• 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:
    A process is disclosed for the elimination of accumulated iron in the organic phase of a fluid-fluid extraction that contains di-2-ethyl-hexyl phosphoric acid. This process involves treating said organic phase with an aqueous acidic solution of chloride ions, subsequently extracting the iron with an anionic ion exchanger leaving the di-2-ethyl-hexyl phosphoric acid iron-free for subsequent re-use, and regenerating the anionic exchanger by treatment with water to provide a relatively concentrated aqueous ferric chloride solution. Di-2-ethyl-hexyl phosphoric acid is used commercially as a cationic exchanger in the extraction of hexavalent uranium from sulfate solutions, in the separation of uranium and vanadium, in the separation and purification of rare earths, in the separation of cobalt and nickel, and in many other such applications.
    公开号:SU712025A3
    申请号:SU762410954
    申请日:1976-10-05
    公开日:1980-01-25
    发明作者:Диас Ногейра Эдуардо；Луис Редондо Абад Анхель；Мануэль Рехифе Вега Хосе
    申请人:Diaz Nogueira Eduardo；Redondo Abad Angel Luis；Regife Vega Jose Manuel；
    IPC主号:
    专利说明:

    You are in a concentration of from 5 to 50% by volume of 1 or 1G metal chloride in a concentration of from 0.1 m / l to saturation, or with an aqueous solution of hydrochloric acid in a concentration of from 3 to 30% by volume and metal chloride of group 1 or II at a concentration of from 0.1 mol / l to saturation or with an aqueous solution of hydrochloric acid at a concentration of from 3 to 25% by volume of sulfuric acid at a concentration of from 5 to 40% by volume and metal chloride of group 1 or II in a concentration of from 0.1 m / l to saturation and the process is carried out at a ratio of extractant and aqueous solution of 5-30: 1 and a temperature of 10-50s, the resulting extract is subjected to processing liquids followed by regeneration of the anion exchanger (anion exchanger with water.
    As a liquid anion exchanger, it is desirable to use an organic solution containing primary, or tert, amine, aliphatic with 8-14 carbon atoms and a mixture of hydrocarbons.
    A distinctive feature of the method is that an aqueous solution of an aqueous solution of sulfuric acid in a concentration of from 5 to 50% by volume and metal chloride of group 1 or group II in a concentration of from 0.1 mol / l; up to saturation; or an aqueous solution hydrochloric acid in concentration from 3 to 30 vol.% and metal chloride in concentration from 0.1 mol / l to saturation or aqueous solution of hydrochloric acid in concentration from 3 to 25 vol.%,. sulfuric acid in concentration from 5 to 40 vol.% And metal chloride 1 or group II in a concentration of from 0.1 m / l to saturation, and the process is carried out at a ratio of In extracting agents and an aqueous solution of 5–30: 1 and a temperature of 10–50 ° C, the extract obtained is subjected to treatment with a liquid anion exchanger, followed by regeneration of the anion exchanger with water.
    The described method allows to increase the degree of purification up to 90%.
    The method consists of three stages. In the first stage, the organic phase containing di-2-ethylhexylphosphoric acid, poisoned by iron, along the line; 1 is fed to a mixer-precipitator 2, where it is treated with an aqueous solution of a mineral acid containing chloride ions, and the purified organic phase is removed via line 3. This process achieves iron removal from the organic phase and the possibility of its new use.
    Next, an aqueous solution containing iron, through line 4 is fed to the mixer-precipitator 5, where it is treated with anion exchange. This second stage achieves the regeneration of the solution of acid, d.dg, of the chloride ions, which means that
    use this solution again in the first stage. Purified aqueous solution in line b is returned to the precipitator mixer 2. Next, the iron-containing anion exchanger, through line 7, is fed to the precipitator mixer 8, where it is treated with water coming in line 9. This third stage achieves iron removal from the anion exchanger. line 10 delivers in the mixer-precipitator 5, where it is used again. Along line 11, an aqueous solution containing iron is withdrawn.
    The anion exchanger consists of three components: an extracting substance, which can be used as primary, secondary or tertiary amines, or a quaternary ammonium base with a long alkyl chain, slightly soluble in water, with a molecular weight above 200; a modifier designed to facilitate phase separation during extraction, which uses alcohols with 8-14 carbon atoms; and a diluent which plays the role of a carrier for the first two components and reduces the viscosity of the medium. A hydrocarbon or a mixture of hydrocarbons is used as a diluent, for example, in the distillation of petroleum.
    Example 1. The following substances are contained in the organic phase: 10 vol.% D2EHPK, 90 vol.% Oil product.
    The oil product has the following technical characteristics: density at 15 ° С 0.780; distillate - the initial point is not limited, 50% selection 220C, 90% selection 250 ° C, end point 275 ° C, ignition point 38 °
    Iron is loaded into this organic phase to a concentration of 0.338 g / l and mixed once with a solution of 5.9 M hydrochloric acid. The ratio of the organic phase to the aqueous phase is 10. The concentration of iron in the organic phase is 0.110 g / l and the concentration of iron in the aqueous phase is 2.19 g / l; extraction of 67.45%.
    In tab. 1 shows the concentrations of hydrochloric acid in the aqueous solution used to purify D2EHPA from iron.
    When a single contact of both phases receive the results shown in table. 2
    Example 2. The composition of the organic phase is the same as in the previous examples. In tab. 3 shows the concentration of iron in the organic phase, the composition of the extracting solution and the flow ratio of the organic and aqueous phases.
    When a single contact of both phases receive the following results, shown in table. four.
    Example 3. The process of removing iron from an aqueous acid solution. Composition of anion exchanger: 15% ailberly A-2 (industrial secondary amine), 6% isodecanol, 79% mixture of hydrocarbons.
    The anion exchanger is mixed with an aqueous solution of an acid containing iron. Then the anion exchanger contaminated with iron is treated once with water.
    In tab. 5 shows the initial concentrations and ratios.
    The results are shown in Table. 6
    PRI me R 4. Continuous process on the pilot plant.
    Hydrochloric acid with a concentration of 4.9 mol / l is used as an aqueous solution containing chloride ions.
    .In tab. 7 shows the concentration of Fe, Zn and her in various flows of the circuit.
    The extraction of the organic phase containing D2EHPA is 72.41%. The removal of iron from the aqueous acid solution by an anion exchanger is 99.30%.
    Example 5. An organic phase containing iron and having the composition: 10 vol% D2EHPK, 90 vol% oil product, 0.3 g / l iron is brought into contact with the composition solutions: 2 mol / l hydrochloric acid, 4 mol / l calcium chloride; 2 mol / l hydrochloric acid, 2 mol / l sodium chloride and 2 mol / l calcium chloride; 2 mol / l sulfuric acid and 4 mol / l sodium chloride.
    The ratio of organic and aqueous phases is 10: 1. After stirring, the organic and aqueous phases are separated and the iron content is determined. In tab. 8 shows the results obtained.
    Example b. Use as anion exchanger of four types of amines.
    Use four organic phases of the composition, vol.%: 20 primary. amine + 8 isodecyl alcohol + 32 kerosene; 15 secondary amine + 6 isodecyl alcohol + 79 kerosene; 10 tert, amine + 4 isodecyl alcohol + 86 kerosene; b quarter ammonium base + 4 isodecyl alcohol + 90 kerosene.
    The organic phases are contacted with an aqueous acidic solution containing iron, when the organic phase is separated into an aqueous phase of 2: 1. The aqueous phase has the following composition: 5.5 mol / l hydrochloric acid; 0.5 mol / L calcium chloride; 3.2 g / l of iron.
    After mixing, both phases are anashised. In tab. 9 shows the results obtained.
    Iron extracted by anion exchange can be re-extracted with water.
    The organic phase is treated
    0 water at the ratio of organic and aqueous phase. The results are shown in Table. ten.
    Example 7. As an aqueous acidic solution using a mixture
    5 from 5 to 50% by volume of sulfuric acid and from 0.1 mol / l to saturation of the metal chloride .:
    The initial organic phase consists of 10 vol.% D2EHPK, 90 vol.% oil product.
    In tab. 11 shows the initial concentrations and ratios.
    Both phases are in contact.
    The results are shown in Table. 12.
    five
    Example 8. A mixture of from 3 to 30% by volume of hydrochloric acid and metal chloride in a concentration of from 0.1 mol / l to saturation is used as the aqueous acidic solution. Composition
    0 source
    In tab. 13 shows the initial concentrations and ratios.
    Both. the phases are contacted for b min.
    five
    Example 9. A mixture of from 3 to 18 vol.% Hydrochloric acid, from 5 to 30 vol.% Of sulfuric acid and metal chloride from 1 mol / l is used as an aqueous acidic solution.
    0 to saturation.,
    In tab. 14 shows the initial concentrations and ratios.
    Both phases are contacted for 5 minutes.
    five
    The results are shown in Table. 15.
     PR and measure 10. The purification of the organic phase containing D2EHPA is carried out at a temperature of 10-50 ° C.
    The composition of the organic phase such
    0 is the same as in the previous examples. The aqueous solution is a saturated NaCl solution containing
    19% by volume of it. ;
    Both phases are organic and aqueous with
    5 10: 1 ratio contact for 5 minutes in one stage at different temperatures, pax. The results are shown in Table. sixteen.
    Table
    T a 6 persons
    T a b l and c a 3
    1. An organic phase containing
    D2EHPH and iron contaminated
    3. Purified from organo iron phase
    Table 5
    Table
    0.29 0.26 0.5
    1119 0.08 0.013 0.5
    1119
    Iron-purified aqueous acid solution
    Aqueous acidic solution containing extractive grade
    Continued Table 7
    114
    0.014 1.70 161.0
    Table 9
    3
    0.33
    b 0.33
    9 0.33 18 0.33
    Table 11
    Table 12
    Table 13
    Table 14
    10 10 10 10
    one
    2 3 Satisfaction
    15
    71202516
    That blitz15
    Table 16
    权利要求:
    Claims (2)
    [1]
    Claim
    1. The method of purification of extractants based on di-2-ethylhexylphosphoric acid from iron (SH) by extraction, its aqueous acid solution containing chloride ions, characterized in that, in order to increase the degree of purification, as an aqueous solution, use an aqueous solution of sulfuric acid in a concentration of from 5 to 40 50 vol.% and metal chloride of group I or I in a concentration of 0.1 mol / l to saturation, or an aqueous solution of hydrochloric acid in a concentration of from 3 to 30 vol.% chloride metal of group I or II of group 45 in a concentration of 0.1 mol / l to saturation, or an aqueous solution with hydrochloric acid at a concentration of 3 to 25 vol.%, sulfuric acid at a concentration of 5 to 40 vol.% and metal chloride of group I and II at a concentration of 0.1 mol / l to saturation, and the process is carried out at a ratio extractant and an aqueous solution of 5-30: 1 and a temperature of 10-50 ° C, the resulting extract is subjected to treatment with a liquid anion exchanger, followed by regeneration of the anion exchanger with water.
    [2]
    2. The method of pop. 1, different from the fact that as a liquid anion exchanger an organic solution is used containing primary, secondary, or tert, amine, an aliphatic alcohol with 8-14 carbon atoms and a mixture of hydrocarbons.
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    同族专利:
    公开号 | 公开日
    JPS5289566A|1977-07-27|
    BR7606683A|1977-11-16|
    CA1086076A|1980-09-23|
    JPS6026049B2|1985-06-21|
    ES441536A1|1977-04-01|
    MX144484A|1981-10-20|
    DE2645130A1|1977-04-14|
    SE7610999L|1977-04-07|
    FR2327199A1|1977-05-06|
    IT1068260B|1985-03-21|
    PT65683A|1976-11-01|
    PL107319B1|1980-02-29|
    ZA765992B|1977-09-28|
    PT65683B|1978-04-14|
    RO72871A|1981-06-26|
    IL50629D0|1976-12-31|
    AU1843376A|1978-04-13|
    FI762829A|1977-04-07|
    AU512317B2|1980-10-02|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    FR1354812A|1962-03-19|1964-03-13|Int Nickel Canada|Process for the concentration of nickel and cobalt present in aqueous solutions|
    AU487596B2|1974-06-03|1975-12-04|Thorsen Gunnar|Process for extraction and separation of metals using liquid cation exchangers|LU81600A1|1979-08-13|1981-03-24|Metallurgie Hoboken|METHOD FOR TREATING AN ORGANIC PHASE CONTAINING IRON CHLORIDE, MOLYBDENE CHLORIDE AND HCl|
    EP0030067A1|1979-11-30|1981-06-10|The Board Of Trustees Of The Michigan State University|Process for the extraction of metal ions|
    JP4670685B2|2006-03-03|2011-04-13|トヨタ自動車株式会社|Power transmission device|
    EP1925698B1|2006-11-24|2010-03-17|Groz-Beckert KG|Transmission for a heald drive|
    CN108642282A|2018-03-26|2018-10-12|杨秋良|The recovery method of vanadium in a kind of fluorine-containing extracting vanadium from stone coal pickle liquor|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ES441536A|ES441536A1|1975-10-06|1975-10-06|Method of eliminating iron accumlated in liquiddliquid extraction organic phase containing dii22ethyl hexyl phosphoric acid|
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