139 results about "Distillation method" patented technology

The invention relates to the technical field of chemical metallurgy, and discloses a preparation and purification method of high-purity sponge vanadium, which comprises the following steps: preparing a vertical vacuum reduction furnace, adding a reducing agent, discharging air in the furnace, and introducing shielding gas; heating, adding vanadium chloride for smelting, taking out, putting into a distillation furnace, and carrying out heating and heat preservation treatment; and finally, putting the product into a crucible in an electron beam furnace, vacuumizing, heating and smelting, introducing protective gas into the electron beam furnace after smelting, and cooling to room temperature to obtain a sponge vanadium product. The high-purity sponge vanadium is prepared by adopting a novel vanadium chloride metal thermal reduction-distillation method, and the sponge vanadium is further purified through vacuum electron beam refining, so that the common technical problems of long flow, low product purity and the like of a traditional method for preparing the high-purity metal vanadium are solved.

The invention discloses an ammonia distillation method for a garbage incinerator SCR (Selective Catalytic Reduction) system. The problems that existing equipment is high in ammonia water steaming energy consumption and inconvenient to control are solved. The method comprises the following steps; the method comprises the following steps: S1, taking a 20-25% concentrated ammonia water solution as a raw material, and filling the concentrated ammonia water solution into a concentrated ammonia water storage tank for storage; s2, conveying 20-25% of concentrated ammonia water solution in a concentrated ammonia water storage tank into an ammonia distillation tower by using a first metering pump; ammonia gas in the concentrated ammonia water solution is separated out by using an ammonia distillation tower and is used for SCR (Selective Catalytic Reduction) denitration reaction; s3, dilute ammonia water generated at the bottom of the ammonia still is pumped out by a second metering pump and conveyed into a dilute ammonia water buffer tank for temporary storage, and the concentration of the dilute ammonia water is below 5%; s4, denitration is completed through a catalyst. The method has the beneficial effects that ammonia for SCR and SNCR in flue gas treatment equipment of the garbage incinerator is combined together, the ammonia still is used for separation and purification, ammonia gas is sprayed into the SCR, and raw materials of a reducing agent, the equipment cost and the operation cost are saved.

The present invention introduces a capillary distillation method comprising the following steps: heating wastewater, subsequently directing the heated wastewater to one end of a water-diversion fiber material. Through capillary action, the heated wastewater permeates the water-diversion fiber material, diffusing downward along microchannel pathways within the material. Upon reaching the surface of the water-diversion fiber material, the wastewater evaporates. Water vapor is then directed to a condensation module, where it undergoes condensation and collection, resulting in the production of fresh water.

A manufacturing process of metal-organic framework porous material of aluminium and terephthalic acid comprises the steps of aluminium substrate synthesis with elution of aluminium ions from the aluminium substrate using a basic solution followed by adjustment of pH using an acidic solution; terephthalic acid synthesis from polyethylene terephthalate (PET) by distillation method in a basic solution followed by adjustment of pH using an acidic solution to yield terephthalic acid precipitate, filtering, drying and dissolving of the obtained terephthalic acid in a basic solution until equivalent; addition of the aluminium substrate for a reaction; separation of the obtained precipitate of the metal-organic framework porous material product from solution; and drying.

The invention provides a production method of high-purity sponge titanium. The production method comprises the following steps: firstly, obtaining refined magnesium and refined titanium tetrachloride after secondary refining; then feeding the refined magnesium and the refined titanium tetrachloride into a reactor subjected to titanizing treatment, and carrying out reduction and vacuum distillation in a protective atmosphere by adopting a reduction distillation method to obtain a sponge titanium lump; and finally, the sponge titanium lumps are subjected to surface impurity material stripping, then temperature-controlled crushing and screening are conducted, four-stage sorting including color sorting, magnetic sorting, winnowing and manual sorting is conducted, and the high-purity sponge titanium is obtained. According to the method, the refined titanium tetrachloride is used for purifying the crude magnesium, so that the high-purity production raw material is obtained; in the magnesiothermic reduction vacuum distillation process of titanium tetrachloride, a blocking method of impurities of Fe, Cr and Ni is adopted, and a pure sponge titanium lump is obtained; and identifying and separating high-iron, high-chlorine, high-oxygen and high-nitrogen impurity materials in the sponge titanium by adopting sorting methods such as color sorting, winnowing, screening, magnetic separation and the like to finally obtain the high-purity sponge titanium.

The invention discloses a method for preparing high-purity octamethylcyclotetrasiloxane, and belongs to the technical field of octamethylcyclotetrasiloxane purification. The invention treats crude octamethylcyclotetrasiloxane by combining distillation-adsorption-re-distillation, thereby overcoming the problem that trace impurities are difficult to be removed by a single distillation method. The distillation-adsorption-re-distillation method is combined for operation, and the advantages of each method are brought into play, and impurities such as hexamethylcyclotrisiloxane and decamethylcyclopentasiloxane with similar boiling points are reduced, so that the octamethylcyclotetrasiloxane product reaches a very high purity. The invention adopts an adsorption treatment method to adsorb and separate phosphorus-containing and boron impurities and metal impurities in alkane residues in the octamethylcyclotetrasiloxane, thereby obtaining electronic-grade octamethylcyclotetrasiloxane, and the product purity can reach more than 99.99%.

The invention discloses a rectification method for efficiently producing high-purity methanol by using low-temperature heat. According to the technology, a pressurized tower and an atmospheric tower are connected in parallel, so that crude methanol from a pre-tower kettle enters the two towers in a split-flow manner, low-temperature heat is used for supplying heat, and steam at the top of the pressurized tower serves as a heat source of a reboiler of the atmospheric tower; a tower section heat exchanger which can be flexibly arranged is arranged in the vacuum tower to utilize low-temperature heat; and thirdly, a recovery tower is changed into a vacuum tower, and low-temperature heat is used as a heat source of a reboiler. The technology can be flexibly implemented partially or completely, and a remarkable energy-saving effect can be achieved. The embodiment shows that the technology can stably produce high-precision methanol with the ethanol content as low as 10 ppm or below, the fresh steam consumption per ton of methanol is reduced to 0.2 ton or below, the productivity of the device can also be improved, and compared with a traditional four-tower double-effect rectification technology (the ethanol content is about 50 ppm, and the fresh steam consumption per ton of methanol is 1.0-1.2 tons), the technology has remarkable advantages in the aspects of product purity reduction and energy consumption reduction. The method effectively solves the problems of difficult production of high-precision methanol, high energy consumption and insufficient utilization of low-temperature heat in the prior art, and has good economic and environment-friendly benefits.

The continuous production heat pump assisted integrated extractive distillation device is adopted to realize high-purity separation and recovery of the diethyl ether-methyl formate-n-pentane azeotrope, and separation is realized by utilizing the characteristic that the extraction agent has great influence on the relative volatility of the diethyl ether-methyl formate-n-pentane azeotrope. The purity of the separated diethyl ether, n-pentane and methyl formate reaches 99.9% or above, high-purity recycling of the extraction agent can be achieved, the separation cost is greatly reduced, and the method is low in energy consumption and flexible to operate.

A distillation method includes supplying a batch type distillation column with a liquid that is a process fluid; increasing pressure and temperature of a fluid, with a compressor and supplying the fluid to a reboiler; exchanging heat in the reboiler between the liquid, which has been supplied to the distillation column, and the fluid, which has been increased in pressure and temperature, to heat the liquid and acquire overhead vapor and to condense the fluid; delivering the overhead vapor to a condenser and condensing the overhead vapor into a condensate through heat exchange, removing the condensate; removing residual liquid from the distillation column; and regulating pressure of the distillation column to distill the liquid with heat generated by a heat pump operated over a narrower temperature rising range in the pressure-temperature increasing step.

The invention relates to the technical field of distillation, in particular to a distillation device for production and collection of triisopropyl borate and a distillation method.The distillation device comprises a distillation device body, the distillation device body comprises a distillation retort, the distillation retort comprises a retort body and a cover body internally provided with a rotating core structure, and the rotating core structure is composed of a mixing component and a guiding component which are coaxially connected; the mixing part is of a hollow spiral structure, and the guiding part is of a solid spiral structure. Heat generated by the spiral heating pipe in the wall of the tank body and the annular heat-conducting oil disc at the bottom can be quickly conducted into materials in the distillation cavity through a through heat conduction channel in the hollow mixing screw piece, the drainage screw piece rotates to drive the heated gaseous materials to form a spiral ascending flow field, and the spiral ascending flow field is formed by combining an umbrella-shaped flow guide cover; steam can be directionally guided to a gas state conveying opening, and disordered diffusion and reverse mixing of the steam are reduced; in addition, the raw materials directly enter the gas-liquid balance area through the middle feeding port, and the back-mixing probability is further reduced.

This invention relates to the field of separation and purification, and particularly to a distillation method for Forsythia suspensa volatile oil, comprising the following steps: Step (1) Crush dried Forsythia suspensa fruit and mix it with water at a mass ratio of 1:3-5, grinding until the particle size D90≤50μm to obtain Forsythia suspensa slurry; Step (2) Add porous medium A particles with a particle size of 0.5-1mm and water-absorbing medium B to the Forsythia suspensa slurry obtained in Step (2), stir and mix for 20-40min to obtain a cake; Step (3) Mix the cake with moistened porous medium C particles with a particle size of 1-3cm, then load it into a distillation kettle for distillation, collect the distillate and separate to obtain Forsythia suspensa volatile oil. This scheme optimizes the distillation process, improves distillation efficiency, and solves the clogging problem caused by excessively fine grinding of raw materials, thereby meeting the industrial production demand for efficient and stable extraction of Forsythia suspensa volatile oil.

This invention discloses a method for preparing high-purity Si-75, comprising: S1, adding sodium sulfide, sulfur, and deionized water in a molar ratio of 1:(1.0~1.1):(5~8) to a reaction vessel, adding a buffer, and reacting at 80~90℃ for 1~2h; S2, adding a phase transfer catalyst and a hydrolysis inhibitor to the system, adding γ-chloropropyltriethoxysilane dropwise, and reacting at 85~95℃ for 3~5h, allowing the mixture to stand and separate into layers after the reaction, to obtain an organic phase; S3, subjecting the organic phase to short-path distillation and then filtering to obtain high-purity Si-75. Compared with existing technologies, this invention uses a phosphorus-free buffer system, which simplifies waste treatment. It uses water as the reaction medium and does not use large amounts of organic solvents, making it suitable for continuous industrial production. By adding hydrolysis inhibitors, hydrolysis can be effectively prevented during the reaction, increasing safety. The short-path distillation method provides high purification efficiency and can quickly remove impurities. The product has a disulfide content of ≥98.5% and a color of 0 (Gardner color number), which is of great significance to the light-colored rubber industry.

The application provides a purification method and dichloroisocyanurate obtained by using the method. The purification method of dichloroisocyanurate comprises the following steps: repeatedly crystallizing crude dichloroisocyanurate obtained in a production synthesis process to obtain purified dichloroisocyanurate. The purification method of dichloroisocyanurate of the application utilizes the different melting points of dichloroisocyanurate and other impurities, and is designed to be repeatedly crystallized at different gradient temperatures. By adjusting the crystallization temperature and the crystallization time, the impurities in the dichloroisocyanurate can be removed. Compared with the crude distillation method, the obtained dichloroisocyanurate has higher purity, and is safer and easier to operate.

The embodiment of the present application belongs to the technical field of seawater desalination, and particularly relates to a seawater distillation module, a seawater distillation device, a seawater distillation system and a distillation method. The seawater distillation module comprises a material liquid layer, an air gap layer, a gas permeable layer and a condensation layer. The material liquid layer has an inlet liquid side for guiding seawater to enter and an outlet liquid side for guiding seawater to flow out. The air gap layer is arranged opposite to the material liquid layer. The gas permeable layer is arranged between the material liquid layer and the air gap layer, and is used for separating the material liquid layer and the air gap layer. The gas permeable layer is used for allowing the seawater in the material liquid layer to pass through after being heated, and enter the air gap layer. The condensation layer is used for condensing the water vapor entering the air gap layer, so as to produce fresh water. Compared with the prior art, the seawater distillation device can meet the production of fresh water in island reef areas.

The application discloses a distillation device and method for nitric acid purification, and relates to the technical field of nitric acid distillation.The distillation device for nitric acid purification comprises a device frame, a motor is fixedly installed above the device frame, an exhaust pipe is fixedly installed on the circumferential surface of the device frame, a feed pipe is fixedly penetrated through the circumferential surface of the device frame, an air outlet pipe is fixedly penetrated through the circumferential surface of the device frame, a condenser pipe is fixedly installed in the device frame, and the device frame is internally provided with a rotating rod, a connecting pipe, a rotating shaft, a fan blade, a convex plate, a supporting block, a connecting plate, a sleeve, a circular plate, an arc block, a supporting plate and an arc plate.The rotating rod is fixedly installed at the output end of the motor, the connecting pipe is fixedly installed in the device frame, and the rotating shaft is rotatably installed on the circumferential surface of the connecting pipe.The distillation device for nitric acid purification realizes the up-and-down movement of the fan blade while rotating, prevents the internal stratification of nitric acid, and causes incomplete distillation.

The embodiment of the invention relates to the technical field of low-temperature rectification, in particular to a low-temperature rectification system and a low-temperature rectification method.The system comprises a condensation part used for conducting gas-liquid separation on tower top process materials and conveying liquid materials to a reboiling part, and steam is conveyed to a first heat regeneration part; the first heat regeneration part and the second heat regeneration part are used for heating the steam to a preset temperature; the compression assembly is used for compressing steam and conveying the steam to the reboiling part and the first heat exchange part; the reboiling part is used for heating the liquid material to gasify the liquid material and conveying the gas material to the condensing part; the first heat exchange piece is used for heat exchange of steam; the first heat exchange piece and the reboiling piece are used for conveying liquid materials into the first heat return piece to be cooled, and the circulation driving piece is used for circulating the materials to the condensation piece. According to the low-temperature rectification system, heat can be provided for the reboiling part, the energy consumption of the reboiling part is reduced, cold energy can be provided for the condensation part, the energy consumption of the condensation part is reduced, and then the energy consumption of the whole low-temperature rectification system is reduced.

This invention discloses an energy-saving five-tower methanol distillation method based on multi-effect thermal coupling. Crude methanol is fed to a pre-tower for distillation; the bottom product of the pre-tower is fed to an atmospheric distillation tower, the bottom product of the atmospheric distillation tower is fed to a negative pressure distillation tower, and the bottom product of the negative pressure distillation tower is fed to a pressurized distillation tower; the bottom product of the pressurized distillation tower is fed to a secondary pressure distillation tower; refined methanol is collected from the tops of the pressurized distillation tower, the atmospheric distillation tower, the negative pressure distillation tower, and the secondary pressure distillation tower; the top product of the pressurized distillation tower heats the reboiler of the secondary pressure distillation tower, and the top product of the secondary pressure distillation tower heats both the reboilers of the pre-tower and the atmospheric distillation tower; the top products of the pre-tower and the atmospheric distillation tower heat the reboiler of the negative pressure distillation tower. This process improves the heat recovery efficiency within the system, significantly reduces the condensation load of the top vapor, lowers the overall energy consumption of the distillation process, and achieves efficient multi-stage heat recovery and utilization within the system, reducing the ethanol content in the refined methanol product and improving methanol recovery efficiency.

The invention discloses a preparation method for continuous production of phosphorus trifluoride, and belongs to the technical field of chemical synthesis, and the key point of the technical scheme is that the preparation method for continuous production of phosphorus trifluoride comprises the following preparation steps: S1, adding phosphorus trichloride into the upper part of a rectifying tower, adding anhydrous hydrogen fluoride gas into the lower part of the rectifying tower, and stirring; contacting the two raw materials on the surface of the rectifying tower filler to complete reaction; s2, a product obtained through reaction is discharged from the top of the rectifying tower and enters a purification system, and phosphorus trifluoride is obtained.When phosphorus trifluoride is prepared through the rectifying method, the reaction process is stable, the temperature is easy to control, the gas-liquid contact area is large, the reaction is complete, the reaction speed is high, and large-batch production is facilitated.

A micro-distillation device comprises: a distillation unit including a liquid introduction port for introducing a mixed liquid containing at least two components having different boiling points, a vapor introduction port for separately introducing vapors originating from the mixed liquid, a gas-liquid contact flow path in which the mixed liquid introduced from the liquid introduction port and the vapor originating from the mixed liquid introduced from the vapor introduction port are brought into contact with each other in counterflow, a liquid discharge port for discharging the mixed liquid flowing through the gas-liquid contact flow path, and a vapor discharge port for discharging the vapor originating from the mixed liquid flowing through the gas-liquid contact flow path; a first circulation unit in which a condensate obtained by condensing the vapor originating from the mixed liquid discharged from the vapor discharge port is circulated to the liquid introduction port; and a second circulation unit in which a vapor obtained by evaporating the mixed liquid discharged from the liquid discharge port is circulated to the vapor introduction port.

The utility model discloses a novel motherwort biochemical mixture distillation extraction device in the related technical field of veterinary drug production, which comprises a distillation box and a filter box, the top of the distillation box is provided with an upper top cover, the upper top cover is provided with a hanging ring, the inner bottom of the distillation box is provided with a heater, and the filter box is provided with a filter screen. A limiting sleeve is arranged on the inner side of the lower portion of the distillation box, a supporting block is arranged on the inner side of the limiting sleeve, a containing basket is placed on the supporting block, a partition supporting plate is arranged at the position, close to the upper portion, in the containing basket, and the partition supporting plate is rotationally connected with a containing basket body through a rotation matching base. According to the utility model, the containing basket is arranged in the distillation box, and the separation supporting plate which is rotatably mounted is arranged in the containing basket, so that medicinal raw materials can be classified and placed according to the leaching temperature conditions of different medicinal materials, and two distillation modes of water boiling and steam fumigation are divided, so that medicinal components in the medicinal materials are fully released.

The invention discloses a vacuum distillation device and a distillation method, belonging to the technical field of distillation devices, wherein the vacuum distillation device comprises a tank body for distillation, a water tank is arranged below the tank body, a partition is slidably arranged between the tank body and the water tank, a fixed pipe is installed on the tank body, a sleeve is rotatably installed on the partition, and a base is arranged in the water tank; the water volume in the water tank can be adjusted by cooperating with the set guide pipe and the fixed pipe, when the water volume in the water tank is small, the sleeve can drive the guide pipe to rotate during the counterclockwise rotation process, and in the process of multiple alignment of the through hole and the guide hole, the water on the top of the partition can flow back into the water tank, so that the water level in the water tank is higher than the liquid level of the raw material in the tank body, therefore, the water tank can be replenished with water in time by utilizing this structure, which is beneficial to uniformly heating the raw material in the tank body.

A distillation device includes a batch type distillation column, a reboiler that heats and vaporizes liquid, which is a process fluid supplied to the distillation column, into vapor, a displacement compressor that draws in fluid for heating the liquid and increases the fluid in pressure and temperature, and supplies the fluid to the reboiler, a condenser that condenses overhead vapor of the distillation column into a condensate, a distillate withdrawal portion that removes the condensate condensed by the condenser, and a discharged liquid withdrawal portion that removes residual liquid from the distillation column. The compressor includes an actual volume flow rate regulation mechanism that varies an actual volume flow rate of the fluid, which is increased in pressure and temperature by the compressor, in accordance with a change in a required heating temperature of the reboiler during operation of the distillation device.

The present invention relates to a method for cleaning rock samples from petroleum systems based on the use of nanofluids, which is able to significantly accelerate the process. The developed method combines the solubilization potential of nanofluids for oil under the temporary action of an ultrasound system, which is faster and more effective than the traditionally used distillation methods described in the prior art. The adopted process reduces the time required for the removal of oil and salts (a key step in the characterization process of rock samples, which usually takes 120 to 365 days) to 3 to 7 days, using water-based nanofluids of low toxicity that do not alter the properties of the rock.

The invention belongs to the technical field of drilling fluid measurement, and particularly provides an optical measurement device and measurement method for the solid phase content of composite brine drilling fluid, a multi-wavelength laser emits a light beam, the light beam passes through a sample test bench, a cuvette and a drilling fluid sample in the cuvette, and then enters a photoelectric detector; the photoelectric detector is used for measuring the transmission light intensity of the drilling fluid sample in the sample test bench, and the data acquisition display is used for acquiring and transmitting the transmission light intensity of the measured drilling fluid sample to SCOM calculation processing software of the computer; the problems that when an existing composite brine drilling fluid adopts a distillation method to measure the insoluble solid content, the measurement process is complex, distillation and titration experiments consume a long time, and the measurement error is large are solved. According to the method, the influence of precipitation of inorganic salt or organic salt in the distillation process on solid phase content measurement when the solid phase content of the composite brine drilling fluid is measured by a traditional distillation method is eliminated, the measurement process is simplified, the measurement time is shortened, and the measurement precision and the measurement efficiency are improved.

Title of the invention: Method for defrosting an air separation apparatus by cryogenic distillation. During the defrosting of an air separation apparatus by cryogenic distillation, defrosting gas is sent to a heat exchanger (15) and from the heat exchanger to the top of a column (21) via a line (C6) used in normal operation to draw nitrogen, entering the column, defrosting gas is drawn from the tank of the second column via a line and sent to the heat exchanger and then to the air, a flow of defrosting gas is sent to the top of another column via a line (C7) at a temperature above 0°C, defrosting gas is drawn from the other column via the line used in normal operation to send air to the other column, sent to the heat exchanger and sent to the air. Abstract figure: Fig. 2

The present invention provides a method for distilling liquor using superheated steam and a distiller, the distillation method comprising: a superheated steam generator is powered on, and a heater inside the generator heats pure water into saturated steam and then further heats it into superheated steam; after the superheated steam enters the superheated steam desuperheater, the superheated steam uses its own pressure to pass through a diffuser flow channel at high speed, the steam flow rate generates a vacuum pressure, and the light alcohol and tail liquor are vacuum-sucked into the diffuser flow channel through a liquid inlet pipe, and are blown away and atomized under the action of vacuum and high flow rate, while the superheated steam mixes and absorbs the atomized light alcohol and tail liquor at high speed in the ejector flow channel to become mixed steam, and the mixed steam reduces the temperature, pressure and flow rate in the amplification section of the ejector bell mouth; the superheated steam technology used in the present invention is mature, safe and reliable, and similar types of technologies have been widely used in the thermal industry, so the use risk in the industry is relatively small, the production cost is low, and the operation is stable.

This application discloses an automated distillation method and system for Maotai-flavor liquor based on dual-stillation collaboration, belonging to the field of Maotai-flavor liquor brewing technology. The method is implemented using a system with a dual-stillation shared detection module, an intelligent decision-making module, and a valve island control execution module. It includes first calibrating the alcohol content thresholds and process parameters for the heads, main body, and tails of the liquor according to the brewing cycle; then completing system self-checks such as pipeline cleaning and sensor calibration; scheduling dual-stillation operations based on the distillation time difference; collecting liquor parameters in real time; automatically completing the graded distillation and path switching for the heads, main body, and tails; determining distillation termination based on alcohol content and duration; supporting rotation of dual-stillation detection stations; and finally, resetting the system and archiving data. This technical solution achieves full automation and standardization of the distillation process, improves the yield and quality stability of high-quality liquor, reduces hardware investment and labor costs, avoids the subjective errors and timeliness issues caused by manual operation, and is suitable for large-scale dual-stillation production of Maotai-flavor liquor.

The present disclosure provides an equipment for production of butanol and octanol and a triple-effect distillation method, comprising two processes: butanol separation and octanol separation, both processes use same feedstocks to obtain n-butanol, iso-butanol and octanol products through different procedures, respectively, wherein butanol separation process is sequentially divided into hydrogenation, removal of light and heavy components and separation of isomeric; and octanol separation process is sequentially divided into separation of isomeric, hydrogenation and removal of light and heavy components; the removal of light and heavy components for butanol is carried out by a butanol pre-distillation column and a butanol distillation column, and the separation of isomeric for butanol is carried out by a first butanol isomer column and a second butanol isomer column; and the separation of isomeric for octanol is carried out by a first butyraldehyde isomer column and a second butyraldehyde isomer column.

The present invention relates to the technical field of chemical metallurgy, and provides a method for preparing and purifying high-purity vanadium sponge. The method comprises: preparing a vertical vacuum reduction furnace, adding a reducing agent thereto, removing air from the furnace and introducing a protective gas thereinto; performing heating, adding vanadium chloride, then performing smelting, and after removal, placing same into a distillation furnace for heating and temperature-holding treatments; and finally, placing a product into a crucible in an electron beam furnace, performing evacuation, heating same to perform smelting, introducing a protective gas into the electron beam furnace after smelting, and cooling same to room temperature, so as to obtain a vanadium sponge product. In the present invention, high-purity vanadium sponge is prepared from a chloride of vanadium by means of a new metallothermic reduction-distillation method, and is further purified by means of vacuum electron beam refining. Therefore, the common technical problems of a long process, a low product purity, etc., during the preparation of high-purity vanadium metal by means of traditional methods are solved.

The invention provides a black shale Carius pipe complete sample dissolving method which comprises the following steps: weighing a black shale sample, adding the black shale sample into a sample dissolving tank, adding HF into the sample dissolving tank, and standing to dissolve the sample to obtain a pre-dissolved solution; the pre-dissolved solution is heated, HCl is added for acid removal when the pre-dissolved solution is heated to be nearly dry, and acid removal is repeated for multiple times so that HF can be removed; adding HCl into the pre-dissolved solution after acid removal, completely transferring the pre-dissolved solution into a Carius tube, adding a mixed diluent and a sample dissolving reagent into the Carius tube, and carrying out Carius tube sealing and complete sample dissolving to obtain a sample dissolving solution; separating Re and Os in the sample dissolving solution by adopting a direct distillation method; and enriching and purifying Re in the distillation residual solution and Os in the distillation absorption liquid to respectively obtain a to-be-measured Re sample and an Os sample. According to the method, it is guaranteed that Re and Os are almost not lost, and meanwhile complete sample dissolving of organic matter-rich sedimentary rock samples such as black shale is effectively achieved.