933 results about "Vacuum distillation" patented technology

The present application belongs to the technical field of non-ferrous metal smelting, and provides a method for the vacuum directional vulcanization and arsenic removal of arsenic-containing solid waste from copper smelting. In the present application, black copper sludge and contaminated acid sulfide slag are mixed and then smelted under vacuum conditions to achieve the directional vulcanization of the black copper sludge by the contaminated acid sulfide slag, so as to generate Cu2S and metal As; and then the vulcanization product is subjected to vacuum distillation according to the difference of saturated vapor pressures, such that As is condensed in a condensation area in a vapor form; and Cu2S is not volatilized and left in residues, thereby achieving the separation of Cu2S and metal As. The present application achieves the recovery of arsenic from the black copper sludge and the contaminated acid sulfide slag, such that non-toxic metal arsenic having an economic value is obtained; in addition, the generated Cu2S can be directly returned to a copper blowing system, thereby achieving the comprehensive utilization of valuable elements. After the treatment by means of the method of the present application, the recovery rate of Cu2S is higher than 90%, and the purity is greater than 95%, thereby satisfying the purity standard of copper matte in copper blowing; and the direct recovery rate of condensed As is higher than 90%, and the purity is greater than 99.5%.

The present invention provides a method for refining crude lithium, and belongs to the technical field of metal purification. The present invention melts the crude lithium material and then performs a first static sedimentation to obtain a supernatant melt 1, a low-impurity crude lithium melt, and a high-impurity crude lithium melt from top to bottom; the supernatant melt 1 is subjected to vacuum distillation under the condition of electromagnetic stirring without a paddle to volatilize low-boiling impurities, and then subjected to a second static sedimentation to form a bottom lithium melt and a supernatant melt 2; the supernatant melt 2 is separated to obtain purified lithium. The present invention performs vacuum distillation under the condition of electromagnetic stirring without a paddle, which not only realizes dynamic distillation of materials, reduces the distillation temperature, and improves the direct recovery rate of lithium, but also prevents the occurrence of cold zones inside to cause condensation and reflux of Na and K, thereby reducing the distillation efficiency and preventing secondary contamination of the product.

The invention discloses a method for preparing 6N high-purity zinc, comprising the following steps: S1, alkali dissolution: dissolving electro zinc with sodium hydroxide, filtering after the reaction is completed; S2, acidification: adding hydrochloric acid to the filtered solution for acidification; S3, evaporation concentration: putting the acidified solution into an evaporating kettle for evaporation concentration; S4, freezing crystallization: filtering and drying the concentrated solution after cooling in a freezing tank; S5, secondary dissolution: dissolving the dried zinc chloride solid in an ether solution at room temperature, filtering; S6, vacuum distillation: putting the filtered ether solution into a vacuum distillation device, S7, heating and decomposing; S8, vacuum distillation. This method can achieve the purpose of preparing 6N high-purity zinc from electro zinc, and realize the low-cost recycling of zinc resources; at the same time, the alkali dissolution-acidification-ether secondary dissolution process can be used to effectively separate metals such as cadmium with a segregation coefficient close to 1 in zinc, which is convenient for the rear-end pyrometallurgical method to purify 6N high-purity zinc.

The invention discloses a method for preparing 6N-grade high-purity zinc through twice vacuum distillation based on a uniform temperature field. The method comprises the following steps: pretreatment; first-stage distillation: putting the zinc ingot subjected to vacuum drying into a crucible of a vacuum distillation furnace, mounting a plurality of stages of condensation collecting trays on the top of the crucible in an overlapping manner, and then performing high-vacuum pumping, heating and heat preservation; second-stage distillation: after the heat preservation of the first-stage distillation is finished, heating and heat preservation are continued under high vacuum; a plurality of samples are respectively obtained from the multistage condensation collecting disc, and the samples with the zinc content not lower than 99.9999% are collected, namely the 6N-grade high-purity zinc product. According to the method, zinc ingots with the purity of 99.99%-99.995% are used as raw materials, a conventional vacuum distillation furnace is used as distillation equipment, multiple stages of condensation collecting plates are mounted on the top of a crucible in an up-and-down overlapping manner, a novel two-stage distillation process is developed in a matched manner, key parameters such as the vacuum degree, the heating temperature, the heating rate and the heat preservation time are accurately controlled, and the high-purity zinc ingot is obtained. And a 6N-grade high-purity zinc product is successfully prepared.

The invention discloses dibutyl adipate as well as a preparation method and application thereof, preparation raw materials comprise adipic acid, n-butyl alcohol and a catalyst, and the molar ratio of the adipic acid to the n-butyl alcohol to the catalyst is 1: (3-8): (0.001-0.005). Excessive n-butyl alcohol obtained through distillation and kettle residues obtained after vacuum rectification can be directly applied to the next batch of reaction, continuous circular reaction can be achieved by supplementing a small amount of catalyst, maximum utilization of raw materials is achieved, and the production cost is reduced. Compared with the product obtained by the prior art, the content of the product obtained by simple rectification is higher, the content of dibutyl adipate in the product is 99.8% or above, the risk of trace activated carbon residue after activated carbon adsorption treatment is avoided, and the cosmetic grade product standard is met.

The invention discloses a resource regeneration method of waste lubricating oil, relates to the technical field of petrochemical engineering, and belongs to the patent classification number C10M175 / 06. The preparation method comprises the following steps: adding a composite flocculant into the waste lubricating oil, heating and stirring, and then carrying out magnetic separation to obtain pretreated waste lubricating oil; uniformly mixing the pretreated waste lubricating oil, glycerol and a Ni / Al2O3 catalyst, then heating and reacting under pressure, and cooling to room temperature to obtain a catalytic hydrogenation product; and carrying out reduced pressure distillation on the catalytic hydrogenation product, recovering the lubricant base oil fraction, adding methanol and concentrated sulfuric acid into the distillation residual liquid, heating for esterification reaction, and separating the liquid to obtain the biodiesel. In the pretreatment process, the composite flocculant is used for removing acid and particle impurities in the lubricating oil, a traditional alkali adding neutralization precipitation process is replaced, the method is environmentally friendly, and the recovery cost of enterprises is reduced.

The invention relates to the technical field of petrochemical corrosion failure and protection, and discloses a dew point corrosion high-risk area prediction method suitable for an atmospheric and vacuum distillation unit, and the method comprises the steps: firstly obtaining the technological characteristics of a to-be-tested device and the physical property data of processing raw oil; constructing a process calculation model of the to-be-tested device according to the process characteristics and the physical property data; solving logistics parameters in the device to be tested by using the process calculation model, and analyzing logistics distribution characteristics in the device; the material flow distribution characteristics comprise phase distribution characteristics, temperature distribution characteristics, component distribution characteristics and concentration distribution characteristics; calculating the dew point temperature in the device to be measured; and finally, determining a high-risk area in which low-temperature dew point corrosion occurs in the device to be detected in combination with the material flow distribution characteristics and the dew point temperature. According to the method, quick and accurate prediction of the corrosive components in the dew point corrosion high-risk area in the atmospheric and vacuum distillation unit is realized.

A process for purifying a crude cis-2-olefine acid by thermal separation, the process comprising subjecting the crude cis-2-olefine acid to wiped-film evaporation or vacuum distillation under a temperature-reduced pressure curve, thereby minimizing the isomerization of the cis-2-olefine acid to trans-2-olefine acid.

The invention provides a preparation method and system of high-purity metal rubidium or cesium, the method comprises the following steps: taking metal rubidium or cesium as a raw material, taking molten metal Ag as an extraction medium, utilizing the characteristics that Na, Li and K have certain solubility in metal Ag and rubidium and cesium are insoluble in Ag, reducing the content of impurities Na, Li and K in the metal raw material rubidium or cesium, and then carrying out vacuum distillation to obtain the high-purity metal rubidium or cesium. According to the method, purification and impurity removal are conducted on the metal rubidium or cesium through melt extraction, the metal raw material rubidium or cesium can be treated to prepare the high-purity metal rubidium or cesium product, the purification rate of Na and Li is 80% or above, the purification rate of K is 50% or above, the purity of the prepared high-purity rubidium is 99.90% or above, the purity of the prepared high-purity cesium is 99.95% or above, the yield is 95% or above, the technological process is short, equipment is simple, and the method is suitable for industrial production. The problems of low efficiency and unobvious impurity removal effect of traditional distillation are solved.

The invention relates to a preparation method of soybean oil base polyhydric alcohol, in particular to a method for preparing soybean oil base polyhydric alcohol by directly using soybean oil. The soybean oil diluted by using a solvent reacts with hydrogen peroxide with the weight percentage being 30% for 2-5 hours at the temperature of 60-70 DEG C under catalysis of a catalyst with the weight percentage being 3-5%; vacuum distillation is conducted after the reaction is ended, and the solvent is evaporated; then low alcohol is added in a reactor to be subjected to a reaction for 4-6 hours under the pressure of 0.3-0.4 MPa and at the temperature of 70-80 DEG C, then the reaction is stopped, and the soybean oil base polyhydric alcohol is obtained. The method saves the using amount of hydrogen peroxide, reduces the post-treatment steps, and simplifies the production procedures, and accordingly the product cost is declined directly.

The invention discloses a molecular-level atmospheric and vacuum corrosion simulation method and device, and the method comprises the steps: obtaining first macroscopic property data of current crude oil according to a crude oil physical property analysis model; according to a preset corrosion molecule library and the first macroscopic property data, obtaining a first molecule concentration of corrosion molecules in the current crude oil; acquiring virtual components of corrosion molecules in the current crude oil according to a preset physical property database and the first molecular concentration; and according to preset DCS data and the virtual components of the corrosion molecules, carrying out corrosion iteration simulation on the atmospheric and vacuum distillation unit, and outputting a simulation result of the distribution of the corrosion molecules at each part in the atmospheric and vacuum distillation unit. Compared with the prior art, the accuracy and timeliness of corrosion molecule distribution prediction of each part of the atmospheric and vacuum distillation unit can be improved.

The utility model relates to the technical field of paste reaction equipment, in particular to a reduced pressure distillation device of a paste reaction kettle, which comprises a reaction kettle, an inner barrel is arranged in the reaction kettle, a spiral conveying plate is rotatably mounted in the inner barrel, and the bottom end of the spiral conveying plate extends out of the inner barrel; the paste stirring device has the beneficial effects that the inner barrel is arranged in the reaction kettle, the spiral conveying plate is arranged in the inner barrel, paste at the bottom of the reaction kettle can be conveyed upwards through the inner barrel through rotation of the spiral conveying plate, and then the paste falls into the reaction kettle from the top end of the inner barrel, so that the paste stirring effect can be achieved, and the paste can be uniformly stirred; and the temperature of the hot water flowing from top to bottom through the spiral pipe is gradually reduced from top to bottom due to heating of the paste, and at the moment, the lower temperature at the bottom preheats the upward paste in advance, and then the higher temperature at the top quickly heats the paste, so that the reaction efficiency is improved.

The invention discloses a method for synthesizing and purifying a lybula intermediate, and belongs to the technical field of organic synthesis. In order to solve the problems of complicated operation, low yield, low purity and the like in the prior art, the invention provides a synthesis and purification method of a lyboxadone intermediate, which comprises the following steps: taking a compound II as a raw material, carrying out oxidation reaction in a toluene aqueous solution under the action of a catalyst and an oxidizing agent to generate a compound I, carrying out quenching reaction, adjusting pH, and collecting a water phase to obtain the lyboxadone intermediate. Under the action of acetonitrile and acetone, crystallizing to obtain a compound I; according to the method, the crystallization solvent is optimized and screened, the adding sequence and proportion of the solvent and the crystallization temperature are controlled, the high-purity intermediate compound I of the Lescalobolifera is obtained at high yield, seed crystal preparation, gradient cooling, reduced pressure distillation and the like are not needed, and operation is greatly simplified.

The invention discloses a method for preventing a vacuum distillation channel for producing sponge titanium in an inverted U-shaped furnace from being blocked, which comprises a distillation electric furnace heating step, a low-vacuum distillation step and a high-vacuum distillation step, in the distillation electric furnace heating step, the temperatures of a first area and a second area of a distillation electric furnace are controlled to be 950-980 DEG C, the temperatures of a third area and a fourth area of the distillation electric furnace are controlled to be 900-980 DEG C, and the temperature of a third area and the temperature of a fourth area of the distillation electric furnace are controlled to be 950-980 DEG C; the temperatures of the fifth area and the sixth area of the electric distillation furnace are controlled to be 920-980 DEG C; according to the method, the evaporated Mg and MgCl2 gas can be prevented from being condensed at the condenser channel, and the quality of the sponge titanium is guaranteed.

A preparation method of 5N high-purity antimony comprises the following steps: (1) hydrolysis: taking ethylene glycol antimony as a raw material, and carrying out pyrohydrolysis pretreatment to obtain antimony trioxide; (2) biological reduction: uniformly mixing antimony trioxide with an organic catalytic reduction covering agent, and carrying out reduction smelting to prepare 4N antimony; and (3) vacuum distillation: the 4N antimony is subjected to two-stage vacuum distillation, namely first-stage high-temperature vacuum distillation and second-stage low-temperature vacuum distillation, and the 5N high-purity antimony is obtained. According to the method, an ethylene glycol antimony product is adopted as a raw material and subjected to hydrolysis-biological reduction and multi-field synergistic enhanced vacuum distillation to obtain 5N high-purity antimony, the total amount of impurity elements of the product is controlled to be 10 ppm or below, the content of key impurity elements As is controlled to be 1 ppm or below, the content of Pb is controlled to be 0.2 ppm or below, the content of Bi is controlled to be 0.2 ppm or below, the content of Cu is controlled to be 0.05 ppm or below, and the content of Fe is controlled to be 0.5 ppm or below.

The invention relates to a method for preparing a rosuvastatin calcium intermediate, and belongs to the technical field of drug intermediate synthesis. The method comprises the following steps: under the protection of nitrogen, carrying out reflux reaction on raw materials including 4-fluorobenzaldehyde and ethyl 4-methyl-3-oxovalerate under the catalysis of piperidine acetate and a co-catalyst, and carrying out reduced pressure distillation recovery to obtain a compound shown as a formula V; dropwise adding 2-ethyl-2-isothiourea and a compound shown in a formula VI, carrying out cyclization reaction under a non-violent reflux condition, and then adding DDQ in batches for oxidation to obtain a compound shown in a formula IV; oxidizing the compound as shown in the formula IV, and immediately quenching by using saturated NaHCO3 after the reaction is finished to obtain a compound as shown in a formula III; the preparation method comprises the following steps: firstly, treating a compound shown as a formula III by using methylamine, and slowly dropwise adding methylsulfonyl chloride under ice bath temperature control to obtain a compound shown as a formula II; reducing the ester group of the compound shown in the formula II in anhydrous toluene by using DIBAL to obtain an alcohol intermediate; then, selective oxidation is performed to obtain a final product; the method integrally has the advantages of high product yield and purity, few byproducts and low production difficulty.

A device and method for preparing high-purity metals by vacuum distillation and bidirectional step condensation, the device comprising an atmosphere control device, a vacuum distillation device, a charging device, an intelligent control device, and an exhaust gas treatment device. The atmosphere control device comprises a nitrogen bottle and a control valve located above the bottle mouth for controlling the opening and closing of the nitrogen bottle. The vacuum distillation device comprises a vacuum distillation device and a vacuum pump connected to the vacuum distillation device via a pipeline. The charging device is located in the middle of the vacuum distillation device, and the intelligent control device is connected to the vacuum distillation device. The exhaust gas treatment device comprises an impurity removal device. The vacuum distillation device is provided with a plurality of heaters, which are arranged in parallel along the length direction of the charging device and the condensation zone on both sides of the vacuum distillation device. The present invention also includes a method for preparing high-purity metals using the device. The device of the present invention has a simple structure, is not restricted by the gravity field, is convenient for sampling, and has high impurity removal efficiency.

The invention discloses a method for treating copper anode slime through combination of reduction smelting, vacuum distillation and oxidation refining. The method comprises the following steps: firstly, adding a reducing agent and a slagging constituent into tellurium slag obtained by removing copper, selenium and tellurium from copper anode slime by a conventional method, and uniformly mixing to obtain a mixed material; the obtained mixed material is added into a converter to be subjected to a heating reduction smelting reaction, and reducing slag and high-gold precious lead are generated in the converter; the method comprises the following steps: putting high-gold precious lead into a vacuum furnace for vacuum distillation, cooling after distillation, filling nitrogen for protection after cooling, and opening the vacuum furnace to discharge lead-bismuth alloy and residues when the pressure reaches the standard atmospheric pressure; and the obtained residues are placed in a refining furnace to be subjected to oxidation refining, and lead bismuth slag, tellurium slag, alloy slag and an alloy plate are generated. By means of the technical scheme, the direct recovery rate of precious metal is high, the field environment is good, the production cost is low, the additional value of by-products is high, and the technical problems existing in an existing copper anode slime treatment process can be effectively solved.

The invention discloses a petroleum product high-boiling-point high-vacuum distillation distillation range full-automatic measuring system, which is characterized by comprising a main control unit, and the main control unit comprises a signal detection and control device for performing signal detection and signal control on signals fed back by other units; the signal detection and control device is controlled by a man-machine interaction control device; the distillation chamber unit comprises a detected distillation temperature detection device, a distillation chamber heat preservation device, a distillation chamber heating control device and a distillation chamber heat dissipation device; the condensing unit is used for condensing wax-oil-containing steam in the distillation process and naturally cooling non-wax-oil-containing steam, so that liquid drops obtained by condensing oil-containing steam enter the receiving unit; the receiving unit comprises a liquid level detection device, a liquid level tracking device, a receiving room temperature control device, an initial boiling point detection device and a flow guide device; the vacuum degree control unit comprises a vacuum degree detection device and a vacuum degree control device. According to the device disclosed by the invention, the process detection and control of a distillation experiment of a petroleum product under high vacuum can be more intelligent and safer.

The invention belongs to the field of separation and purification of bio-based chemicals, and particularly relates to a method for separating and purifying levoglucosenone from bio-oil. According to the method, the bio-oil obtained in the process of preparing levoglucosenone (LGO) through selective pyrolysis of biomass is used as a raw material, organic acid in the bio-oil is removed through a supersaturated carbonate solution, and then an oil phase is obtained through step-by-step extraction. And then adjusting working conditions, carrying out echelon reduced pressure distillation on the oil phase, and sequentially removing the extracting agent, low-boiling-point impurities and high-boiling-point oligomers, so as to obtain high-purity LGO. The pyrolysis bio-oil is subjected to coupling treatment of deacidification, step-by-step extraction and echelon reduced pressure distillation, so that the aim of separating and purifying high-added-value chemicals from low-value and complex-component bio-oil is fulfilled. The raw materials are cheap and easy to obtain, the process is simple, and the method is a biomass resource utilization method with great prospects.

The invention discloses lithium sulfide and a preparation method thereof. The preparation method comprises the following steps: (1) carrying out ball-milling mixing on iron powder, sodium sulfide and lithium sulfate in a first inert atmosphere to obtain a mixture; (2) calcining the mixture in a second inert atmosphere for the first time to obtain a reaction material; (3) stirring and washing the reaction material with an alcohol solvent in a third inert atmosphere, filtering to obtain filtrate and a filter cake, performing reduced pressure distillation on the filtrate to obtain a lithium sulfide crude product, washing the filter cake with deionized water, and filtering to obtain a solid by-product; and (4) carrying out secondary calcination on the lithium sulfide crude product in a fourth inert atmosphere to obtain lithium sulfide. The preparation method provided by the invention has the advantages of few synthesis steps, simple product purification and environmental protection.

The invention discloses a photoresist stripping waste liquid recovery method, which belongs to the technical field of waste liquid treatment, and comprises the following steps: carrying out centrifugal separation treatment on photoresist stripping waste liquid to remove polymer solid impurities in the photoresist stripping waste liquid to obtain pretreated stripping waste liquid; adding a bentonite-based adsorption material into the pretreated stripping waste liquid, stirring, and performing magnetic separation through a magnet to obtain purified stripping waste liquid; carrying out reduced pressure rectification treatment on the purified stripping waste liquid to obtain a recovered stripping liquid and a high-boiling-point substance; according to the recycling method, the high-concentration stripping liquid can be recycled, meanwhile, metal ions, moisture and high-molecular solid impurities influencing the product quality are removed, a dehydrating tower is not needed for dehydration treatment, and the recycling method has the advantages of being simple in process, small in occupied area of equipment and the like; and meanwhile, the pollution of the stripping waste liquid to the environment is also reduced.

The invention relates to a preparation method and device of 2-phenylimidazoline and an obtained product. The method comprises the following steps: adding benzonitrile, ethidene diamine and a catalyst into a reaction kettle, heating the reaction kettle to a reaction temperature in an inert gas atmosphere, starting a reaction, timing from 80 DEG C when the temperature is automatically increased to 155-180 DEG C, preferably 160-170 DEG C and is not increased any more, and reacting for 4-12 hours, preferably about 5-10 hours, after the reaction is finished, carrying out vacuum distillation on the reaction kettle, the product is obtained from the bottom of the reaction kettle (1), the material ratio is that the molar ratio of benzonitrile to ethylenediamine is 1: (1.03-1.20), and the molar ratio of the addition amount of the catalyst to ethylenediamine is (0.004-0.01): 1. The cyanobenzene is almost completely converted, the conversion rate is greater than 99.9%, and the residual quantity of cyanobenzene in the product is less than 0.01%, which is far superior to that of the existing production process.

The utility model provides a device for desalinating seawater and assisting in driving a ship by using RO (Reverse Osmosis), which comprises a water producing pipeline, a water using pipeline and a cleaning pipeline, and the water producing pipeline is sequentially provided with a lift pump, a security filter, a water inlet tank, a water inlet pump, a precision filter, a booster pump, an RO membrane group and a water producing tank along the water inlet direction; the water pipeline and the cleaning pipeline are both connected with the water outlet end of the water production tank, and the cleaning pipeline is connected with the security filter and the precision filter respectively. The volume and the weight of the device are smaller than those of a traditional vacuum distillation type desalting device, and the ship carrying capacity can be improved; the RO membrane group is simple and easy to operate, and can operate without heating seawater and an additional vacuum pump, so that manual operation is reduced; bacteria and viruses can be treated simultaneously when the RO membrane group is used for desalination treatment, and the treated fresh water can be used without disinfection; by-product high-pressure concentrated water generated by manufacturing fresh water through the RO membrane module can be used for assisting or directly driving the ship, so that the energy loss of ship maneuvering is reduced.

The invention discloses a method for efficiently removing impurity lead in bismuth, and belongs to the technical field of non-ferrous metal refining. The method comprises the working procedures of material mixing, smelting and distillation, wherein crude bismuth and a vulcanizing agent are evenly mixed according to the mass ratio of 1000: (1-10) and then placed in a smelting container. Placing the smelting container in a smelting furnace for negative pressure smelting, and then placing a smelting product in a vacuum furnace for vacuum distillation. Lead sulfide is volatilized and enriched in the condensate, and bismuth is not volatilized, so that refined bismuth is obtained. According to the method, the vulcanizing agent reacts with the impurity lead to generate lead sulfide, the volatility of the lead sulfide is remarkably different from that of bismuth, the separation efficiency is improved, the separation process is simplified, the impurity lead in the crude bismuth can be efficiently removed, the content of lead in the obtained refined bismuth is smaller than or equal to 1 ppm, the additional value of the refined bismuth is high, the production process is simple, and the method is suitable for industrial production. High popularization and application values are realized.

The invention discloses a method for purifying p-dioxanone by coupling vacuum distillation with melt crystallization, which comprises the following steps: removing light and heavy impurity components contained in a crude product of p-dioxanone by vacuum distillation, and carrying out melt crystallization, sweating and filtering on the p-dioxanone subjected to vacuum distillation purification to obtain the p-dioxanone. High-purity p-dioxanone is obtained, and uncrystallized mother liquor is returned to the step of vacuum rectification.

The invention relates to a method for preparing metallic titanium through two-step electrolysis in halide molten salt, and belongs to the technical field of metallurgy. The method comprises the following steps: by taking fluorine-chloride mixed molten salt as primary electrolytic molten salt, adding TiO2 into the fluorine-chloride mixed molten salt, uniformly mixing, heating the fluorine-chloride mixed molten salt containing TiO2 to the electrolytic temperature of 650-850 DEG C in an inert atmosphere, inserting a cathode and an anode, carrying out primary molten salt electrolysis, taking out a cathode product, and carrying out secondary electrolytic treatment on the cathode product to obtain the TiO2 / TiO2 composite material. Performing vacuum distillation or washing on the cathode product to remove impurities, and drying to remove attached electrolyte to obtain a primary electrolytic product crude titanium; the method comprises the following steps: by taking primary electrolysis product crude titanium as a soluble anode, high-purity metal titanium as a cathode and chloride molten salt as secondary electrolysis molten salt, heating the chloride molten salt to the electrolysis temperature of 550-750 DEG C in an inert atmosphere, inserting the cathode and the anode, performing electrolytic refining, and washing the electrolysis product with diluted hydrochloric acid and deionized water to remove impurities, thereby obtaining the low-oxygen metal titanium powder. A low-melting-point molten salt system is adopted in two-step electrolysis, and energy consumption can be effectively reduced.

The invention relates to the technical field of chemical experiments, in particular to a micro-negative pressure distillation device which comprises a multi-port distiller, a condenser, a liquid outlet device, an air pump, an air supply pipe and a refrigeration pump which are connected with one another. The multi-port distiller comprises a distillation chamber, a vapor-liquid separation plate, a gas guide port, a distillation port, a gas return port and a liquid collection port; the condenser comprises an air inlet, an air outlet, a refrigerant fluid inlet and a refrigerant fluid outlet; the liquid collector comprises a liquid receiving opening and a liquid collecting cavity; the air supply pipe comprises an upper port, an expansion pipe and a lower port. When the micro-negative-pressure distillation device operates, a micro-negative-pressure environment is formed in a closed system, and solvent steam is driven by non-condensable gas to realize efficient distillation and recovery of a solvent through the liquefaction effect of the condenser. The micro-negative pressure distillation device has the beneficial effects that the bumping phenomenon of reduced pressure distillation can be completely eradicated, and the micro-negative pressure distillation device has the advantages of high distillation efficiency, environment friendliness, high safety and the like.

The utility model relates to low-temperature vacuum distillation equipment convenient for material separation, and aims to solve the technical problems that the stirring range is still limited because stirring blades of the low-temperature vacuum distillation equipment can only stir in a horizontal fixed direction, the stirring is insufficient, the temperature rise of materials is non-uniform, and the material separation efficiency is reduced, and the low-temperature vacuum distillation equipment comprises a low-temperature distillation tank, according to the device disclosed by the utility model, the rotating shaft is effectively driven to rotate through the motor, so that the spiral blade and the stirring rod are driven to rotate, materials can be stirred in the vertical direction through the rotation of the spiral blade, and the materials can be stirred in the horizontal direction through the rotation of the stirring rod; the stirring effect is improved, uniform temperature rise of materials is facilitated, accordingly, the material separation efficiency is improved, the stirring rod can effectively drive the scraping plate to move when rotating, the scraping plate effectively scrapes and cleans the inner wall of the tank body, and adhesion of the materials to the inner wall of the tank body is reduced.

The invention belongs to the field of high-purity indium preparation, and provides a method for preparing high-purity indium based on ultrasonic vacuum distillation-electromagnetic pulse zone melting purification, the method combines vacuum distillation and zone melting purification technologies, ultrasonic waves are applied in the vacuum distillation process to assist in removing low-boiling-point impurities such as Cd, Zn and the like, and the purity of the high-purity indium is improved. In the zone melting process, pulse current is applied through an induction coil to assist in removing impurities mainly including Sn, Pb and Fe, and stable preparation of a high-purity indium product with the purity larger than or equal to 99.9995% and the oxygen content smaller than or equal to 2 ppm is achieved by screening and controlling technological conditions. According to the method, the requirement for the purity of the raw material indium is low, and the preparation cost of a high-purity indium product can be reduced.