10results about "Germanium dioxide" patented technology

The invention discloses tetragonal system germanium dioxide and a hydrothermal synthesis method thereof. According to the method, hexagonal crystal system germanium dioxide is taken as a raw material, a hydrothermal reaction is carried out in an acidic aqueous solution, and efficient conversion from a hexagonal crystal system to a tetragonal crystal system is realized by controlling the reaction temperature to be 120-240 DEG C, the reaction time to be 24-48 hours and the pH value to be 1-3. According to the preferable scheme, the raw materials are subjected to calcination pretreatment at the temperature of 500-600 DEG C, the yield of the tetragonal crystal phase can be remarkably increased, and the synthesis temperature can be reduced to 120 DEG C. According to the invention, stable synthesis of tetragonal system germanium dioxide is realized for the first time under the mild condition of 240 DEG C and below, and the technical problem that high-temperature transformation at 1000 DEG C or above is needed in the traditional method is solved. The tetragonal crystal system germanium dioxide prepared by the method is of a regular polyhedral structure, has the particle size of 400-500nm, and can be used as a high-efficiency catalyst for polyester synthesis. The process is energy-saving and environment-friendly, the total utilization rate of the raw materials is increased by recycling the waste liquid, and the process has remarkable industrial application value.

The invention discloses an efficient sedimentation and recycling process based on germanium dioxide in hydrogen peroxide tail gas absorption liquid and application, and belongs to the technical field of industrial waste gas treatment and scattered metal recycling in the special gas industry. The process comprises the following steps: carrying out standing separation on hydrogen peroxide tail gas absorption liquid, and carrying out synergistic regulation on a sedimentation layer through pH and a composite flocculant to realize efficient sedimentation of germanium dioxide; dehydrating the germanium dioxide concentrated phase to form a filter cake, and carrying out three-stage countercurrent washing and staged heating drying to obtain a crude germanium dioxide solid product; the filtrate and the settled supernate are subjected to primary pH regulation, secondary membrane separation and adsorption and three-stage closed-loop hydrogen peroxide replenishing three-stage purification systems, so that efficient cyclic utilization of hydrogen peroxide is realized; the germanium dioxide recovery rate reaches 99% or above, the hydrogen peroxide recovery rate reaches 95%, the process cost is reduced by 40% or above, and the method has the advantages of being simple in process, high in resource recovery rate and low in operation cost and is suitable for treatment and resource utilization of germanium-containing tail gas in production of semiconductors, photovoltaic materials and special gases.

The application discloses a method for recovering germanium by means of joule heat chlorination of germanium-containing fly ash, and relates to the technical field of resource recovery, comprising the following steps: mixing germanium-containing fly ash, a solid chlorinating agent and a conductive additive to obtain uniform reaction materials; pressing the reaction materials to form a porous conductive reaction body, and placing the porous conductive reaction body in a joule heat reaction device; making the porous conductive reaction body generate joule heat by electrification, and making the reaction materials generate a chlorination reaction in a chlorine-containing reaction atmosphere and generate gaseous germanium chloride; and setting a temperature gradient regulation zone inside the joule heat reaction device along the gas flow direction, so that the gaseous germanium chloride migrates along the direction of temperature reduction in the temperature gradient regulation zone and maintains a gas phase transport state; by means of the steady-state regulation of the path temperature gradient and the joule heat driving of the porous conductive reaction body, and in combination with the temperature difference induced condensation of the trapping interface, the gaseous germanium chloride is realized to be directionally transported and recovered and enriched without increasing complex gas separation equipment.

This invention relates to a method for the efficient preparation of GeO2 by ultrasonic spray hydrolysis of GeCl4 and particle size control, belonging to the field of rare and precious metal extraction technology. The invention employs an apparatus for the efficient preparation of GeO2 by ultrasonic spray hydrolysis of GeCl4 and particle size control. The apparatus includes an ultrasonic atomization hydrolysis system, a liquid-solid separation system, and an atomization drying system connected in sequence. GeCl4 solution and electronic-grade water are atomized by the GeCl4 solution ultrasonic atomization system and the H2O ultrasonic atomization system, respectively, and then the hydrolysis reaction is carried out in the atomization hydrolysis tower. This avoids the problem of GeO2 reversing to GeCl4 due to conventional stirring. The particle size of the product GeO2 is controlled by the ultrasonic atomization frequency. Simultaneously, the impact reaction between GeCl4 and H2O is achieved using the ultrasonic shock wave effect, preventing the formation of a GeO2 product layer. The purity of GeO2 can reach up to 6N. Furthermore, atomization drying prevents grain aggregation, achieving precise control of GeO2 particle size. The particle size uniformity index (PDI) of GeO2 can reach up to 1.00.

This invention discloses a high-efficiency sedimentation and recycling process and application of germanium dioxide in hydrogen peroxide tail gas absorbent, belonging to the field of industrial waste gas treatment and rare dispersed metal recovery technology in the specialty gas industry. The process includes: static separation of the hydrogen peroxide tail gas absorbent; efficient sedimentation of germanium dioxide by synergistic adjustment of pH and composite flocculant in the sedimentation layer; dehydration of the concentrated germanium dioxide phase to form a filter cake, followed by three-stage countercurrent washing and staged heating drying to obtain crude germanium dioxide solid; and a three-stage purification system for the filtrate and supernatant after sedimentation, consisting of primary pH adjustment, secondary membrane separation adsorption, and tertiary closed-loop hydrogen peroxide replenishment, to achieve efficient recycling of hydrogen peroxide. This results in a germanium dioxide recovery rate of over 99%, a hydrogen peroxide recovery rate of over 95%, and a reduction in process cost of over 40%. The process is simple, has high resource recovery rate, and low operating cost, and is suitable for the treatment and resource utilization of germanium-containing tail gas in semiconductor, photovoltaic material, and specialty gas production.

The invention discloses a method for preparing SiO2 while recycling germanium in a waste optical fiber preform, and belongs to the technical field of metallurgy and chemical industry. The method comprises the following steps: sequentially grinding, screening, wet ball-milling and drying the waste optical fiber preform to obtain optical fiber preform powder, dipping the optical fiber preform powder in an organic acid solution, carrying out solid-liquid separation to obtain a germanium-rich solution and SiO2-containing leaching residues, and treating the germanium-rich solution and the SiO2-containing leaching residues to respectively obtain GeO2 and SiO2. The method has the advantages of being simple in process, high in metal germanium recovery rate, environmentally friendly and the like, in addition, high-purity SiO2 is produced while metal germanium is recovered, and high-value utilization of the waste optical fiber preform is achieved.

A germanium oxide processing system is provided, including a calcination furnace, a dross tank, and a collection module. The calcination furnace is configured to heat and dry germanium oxide material in a flowing vacuum oxygen-free environment and discharge water vapor to the collection module, and to heat and calcine the germanium oxide material at a temperature at which the germanium oxide does not sublimate in a flowing vacuum oxygen-free environment with nitrogen gas admitted and discharge water vapor and nitrogen gas to the collection module and dross gas and nitrogen gas to the dross tank. The dross tank is configured to receive the dross gas and nitrogen gas, condense to form a viscous liquid, and discharge the nitrogen gas to the collection module. The collection module is configured to form a flowing vacuum with the calcination furnace, receive and condense and collect the heat and dry water vapor, receive and condense and collect the heat and calcine water vapor and nitrogen gas, receive and cool the nitrogen gas discharged from the dross tank during the heat and calcine.

The invention relates to a method for cooperatively treating germanium deep processing wastewater and recovering germanium, belongs to the technical field of germanium deep processing wastewater treatment, and aims at the composition characteristics that germanium-containing wastewater such as distillation raffinate, tail absorption liquid, hydrolysis mother liquor, material washing water and ingot washing water generated in the germanium deep processing process is wide in source and different in component such as pH value, germanium concentration and impurity content. Germanium is directly and efficiently recovered from the germanium-containing wastewater by adopting a synergistic mixing-ion exchange process and is output in a high-purity GeO2 product form, chlorine is output in a hydrochloric acid form and is used in the process, the germanium recovery process is greatly simplified, the germanium recovery rate is remarkably increased, meanwhile, the treatment cost of the chlorine-containing wastewater is reduced, and the method is suitable for industrial production. The method has the technical advantages of simple process flow, high comprehensive recovery rate, cleanness, high efficiency and the like.

The invention discloses a spherical powder material as well as a preparation method and application thereof, and relates to the technical field of new materials, and the preparation method mainly comprises the steps of pulping, loading, spheroidizing granulation or high-temperature treatment and the like. The preparation method is simple in production process, low in production cost and suitable for large-scale production, and the obtained product has the characteristics of high sphericity degree, controllable particle size, high tap density and the like, can be widely applied to new energy devices such as electro-catalysis, fuel cells, capacitors, batteries and the like, and can also be widely applied to the fields of catalysis, sensing, stealth wave absorption and the like.

The invention provides a germanium tetrachloride hydrolysis-germanium dioxide drying and calcining integrated device, and relates to germanium tetrachloride, the germanium tetrachloride hydrolysis-germanium dioxide drying and calcining integrated device comprises a hydrolysis reaction part, a sedimentation washing part and a drying and calcining part, and the hydrolysis reaction part, the sedimentation washing part and the drying and calcining part are sequentially connected from top to bottom to jointly form an integrated tower body; a mixing reaction cavity is formed in the hydrolysis reaction part, the top of the hydrolysis reaction part is connected with a gas input pipe and a liquid input pipe, and a stirring and mixing unit is arranged below the gas input pipe and the liquid input pipe. The core of the hydrolysis reaction part is provided with a composite stirring and mixing unit comprising a turbulent flow filter screen cylinder, a hollow self-suction turbine stirring piece and an outer turbulent flow stirring piece. In the working process, the hollow self-suction type turbine stirring piece rotates at a high speed, liquid can be sheared violently, germanium tetrachloride liquid can be sucked from the position above the liquid level and dispersed into fine bubbles, and the contact area of the gas phase and the liquid phase is greatly increased.