• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Process for the recovery of H2SO4 from dilute sulfuric acid solutions containing combined acid sulfates by heating these solutions in the presence of excess ammonium sulfate to a temperature from between about 100 DEG and 160 DEG C. until a concentration of free H2SO4 between 50 and 59% by weight is obtained to precipitate the combined acid sulfates.
    公开号:SU786878A3
    申请号:SU762414008
    申请日:1976-10-20
    公开日:1980-12-07
    发明作者:Соен Жозеф；Аджемян Ален
    申请人:Алюминиюм Пешинэ (Фирма)；
    IPC主号:
    专利说明:

    (54) METHOD FOR CLEANING SULFUR ACID SOLUTIONS
    This invention relates to methods for purifying dilute sulphate solutions containing at least one of the metals, iron, titanium, aluminum. There is a method for regenerating sulfuric acid solutions containing sulphate of iron, aluminum and other elements by multistage evaporation in the presence of a seed from the crystals isolated in the previous stages. At the same time, in the first stage, the evaporation of sulfuric acid is carried out to 47%, and in the second to 78%. Determination of impurities is carried out by cooling the evaporated solution to 25-ZOOc 1. Also known is a method of purification of sulfuric acid solutions, in particular hydrolytic acid from gel impurities, including evaporation of the initial solution in the presence of an excess of ammonium sulfate at a temperature of 20 ° C, crystallization of impurities during cooling of the evaporated solution to 40c. Iron ammonium alum formed in this process is separated from. solution and used as a govol product, and the solution is further evaporated to 220 ° C, obtaining a concentrated solution of sulfuric acid 2j. A disadvantage of the known methods is that they do not provide for the purification of solutions from titanium, and, in addition, high energy costs due to the need to cool the solution to 20-40 ° C, and then reheat it to 220 ° C. The aim of the invention is the simultaneous purification of sulphate solutions from titanium, as well as reducing energy costs. The goal is achieved by the described method, which consists in that the initial sulphate solution is evaporated to a free sulfuric acid content of 50-59% in the presence of an excess of ammonium sulfate at a temperature of 100-120 ° C with the introduction of seed from separated impurity crystals, after which the solution is maintained at this temperature for 2-3 hours with stirring and then separated crystals of impurities are separated. Distinctive features of the predicted method are that the evaporation of sulfate solutions lead
    when the content of free sulfuric acid is 50-59% in the presence of a seed from the crystals of separated impurities, as well as crystallization of the latter at an evaporation temperature for 2-3 hours.
    Under these conditions, most of the iron and titanium fall out as a conical sediment in which crystals of iron-ammonium sulfate and crystals of ammonium and titanyl sulfates double salt can be distinguished together with a third solid phase, which is probably triple iron sulfate, titanyl and ammonium
    In addition, it has also been established that other impurities are released with this precipitate, for example, magnesium in the form of sulfate and phosphorus.
    The presence of seed remaining from the previous operation, the amount of which is 0.5-3% by weight of the solution, is a condition for the rapid precipitation of the complex sludge.
    The choice of sulfuric acid concentration of 50–59% is due to the fact that, at a concentration of less than 50% and more than 59%, the solubility of the sulphates released increases, which can lead to incomplete release of impurities into the sediment.
    An increase in the residence time of the solution over 3 hours at the evaporation temperature does not lead to a considerable one. increase the amount of sediment.
    When the concentration of free sulfuric acid in the initial solution is less than 44-47%, the latter is pre-evaporated at 80 ° C until the specified concentration of H SO is reached. According to the invention, liquid waste resulting from various stages can be treated with residual sulfur solutions containing ferrous sulfate. ui) and / or titanyl sulphate. These liquid wastes may have different formulations, and the solution being treated may be the result of mixing at least two of them.
    Example. The mixture of liquid waste in the amount of 1000 g of the following composition is evaporated: 0.94% A1% 0l in the form of aluminum sulfate. mini
    0.30% FejO-j in the form of ferrous sulfate (III)
    0.37% TiOj in the form of titanyl sulfate
    2.47% NH-j, in the form of ammonium sulfate, 41.4% SOojoew, of which 32.6% as free H2S04v. After adding 11.6 g of seed as a result of the previous operation, the solution is evaporated at, resulting in a loss of 267 g water, after which the concentration of free HjSC rises to 54.3%.
    Next, the evaporated solution is kept under stirring for 3 hours, after which the precipitated precipitate is separated.
    For 1000 T of the initial solution, the filtration method separated 656 g of the solution, which now contained only 0.39% TiOj; 0.1U FcgO, 1.10. The isolated precipitate has the composition: 44.9% titanium, 74.8% iron and 23% Al, jOj.
    Example2. As the initial solution, 2 fluxes are taken, obtained as a result of treating the silico-aluminous ores with sulfuric acid with a concentration of free H and - 50.6.
    The first effluent contains: 1.1U, 0.41 Fe / pOj, 0.5 TiOg,
    3, NHj, (9.7 - yoyl (s mixture as sulphate and for all examples).
    The second effluent contains,%: 0.75 AljOj-, 0.35 - RegOz, 0.34 1.82 - 32.8 - 5050.614,.
    A seed is added to the first effluent at the rate of 21 g per 979 g of the solution and this is kept for 3 hours at 80 s. To the resulting suspension, 869 g of the second effluent per 1000 g of suspension is added and the temperature of the mixture is raised to 110 C and maintained for 3 hours with stirring, after which the suspension is filtered.
    The extraction efficiency for T i 0 was 73%, for FegO, 9.1% and only 18.7% for AljOj.
    Example 3. Two effluents are taken, the first of which is content,%: 1.4AljOj, O, - GeOs, 0.51-Ti0.2-, 0, 57MdO, 0.23 - P Of. 3.0 - NH,
    3 37.8 - Н2504с-vB.
    The second effluent content,%;
    0.7 A12P5,
    0.3 Fe., 0,
    Oh, 23 Ti02,
    1.6 - NH, 0.31 - MgO, 0.12 P2 0, i40.2 - COT
    权利要求:
    Claims (2)
    [1]
    In the first effluent, the seed from the previous operation was injected at the rate of 22 g per 10,000 g and kept at 30 ° C for 3 hours. Next, 1131 g of the second effluent is added to the suspension and the temperature is brought to 110 ° C and 551 g of water is evaporated under vacuum. Then the concentrated suspension is kept under stirring for 3 hours at 110 ° C. So ya. 978 g of the first effluent and 113 g of the second effluent were separated 1331 g of the solution, which contains,%: 1.29 - 0.14 -,; 0.16 1102, 0.52 - MDO; 0.22 - P / iOj, 3-j28 NH3 ,; 53.7 - H-2S04CB06 The extraction efficiency was,%: 74, .7 -Ti02-9-6.5 25.9 MgO, 18.7 - 20.6 - A120z. DETAILED DESCRIPTION A method for purifying sulfuric acid solutions from iron impurities, including evaporation of the initial solution at a temperature of the order in the presence of an excess of ammonium sulfate, crystallization and separation of admixtures, is distinguished by the fact that, in order to simultaneously remove titanium and reduce energy costs, the evaporation of the initial solution of 86 ra is carried out to a free sulfuric acid content of 50-59% with the introduction of a seed from the crystals of released impurities, and the crystallization of the latter is carried out at an evaporation temperature for 2-3 an hour Sources of information taken into account during the examination 1. Khazin L, G. Titanium dioxide :. L., Himi, 1970, p. 78
    [2]
    2. USSR author's certificate number 199133, cl. From 01 G 23/06, 1967.
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    同族专利:
    公开号 | 公开日
    RO72145A|1981-06-30|
    NL186505C|1990-12-17|
    NO763551L|1977-04-21|
    BE847415A|1977-04-19|
    BR7606981A|1977-09-06|
    ATA777076A|1979-08-15|
    DE2647084C2|1985-04-11|
    AR208631A1|1977-02-15|
    ES452484A1|1977-11-16|
    JPS5250993A|1977-04-23|
    DK470776A|1977-04-21|
    SE416638B|1981-01-26|
    IL50700A|1979-11-30|
    NZ182354A|1979-01-11|
    IL50700D0|1976-12-31|
    FR2328658A1|1977-05-20|
    FR2328658B1|1979-05-04|
    SE7611607L|1977-04-21|
    DD127453A5|1977-09-21|
    LU76024A1|1977-05-31|
    US4155984A|1979-05-22|
    NL7611385A|1977-04-22|
    IN145507B|1978-10-28|
    NO150034C|1984-08-15|
    ZA766216B|1977-09-28|
    MX143150A|1981-03-25|
    DE2647084A1|1977-04-21|
    BG39461A3|1986-06-16|
    EG13008A|1980-07-31|
    NO150034B|1984-04-30|
    HU174053B|1979-10-28|
    CA1096138A|1981-02-24|
    GB1563604A|1980-03-26|
    JPS5635602B2|1981-08-18|
    CH613913A5|1979-10-31|
    OA05455A|1981-03-31|
    AT355594B|1980-03-10|
    IT1070943B|1985-04-02|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2500614C1|2012-05-10|2013-12-10|Открытое акционерное общество "Казанский завод синтетического каучука" |Method of sulfuric acid wastes utilisation|FR870125A|1940-05-04|1942-03-03|Konink Ind Mij Voorheen Noury|Purification process for sulfuric solutions|
    NL258598A|1959-12-03|
    US3057685A|1960-05-23|1962-10-09|Edna Y Kamlet|Cyclic process for the beneficiation of titania ores and slags|
    US3984312A|1973-04-23|1976-10-05|Industrial Resources, Inc.|Process for insolubilizing potentially water pollutable wastes from sodium or ammonium type sulfur dioxide air pollution control systems|IT1086096B|1977-09-21|1985-05-28|Montedison Spa|PROCEDURE FOR THE CONCENTRATION OF AQUEOUS SOLUTIONS OF SULFURIC ACID|
    JPH0342403Y2|1983-07-19|1991-09-05|
    JPS6191610U|1984-11-22|1986-06-13|
    DE3726047A1|1987-08-06|1989-02-16|Bayer Ag|METHOD FOR SEPARATING METAL SULFATES FROM SULFURIC ACID|
    JP2968877B2|1991-11-08|1999-11-02|日鉄鉱業株式会社|Method for recovering sulfuric acid from waste sulfuric acid containing metal sulfate|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7532026A|FR2328658B1|1975-10-20|1975-10-20|
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