CN110668479B - Method for preparing 5N-grade magnesium sulfate solution - Google Patents
Method for preparing 5N-grade magnesium sulfate solution Download PDFInfo
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- CN110668479B CN110668479B CN201911097752.3A CN201911097752A CN110668479B CN 110668479 B CN110668479 B CN 110668479B CN 201911097752 A CN201911097752 A CN 201911097752A CN 110668479 B CN110668479 B CN 110668479B
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- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 title claims abstract description 216
- 229910052943 magnesium sulfate Inorganic materials 0.000 title claims abstract description 108
- 235000019341 magnesium sulphate Nutrition 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000000605 extraction Methods 0.000 claims abstract description 285
- 239000011777 magnesium Substances 0.000 claims abstract description 219
- 239000000243 solution Substances 0.000 claims abstract description 86
- 238000000926 separation method Methods 0.000 claims abstract description 78
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000011734 sodium Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 35
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 33
- 239000011575 calcium Substances 0.000 claims abstract description 29
- 239000011133 lead Substances 0.000 claims abstract description 29
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 28
- 239000000460 chlorine Substances 0.000 claims abstract description 28
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 28
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 28
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 28
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 19
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 13
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000011591 potassium Substances 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000012074 organic phase Substances 0.000 claims description 152
- 238000005194 fractionation Methods 0.000 claims description 129
- 239000012071 phase Substances 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000003599 detergent Substances 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- 239000008346 aqueous phase Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 11
- 238000007127 saponification reaction Methods 0.000 claims description 8
- 229910018084 Al-Fe Inorganic materials 0.000 claims description 5
- 229910018192 Al—Fe Inorganic materials 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 239000003350 kerosene Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- -1 magnesium-calcium-lead-aluminum-iron Chemical compound 0.000 description 4
- 239000013078 crystal Substances 0.000 description 2
- HZIUHEQKVCPTAJ-UHFFFAOYSA-N 3-(2-ethylhexoxyphosphonoyloxymethyl)heptane Chemical compound CCCCC(CC)COP(=O)OCC(CC)CCCC HZIUHEQKVCPTAJ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a method for preparing 5N-grade magnesium sulfate solution, which takes industrial-grade magnesium sulfate aqueous solution as feed liquid and P229 as an extracting agent and consists of three steps of full-load fractional extraction separation of NaKMg/MgCaPbAlFe, full-load fractional extraction separation of NaK/Mg and fractional extraction separation of Mg/CaPbAlFe; separating and removing metallic element impurities such as sodium, potassium, calcium, lead, aluminum and iron in the feed liquid, and separating and removing nonmetallic element impurities such as chlorine, silicon and arsenic to prepare a 5N-grade magnesium sulfate solution; the purity of the target product 5N grade magnesium sulfate solution is 99.9991% -99.9997%, and the yield of magnesium in the industrial grade magnesium sulfate solution 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 a 5N-grade magnesium sulfate solution, in particular to a method for preparing a 5N-grade magnesium sulfate solution by taking an industrial-grade magnesium sulfate aqueous solution as a feed liquid and P229 as an extracting agent, separating and removing metal elements such as sodium, potassium, calcium, lead, aluminum, iron and the like in the feed liquid and separating and removing non-metal elements such as chlorine, silicon, arsenic and the like. The invention belongs to the technical field of preparation of 5N-grade magnesium sulfate.
Background
The grade 5N magnesium sulfate is one of basic raw materials for preparing other grade 5N magnesium products, but no method for preparing the grade 5N magnesium sulfate exists at present.
The invention aims at the method for preparing 5N-grade magnesium sulfate which is not available at present, and establishes a method for preparing 5N-grade magnesium sulfate solution by taking industrial-grade magnesium sulfate aqueous solution as feed liquid. The main impurities in the industrial grade magnesium sulfate comprise metallic element impurities such as sodium, potassium, calcium, lead, aluminum, iron and the like, and non-metallic element impurities such as chlorine, silicon, arsenic and the like.
Disclosure of Invention
The invention aims at the method for preparing 5N-grade magnesium sulfate which is not available at present, and establishes a method for preparing 5N-grade magnesium sulfate solution by taking industrial-grade magnesium sulfate aqueous solution as feed liquid.
The invention discloses a method for preparing a 5N-grade magnesium sulfate solution, which takes an industrial-grade magnesium sulfate aqueous solution as a feed liquid and di (2-ethylhexyl) phosphonic acid (P229 for short) as an extracting 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 to prepare the 5N-grade magnesium sulfate solution.
The invention relates to a method for preparing 5N-grade magnesium sulfate solution, which comprises 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 P229 organic phase obtained by a NaK/Mg feeding level separated by full-load fractionation extraction is used as an extraction organic phase, and a balanced aqueous phase obtained by a Mg/CaPbAlFe feeding level separated 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 the 5N-grade magnesium sulfate solution 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 P229 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, an industrial-grade magnesium sulfate aqueous solution 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 P229 organic phase obtained from the feed stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the industrial grade magnesium sulfate aqueous solution enters the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the feed stage, and the equilibrium aqueous phase obtained from the feed stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters the NaKMg/MgCaPbAlFe full-load fractionation 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 P229 organic phase loaded with Mg-Ca-Pb-Al-Fe from the last grade 1 outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P229 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. An ammonia saponification P229 organic phase is used As an extraction organic phase, a magnesium sulfate solution containing Na, K, Cl, Si and As, which is obtained by full-load NaKMg/MgCaPbAlFe full-load fractionation of an extraction system at the 1 st-stage outlet water phase in the step 1, is used As a feed liquid, and a 5N-stage magnesium sulfate solution which is obtained by the Mg/CaPbAlFe fractionation of the extraction system at the 1 st-stage outlet water phase in the step 3 is used As a detergent. The saponified P229 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 5N-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 P229 organic phase of a feed grade of a NaK/Mg full-load fractional extraction system, and using the balanced load P229 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 P229 organic phase from the last grade 1 outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the magnesium-loaded P229 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 P229 organic phase loaded with magnesium obtained from the last stage 1 of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P229 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the last stage 1 of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 3.0mol/L sulfuric acid as a washing acid. The magnesium-loaded P229 organic phase obtained from the last stage 1 of the NaK/Mg full-load fractionation extraction system in the step 2 enters the Mg/CaPbAlFe fractionation extraction system from the stage 1, the magnesium-calcium-lead-aluminum-iron-loaded P229 organic phase obtained from the last stage 1 of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters the Mg/CaPbAlFe fractionation extraction system from the feeding stage, and 3.0mol/L of sulfuric acid washing acid enters the Mg/CaPbAlFe fractionation extraction system from the last stage 1. Obtaining a target product 5N-grade magnesium sulfate solution from a 1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 5N-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 P229 organic phase loaded with calcium, lead, aluminum and iron from the organic phase at the last stage 1 outlet of the Mg/CaPbAlFe fractional extraction system.
The P229 organic phase is a sulfonated kerosene solution of P229, wherein the concentration of P229 is 1.0 mol/L. When used, the P229 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed P229 organic phase.
The element concentrations in the industrial-grade magnesium sulfate aqueous solution are respectively as follows: cl 1.0-3.0 g/L, Si 0.0010.0010 g/L-0.0030 g/L, As 0.00010.00010 g/L-0.00030 g/L, Na 0.010.010 g/L-0.030 g/L, K0.010.010 g/L-0.030 g/L, Mg 65.0.0 g/L-75.0 g/L, Ca 0.010.010 g/L-0.050 g/L, Pb 0.0010.0010 g/L-0.0030 g/L, Al 0.0010.0010 g/L-0.0030 g/L, Fe 0.0010.0010 g/L-0.0050 g/L.
The element concentrations in the 5N-grade magnesium sulfate solution are respectively as follows: cl 0.00010 g/L-0.00030 g/L, Si 0.000010.000010 g/L-0.000030 g/L, As 0.000010 g/L-0.000030 g/L, Na 0.000010.000010 g/L-0.000030 g/L, K0.000010.000010 g/L-0.000030 g/L, Mg 68.0.0 g/L-72.0 g/L, Ca 0.00010.00010 g/L-0.00050 g/L, Pb 0.000010.000010 g/L-0.000030 g/L, Al 0.000010.000010 g/L-0.000030 g/L, Fe 0.000010.000010 g/L-0.000030 g/L.
The invention has the beneficial effects that: 1) the 5N grade magnesium sulfate solution is directly obtained from the industrial grade magnesium sulfate aqueous solution. After the 5N-grade magnesium sulfate solution is subjected to post-treatment such as concentration crystallization or precipitation, a series of 5N-grade magnesium-containing compounds such as 5N-grade magnesium sulfate crystals and 5N-grade magnesium phosphate crystals can be obtained. 2) The product purity is high, and the yield of magnesium is high: the purity of the target product 5N grade magnesium sulfate solution is 99.9991% -99.9997%, and the yield of magnesium in the industrial grade magnesium sulfate solution is 96% -98%. 3) The 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 and non-metal impurities such as chlorine, silicon, arsenic and the like in the industrial-grade magnesium sulfate aqueous solution. 5) The process flow is short: the process for the preparation of 5N grade magnesium sulfate from technical grade aqueous magnesium sulfate solution consists of 3 separation stages. The method is characterized in that NaKMg/MgCaPbAlFe is separated by full-load fractionation and extraction, and a balanced load P229 organic phase obtained by full-load fractionation and extraction 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 and extraction separation of NaKMg/MgCaPbAlFe; the equilibrium water phase obtained by fractionating, extracting and separating Mg/CaPbAlFe feeding grade is used as a detergent, so that a stripping section is not needed for full-load fractionation, extraction and separation of 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 5N-grade magnesium sulfate solution. In FIG. 1, LOP denotes the loaded organic phase; w represents a detergent; 5N Mg represents a 5N grade magnesium sulfate solution.
Detailed Description
A method of preparing a 5N grade magnesium sulfate solution according to the present invention is further described below with reference to specific examples.
Example 1
The P229 organic phase is a sulfonated kerosene solution of P229, wherein the concentration of P229 is 1.0 mol/L. When used, the P229 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed P229 organic phase.
The element concentrations in the industrial-grade magnesium sulfate aqueous solution are respectively as follows: cl 1.0g/L, Si 0.0010.0010 g/L, As 0.00010.00010 g/L, Na 0.010g/L, K0.010.010 g/L, Mg 65.0.0 g/L, Ca 0.010.010 g/L, Pb 0.0010.0010 g/L, Al 0.0010g/L, Fe 0.0010.0010 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking the equilibrium loaded P229 organic phase obtained from the 32 th level of the NaK/Mg full-loaded fractional extraction system in the step 2 as an extraction organic phase, taking an industrial-grade magnesium sulfate aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 30 th level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P229 organic phase obtained from the 32 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 industrial grade magnesium sulfate aqueous solution enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 12 th stage, and the equilibrium aqueous phase obtained from the 30 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 26 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 P229 organic phase loaded with Mg-Ca-Pb-Al-Fe from the 26 th grade outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P229 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
An ammonia saponification P229 organic phase is used As an extraction organic phase, a magnesium sulfate solution containing Na, K, Cl, Si and As, which is obtained by full-load NaKMg/MgCaPbAlFe full-load fractionation of an extraction system at the 1 st-stage outlet water phase in the step 1, is used As a feed liquid, and a 5N-stage magnesium sulfate solution which is obtained by the Mg/CaPbAlFe fractionation of the extraction system at the 1 st-stage outlet water phase in the step 3 is used As a detergent. The saponified P229 organic phase is an extracted organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, 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 is fed into the NaK/Mg full-load fractionation extraction system from the 32 nd level, and 5N grade 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 is fed into the NaK/Mg full-load fractionation extraction system from the 62 nd 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 32 th-level equilibrium load P229 organic phase of a NaK/Mg full-load fractional extraction system, and using the organic phase as an extraction organic phase for separating NaKMg/MgCaPbAlFe by full-load fractional extraction in the step 1; and obtaining a P229 organic phase loaded with magnesium from the 62 nd stage outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the P229 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 P229 organic phase loaded with magnesium obtained from the 62 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P229 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 26 th stage of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 3.0mol/L sulfuric acid as a washing acid. The magnesium-loaded P229 organic phase obtained from the 62 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters the Mg/CaPbAlFe fractionation extraction system from the 1 st level, the magnesium-calcium-lead-aluminum-iron-loaded P229 organic phase obtained from the 26 th level of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters the Mg/CaPbAlFe fractionation extraction system from the 30 th level, and 3.0mol/L sulfuric acid washing acid enters the Mg/CaPbAlFe fractionation extraction system from the 60 th level. Obtaining a target product 5N-grade magnesium sulfate solution from a 1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 5N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a 30 th-grade equilibrium water phase of a Mg/CaPbAlFe fractional extraction system, and using the 30 th-grade equilibrium water phase as a detergent for separating NaKMg/MgCaPbAlFe through full-load fractional extraction in the step 1; and obtaining a P229 organic phase loaded with calcium, lead, aluminum and iron from the 60 th stage outlet organic phase of the Mg/CaPbAlFe fractional extraction system.
The element concentrations in the 5N-grade magnesium sulfate solution are respectively as follows: cl 0.00010g/L, Si 0.000010.000010 g/L, As 0.000010g/L, Na 0.000010g/L, K0.000010 g/L, Mg 68.0.0 g/L, Ca 0.00010g/L, Pb 0.000010g/L, Al 0.000010g/L, Fe 0.000010.000010 g/L. The purity of the magnesium sulfate solution was 99.9997%, and the yield of magnesium was 96%.
Example 2
The P229 organic phase is a sulfonated kerosene solution of P229, wherein the concentration of P229 is 1.0 mol/L. When used, the P229 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed P229 organic phase.
The element concentrations in the industrial-grade magnesium sulfate aqueous solution are respectively as follows: cl 2.0g/L, Si 0.0020.0020 g/L, As 0.00020.00020 g/L, Na 0.020g/L, K0.020.020 g/L, Mg 70.0.0 g/L, Ca 0.030.030 g/L, Pb 0.0020.0020 g/L, Al 0.0020g/L, Fe 0.0020.0020 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking the equilibrium loaded P229 organic phase obtained from the 28 th level of the NaK/Mg full-loaded fractional extraction system in the step 2 as an extraction organic phase, taking an industrial-grade magnesium sulfate aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 36 th level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P229 organic phase obtained from the 28 th stage of the NaK/Mg full-load fractionation extraction system of the step 2 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the industrial grade magnesium sulfate aqueous solution enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 26 th stage, and the equilibrium aqueous phase obtained from the 36 th stage of the Mg/CaPbAlFe fractionation extraction system of 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 P229 organic phase loaded with Mg-Ca-Pb-Al-Fe from the 32 th-stage outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P229 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
An ammonia saponification P229 organic phase is used As an extraction organic phase, a magnesium sulfate solution containing Na, K, Cl, Si and As, which is obtained by full-load NaKMg/MgCaPbAlFe full-load fractionation of an extraction system at the 1 st-stage outlet water phase in the step 1, is used As a feed liquid, and a 5N-stage magnesium sulfate solution which is obtained by the Mg/CaPbAlFe fractionation of the extraction system at the 1 st-stage outlet water phase in the step 3 is used As a detergent. The saponified P229 organic phase is an extracted 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 the 28 th level, and a 5N-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 60 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 28 th-level equilibrium load P229 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 P229 organic phase loaded with magnesium from the 60 th stage outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the P229 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 P229 organic phase loaded with magnesium obtained from the 60 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P229 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 32 nd stage of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 3.0mol/L sulfuric acid as a washing acid. The magnesium-loaded P229 organic phase obtained from the 60 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into the Mg/CaPbAlFe fractionation extraction system from the 1 st stage, the magnesium-calcium-lead-aluminum-iron-loaded P229 organic phase obtained from the 32 nd stage of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaPbAlFe fractionation extraction system from the 36 th stage, and 3.0mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the 64 th stage. Obtaining a target product 5N-grade magnesium sulfate solution from a 1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 5N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating the 36 th-level 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 P229 organic phase loaded with calcium, lead, aluminum and iron from a 64 th-stage outlet organic phase of the Mg/CaPbAlFe fractional extraction system.
The element concentrations in the 5N-grade magnesium sulfate solution are respectively as follows: cl 0.00020g/L, Si 0.000020.000020 g/L, As 0.000020g/L, Na 0.000020g/L, K0.000020 g/L, Mg 70.0.0 g/L, Ca 0.00030g/L, Pb 0.000020g/L, Al 0.000020g/L, Fe 0.000020.000020 g/L. The purity of the magnesium sulfate solution was 99.9994%, and the yield of magnesium was 97%.
Example 3
The P229 organic phase is a sulfonated kerosene solution of P229, wherein the concentration of P229 is 1.0 mol/L. When used, the P229 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed P229 organic phase.
The element concentrations in the industrial-grade magnesium sulfate aqueous solution are respectively as follows: cl 3.0g/L, Si 0.0030.0030 g/L, As 0.00030.00030 g/L, Na 0.030g/L, K0.030.030 g/L, Mg 75.0.0 g/L, Ca 0.050.050 g/L, Pb 0.0030.0030 g/L, Al 0.0030g/L, Fe 0.0050.0050 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaPbAlFe
And (3) taking the equilibrium loaded P229 organic phase obtained from the 28 th level of the NaK/Mg full-loaded fractional extraction system in the step 2 as an extraction organic phase, taking an industrial-grade magnesium sulfate aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 40 th level of the Mg/CaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded P229 organic phase obtained from the 28 th stage of the NaK/Mg full-load fractionation extraction system of the step 2 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 1 st stage, the industrial grade magnesium sulfate aqueous solution enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 18 th stage, and the equilibrium aqueous phase obtained from the 40 th stage of the Mg/CaPbAlFe fractionation extraction system of the step 3 enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the 34 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 P229 organic phase loaded with Mg-Ca-Pb-Al-Fe from the 34 th grade outlet organic phase of the NaKMg/MgCaPbAlFe full-load fractional extraction system, and using the P229 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
An ammonia saponification P229 organic phase is used As an extraction organic phase, a magnesium sulfate solution containing Na, K, Cl, Si and As, which is obtained by full-load NaKMg/MgCaPbAlFe full-load fractionation of an extraction system at the 1 st-stage outlet water phase in the step 1, is used As a feed liquid, and a 5N-stage magnesium sulfate solution which is obtained by the Mg/CaPbAlFe fractionation of the extraction system at the 1 st-stage outlet water phase in the step 3 is used As a detergent. The saponified P229 organic phase is an extracted organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, 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 is fed into the NaK/Mg full-load fractionation extraction system from the 28 th level, and 5N grade 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 is fed into the NaK/Mg full-load fractionation extraction system from the 62 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 28 th-level equilibrium load P229 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 P229 organic phase loaded with magnesium from the 62 nd stage outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the P229 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 P229 organic phase loaded with magnesium obtained from the 62 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a P229 organic phase loaded with magnesium, calcium, lead, aluminum and iron obtained from the 34 th stage of the NaKMg/MgCaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 3.0mol/L sulfuric acid as a washing acid. The magnesium-loaded P229 organic phase obtained from the 62 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into the Mg/CaPbAlFe fractionation extraction system from the 1 st level, the magnesium-calcium-lead-aluminum-iron-loaded P229 organic phase obtained from the 34 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 40 th level, and 3.0mol/L sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the 66 th level. Obtaining a target product 5N-grade magnesium sulfate solution from a 1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 5N-grade magnesium sulfate solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating the 40 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 P229 organic phase loaded with calcium, lead, aluminum and iron from a 66 th grade outlet organic phase of the Mg/CaPbAlFe fractional extraction system.
The element concentrations in the 5N-grade magnesium sulfate solution are respectively as follows: cl 0.00030g/L, Si 0.000030g/L, As 0.000030g/L, Na 0.000030g/L, K0.000030 g/L, Mg 72.0.0 g/L, Ca 0.00050.00050 g/L, Pb 0.000030g/L, Al 0.000030g/L, Fe 0.000030 g/L. The purity of the magnesium sulfate solution was 99.9991%, and the yield of magnesium was 98%.
Claims (4)
1. A method for preparing 5N-grade magnesium sulfate solution is characterized by comprising the following steps: the method takes industrial-grade magnesium sulfate aqueous solution as feed liquid and P229 as an extracting agent, separates and removes metallic element impurities of sodium, potassium, calcium, lead, aluminum and iron in the feed liquid, and separates and removes nonmetallic element impurities of chlorine, silicon and arsenic to prepare 5N-grade magnesium sulfate solution; comprises 3 steps, namely full-load fractionation extraction separation NaKMg/MgCaPbAlFe, full-load fractionation extraction separation NaK/Mg and fractionation 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; full-load fractionation, extraction and separation of NaKMg/MgCaPbAlFe, namely, a balanced load P229 organic phase obtained by full-load fractionation, extraction and separation of NaK/Mg feeding level is used as an extraction organic phase, and a balanced water phase obtained by fractionation, extraction and separation of Mg/CaPbAlFe feeding 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 P229 organic phase obtained from the feed stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, an industrial grade magnesium sulfate aqueous solution as a feed liquid, and a balanced water phase obtained from the feed stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 as a detergent; the equilibrium loaded P229 organic phase obtained from the feed 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 industrial grade magnesium sulfate aqueous solution enters into the NaKMg/MgCaPbAlFe full-load fractionation extraction system from the feed stage, and the equilibrium aqueous phase obtained from the feed stage of the Mg/CaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaPbAlFe full-load fractionation 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; obtaining a P229 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 P229 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 an ammonia saponification P229 organic phase As an extraction organic phase, taking a magnesium sulfate solution containing Na, K, Cl, Si and As obtained by full-load NaKMg/MgCaPbAlFe full-load fractionation extraction system 1 level outlet water phase in the step 1 As a feed liquid, and taking a 5N level magnesium sulfate solution obtained by Mg/CaPbAlFe fractionation extraction system 1 level outlet water phase in the step 3 As a detergent; the saponified P229 organic phase is an extracted 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 5N-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 P229 organic phase of a feed grade of a NaK/Mg full-load fractional extraction system, and using the balanced load P229 organic phase as an extraction organic phase for full-load fractional extraction separation of NaKMg/MgCaPbAlFe in the step 1; obtaining a P229 organic phase loaded with magnesium from the organic phase at the last level 1 outlet of the NaK/Mg full-load fractionation extraction system, and using the P229 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 P229 organic phase loaded with magnesium and 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 P229 organic phase loaded with magnesium, calcium, lead, aluminum and iron and 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 3.0mol/L sulfuric acid as a washing acid; the P229 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 P229 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 3.0mol/L of sulfuric acid washing acid enters into the Mg/CaPbAlFe fractionation extraction system from the last 1 level; obtaining a target product 5N-grade magnesium sulfate solution from a 1 st grade outlet water phase of the Mg/CaPbAlFe fractional extraction system, and taking the 5N-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 P229 organic phase loaded with calcium, lead, aluminum and iron from the organic phase at the last stage 1 outlet of the Mg/CaPbAlFe fractional extraction system.
2. A process for the preparation of a grade 5N magnesium sulfate solution as claimed in claim 1, wherein: the P229 organic phase is a sulfonated kerosene solution of P229, wherein the concentration of P229 is 1.0 mol/L; when used, the P229 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed P229 organic phase.
3. A process for the preparation of a grade 5N magnesium sulfate solution as claimed in claim 1, wherein: the element concentrations in the industrial-grade magnesium sulfate aqueous solution are respectively as follows: cl 1.0-3.0 g/L, Si 0.0010.0010 g/L-0.0030 g/L, As 0.00010.00010 g/L-0.00030 g/L, Na 0.010.010 g/L-0.030 g/L, K0.010.010 g/L-0.030 g/L, Mg 65.0.0 g/L-75.0 g/L, Ca 0.010.010 g/L-0.050 g/L, Pb 0.0010.0010 g/L-0.0030 g/L, Al 0.0010.0010 g/L-0.0030 g/L, Fe 0.0010.0010 g/L-0.0050 g/L.
4. A process for the preparation of a grade 5N magnesium sulfate solution as claimed in claim 1, wherein: the element concentrations in the 5N-grade magnesium sulfate solution are respectively as follows: cl 0.00010 g/L-0.00030 g/L, Si 0.000010.000010 g/L-0.000030 g/L, As 0.000010 g/L-0.000030 g/L, Na 0.000010.000010 g/L-0.000030 g/L, K0.000010.000010 g/L-0.000030 g/L, Mg 68.0.0 g/L-72.0 g/L, Ca 0.00010.00010 g/L-0.00050 g/L, Pb 0.000010.000010 g/L-0.000030 g/L, Al 0.000010.000010 g/L-0.000030 g/L, Fe 0.000010.000010 g/L-0.000030 g/L.
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