89 results about "Ammonium perrhenate" patented technology

The invention relates to a method for preparing ammonium perrhenate from waste liquid containing molybdenum and rhenium. In the technical scheme of the invention, the method comprises the following steps of: adding hydrogen peroxide into the waste liquid containing molybdenum and rhenium until the solution turns to yellow, then adding a mixed agent until the pH of the solution is 6 to 7, separating by filter pressing, collecting the filtrate, absorbing the filtrate by a resin exchange column, stopping adsorption until the concentration of rhenium in effluent is constant, eluting with NH3.H2O,collecting the eluate, heating to concentrate the eluate at 98-100 DEG C, cooling, and crystallizing to obtain ammonium perrhenate. The mixed agent is a mixture of calcium hydroxide and calcium oxidein a weight ratio of 5:1. According to the invention, the waste liquid containing molybdenum and rhenium, particularly the absorption liquid of the flue gas during molybdenum roasting, is used as theraw material; the enrichment of rhenium is increased by about 20 times; ammonia water is determined as the eluent of rhenium; the elution rate of rhenium is higher than 98%; the recovery rate of rhenium is higher than 93%, the purity of the ammonium perrhenate product is higher than 99.5%, and the economic, social and environmental benefits are significantly improved.

The invention relates to the technical field of rhenium recycling and use, in particular to a method for preparing metallic rhenium. According to the method provided by the invention, the high-purity metallic rhenium is prepared by taking ammonium perrhenate as a raw material through two steps; in the first step, high-purity ultrafine ammonium perrhenate is first prepared; in the second step, the ammonium perrhenate is reduced into high-purity metallic rhenium powder through a reducing method; ultrasonic auxiliary crystallization and vacuum drying are adopted; in the process of ultrasonic crystallization, an ultrasonic crystallizer with an opened kettle body and a detachable ultrasonic transducer are adopted. Due to the adoption of an ultrasonic crystallization-hydrogen reduction combined process, the ammonium perrhenate serving as the raw material is used for preparing the high-purity metallic rhenium, so that the flow is simplified, the reaction time is shortened, the energy is saved, and the consumption is reduced; the raw material is high in adaptability, so that the requirement on the raw material is lowered; ultrasonic waves directly act on the ammonium perrhenate material, and the utilization rate is high; the detachable structure is easy to check and replace, and favorable for industrialization.

The invention discloses a method for preparing rhenium disulfide nanosheets, and belongs to the field of preparation of novel two-dimensional nanomaterials. The method includes the steps that ammonium perrhenate serves as a rhenium source, thiourea serves as a sulfur source, hydroxylamine hydrochloride serves as a reducing agent, the three reactants are dissolved in solvent water, and a chemical reaction is carried out by regulating the reaction temperature and reaction time; then, a product is cleaned and dried; finally, rhenium disulfide nanosheets are synthesized. The method is simple in operation process, high in efficiency, good in repeatability and low in cost, and high-quality rhenium disulfide nanosheets can be papered in a large batch; meanwhile, the method provides a reliable sample preparation method for application of rhenium disulfide nanosheets in electrics and optics.

The invention relates to a rhenium tungsten based cathode material and a preparation method thereof and belongs to the technical field of a refractory metal thermal cathode material. BaO, CaO and Al2O3 are loaded in pores of a porous rhenium tungsten base; the rhenium tungsten base is formed by coating tungsten grains by rhenium. The preparation method comprises the following steps: dissolving ammonium perrhenate in water, thereby preparing into a solution; adding tungsten powder into the ammonium perrhenate solution and stirring; drying; resolving and reducing in two steps under the hydrogen atmosphere, thereby obtaining rhenium tungsten powder; and pressing and sintering the rhenium tungsten powder under the hydrogen atmosphere, thereby obtaining a rhenium tungsten base and steeping into a molten barium aluminate calcium salt. The preparation method provided by the invention has the advantages that the preparation process is simple, the introduction of impurity element during the preparation process is avoided, the repeatability is strong, the prepared cathode material is excellent in emitting property, and the ion bombardment resistance of a traditional barium tungsten cathode is enhanced.

The invention discloses a process of recycling platinum-rhenium aluminum from platinum-rhenium waste catalyst of an alumina carrier. The process includes the steps that (1) the platinum-rhenium catalyst of the alumina carrier is conducted to roasting; (2) the carrier alumina is leached; (3) R410 negative ion exchange resin is used by leaching agent to adsorb rhenium, resin containing the rhenium is obtained and effluent goes to the next step; (4) the effluent from the last step is added with ammonia liquor to react, solid ammonium aluminum sulfate is produced; (5) leaching residue in step (2)is added with lime to conducted to roast; (6) roasting material of (5) is leaching by water; (7) residue containing platinum in step (6) is leaching, spongy platinum is produced by nitre; and (8) 001*7 positive ion exchange resin is used for exchanging, the effluent is neutralized, concentrated, froze through the ammonium hydroxide to produce ammonium perrhenate. The process has the characteristics of short circulation, high recovery rate and simple operation. The alumina carriers are all recycled, no waste water, waste residue is produced of all-wet technology. Platinum recovery rate is greater than 99.0%, rhenium recovery rate is greater than 97.0% and alumina recovery rate is greater than 98.0%.

The invention relates to a selenium rhenium sulfide composite two-dimensional material and a preparation method and application thereof; the preparation method comprises the steps of (a) dissolving ammonium perrhenate and thiourea in an organic solvent to form a first solution; (b) dissolving selenium powder in hydrazine hydrate to obtain a second solution; (c) mixing the first solution and the second solution, and pouring the mixture in a reactor with a substrate to carry out hydrothermal reaction; after the hydrothermal reaction, cooling, and taking out the substrate. By controlling minor doping of sulfur, a selenium rhenium sulfide nanosheet with high coverage, good distribution uniformity and small size is obtained on the substrate, the size of the nanosheet reaches 50-100 nm; the nanosheet with high coverage and vertical growth can provide larger specific surface area, and greater current density is provided in electric catalysis. By adjusting doping quantity of sulfur, the electronic structure of the material is adjusted, hydrogen absorption free energy of the material is lowered, conductivity of the material is improved, more defects and active sites are created, and the electrocatalytic performance of the material is improved.

The invention discloses a recovery method of molybdenum concentrates. The method comprises the following steps of: carrying out a hot pressing natural reaction of materials to be processed under an alkaline condition; enriching molybdenite through flotation from natural oxide slag after natural leaching, returning for hot pressing oxidation and floating tailing slag to recover copper; producing high-purity ammonium molybdate and ammonium perrhenate from leached liquid after the natural leaching through the process of extraction, purification, acid precipitation, ammonia dissolution, concentration and crystallization; and removing sodium sulfate by evaporating or freezing and crystallizing raffinate to produce a sodium sulfate product. According to the invention, the recovery rate of the molybdenum concentrates is improved.

The invention relates to the technical field of rhenium recycling and in particular relates to a method for preparing ammonium perrhenate. The ammonium perrhenate is prepared by purifying rhenium-enriched recovery liquid obtained by enrichment of poor-rhenium stock solution, and the rhenium-enriched recovery liquid is subjected to vacuum concentration, heating decomposition and dissolution-crystallization so as to prepare ammonium perrhenate. The method comprises the following steps: step 1, performing vacuum concentration to prepare a concentrated crystal; step 2, performing heating decomposition to collect rhenium heptoxide solids; step 3, performing dissolution-crystallization to prepare ammonium perrhenate; and step 4, recycling molybdenum and rhenium. According to the method disclosed by the invention, molybdenum and rhenium can be effectively separated from each other, and high-grade ammonium perrhenate can be prepared; and moreover, the poor-rhenium stock solution serves as a raw material, the raw materials are wide and readily available, and integrated resource recycling is realized.

The invention discloses less-layer rhenium disulfide nanosheet/hollow carbon spheres for a sodium-ion battery negative electrode material and a preparation method thereof. The negative electrode material is formed by attaching rhenium disulfide nanosheets to carbon shells inside and outside the porous hollow carbon spheres. The preparation method of the negative electrode material comprises the following steps: taking ammonium perrhenate as a precursor, taking thioacetamide as a sulfur source, taking hydrazine hydrate as a reducing agent, and taking the porous hollow carbon spheres as a rhenium disulfide growth framework, thereby obtaining the negative electrode material. According to the negative electrode material prepared in the invention, the porous hollow carbon spheres of uniform particle size are taken as the framework, and the rhenium disulfide sheet structures are uniformly dispersed on the carbon shells. According to use of the porous hollow carbon spheres, the number of growth layers of the rhenium disulfide nanosheets is limited as 2-7. The less-layer rhenium disulfide nanosheet/hollow carbon sphere nanocomposite material has many sodium-embedded active sites and high conductivity, the volume effect can be buffered by the inner cavity, the sheet layers are prevented from dropping to maintain the structural stability, and the rhenium disulfide nanosheets do not haveany obvious agglomeration phenomenon.

The invention discloses a method for purifying ammonium perrhenate. The method specifically comprises the steps: firstly, adding crude ammonium perrhenate into ultrapure water, dissolving, then sequentially filtering through three stage of screens to obtain a crude ammonium perrhenate solution, then adding hydrogen peroxide and ammonia water, stirring, then adsorbing through two cation exchange resins connected in series, evaporating, concentrating, freezing, crystallizing, filtering and drying to obtain ammonium perrhenate. The purity of the ammonium perrhenate prepared by the method disclosed by the invention is 99.99% or above, the loss of the ammonium perrhenate subjected to multiple evaporative crystallization can be effectively reduced, and the recovery rate of the ammonium perrhenate is 95% or above.

The invention discloses a ReS2/CdS photocatalyst and a preparation method and application thereof. The preparation method of the ReS2/CdS photocatalyst comprises the following steps that 1, ammonium perrhenate, thioacetamide, hexamine and cadmium sulfide are weighed and dissolved in distilled water to obtain a mixed solution B; 2, the mixed solution B obtained in the step 1 is placed in a hydrothermal reactor for hydrothermal reaction; 3, after the reaction is completed, when the hydrothermal reactor is cooled to a room temperature, dark green ReS2/CdS in the hydrothermal reactor is subjectedto ethanol washing, washing and drying for use. According to the preparation method of the ReS2/CdS photocatalyst, the obtained ReS2/CdS photocatalyst greatly improves the performance of CdS semiconductor photocatalysis hydrogen production, a flexible ReS2 load is used as a promoter on the CdS surface, not only are the problems of the scarcity and high cost of Pt solved, but also CdS semiconductorphotocatalytic material electron transferring is accelerated, the carrier compound probability of a CdS semiconductor photocatalytic material is reduced, and a brand new way is provided for a CdS photocatalysis hydrogen production technology.

The invention provides a method for recycling rhenium and bismuth from an acidic waste solution. The method comprises the following steps that firstly, ion exchange adsorption treatment is conducted on the acidic waste solution through ion exchange resin, and the rhenium and the bismuth in the acidic waste solution are adsorbed to the ion exchange resin; secondly, a mixed solution of sodium hydroxide and tartaric acid is utilized for desorbing the bismuth adsorbed to the ion exchange resin to a liquid phase, bismuth-containing desorption liquid is obtained, the rhenium adsorbed to the ion exchange resin is desorbed to the liquid phase through an ammonium thiocyanate solution, and rhenium-containing desorption liquid is obtained; and thirdly, concentrated hydrochloric acid is dripped into the bismuth-containing desorption liquid to enable the bismuth to be subjected to the precipitation reaction, bismuth enrichment slag is obtained, after heating and concentrating are conducted on the rhenium-containing desorption liquid, crystallization treatment is conducted, and ammonium perrhenate is obtained. According to the method, the rhenium and the bismuth in the acidic waste solution can be efficiently separated and recycled, the separation effect is obvious, the technology is simple and feasible, the equipment investment is small, and industrial application is facilitated.

The invention provides a method for producing ammonium perrhenate from rhenium-enriched residues. The method comprises the following steps: S1) mixing the rhenium-enriched residues and an oxidant solution for oxidizing leaching to obtain an oxidizing leaching solution; S2) adding an alkali compound into the oxidizing leaching solution to remove impurities so as to obtain an impurity removal solution; and S3) allowing the impurity removal solution to pass through a cation exchange resin to obtain the ammonium perrhenate. Compared with the prior art, the method disclosed by the invention has the advantages that the rhenium-enriched residues are subjected to oxidizing leaching and impurity removal by virtue of the alkali compound and adsorbed to further remove the impurities by virtue of the cation exchange resin, and then ammonium perrhenate can be obtained. The process flow is short, the treatment quantity is great, the equipment and raw material input is cheap, and the method can be operated at normal pressure. Moreover, the whole process is an all wet process metallurgy method, the problem of environmental pollution is solved, and the recovery efficiency is high.

The invention relates to a supported perrhenate ionic liquid as well as a preparation method thereof. The technical scheme adopted is as follows: the preparation method comprises the following steps: selecting MCM-41 (Mobil Composition of Matters) as a carrier material; firstly, carrying out a reaction on chloropropyl triethoxysilane and the MCM-41; grafting a chloropropyl silicon structure to the surface of the MCM-41, and removing the byproduct ethanol; then, adding N-methyl imidazole so as to quaternize to obtain MCM-41 supported alkyl imidazole chlorine salt; and further adding ammonium perrhenate, and converting the chlorine salt into perrhenate through double-decompose reaction to obtain the MCM-41 supported alkyl imidazole perrhenate ionic liquid. The molar ratio of the reaction materials chloropropyl triethoxysilane, N-methyl imidazole, the MCM-41 and perrhenate is 1:(4-1):(3-1):(10-0.1). The method is applicable to support of various different types of alkyl imidazole perrhenate ionic liquids.

The invention discloses a method for preparing ammonium perrhenate, which is characterized by comprising the following steps: 1. washing and cooling flue gas generated by tungsten gold ore roasting through an eluting tower, so that perrhenic acid contained in the flue gas is dissolved in water, and the water solution containing the perrhenic acid is used for circularly eluting the roasting flue gas to increase the concentration; 2. collecting the perrhenic acid water solution, carrying out rough filtration, and carrying out nanofiltration concentration on the filtrate with nanofiltration membrane equipment to obtain a perrhenic acid nanofiltration concentrated solution; and 3. passing the perrhenic acid nanofiltration concentrated solution through continuous ion exchange equipment, eluting rhenium with a resolving agent, heating to concentrate the collected eluate at 100 DEG C, cooling, and crystallizing to obtain the ammonium perrhenate. By using the flue gas generated by tungsten gold ore roasting as the raw material, the nanofiltration membrane equipment and continuous ion exchange equipment are utilized to recover the ammonium perrhenate, thereby achieving the goals of resource recovery and environment protection; and thus, the method has favorable economic value and environmental benefit.

The invention relates to a method for preparing dissipated metal rhenium ionic liquid. The adopted technical scheme is as follows: the preparation method comprises the following steps: taking a certain amount of alkyl bromide pyridine compound, adding 2-4 times of deionized water for dissolution, adding into OH type anion exchange resin for carrying out ion exchange, and collecting effluent solution which is hydroxyalkyl pyridine; adding the hydroxyalkyl pyridine into ammonium perrhenate water solution, leading the molar ratio of the hydroxyalkyl pyridine to the ammonium perrhenate to be 1:1-1:2, stirring for 3-5 hours at the temperature of 70-90 DEG C, carrying out vacuum distillation for removing water, cooling, then adding mixed solution of anhydrous methanol and acetonitrile, sealing, churning, placing at the temperature of minus 30-minus 40 DEG C for 10-15 hours, carrying out the vacuum distillation, removing the methanol and the acetonitrile and carrying out vacuum drying. The ionic liquid has high yield and is stable to air and water.

The chemical plating liquid for preparing high temperature self lubricating composite coating consists of nickel sulfate 15-36 g/L, ammonium perrhenate 0.8-2.2 g/L, sodium citrate 10-20 g/L, lactic acid 20-30 g/L, sodium hypophosphorate 15-30 g/L, barium fluoride 5-25 g/L, calcium fluoride 5-25 g/L and lead nitrate 2-10 mg/L. The chemical plating process includes cleaning and activating the surface of the workpiece, immersion plating the workpiece inside the chemical plating liquid of pH 5-7 at 85-95 for 10-60 min. The present invention can form composite Ni-Re-P/barium fluoride + calcium fluoride coating on the surface of mechanical parts to raise the surface friction reducing and wear resisting performance at very high temperature work condition and to increase the service life. The present invention is especially suitable for turbine blade, jet engine, etc.

The invention discloses a method for synergistic recovery of molybdenum and rhenium from a molybdenum concentrate roasting eluent, which belongs to the technical field of comprehensive recycling of metal rhenium and molybdenum. The method comprises the following steps: mixing the molybdenum smelting waste acid and a pretreatment agent, stirring a mixture, and then performing solid-liquid separation; introducing a filtrate to an exchange column containing weakly basic anion exchange resin A to adsorb rhenium, and introducing the adsorbed liquid in an exchange column filled with the weakly basicanion exchange resin B to adsorb molybdenum; performing desorption with the adsorbed saturated A column, collecting a desorption solution, and performing evaporation crystallization to obtain an ammonium perrhenate product; performing desorption with the adsorbed saturated B column, collecting the desorption solution, and performing evaporation crystallization to obtain an ammonium molybdate product. In a pretreatment step in the process, no rhenium loss is generated, the molybdenum loss rate is less than 8%, after treatment, the liquid is introduced into ion exchange, compared with the direct adsorption process, the method can increase the adsorption capacity of the resin A to the rhenium, and by changing the acidity of the solution and the impurity ion content, the high-efficiency adsorption of the resin B to the molybdenum is achieved.

The invention discloses ammonium rhenate with uniform granularity and a preparation method thereof, and belongs to the technical field of ammonium rhenate purification. The method includes: with industrial crude ammonium rhenate crystals as raw materials, adding distilled water, and heating the solution until the distilled water is completely dissolved, evaporating the distilled water by using a rotary evaporator to form a supersaturated ammonium rhenate solution, adding the solution into a homogeneous crystallization reaction kettle to perform cooling and stirring crystallization, carrying out suction filtration on the recrystallized ammonium perrhenate, and naturally air-drying the product to obtain ammonium perrhenate crystal powder with uniform particle size distribution and high purity. The method has the advantages that compared with a traditional recrystallization method, the recrystallization process of ammonium rhenate can be effectively controlled, and the granularity and purity of ammonium rhenate particles are uniformly refined.

The invention provides a method for recovering rhenium, copper, selenium and sulfur in rhenium concentrates. The method comprises the following steps: A) washing the rhenium concentrates, and filtering the rhenium concentrates to obtain a filtrate A and filter residues A; B) oxidatively leaching the filter residues A, and filtering the leached filter residues A to obtain a filtrate B and filter residues B; C) neutralizing the filtrate B for copper sedimentation to obtain copper hydroxide and a crude ammonium perrhenate solution, carrying out ion exchange on the crude ammonium perrhenate solution, carrying out thickening crystallization on the obtained solution to obtain ammonium perrhenate, carrying out sulfidation reaction on the filter residues B, and filtering the treated filter residues B to obtain a filtrate C and filter residues C. The method for recovering the rhenium, the copper, the selenium and the sulfur in the rhenium concentrates provided by the invention fully recovers and utilizes the copper, the selenium and the sulfur in the rhenium concentrates while treating the rhenium concentrates to recover the rhenium.

The present invention relates to a method of recovering rhenium (Re) and other metals from Re-bearing materials including, as an exemplary process, the steps: (i) adding Re-bearing materials into a leaching slurry; (ii) adjusting the pH of the slurry to obtain Re in soluble form in a metal salt solution and insoluble residues; (iii) filtering the metal salt solution to remove the insoluble residues; (iv) selectively precipitating Re from the metal salt solution; (v) filtering the Re precipitate from the metal salt solution to obtain a Re filtercake; (vi) formulating and drying the Re filtercake to obtain a Re sulfide product; (vii) combining the Re sulfide product with a Molybdenum (Mo) concentrate containing Re to obtain a Mo/Re concentrate; (viii) roasting the Mo/Re concentrate to obtain Mo oxide product and a flue gas containing Re; and (ix) treating the flue gas containing Re to obtain ammonium perrhennate.

The invention relates to a method for producing temperature measuring tungsten-rhenium thermocouple wires in high-reliability manner through a combined technology. Through the technical scheme, ammonium tungstate with purity 4N and ammonium perrhenate with purity 4N are made into a solution, through spray crystallization, tungsten-rhenium alloy compund powder is made, the powder is pressed into broken pieces and then is subjected to hydrogen reduction, then, the pieces are pressed and sintered into metal bars, and through rotary swaging, annealing and wire drawing, the needed diameter is obtained; the problems that the full-liquid-phase mixed powder grains are too fine, bar making is difficult, after process penetrating, components of all segments of the head, the middle and the tail of the wire strip are not consistent, thermoelectric potential difference is too large, and the subsequent pairing is not accurate are solved. Through the method, making convenience degree of the temperature measuring tungsten-rhenium thermocouple wires and the temperature measuring precision of the temperature measuring tungsten-rhenium thermocouple wires are obviously improved, and the method has thegiant scientific significance and application value in improving the process control level, and reducing the control material part unit cost in many industries, particularly, the high-technology manufacturing industry, in the national economy.

The invention discloses a method for detecting the content of rhenium in a rhenium containing test solution.The to-be-tested test solution is transferred into a beaker, distilled water, EDTA and tartaric acid are added, the pH value is adjusted, a tetraphenylarsonium chloride hydrochloride solution is added, and the solution is transferred into a separating funnel; extraction is conducted with trichloromethane three times, organic phases on lower layers are combined, the organic phases are washed with a tetraphenylarsonium chloride hydrochloride washing solution two times, and the organic phases are completely transferred into the beaker; after a sodium chloride solution is added, water bath evaporation to dryness is conducted for about 20 min, hydrochloric acid is added after evaporation to dryness is conducted, and after water bath heating, the mixture is cooled to room temperature and transferred to a colorimetric tube; distilled water, potassium thiocyanate and stannous chloride are added, and the mixture is shaken up and developed; after ethyl acetate is transferred into the colorimetric tube for extraction, the organic phases are taken for ultraviolet measurement at the 426nm position.Compared with the prior art, the method is designed aiming at the rhenium containing test solution generated in the production process of ammonium perrhenate, the method is simple and easy and convenient to operate, mistakes are not easy to make, especially, the test result is accurate, and use and popularization value is achieved.