CN114686702B - Method for purifying magnesium by serpentine normal pressure sulfuric acid leaching solution in one pot - Google Patents
Method for purifying magnesium by serpentine normal pressure sulfuric acid leaching solution in one pot Download PDFInfo
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- 239000011777 magnesium Substances 0.000 title claims abstract description 106
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 100
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 93
- 238000002386 leaching Methods 0.000 title claims abstract description 79
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 68
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 title claims abstract description 53
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 47
- 230000003647 oxidation Effects 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 22
- 239000007800 oxidant agent Substances 0.000 claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 17
- 230000001105 regulatory effect Effects 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 230000001276 controlling effect Effects 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 76
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 49
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 31
- 239000000347 magnesium hydroxide Substances 0.000 claims description 31
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 31
- 229910052759 nickel Inorganic materials 0.000 claims description 23
- 238000001556 precipitation Methods 0.000 claims description 15
- 239000000395 magnesium oxide Substances 0.000 claims description 13
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 8
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims 2
- 150000002500 ions Chemical class 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000006757 chemical reactions by type Methods 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 58
- 238000011084 recovery Methods 0.000 description 55
- 238000001914 filtration Methods 0.000 description 27
- 229910052742 iron Inorganic materials 0.000 description 27
- 239000011651 chromium Substances 0.000 description 21
- 239000011572 manganese Substances 0.000 description 20
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 229910052748 manganese Inorganic materials 0.000 description 15
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 14
- 229910052804 chromium Inorganic materials 0.000 description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 9
- 239000000706 filtrate Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- 229910052717 sulfur Inorganic materials 0.000 description 9
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 8
- 235000021110 pickles Nutrition 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 2
- 229910052620 chrysotile Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- CWBIFDGMOSWLRQ-UHFFFAOYSA-N trimagnesium;hydroxy(trioxido)silane;hydrate Chemical compound O.[Mg+2].[Mg+2].[Mg+2].O[Si]([O-])([O-])[O-].O[Si]([O-])([O-])[O-] CWBIFDGMOSWLRQ-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052898 antigorite Inorganic materials 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 229910052899 lizardite Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000002364 soil amendment Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- IBPRKWGSNXMCOI-UHFFFAOYSA-N trimagnesium;disilicate;hydrate Chemical compound O.[Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IBPRKWGSNXMCOI-UHFFFAOYSA-N 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B47/00—Obtaining manganese
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the field of mineral resource utilization, and particularly discloses a method for purifying magnesium by using serpentine normal-pressure sulfuric acid leaching liquid in one pot, wherein the serpentine sulfuric acid normal-pressure acid leaching liquid is subjected to one-pot three-stage reaction treatment, and then solid-liquid separation is carried out to obtain a purified magnesium solution; the one-pot three-stage reaction process comprises the following steps: regulating the pH A of the leaching solution to 2.0-3.0, and adding an oxidant to perform first-stage oxidation treatment; then regulating the pH of the system to B to 4.5-6, adding an oxidant to carry out second-stage oxidation treatment; regulating and controlling the pH of the system to be C -7-8, and then carrying out a third-stage reaction; in the one-pot three-stage reaction process, the temperature of the first-stage oxidation reaction and the second-stage oxidation reaction is 60-80 ℃, and the temperature of the third-stage reaction is 80-90 ℃. Under the one-pot three-stage treatment process, the invention can realize synergy by matching with the joint control of the reaction types, pH values and temperatures of the stages, can effectively realize the one-pot high-selectivity separation of magnesium and ions, and is beneficial to obtaining high-purity magnesium solution.
Description
Technical Field
The invention relates to the field of comprehensive utilization of resources, in particular to a serpentine wet method pure magnesium method.
Background
Serpentine is a general term for water-containing magnesium-rich silicate minerals, the chemical composition of which is 3MgO.2SiO 2·2H2 O, which is dark greenish, brown or yellow, and has spots in most cases, the hardness of which is 2-3.5 and the density of which is 2.2-3.69/cm 3 because of the fact that the grinding surface looks like a snake vein. The crystal structure of the material is a double-layer structure formed by combining a layer of silicon oxygen tetrahedron and a layer of brucite octahedron in a ratio of 1:1. Serpentine can be generally classified into three types according to mineral structure: (1) chrysotile (Chrysotile) with a cylindrical structure; (2) lixiviate (Lizardite) having a flat structure; (3) Serpentine (Antigorite) having an alternating wave structure. All serpentine minerals, whether or not having fibrous character, are of lamellar structure, similar to kaolinite. Six-coordinated Mg 2+ in the ore may be replaced with A1 3+、Ni2+、Fe2+、Fe3+、Mn2+ or the like, particularly in aluminum serpentine (zoblitzite), nickel serpentine (gamierite), iron serpentine (greenallte) or the like. Serpentine generally contains small amounts of metals such as iron, aluminum, chromium, nickel, cobalt, manganese, etc. Serpentine is therefore an important potential source of nickel and cobalt.
The wet smelting of serpentine is a main means of resource utilization, and the wet smelting process in the industry at present mainly comprises a hydrochloric acid leaching process, a high-pressure sulfuric acid leaching process and a normal-pressure sulfuric acid leaching process. The hydrochloric acid leaching process has mild leaching conditions, small equipment investment, and the Cl - can effectively destroy colloid stability, reduce solution viscosity, and is beneficial to operation and separation, but has higher requirements on recycling of hydrochloric acid due to easy volatilization and high cost, thus being unfavorable for industrial large-scale application. The high-pressure sulfuric acid leaching process is commonly applied to smelting treatment of serpentine ores with high nickel grade, can effectively control iron leaching, and is commonly used for extracting nickel in serpentine ores; however, the high-temperature leaching process has high energy consumption, high cost and high requirements on ore grade. Compared with the high-pressure sulfuric acid leaching process, the normal-pressure sulfuric acid leaching process is commonly used for smelting low-grade serpentine, the leaching selectivity is not ideal, the metal ions of the leaching solution are various, and the leaching solution has the characteristics of high iron, high magnesium, low nickel and the like.
For element recovery of low-grade sulfuric acid normal pressure leaching solution, the main means in industry is fractional classification recovery, for example, publication No. CN103395796A discloses a comprehensive utilization method of serpentine, which comprises the following steps: leaching serpentine with sulfuric acid, and filtering to obtain a first filtrate; adding an oxidant to the first filtrate; adding a pH value regulator to perform precipitation reaction, and filtering to obtain an iron-aluminum mixture and a second filtrate; adding water and sodium hydroxide into the iron-aluminum mixture, and filtering to obtain an iron precipitate and a sodium metaaluminate solution; adding sulfide into the second filtrate for reaction, and filtering to obtain a nickel-cobalt mixture and a third filtrate; adding an oxidant into the third filtrate for reaction; then adding alkaline adsorbent, filtering to obtain magnesium sulfate solution, and adding ammonia water to prepare magnesium hydroxide.
For smelting of low-grade serpentine sulfuric acid normal pressure leaching liquid, most of industries are classified smelting by multi-step separation process, the process treatment efficiency is low, the process operability is not strong, and the recovery rate of target elements and the purity of products are required to be improved.
Disclosure of Invention
Aiming at the problems of easy gel formation, high viscosity, unsatisfactory magnesium recovery rate and purity and the like in the wet process of extracting magnesium from serpentine normal pressure sulfuric acid leaching solution, the invention aims to provide a method for purifying magnesium from serpentine normal pressure sulfuric acid leaching solution (also called leaching solution for short) in one pot, and aims to provide a method for realizing selective separation of magnesium ions and other ions in leaching solution under one pot system and improving the recovery rate and purity of magnesium.
For the treatment value consideration, the low-grade serpentine is recovered by adopting a sulfuric acid normal pressure acid leaching process, the leaching solution obtained by the process is a sulfuric acid system of high iron, high magnesium, low nickel and rich trace impurity elements, and the leaching solution of the type is difficult to realize one-pot separation and recovery of magnesium, and is mainly characterized in that: (1) The system is a high-iron sulfuric acid system, a solution is easy to form colloid, sulfate ions are difficult to destroy the colloid structure, so that separation and recovery of magnesium and other components are influenced, and the process operation is difficult, for example, filtration is difficult; (2) Under the system, abundant metal impurity components exist, and the components are difficult to realize one-pot high-selectivity separation with magnesium; (3) recovery, purity and whiteness of magnesium are not ideal. Aiming at the problem that serpentine sulfuric acid normal pressure acid leaching solution is difficult to realize one-pot high selectivity separation, the invention provides the following improved process:
A method for purifying magnesium from serpentine normal pressure sulfuric acid leaching solution (also referred to as pickle liquor for short) in one pot comprises the steps of carrying out one-pot three-stage reaction treatment on serpentine sulfuric acid normal pressure acid leaching solution, and then carrying out solid-liquid separation to obtain a purified magnesium solution;
fe, cr, mn and Mg are dissolved in the leaching solution;
The one-pot three-stage reaction process comprises the following steps: regulating the pH A of the leaching solution to 2.0-3.0, and adding an oxidant to perform first-stage oxidation treatment; then regulating the pH of the system to B to 4.5-6, adding an oxidant to carry out second-stage oxidation treatment; regulating and controlling the pH of the system to be C -7-8, and then carrying out a third-stage reaction;
In the one-pot three-stage reaction process, the temperature of the first-stage oxidation reaction and the second-stage oxidation reaction is 60-80 ℃, and the temperature of the third-stage reaction is 80-90 ℃.
Aiming at the problems that magnesium is difficult to purify by one pot and the operation difficulty of the process is high due to the characteristics of normal pressure sulfuric acid pickle liquor components, the invention innovatively provides that under the one-pot three-stage treatment process, the cooperation of the joint control of the reaction types, pH values and temperatures of all the stages can be realized, the problem that the impurity elements and magnesium are difficult to separate in a one pot manner due to a normal pressure acid leaching system, high iron, high impurity elements and a sulfuric acid system can be solved, the magnesium and each ion can be effectively separated in a one pot manner, and the method is beneficial to obtaining a high-purity magnesium solution.
The research of the invention discovers that the three-stage reaction process of the first stage oxidation, the second stage oxidation and the third stage reaction under the one-pot system and the combined control of the pH value and the temperature of each stage reaction are key to cooperatively solve the problem that the normal pressure leaching solution is difficult to be treated in one pot and improve the magnesium extraction and purification effect.
In the invention, the pickle liquor is obtained by low-grade serpentine normal-pressure sulfuric acid pickling.
In the invention, the leaching solution is sulfuric acid leaching solution under the normal pressure of serpentine. The sulfuric acid concentration is, for example, 2 to 5 mol.L -1. The temperature of the atmospheric acid leaching is, for example, 80 to 100 ℃, preferably 80 to 95 ℃.
In the invention, the leaching solution is a sulfuric acid system with high iron, low nickel and high magnesium. The concentrations thereof are, for example, respectively: the concentration of Fe is 5-18 g/L; the concentration of Mn (II) is 0.2-0.5 g/L, cr (III) is 0.10-0.40 g/L, mg and 50-65 g/L. Further preferably, the concentration of Fe is 6 to 12g/L; the concentration of Mn (II) is 0.12-0.4 g/L, cr (III) is 0.20-0.4 g/L, mg and 50-65 g/L. According to the technical scheme, the method can show better industrial application value for one-pot treatment of the leaching solution, but does not exclude application of the method to other leaching solutions.
In the invention, the pickle liquor is also allowed to contain at least one of nickel, cobalt and aluminum; wherein, the concentration of Ni in the leaching solution is 0.20-0.6 g/L; the concentration of Co is 0.01-0.04 g/L; the concentration of Al is 0.2-2 g/L; further preferably, the concentration of Ni is, for example, 0.30 to 0.6g/L; the Co concentration is, for example, 0.02 to 0.03g/L; the concentration of Al is 0.3-1.8 g/L. According to the technical scheme, the high-selectivity separation of magnesium and iron, manganese, chromium, nickel, aluminum and cobalt in the sulfuric acid system in the next pot can be realized, and the magnesium smelting effect and the magnesium smelting efficiency are excellent.
In the invention, in the one-pot three-stage treatment process, the pH value of the system is regulated by adopting an alkaline substance, wherein the alkaline substance is at least one of magnesium oxide, alkali metal hydroxide, calcium oxide and ammonia water. The alkaline substance can be used in the form of solid or solution.
In the invention, in the one-pot three-stage treatment process, the oxidant is at least one of chlorate, oxygen or hydrogen peroxide.
In the invention, alkaline substances are added into normal pressure leaching liquid in advance, the pH of the system is regulated to be the required pH A, and oxidant is introduced at the required temperature of 60-80 ℃ to perform first stage oxidation treatment in one-pot reaction. According to the research of the invention, the nucleation behavior and morphology of iron can be unexpectedly regulated and controlled at the temperature and pH, so that the separation selectivity of magnesium, iron and other elements in a one-pot system can be unexpectedly and further synergistically improved, and the processing performance of one-pot treatment is improved.
In the invention, the dosage of the oxidant in the first stage oxidation reaction stage is 1.2-1.5 times of the theoretical molar quantity of Fe in the system. Preferably, the pH A is 2.0 to 3.0. The temperature of the first stage oxidation treatment is preferably 60 to 70 ℃, more preferably 60 to 65 ℃.
In the present invention, the time of the first stage oxidation treatment is preferably 0.5 to 1.0h.
In the invention, after the first stage oxidation treatment, solid-liquid separation is not needed, the pH of the system is directly regulated and controlled to be B, and an oxidant is introduced at the required temperature of 60-80 ℃ to perform the second stage oxidation treatment in the one-pot reaction. According to the invention, under the synergistic premise of the first-stage oxidation treatment, the combined control of the process and the temperature of the second-stage oxidation treatment is further matched, so that the selective oxidation of Mn in the system can be realized, the concomitant oxidation of Cr in the system is avoided, and the method can be combined with the first oxidation reaction to synergistically improve the one-pot separation selectivity of magnesium and other components and improve the one-pot separation recovery rate and purity of magnesium.
Preferably, in the second stage of the oxidation reaction, the amount of the oxidizing agent is 1.2 to 1.5 times the theoretical molar amount of oxidation of Mn in the system to Mn (IV).
In the present invention, the temperature of the second stage oxidation reaction process is preferably 60 to 70 ℃.
Preferably, the pH B is 5.0 to 6.0.
Preferably, the time of the second stage oxidation reaction is 0.5 to 1.0h.
In the invention, after the second stage oxidation treatment, the pH of the system is directly regulated to be C without solid-liquid separation, and the third stage reaction is carried out at the required temperature of 80-90 ℃ to realize other selective precipitation of other ions such as Cr and the like except magnesium and improve nucleation behavior, so that the separation effect of magnesium and other ions can be unexpectedly and synergistically improved, the recovery rate and purity of magnesium are improved, and the enrichment effect of other elements in slag is improved.
Preferably, the pH C is 7.0 to 8.0.
Preferably, the time of the third reaction is 2.0 to 3.0 hours.
According to the invention, under the one-pot three-stage reaction, the pH and temperature of each stage are matched to realize coordination, so that the nucleation behavior and morphology of elements in a one-pot system can be controlled, the morphology of slag constructed under the conditions can cooperatively induce the nucleation selectivity of other elements with the subsequent conditions, the separation selectivity of Mg and other components can be controlled, the recovery rate and purity of magnesium can be improved, the filtering difficulty can be reduced, and the process operability can be improved.
In the present invention, the magnesium solution may be treated by known means. For example, a precipitant is added to the magnesium solution to perform a magnesium precipitation reaction to prepare magnesium hydroxide.
The precipitant is at least one of ammonia water and alkali metal hydroxide. The precipitant is in the form of a solution, the concentration of which is, for example, 1 mol.L -1～13mol·L-1.
Preferably, the pH value of the reaction end point in the magnesium precipitation reaction process is 8.8-9.5;
Preferably, the temperature of the magnesium precipitation reaction process is 70-80 ℃;
Preferably, the time of the magnesium precipitation reaction is 1-2 h.
In the invention, magnesium hydroxide is put into alkali liquor for aging treatment, and then solid-liquid separation and washing are carried out to obtain purified magnesium hydroxide;
Preferably, the alkali liquor is an aqueous solution of alkali metal hydroxide, and the concentration of a preferable solute is 0.2 mol.L -1～0.5mol·L-1;
preferably, the temperature of aging is 70-80 ℃;
preferably, the aging time is 60 to 120 minutes.
The invention relates to a method for preparing high-purity magnesium hydroxide by utilizing leaching liquid, which comprises the following steps:
(1) Adding alkaline substances into serpentine sulfuric acid leaching solution, and regulating the pH value of the system to be 2.0-3.0; then adding an oxidant, and carrying out a first-stage reaction at the temperature of 60-70 ℃; then continuously adding alkaline substances until the pH value of the system is 4.5-6.0 without filtering, adding an oxidant and carrying out second-stage oxidation treatment at the temperature of 50-60 ℃; filtering is not needed after the treatment, alkaline substances are added until the pH value of the system is 7.0-8.0, and the third-stage reaction is carried out at the temperature of 80-90 ℃; and then filtering for one time to obtain pure magnesium sulfate solution.
(2) And adding a certain amount of precipitant into the filtered magnesium sulfate solution at a certain temperature to carry out magnesium precipitation reaction. Controlling the pH value in the reaction process to 8.8-9.5 and the temperature to 70-80 ℃; the time is 1-2 h, and then the Mg (OH) 2 is obtained by filtering. The magnesium sulfate solution and the precipitant in the step (2) are added in a bidirectional dropwise manner.
(3) Washing magnesium hydroxide with hot water for 3-5 times.
(4) Adding sodium hydroxide solution with a certain concentration into magnesium hydroxide for reaction, filtering and washing, controlling the reaction temperature to be 70-80 ℃ and the reaction time to be 60-120 min, and obtaining the high-purity magnesium hydroxide product meeting the quality standard.
Compared with the prior art, the invention has the following advantages and beneficial effects:
aiming at the problems that magnesium purification and great process operation difficulty are difficult to realize by the characteristic of lixivium components of serpentine normal pressure sulfuric acid leaching, the invention innovatively provides that under the one-pot three-stage treatment process, the combination control of reaction types, pH values and temperatures of all stages is matched, the synergy can be realized, the problem that magnesium is difficult to realize high-selectivity separation by one pot due to high iron content and rich impurity elements of a normal pressure acid leaching system can be solved, the magnesium and each ion can be effectively separated by one pot, and the recovery rate of magnesium and the enrichment recovery rate of other components in slag are improved by utilizing the obtained high-purity magnesium solution.
Drawings
FIG. 1 is an XRD pattern for the product of example 1;
FIG. 2 is an SEM image of the product of example 1;
The specific embodiment is as follows:
the following describes the technical scheme of the present application in detail by referring to examples:
from the chemical industry standard HG/T3607-2007 for industrial magnesium hydroxide, it is known that industrial magnesium hydroxide can be classified into three types:
Class I: the material is mainly used as a raw material of a flame retardant, [ Mg (OH) 2 ] with the mass fraction/% > or more than 97.5;
class II: the magnesium oxide is mainly used as a raw material for producing magnesium oxide and magnesium salt; [ Mg (OH) 2 ] mass fraction/% > or more than 93
Class III: the method is mainly used for flue desulfurization, wastewater treatment, agricultural fertilizers, soil amendments and the like; [ Mg (OH) 2 ] mass fraction/% > 92.
Therefore, the purity requirement of Mg (OH) 2 produced by the process of the invention meets the class I standard of the industry.
The following cases are that the pickle liquor is obtained by low-grade serpentine through sulfuric acid normal pressure acid leaching, and the main element concentration (g.L -1) in the serpentine normal pressure sulfuric acid leaching solution is as follows: mg 60,Fe 12.89,Al 1.54,Cr (III) 0.33, co (II) 0.025, mn (II) 0.40, ni (II) 0.55.
The present invention will be described in further detail with reference to the following examples, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, and the description thereof is merely illustrative of the present invention and not intended to be limiting.
Example 1:
Step (1): and (3) one-pot treatment:
Adding sodium chlorate with the iron content of 1.3 times when the pH A of the lixivium is regulated to 2.0 by 10% MgO slurry and carrying out first stage oxidation treatment at 60 ℃ for 30 minutes; continuously adopting 10% MgO slurry to adjust the pH B of the leaching solution to 5.5 without filtering, introducing oxygen (1.3 times of the molar quantity of manganese), and carrying out second-stage oxidation treatment at 70 ℃ for 30 minutes; continuously adjusting the pH to C to 7.0 by using 10 percent MgO slurry without filtering, and carrying out a third-stage reaction for 2 hours at the temperature of 80 ℃;
After one-pot three-stage treatment is completed, filtering is carried out, the filtering speed is 12mg/min cm 2, the nickel content in the filtrate after filtering is 0.13mg L -1, the cobalt content is 0.07mg L -1, the manganese content is 0.43mg L -1, and the content of chromium and iron is extremely low, so that ICP is not detected; the method has the advantages that the recovery rate of iron in slag is more than 99.99%, the recovery rate of nickel is 99.97%, the recovery rate of manganese is 99.87%, the recovery rate of chromium is more than 99.99%, and the loss rate of magnesium is less than 0.7%.
Step (2): magnesium precipitation and aging:
Dropping ammonia water into the purified and purified solution for precipitation reaction at 70 ℃ and pH of 8.9 in the reaction process and the reaction end point; the reaction time was 1.0h, and Mg (OH) 2 was obtained by filtration and washing, and Mg (OH) 2 obtained by washing was aged with 0.10 mol.L -1 NaOH (temperature: 70 ℃ C.) for 1.0h. The sulfur content of magnesium hydroxide was 0.17%, the total recovery rate of magnesium was 80%, no Cr element was detected in magnesium hydroxide, the purity of magnesium hydroxide was 98.63%, and the whiteness was 98.6%. The XRD and SEM images of magnesium hydroxide are shown in FIGS. 1 and 2.
Example 2:
Step (1): and (3) one-pot treatment:
Serpentine leaching solution (pickle liquor, same as in example 1) is 300mL, when the pH of the leaching solution is adjusted to 3 by 10% MgO slurry, sodium chlorate with the iron content of 1.4 times is added, and the first stage oxidation treatment is carried out at 60 ℃ for 40 minutes; when the pH of the leaching solution is adjusted to 6 by 10 percent MgO slurry, hydrogen peroxide with the manganese content of 1.4 times is introduced, and the second stage oxidation treatment is carried out at the temperature of 60 ℃ for 40min; continuously adjusting the pH with 10% MgO slurry until the pH is adjusted to 8, and carrying out a third-stage reaction for 2H at 90 ℃;
After one-pot three-stage treatment is completed, filtering is carried out, wherein the filtering speed is 15mg/min cm 2, the nickel content in the filtrate after filtering is 0.074mg.L -1, the cobalt content is 0.019 mg.L -1, the manganese content is 1.48 mg.L -1, the chromium content is 0.041 mg.L -1, and the iron content is 0.014 mg.L -1; the method has iron recovery rate of more than 99.9%, nickel recovery rate of 99.92%, manganese recovery rate of 99.57%, chromium recovery rate of more than 99.99%, and magnesium loss rate of less than 0.8%
Step (2): magnesium precipitation and aging:
Adding ammonia water into the purified and impurity-removed solution, controlling the feeding temperature to be 30 ℃, heating to 80 ℃ after the pH value of the system reaches 9, and controlling the pH value of the reaction process and the end point to be 9.2; the reaction time was kept at 1.5 hours, then Mg (OH) 2 was obtained by filtration and washing, and the washed Mg (OH) 2 was aged with 0.15 mol.L -1 NaOH (temperature 80 ℃ C.) for 1.5 hours, the total recovery rate of magnesium was 82%, the sulfur content of magnesium hydroxide was 0.18%, cr element was not detected in magnesium hydroxide, the purity of magnesium hydroxide was 98.71%, and the whiteness was 99.6%.
Example 3:
step (1): one pot treatment (pilot treatment):
Serpentine leaching solution (pickle liquor, same as in example 1) is 300L, when the pH of the leaching solution is adjusted to 2.5 by 10% MgO slurry, sodium chlorate with the iron content of 1.5 times is added, and the temperature is kept at 65 ℃ for carrying out first stage oxidation treatment, and oxidation is carried out for 50 minutes; when the pH of the leaching solution is adjusted to 5 by 10 percent MgO slurry, introducing oxygen with the manganese content of 1.5 times, and carrying out second-stage oxidation treatment for 50 minutes at the temperature of 65 ℃; continuously adjusting the pH with 10% MgO slurry until the pH is adjusted to 7.5, and carrying out a third-stage reaction for 2h at 85 ℃;
After one-pot three-stage treatment is completed, filtering is carried out, the filtering speed is 73 g/h.dm 2, the nickel content in the filtered filtrate is 0.11 mg.L -1, the cobalt content is 0.09 mg.L -1, the manganese content is 0.41 mg.L -1, the chromium content is 0.85 mg.L -1, and the ICP is not detected because the iron content is extremely low; in the method, the recovery rate of iron is more than 99.9%, the recovery rate of nickel is 99.98%, the recovery rate of manganese is 99.89%, the recovery rate of chromium is 99.7%, and the loss rate of magnesium is 1.2%.
Step (2): magnesium precipitation and aging:
Adding ammonia water into the solution after purification and impurity removal in the step (1), controlling the feeding temperature to be 40 ℃, heating to 75 ℃ for heat preservation reaction after the pH value of the system reaches 8.8, controlling the pH value of the reaction process and the reaction end point to be 9.1, reacting for 2.0h, then filtering and washing to obtain Mg (OH) 2, ageing the washed Mg (OH) 2 with 0.20mol.L -1 NaOH (the temperature is 75 ℃) for 2.0h, the total recovery rate of magnesium is 75%, the sulfur content of magnesium hydroxide is 0.16%, cr element is not detected in the magnesium hydroxide, the purity of the magnesium hydroxide is 98.5%, and the whiteness of the magnesium hydroxide is 99.3%.
Comparative example 1:
The only difference compared to example 1 is that the temperature of the first stage oxidation process in the one-pot process is 50 ℃; other operations and parameters were the same as in example 1.
The results were: in the step (1), the filtration efficiency is 6mg/min cm 2; the recovery rate of iron is 80%, the recovery rate of nickel is 95%, and the recovery rate of manganese is 96%; the recovery rate of chromium is 94%; the loss rate of magnesium is 10%; in the step (2), the total recovery yield of the magnesium hydroxide is 70%, the purity is 98.5%, and the whiteness is 98.6%; the Cr element in the magnesium hydroxide is 0.0334 percent and the sulfur content is 0.2 percent. The filtration performance, product quality such as purity, whiteness, etc. of the process were inferior to those of example 1.
Comparative example 2:
the only difference compared to example 1 is that the temperature of the second stage oxidation treatment process in the one-pot treatment process is 50 ℃; other operations and parameters were the same as in example 1.
The results were: in the step (1), the recovery rate of iron is 98.8%, the recovery rate of nickel is 97.5%, the recovery rate of manganese is 70%, and the recovery rate of chromium is 94%; the loss rate of magnesium is lower than 0.8%; in the step (2), the total yield of magnesium is 79%, the purity is 96.8%, and the whiteness is 89%; the sulfur content is 0.18%, and the Cr element is 0.0771%.
Comparative example 3:
The only difference compared to example 1 is that the second stage oxidation treatment in the one-pot treatment is 90 ℃; other operations and parameters were the same as in example 1.
The results were: in the step (1), the recovery rate of iron is 97.7%, the recovery rate of nickel is 98%, and the recovery rate of manganese is 96%; the recovery rate of chromium is 80 percent, and the loss rate of magnesium is lower than 0.8 percent; in the step (2), the total yield of magnesium is 76%, the purity is 95.4% and the whiteness is 87%; the sulfur content in the magnesium hydroxide is 0.21 percent, and the Cr element is 0.0419 percent.
Comparative example 4:
the only difference compared to example 1 is that the third stage of treatment in the one-pot treatment is 60 ℃; other operations and parameters were the same as in example 1.
The results were: in the step (1), the recovery rate of iron is 97%, the recovery rate of nickel is 96.4%, and the recovery rate of manganese is 94%; the recovery rate of chromium is 95%; the loss rate of magnesium is 3%; in the step (2), the total yield of magnesium is 77%, the purity is 97.5% and the whiteness is 98%; the sulfur content in the magnesium hydroxide was 0.18%.
Comparative example 5:
The only difference compared to example 1 is that during the second stage of the one-pot process of step (1), the pH B is 4.0. Other parameters were the same as in example 1.
The results were: in the step (1), the recovery rate of iron is 98%, the recovery rate of nickel is 97%, the recovery rate of manganese is 73%, and the recovery rate of chromium is 94%; the loss rate of magnesium was 1%.
In the step (2), the total recovery rate of magnesium was 80%, the sulfur content of magnesium hydroxide was 0.2%, the purity of magnesium hydroxide was 96.4%, and the whiteness was 87%.
Comparative example 6:
The only difference compared to example 1 is that during the second stage of the one-pot process of step (1), the pH B is 6.5.
The results were: in the step (1), the recovery rate of iron is 96%, the recovery rate of nickel is 97%, the recovery rate of chromium is 82%, and the recovery rate of manganese is 96%; the loss rate of magnesium was 0.9%.
In the step (2), the total recovery rate of magnesium is 78%; the purity of the magnesium hydroxide is 95.1%, the sulfur content is 0.23%, and the whiteness is 88%.
Claims (17)
1. The method for purifying magnesium by using serpentine normal-pressure sulfuric acid leaching solution in one pot is characterized in that the serpentine normal-pressure sulfuric acid leaching solution is subjected to one-pot three-stage reaction treatment, and then solid-liquid separation is carried out to obtain a purified magnesium solution;
fe, mn, cr and Mg are dissolved in the leaching solution;
The one-pot three-stage reaction process comprises the following steps: regulating the pH A of the leaching solution to 2.0-3.0, and adding an oxidant to perform first-stage oxidation treatment; then regulating and controlling the pH of the system to B -4.5-6, adding an oxidant, and performing second-stage oxidation treatment; regulating and controlling the pH of the system to C -7 to 8, and then carrying out a third-stage reaction;
in the one-pot three-stage reaction process, the temperature of the first-stage oxidation reaction and the second-stage oxidation reaction is 60-80 ℃, and the temperature of the third-stage reaction is 80-90 ℃;
The sulfuric acid concentration in the normal pressure sulfuric acid leaching process is 2-5 mol.L -1; the temperature of the acid leaching process is 80-100 ℃;
The concentration of Fe in the leaching solution is 5-18 g/L; the concentration of Mn is 0.2-0.5 g/L, cr, the concentration is 0.10-0.40 g/L, mg and the concentration is 50-65 g/L;
In the first stage of oxidation reaction, the dosage of the oxidant is 1.2-1.5 times of the theoretical molar quantity of Fe 2+ in the system;
In the second stage of oxidation reaction, the dosage of the oxidant is 1.2-1.5 times of the theoretical molar quantity of Mn (II) oxidation to Mn (IV) oxidation in the system.
2. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 1, wherein the pickling solution further comprises at least one of nickel, cobalt and aluminum.
3. The method for purifying magnesium from serpentine normal pressure sulfuric acid leaching solution in one pot according to claim 2, wherein the concentration of Ni in the leaching solution is 0.20-0.6 g/L; the concentration of Co is 0.01-0.04 g/L; the concentration of Al is 0.2-2 g/L.
4. The method for purifying magnesium by one-pot from serpentine normal-pressure sulfuric acid leaching solution according to claim 1, wherein in the one-pot three-stage treatment process, an alkaline substance is adopted to regulate and control the pH of a system, and the alkaline substance is at least one of magnesium oxide, calcium oxide, alkali metal hydroxide and ammonia water.
5. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 1, wherein the oxidant is at least one of chlorate, oxygen and hydrogen peroxide in a one-pot three-stage treatment process.
6. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 1, wherein the time of the first stage oxidation reaction is 0.5 to 1 hour.
7. The method for purifying magnesium by one-pot serpentine normal-pressure sulfuric acid leaching solution according to claim 1, wherein the time of the second stage oxidation reaction is 0.5-1 h.
8. The method for purifying magnesium by one pot from serpentine normal pressure sulfuric acid leaching solution according to claim 1, wherein the time of the third reaction is 2.0-3.0 h.
9. The method for purifying magnesium by one pot from serpentine normal pressure sulfuric acid leaching solution according to claim 1, wherein a precipitant is added into the magnesium solution to perform a magnesium precipitation reaction, thereby obtaining magnesium hydroxide.
10. The method for purifying magnesium by one pot from serpentine normal pressure sulfuric acid leaching solution according to claim 1, wherein the pH of the magnesium precipitation reaction process and end point is 8.8-9.5.
11. The method for purifying magnesium by one pot from serpentine normal pressure sulfuric acid leaching solution according to claim 1, wherein the temperature of the magnesium precipitation reaction process is 70 ℃ to 80 ℃.
12. The method for purifying magnesium by one-pot serpentine normal-pressure sulfuric acid leaching solution according to claim 1, wherein the time of the magnesium precipitation reaction is 1-2 hours.
13. The method for purifying magnesium from serpentine normal pressure sulfuric acid leaching solution in one pot according to claim 9, wherein the magnesium hydroxide is aged in an alkali solution, and then subjected to solid-liquid separation, washing and obtaining purified magnesium hydroxide.
14. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 13, wherein the alkaline solution is an aqueous solution of alkali metal hydroxide.
15. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 14, wherein the concentration of solute in the alkaline solution is 0.2 mol-L -1～0.5mol·L-1.
16. The method for purifying magnesium from serpentine atmospheric sulfuric acid leach solution in one pot of claim 13, wherein the aging temperature is 70 ℃ to 80 ℃.
17. The method for purifying magnesium from serpentine atmospheric sulfuric acid leaching solution in one pot according to claim 13, wherein the aging time is 60 to 120 min.
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