12 results about "Germanium chloride" patented technology

The invention provides a novel method for purifying crude germanium tetrachloride, which comprises the processes of first-stage low-temperature evaporation, second-stage medium-temperature evaporation, third-stage negative-pressure evaporation, recovery of germanium tetrachloride tailings and the like. In the staged evaporation process of first-stage low-temperature evaporation, second-stage medium-temperature evaporation and third-stage negative-pressure evaporation, low-boiling-point impurities (such as chlorine and other volatile impurities) in germanium tetrachloride can be effectively removed, germanium tetrachloride is separated and purified in different stages by gradually increasing the temperature and adjusting the pressure, and the purity of germanium tetrachloride is improved. Finally, germanium tetrachloride with the purity of 99.9% or above is obtained. According to the method, the introduction of chemical materials such as concentrated hydrochloric acid, chlorine and the like is avoided while the coarse germanium tetrachloride is fully and preliminarily purified, so that the safety and environmental risks are reduced; and the method has the remarkable advantages of good purification effect, environmental friendliness and the like.

The present invention discloses a short-process method for preparing high-purity germanium from germanium tetrachloride and treating tail gas in a cycle. The device for preparing high-purity germanium by short-process hydrogen reduction of germanium tetrachloride according to the present invention includes a gas storage tank, a high-purity germanium tetrachloride hydrogen reduction furnace, a reaction tail gas rectification system, and a germanium dichloride chlorination system. The method of the present invention is to use high-purity hydrogen to carry high-purity germanium tetrachloride into the reduction furnace for reaction to deposit germanium metal on germanium rods, and then perform zone melting purification according to purity requirements; the unreacted gas passes through the subsequent rectification and chlorination systems to obtain high-purity hydrogen and germanium tetrachloride again, realizing the treatment of tail gas in a cycle.

The invention relates to a method for synchronously recovering germanium tetrachloride from a metal-state regenerated germanium raw material through oxychlorination, and belongs to the technical field of germanium extraction metallurgy. The method comprises the following steps: mixing a metal-state regenerated germanium raw material with hydrochloric acid in a chlorination distillation kettle, dropwise adding a hydrogen peroxide solution in sections to react with hydrochloric acid to generate a high-activity chlorine species, and directly oxidizing and chlorinating metal germanium to generate germanium tetrachloride. In the process, the reaction is a strong exothermic reaction, a product is distilled out by using heat released by the reaction, and the reaction temperature is controlled at 82-84 DEG C through a cooling medium. And after the reaction is basically completed, carrying out deep distillation through a heating medium, and finally condensing and collecting to obtain a germanium tetrachloride product. According to the method, a traditional multi-step process is integrated into one step, the process is short, alkali liquor does not need to be added, reaction heat is fully utilized, the energy-saving effect is remarkable, the germanium direct recovery rate is high, and the problems that a traditional method is long in process, high in energy consumption, large in auxiliary material consumption and low in direct recovery rate are effectively solved.

The invention discloses a method and device for extracting germanium from germanium tetrafluoride production tail gas absorption liquid, and belongs to the technical field of semiconductor germanium material production processes. The device comprises a concentration and distillation reaction kettle, a stirrer, a heater, a condenser, a multi-stage absorber, an air draft system and a spray tower. The device is used for stirring, concentrating and distilling for three times to extract germanium, the rotating speed of a stirrer for the first time is 60 r / min-200 r / min, the heating and distilling temperature is 90-100 DEG C, boric acid is added for the second time, the heating and distilling temperature is raised to 100-115 DEG C, industrial hydrochloric acid is added for the third time, and the distilling temperature is 100-120 DEG C. After concentration and distillation are completed, a concentrated solution is collected and sampled, the fluorine content and the germanium content in the concentrated solution are analyzed, and the result shows that the recovery rate of germanium in the method reaches 98% or above, and the fluorine content in germanium tetrachloride obtained through distillation is lower than 0.3% and does not exceed the requirement of the germanium tetrachloride product standard. And the method can be used for producing a high-purity germanium tetrachloride product in the next step of rectification and purification.

The large rectifying tower comprises a tower kettle, a tower rod and a tower head which are sequentially connected from bottom to top, the top of the tower kettle is provided with a connector connected with the tower rod, the bottom of the tower kettle is provided with a liquid outlet, and the tower head is provided with an exhaust port and a product outlet. The tower kettle is an enamel kettle which has the capacity of 1000L and is provided with a heating temperature control device, and a feeding hole and a temperature sensor A are arranged at the top of the tower kettle; the tower pole is formed by connecting a plurality of temperature compensators in series; and a temperature sensor B is mounted at the bottom of the tower head. According to the utility model, the purification space is enlarged, the rectifying tower is enlarged, meanwhile, the large-scale and continuous production of germanium tetrachloride is realized by adopting the large-scale tower kettle capable of accurately controlling the heating temperature, and the tower pole is replaced by the temperature compensator consisting of the steel lining polytetrafluoroethylene and the polytetrafluoroethylene sieve plate, so that the temperature change in the tower pole is stabilized after the tower pole is heightened.

This invention discloses a method for recovering germanium and hydrochloric acid from germanium tetrachloride hydrolysis mother liquor, comprising the following steps: (1) Acidification: sulfuric acid is added to the hydrolysis mother liquor to increase its acidity, which is beneficial for the distillation of germanium tetrachloride; (2) Distillation: a negative pressure segmented distillation technique is adopted, with an operating pressure of -0.007 to -0.06 MPa and a time of 7 to 8 hours. Since the boiling point of germanium tetrachloride is 83.1℃ and the boiling point of hydrochloric acid is higher, germanium tetrachloride is preferentially distilled out during the distillation process, followed by concentrated hydrochloric acid, and finally dilute hydrochloric acid; (3) Wastewater treatment: the dilute hydrochloric acid is discharged into a wastewater treatment plant for wastewater treatment. This method for recovering germanium and hydrochloric acid from germanium tetrachloride hydrolysis mother liquor has high purity of distilled germanium tetrachloride and a comprehensive recovery rate of germanium greater than 99.5%. The entire process is simple to operate, requires less equipment investment, has low energy consumption, and causes less environmental pollution, making it suitable for large-scale production.

The invention relates to the technical field of metallurgy, in particular to a method for recovering zinc and germanium from germanium-containing zinc concentrate. The specific technical scheme is as follows: after pulpifying and grinding the zinc concentrate, directly carrying out leaching reaction under the conditions of high temperature and high pressure, carrying out settling separation on the reacted slurry, adding zinc and germanium in supernate, adding zinc oxide powder into the supernate for neutralization reaction, filtering to obtain neutralization liquid, adding zinc powder into the neutralization liquid for replacing germanium, and finally adding the zinc powder into the neutralization liquid for replacing germanium. And filtering to obtain germanium precipitation slag and a solution containing zinc and iron. Drying the germanium precipitation slag, performing chlorination distillation treatment to obtain germanium tetrachloride, and performing hydrolysis, filtration, drying and hydrogen high-temperature reduction on the germanium tetrachloride to obtain a metal germanium ingot; the zinc and iron-containing solution is subjected to iron removal, zinc powder replacement, electrolysis and casting to obtain a zinc ingot. According to the method, zinc and scattered metal can be directly leached into the solution to the maximum extent through oxygen pressure leaching, the leaching rate of zinc and germanium is high, the germanium recovery process of the whole process is short, and the recovery rate is high.

The utility model relates to a germanium tetrachloride tail gas treatment device with a multi-stage alkali liquor spraying function, belongs to the technical field of tail gas treatment, and solves the technical problem that a pipeline and tail gas treatment equipment are inconvenient to connect during germanium tetrachloride tail gas treatment. The germanium tetrachloride tail gas treatment device comprises a tail gas treatment mechanism, a gas inlet connector, a gas inlet pipe, a first pipe body and a second pipe body, the tail gas treatment mechanism is provided with a cavity, a plurality of spraying pipes are arranged in the cavity, the gas inlet connector is installed on the tail gas treatment mechanism, one end of the gas inlet pipe is installed on the gas inlet connector, and the other end of the gas inlet pipe is installed on the second pipe body. One end of the first pipe body is installed on the gas inlet connector, one end of the second pipe body is installed on the gas inlet pipe, the other end of the second pipe body is connected to the first pipe body in a clamped mode, and the first pipe body and the second pipe body define a sealing cavity. Therefore, according to the germanium tetrachloride tail gas treatment device capable of spraying the multi-stage alkali liquor, the gas inlet pipe is conveniently connected with the gas inlet connector, leakage of germanium tetrachloride tail gas is reduced, and the germanium tetrachloride tail gas treatment device is more convenient to use.

To provide a rutile-type germanium dioxide free-standing substrate and a method for producing the same, a rutile-type germanium dioxide template and a method for producing the same, a rutile-type germanium dioxide device wafer and a method for producing the same, a method for producing a germanium tetrachloride gas which can grow a rutile-type germanium dioxide crystal, a method for producing a rutile-type germanium dioxide monocrystal which can grow a rutile-type germanium dioxide crystal, and a device for producing a rutile-type germanium dioxide monocrystal which can grow a rutile-type germanium dioxide crystal.SOLUTION: A rutile-type germanium dioxide free-standing substrate comprises a rutile-type germanium dioxide monocrystal. In the germanium dioxide free-standing substrate, the planar density of macro defects appearing on the surface is 5000 / cm2 or less in at least a part of the plane.SELECTED DRAWING: None

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.

The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a lithium-containing single-phase high-entropy negative electrode material and application of the lithium-containing single-phase high-entropy negative electrode material in a lithium battery negative electrode material.The preparation method comprises the following steps that S1, a container A and a container B are taken respectively, deionized water and absolute ethyl alcohol are added into the container A and the container B respectively, and then glacial acetic acid is added; s2, sequentially adding tetraethyl silicate, indium nitrate, germanium chloride, aluminum nitrate, lithium nitrate and citric acid into the container A, and adding tetrabutyl titanate into the container B; s3, mixing the solutions in the container A and the container B, heating and stirring to form gel; s4, drying the gel; and S5, drying and annealing the gel to obtain powder. According to the method, the pure-phase high-entropy oxide is synthesized, the mixed entropy of the high-entropy material is improved while pre-lithiation is performed, the high-entropy effect of the material is enhanced, and therefore the structural stability and thermodynamic stability of the material can be improved.

The invention belongs to the technical field of organic synthesis and relates to a germanium-substituted polymethylene borate compound and a preparation method thereof. The invention uses a polychlorogermanium compound as a starting raw material, has a safe and simple synthesis method, uses inexpensive and readily available reagents, has mild reaction conditions, and has a wide substrate applicability. Various germanium-substituted polymethylene borate esters can be synthesized using a variety of different germanium metal compounds, such as germanium tetrachloride, phenylgermanium trichloride, methylgermanium trichloride, and benzylgermanium trichloride and bis[(pinacol)boryl]methane in the presence of potassium tert-butoxide and an inert gas atmosphere. Developing an efficient method for preparing germanium-substituted polymethylene borate esters from germanium metal compounds has important practical significance in organic synthesis and industrial application.