐기물인 산화철을 황산제2철로 재생시켜 유용한 산업자원을 얻는 것이다.The present invention obtains useful industrial resources by regenerating iron oxide, which is a waste of the wire manufacturing process, which is eliminated by eliminating the above drawbacks with ferric sulfate.
본 고안에서는 이러한 산화철의 물은 황산에 용해안되는 물성을 고려하여, 농황산(98%)을 사용하고 재질은 철판을 용기로하여 반응을 유도하거나 킬런리본타입 대상, 벽돌구축한 반응용기를 사용하고 반응온도를 150∼250℃ 유지하면서 반응을 유도하는데 성공하고 건식, 농황산 반층시에 대량공기 접촉을 유도하여 황산1철을 2철로 2철산화물은 2철황산염으로 제조하고 제질및 대량생산에 성공할수 있었다.In the present design, the iron oxide water is concentrated sulfuric acid (98%) in consideration of the physical properties that are not dissolved in sulfuric acid, and the material is a steel plate as a container to induce a reaction or use a reaction vessel made of a kiln ribbon type object, brick construction It succeeded in inducing the reaction while maintaining the temperature of 150-250 ℃ and inducing mass air contact in dry and concentrated sulfuric acid semiferrous layers. It was able to manufacture ferric sulfate as ferric sulfate and ferric oxide as ferric sulfate, and to make quality and mass production. .
그 방정식은 다음과 같다.The equation is as follows.
1. 2FeO + 3H2S04+ O2→ Fe2(SO4)3+ 3H2O1.2FeO + 3H 2 S0 4 + O 2 → Fe 2 (SO 4 ) 3 + 3H 2 O
2. Fe2O3+ 3H2SO4→ Fe2(SO4)3+ 3H2O2.Fe 2 O 3 + 3H 2 SO 4 → Fe 2 (SO 4 ) 3 + 3H 2 O
농황산및 산화철의 반응은 온도및 교반력에 의하여 그 반응이 진행되며 교반시에 많은 공기가 1철산화물을 2철로 산화공정이 진행되므로 별도의 산화공정을 선택할 필요성이 없다.The reaction of concentrated sulfuric acid and iron oxide proceeds according to the temperature and the stirring force, and when a lot of air oxidizes ferrous oxide to ferric oxide, there is no need to select a separate oxidation process.
즉, 농황산(96-98%)및 산화철의 반응조건은 온도 150∼250℃및 교반에 의한 공기 산화가 동시 행해지는 특성을 활용하여 고순도의 황산 제2철 생산완료하게 되었다.In other words, the reaction conditions of concentrated sulfuric acid (96-98%) and iron oxide were completed production of high-purity ferric sulfate by utilizing the characteristics that the air oxidation is carried out simultaneously with the temperature of 150 to 250 ℃ and stirring.
농황산및 산하철의 반응이 완료되면 분말형태도 존재한다.When the reaction of concentrated sulfuric acid and ferric acid is completed, there is also a powder form.
이러한 분말의 고철황산제2철에는 미반응한 산화철이 많이 있으므로 이제품을 FRP 재질의 용기에 넣고 수용액 70∼80℃ 가온된 조건에서 용해한다.Since ferric sulfate of the powder contains a lot of unreacted iron oxide, the product is placed in a container made of FRP material and dissolved in an aqueous solution of 70 to 80 ° C.
용해가 진행되면 적갈생 40∼45% 수용액으로 유도하여 여과한다.As the dissolution proceeds, the solution is led to a reddish red 40-45% aqueous solution and filtered.
여액은 제품으로 하고 미반응한 산화철 케일은 회수하여 제반응기에 넣고 반응을 한다.The filtrate is used as a product, and unreacted iron oxide kale is collected and put in a reactor to react.
즉, 순도가높은 산화철의 원료에 농황산을 직접 가온된 조건에서 반응을 유도하고 교반하여 대량공기를 접촉시켜 제1철황산염을 제2철황산염으로 유도하는 것이다.That is, the ferrous sulfate is induced to ferric sulfate by contacting a large amount of air by inducing and stirring a concentrated sulfuric acid directly to a raw material of high purity iron oxide.
<실시예><Example>
철사제조공정에서 부산물로 발생하는 산화철(Fe3O4) 2kg을 철용기15ℓ용량에 넣고 농황산4kg 서서히 추가하면서 온도 150∼250℃가온하면서 2시간 동안 반응완료하고 시료를 물 3.5ℓ용해하여 여액을 여과분리하고 황산제2철용액 45%, 액체3ℓ얻고 미반응한 산화철 200g회수했다.2 kg of iron oxide (Fe 3 O 4 ) produced as a by-product from the wire manufacturing process was added to a 15 liter capacity of iron container, and 4 kg of concentrated sulfuric acid was added slowly, and the reaction was completed for 2 hours while the temperature was heated to 150-250 ° C. The resulting mixture was separated by filtration, 45% of ferric sulfate solution and 3 liters of liquid were recovered, and 200 g of unreacted iron oxide was recovered.
본 제품의 품위분석표Grade analysis table of this product
1. 황산제2철 순도 99.2%Ferric Sulfate Purity 99.2%
2. 황산1철 0.1%2. Ferrous sulfate 0.1%
3. 황산망간 0.03%3. Manganese sulfate 0.03%
4. 소다염트레스4. Soda Salt Stress
5. 질산염트레스5. Nitrate Stress
6. Pb2PPM6. Pb2PPM
7. cd트레스7. cd stress
이렇게하므로서 철사생산공정에 나오는 사삼산화철을 폐기하지 않고 산업자원으로 재생할수 있는 이점이 있다.In this way, there is an advantage that can be recycled to industrial resources without discarding the iron trioxide in the wire production process.
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