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WO2018088727A1 - Procédé de purification d'acide chlorhydrique résiduaire - Google Patents

Procédé de purification d'acide chlorhydrique résiduaire Download PDF

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Publication number
WO2018088727A1
WO2018088727A1 PCT/KR2017/011869 KR2017011869W WO2018088727A1 WO 2018088727 A1 WO2018088727 A1 WO 2018088727A1 KR 2017011869 W KR2017011869 W KR 2017011869W WO 2018088727 A1 WO2018088727 A1 WO 2018088727A1
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Prior art keywords
hydrochloric acid
organic solvent
waste hydrochloric
waste
purification method
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PCT/KR2017/011869
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English (en)
Korean (ko)
Inventor
엄희준
이동철
김연이
최정호
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LG Chem Ltd
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LG Chem Ltd
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Priority claimed from KR1020170138499A external-priority patent/KR102045523B1/ko
Application filed by LG Chem Ltd filed Critical LG Chem Ltd
Priority to JP2018538688A priority Critical patent/JP6660476B2/ja
Priority to US15/774,915 priority patent/US11472702B2/en
Priority to CN201780004237.9A priority patent/CN108290083B/zh
Priority to EP17863300.4A priority patent/EP3539636A4/fr
Publication of WO2018088727A1 publication Critical patent/WO2018088727A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/02—Solvent extraction of solids

Definitions

  • the present invention relates to a method for purifying waste hydrochloric acid.
  • Ethylene dichloride (1,2-dichloroethane, EDC) is a substance produced during the reaction of vinyl chloride monomer synthesis (see Scheme 1 below), which is a direct chlorine method through the reaction of ethylene and chlorine, ethylene, hydrogen chloride and air (oxygen). It can be prepared by the chlorine oxide method by the reaction of).
  • waste hydrochloric acids are recycled into hydrochloric acid in the chlor-alkali electrolyzer anolyte, or recycled as oxy-chlorination raw materials
  • the plant can reduce the emissions of hazardous substances and reduce the cost of purchasing hydrogen chloride. Red and economic benefits can occur. Therefore, various methods for purifying and recycling waste hydrochloric acid have been studied in order to reduce manufacturing costs.
  • the free residual chlorine present in the spent hydrochloric acid causes severe deactivation of the active site of the ion exchange resin, the free residual chlorine must be removed before the Fe refining process is performed.
  • the free residual chlorine is removed by vacuum dechlorination, steam / air stripping, sulfite addition, active carbon, and UV method. Etc. can be used.
  • the vacuum (decompression) desalting method is a method of removing Cl 2 through pressure control, and can be combined with the existing anolyte desalting method.
  • the steam / air stripping method has a disadvantage in that energy consumption is large and additional investment costs are generated by stripping through steam or air.
  • the sulfite addition method is a method of reducing Cl 2 through an oxidation reaction of sulfite, such as Na 2 SO 3 , NaHSO 3 , to sulfate, as in Scheme 2 below, and this method also removes free residual chlorine efficiency.
  • This low, existing SRS system Sulfate Removal System
  • the method of using activated carbon is a method of adsorbing Cl 2 using activated carbon, and it is troublesome to consider efficiency in a strong acid atmosphere and to consider a gas target and a liquid target.
  • the UV method is a process of selectively removing free residual chlorine using UV energy as shown in Scheme 3, and it is reported that HOCl is well absorbed at a wavelength of 238 nm.
  • this method also has the disadvantage of increased process cost and low free chlorine removal efficiency.
  • the conventional method of removing Fe from waste hydrochloric acid has a problem of not only high energy and cost consumption because of complicated process steps, but also low free chlorine removal efficiency from waste hydrochloric acid.
  • Patent Document 1 US Patent No. 2,787,525
  • Patent Document 2 Japanese Patent Publication No. 3511244
  • a first object of the present invention is to provide a waste hydrochloric acid purification method using a solvent extraction method.
  • the amount of the extractant is 40 mol or more based on 1 mol of iron (Fe) ions among the metal components contained in the waste hydrochloric acid,
  • the waste hydrochloric acid: extract solution is 1: 1 to 1: 1 to provide a waste hydrochloric acid purification method to be mixed.
  • the organic solvent used to prepare the extraction solution may include at least one solvent selected from the group consisting of an aromatic hydrocarbon solvent, an aliphatic hydrocarbon solvent, and an alcohol.
  • the aromatic hydrocarbon solvent may include at least one selected from the group consisting of toluene and xylene.
  • the aliphatic hydrocarbon solvent is at least one cycloaliphatic hydrocarbon solvent selected from the group consisting of methyl cyclohexane and cyclohexane, or a linear hydrocarbon solvent having 6 to 20 carbon atoms, such as kerosene (kerosene, kerosene), normal hexane, heptane, octane, And one or more selected from the group consisting of nonane, decane, and dodetan.
  • kerosene kerosene, kerosene
  • normal hexane normal hexane
  • heptane heptane
  • octane octane
  • the alcohol may include a monohydric alcohol having 6 to 20 carbon atoms.
  • the extracting agent may be at least one or more selected from the group consisting of trioctylamine, methyl isobutyl ketone, trialkylphosphine oxide and tributyl phosphate, specifically selected from the group consisting of trioctylamine and methyl isobutyl ketone It may be at least one, more specifically trioctylamine.
  • the amount of the extractant may be 40 mol to 60 mol based on 1 mol of the iron (Fe) ion component among the metal components contained in the waste hydrochloric acid.
  • the metal component, especially the iron (Fe) ion component can be effectively removed to 1 ppm or less from the waste hydrochloric acid, the recycling efficiency of hydrochloric acid Can improve.
  • waste hydrochloric acid purification method using the solvent extraction method of the present invention can be repeated several times through the regeneration of the solvent used, resulting in a simplification of the process compared to the existing process, thereby reducing energy and manufacturing costs have.
  • FIG. 1 is a flowchart illustrating a waste hydrochloric acid purification method using the solvent extraction method of the present invention.
  • FIG. 2 is a process schematic diagram of a method for purifying waste hydrochloric acid using the solvent extraction method of the present invention.
  • Figure 3 is a photograph comparing the color change of hydrochloric acid before and after purification of the purified hydrochloric acid using the solvent extraction method of the present invention.
  • the metal component particularly the iron (Fe) ion component
  • the metal component can be effectively removed to 1 ppm or less, specifically 0.1 ppm or less. It is possible to reduce the energy consumption and cost, and at the same time provide a method for purifying waste hydrochloric acid with high purity.
  • the amount of the extractant is 40 mol or more based on 1 mol of iron (Fe) ions among the metal components contained in the waste hydrochloric acid,
  • the waste hydrochloric acid: extract solution is 1: 1 to 1: 1 to provide a waste hydrochloric acid purification method to be mixed.
  • FIG. 1 is a flowchart illustrating a waste hydrochloric acid purification method using the solvent extraction method of the present invention according to exemplary embodiments.
  • 2 is a process schematic diagram of a method for purifying waste hydrochloric acid using the solvent extraction method of the present invention.
  • the method for purifying hydrochloric acid of the present invention may further include a step (S0) of measuring the concentration of iron (Fe) ion component among the metal components included in the waste hydrochloric acid before the step (S1) of preparing the extraction solution. have.
  • the concentration of iron (Fe) ions of the metal components contained in the waste hydrochloric acid can be measured by an inductively coupled plasma mass spectrometry (Inductively coupled plasma mass spectrometry). Specifically, the method measured about 5g of the sample in a corning tube (corning tube) was added as an internal standard, diluted with 25 mL of ultrapure water and analyzed using an ICP-OES (Optima 7300 DV) apparatus.
  • ICP-OES Optima 7300 DV
  • the hydrochloric acid purification method of the present invention may include the step of preparing an extraction solution by dissolving the extractant in an organic solvent (S1).
  • the organic solvent is a (dilution) solvent used to improve the physical properties such as viscosity, specific gravity, etc. of the organic phase, and to control the concentration of the extractant, and representative examples thereof include aromatic hydrocarbon solvents, aliphatic hydrocarbon solvents, and alcohols. It may include at least one solvent selected from the group consisting of.
  • the aromatic hydrocarbon solvent may include at least one selected from the group consisting of toluene and xylene.
  • the aliphatic hydrocarbon solvent is at least one cycloaliphatic hydrocarbon solvent selected from the group consisting of methyl cyclohexane and cyclohexane, or a linear hydrocarbon solvent having 6 to 20 carbon atoms, specifically kerosene (kerosene, kerosene), normal hexane, heptane, octane And nonane, decane, and dodetan.
  • the alcohol may include a monohydric alcohol having 6 to 20 carbon atoms, and representative examples thereof include 2-ethyl hexanol, 2-dodecanol, and the like.
  • the organic solvent may be affected by the extraction equilibrium and the extraction rate according to the hydrocarbon content, specifically, the organic solvent is a phase separation with water smoothly, selectivity to the metal (selectivity) ) Is higher than water, and it is preferable to use toluene which shows the lowest value of TOC (total organic carbon) after the extraction process.
  • the TOC value is a value that can know how much the extractant or diluent is contained by checking the concentration of organic impurities contained in the purified high purity hydrochloric acid after the extraction process.
  • the extractant may be used as a compound for ion exchange reaction, at least one selected from the group consisting of trioctylamine, methyl isobutyl ketone, trialkylphosphine oxide and tributyl phosphate as a representative example, Among them, the phase separation effect is higher than that of the trialkylphosphine oxide or tributyl phosphate, which is a phosphorus-based extractant, and it is easy to remove metal components, particularly iron (Fe) ions, from waste hydrochloric acid, and reuse the organic solvent used in the purification process And it is more preferable to use trioctylamine and methyl isobutyl ketone which can implement a cost-saving effect and the like, more preferably trioctylamine.
  • Alamine 336 or Aliquat 336 which is a nitrogen-based extractant (containing trioctylamine), or Cyanex 923, which is a phosphorus-based extractant (containing trialkylphosphine oxide), may be used alone or in addition. have.
  • the amount of the extractant is 40 moles or more, specifically 40 moles to 60 moles, more specifically 40 moles to 50 moles, and more specifically 40 moles based on 1 mole of iron (Fe) ions in the metal components included in the spent hydrochloric acid Moles to 45 moles.
  • the effect of removing metal components, particularly iron (Fe) ions may be insignificant.
  • the amount of the extractant exceeds 60 moles, the effect of removing the metal components, particularly iron (Fe) ions component is not significantly different, but the manufacturing cost may increase because a large amount of the extractant is used. Therefore, considering the proper manufacturing cost and the efficiency of iron (Fe) ion component removal, it can be used in less than 60 moles.
  • the waste hydrochloric acid is added to a reaction vessel, and then, an extraction solution is added and the metal component contained in the waste hydrochloric acid is extracted with an organic solvent while stirring. It can be carried out (S2).
  • the metal component included in the spent hydrochloric acid mainly contains iron ions, and in addition to the metal components, such as Al 3+ , Ca 2+ , K + , Mg 2+ , Ni 2+ may be further included. .
  • the hydrochloric acid the extraction solution may be mixed in a 1: 0.1 to 1: 1 volume ratio, specifically 1: 1 volume ratio. If the extraction solution is added in less than 0.1 volume ratio (1/10) with respect to the waste hydrochloric acid, there is a disadvantage in that an emulsion occurs in the waste hydrochloric acid layer and thus phase separation is impossible. In addition, when the extraction solution is added in more than 1 volume ratio, there is a disadvantage that the process cost increases.
  • the extraction step (S2) may be carried out for 10 seconds to 60 seconds, specifically 20 seconds to 60 seconds while stirring the mixed solution of the hydrochloric acid and the extraction solution at a speed of 200 rpm to 600 rpm at an atmospheric temperature.
  • the room temperature is the average temperature or the temperature in the atmosphere throughout the year, specifically, means a temperature of 20 ⁇ 5 °C range.
  • the stirring speed is less than 200 rpm, the mixing is not smooth, there is a disadvantage in that the extraction efficiency of the metal component or the iron ion component is reduced.
  • the stirring speed exceeds 600 rpm, the metal component extraction effect is insignificant while the energy consumption may increase.
  • stirring step may be performed using a magnetic bar stirring plate or a static mixer.
  • the mixing step for the phase separation may be carried out within 20 seconds.
  • purified hydrochloric acid may be obtained by recovering the waste hydrochloric acid layer which is an phase separated from the phase separation step (S3) and is located at the bottom (S4). ).
  • the purified hydrochloric acid may effectively remove the metal component, particularly the iron (Fe) ion component, the iron (Fe) ion component may remain at a concentration of 1 ppm or less, specifically 0.1 ppm or less.
  • the waste hydrochloric acid purification method of the present invention may further comprise the step of purifying the organic solvent used in the waste hydrochloric acid, in order to increase the regeneration efficiency of the organic solvent used in the waste hydrochloric acid purification.
  • Recovering the phase-separated organic solvent and the water layer, respectively (S7); may further include.
  • the organic solvent recovered by phase separation after waste hydrochloric acid purification may be added to the reactor once again, and then distilled water may be added to remove metal components remaining in the organic solvent (S5).
  • the residual metal component in the organic solvent can be extracted with water.
  • the organic solvent: distilled water may be mixed in a volume ratio of 1: 0.1 to 1: 1, specifically 1: 1 volume ratio. If the distilled water is less than 0.1, the extraction effect of the metal component is reduced, and when the distilled water is added in more than 1 volume ratio (1/1), the emulsion may occur and phase separation may not occur.
  • the stripping step (S5) may be performed for 10 seconds to 60 seconds, specifically 20 seconds to 60 seconds while stirring the mixed solution of the separated organic solvent and distilled water at a speed of 200 rpm to 600 rpm at room temperature.
  • the room temperature is the average temperature or the temperature in the atmosphere throughout the year, specifically, means a temperature of 20 ⁇ 5 °C range.
  • the stirring speed is less than 200 rpm, the mixing is not smooth, there is a disadvantage in that the extraction efficiency of the metal component is reduced.
  • the stirring speed exceeds 600 rpm, the metal component extraction effect is insignificant while the energy consumption may be increased.
  • the stirring time for the stripping is less than 20 seconds, there is a disadvantage in that sufficient time for extracting the metal is not secured, thereby reducing the extraction efficiency of the metal component.
  • the stirring time exceeds 60 seconds, the amount of the extracted metal component does not show a big difference, but the process time and cost increases because the amount of waste organic solvent that can be processed in the process is limited.
  • the stripping step (S5) may be used a variety of mixing device, as a representative example may use a magnetic bar stirring plate or a static mixer.
  • the phase separation step may be carried out within 20 seconds.
  • the distilled water layer which is the phase separated and the extracted phase located at the bottom, is removed, and the organic layer located at the top is recovered (S7), thereby effectively regenerating the organic phase used for waste hydrochloric acid purification.
  • the method of the present invention further comprises the step of regenerating the organic solvent used in the waste hydrochloric acid purification method, it is possible to repeat the use of the organic solvent several times, significantly reducing the process operating costs and the like compared to the existing process can do.
  • the concentration of iron (Fe) ions contained in 100 ml of waste hydrochloric acid was measured by an inductively coupled plasma mass spectrometry (S0).
  • the extraction solution was added to 100 ml of waste hydrochloric acid, and metal components contained in the waste hydrochloric acid were extracted with an organic solvent while stirring at room temperature for 60 seconds at a speed of 200 rpm (S2).
  • the residual metal concentration was measured using Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES), and the total organic carbon (TOC) component was analyzed by a TOC analyzer (analyzer).
  • ICP-OES Inductively Coupled Plasma Atomic Emission Spectroscopy
  • TOC total organic carbon
  • the residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 1 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that cyclohexane was used instead of toluene in Example 1.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Example 3 The hydrochloric acid purified in the same manner as in Example 3 was obtained except that the waste hydrochloric acid layer separated in Example 3 was extracted once more using cyclohexane in which 40 moles of the extractant was dissolved (S2). The residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that xylene was used instead of toluene in Example 1.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Example 2 The hydrochloric acid purified in the same manner as in Example 1 was obtained except that the waste hydrochloric acid layer separated in Example 5 was extracted once more using xylene in which 40 moles of the extractant was dissolved (S2). The residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that in Example 1, a mixed solution of octane and 2-ethyl hexanol (1: 1 volume ratio) was used instead of toluene.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that in Example 1, a mixed solution of decane and 2-ethyl hexanol (1: 1 volume ratio) was used instead of toluene.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that a mixed solution (1: 1 volume ratio) of dodecane and 2-ethyl hexanol was used instead of toluene in Example 1.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that a mixed solution of kerosene and 2-ethyl hexanol (1: 1 volume ratio) was used instead of toluene in Example 1.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that in Example 1, a mixed solution of kerosene and 2-dodecanol (1: 1 by volume) was used instead of toluene.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that in the step (S1) of Example 1, an extraction solution was prepared by dissolving trialkylphosphine oxide instead of trioctylamine as an extractant.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 3, except that in the step (S1) of Example 3, an extraction solution was prepared by dissolving trialkylphosphine oxide instead of trioctylamine as an extractant.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that methyl cyclohexane was used instead of toluene when preparing the extraction solution in the step (S1) of Example 1.
  • the residual metal concentration and TOC in the purified hydrochloric acid were measured, and the results are shown in Tables 1 and 2 below.
  • Purified hydrochloric acid was obtained in the same manner as in Comparative Example 1 except for using the ion exchange resin (IRA-910) instead of the ion exchange resin (IRA-900) in Comparative Example 1.
  • the residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 1 below.
  • the reaction was then filtered to remove the ion exchange resin and to obtain purified hydrochloric acid.
  • the residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 1 below.
  • reaction was then filtered to remove the ion exchange resin and to obtain purified hydrochloric acid.
  • Example 3 Trioctylamine Cyclohexane 5 16 ⁇ 0.1 5 5
  • Example 4 Trioctylamine Cyclohexane (twice) 5 16 ⁇ 0.1 5 5
  • Example 5 Trioctylamine xylene 6 16 ⁇ 0.1 5
  • Example 6 Trioctylamine Xylene (2 times) 6 17 ⁇ 0.1 5 5
  • Example 7 Trioctylamine Octane + 2-ethyl hexanol 7 17 ⁇ 0.1 5 5
  • Example 8 Trioctylamine Decane + 2-ethyl hexanol 7 16 ⁇ 0.1 5 5
  • Example 9 Trioctylamine Dodecane + 2-ethyl hexanol 7 16 ⁇ 0.1 5
  • the concentration of the residual iron (Fe) ion component is 1 ppm or less (95% or more removed) regardless of the type of the organic solvent. You can see that.
  • Comparative Examples 1 to 3 using ion exchange resins to remove iron (Fe) ions in the waste hydrochloric acid the concentration of residual iron (Fe) ions is 1 ppm or more (about 80%). You can see that. In particular, in the case of Comparative Example 3 in which NaSO 3 was added to remove free residual chlorine, it was confirmed that the Fe removal efficiency is not affected.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that 50 ml of the organic solvent was used instead of 100 ml in Example 1. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 3 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that 30 ml of the organic solvent was used instead of 100 ml in Example 1. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 3 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that 10 ml of the organic solvent was used instead of 100 ml in Example 1. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 3 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the extraction time by stirring the organic solvent and the spent hydrochloric acid in Example 1 was performed at 50 seconds. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 4 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the extraction time by stirring the organic solvent and the spent hydrochloric acid in Example 1 was performed for 30 seconds.
  • the concentration of iron (Fe) ions in the purified hydrochloric acid was measured, and the results are shown in Table 4 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the extraction time by stirring the organic solvent and the spent hydrochloric acid in Example 1 was performed for 20 seconds.
  • the concentration of iron (Fe) ions in the purified hydrochloric acid was measured, and the results are shown in Table 4 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the extraction time by stirring the organic solvent and the spent hydrochloric acid in Example 1 was performed for 10 seconds.
  • the concentration of iron (Fe) ions in the purified hydrochloric acid was measured, and the results are shown in Table 4 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the stirring speed of the organic solvent and the hydrochloric acid for extraction in Example 1 was performed at 600 rpm instead of 200 rpm. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 5 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the stirring speed of the organic solvent and the hydrochloric acid for extraction in Example 1 was performed at 300 rpm instead of 200 rpm.
  • the residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 5 below.
  • Purified hydrochloric acid was obtained in the same manner as in Example 1, except that the stirring speed of the organic solvent and the hydrochloric acid for extraction in Example 1 was performed at 100 rpm instead of 200 rpm. The residual metal concentration in the purified hydrochloric acid was measured and the results are shown in Table 5 below.
  • the extraction solution was added to 100 ml of hydrochloric acid, and the metal components contained in the hydrochloric acid were extracted with an organic solvent while stirring at room temperature for 60 seconds at a speed of 200 rpm (S2).
  • the mixed solution of the organic solvent (1) and the water layer removed in the separator was phase-separated for about 20 seconds, to separate the organic solvent and the water layer (S6).
  • the separated water layer 1 was recovered (S7).
  • the organic solvent (1) recovered by phase separation from the waste hydrochloric acid layer of Example 25 was re-injected into 100 ml of waste hydrochloric acid, and the organic solvent was mixed with the metal components contained in the waste hydrochloric acid while stirring at room temperature for 1 hour at a speed of 200 rpm. Extracted with (S2-2).
  • the organic solvent (2) recovered by phase separation from the waste hydrochloric acid layer of Example 26 was recycled to 100 ml of waste hydrochloric acid, and the metal components contained in the waste hydrochloric acid were stirred at room temperature for 1 hour at 200 rpm. Extracted with (S2-3).
  • the mixed solution of the organic solvent (3) and the water layer removed in the separator was phase-separated for about 20 seconds, to separate the organic solvent and the water layer (S6-3).
  • the separated water layer 3 was recovered (S7-3).
  • the organic solvent (3) recovered by phase separation from the waste hydrochloric acid layer of Example 27 was re-injected into 100 ml of waste hydrochloric acid, and the metal components contained in the waste hydrochloric acid were stirred at room temperature for 1 hour at 200 rpm. Extracted with (S2-4).
  • the extraction solution was added to 100 ml of waste hydrochloric acid, and metal components contained in the waste hydrochloric acid were extracted with an organic solvent while stirring at room temperature for 60 seconds at a speed of 200 rpm (S'2).
  • the extraction solution was added to 100 ml of waste hydrochloric acid, and metal components contained in the waste hydrochloric acid were extracted with an organic solvent while stirring at room temperature for 60 seconds at a speed of 200 rpm (S'2).

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Abstract

La présente invention concerne un procédé de purification d'acide chlorhydrique résiduaire et, plus précisément, un procédé de purification d'acide chlorhydrique résiduaire, comprenant les étapes consistant à : (S1) préparer une solution d'extraction par dissolution d'un agent d'extraction dans un solvant organique; (S2) extraire un composant métallique avec un solvant organique par injection de la solution d'extraction dans de l'acide chlorhydrique résiduaire; (S3) séparer la phase d'une couche d'acide chlorhydrique aqueux et du solvant organique contenant le composant métallique; et (S4) obtenir de l'acide chlorhydrique purifié par récupération de la couche d'acide chlorhydrique aqueux (fractionnée) à séparation de phase. Dans ce procédé au moins 40 moles de l'agent d'extraction sont utilisées sur la base d'une mole de Fe contenu dans l'acide chlorhydrique résiduaire, et l'acide chlorhydrique résiduaire et la solution d'extraction sont mélangés dans un rapport volumique d'acide chlorhydrique résiduaire : une solution d'extraction de 1 à 0,1-1.
PCT/KR2017/011869 2016-11-09 2017-10-25 Procédé de purification d'acide chlorhydrique résiduaire Ceased WO2018088727A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2018538688A JP6660476B2 (ja) 2016-11-09 2017-10-25 廃塩酸の精製方法
US15/774,915 US11472702B2 (en) 2016-11-09 2017-10-25 Method of purifying waste hydrochloric acid
CN201780004237.9A CN108290083B (zh) 2016-11-09 2017-10-25 纯化废盐酸的方法
EP17863300.4A EP3539636A4 (fr) 2016-11-09 2017-10-25 Procédé de purification d'acide chlorhydrique résiduaire

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KR1020170138499A KR102045523B1 (ko) 2016-11-09 2017-10-24 폐염산 정제 방법

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Citations (7)

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JPS511244B1 (fr) 1971-05-13 1976-01-16
KR890000355B1 (ko) * 1981-01-14 1989-03-14 디.제이.삭커스 신호의 자기기록 및 재생장치와 이에 부속된 자기 변환 헤드
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