CN115821063A - Method for purifying magnesium from serpentine - Google Patents
Method for purifying magnesium from serpentine Download PDFInfo
- Publication number
- CN115821063A CN115821063A CN202211581459.6A CN202211581459A CN115821063A CN 115821063 A CN115821063 A CN 115821063A CN 202211581459 A CN202211581459 A CN 202211581459A CN 115821063 A CN115821063 A CN 115821063A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- serpentine
- resin
- acid
- purifying
- 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.)
- Pending
Links
- 239000011777 magnesium Substances 0.000 title claims abstract description 100
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 91
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 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 38
- 238000000034 method Methods 0.000 title claims abstract description 30
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000011347 resin Substances 0.000 claims abstract description 39
- 229920005989 resin Polymers 0.000 claims abstract description 39
- 238000001179 sorption measurement Methods 0.000 claims abstract description 39
- 239000002253 acid Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000010941 cobalt Substances 0.000 claims abstract description 29
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 29
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 29
- 238000002386 leaching Methods 0.000 claims abstract description 28
- 239000011572 manganese Substances 0.000 claims abstract description 27
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 23
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 15
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 13
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 12
- 238000000746 purification Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- 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 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000008267 milk Substances 0.000 claims description 4
- 210000004080 milk Anatomy 0.000 claims description 4
- 235000013336 milk Nutrition 0.000 claims description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 3
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 3
- 239000004571 lime Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 150000004965 peroxy acids Chemical class 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 14
- 239000011651 chromium Substances 0.000 abstract description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 229910052742 iron Inorganic materials 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 description 20
- 238000005406 washing Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 229910020632 Co Mn Inorganic materials 0.000 description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 4
- 229910001626 barium chloride Inorganic materials 0.000 description 4
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 4
- 235000019341 magnesium sulphate Nutrition 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000008234 soft water Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 238000013016 damping Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005580 one pot reaction Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 229910052604 silicate mineral Inorganic materials 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052898 antigorite Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052620 chrysotile Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052899 lizardite Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of magnesium ore treatment, and particularly relates to a method for purifying magnesium from serpentine. The method for purifying magnesium by using serpentine provided by the invention comprises the following steps: (1) Grinding serpentine, then carrying out acid leaching, and filtering to obtain a leaching solution; (2) Adding a neutralizing agent into the leachate obtained in the step (1), and performing solid-liquid separation to obtain a neutralized liquid; (3) And (3) introducing the neutralized liquid obtained in the step (2) into an ion exchange resin adsorption system for adsorption treatment to obtain adsorbed resin and an adsorbed high-magnesium solution. The method not only can separate iron, aluminum and chromium in the leachate, but also can effectively realize the separation of nickel, cobalt, manganese and magnesium in the leachate, and realize the deep purification of the high-magnesium solution.
Description
Technical Field
The invention belongs to the technical field of magnesium ore treatment, and particularly relates to a method for purifying magnesium from serpentine.
Background
Magnesium is one of the lightest structural metal materials, and has the advantages of high specific strength and specific rigidity, good damping property and machinability, easy recovery and the like. Magnesium alloy is applied to the automobile industry at home and abroad to reduce weight, save energy, reduce pollution and improve environment. Compared with plastics, the magnesium alloy has the advantages of light weight, high specific strength, good vibration damping property, good thermal fatigue property, difficult aging, good thermal conductivity, strong electromagnetic shielding capability, very good die casting process performance, easy recovery and the like, and is a new generation of high-performance structural material for replacing steel, aluminum alloy and engineering plastics.
Serpentine, which is a corrosion product of olivine, is a generic name for hydrous magnesium-rich silicate minerals of general formula Mg 3 Si 2 O 5 (OH) 4 The structure is 1:1 layered silicate mineral formed by combining silicon-oxygen tetrahedron and magnesium hydroxide octahedron. Serpentine ore contains silica of 34% or more, magnesia of 36% or more, iron oxide of 8% or more, calcium oxide of about 0.7% or so and other minor components, and is a valuable mineral resource, in which the contents of magnesia and silica are more than 1/3 of the total weight of the ore, and if these serpentines can be properly treated, not only the problem of waste accumulation can be solved, but also metal magnesium and the like with wide application can be obtained.
Disclosure of Invention
The present invention is based on the discovery and recognition by the inventors of the following facts and problems:
the prior patent application CN113548683A discloses a method for preparing magnesium-based and silicon-based materials by utilizing serpentine Dan Mofei, which comprises the steps of leaching with acid, primarily separating magnesium and silicon, and respectively crystallizing, redissolving, precipitating and the like a magnesium-containing filtrate to obtain a high-grade magnesium-based material.
The prior patent application CN114686702A provides a method for purifying magnesium from a serpentine Dan Changya sulfuric acid leaching solution in one pot, and the leaching solution subjected to normal-pressure acid leaching of the serpentine Dan Liusuan is subjected to one-pot three-section reaction treatment, and then solid-liquid separation is carried out to obtain a purified magnesium solution.
In the prior art, magnesium metal is prepared by processing serpentine through an acid leaching method, magnesium and other metals enter a leaching solution after the acid leaching treatment, a neutralizing agent is added to adjust the pH value, so that most of iron, aluminum and chromium can be separated, but the separation of nickel, cobalt and manganese is difficult to realize, and the purity of the product can be influenced when the magnesium is used for preparing a subsequent magnesium product.
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, the embodiment of the invention provides a method for purifying magnesium from serpentine, which can effectively realize the separation of nickel, cobalt, manganese and magnesium in the serpentine leachate and realize the deep purification of a high-magnesium solution.
The method for purifying magnesium by using serpentine comprises the following steps:
(1) Grinding serpentine, then carrying out acid leaching, and filtering to obtain a leaching solution;
(2) Adding a neutralizing agent into the leachate obtained in the step (1), and performing solid-liquid separation to obtain a neutralized liquid;
(3) And (3) introducing the neutralized liquid obtained in the step (2) into an ion exchange resin adsorption system for adsorption treatment to obtain adsorbed resin and an adsorbed high-magnesium solution.
The method for preparing the serpentine Dan Dichun magnesium provided by the embodiment of the invention has the advantages and technical effects that 1, in the embodiment of the invention, a neutralizing agent is added into a leaching solution, and iron, aluminum and chromium are precipitated by adjusting the pH value of the leaching solution so as to be effectively separated; 2. in the embodiment of the invention, the effective separation of nickel, cobalt, manganese and magnesium can be realized through an ion exchange resin adsorption system, and the deep purification of a high-magnesium solution is realized; 3. in the embodiment of the invention, the method is simple and easy to operate, and is convenient to popularize and apply in industrial production.
In some embodiments, in the step (1), the acid used in the acid leaching is any one of sulfuric acid and hydrochloric acid.
In some embodiments, in the step (2), the neutralizing agent includes at least one of sodium hydroxide, lime milk, and magnesium oxide emulsion, and the neutralizing agent is added in an amount to adjust the pH of the leachate to 3 to 5.
In some embodiments, in step (3), the ion exchange resin is an IDA resin.
In some embodiments, the adsorption system is a single column or a multi-column series system.
In some embodiments, the column passing rate of the adsorption treatment is 1-3BV/h.
In some embodiments, in the step (3), dilute acid is introduced into the resin after adsorption to wash the co-adsorbed magnesium, so as to obtain a resin after washing and a magnesium-rich washing liquid, and preferably, the magnesium-rich washing liquid is returned to the step (1) for acid leaching.
In some embodiments, the dilute acid comprises 15-20g/L sulfuric acid or 10-15g/L hydrochloric acid.
In some embodiments, high acid is introduced into the washed resin to desorb nickel, cobalt and manganese, so as to obtain a desorbed resin and a nickel, cobalt and manganese mixed solution.
In some embodiments, the high acid comprises sulfuric acid at a concentration of no less than 50g/L or hydrochloric acid at a concentration of no less than 37 g/L.
Detailed Description
The following detailed description of embodiments of the invention is intended to be illustrative, and not to be construed as limiting the invention.
The method for purifying magnesium by using serpentine comprises the following steps:
(1) Grinding serpentine, then carrying out acid leaching, and filtering to obtain a leaching solution;
(2) Adding a neutralizing agent into the leachate obtained in the step (1), and performing solid-liquid separation to obtain a neutralized liquid;
(3) And (3) introducing the neutralized liquid obtained in the step (2) into an ion exchange resin adsorption system for adsorption treatment to obtain adsorbed resin and an adsorbed high-magnesium solution.
According to the method for purifying magnesium by using serpentine, provided by the embodiment of the invention, a neutralizer is added into the leachate, and the pH value of the leachate is adjusted to enable iron, aluminum and chromium to generate precipitates so as to be effectively separated; the effective separation of nickel, cobalt, manganese and magnesium can be realized through an ion exchange resin adsorption system, and the deep purification of a high-magnesium solution is realized; the method is simple and easy to operate, and is convenient to popularize and apply in industrial production.
In some embodiments, preferably, in the step (1), the acid used for acid leaching is any one of sulfuric acid and hydrochloric acid. Further preferably, when the acid is hydrochloric acid, magnesium sulfate and barium chloride are sequentially added into the adsorbed high-magnesium solution, and the deeply-purified magnesium solution is obtained through solid-liquid separation; wherein magnesium sulfate is added equimolar to the calcium ion content and barium chloride is added equimolar to the sulfate ion content. In the embodiment of the invention, the hydrochloric acid or the sulfuric acid is used for fully dissolving the metal in the serpentine, thereby being beneficial to improving the purity of magnesium; when the acid is hydrochloric acid, magnesium sulfate and barium chloride are added in sequence to respectively precipitate and remove calcium and sulfate radicals in the liquid phase, so as to obtain the deeply-purified magnesium liquid.
In some embodiments, preferably, in the step (2), the neutralizer comprises at least one of sodium hydroxide, lime milk and magnesium oxide emulsion, and the neutralizer is added in an amount to adjust the pH of the leachate to 3-5. In the embodiment of the invention, the alkaline neutralizing agent is added into the leachate to precipitate and separate iron, aluminum and chromium, and the addition amount of the neutralizing agent is further optimized, so that iron, aluminum and chromium can be sufficiently removed, and new impurity elements are not introduced into the leachate.
In some embodiments, preferably, in the step (3), the ion exchange resin is an IDA resin. Further preferably, the adsorption system is a single column or a multi-column series system. Still preferably, the column passing rate of the adsorption treatment is 1-3BV/h. In the embodiment of the invention, the type of the ion exchange resin is optimized, which is beneficial to selectively adsorbing nickel, cobalt and manganese in the neutralized liquid, and further limits the adsorption column passing rate, so that the adsorption of nickel, cobalt and manganese is carried out more fully, the effective separation of the nickel, cobalt and manganese is realized, and the purity of the magnesium solution is further improved.
In some embodiments, preferably, in the step (3), dilute acid is introduced into the resin after adsorption to wash the co-adsorbed magnesium, so as to obtain a resin after washing and a magnesium-rich washing liquid, and preferably, the magnesium-rich washing liquid is returned to the step (1) for acid leaching. Further preferably, the dilute acid comprises 15-20g/L sulfuric acid or 10-15g/L hydrochloric acid. In the embodiment of the invention, the magnesium adsorbed in the adsorbed resin is washed by dilute acid to obtain magnesium-rich washing liquid, and the magnesium-rich washing liquid is returned to the step (1) for acid leaching treatment, so that the recovery rate of magnesium can be higher than 95%.
In some embodiments, preferably, high acid is introduced into the washed resin to desorb nickel, cobalt and manganese, so as to obtain a desorbed resin and a nickel, cobalt and manganese mixed solution. Further preferably, the high acid comprises sulfuric acid having a concentration of not less than 50g/L or hydrochloric acid having a concentration of not less than 37 g/L. In the embodiment of the invention, the washed resin is desorbed by using high acid so as to desorb nickel, cobalt and manganese from the resin, and the nickel, cobalt and manganese are recovered.
In some embodiments, preferably, the neutralizer is added into the nickel, cobalt and manganese mixed solution for precipitation or extraction separation, and then the nickel, cobalt and manganese mixed solution is respectively recycled. Further preferably, soft water is introduced into the desorbed resin to wash the resin. In the embodiment of the invention, nickel, cobalt and manganese are recycled, so that the utilization value of serpentine is improved. In addition, the desorbed resin is washed by soft water, and the residual acid can be washed off and then returned to the adsorption step in the step (2) for repeated use, so that the cost of industrial production is reduced.
The present invention will be described in detail with reference to specific examples.
Example 1
(1) The serpentine is ground and then leached by hydrochloric acid, and the components of the leaching solution are shown in the following table 1:
TABLE 1 Serpentine Dan Liusuan leachate composition (mg/L)
| Mg | Co | Mn | Ni | Ca | Fe | Al | Cr |
| 55514 | 32.62 | 134.95 | 266.02 | 3497.5 | 4523 | 3306 | 2189 |
(2) Adding magnesium oxide emulsion into the obtained leachate, adjusting pH =4.2 to precipitate iron, aluminum and chromium, and performing solid-liquid separation to obtain a neutralized liquid, wherein the components of the neutralized liquid are shown in Table 2 below.
TABLE 2 ingredients of neutralized liquid (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 55510 | 32.62 | 134.95 | 266.02 | 3497.5 |
(3) And (3) introducing the neutralized liquid into a 3-stage IDA ion exchange resin adsorption system connected in series, removing nickel, cobalt, manganese and the like at an adsorption column passing rate of 1BV/h to obtain a high-magnesium solution after adsorption, wherein the components of the high-magnesium solution after adsorption are shown in the following table 3.
TABLE 3 composition of post-adsorption solution (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 55503 | ＜0.1 | ＜0.1 | ＜0.1 | 3495 |
(4) Adding magnesium sulfate with the same molar amount as that of calcium ions into the adsorbed high-magnesium solution, adding barium chloride with the same molar amount as that of sulfate ions, and respectively precipitating to remove calcium and sulfate in the liquid phase to obtain a deeply-purified magnesium solution, wherein the components of the deeply-purified magnesium solution are shown in the following table 4.
TABLE 4 deep purification of magnesium solution composition (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 54518 | ＜0.1 | ＜0.1 | ＜0.1 | ＜0.1 |
(5) And (3) introducing 10g/L of dilute hydrochloric acid into the resin after adsorption to wash the co-adsorbed magnesium to obtain the resin after washing and a magnesium-rich washing liquid, wherein the components of the magnesium-rich washing liquid are shown in the following table 5, and returning to the step (1) of serpentine acid leaching process.
TABLE 5 magnesium-rich post-wash liquor composition (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 35 | 8 | 12 | 3 | ＜0.1 |
(6) And (3) introducing 40g/L hydrochloric acid into the washed resin for desorption to obtain a mixed solution of the desorbed resin and the nickel, cobalt and manganese, wherein the components of the mixed solution of the nickel, cobalt and manganese are shown in the following table 6.
TABLE 6 composition (mg/L) of mixed solution of nickel, cobalt and manganese
| Co | Mn | Ni |
| 301 | 1220 | 2538 |
(7) And introducing soft water into the resolved resin to wash away residual acid so as to return to the adsorption process for repeated use.
(8) The mixed solution of nickel, cobalt and manganese is extracted by P204 and P507 in sequence and is recycled after separation.
In this example, the calculated recovery rate of magnesium was 98.2%, the recovery rate of Ni was 98.1%, the recovery rate of Co was 99.0%, and the recovery rate of Mn was 95.4%.
Example 2
This example was the same as example 1 except that a single-column adsorption system was used in step (3), the adsorption column rate was 3BV/h, and nickel, cobalt, manganese, etc. were removed by adsorption to obtain a high-magnesium solution after adsorption, the composition of which is shown in table 7 below.
TABLE 7 composition of post-adsorption solution (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 55481 | ＜0.1 | ＜0.1 | ＜0.1 | 3276 |
In this example, the calculated recovery rate of magnesium was 99.9%, the recovery rate of Ni was 96%, the recovery rate of Co was 97%, and the recovery rate of Mn was 84%.
Example 3
This example was the same as example 1 except that 15g/L of dilute hydrochloric acid was passed through the resin after adsorption in step (5) to wash the co-adsorbed magnesium, thereby obtaining a resin after washing and a magnesium-rich washed solution, and the magnesium-rich washed solution components were as shown in Table 8 below, and the process was returned to the step (1) of serpentine acid leaching.
TABLE 8 magnesium-rich post-wash liquor composition (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 67 | 18 | 44 | 25 | ＜0.1 |
In this example, the calculated recovery rate of magnesium was 97.3%, the recovery rate of Ni was 97%, the recovery rate of Co was 98%, and the recovery rate of Mn was 88%.
Example 4
This example was the same as example 1 except that 25g/L of dilute hydrochloric acid was passed through the resin after adsorption in step (5) to wash the co-adsorbed magnesium, thereby obtaining a resin after washing and a magnesium-rich washed solution, the components of which are shown in Table 9 below, and the magnesium-rich washed solution was returned to the step (1) of the serpentine acid leaching step.
TABLE 9 magnesium-rich post-wash liquor composition (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 542 | 43 | 85 | 34 | ＜0.1 |
In this example, the calculated recovery rates for magnesium were 95%, ni 60%, co 58% and Mn 43%.
Example 5
This example is the same as example 1 except that step (5) was omitted and 40g/L hydrochloric acid was directly introduced into the resin after adsorption to effect desorption, thereby obtaining a mixed solution of the resin after desorption and nickel, cobalt and manganese, the components of which are shown in Table 10 below.
TABLE 10 composition (mg/L) of mixed solution of nickel, cobalt, manganese
| Co | Mn | Ni | Mg |
| 301 | 1220 | 2538 | 1304 |
In this example, the calculated recovery rate of magnesium was 73%, the recovery rate of Ni was 98.1%, the recovery rate of Co was 99.0%, and the recovery rate of Mn was 95.4%.
Comparative example 1
This comparative example is identical to the procedure of example 1 except that the resin of the ion exchange resin used in step (3) is an anionic resin, nickel, cobalt, manganese, etc. are removed to obtain a high magnesium solution after adsorption, the composition of which is shown in table 11 below.
TABLE 11 liquid composition after adsorption (mg/L)
| Mg | Co | Mn | Ni | Ca |
| 55510 | 32.62 | 134.95 | 266.02 | 3497.5 |
In the comparative example, the anion resin was used as the ion exchange resin, and the nickel, cobalt, manganese and magnesium in the neutralized solution could not be separated, and the deep purification of the high-magnesium solution could not be achieved.
In the present disclosure, the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples" and the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although the above embodiments have been shown and described, it should be understood that they are exemplary and should not be construed as limiting the present invention, and that many changes, modifications, substitutions and alterations to the above embodiments may be made by those of ordinary skill in the art without departing from the scope of the present invention.
Claims (10)
1. A method for purifying magnesium from serpentine is characterized by comprising the following steps:
(1) Grinding serpentine, then carrying out acid leaching, and filtering to obtain a leaching solution;
(2) Adding a neutralizing agent into the leachate obtained in the step (1), and performing solid-liquid separation to obtain a neutralized liquid;
(3) And (3) introducing the neutralized liquid obtained in the step (2) into an ion exchange resin adsorption system for adsorption treatment to obtain adsorbed resin and an adsorbed high-magnesium solution.
2. The method for purifying magnesium from serpentine as recited in claim 1, wherein in the step (1), the acid used in the acid leaching is any one of sulfuric acid and hydrochloric acid.
3. The method for purifying magnesium from serpentine as recited in claim 1, wherein the neutralizing agent in the step (2) comprises at least one of sodium hydroxide, lime milk, and magnesium oxide milk, and the neutralizing agent is added in an amount to adjust the pH of the leachate to 3 to 5.
4. The method for purifying magnesium using serpentine as claimed in claim 1, wherein said ion exchange resin in step (3) is IDA resin.
5. The method for purifying magnesium using serpentine according to claim 1 or 4, wherein the adsorption system is a single column or a multi-column series system.
6. The method for purifying magnesium with serpentine according to claim 1 or 4, wherein the column passing rate of the adsorption treatment is 1 to 3BV/h.
7. The method for purifying magnesium from serpentine as recited in claim 1 or 4, wherein in the step (3), dilute acid is introduced into the resin after adsorption to wash the co-adsorbed magnesium, thereby obtaining a washed resin and a magnesium-rich washed liquid, and preferably, the magnesium-rich washed liquid is returned to the step (1) for acid leaching.
8. The method for purifying magnesium from serpentine as recited in claim 7, wherein said dilute acid comprises 15-20g/L sulfuric acid or 10-15g/L hydrochloric acid.
9. The method for producing the serpentine Dan Dichun magnesium as claimed in claim 7 or 8, wherein a peracid is introduced into the washed resin to desorb nickel, cobalt and manganese, and a desorbed resin and a mixed solution of nickel, cobalt and manganese are obtained.
10. The method of serpentine purification of magnesium according to claim 9, wherein the high acid includes sulfuric acid having a concentration of not less than 50g/L or hydrochloric acid having a concentration of not less than 37 g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211581459.6A CN115821063A (en) | 2022-12-09 | 2022-12-09 | Method for purifying magnesium from serpentine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211581459.6A CN115821063A (en) | 2022-12-09 | 2022-12-09 | Method for purifying magnesium from serpentine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115821063A true CN115821063A (en) | 2023-03-21 |
Family
ID=85546113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211581459.6A Pending CN115821063A (en) | 2022-12-09 | 2022-12-09 | Method for purifying magnesium from serpentine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115821063A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020006370A1 (en) * | 1999-11-03 | 2002-01-17 | J. Carlos Arroyo | Method for leaching nickeliferous laterite ores |
| CN101456565A (en) * | 2009-01-09 | 2009-06-17 | 昆明理工大学 | Method for preparing magnesium hydrate nano powder by active acid leaching nickel-containing serpentine |
| CN113249571A (en) * | 2021-05-28 | 2021-08-13 | 中国恩菲工程技术有限公司 | Method for recovering nickel and cobalt from laterite-nickel ore by resin adsorption method |
| CN113293293A (en) * | 2021-05-26 | 2021-08-24 | 中国恩菲工程技术有限公司 | Method for recovering nickel and cobalt from laterite-nickel ore by resin adsorption method |
| CN114686702A (en) * | 2022-04-06 | 2022-07-01 | 北京华夏建龙矿业科技有限公司 | Method for purifying magnesium from serpentine normal-pressure sulfuric acid leaching solution in one pot |
-
2022
- 2022-12-09 CN CN202211581459.6A patent/CN115821063A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020006370A1 (en) * | 1999-11-03 | 2002-01-17 | J. Carlos Arroyo | Method for leaching nickeliferous laterite ores |
| CN101456565A (en) * | 2009-01-09 | 2009-06-17 | 昆明理工大学 | Method for preparing magnesium hydrate nano powder by active acid leaching nickel-containing serpentine |
| CN113293293A (en) * | 2021-05-26 | 2021-08-24 | 中国恩菲工程技术有限公司 | Method for recovering nickel and cobalt from laterite-nickel ore by resin adsorption method |
| CN113249571A (en) * | 2021-05-28 | 2021-08-13 | 中国恩菲工程技术有限公司 | Method for recovering nickel and cobalt from laterite-nickel ore by resin adsorption method |
| CN114686702A (en) * | 2022-04-06 | 2022-07-01 | 北京华夏建龙矿业科技有限公司 | Method for purifying magnesium from serpentine normal-pressure sulfuric acid leaching solution in one pot |
Non-Patent Citations (2)
| Title |
|---|
| A. CHAREWICZ;高世章;: "波兰蛇纹石矿的水冶工艺", 矿产综合利用, no. 02, pages 27 - 30 * |
| 蒋开喜主编: "《加压湿法冶金》", 31 January 2016, 冶金工业出版社, pages: 526 - 527 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101870461B (en) | Method for treating waste liquid containing magnesium | |
| CN108298581B (en) | System for extracting vanadium from leaching solution containing vanadium, chromium and silicon and preparing vanadium pentoxide and treatment method thereof | |
| WO2015161660A1 (en) | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon | |
| CN109234526B (en) | Treatment method of laterite-nickel ore | |
| AU2019350100A1 (en) | Method for treating low-magnesium limonite type laterite nickel ore | |
| CN102660687A (en) | Method for recycling heavy metal resources of stainless steel pickling waste water neutralization sludge | |
| WO2015161659A1 (en) | Method for simultaneously preparing high-purity vanadium and heteropolyacid catalyst | |
| CN103993172B (en) | The processing method of iron-containing liquor | |
| CN110846500A (en) | Comprehensive recycling method for cobalt smelting ammonia nitrogen wastewater | |
| CN115341105A (en) | Washing process method for improving nickel-cobalt separation rate of nickel adsorption resin | |
| CN112593080A (en) | Method for treating laterite-nickel ore by combination of pyrogenic process and wet process | |
| CN105753219A (en) | Process for purifying and treating vanadium-containing wastewater in advanced manner and process for recycling vanadium and chromium | |
| CN102345020A (en) | Method for separating and recycling vanadium and chromium in solution | |
| CN111498917B (en) | Treatment method of laterite-nickel ore | |
| CN112142073A (en) | Method for resource utilization of chromium-containing sodium bisulfate | |
| CN115821063A (en) | Method for purifying magnesium from serpentine | |
| CN111235390A (en) | Resource recycling method for pyrolusite leaching slag | |
| CN101880772B (en) | Method for recycling magnesium from magnesium-containing waste solution | |
| CN104030510A (en) | Method for recycling acid and heavy metal in gold smelting acid wastewater | |
| CN110819800A (en) | Method for recovering metal from laterite-nickel ore leaching solution by resin | |
| CN113088693B (en) | Method for recovering vanadium, nickel and aluminum from sulfuric acid slaking leachate | |
| CN112391537B (en) | Method for extracting vanadium by using hydrochloric acid, sulfuric acid and vanadium-containing high-calcium high-phosphorus slag | |
| CN110983039B (en) | Method for removing impurities in pyrolusite sulfur dioxide leaching solution | |
| CN110777270B (en) | Method for selective flotation separation of molybdenum-rhenium acid radicals in alkali immersion liquid | |
| CN105217669A (en) | A kind of method reclaiming nickel and aluminium from waste nickel catalyst |
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 |