CN110642276B - Method for preparing 6N-grade magnesium chloride solution - Google Patents
Method for preparing 6N-grade magnesium chloride solution Download PDFInfo
- Publication number
- CN110642276B CN110642276B CN201911095103.XA CN201911095103A CN110642276B CN 110642276 B CN110642276 B CN 110642276B CN 201911095103 A CN201911095103 A CN 201911095103A CN 110642276 B CN110642276 B CN 110642276B
- Authority
- CN
- China
- Prior art keywords
- full
- organic phase
- extraction
- load
- cabapbalfe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
-
- 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
Abstract
The invention relates to a method for preparing a 6N-grade magnesium chloride solution, which takes a 4N-grade magnesium chloride aqueous solution as a feed liquid and C272 as an extracting agent, and comprises three steps of full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe, full-load fractional extraction separation of NaK/Mg and fractional extraction separation of Mg/CaBaPbAlFe, and is used for separating and removing metal element impurities such as sodium, potassium, calcium, barium, lead, aluminum, iron and the like in the feed liquid and non-metal element impurities such as sulfur, boron, silicon and the like to prepare the 6N-grade magnesium chloride solution. The purity of the 6N grade magnesium chloride solution of the target product is 99.99992-99.99998%, and the yield of magnesium in the 4N grade magnesium chloride aqueous solution is 95-97%. 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 6N-grade magnesium chloride solution, in particular to a method for preparing a 6N-grade magnesium chloride solution by taking a 4N-grade magnesium chloride aqueous solution as a feed liquid and C272 as an extracting agent, separating and removing metal elements such as sodium, potassium, calcium, barium, lead, aluminum, iron and the like in the feed liquid and non-metal elements such as sulfur, boron, silicon and the like. The invention belongs to the technical field of preparation of 6N-grade magnesium chloride.
Background
The 6N-grade magnesium chloride is one of basic raw materials for preparing other 6N-grade magnesium products and 6N-grade magnesium materials, but no method for preparing the 6N-grade magnesium chloride exists at present.
Aiming at the method for preparing 6N-grade magnesium chloride which is not available at present, the invention establishes a method for preparing 6N-grade magnesium chloride solution by taking 4N-grade magnesium chloride aqueous solution as feed liquid. The main impurities in the 4N-grade magnesium chloride aqueous solution comprise metallic element impurities such as sodium, potassium, calcium, barium, lead, aluminum, iron and the like, and non-metallic element impurities such as sulfur, boron, silicon and the like.
Disclosure of Invention
The invention provides a method for preparing a 6N-grade magnesium chloride solution, and provides a method for preparing the 6N-grade magnesium chloride solution from a 4N-grade magnesium chloride aqueous solution aiming at the situation that no method for preparing the 6N-grade magnesium chloride exists at present.
The invention relates to a method for preparing a 6N-grade magnesium chloride solution, which takes a 4N-grade magnesium chloride aqueous solution as a feed liquid and di (2,4, 4-trimethylpentyl) phosphonic acid (C272 or Cyanex272 for short) as an extracting agent, separates and removes metal elements such as sodium, potassium, calcium, barium, lead, aluminum, iron and the like in the feed liquid, and separates and removes non-metal elements such as sulfur, boron, silicon and the like to prepare the 6N-grade magnesium chloride solution.
The invention relates to a method for preparing 6N-grade magnesium chloride solution, which comprises 3 steps, namely full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe, full-load fractional extraction separation of NaK/Mg and fractional extraction separation of Mg/CaBaPbAlFe; the extraction section of full-load fractionation, extraction and separation NaKMg/MgCaBaPbAlFe realizes the separation of NaKMg/CaBaPbAlFe, and the washing section realizes the separation of NaK/MgCaBaPbAlFe; the method is characterized in that NaKMg/MgCaBaPbAlFe is separated by full-load fractionation extraction, a balanced loaded C272 organic phase obtained by separating NaK/Mg feeding level by full-load fractionation extraction is used as an extraction organic phase, and a balanced aqueous phase obtained by separating Mg/CaBaPbAlFe feeding level by fractionation extraction is used as a detergent. Full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaBaPbAlFe are directly connected in series; the outlet organic phase which is fully loaded with NaK/Mg and is separated by fractional extraction is used as an extraction organic phase for separating Mg/CaBaPbAlFe by fractional extraction, and directly enters the 1 st stage of separating Mg/CaBaPbAlFe by fractional extraction; the 1 st stage outlet aqueous phase of the Mg/CaBaPbAlFe separation by fractional extraction is used as a washing agent for full-load fractional extraction and separation of NaK/Mg.
The method for preparing the 6N-grade magnesium chloride solution comprises the following 3 steps:
step 1: full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe
Step 1 is full-load fractionation, extraction and separation of NaKMg/MgCaBaPbAlFe, the extraction section realizes the separation of NaKMg/CaBaPbAlFe, and the washing section realizes the separation of NaK/MgCaBaPbAlFe. And (3) taking a balanced loaded C272 organic phase obtained by the feed stage of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking a 4N-grade magnesium chloride aqueous solution as a feed liquid, and taking a balanced aqueous phase obtained by the feed stage of the Mg/CaBaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded C272 organic phase obtained from the feed stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the 1 st stage, the 4N-stage magnesium chloride aqueous solution enters the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the feed stage, and the equilibrium aqueous phase obtained from the feed stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the last 1 st stage. Obtaining a magnesium chloride solution containing Na, K, S, B and Si from the water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the magnesium chloride solution as feed liquid for full-load fractional extraction separation of NaK/Mg in the step 2; and (3) obtaining a C272 organic phase loaded with Mg-Ca-Ba-Pb-Al-Fe from the final 1-stage outlet organic phase of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the C272 organic phase as the feed liquid for fractional extraction and separation of Mg/CaBaPbAlFe 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 sulfur, boron and silicon in the magnesium chloride solution. An ammonia saponification C272 organic phase is used as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si, which is obtained from a No. 1 outlet water phase of a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1, is used as a feed liquid, and a 6N grade magnesium chloride solution which is obtained from a No. 1 outlet water phase of a Mg/CaBaPbAlFe fractionation extraction system in the step 3 is used as a washing agent. The saponification C272 organic phase enters a NaK/Mg full-load fractionation extraction system from the 1 st level as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si obtained from a water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters the NaK/Mg full-load fractionation extraction system from a feeding level, and a 6N-level magnesium chloride solution obtained from a water phase at the 1 st level outlet of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the Mg/CaBaPbAlFe fractionation extraction system from the last 1 level. Obtaining sodium chloride and potassium chloride mixed solution containing S, B and Si from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a balanced load C272 organic phase of a feed level 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/MgCaBaPbAlFe in the step 1; and obtaining a C272 organic phase loaded with magnesium from the organic phase at the outlet of the last stage 1 of the NaK/Mg full-load fractional extraction system, and using the C272 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaBaPbAlFe
And 3, fractionating, extracting and separating Mg/CaBaPbAlFe to realize the separation of magnesium from calcium, barium, lead, aluminum and iron. Taking a C272 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 C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron obtained from the last level 1 of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 6.0mol/L HCl as a washing acid. The C272 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 enters the Mg/CaBaPbAlFe fractionation extraction system from the level 1, the C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the last level 1 of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters the Mg/CaBaPbAlFe fractionation extraction system from the feeding level, and 6.0mol/L HCl washing acid enters the Mg/CaBaPbAlFe fractionation extraction system from the last level 1. Obtaining a target product 6N-grade magnesium chloride solution from a 1 st-grade outlet water phase of the Mg/CaBaPbAlFe fractional extraction system, and taking the 6N-grade magnesium chloride 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/CaBaPbAlFe fractional extraction system, and using the balance water phase as a detergent for separating NaKMg/MgCaBaPbAlFe through full-load fractional extraction in the step 1; and obtaining a C272 organic phase loaded with calcium, barium, lead, aluminum and iron from the final level 1 outlet organic phase of the Mg/CaBaPbAlFe fractional extraction system.
The C272 organic phase is a sulfonated kerosene solution of C272, wherein the concentration of the C272 is 1.0 mol/L. When used, the C272 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed C272 organic phase.
The element concentrations in the 4N-grade magnesium chloride aqueous solution are respectively as follows: s0.00010 g/L-0.00050 g/L, B0.00010.00010 g/L-0.00030 g/L, Si 0.00010.00010 g/L-0.00030 g/L, Na 0.00020.00020 g/L-0.00080 g/L, K0.00010.00010 g/L-0.00070 g/L, Mg 92.0.0 g/L-96.0 g/L, Ca 0.0010.0010 g/L-0.0050 g/L, Ba 0.0005.0 g/L-0.0020 g/L, Pb 0.00010 g/L-0.00030 g/L, Al 0.00010.00010 g/L-0.00030 g/L, Fe 0.00010.00010 g/L-0.00030 g/L.
The element concentrations in the 6N-grade magnesium chloride solution are respectively as follows: s0.0000010 g/L-0.0000030 g/L, B0.0000010 g/L-0.0000030 g/L, Si 0.0000010.0000010 g/L-0.0000030 g/L, Na 0.0000010.0000010 g/L-0.0000050 g/L, K0.0000010 g/L-0.0000050 g/L, Mg 68.0.0 g/L-72.0 g/L, Ca 0.000010.000010 g/L-0.000050 g/L, Ba 0.0000010.0000010 g/L-0.0000030 g/L, Pb 0.0000010.0000010 g/L-0.0000030 g/L, Al 0.0000010 g/L-0.0000030 g/L, Fe 0.0000010 g/L-0.0000030 g/L.
The invention has the beneficial effects that: 1) directly obtaining a 6N grade magnesium chloride solution from a 4N grade magnesium chloride aqueous solution. After the 6N-grade magnesium chloride solution is subjected to post-treatment such as concentration crystallization or precipitation, a series of 6N-grade magnesium-containing compounds such as 6N-grade magnesium chloride crystals and 6N-grade magnesium phosphate crystals can be obtained. 2) The product purity is high, and the yield of magnesium is high: the purity of the 6N grade magnesium chloride solution of the target product is 99.99992-99.99998%, and the yield of magnesium in the 4N grade magnesium chloride aqueous solution is 95-97%. 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/CaBaPbAlFe by fractional extraction, and directly enters the 1 st stage of separating Mg/CaBaPbAlFe by fractional extraction, so that saponification alkali for separating Mg/CaBaPbAlFe by fractional extraction is saved. The water phase at the 1 st stage outlet for fractionating, extracting and separating Mg/CaBaPbAlFe is used as a detergent for separating NaK/Mg by full-load fractionating, extracting and separating, and the washing acid for separating NaK/Mg by full-load fractionating, extracting and separating is saved. 4) The separation efficiency is high: and 3 separation steps (full-load fractional extraction separation NaKMg/MgCaBaPbAlFe, full-load fractional extraction separation NaK/Mg, fractional extraction separation Mg/CaBaPbAlFe) are adopted to separate and remove metal impurities such as sodium, potassium, calcium, barium, lead, aluminum, iron and the like and non-metal impurities such as sulfur, boron, silicon and the like in the 4N-grade magnesium chloride aqueous solution. 5) The process flow is short: the process for the preparation of magnesium chloride of grade 6N from an aqueous solution of magnesium chloride of grade 4N consists of 3 separation steps. The method is characterized in that NaKMg/MgCaBaPbAlFe is separated by full-load fractionation and extraction, and a balanced loaded C272 organic phase obtained by full-load fractionation, extraction and separation of NaK/Mg feeding level is used as an extraction organic phase, so that a saponification section is not needed for full-load fractionation, extraction and separation of NaKMg/MgCaBaPbAlFe; the equilibrium water phase obtained by fractionating, extracting and separating the Mg/CaBaPbAlFe feeding level is a detergent, so that a stripping section is not needed for full-load fractionating, extracting and separating NaKMg/MgCaBaPbAlFe. The full-load fractional extraction separation NaKMg/MgCaBaPbAlFe and the full-load fractional extraction separation NaK/Mg share a saponification section. The outlet organic phase which is fully loaded with NaK/Mg and is separated by fractional extraction is used as the extraction organic phase for separating Mg/CaBaPbAlFe by fractional extraction, so that the saponification section is not needed for separating Mg/CaBaPbAlFe 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/CaBaPbAlFe, so the fractional extraction for separating the full-load fractional extraction for separating the NaK/Mg does not need a washing section. 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 diagram of a method for preparing 6N-grade magnesium chloride solution;
in FIG. 1, LOP denotes the loaded organic phase; w represents a detergent; 6N Mg represents a 6N grade magnesium chloride solution.
Detailed Description
A method for preparing a 6N grade magnesium chloride solution according to the present invention is further described with reference to the following specific examples.
Example 1
The C272 organic phase is a sulfonated kerosene solution of C272, wherein the concentration of the C272 is 1.0 mol/L. When used, the C272 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed C272 organic phase.
The element concentrations in the 4N-grade magnesium chloride aqueous solution are respectively as follows: s0.00010 g/L, B0.00010.00010 g/L, Si 0.00010.00010 g/L, Na 0.00020.00020 g/L, K0.00010.00010 g/L, Mg 92.0.0 g/L, Ca 0.0010.0010 g/L, Ba 0.00050.00050 g/L, Pb 0.00010.00010 g/L, Al 0.00010.00010 g/L, Fe 0.00010.00010 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe
And (3) taking the equilibrium loaded C272 organic phase obtained from the 42 th level of the NaK/Mg full-loaded fractional extraction system in the step 2 as an extraction organic phase, taking a 4N level magnesium chloride aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 32 nd level of the Mg/CaBaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded C272 organic phase obtained from the 42 th stage of the NaK/Mg full-loaded fractionation extraction system in the step 2 enters into a NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 1 st stage, the 4N-stage magnesium chloride aqueous solution enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 8 th stage, and the equilibrium aqueous phase obtained from the 32 th stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 16 th stage. Obtaining a magnesium chloride solution containing Na, K, S, B and Si from the water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the magnesium chloride solution as feed liquid for full-load fractional extraction separation of NaK/Mg in the step 2; and (3) obtaining a C272 organic phase loaded with Mg-Ca-Ba-Pb-Al-Fe from a 16 th-stage outlet organic phase of a NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the C272 organic phase as feed liquid for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
An ammonia saponification C272 organic phase is used as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si, which is obtained from a No. 1 outlet water phase of a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1, is used as a feed liquid, and a 6N grade magnesium chloride solution which is obtained from a No. 1 outlet water phase of a Mg/CaBaPbAlFe fractionation extraction system in the step 3 is used as a washing agent. The saponification C272 organic phase enters a NaK/Mg full-load fractionation extraction system from the 1 st level as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si, which is obtained from the 1 st level outlet aqueous phase of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1, enters the NaK/Mg full-load fractionation extraction system from the 42 th level, and a 6N level magnesium chloride solution obtained from the 1 st level outlet aqueous phase of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 58 th level. Obtaining sodium chloride and potassium chloride mixed solution containing S, B and Si from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a 42 th-level equilibrium loaded C272 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/MgCaBaPbAlFe in the step 1; and obtaining a C272 organic phase loaded with magnesium from the 58 th grade outlet organic phase of the NaK/Mg full-load fractional extraction system, and using the C272 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaBaPbAlFe
Taking a C272 organic phase loaded with magnesium obtained from the 58 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 as an extraction organic phase, taking a C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron obtained from the 16 th stage of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 6.0mol/L HCl as a washing acid. The C272 organic phase loaded with magnesium and obtained from the 58 th level of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaBaPbAlFe fractionation extraction system from the 1 st level, the C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the 16 th level of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaBaPbAlFe fractionation extraction system from the 32 th level, and 6.0mol/L HCl washing acid enters into the Mg/CaBaPbAlFe fractionation extraction system from the 70 th level. Obtaining a target product 6N-grade magnesium chloride solution from a 1 st-grade outlet water phase of the Mg/CaBaPbAlFe fractional extraction system, and taking the 6N-grade magnesium chloride solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a 32 th-level equilibrium water phase of the Mg/CaBaPbAlFe fractional extraction system, and using the 32 th-level equilibrium water phase as a detergent for separating NaKMg/MgCaBaPbAlFe through full-load fractional extraction in the step 1; and obtaining a C272 organic phase loaded with calcium, barium, lead, aluminum and iron from a 70 th-stage outlet organic phase of the Mg/CaBaPbAlFe fractional extraction system.
The element concentrations in the 6N-grade magnesium chloride solution are respectively as follows: s0.0000010 g/L, B0.0000010 g/L, Si 0.0000010g/L, Na 0.0000010g/L, K0.0000010 g/L, Mg 68.0.0 g/L, Ca 0.000010g/L, Ba 0.0000010g/L, Pb 0.0000010g/L, Al 0.0000010.0000010 g/L, Fe 0.0000010.0000010 g/L. The purity of the magnesium chloride solution was 99.99998%, and the yield of magnesium was 95%.
Example 2
The C272 organic phase is a sulfonated kerosene solution of C272, wherein the concentration of the C272 is 1.0 mol/L. When used, the C272 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed C272 organic phase.
The element concentrations in the 4N-grade magnesium chloride aqueous solution are respectively as follows: s0.00030 g/L, B0.00020.00020 g/L, Si 0.00020.00020 g/L, Na 0.00050.00050 g/L, K0.00040.00040 g/L, Mg 94.0.0 g/L, Ca 0.0030.0030 g/L, Ba 0.0010g/L, Pb 0.00020.00020 g/L, Al 0.00020.00020 g/L, Fe 0.00020.00020 g/L.
Step 1: full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe
And (3) taking the equilibrium loaded C272 organic phase obtained from the 40 th level of the NaK/Mg full-loaded fractional extraction system in the step 2 as an extraction organic phase, taking a 4N level magnesium chloride aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 40 th level of the Mg/CaBaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded C272 organic phase obtained from the 40 th stage of the NaK/Mg full-loaded fractionation extraction system in the step 2 enters into a NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 1 st stage, the 4N-stage magnesium chloride aqueous solution enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 10 th stage, and the equilibrium aqueous phase obtained from the 40 th stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 22 th stage. Obtaining a magnesium chloride solution containing Na, K, S, B and Si from the water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the magnesium chloride solution as feed liquid for full-load fractional extraction separation of NaK/Mg in the step 2; and (3) obtaining a C272 organic phase loaded with Mg-Ca-Ba-Pb-Al-Fe from the 22 th-stage outlet organic phase of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the C272 organic phase as the feed liquid for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
An ammonia saponification C272 organic phase is used as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si, which is obtained from a No. 1 outlet water phase of a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1, is used as a feed liquid, and a 6N grade magnesium chloride solution which is obtained from a No. 1 outlet water phase of a Mg/CaBaPbAlFe fractionation extraction system in the step 3 is used as a washing agent. The saponification C272 organic phase enters a NaK/Mg full-load fractionation extraction system from the 1 st level as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si and obtained from the 1 st level outlet aqueous phase of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters the NaK/Mg full-load fractionation extraction system from the 40 th level, and a 6N level magnesium chloride solution obtained from the 1 st level outlet aqueous phase of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 60 th level. Obtaining sodium chloride and potassium chloride mixed solution containing S, B and Si from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a balance load C272 organic phase of the 40 th level 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/MgCaBaPbAlFe in the step 1; and obtaining a C272 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 C272 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaBaPbAlFe
Taking a C272 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 C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron obtained from the 22 nd stage of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 6.0mol/L HCl as a washing acid. The C272 organic phase loaded with magnesium and obtained from the 60 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaBaPbAlFe fractionation extraction system from the 1 st stage, the C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the 22 nd stage of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaBaPbAlFe fractionation extraction system from the 40 th stage, and 6.0mol/L HCl washing acid enters into the Mg/CaBaPbAlFe fractionation extraction system from the 76 th stage. Obtaining a target product 6N-grade magnesium chloride solution from a 1 st-grade outlet water phase of the Mg/CaBaPbAlFe fractional extraction system, and taking the 6N-grade magnesium chloride solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating the 40 th-level equilibrium water phase of the Mg/CaBaPbAlFe fractional extraction system, and using the balance water phase as a detergent for separating NaKMg/MgCaBaPbAlFe through full-load fractional extraction in the step 1; and obtaining a C272 organic phase loaded with calcium, barium, lead, aluminum and iron from the 76 th-stage outlet organic phase of the Mg/CaBaPbAlFe fractional extraction system.
The element concentrations in the 6N-grade magnesium chloride solution are respectively as follows: s0.0000020 g/L, B0.0000020 g/L, Si 0.0000020g/L, Na 0.0000030g/L, K0.0000030 g/L, Mg 702.0g/L, Ca 0.000030g/L, Ba 0.0000020g/L, Pb 0.0000020g/L, Al 0.0000020g/L, Fe 0.0000020 g/L. The purity of the magnesium chloride solution was 99.99995% and the yield of magnesium was 96%.
Example 3
The C272 organic phase is a sulfonated kerosene solution of C272, wherein the concentration of the C272 is 1.0 mol/L. When used, the C272 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed C272 organic phase.
The element concentration in the 4N grade magnesium chloride aqueous solution is S0.00050 g/L, B0.00030.00030 g/L, Si 0.00030.00030 g/L, Na 0.00080.00080 g/L, K0.00070.00070 g/L, Mg 96.0.0 g/L, Ca 0.0050.0050 g/L, Ba 0.0020.0020 g/L, Pb 0.00030g/L, Al 0.00030.00030 g/L, Fe 0.00030.00030 g/L respectively.
Step 1: full-load fractional extraction separation of NaKMg/MgCaBaPbAlFe
Taking the equilibrium loaded C272 organic phase obtained from the 38 th level of the NaK/Mg full-load fractional extraction system in the step 2 as an extraction organic phase, taking a 4N level magnesium chloride aqueous solution as a feed liquid, and taking the equilibrium aqueous phase obtained from the 42 th level of the Mg/CaBaPbAlFe fractional extraction system in the step 3 as a detergent. The equilibrium loaded C272 organic phase obtained from the 38 th stage of the NaK/Mg full-loaded fractionation extraction system in the step 2 enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 1 st stage, the 4N-stage magnesium chloride aqueous solution enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 12 th stage, and the equilibrium aqueous phase obtained from the 42 th stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters into the NaKMg/MgCaBaPbAlFe full-loaded fractionation extraction system from the 26 th stage. Obtaining a magnesium chloride solution containing Na, K, S, B and Si from the water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the magnesium chloride solution as feed liquid for full-load fractional extraction separation of NaK/Mg in the step 2; and (3) obtaining a C272 organic phase loaded with Mg-Ca-Ba-Pb-Al-Fe from the 26 th-stage outlet organic phase of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the C272 organic phase as the feed liquid for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
Step 2: full-load fractional extraction for separating NaK/Mg
An ammonia saponification C272 organic phase is used as an extraction organic phase, a magnesium chloride solution containing Na, K, S, B and Si, which is obtained from a No. 1 outlet water phase of a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1, is used as a feed liquid, and a 6N grade magnesium chloride solution which is obtained from a No. 1 outlet water phase of a Mg/CaBaPbAlFe fractionation extraction system in the step 3 is used as a washing agent. The saponified C272 organic phase is an extracted organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium chloride solution containing Na, K, S, B and Si and obtained from a water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters the NaK/Mg full-load fractionation extraction system from the 38 th level, and a 6N-level magnesium chloride solution obtained from a water phase at the 1 st level outlet of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the NaK/Mg full-load fractionation extraction system from the 60 th level. Obtaining sodium chloride and potassium chloride mixed solution containing S, B and Si from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a 38 th-level equilibrium loaded C272 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/MgCaBaPbAlFe in the step 1; and obtaining a C272 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 C272 organic phase as an extraction organic phase for fractional extraction and separation of Mg/CaBaPbAlFe in the step 3.
And step 3: fractionation, extraction and separation of Mg/CaBaPbAlFe
Taking a C272 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 C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron obtained from the 26 th stage of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 6.0mol/L HCl as a washing acid. The C272 organic phase loaded with magnesium and obtained from the 60 th stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters into a Mg/CaBaPbAlFe fractionation extraction system from the 1 st stage, the C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the 26 th stage of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaBaPbAlFe fractionation extraction system from the 42 th stage, and 6.0mol/L HCl washing acid enters into the Mg/CaBaPbAlFe fractionation extraction system from the 76 th stage. Obtaining a target product 6N-grade magnesium chloride solution from a 1 st-grade outlet water phase of the Mg/CaBaPbAlFe fractional extraction system, and taking the 6N-grade magnesium chloride solution as a detergent of the NaK/Mg full-load fractional extraction system in the step 2; separating a 42 th-level equilibrium water phase of a Mg/CaBaPbAlFe fractional extraction system, and using the balance water phase as a detergent for separating NaKMg/MgCaBaPbAlFe through full-load fractional extraction in the step 1; and obtaining a C272 organic phase loaded with calcium, barium, lead, aluminum and iron from the 76 th-stage outlet organic phase of the Mg/CaBaPbAlFe fractional extraction system.
The element concentrations in the 6N-grade magnesium chloride solution are respectively as follows: S0.0000030g/L, B0.0000030 g/L, Si 0.0000030g/L, Na 0.0000050g/L, K0.0000050 g/L, Mg 72.0.0 g/L, Ca 0.000050.000050 g/L, Ba 0.0000030g/L, Pb 0.0000030g/L, Al 0.0000030g/L, Fe 0.0000030 g/L. The purity of the magnesium chloride solution was 99.99992%, and the yield of magnesium was 97%.
Claims (4)
1. A method for preparing 6N grade magnesium chloride solution is characterized by comprising the following steps: the method takes 4N-grade magnesium chloride aqueous solution as feed liquid and C272 as an extracting agent, separates and removes metallic element impurities of sodium, potassium, calcium, barium, lead, aluminum and iron in the feed liquid, and separates and removes non-metallic element impurities of sulfur, boron and silicon to prepare 6N-grade magnesium chloride solution; comprises 3 steps, namely full-load fractionation, extraction and separation of NaKMg/MgCaBaPbAlFe, full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaBaPbAlFe; the extraction section of full-load fractionation, extraction and separation NaKMg/MgCaBaPbAlFe realizes the separation of NaKMg/CaBaPbAlFe, and the washing section realizes the separation of NaK/MgCaBaPbAlFe; full-load fractionation, extraction and separation of NaKMg/MgCaBaPbAlFe, namely, a balanced load C272 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/CaBaPbAlFe feeding level is used as a detergent; full-load fractionation, extraction and separation of NaK/Mg and fractionation, extraction and separation of Mg/CaBaPbAlFe are directly connected in series; the outlet organic phase which is fully loaded with NaK/Mg and is separated by fractional extraction is used as an extraction organic phase for separating Mg/CaBaPbAlFe by fractional extraction, and directly enters the 1 st stage of separating Mg/CaBaPbAlFe by fractional extraction; the 1 st level outlet water phase of the Mg/CaBaPbAlFe 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/MgCaBaPbAlFe
Step 1, full-load fractionation, extraction and separation of NaKMg/MgCaBaPbAlFe, wherein the extraction section realizes the separation of NaKMg/CaBaPbAlFe, and the washing section realizes the separation of NaK/MgCaBaPbAlFe; using a balanced loaded C272 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, using a 4N-grade magnesium chloride aqueous solution as a feed liquid, and using a balanced aqueous phase obtained from the feed stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 as a detergent; the equilibrium loaded C272 organic phase obtained from the feed stage of the NaK/Mg full-load fractionation extraction system in the step 2 enters a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the 1 st stage, the 4N-stage magnesium chloride aqueous solution enters the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the feed stage, and the equilibrium aqueous phase obtained from the feed stage of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system from the last 1 st stage; obtaining a magnesium chloride solution containing Na, K, S, B and Si from the water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractional extraction system, and using the magnesium chloride solution as feed liquid for full-load fractional extraction separation of NaK/Mg in the step 2; obtaining a C272 organic phase loaded with Mg-Ca-Ba-Pb-Al-Fe from the last 1-level outlet organic phase of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system, and using the C272 organic phase as feed liquid for fractionating, extracting and separating Mg/CaBaPbAlFe in the step 3;
step 2: full-load fractional extraction for separating NaK/Mg
Step 2, separating NaK/Mg by full-load fractional extraction, and separating and removing metallic element impurities of sodium and potassium and non-metallic element impurities of sulfur, boron and silicon in the magnesium chloride solution; taking an ammonia saponification C272 organic phase as an extraction organic phase, taking a magnesium chloride solution containing Na, K, S, B and Si obtained from a No. 1 outlet water phase of a NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking a 6N grade magnesium chloride solution obtained from a No. 1 outlet water phase of a Mg/CaBaPbAlFe fractionation extraction system in the step 3 as a washing agent; a saponified C272 organic phase is an extraction organic phase and enters a NaK/Mg full-load fractionation extraction system from the 1 st level, a magnesium chloride solution containing Na, K, S, B and Si and obtained from a water phase at the 1 st level outlet of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters the NaK/Mg full-load fractionation extraction system from a feeding level, and a 6N-level magnesium chloride solution obtained from a water phase at the 1 st level outlet of the Mg/CaBaPbAlFe fractionation extraction system in the step 3 enters the Mg/CaBaPbAlFe fractionation extraction system from the last 1 st level; obtaining sodium chloride and potassium chloride mixed solution containing S, B and Si from the water phase at the 1 st stage outlet of a NaK/Mg full-load fractional extraction system; separating a balanced load C272 organic phase of a feed level 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/MgCaBaPbAlFe in the step 1; obtaining a C272 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 C272 organic phase as an extraction organic phase for fractionating, extracting and separating Mg/CaBaPbAlFe in the step 3;
and step 3: fractionation, extraction and separation of Mg/CaBaPbAlFe
Step 3, fractionating, extracting and separating Mg/CaBaPbAlFe to realize the separation of magnesium from calcium, barium, lead, aluminum and iron; taking a C272 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 C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the last level 1 of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 as a feed liquid, and taking 6.0mol/L HCl as a washing acid; the C272 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 enters into a Mg/CaBaPbAlFe fractionation extraction system from the level 1, the C272 organic phase loaded with magnesium, calcium, barium, lead, aluminum and iron and obtained from the last level 1 of the NaKMg/MgCaBaPbAlFe full-load fractionation extraction system in the step 1 enters into the Mg/CaBaPbAlFe fractionation extraction system from a feeding level, and 6.0mol/L HCl washing acid enters into the Mg/CaBaPbAlFe fractionation extraction system from the last level 1; obtaining a target product 6N-grade magnesium chloride solution from a 1 st-grade outlet water phase of the Mg/CaBaPbAlFe fractional extraction system, and taking the 6N-grade magnesium chloride 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/CaBaPbAlFe fractional extraction system, and using the balance water phase as a detergent for separating NaKMg/MgCaBaPbAlFe through full-load fractional extraction in the step 1; and obtaining a C272 organic phase loaded with calcium, barium, lead, aluminum and iron from the final level 1 outlet organic phase of the Mg/CaBaPbAlFe fractional extraction system.
2. A process for preparing a 6N grade magnesium chloride solution according to claim 1, characterized in that: the C272 organic phase is a sulfonated kerosene solution of C272, wherein the concentration of the C272 is 1.0 mol/L; when used, the C272 organic phase is saponified with aqueous ammonia to obtain an ammonolyzed C272 organic phase.
3. A process for preparing a 6N grade magnesium chloride solution according to claim 1, characterized in that: the element concentrations in the 4N-grade magnesium chloride aqueous solution are respectively as follows: s0.00010 g/L-0.00050 g/L, B0.00010.00010 g/L-0.00030 g/L, Si 0.00010.00010 g/L-0.00030 g/L, Na 0.00020.00020 g/L-0.00080 g/L, K0.00010.00010 g/L-0.00070 g/L, Mg 92.0.0 g/L-96.0 g/L, Ca 0.0010.0010 g/L-0.0050 g/L, Ba 0.0005.0 g/L-0.0020 g/L, Pb 0.00010 g/L-0.00030 g/L, Al 0.00010.00010 g/L-0.00030 g/L, Fe 0.00010.00010 g/L-0.00030 g/L.
4. A process for preparing a 6N grade magnesium chloride solution according to claim 1, characterized in that: the element concentrations in the 6N-grade magnesium chloride solution are respectively as follows: s0.0000010 g/L-0.0000030 g/L, B0.0000010 g/L-0.0000030 g/L, Si 0.0000010.0000010 g/L-0.0000030 g/L, Na 0.0000010.0000010 g/L-0.0000050 g/L, K0.0000010 g/L-0.0000050 g/L, Mg 68.0.0 g/L-72.0 g/L, Ca 0.000010.000010 g/L-0.000050 g/L, Ba 0.0000010.0000010 g/L-0.0000030 g/L, Pb 0.0000010.0000010 g/L-0.0000030 g/L, Al 0.0000010 g/L-0.0000030 g/L, Fe 0.0000010 g/L-0.0000030 g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911095103.XA CN110642276B (en) | 2019-11-11 | 2019-11-11 | Method for preparing 6N-grade magnesium chloride solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911095103.XA CN110642276B (en) | 2019-11-11 | 2019-11-11 | Method for preparing 6N-grade magnesium chloride solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110642276A CN110642276A (en) | 2020-01-03 |
| CN110642276B true CN110642276B (en) | 2022-01-25 |
Family
ID=68995733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911095103.XA Active CN110642276B (en) | 2019-11-11 | 2019-11-11 | Method for preparing 6N-grade magnesium chloride solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110642276B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721559A (en) * | 2004-12-15 | 2006-01-18 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
| CN1730680A (en) * | 2005-09-05 | 2006-02-08 | 有研稀土新材料股份有限公司 | Rare-earth element extraction separation process using nonsaponifying organic extractant |
| CN101994004A (en) * | 2009-08-11 | 2011-03-30 | 北京有色金属研究总院 | Process for extracting and separating rare-earth elements |
| CN105779762A (en) * | 2016-05-17 | 2016-07-20 | 南昌航空大学 | Process for preparing 5N erbium by extracting and separating |
| CN107099681A (en) * | 2017-05-16 | 2017-08-29 | 广东富远稀土新材料股份有限公司 | A kind of method of extract and separate yttrium |
| CN107299225A (en) * | 2017-06-22 | 2017-10-27 | 南昌航空大学 | A kind of method that C272 fractional extractions prepare 6N grades of cobalt chlorides |
| CN109319819A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of technique preparing 6N grades of strontium nitrates |
| CN110066925A (en) * | 2019-04-28 | 2019-07-30 | 浙江天能新材料有限公司 | The recovery method of valuable metal in a kind of waste and old nickel-cobalt-manganese ternary lithium battery |
-
2019
- 2019-11-11 CN CN201911095103.XA patent/CN110642276B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721559A (en) * | 2004-12-15 | 2006-01-18 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
| CN1730680A (en) * | 2005-09-05 | 2006-02-08 | 有研稀土新材料股份有限公司 | Rare-earth element extraction separation process using nonsaponifying organic extractant |
| CN101994004A (en) * | 2009-08-11 | 2011-03-30 | 北京有色金属研究总院 | Process for extracting and separating rare-earth elements |
| CN105779762A (en) * | 2016-05-17 | 2016-07-20 | 南昌航空大学 | Process for preparing 5N erbium by extracting and separating |
| CN107099681A (en) * | 2017-05-16 | 2017-08-29 | 广东富远稀土新材料股份有限公司 | A kind of method of extract and separate yttrium |
| CN107299225A (en) * | 2017-06-22 | 2017-10-27 | 南昌航空大学 | A kind of method that C272 fractional extractions prepare 6N grades of cobalt chlorides |
| CN109319819A (en) * | 2018-11-26 | 2019-02-12 | 南昌航空大学 | A kind of technique preparing 6N grades of strontium nitrates |
| CN110066925A (en) * | 2019-04-28 | 2019-07-30 | 浙江天能新材料有限公司 | The recovery method of valuable metal in a kind of waste and old nickel-cobalt-manganese ternary lithium battery |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110642276A (en) | 2020-01-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109319818B (en) | Method for preparing 5N-grade strontium chloride | |
| CN109264758B (en) | Method for preparing 6N-grade strontium chloride | |
| CN109319819B (en) | Process for preparing 6N-grade strontium nitrate | |
| CN110776040B (en) | Method for preparing 4N-grade calcium chloride by extracting and separating calcium saponification wastewater with rare earth | |
| CN110668479B (en) | Method for preparing 5N-grade magnesium sulfate solution | |
| CN110790296B (en) | Method for preparing 5N-grade calcium nitrate solution | |
| CN109292807B (en) | Method for preparing 5N-grade strontium nitrate | |
| CN111039315B (en) | Method for preparing 5N-grade calcium chloride solution | |
| CN110642276B (en) | Method for preparing 6N-grade magnesium chloride solution | |
| CN103787396A (en) | Method for preparing high-purity potassium alum and aluminum sulfate from alunite ore | |
| CN109231251B (en) | Method for directly preparing 4N-grade strontium chloride | |
| CN110787485B (en) | Method for preparing 6N-grade calcium chloride solution | |
| CN109485082B (en) | Process for directly preparing 4N-grade strontium nitrate | |
| CN111204781B (en) | Method for preparing 6N-grade magnesium nitrate solution | |
| CN110627096B (en) | Method for preparing 5N-grade magnesium chloride solution | |
| CN110885092B (en) | Method for preparing 6N-grade magnesium sulfate solution | |
| CN110668484B (en) | Method for preparing 4N-grade calcium nitrate solution | |
| CN110921690B (en) | Method for preparing 5N-grade magnesium nitrate solution | |
| CN110697743B (en) | Method for preparing 4N-grade magnesium sulfate | |
| CN110615460A (en) | Method for preparing 6N-grade calcium nitrate solution | |
| CN110668478B (en) | Method for preparing 4N-grade magnesium chloride | |
| CN110697742B (en) | Method for preparing 4N-grade magnesium nitrate solution | |
| CN109133143B (en) | Simple method for co-producing pure lanthanum, cerium-rich and pure yttrium | |
| CN114702057B (en) | Method for preparing 6N-grade neodymium chloride by fractional extraction separation process | |
| CN114804183B (en) | Method for preparing 6N-level lanthanum chloride by Y-shaped fractional extraction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |