15results about "Ammonium fluoride" patented technology

The invention relates to a method for green recovery of lithium and fluorine in lithium-rich aluminum slag and preparation of battery-grade lithium dihydrogen phosphate and electronic-grade ammonium fluoride, and belongs to the technical field of comprehensive utilization of mineral resources. The method comprises the following steps: crushing and levigating lithium-rich aluminum slag obtained by electrolytic aluminum, adding deionized water, and then carrying out wet ball milling to obtain lithium-rich aluminum slag slurry; adding the lithium-rich aluminum slag slurry into a eutectic solvent for leaching, and carrying out suction filtration to obtain a leaching solution and insoluble slag; slowly dropwise adding ammonia water into the leachate, and filtering to obtain a neutralized solution and a precipitate; injecting the neutralization solution into a selective ion exchange column to obtain selective exchange resin enriched with lithium ions and ion exchange effluent; and eluting the lithium-rich resin with an H2C2O4 solution and preparing battery-grade lithium dihydrogen phosphate, and preparing electronic-grade ammonium fluoride from ion exchange effluent. According to the method, the production cost is effectively reduced through the modes of optimizing the process, reducing the energy consumption and the like, and maximization of economic benefits is achieved while the product competitiveness is improved.

This invention provides a method for producing high-purity aluminum-niobium-tantalum master alloys and co-producing ammonium fluoride, belonging to the fields of metallic materials and inorganic chemicals. The invention involves mixing fluoroniobic acid, fluorotantalic acid, and ammonia water for a precipitation reaction to obtain a precipitate and an ammonium fluoride solution. The ammonium fluoride solution is then concentrated, cooled for crystallization, dehydrated, and dried sequentially to obtain ammonium fluoride. The precipitate is then dried and oxidized and calcined sequentially to obtain an oxide. The oxide, aluminum powder, potassium chlorate, and calcium fluoride are mixed and subjected to a vacuum aluminothermic reaction to obtain the high-purity aluminum-niobium-tantalum master alloy. This invention, considering both broadening the range of raw material selection and optimizing the production process, reacts fluoroniobic acid, fluorotantalic acid, and ammonia water to produce niobium hydroxide and tantalum hydroxide precipitates, which are then oxidized and calcined to form niobium and tantalum oxides. The high-purity aluminum-niobium-tantalum alloy is then prepared using a vacuum aluminothermic reaction. Simultaneously, ammonium fluoride can be co-produced, resulting in high raw material utilization.

The invention discloses a method for recovering ammonium fluoride from semiconductor photovoltaic wastewater. The method comprises the following steps: adjusting pH in a pretreatment stage, and adding sodium citrate to complex metal ions; a composite extraction agent composed of diisooctyl phosphate, trialkyl phosphine oxide and methyl trioctyl ammonium chloride is adopted for multi-stage counter-current extraction; sequentially carrying out washing and two-stage gradient ammonia water reverse extraction to improve the selectivity and inhibit silicon-boron co-dissolution; the strip liquor is subjected to calcium and magnesium salt impurity removal, reduced pressure evaporation, graded cooling crystallization and vacuum drying, an ammonium fluoride product with the purity larger than or equal to 94% and the water content smaller than or equal to 0.5% is finally obtained, the extracting agent can be recycled, mother liquor and washing liquor are recycled, and the process is closed, environmentally friendly, economical and suitable for industrial application.

The present application relates to a kind of fluorine ammonium salt solution impurity removal method, fluorine ammonium salt preparation method, belong to fluorine chemical technology field.The fluorine ammonium salt solution impurity removal method of the present application, first fluorine ammonium salt solution and fluorine silicic acid solution are mixed, the mixed solution with pH 2~3 is obtained, then lead compound and mixed solution are mixed, lead compound produces lead ion in liquid environment, and then lead ion and phosphate ion and sulfate ion in mixed solution occur precipitation reaction, then excess lead ion is removed using lead adsorbent, finally solid-liquid separation is carried out, and impurity removal liquid is obtained.The fluorine ammonium salt solution impurity removal method of the present application is simple to operate, can efficiently remove phosphate ion and sulfate ion in fluorine ammonium salt solution and / or fluorine silicic acid solution, without introducing other impurity ions.

Disclosed herein are fluoride-containing ammonium salts and methods of production and uses thereof. For example, methods of producing ammonium fluoride by combining a material comprising a fluorosilicate with an amine are disclosed. In some examples, the material comprising a fluorosilicate comprises a waste product, such as a waste product from ore processing (e.g., phosphate ore processing), fertilizer production, and / or aluminum production and / or refinement.

The invention provides a multi-stage condensation recovery and closed-loop fluorinating agent regeneration process. The process comprises the following steps: introducing ammonia gas, ammonium fluoride and hydrogen fluoride volatilized from a titanium-containing compound in fluorination, sublimation and hydrolysis processes into a condensing tower; the condensing tower is used for recovering ammonium bifluoride residues in a first condensing stage, collecting ammonium fluoride and hydrogen fluoride in a second condensing stage and condensing ammonia gas in a third condensing stage; introducing the condensed ammonia gas and ammonium fluoride into an absorption tower, absorbing with a hydrofluoric acid solution, and reacting to generate an ammonium bifluoride solution; and the ammonium bifluoride solution is regenerated into solid ammonium bifluoride through vacuum evaporative crystallization.

This invention provides an integrated process for processing ammonium fluorosulfate, a by-product generated in the production of bis(fluorosulfonyl)imides. [Solution] A process for processing ammonium fluorosulfate byproducts includes providing an ammonium fluorosulfate byproduct mainly comprising ammonium fluorosulfate and smaller amounts of fluorosulfonic acid and bis(fluorosulfonyl)imide; mixing the ammonium fluorosulfate byproduct with water; reacting the mixture of ammonium fluorosulfate byproducts and water at a hydrolysis reaction temperature to hydrolyze ammonium fluorosulfate, fluorosulfonic acid and bis(fluorosulfonyl)imide to form ammonium bicarbonate and an aqueous hydrogen fluoride solution; and separating ammonium bicarbonate from the aqueous hydrogen fluoride solution.

The present application relates to a kind of removal methods of phosphate in fluorine salt solution, belong to fluoride dephosphorization technical field.The removal method of phosphate in fluorine salt solution of the present application, it includes the following steps: mixing in fluorine salt solution metal Zn and / or Zn-containing compound is reacted, after reaction, if system pH is 5.0~8.0, then the system is carried out solid-liquid separation, if system pH <5.0 or >8.0, then add pH regulator to adjust the pH of system to 5.0~8.0 to carry out reaction, then carry out solid-liquid separation;The fluorine salt is ammonium hydrogen fluoride and / or ammonium fluoride, and the pH value of the fluorine salt solution is <5.0 or >8.0.The removal method of phosphate in fluorine salt solution of the present application, while removing phosphate, does not reduce the content of fluoride ion in fluorine salt solution, and the dephosphorization effect is good.

This invention belongs to the field of chemical production technology, specifically disclosing a method for preparing high-purity silica, comprising the following steps: S1, grinding: crushing and grinding minerals or waste containing silica or silicates; S2, leaching: mixing with a leaching agent in a certain proportion to carry out a leaching reaction, followed by solid-liquid separation to obtain a fluoride ion complex solution containing fluorosilicic acid; S3, extraction: separating fluorosilicic acid from fluoride ion complex impurities using an extraction method to obtain a high-purity fluorosilicic acid or fluorosilicate solution; S4, pH adjustment: performing a metathesis reaction by adjusting the pH, followed by solid-liquid separation to obtain solid silica and soluble fluorides; S5, obtaining high-purity silica. This invention, employing the above-mentioned method for preparing high-purity silica, is applicable to most silicon-containing raw materials, effectively reducing the impurity content in silicon slag, and preparing high-purity silica with a purity of up to 99.99%.

The present application relates to a kind of phosphorus removal in system when fluorosilicic acid is used to prepare fluorinated salt, belong to inorganic fluoride preparation technical field.The present application removes phosphorus in system when fluorosilicic acid is used to prepare fluorinated salt, first the solution containing ferrous fluorosilicate and fluorosilicic acid is ammoniated, obtain the ammoniated treatment liquid with pH 1.5~3, can avoid the precipitation of silicon dioxide when ammoniated and subsequent ammoniated treatment liquid and oxidant mixed reaction, then ammoniated treatment liquid and oxidant are mixed, divalent iron in ammoniated treatment liquid is oxidized into trivalent iron and reacts with phosphorus to generate iron phosphate precipitate, finally through solid-liquid separation, iron phosphate precipitate is dried and can be sold as iron phosphate product.The present application removes phosphorus in system when fluorosilicic acid is used to prepare fluorinated salt under the premise of not introducing impurity ion, can make each element in system be utilized to maximum limit, and wide application range.

The application discloses a resource utilization method of fluorinated aluminum silicon slag. The resource utilization method comprises the following steps: adding the fluorinated aluminum silicon slag into an alkali solution to react, and then performing solid-liquid separation to obtain a solid and a liquid; the solid is recycled; the pH of the liquid is adjusted to 1.5-3.0 to obtain a fluorosilicate solution; ammonia water and a template agent are added into the fluorosilicate solution to obtain a silica sol; a fluorotitanate solution is prepared and added into the silica sol to obtain a precursor solution; after static crystallization of the precursor solution, solid-liquid separation is performed; the obtained solid is stirred in water overnight, and then suction filtration is performed to obtain a liquid phase and a solid phase; after water removal, the liquid phase is used to prepare ammonium fluoride; the solid phase is dried to obtain a precursor; and the precursor is calcined to obtain TS-1 molecular sieve. The application uses the fluorinated aluminum silicon slag as a silicon source, uses various different fluorotitanate as a titanium source, and combines a template agent to synthesize the TS-1 molecular sieve, and meanwhile, the fluorinated aluminum and the ammonium fluoride can be recycled, thereby providing a new idea for processing of industrial fluorosilicic acid by-products.

The application discloses a system for waste gas purification and resource recovery in lithium battery recycling, comprising a pyrolysis device, a second dust removal device, a gas mixer, a combustion chamber and a boiler which are sequentially connected, a splitting device, a first dust removal device and the gas mixer which are sequentially connected, a hydration tower, a primary phosphoric acid catcher, a mixed acid pool, a secondary phosphoric acid catcher, a hydrofluoric acid recovery tower and a purification tower which are sequentially connected, and a method for waste gas purification and resource recovery in lithium battery recycling. The application has the advantages that P2O5 and HF are separated and purified, the energy of carbonic acid ester combustion is utilized, by-product phosphoric acid, hydrofluoric acid or ammonium fluoride products are extracted in stages, the treatment difficulty of waste water and waste residue is greatly reduced, and the environment is friendly. In addition, since the by-products have high market value, the environmental protection project has good economic benefits and resources are saved.

The application discloses a kind of resource processing technology of nickel-containing etching waste liquid, comprising the following steps: S1, pretreatment: adding lye to nickel-containing etching waste liquid to adjust pH to 3.5~4.0, then heated stirring treatment, again, standing aging treatment, obtain containing nickel fluoride turbidity liquid;S2, centrifugal: the centrifugal treatment of containing nickel fluoride turbidity liquid;S3, main reaction: with hot water to clean nickel fluoride by-product, cleaning wastewater is added to the etching waste liquid after pretreatment, then add hydrofluoric acid to adjust the ratio of ammonium fluoride and hydrofluoric acid to 0.9~1.2:1, after reaction, obtain reaction liquid;S4, concentration;S6, centrifugal;S7, drying: ammonium bifluoride crystal is dried to obtain ammonium bifluoride product.The application controls precipitated nickel fluoride by adjusting process conditions, solves the influence of nickel-ammonium complexation on the direction of treating nickel-containing etching waste liquid by precipitation method by pH control, reduces auxiliary material addition and environmental pollution, realizes resource recycling, and reduces production cost.

The application discloses a novel method and device for resource conversion of sulfur hexafluoride. The method comprises the following steps: firstly, performing primary discharge treatment on SF6 to dissociate SF6 into fluorine atoms and low-fluorine sulfides; secondly, performing fluorination reaction of the fluorine atoms and the low-fluorine sulfides with tungsten to convert the fluorine atoms and the low-fluorine sulfides into WF6 and reduce sulfur into elemental sulfur; thirdly, controlling the fluorination reaction temperature to be 120-160 DEG C to make the generated elemental sulfur into liquid state, so that the elemental sulfur is conveniently collected; fourthly, condensing mixed gas containing WF6, collecting the liquefied WF6, mixing the condensed mixed gas with water vapor, and performing secondary discharge treatment on the mixed gas containing water vapor; under the action of the water vapor, the mixed gas is further degraded, and the degradation products tend to be SO2 and HF; fifthly, separating the SO2 and the HF; sixthly, treating the HF by using a "hydrogen fluoride-liquid ammonia" liquid phase method to obtain ammonium fluoride and ammonium bifluoride; and seventhly, treating the SO2 by using a wet ammonia method to obtain ammonium sulfite and ammonium sulfate.

The application provides a recycling treatment process for tantalum-niobium wet smelting alkaline wastewater, and belongs to the technical field of tantalum-niobium wet smelting wastewater treatment. The low-fluorine pure water and the ammonia-containing recycling water used in the treatment process are both reused wastewater of the tantalum-niobium wet smelting alkaline wastewater, so that the alkaline wastewater can be recycled to the maximum extent, and the water consumption of new water in the alkaline wastewater treatment process can be greatly reduced. In the whole treatment process of the application, a small amount of chemical pure hydrofluoric acid is added, and no other chemicals are additionally added, and no waste residue is discharged, so that the operation cost is significantly reduced, and a high-purity high-value ammonium fluoride product can be produced, and the purity of the ammonium fluoride product can reach more than 98%. The treatment process of the application can effectively recycle and utilize the fluorine and ammonia in the wastewater through resource management, basically realizes zero discharge of the tantalum-niobium wet smelting alkaline wastewater, and the low-fluorine pure water after treatment meets the first standard requirement of Table 1 and Table 4 in the Integrated Wastewater Discharge Standard (GB 8978-1996). The treatment process of the application is aimed at the different ammonia nitrogen concentrations in the condensate water and the recycling water after multi-stage membrane concentration treatment, and the condensate water and the recycling water after multi-stage membrane concentration treatment are treated and reused after being separated according to quality, so that the dosing amount of ammonia and hydrofluoric acid can be greatly reduced, and the production cost can be significantly reduced.