CN110697743A - Method for preparing 4N-grade magnesium sulfate - Google Patents
Method for preparing 4N-grade magnesium sulfate Download PDFInfo
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- CN110697743A CN110697743A CN201911083634.7A CN201911083634A CN110697743A CN 110697743 A CN110697743 A CN 110697743A CN 201911083634 A CN201911083634 A CN 201911083634A CN 110697743 A CN110697743 A CN 110697743A
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Abstract
The method for preparing 4N-grade magnesium sulfate directly prepares 4N-grade magnesium sulfate solution by using magnesium-containing brine as feed liquid, P507 as an extracting agent and sec-octanol as a modifying agent and comprising three steps of full-load fractional extraction and separation of NaKMg/MgCaPbAlFe, full-load fractional extraction and separation of NaK/Mg and fractional extraction and separation of Mg/CaPbAlFe. The purity of the 4N-grade magnesium sulfate solution of the target product is 99.991-99.998%, and the yield of magnesium is 96-98%. The method has the advantages of high product purity, high magnesium yield, low reagent consumption, high separation efficiency, short process flow, low production cost and the like.
Description
Technical Field
The invention relates to a method for preparing 4N-grade magnesium sulfate, in particular to a method for directly preparing a 4N-grade magnesium sulfate solution by taking magnesium-containing brine as a feed liquid, P507 as an extracting agent and octanol as a modifying agent to separate and remove metal elements such as sodium, potassium, calcium, lead, aluminum, iron and the like in the feed liquid and non-metal elements such as chlorine, silicon, arsenic and the like. The invention belongs to the technical field of preparation of 4N-grade magnesium sulfate.
Background
The bittern is an important resource for extracting magnesium, and mainly contains metal elements of magnesium, sodium, potassium, calcium, aluminum and iron, nonmetal elements of sulfur (sulfate radical) and chlorine (chloride ion), and trace elements of lead, cadmium, silicon, arsenic and the like. Currently, the purity of magnesium sulfate extracted from magnesium-containing brine can only reach 3N grade at most, and the purity of magnesium sulfate extracted from other magnesium-containing primary raw materials (magnesium ore) is 2N grade generally. The existing method for preparing 4N-grade magnesium sulfate uses 2N-grade magnesium sulfate (industrial grade) as raw material. Therefore, no method for directly preparing 4N-grade magnesium sulfate from magnesium-containing brine exists at present. The method for indirectly preparing the 4N-grade magnesium sulfate has the defects of long process, low magnesium yield, high production cost and the like.
Aiming at the defects of long flow, low magnesium yield, high production cost and the like of the method for indirectly preparing the 4N-grade magnesium sulfate, which is not a method for directly preparing the 4N-grade magnesium sulfate from magnesium-containing brine at present, the invention establishes the method for efficiently separating metal and non-metal impurities in the magnesium-containing brine and directly preparing the 4N-grade magnesium sulfate solution.
Disclosure of Invention
Aiming at the defects that no method for directly preparing 4N-grade magnesium sulfate from magnesium-containing brine exists, but the method for indirectly preparing 4N-grade magnesium sulfate has the defects of long process, low magnesium yield, high production cost and the like, the method for preparing 4N-grade magnesium sulfate solution directly from magnesium-containing brine is provided.
The invention relates to a method for preparing 4N-grade magnesium sulfate, which takes magnesium-containing brine as a feed liquid, 2-ethylhexyl phosphonic acid mono-2-ethylhexyl hexyl phosphonic acid (P507 for short) as an extracting agent and sec-octanol as a modifier, separates and removes metal elements such as sodium, potassium, calcium, lead, aluminum, iron and the like in the feed liquid, and separates and removes non-metal elements such as chlorine, silicon, arsenic and the like, thereby directly preparing 4N-grade magnesium sulfate solution.
The invention relates to a method for preparing 4N-grade magnesium sulfate, which consists of 3 steps, namely full-load fractional extraction separation NaKMg/MgCaPbAlFe, full-load fractional extraction separation NaK/Mg and fractional extraction separation Mg/CaPbAlFe; the extraction section of full-load fractionation, extraction and separation NaKMg/MgCaPbAlFe realizes the separation of NaKMg/CaPbAlFe, and the washing section realizes the separation of NaK/MgCaPbAlFe; the method is characterized in that NaKMg/MgCaPbAlFe is separated by full-load fractionation extraction, a balanced load P507 organic phase obtained by separating NaK/Mg feed grade by full-load fractionation extraction is used as an extraction organic phase, and a balanced water phase obtained by separating Mg/CaPbAlFe feed grade by fractionation extraction is used as a detergent. Full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaPbAlFe are directly connected in series; the outlet organic phase which is fully loaded with NaK/Mg and separated by fractional extraction is used as an extraction organic phase for separating Mg/CaPbAlFe by fractional extraction, and directly enters the 1 st stage for separating Mg/CaPbAlFe by fractional extraction; the 1 st stage outlet aqueous phase of the Mg/CaPbAlFe separation by fractional extraction is used as a washing agent for full-load fractional extraction separation of NaK/Mg.
The method for preparing 4N-grade magnesium sulfate comprises the following 3 steps:
step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
Step 1 is full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe, the extraction section realizes the separation of NaKMg/CaPbAlFe, and the washing section realizes the separation of NaK/MgCaPbAlFe. And (3) taking a balanced load P507 organic phase obtained from the feed stage of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking magnesium-containing brine as a feed liquid, and taking a balanced water phase obtained from the feed stage of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. And (3) feeding the balanced load P507 organic phase obtained from the feed stage of the NaK/Mg full-load fractional extraction system in the step 2 into a NaKMg/MgCaPbAlFe full-load fractional extraction system from the 1 st stage, feeding magnesium-containing brine into the NaKMg/MgCaPbAlFe full-load fractional extraction system from the feed stage, and feeding the balanced water phase obtained from the feed stage of the Mg/CaPbAlFe fractional extraction system in the step 3 into the NaKMg/MgCaPbAlFe full-load fractional extraction system from the last stage 1. Obtaining a magnesium sulfate solution containing Na, K, Cl, Si and As from the water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the magnesium sulfate solution As a feed liquid for full-load fractional extraction and separation of NaK/Mg in the step 2; and (3) obtaining a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron from the last grade 1 outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P507 organic phase as feed liquid for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
And step 2, full-load fractionation, extraction and separation of NaK/Mg, and separation and removal of metallic element impurities of sodium and potassium and non-metallic element impurities of chlorine, silicon and arsenic in the magnesium sulfate solution. Taking a saponified P507 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from a No. 1 outlet water phase of a NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 As a feed liquid, and taking a 4N grade magnesium sulfate solution obtained from a No. 1 outlet water phase of a Mg/CaPbAlFe fractionation extraction system in the step 3 As a detergent. The saponified P507 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from the aqueous phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters the NaK/Mg full-load fractionation extraction system from a feeding level, and a 4N-level magnesium sulfate solution obtained from the aqueous phase at the 1 st level outlet of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the last 1 level. Obtaining a mixture solution containing sodium, potassium, chlorine, silicon and arsenic from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a balanced load P507 organic phase of a feed grade of a NaK/Mg full-load fractional extraction system, and using the balanced load P507 organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; and obtaining a magnesium-loaded P507 organic phase from the last grade 1 outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the magnesium-loaded P507 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaPbAlFe
And 3, fractionating, extracting and separating Mg/CaPbAlFe to realize the separation of magnesium from calcium, lead, aluminum and iron. Taking a P507 organic phase loaded with magnesium obtained from the last level 1 of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the last level 1 of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 2.5mol/L sulfuric acid as a washing acid. The P507 organic phase loaded with magnesium and obtained from the last 1 level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaPbAlFe fractionation extraction system from the 1 st level, the P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron and obtained from the last 1 level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from a feeding level, and 2.5mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the last 1 level. Obtaining a target product 4N-grade magnesium sulfate solution from a1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 4N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a feed-grade equilibrium water phase of the Mg/CaPbAlFe fractional extraction system to be used as a detergent for separating NaKMg/MgCaPbAlFe by full-load fractional extraction in the step 1; and obtaining a P507 organic phase loaded with calcium, lead, aluminum and iron from the final level 1 outlet organic phase of the Mg/CaPbAlFe fractional extraction system, and recovering valuable elements after back extraction.
The P507 organic phase is a kerosene solution of P507 and sec-octanol, wherein the concentration of the P507 is 1.0mol/L, and the concentration of the sec-octanol is 0.05 mol/L. When used, the P507 organic phase is saponified by sodium saponification to obtain a saponified P507 organic phase.
The magnesium-containing brine comprises the following relevant elements in concentration: cl 10.0-50.0 g/L, Si 0.010.010-0.030 g/L, As 0.010-0.030 g/L, Na 10.0.0-30.0 g/L, K0.10.10-0.50 g/L, Mg20.0-40.0 g/L, Ca 0.10.10-0.50 g/L-0.50 g/L, Pb 0.010.010-0.030 g/L, Al 0.10.10 g/L-0.50 g/L, Fe 0.010-0.030 g/L.
The concentration of related elements in the 4N-grade magnesium sulfate solution is respectively as follows: cl 0.00010 g/L-0.00050 g/L, Si 0.00010.00010 g/L-0.00030 g/L, As 0.00010.00010 g/L-0.00030 g/L, Na 0.00010.00010 g/L-0.00070 g/L, K0.00010.00010 g/L-0.00050 g/L, Mg 58.0.0 g/L-62.0 g/L, Ca 0.0010.0010 g/L-0.0050 g/L, Pb0.00010g/L-0.00030 g/L, Al0.10g/L-0.00030 g/L, Fe 0.00010 g/8583.00010 g/L-0.00030 g/L.
The invention has the beneficial effects that: 1) directly obtaining 4N grade magnesium sulfate solution from magnesium-containing brine. After the 4N-grade magnesium sulfate solution is subjected to post-treatment such as concentration crystallization or precipitation, a series of 4N-grade magnesium-containing compounds such as 4N-grade magnesium sulfate crystals and 4N-grade magnesium phosphate crystals can be obtained. 2) The product purity is high, and the yield of magnesium is high: the purity of the 4N-grade magnesium sulfate solution of the target product is 99.991-99.997%, and the yield of magnesium is 96-98%. 3) Zero reagent consumption is less: the outlet organic phase which is fully loaded with NaK/Mg and separated by fractional extraction is used as an extraction organic phase for separating Mg/CaPbAlFe by fractional extraction, and directly enters the 1 st stage of separating Mg/CaPbAlFe by fractional extraction, so that saponified alkali for separating Mg/CaPbAlFe by fractional extraction is saved. The water phase at the 1 st level outlet for separating Mg/CaPbAlFe by fractional extraction is used as a detergent for separating NaK/Mg by full-load fractional extraction, so that the washing acid for separating NaK/Mg by full-load fractional extraction is saved. 4) The separation efficiency is high: and 3 separation sections (full-load fractionation extraction separation NaKMg/MgCaPbAlFe, full-load fractionation extraction separation NaK/Mg, fractionation extraction separation Mg/CaPbAlFe) separate and remove metal impurities such as sodium, potassium, calcium, lead, aluminum, iron and the like in the magnesium-containing brine and non-metal impurities such as chlorine, silicon, arsenic and the like. 5) The process flow is short: the process for directly preparing 4N-grade magnesium sulfate from magnesium-containing brine consists of 3 separation sections. The method is characterized in that NaKMg/MgCaPbAlFe is separated by full-load fractionation and extraction, and a balanced load P507 organic phase obtained by full-load fractionation, extraction and separation of NaK/Mg feeding grade is used as an extraction organic phase, so that a saponification section is not needed for full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe; the equilibrium water phase obtained by fractionating, extracting and separating the Mg/CaPbAlFe feeding grade is a detergent, so that a stripping section is not needed for fully loading, fractionating, extracting and separating NaKMg/MgCaPbAlFe. The NaKMg/MgCaPbAlFe full-load fractional extraction separation and the NaK/Mg full-load fractional extraction separation share a saponification section. The outlet organic phase loaded with NaK/Mg separated by fractional extraction is used as the extraction organic phase for separating Mg/CaPbAlFe by fractional extraction, so that the saponification section is not needed for separating Mg/CaPbAlFe by fractional extraction. The outlet organic phase of the full-load fractional extraction for separating the NaK/Mg is used as an extraction organic phase of the fractional extraction for separating the Mg/CaPbAlFe, so that a back-extraction section is not needed for separating the NaK/Mg by the full-load fractional extraction. 6) The production cost is low: high separation efficiency, short process flow and less reagent consumption.
Drawings
FIG. 1: the invention discloses a process flow schematic diagram of a method for preparing 4N-grade magnesium sulfate. In FIG. 1, LOP denotes the loaded organic phase; w represents a detergent; 4N Mg represents a 4N grade magnesium sulfate solution.
Detailed Description
A process for preparing 4N grade magnesium sulfate according to the present invention is further described below with reference to specific examples.
Example 1
The P507 organic phase is a kerosene solution of P507 and sec-octanol, wherein the concentration of P507 is 1.0mol/L, and the concentration of sec-octanol is 0.05 mol/L. When used, the P507 organic phase is saponified by sodium saponification to obtain a saponified P507 organic phase.
The concentration of relevant elements of the magnesium-containing brine is respectively as follows: cl 10.0g/L, Si 0.010.010 g/L, As 0.010.010 g/L, Na10.0g/L, K0.10 g/L, Mg 20.0.0 g/L, Ca 0.10.10 g/L, Pb 0.010.010 g/L and Al0.10g/L, Fe 0.010.010 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking a balanced load P507 organic phase obtained from the 10 th level of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking magnesium-containing brine as a feed liquid, and taking a balanced water phase obtained from the 22 nd level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P507 organic phase obtained from the 10 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the magnesium-containing brine enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 8 th stage, and the equilibrium aqueous phase obtained from the 22 nd stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 32 th stage. Obtaining a magnesium sulfate solution containing Na, K, Cl, Si and As from the water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the magnesium sulfate solution As a feed liquid for full-load fractional extraction and separation of NaK/Mg in the step 2; and (3) obtaining a P507 organic phase loaded with Mg-Ca-Pb-Al-Fe from a 32-stage outlet organic phase of a NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P507 organic phase as feed liquid for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
Taking a saponified P507 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from a No. 1 outlet water phase of a NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 As a feed liquid, and taking a 4N grade magnesium sulfate solution obtained from a No. 1 outlet water phase of a Mg/CaPbAlFe fractionation extraction system in the step 3 As a detergent. The saponified P507 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from the aqueous phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters a NaK/Mg full-load fractionation extraction system from the 10 th level, and a 4N-level magnesium sulfate solution obtained from the aqueous phase at the 1 st level outlet of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 24 th level. Obtaining a mixture solution containing sodium, potassium, chlorine, silicon and arsenic from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a10 th-level equilibrium load P507 organic phase of a NaK/Mg full-load fractional extraction system, and using the organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; and obtaining a magnesium-loaded P507 organic phase from a 24 th grade outlet organic phase of a NaK/Mg full-loaded fractional extraction system, and using the magnesium-loaded P507 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaPbAlFe
Taking a P507 organic phase loaded with magnesium obtained from the 24 th level of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 32 th level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 2.5mol/L sulfuric acid as a washing acid. The P507 organic phase loaded with magnesium and obtained from the 24 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaPbAlFe fractionation extraction system from the 1 st level, the P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron and obtained from the 32 th level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from the 22 th level, and 2.5mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the 38 th level. Obtaining a target product 4N-grade magnesium sulfate solution from a1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 4N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a 22 th-grade equilibrium water phase of the Mg/CaPbAlFe fractional extraction system, and using the 22 th-grade equilibrium water phase as a detergent for separating NaKMg/MgCaPbAlFe through full-load fractional extraction in the step 1; and obtaining a P507 organic phase loaded with calcium, lead, aluminum and iron from a 38 th-level outlet organic phase of a Mg/CaPbAlFe fractional extraction system, and recovering valuable elements after back extraction.
The concentrations of relevant elements in the 4N-grade magnesium sulfate solution are respectively as follows: cl 0.00010g/L, Si 0.00010.00010 g/L, As0.00010g/L, Na 0.00010.00010 g/L, K0.00010.00010 g/L, Mg 58.0.0 g/L, Ca 0.0010.0010 g/L, Pb 0.00010.00010 g/L, Al 0.00010.00010 g/L, Fe 0.00010 g/L. The purity of the magnesium sulfate solution was 99.998%, and the yield of magnesium was 96%.
Example 2
The P507 organic phase is a kerosene solution of P507 and sec-octanol, wherein the concentration of P507 is 1.0mol/L, and the concentration of sec-octanol is 0.05 mol/L. When used, the P507 organic phase is saponified by sodium saponification to obtain a saponified P507 organic phase.
The concentration of relevant elements of the magnesium-containing brine is respectively as follows: cl 30.0g/L, Si 0.020.020 g/L, As 0.020g/L, Na20.0g/L, K0.30 g/L, Mg 30.0.0 g/L, Ca 0.30.30 g/L, Pb 0.020.020 g/L, Al 0.30g/L, Fe 0.020 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking a balanced load P507 organic phase obtained from the 10 th level of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking magnesium-containing brine as a feed liquid, and taking a balanced water phase obtained from the 18 th level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P507 organic phase obtained from the 10 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the magnesium-containing brine enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 10 th stage, and the equilibrium aqueous phase obtained from the 22 nd stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 32 th stage. Obtaining a magnesium sulfate solution containing Na, K, Cl, Si and As from the water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the magnesium sulfate solution As a feed liquid for full-load fractional extraction and separation of NaK/Mg in the step 2; and (3) obtaining a P507 organic phase loaded with Mg-Ca-Pb-Al-Fe from a 32-stage outlet organic phase of a NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P507 organic phase as feed liquid for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
Taking a saponified P507 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from a No. 1 outlet water phase of a NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 As a feed liquid, and taking a 4N grade magnesium sulfate solution obtained from a No. 1 outlet water phase of a Mg/CaPbAlFe fractionation extraction system in the step 3 As a detergent. The saponified P507 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from the aqueous phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters a NaK/Mg full-load fractionation extraction system from the 10 th level, and a 4N-level magnesium sulfate solution obtained from the aqueous phase at the 1 st level outlet of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 24 th level. Obtaining a mixture solution containing sodium, potassium, chlorine, silicon and arsenic from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a10 th-level equilibrium load P507 organic phase of a NaK/Mg full-load fractional extraction system, and using the organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; and obtaining a magnesium-loaded P507 organic phase from a 24 th grade outlet organic phase of a NaK/Mg full-loaded fractional extraction system, and using the magnesium-loaded P507 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaPbAlFe
Taking a P507 organic phase loaded with magnesium obtained from the 24 th level of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 32 th level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 2.5mol/L sulfuric acid as a washing acid. The P507 organic phase loaded with magnesium and obtained from the 24 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaPbAlFe fractionation extraction system from the 1 st level, the P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron and obtained from the 32 nd level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from the 18 th level, and 2.5mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the 32 nd level. Obtaining a target product 4N-grade magnesium sulfate solution from a1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 4N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating the 18 th-grade equilibrium water phase of the Mg/CaPbAlFe fractional extraction system, and using the balance water phase as a detergent for separating NaKMg/MgCaPbAlFe through full-load fractional extraction in the step 1; and obtaining a P507 organic phase loaded with calcium, lead, aluminum and iron from a 32 th-level outlet organic phase of a Mg/CaPbAlFe fractional extraction system, and recovering valuable elements after back extraction.
The concentrations of relevant elements in the 4N-grade magnesium sulfate solution are respectively as follows: cl 0.00030g/L, Si 0.00020.00020 g/L, As0.00020g/L, Na 0.00040.00040 g/L, K0.00030.00030 g/L, Mg 60.0.0 g/L, Ca 0.0030.0030 g/L, Pb 0.00020.00020 g/L, Al 0.00020.00020 g/L, Fe 0.00020 g/L. The purity of the magnesium sulfate solution was 99.994%, and the yield of magnesium was 97%.
Example 3
The P507 organic phase is a kerosene solution of P507 and sec-octanol, wherein the concentration of P507 is 1.0mol/L, and the concentration of sec-octanol is 0.05 mol/L. When used, the P507 organic phase is saponified by sodium saponification to obtain a saponified P507 organic phase.
The concentration of relevant elements of the magnesium-containing brine is respectively as follows: cl 50.0g/L, Si 0.030.030 g/L, As 0.030g/L, Na30.0g/L, K0.50 g/L, Mg 40.0.0 g/L, Ca 0.50.50 g/L, Pb 0.030.030 g/L, Al 0.50g/L, Fe 0.030 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking a balanced load P507 organic phase obtained from the 12 th level of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking magnesium-containing brine as a feed liquid, and taking a balanced water phase obtained from the 16 th level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P507 organic phase obtained from the 12 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the magnesium-containing brine enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 10 th stage, and the equilibrium aqueous phase obtained from the 22 th stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 30 th stage. Obtaining a magnesium sulfate solution containing Na, K, Cl, Si and As from the water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the magnesium sulfate solution As a feed liquid for full-load fractional extraction and separation of NaK/Mg in the step 2; and (3) obtaining a P507 organic phase loaded with Mg-Ca-Pb-Al-Fe from a30 th grade outlet organic phase of a NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P507 organic phase as feed liquid for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
Taking a saponified P507 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from a No. 1 outlet water phase of a NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 As a feed liquid, and taking a 4N grade magnesium sulfate solution obtained from a No. 1 outlet water phase of a Mg/CaPbAlFe fractionation extraction system in the step 3 As a detergent. The saponified P507 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from the aqueous phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters a NaK/Mg full-load fractionation extraction system from the 12 th level, and a 4N-level magnesium sulfate solution obtained from the aqueous phase at the 1 st level outlet of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 26 th level. Obtaining a mixture solution containing sodium, potassium, chlorine, silicon and arsenic from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a 12 th-level equilibrium load P507 organic phase of a NaK/Mg full-load fractional extraction system, and using the organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; and obtaining a P507 organic phase loaded with magnesium from the 26 th grade outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the P507 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaPbAlFe
Taking a P507 organic phase loaded with magnesium obtained from the 26 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 30 th stage of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 2.5mol/L sulfuric acid as a washing acid. The P507 organic phase loaded with magnesium and obtained from the 26 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaPbAlFe fractionation extraction system from the 1 st level, the P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron and obtained from the 32 th level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from the 16 th level, and 2.5mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the 28 th level. Obtaining a target product 4N-grade magnesium sulfate solution from a1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 4N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a 16 th-grade equilibrium water phase of the Mg/CaPbAlFe fractional extraction system, and using the 16 th-grade equilibrium water phase as a detergent for separating NaKMg/MgCaPbAlFe through full-load fractional extraction in the step 1; and obtaining a P507 organic phase loaded with calcium, lead, aluminum and iron from a 28 th-level outlet organic phase of a Mg/CaPbAlFe fractional extraction system, and recovering valuable elements after back extraction.
The concentrations of relevant elements in the 4N-grade magnesium sulfate solution are respectively as follows: cl 0.00050g/L, Si 0.00030.00030 g/L, As0.00030g/L, Na 0.00070.00070 g/L, K0.00050.00050 g/L, Mg 62.0.0 g/L, Ca 0.0050.0050 g/L, Pb 0.00030.00030 g/L, Al 0.00030.00030 g/L, Fe 0.00030.00030 g/L. The purity of the magnesium sulfate solution was 99.991%, and the yield of magnesium was 98%.
Claims (4)
1. A method for preparing 4N-grade magnesium sulfate is characterized by comprising the following steps: the method takes magnesium-containing brine as a feed liquid, P507 as an extracting agent and octanol as a modifying agent, separates and removes metallic elements of sodium, potassium, calcium, lead, aluminum and iron in the feed liquid, and non-metallic elements of chlorine, silicon and arsenic, and directly prepares a 4N-grade magnesium sulfate solution; consists of 3 steps, namely full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe, full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaPbAlFe; the extraction section of full-load fractionation, extraction and separation NaKMg/MgCaPbAlFe realizes the separation of NaKMg/CaPbAlFe, and the washing section realizes the separation of NaK/MgCaPbAlFe; full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe, full-load fractionation, extraction and separation of NaK/Mg, a balanced load P507 organic phase obtained at a feed level is used as an extraction organic phase, and a balanced water phase obtained at a feed level is used as a detergent; full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaPbAlFe are directly connected in series; the outlet organic phase which is fully loaded with NaK/Mg and separated by fractional extraction is used as an extraction organic phase for separating Mg/CaPbAlFe by fractional extraction, and directly enters the 1 st stage for separating Mg/CaPbAlFe by fractional extraction; the 1 st level outlet water phase of the Mg/CaPbAlFe separation by fractional extraction is used as a detergent for separating NaK/Mg by full-load fractional extraction;
the 3 steps are as follows:
step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
Step 1, full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe, wherein the extraction section realizes the separation of NaKMg/CaPbAlFe, and the washing section realizes the separation of NaK/MgCaPbAlFe; taking a balanced load P507 organic phase obtained from the feed stage of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking magnesium-containing brine as a feed liquid, and taking a balanced water phase obtained from the feed stage of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent; the equilibrium loaded P507 organic phase obtained from the feed stage of the NaK/Mg full-load fractional extraction system in the step 2 enters a NaKMg/MgCaPbAlFe full-load fractional extraction system from the 1 st stage, magnesium-containing brine enters the NaKMg/MgCaPbAlFe full-load fractional extraction system from the feed stage, and the equilibrium aqueous phase obtained from the feed stage of the Mg/CaPbAlFe fractional extraction system in the step 3 enters the NaKMg/MgCaPbAlFe full-load fractional extraction system from the last 1 st stage; obtaining a magnesium sulfate solution containing Na, K, Cl, Si and As from the water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the magnesium sulfate solution As a feed liquid for full-load fractional extraction and separation of NaK/Mg in the step 2; obtaining a P507 organic phase loaded with Mg-Ca-Pb-Al-Fe from the last 1-level outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P507 organic phase as feed liquid for fractional extraction and separation of Mg/CaPbAlFe in the step 3;
step 2: full-load fractional extraction for separating NaK/Mg
Step 2, full-load fractionation, extraction and separation of NaK/Mg are carried out, and metal element impurities of sodium and potassium and non-metal element impurities of chlorine, silicon and arsenic in the magnesium sulfate solution are removed through separation; taking a saponified P507 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained from a No. 1 outlet water phase of a NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 As a feed liquid, and taking a 4N grade magnesium sulfate solution obtained from a No. 1 outlet water phase of a Mg/CaPbAlFe fractionation extraction system in the step 3 As a detergent; the saponified P507 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium sulfate solution containing Na, K, Cl, Si and As, which is obtained from a water phase at the 1 st level outlet of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1, enters a NaK/Mg full-load fractionation extraction system from a feeding level, and a 4N-level magnesium sulfate solution obtained from a water phase at the 1 st level outlet of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the last 1 level; obtaining a mixture solution containing sodium, potassium, chlorine, silicon and arsenic from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a balanced load P507 organic phase of a feed grade of a NaK/Mg full-load fractional extraction system, and using the balanced load P507 organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; obtaining a P507 organic phase loaded with magnesium from the last level 1 outlet organic phase of the NaK/Mg full-load fractionation extraction system, and using the P507 organic phase as an extraction organic phase for fractionating, extracting and separating Mg/CaPbAlFe in the step 3;
and step 3: fractionation, extraction and separation of Mg/CaPbAlFe
Step 3, fractionating, extracting and separating Mg/CaPbAlFe to realize the separation of magnesium from calcium, lead, aluminum and iron; taking a P507 organic phase loaded with magnesium obtained from the last level 1 of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the last level 1 of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 2.5mol/L sulfuric acid as a washing acid; the P507 organic phase loaded with magnesium and obtained from the last 1 level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaPbAlFe fractionation extraction system from the 1 st level, the P507 organic phase loaded with magnesium, calcium, lead, aluminum and iron and obtained from the last 1 level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from a feeding level, and 2.5mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the last 1 level; obtaining a target product 4N-grade magnesium sulfate solution from a1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 4N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a feed-grade equilibrium water phase of the Mg/CaPbAlFe fractional extraction system to be used as a detergent for separating NaKMg/MgCaPbAlFe by full-load fractional extraction in the step 1; and obtaining a P507 organic phase loaded with calcium, lead, aluminum and iron from the final level 1 outlet organic phase of the Mg/CaPbAlFe fractional extraction system, and recovering valuable elements after back extraction.
2. The method of claim 1, wherein the method comprises the following steps: the P507 organic phase is a kerosene solution of P507 and sec-octanol, wherein the concentration of P507 is 1.0mol/L, and the concentration of sec-octanol is 0.05 mol/L; when used, the P507 organic phase is saponified by sodium saponification to obtain a saponified P507 organic phase.
3. The method of claim 1, wherein the method comprises the following steps: the magnesium-containing brine comprises the following relevant elements in concentration: cl 10.0 g/L-50.0 g/L, Si 0.010 g/L-0.030 g/L, As 0.010 g/L-0.030 g/L, Na 10.0.0 g/L-30.0 g/L, K0.10.10 g/L-0.50 g/L, Mg 20.0.0 g/L-40.0 g/L, Ca 0.10.10 g/L-0.50 g/L, Pb 0.010 g/L-0.030 g/L, Al 0.10.10 g/L-0.50 g/L, Fe 0.010.010 g/L-0.030 g/L.
4. The method of claim 1, wherein the method comprises the following steps: the concentration of related elements in the 4N-grade magnesium sulfate solution is respectively as follows: cl 0.00010 g/L-0.00050 g/L, Si 0.00010.00010 g/L-0.00030 g/L, As 0.00010.00010 g/L-0.00030 g/L, Na 0.00010.00010 g/L-0.00070 g/L, K0.00010.00010 g/L-0.00050 g/L, Mg 58.0.0 g/L-62.0 g/L, Ca 0.0010.0010 g/L-0.0050 g/L, Pb 0.00010.00010 g/L-0.00030 g/L and Al0.00010g/L-0.00030 g/L, Fe 0.00010 g/L-0.00030 g/L.
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| CN106916947A (en) * | 2017-03-28 | 2017-07-04 | 南昌航空大学 | The method that quasi- fractional extraction separates sodium and potassium in lithium sulfate |
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