26results about "Scandium oxides/hydroxides" patented technology

The application discloses a kind of red mud gradient depth purification-rare earth-radioactivity synergistic target purification method, by " hierarchical pretreatment and microwave modification→three-stage gradient dealkalization→rare earth-radioactivity synergistic target purification→full quantization recycling" four-stage integrated process, realize red mud harmless and high-value utilization.The three-stage gradient dealkalization uses microwave-CO2-biological synergic system, after dealkalization pH≤8.0, Na2O content<1%;Rare earth-radioactivity purification is extracted by HDES and coupled with multi-ligand magnetic material system, light rare earth recovery rate≥95%, middle heavy / rare earth recovery rate≥90%, U / Th removal rate≥95%;Full quantization recycling realizes red mud total utilization rate≥98.5%, wastewater reuse rate≥95%, every ton of red mud fixed CO2≥0.2 tons.The application is suitable for various high-alkali, containing radioactive and rare earth red mud treatment, with environmental benefits and economic benefits.

This application belongs to the field of rare earth element recovery technology and discloses a method for recovering scandium oxide from scandium-oxalic acid-containing wastewater. The method involves first mixing a phosphoric acid extractant and a solvent oil to obtain a first mixture. The scandium-oxalic acid-containing wastewater is then filtered. The first mixture is mixed with the filtered scandium-oxalic acid-containing wastewater at a volume ratio of organic phase to aqueous phase of 1:20-30. The mixture is then subjected to countercurrent extraction, stirring, and clarification to obtain a second mixture. Subsequently, the organic phase in the second mixture is back-extracted using an alkaline solution containing ethanol to obtain scandium hydroxide. Scandium hydroxide is then dissolved in hydrochloric acid solution, and finally, scandium is precipitated using oxalic acid solution to obtain scandium oxalate. The scandium oxalate is then calcined at high temperature to obtain scandium oxide. Through the above design, the scandium oxide recovery rate of this application reaches 97.9%, and the scandium oxide recovered by this method has a purity of not less than 99.5%.

The invention relates to a process for producing scandium oxide by comprehensively recovering bauxite. According to the method, scandium compounds in the red mud are activated through bubbling treatment, the pH value of a liquid phase is smaller than or equal to 10.5, after multi-stage filtration, insoluble residues are leached through a sodium carbonate-sodium bicarbonate solution, and a scandium-containing sodium carbonate-sodium bicarbonate solution is obtained; after filtering the obtained solution, mixing a scandium-containing alkaline aluminate solution with a scandium-containing sodium carbonate-sodium bicarbonate solution to prepare a scandium-containing hydrolysis concentrate; carrying out two-stage sulfuric acid leaching on the filtered scandium-containing hydrolysis concentrate; the scandium-containing sulfuric acid solutions obtained after two-stage leaching are mixed, alkali is added to adjust the pH to 4.5-5.5, and scandium sulfate without impurity elements is precipitated; then treating with caustic alkali until the pH is not more than 5.6, and carrying out selective precipitation of scandium; treating scandium sulfate with a sulfuric acid solution to obtain basic scandium sulfate; treating the obtained basic scandium sulfate with oxalic acid to convert the basic scandium sulfate into scandium oxalate; filtering the obtained scandium oxalate precipitate; and calcining scandium oxalate to remove carbon and obtain scandium oxide, wherein the content of Sc2O3 in the calcined product is at least 99.0 mass percent.

The invention provides Sc2O3 porous aerogel as well as a preparation method and application thereof. According to the method, ScCl3. 6H2O is selected as a scandium source and is non-toxic, and the reaction activity of the ScCl3. 6H2O is controllable compared with that of organic metal alkoxide. In addition, compared with supercritical drying and freeze drying, the normal-pressure drying method for graded drying is lower in cost and higher in safety, and graded drying can effectively protect the nano structure and reduce cracking and collapse of the sample as much as possible. In addition, the scandium oxide aerogel is synthesized for the first time, and the product is high in porosity, large in specific surface area and good in heat insulation performance and has positive significance in application of aerogel materials in various fields.

The present application relates to the field of adsorption separation technology, and particularly relates to a selective removal agent, a preparation method and application thereof. The selective removal agent contains calcium-scan double-metal layered hydroxide and diatomite, and the mass ratio of diatomite to calcium-scan double-metal layered hydroxide is greater than or equal to 0.14. The chemical formula of the calcium-scan double-metal layered hydroxide is [Ca x Sc(OH) y ]OH, x is 2-3, and y is 6-8. The selective removal agent provided in the present application has good selectivity to heat-stable salts and hydrogen phosphate, the selectivity adsorption ratio of hydrogen phosphate to heat-stable salt anions is greater than 6000, efficient separation of heat-stable salts and hydrogen phosphate can be achieved, the stability is good, the working cycle can be prolonged, and the selective removal agent is suitable for industrial popularization.

The application belongs to the technical field of scandium separation and purification, and particularly relates to a method for separating and purifying scandium from crude nickel-cobalt hydroxide, which comprises the following steps: using 0.1-0.5 mol / L dilute sulfuric acid to leach the crude nickel-cobalt hydroxide, and filtering to obtain a scandium-containing leaching solution, wherein the ratio of the dilute sulfuric acid to the crude nickel-cobalt hydroxide is (3-5) mL:1 g, and the molar ratio of sulfuric acid to scandium is (3-5):1; using an extractant comprising Cyanex572 and Aliquat336 to treat the scandium-containing leaching solution to obtain a scandium-containing organic phase; using an oxalic acid solution to back-extract the scandium-containing organic phase to obtain scandium oxalate precipitation; and calcining the scandium oxalate precipitation to obtain scandium oxide. The technical scheme adopts a selective leaching process to realize efficient separation of scandium from main metals nickel and cobalt at the front end, has low reagent consumption, a short process, and great cost advantages; a new type of synergistic extraction technology is adopted, which has super-high selectivity and extraction capacity for scandium, the prepared scandium oxide has a purity of greater than or equal to 96%, and the scandium recovery rate is greater than or equal to 89%.

The invention relates to technology for the comprehensive processing of bauxites, specifically red mud, to obtain scandium oxide. The present method includes filtering red mud, reslurrying the red mud cake, sparging the mud slurry, and subjecting same to carbonate-bicarbonate leaching and filtration to obtain a scandium-containing product solution. The obtained solution is mixed with an alkali-aluminate solution to obtain a precipitate which is filtered and releached to obtain a scandium-containing alkali-aluminate solution and an insoluble precipitate. The precipitate is releached to obtain a scandium-containing sodium carbonate-bicarbonate solution. The scandium-containing solutions are mixed to obtain a concentrate from which scandium is extracted by two-stage sulphuric acid leaching to obtain basic scandium sulphate which is then treated with oxalic acid. The obtained scandium oxalate precipitate is filtered and calcined to obtain scandium oxide. The invention makes it possible to achieve high scandium extraction.

The invention belongs to the technical field of scandium separation and purification, and particularly relates to a method for separating and purifying scandium from crude nickel cobalt hydroxide, which comprises the following steps: using 0.1-0.5 mol / L dilute sulphuric acid to leach crude nickel cobalt hydroxide, filtering to obtain scandium-containing leachate, the ratio of dilute sulphuric acid to crude nickel cobalt hydroxide is (3-5) mL: 1g, and the molar ratio of sulphuric acid to scandium is (3-5): 1; carrying out scandium extraction treatment on the scandium-containing leachate by using an extraction agent comprising Cyanex572 and Aliquat 336 to obtain a scandium-containing organic phase; carrying out reverse extraction on the scandium-containing organic phase by using an oxalic acid solution to obtain scandium oxalate precipitate; and calcining the scandium oxalate precipitate to obtain scandium oxide. According to the technical scheme, the selective leaching process is adopted, efficient separation of scandium and main metal nickel and cobalt is achieved at the front end, reagent consumption is low, the process is short, and the large cost advantage is achieved; a novel synergistic extraction technology is adopted, ultrahigh selectivity and extraction capacity on scandium are achieved, the purity of prepared scandium oxide is larger than or equal to 96%, and the recovery rate of scandium is larger than or equal to 89%.

The application discloses a method for separating niobium oxide and scandium oxide from Baiyunebo tailings, which comprises the following steps: normal-pressure acid leaching, precipitating rare earth complex salt by adopting sodium sulfate on the leaching solution, removing iron and titanium in the organic phase by using hydrochloric acid-hydrogen peroxide washing liquid, and obtaining the co-precipitation alkali cake of niobium hydroxide and scandium hydroxide by back-extracting the organic phase by sodium hydroxide, and the alkali cake is reacted with a mixed solution of oxalic acid and ammonia water, so that three products of rare earth sulfate complex salt, niobium oxide and scandium oxide can be obtained.

The present invention relates to a process for treating residues, in particular solid residues, of the alumina refining industry, i.e. for treating red mud, comprising the following steps: - reductive fusion of the red mud or pre-reduction and subsequent treatment, with the production of a scoria enriched in aluminium, titanium and scandium and with a low content of iron; - digestion of said scoria with sulphuric acid, at a concentration of 6 - 18.5M and temperature of 50-250°C, for a duration of 0.5-2h, with the conversion of the aluminium, titanium and scandium oxides into water-soluble sulphates and the obtainment of an aqueous solution of aluminium, titanium and scandium sulphates and a solid residue; - leaching with water of the solid residue obtained from the digestion, with a temperature in the range of 25-75°C, for a duration of 5-30min and with a liquid / solid ratio of from 5 / 1 to 20 / 1, calculated relative to the initial mass of red mud subjected to acid digestion, with a further solubilisation of aluminium, titanium and scandium in said solution and separation of a solid residue; - addition to said solution, after leaching, of ammonium sulphate in an amount equal to 1 -1.5 times the stoichiometric amount relative to the aluminium, with a reaction time of 5-60 minutes, precipitation of aluminium ammonium sulphate and the separation thereof from the residual solution; - purification of said aluminium ammonium sulphate, by means of a plurality of washing cycles with hot water and filtration.

The application discloses a method for recovering scandium and zirconium in scandia-stabilized zirconia ceramics, and belongs to the technical field of ceramic waste resource recovery. The method comprises the following steps: performing alkali leaching pretreatment on scandia-stabilized zirconia ceramic powder to obtain mixed slurry, introducing the mixed slurry into carbon dioxide to perform carbonation selective leaching of scandium, and performing liquid-solid separation to obtain a scandium-containing leaching solution and leaching residue; performing alkali leaching of the leaching residue to extract zirconium, and performing liquid-solid separation to obtain a zirconium-containing leaching solution and tailings. The method realizes separate leaching and extraction of scandium and zirconium in ceramics by performing carbonation after alkali leaching pretreatment to leach scandium, and leaving zirconium in the residue and extracting zirconium components through secondary alkali leaching, so that the recovery rate of scandium and zirconium can be improved, and the product purity can be improved.

Despite the abundance of scandium, its commercial applications continue to be limited by the absence of reliable, secure, stable and long-term production. The subject-matter disclosed herein provides for a method for extracting Rare Earth Elements (REE), scandium and / or Rare-Earth Oxides (REO) from ore and mineral concentrates, the method comprising: providing Rare Earth Elements (REE) and / or scandium bearing feedstock; a high-pressure caustic (HPC) leaching step, comprising leaching the feedstock in an alkali solution at a first temperature for a target period of time and at a given pressure to produce a leachate slurry; extracting a solid residue from the leachate slurry; leaching of the solid residue in a mineral acid to form a primary leach solution; extracting scandium and / or REE from the primary leach solution; and / or precipitating REE remaining in the raffinate to form a mixed REE-carbonate to thereby facilitate the extraction of REO.

The application discloses a kind of pre-transition metal oxide nanoparticles and its preparation method and oxygen reduction synthesis hydrogen peroxide application.The active component of the material is pre-transition metal oxide nanoparticles.Preparation method includes: with soluble pre-transition metal salt and ammonium chloride as raw material, dissolving, evaporating to dryness to obtain mixed precursor, then by calcining at different temperatures in tube furnace to obtain pre-transition metal oxide nanoparticles.The pre-transition metal oxide nanoparticles catalyst prepared can be used for oxygen reduction to prepare hydrogen peroxide, with very high hydrogen peroxide selectivity and excellent stability, greatly improving the energy utilization efficiency.The application has the characteristics of low cost, low energy consumption, simple operation, no security risks, etc., and is suitable for large-scale industrial production.

The invention provides a method for preparing high-purity scandium oxide, which comprises the following steps: S1, dissolving coarse scandium oxide in an acid solution to obtain a scandium-containing solution; s2, adsorbing the scandium-containing solution in the step S1 by using cationic resin, and analyzing the adsorbed cationic resin to obtain a purified scandium-containing solution; wherein the cationic resin has a sulfur group and / or a carboxylic acid group; s3, mixing a surfactant solution, an oxalic acid solution and the purified scandium-containing solution in the step S2, carrying out reaction treatment, and carrying out solid-liquid separation to obtain a scandium oxalate solid phase; and S4, sequentially washing, drying and roasting the scandium oxalate solid phase in the step S3 to obtain the high-purity scandium oxide. According to the method, the high-purity scandium oxide can be prepared through a simple process, the absolute purity of the scandium oxide is high, and the impurity content can be reduced to 5 ppm or below.

The film is formed using one of two film-forming materials. The first film-forming material contains: particles containing a crystal phase of a rare earth element fluoride; particles containing a crystal phase of a rare earth element oxide; and particles containing a crystal phase of a rare earth element ammonium fluoride double salt. The second film-forming material contains: particles containing a crystal phase of a rare earth element fluoride; and particles containing a crystal phase of a rare earth element oxide and a crystal phase of a rare earth element ammonium fluoride double salt. If a spray coated film is to be formed by means of thermal spraying using this film-forming material or film-forming slurry in particular, it is possible to form a rare earth element oxyfluoride spray coated film without the need for excessive heat.

The invention provides a method for preparing scandium oxide from laterite-nickel ore, which comprises the following steps: slurrying and leaching iron-removed aluminum slag of laterite-nickel ore to obtain scandium leachate; ammonium sulfate is added into the scandium leachate for a precipitation reaction, and ammonium scandium sulfate is obtained; re-dissolving ammonium scandium sulfate in water and precipitating again, and then roasting and leaching the re-dissolved and re-precipitated ammonium scandium sulfate to obtain a scandium sulfate solution; after Fe < 3 + > in the scandium sulfate solution is reduced into Fe < 2 + >, scandium reduction extraction is carried out, a loaded organic phase obtained after scandium extraction is washed and reversely extracted, and a purified scandium sulfate solution is obtained; and carrying out precipitation treatment on the purified scandium sulfate solution to obtain a precipitate, and carrying out post-treatment on the precipitate to obtain scandium oxide. According to the process, the high-purity scandium oxide is prepared through the procedures of high-pressure leaching, ammonium scandium sulfate re-dissolution and re-precipitation, Fe < 3 + > reduction, reduction extraction and the like, meanwhile, alkali reverse extraction is not needed in the extraction procedure, and reverse extraction can be achieved through common sulfuric acid.

The invention discloses a comprehensive recovery method of scandium, nickel, cobalt and manganese, and belongs to the technical field of metal production or refining. The method comprises the following steps: adding sulfuric acid into nickel cobalt hydroxide for leaching; introducing oxygen or air to oxidize the ferrous ions to obtain an oxidized leaching solution; carrying out vanadium precipitation and iron removal on the oxidation leaching solution, and separating to obtain scandium-containing jarosite slag and a second leaching solution; sO2 and oxygen / air are introduced into the second lixivium, so that divalent manganese is oxidized, and manganese oxide residues and third lixivium are obtained through separation; an organic phosphoric acid extraction agent and an organic carboxylic acid extraction agent form a composite extraction agent; saponifying the composite extracting agent, and then carrying out nickel-cobalt extraction on the third leaching solution; activating and roasting the scandium-containing jarosite slag by using concentrated sulfuric acid, and leaching after activation to obtain a fourth leaching solution; and performing scandium extraction on the fourth leaching solution by adopting a composite extracting agent, and separating and recycling scandium to realize separation from iron. By adopting the method, the comprehensive recovery of scandium, manganese, nickel and cobalt can be realized, and the efficient extraction of nickel and cobalt and the effective separation of nickel and cobalt from other metals can be realized.

The application discloses a comprehensive recovery method of scandium, nickel, cobalt and manganese, and belongs to the technical field of metal production or refining. The method comprises the following steps: adding sulfuric acid to nickel cobalt hydroxide for leaching; introducing oxygen or air to oxidize the ferrous ions, so that an oxidized leaching solution is obtained; removing iron from the oxidized leaching solution by jarosite precipitation, so that a jarosite residue containing scandium and a second leaching solution are separated; introducing SO2 and oxygen / air into the second leaching solution to oxidize the divalent manganese, so that an oxidized manganese residue and a third leaching solution are separated; forming a composite extractant by mixing an organic phosphoric acid extractant and an organic carboxylic acid extractant; performing nickel cobalt extraction on the third leaching solution after saponification of the composite extractant; activating and roasting the jarosite residue containing scandium by using concentrated sulfuric acid, and then leaching the activated residue to obtain a fourth leaching solution; and performing scandium extraction on the fourth leaching solution by using the composite extractant, so that the scandium is separated and recovered to be separated from iron. The method can realize comprehensive recovery of scandium, manganese, nickel and cobalt, and can realize efficient extraction of nickel and cobalt and effective separation of the nickel and cobalt from other metals.

The invention discloses a method for cleanly preparing high-purity scandium oxide from crude scandium oxalate, which comprises the following steps of: firstly, realizing efficient separation of scandium and most coexisting metal impurities through conversion reaction of the crude scandium oxalate and ammonium bicarbonate; then, an acidic phosphorus-containing extraction agent is adopted to selectively extract scandium in the returned solution, and thorium and rare earth impurities are deeply removed; then, solid oxalic acid is adopted for stripping scandium from the organic phase, and efficient conversion of scandium oxalate and in-situ regeneration of the organic phase are achieved while a traditional water phase is eliminated; and finally, removing an organic phase entrained in scandium oxalate through a secondary carbonate conversion step to obtain refined scandium salt, and roasting to obtain high-purity scandium oxide. The operation of all the units is linked with one another, an efficient, clean and low-consumption closed cycle is formed, and the method is used for purifying low-grade scandium oxalate raw materials with complex components.

The invention belongs to the field of rare earth hydrometallurgy, and discloses a method for preparing a high-purity rare earth compound through complex precipitation, which comprises the following steps: adding a rare earth compound to be purified into an inorganic compound, and dissolving to obtain rare earth feed liquid; adding an organic complexing agent into the rare earth material liquid according to a preset first proportion, adjusting by using an auxiliary adjusting agent, and adjusting the pH value of the system to a preset value to obtain a rare earth complexing material liquid; and adding a precipitant into the rare earth complexing material liquid according to a preset second proportion for precipitation, and filtering, washing and roasting to obtain the purified rare earth oxide. By adding the organic complexing agent, the occurrence form of rare earth and impurity elements is controlled; the addition of the auxiliary regulator further regulates the form distribution of the rare earth and impurity elements, so that the rare earth is selectively precipitated in the precipitation process, impurity precipitation is reduced, the separation effect in the precipitation process is further improved, and the purification method is simple in process operation and low in production cost.

A composite extractant for scandium extraction includes: a first extractant comprising at least one selected from an acidic extractant, a neutral extractant, and an alkaline extractant; a second extractant comprising at least one selected from a ketone compound and an ester compound; and a diluent. The first extractant has an amount of 5-20wt% based on a total weight of the composite extractant, and the second extractant has an amount of 0.5-5wt% based on a total weight of the composite extractant.

This invention provides a method for preparing scandium hydroxyl oxide using an acidic scandium-containing solution. The method includes the following steps: subjecting the acidic scandium-containing solution to a first-stage alkaline precipitation with a first alkaline precipitant to obtain a first-stage alkaline precipitate; subjecting the first-stage alkaline precipitate to a second alkaline precipitant and solid-liquid separation to obtain a second-stage alkaline precipitate and a second-stage alkaline precipitate product; subjecting the second-stage alkaline precipitate to a third-stage alkaline precipitation, aging, and solid-liquid separation with a third alkaline precipitant to obtain scandium hydroxyl oxide; and washing the obtained scandium hydroxyl oxide to obtain final low-impurity scandium hydroxyl oxide. The method of this invention can directly prepare scandium hydroxyl oxide using an acidic scandium-containing solution. Compared with the preparation of other scandium intermediates, it avoids the formation of soluble scandium salts and difficult-to-filter scandium hydroxide, thus directly preparing scandium intermediates with excellent filtration performance and easy processing, ensuring a very high scandium recovery rate, and shortening the production process of scandium intermediates.

The present application relates to an asymmetric metallocene scandium complex precursor and a preparation method and application thereof, and belongs to the technical field of organic chemistry.The asymmetric metallocene scandium complex precursor has a molecular formula of Sc(Cp1Cp2Cp3); wherein Cp1, Cp2 and Cp3 are each independently a substituted or unsubstituted cyclopentadienyl ligand, and the molecular structures of the three are different from each other.The present application first synthesizes a new compound cyclopentadienyl methyl cyclopentadienyl ethyl cyclopentadienyl scandium, which is the first example of a non-uniform ligand trisubstituted metallocene scandium, and the new compound is used as a precursor source material for preparing Sc2O3 thin films by an atomic layer deposition (ALD) method, and has a huge prospect in the fields of semiconductors and scientific research.

The film is formed using one of two film-forming materials. The first film-forming material contains: particles containing a crystal phase of a rare earth element fluoride; particles containing a crystal phase of a rare earth element oxide; and particles containing a crystal phase of a rare earth element ammonium fluoride double salt. The second film-forming material contains: particles containing a crystal phase of a rare earth element fluoride; and particles containing a crystal phase of a rare earth element oxide and a crystal phase of a rare earth element ammonium fluoride double salt. If a spray coated film is to be formed by means of thermal spraying using this film-forming material or film-forming slurry in particular, it is possible to form a rare earth element oxyfluoride spray coated film without the need for excessive heat.

This invention discloses a method for preparing high-purity scandium oxide from crude scandium oxide, comprising the following steps: dissolving crude scandium oxide with hydrochloric acid; adding an amine extractant to remove impurities such as iron and zinc, obtaining a purified solution after primary impurity removal; adding a complexing agent to the raffinate to complex scandium, followed by extraction of major impurities such as calcium, aluminum, magnesium, and manganese using a phosphate ester acidic extractant, obtaining a purified solution after secondary impurity removal; adding a decomplexing agent to the scandium-containing back-extraction solution to decomplex, adding a precipitating agent to the decomplexed scandium-containing solution to precipitate scandium, and subjecting the precipitate to filtration, washing, and calcination to obtain refined high-purity scandium oxide (>99.99%). The process of this invention has the advantages of short process flow, low cost, and high product quality, providing an effective impurity removal method for the preparation of high-purity scandium oxide.

A coating film is formed using a film-forming material containing particles including a crystal phase of a rare earth element fluoride, particles including a crystal phase of a rare earth element oxide, and particles including a crystal phase of a rare earth element ammonium bifluoride complex salt, or a film-forming material containing particles including a crystal phase of a rare earth element fluoride and particles including a crystal phase of a rare earth element oxide and a crystal phase of a rare earth element ammonium bifluoride complex salt. In the film-forming material or film-forming slurry of the present application, particularly if a spray coating film is formed using the film-forming material or film-forming slurry using spraying, a rare earth element oxyfluoride spray coating film can be formed without requiring excess heat, so that even under the atmosphere, the progress of an oxidation reaction caused by spraying heat is suppressed, while a rare earth element oxyfluoride spray coating film having little rare earth element fluoride and rare earth element oxide is obtained, and in addition, film peeling caused by excess heat can be suppressed.