61results about "Titanium halides" patented technology

The invention provides a titanium tetrachloride boiling chlorination process optimization method based on a causal model and electronic equipment, and the method comprises the steps: constructing a generation mechanism between structural equation model expression variables based on the causal relationship between boiling chlorination key process parameters and result variables; the effect of external intervention on the TiCl4 yield and unit cost is simulated through causal inference, and a multi-target optimization model with the minimization of the unit product manufacturing cost and the maximization of the TiCl4 yield as targets is constructed in combination with the structural model and Monte Carlo sampling estimation expectation; and iteratively solving the optimization model by adopting a causal-based non-dominated sorting genetic algorithm, and obtaining a Pareto optimal solution set meeting variable constraint conditions through operations such as causal variable classification, dynamic penalty weighting, non-dominated sorting and sensitive driving disturbance. According to the method, a causal modeling and optimization integrated framework suitable for the boiling chlorination process is constructed, personalized process strategy generation and production operation decision making are supported, and the raw material utilization rate and the process operation economy are improved.

The invention discloses a device and method for ultra-clean emission of tail gas of a large fused salt chlorination furnace, the device comprises a water washing device, an alkali washing device and a tail gas white removal device, an inlet of the water washing device is communicated with a smoke outlet of the chlorination furnace, and an outlet of the water washing device is communicated with an inlet of the alkali washing device; in addition, the tail gas white removal device comprises a heat exchanger, and the heat exchanger enables the temperature of the circulating liquid in the alkali washing device to be lower than 40 DEG C. A trace amount of TiCl4 flue gas in the tail gas is absorbed by utilizing a water washing principle, chlorine, CO2 and HCl in the tail gas are absorbed by utilizing an alkali washing principle, and the temperature of circulating liquid in an alkali washing device is controlled by adopting a heat exchanger, so that an alkali washing byproduct, namely sodium chloride, is prevented from being decomposed, and further, the increase of flue gas particulate matters generated by the decomposition is avoided; therefore, most harmful impurities in the tail gas are removed.

The invention relates to a method for preparing low-valence titanium chloride from gaseous TiCl4 through a molten salt method, and belongs to the technical field of titanium metallurgy. The low-valence titanium chloride preparation device comprises a TiCl4 gasification unit, an argon current-carrying conveying unit and a molten salt reaction unit, crude titanium and chloride molten salt are added into the molten salt reaction unit, the chloride molten salt is heated to 500-800 DEG C through the molten salt reaction unit, liquid molten salt is kept, and the liquid molten salt is located above a crude titanium solid phase; the method comprises the following steps: heating liquid TiCl4 to the temperature of 150-200 DEG C through a TiCl4 gasification unit, and gasifying the liquid TiCl4 into TiCl4 steam; tiCl4 steam is introduced into liquid molten salt of the molten salt reaction unit at a constant speed through argon flow of the argon current-carrying conveying unit, a gas-solid-liquid three-phase interface reaction system is constructed in a normal-pressure inert atmosphere, and the TiCl4 steam and crude titanium in the liquid molten salt are subjected to a multi-phase reduction reaction at the temperature of 500-800 DEG C to obtain low-valence titanium chlorides (TiCl3 and TiCl2). The method is suitable for providing a stable and efficient low-valence titanium chloride raw material for preparing high-purity metal titanium through a fused salt electrolysis method.

The invention relates to a directional purification method and equipment for titanium tetrachloride in the field of preparation and purification of integrated circuit raw materials, the directional purification equipment comprises an oxidation device, the oxidation device comprises an oxidation kettle, a pure copper part and a spraying device, the pure copper part and the spraying device are contained in the oxidation kettle, and the spraying device is suspended above the pure copper part; a feeding hole connected with the spraying device is formed in the oxidation kettle, and a first heating device for heating the pure copper workpiece is arranged on the oxidation kettle; the rectifying system comprises a rectifying still, a rectifying tower connected to the top of the rectifying still and a second heating device used for heating the rectifying still, a material pressing opening and an inert gas opening are formed in the rectifying still, and a tower top condensation structure is formed at the top of the rectifying tower; a plurality of tower plates are arranged in the rectifying tower at intervals along the height direction of the rectifying tower. According to the directional purification method and equipment, the purification difficulty of the titanium tetrachloride can be effectively reduced, the production cost is reduced, and the purity of the titanium tetrachloride is effectively improved.

The utility model discloses a vanadium removal device for producing titanium dioxide by a chlorination process, which comprises a vanadium removal reactor, a vanadium removal tower, a vanadium removal reboiler, a reflux tank, a first inspection tank, a second inspection tank and a vanadium removal condenser, and the vanadium removal reboiler is connected with the vanadium removal tower through a mineral oil adding assembly. The online vanadium analyzer is reasonable in structural design, the online vanadium analyzer is additionally arranged on the pipeline from the titanium tetrachloride outlet of the vanadium removal reboiler to the vanadium removal tower, meanwhile, the pipeline sight glass and the monitoring camera are additionally arranged on the feeding pipeline from the return tank to the inspection tank, and real-time data and monitoring pictures of the online vanadium analyzer are transmitted to the central control room. And central control room personnel monitor the vanadium content of the material at the outlet of the vanadium removal reboiler and the chromaticity of a refined product in real time, so that the problem of control lag caused by untimely discovery is solved, and accurate control on the addition amount of mineral oil is realized.

Provided is lithium potassium titanium oxide which can increase a friction coefficient in a high-load region and can improve the stability of a friction coefficient when used in a friction material.　The lithium potassium titanium oxide is represented by the compositional formula: K0.10 to 0.44Li0.27Ti1.73O3.65-3.82, in which the half width of a peak observed in a range of diffractive angles 2θ of 10.9° to 11.6° in an X-ray diffraction measurement of the lithium potassium titanium oxide is 0.20° or more.

The utility model belongs to the technical field of material separation, and particularly relates to a titanium tetrachloride rectifying device which comprises a reaction kettle and a rectifying tower, the kettle top of the reaction kettle is connected with the tower bottom of the rectifying tower through a gaseous mixture discharging pipeline, copper filler is filled in the rectifying tower, the copper filler is random filler or regular filler, and the reactor top of the reaction kettle is connected with the tower bottom of the rectifying tower through a gaseous mixture discharging pipeline. The reaction kettle is connected with a heating mechanism, and the rectifying tower is connected with a condensation reflux mechanism. According to the utility model, the copper filler is used as the built-in filler of the rectifying tower, VOC (Volatile Organic Compounds) l3 can directly react with the copper filler to generate a substance which is not dissolved in Ti C l4, so that the aim of removing impurities is fulfilled; impurity separation can be achieved without increasing the number of theoretical plates of a rectifying tower and the reflux ratio, the VOC l < 3 > impurity can be removed more simply, and meanwhile the equipment investment cost and the operation energy consumption are greatly reduced.

A method for producing Mg-containing particles by performing a classification process using a centrifugal airflow classifying device, the centrifugal airflow classifying device including: a housing; a rotating body that rotates within the housing; a classification chamber located on an outer edge side of the rotating body; and a flow path formed by an inner surface of the housing and a top surface of the rotating body, connecting an upstream end portion with the classification chamber, wherein the method for producing Mg-containing particles includes: supplying the unclassified Mg-containing particles to the classification chamber so that an average flow velocity of the unclassified Mg-containing particles on a downstream side from the upstream end portion in the flow path is lower than an average flow velocity of the unclassified Mg-containing particles at the upstream end portion flowing inside the flow path; and classifying the unclassified Mg-containing particles in the classification chamber to obtain Mg-containing particles, wherein an attrition durability A (%) of the unclassified Mg-containing particles calculated by the following formula (1) is 85 or less: A = (Z ÷ Y) x 100... (1).

The present invention discloses a hydrogenation reaction residue recovery and treatment system and method, belonging to the technical field of waste liquid recovery and treatment. The system includes: an evaporation kettle, an aluminum removal reactor, a first distillation column, a titanium removal reactor, a second distillation column, a high-boiling substance catalytic cracking reactor, a third distillation column, a condenser, a chlorosilane storage tank, a slurry tank, a screw conveyor and a hydrolysis tank. The present invention fills the blank of the recovery and treatment of chlorosilane residues, and realizes the stable operation of silane production by the disproportionation method through the recovery and treatment process of chlorosilane residues, ensuring the product quality. The recovery and treatment of chlorosilane residues in the present invention is of great significance for energy conservation, consumption reduction and emission reduction in silane production.

The utility model relates to a boiling chlorination furnace gas quenching pipeline which comprises a connecting flange, a steel body shell, a castable and a neck bush pipe, high-temperature furnace gas is arranged in the quenching pipeline and flows in the neck bush pipe at a high speed, the castable is arranged outside the neck bush pipe, and the neck bush pipe and the steel body shell are connected together through the castable. An anchoring part is welded in the steel body shell, connecting flanges are welded to the two ends of the steel body shell, a lifting lug is welded to the outer surface of the steel body shell, and a reinforcing plate is attached between the lifting lug and the steel body shell. The neck bush pipe is arranged, so that the smoothness of the inner wall of the quenching pipeline is improved, and the phenomenon that high-boiling-point impurities in furnace gas are continuously bonded in the cooling pipeline, and consequently the cooling pipeline is blocked can be avoided or greatly relieved. And meanwhile, the castable with low water content and higher acid resistance is adopted, so that the service life of the quenching pipeline is greatly prolonged, and a powerful guarantee is provided for stable production of the chlorination furnace.

The invention discloses a C6 compound, application and a vanadium removal method, the C6 compound is obtained by reacting olefin and TiCl4 at 120-160 DEG C, the volume ratio of the olefin to the TiCl4 is (15-25): (1-5), and the olefin is alpha-olefin or isoprene with the carbon atom number larger than or equal to 9. The C6 compound has a good vanadium removal effect, does not cause the problem of high carbon content impurities in refined TiCl4, does not generate wall-adhered residues to block equipment in a vanadium removal process, is easy to clean, and has a vanadium removal rate of 99.62%; the recycled C6 compound can be reutilized, namely can be used for recycling vanadium-containing compounds, and can also be used for vanadium removal experiments again after being treated.

A process for the preparation of non-fibrous alkaline titanates comprising the steps of: melting alkaline titanate in a furnace at a temperature ranging from 1300° C. to 1500° C. to form a molten product; cooling said molten product by placing it in contact with a material having a temperature equal to or lower than 15° C.

The invention relates to the technical field of titanium tetrachloride, and provides a vanadium removal reagent for removing vanadium impurities in titanium tetrachloride and a use method of the vanadium removal reagent, the vanadium removal reagent is prepared from the following components in percentage by mass: 20-60% of anthracene compounds, 1-10% of phenanthrene compounds, 5-20% of pyrene compounds, 10-30% of thiophene compounds and 10-30% of naphthalene compounds, the sum of the mass percentages of all the components is 100%, and the vanadium removal reagent is used for reacting with vanadium oxychloride in titanium tetrachloride to remove vanadium impurities. According to the scheme, the defects that the vanadium removal efficiency is low, the speed is low, dangerous reagents are used and secondary carbon pollution is introduced in a traditional process are overcome, and the purity of the obtained titanium tetrachloride product completely meets the strict application requirements in the high-end field.

The utility model discloses a kind of feeding devices for refining titanium tetrachloride, it is related to chemical equipment technical field, including mineral oil storage tank, for storing high viscosity mineral oil, the outside of mineral oil storage tank is equipped with steam jacket, steam inlet and steam outlet are equipped on the steam jacket;Coarse titanium storage tank, for storing coarse titanium tetrachloride;Mixing tank, the discharge outlet of mineral oil storage tank is communicated with the mixing tank by feeding assembly, the discharge outlet of coarse titanium storage tank is communicated with the mixing tank by first material transmission pipeline, the mixing tank is communicated with the feed inlet of rectification system by second material transmission pipeline, the second material transmission pipeline is used to send coarse titanium tetrachloride-mineral oil mixed solution into the rectification system.Upper described feeding device for refining titanium tetrachloride, realizes the technical effect of improving refining efficiency and product quality, reduces pipeline jamming risk, guarantees the stable operation of production.

This invention relates to the field of titanium chemical technology, specifically to a method for accelerating the precipitation of solid suspended impurities in crude titanium tetrachloride. A precipitation aid is added to the crude titanium tetrachloride. After reacting with titanium tetrachloride at room temperature, the precipitation aid generates a large amount of flocculent material, which adsorbs and rapidly precipitates the solid suspended impurities. The precipitation aid is a mixture of long-chain alkanes or olefins. This invention, by adding a precipitation aid to crude titanium tetrachloride, operates on a principle similar to flocculants precipitating solid suspended impurities in wastewater. The aid reacts with titanium tetrachloride at room temperature to generate a large amount of flocculent material, which adsorbs and rapidly precipitates the solid suspended impurities, increasing the precipitation rate of solid impurities in crude titanium tetrachloride, shortening the precipitation time, and reducing production costs. After adding the precipitation aid, the solid suspended impurities in crude titanium tetrachloride can be basically precipitated within five minutes, and become clear and transparent in about half an hour. This shortens the precipitation time, improves the efficiency of the settling tank, and also makes the vanadium slag after vanadium removal purer and more valuable.

This invention provides a heat-insulating and corrosion-resistant manhole device for maintenance of a fluidized bed chlorination furnace and a fluidized bed chlorination furnace. The manhole device is installed in the boiling section of the fluidized bed chlorination furnace and includes a manhole connector, a stainless steel pipe, and a manhole cover. The manhole connector is connected to the furnace shell of the fluidized bed chlorination furnace, and the manhole cover is installed at the end of the manhole connector away from the furnace shell. The stainless steel pipe is installed inside the manhole connector, with the inner wall of the manhole connector nested with the outer wall of the stainless steel pipe. The stainless steel pipe extends towards the furnace chamber of the fluidized bed chlorination furnace and penetrates the refractory layer inside the furnace shell until it communicates with the furnace chamber. At least one sealing element is installed in the cavity of the stainless steel pipe, and the sealing element can be removed from or installed inside the stainless steel pipe. This invention, by installing a manhole device in the boiling section of the fluidized bed chlorination furnace, allows for the rapid discharge of slag from the furnace, saving time and effort, ensuring safety and efficiency, and greatly protecting the personal safety of employees.

To provide a method for producing titanium tetrachloride that can improve the yield in the production of titanium tetrachloride.SOLUTION: A method for producing titanium tetrachloride involves forming a fluidized bed including titanium ore containing titanium oxide, coke, and chlorine gas on a dispersion board by using a chlorination furnace equipped with the dispersion board. The method includes an estimation step of estimating a height of the fluidized bed, and in the estimation step, the height of the fluidized bed is estimated based on fluidized bed information obtained by measuring internal pressure in two or more fluidized bed formation regions differing in positions in the height direction.SELECTED DRAWING: None

The utility model relates to the field of chemical production, in particular to a titanium tetrachloride cold recycling device which comprises a cold titanium tetrachloride storage tank, the device further comprises an atomizing spray head and a spray nozzle, the upper end of the cold titanium tetrachloride storage tank is fixedly connected with a supporting frame, the upper end of the supporting frame is fixedly connected with a second-stage condenser, a direct cooler and a third-stage condenser, and the inner wall of the direct cooler is fixedly connected with an annular flow dividing pipe. According to the utility model, through the use of the atomizing spray head and the spray nozzle, spraying is carried out from different angles and positions, mixed gas is further cooled, and part of gas is liquefied and flows into the cold titanium tetrachloride storage tank along the storage hopper, so that the cooling area and the uniformity are increased, and the liquefaction efficiency and the cooling effect are improved; a gas-liquid mixture is fed into a third-stage condenser for deep cooling, residual titanium tetrachloride gas is completely liquefied and flows into a cold titanium tetrachloride storage tank, liquid titanium tetrachloride in the storage tank is pressurized through a circulating system and then is fed back to a direct cooler to be used as a cooling medium, and the cooling and liquefying efficiency is improved.

This invention provides a pre-distillation system for high-boiling-point impurities in crude titanium tetrachloride containing high concentrations of particulate matter. The system includes: a pre-distillation column, in which rising titanium tetrachloride vapor gas, separated from the high-boiling-point impurities, is flash-distilled. Heat and mass transfer are utilized between the crude titanium tetrachloride spray solution and the rising titanium tetrachloride vapor gas gas to wash the rising gas particulate matter and effectively separate the high-boiling-point impurities, thereby directly supplying the gaseous product feed to a primary refining system; a pre-distillation pump tank, which receives the spray solution and partially transports the concentrated crude titanium tetrachloride liquid produced therein to the pre-distillation column reboiler; and the pre-distillation column reboiler, which superheats the received concentrated crude titanium tetrachloride liquid before sending it back to the pre-distillation column for further flash distillation. This pre-distillation system for high-boiling-point impurities in crude titanium tetrachloride containing high concentrations of particulate matter allows for the initial, separate interception of most solid particulate matter in the crude titanium tetrachloride.

The present invention relates to a titanium tetrachloride inhaler, belonging to the technical field of chemical equipment. The device comprises a cylindrical body (1), wherein the upper end of the body (1) is provided with a feed port (11), and the lower end is provided with a discharge port (12); a plurality of feed pipes (2) are provided at intervals along the circumferential direction on the upper side wall of the body (1), and the feed pipes (2) enter the body (1) tangentially and communicate with the interior of the body (1). In the device, gaseous titanium tetrachloride enters from the top feed port (11), while liquid titanium tetrachloride enters from the feed pipe (2) and rotates and flows downward in the body (11), forming a vortex. At the same time, negative pressure is formed in the body (11), accelerating the entry of gaseous titanium tetrachloride from the feed port (11), and achieving uniform mixing of gaseous and liquid titanium tetrachloride in the condenser at the lower part of the body (1). The device solves the problem of low absorption efficiency caused by the empty tower structure of the existing condensation tower.

The invention relates to a feedstock composite comprising a metal oxide fraction and a carbonaceous fraction, a binder composition and the use thereof for obtaining the feedstock composite. Further, the invention refers to a method for obtaining the feedstock composite.

The invention relates to the technical field of metallurgical environmental protection, in particular to a continuous treatment process for titanium tetrachloride refined vanadium removal slurry and an induction furnace system. The continuous treatment process comprises the following steps: continuously and uniformly introducing the organic matter refined vanadium removal slurry into an induction furnace through a feeding control device; an alternating magnetic field generated by an induction furnace is utilized to enable conductive components in the organic matter refined vanadium removal slurry to generate eddy current heating, so that the slurry is heated to be above the boiling point of a titanium tetrachloride solvent, and rapid evaporation and solid-liquid separation of the solvent are realized; the evaporated titanium tetrachloride steam is guided into a condensation system to be condensed and recycled; solid residues obtained after separation are guided out, cooled and collected. The process not only realizes high recovery rate of titanium tetrachloride and enrichment and recovery of vanadium resources, but also greatly reduces energy consumption by virtue of internal heating and high efficiency characteristics of induction heating, and effectively solves the problems of high energy consumption, low efficiency and resource waste in treatment of the vanadium-containing slurry.

The invention provides a fluorination process based on ammonium bifluoride, which comprises the following steps: crushing a titanium-containing compound to a first set mesh number, cleaning the titanium-containing compound, and drying until the moisture content is lower than a set value; grinding ammonium bifluoride powder with set purity until the particle size is smaller than or equal to a second set mesh number; the method comprises the following steps: mixing a titanium-containing compound and ammonium bifluoride into a reaction kettle according to a set mass ratio, and introducing nitrogen into the reaction kettle; raising the temperature in the reaction kettle to a first set temperature T1 at a set temperature raising speed, carrying out constant-temperature reaction in the reaction kettle for a set time length, and stirring the mixture in the reaction kettle at a set stirring speed; transferring the fluorination reaction product in the reaction kettle into a tubular sublimation furnace, heating the interior of the tubular sublimation furnace under the protection of nitrogen, carrying out gradient condensation on the fluorination reaction product in a plurality of temperature sections by utilizing a condensing tower, and recovering fluoride in each condensation temperature section; ammonium hexafluorotitanate in the recovered fluoride is subjected to ammonia precipitation hydrolysis and sintering, and titanium dioxide powder is obtained.

This invention provides a method for preparing fluidized bed chlorination titanium-rich feedstock from vanadium-titanium magnetite concentrate, comprising: mixing vanadium-titanium magnetite concentrate with a calcifying agent to prepare alkaline green pellets of vanadium-titanium magnetite concentrate, followed by calcification and oxidation roasting to obtain calcified oxide pellets; reducing the calcified oxide pellets with a reducing agent to obtain metallized pellets; melting and separating the metallized pellets with a supplementary calcifying agent to obtain molten iron and molten titanium slag; mixing the molten titanium slag with a water-quenching solution for water quenching to obtain water-quenched modified titanium slag; controlling the particle size of the water-quenched modified titanium slag to obtain fluidized bed titanium slag that meets the particle size requirements of the fluidized bed chlorination process; acid leaching and solid-liquid separation of the fluidized bed titanium slag to obtain titanium-rich feedstock; and alkaline leaching and solid-liquid separation of the titanium-rich feedstock to obtain fluidized bed chlorination titanium-rich feedstock. This invention improves the comprehensive utilization rate of vanadium and titanium in vanadium-titanium magnetite concentrate and prepares titanium into high-quality titanium-rich feedstock suitable for the fluidized bed chlorination process, while also possessing advantages such as industrial operability and environmental friendliness.

The invention discloses a calcium-titanium compound recycled from titanium-containing slag and a recycling method and application thereof, and belongs to the technical field of application of titanium-containing slag. The calcium-titanium compound comprises calcium-titanium oxide, the surface and the interior of the calcium-titanium compound are both provided with pore structures, the specific surface area is 0-30 m < 2 > / g, the micropore volume is larger than 0.00008 cm < 3 > / g, and the pore size of the pore structures is 7-100 nm. The recycling method comprises the steps that reconstructed slag particles obtained after titanium-containing slag powder and modifier powder mixed mineral reconstruction are subjected to at least two stages of leaching treatment, an extract, namely the calcium-titanium compound is obtained, and at least one stage of F-containing salt or F-containing acid leaching treatment is included. The calcium-titanium compound provided by the invention has wide application in preparation of titanium-containing products.

This invention relates to a process for the production of fluorinated metal oxide particles, the fluorinated metal oxide particles obtainable with such a process, and use thereof in the preparation of a solid-state electrolyte.

This invention discloses a flow guiding device and method for a low-temperature chlorination furnace. The flow guiding device includes an information collection unit and a vibration assembly. The information collection unit collects temperature signals at different locations within the fluidized bed distribution area of ​​the low-temperature chlorination furnace. The vibration assembly includes a vibration guide tube and a vibration control unit. The vibration control unit is located on the top outer side of the low-temperature chlorination furnace. An eccentric vibration shaft is installed inside the vibration guide tube. The top end of the eccentric vibration shaft is connected to the vibration control unit, and the bottom end of the eccentric vibration shaft extends to the fluidized bed and can move within the fluidized bed. This low-temperature chlorination furnace flow guiding device can promptly perform vibration and flow guiding when a fluidization dead zone occurs in the fluidized bed of the low-temperature chlorination furnace, restoring the normal fluidization state, avoiding localized high temperatures, and significantly improving the Ti recovery efficiency of the low-temperature chlorination furnace.

This invention belongs to the field of high-purity titanium tetrachloride refining technology, specifically relating to a catalytic organic additive, its preparation method, and its application. The catalytic organic additive is composed of organic base oil, alkanes, cycloalkanes, aromatics, and metal oxides in a specific mass ratio, with the following mass ratios: 40–70: 2–10: 10–40: 5–10: 2–10; wherein the organic base oil is glycerol, the alkanes are naphtha, the cycloalkanes are cyclohexane, the aromatics are C9 aromatics, and the metal oxide is alumina. This invention enables the organic additive to possess excellent catalytic cracking performance; in the vanadium removal process of high-vanadium titanium tetrachloride, it can rapidly react with vanadium compounds, significantly improving vanadium removal efficiency while greatly reducing the unit dosage of the organic additive used for vanadium removal. It combines process applicability and economy, and is suitable for the refining stage of high-vanadium titanium tetrachloride in the production of titanium dioxide and sponge titanium.

The invention discloses a purification process of high-purity titanium tetrachloride, which comprises the following steps: pressurizing a raw material by a pump, filtering, feeding into a rectifying tower I, separating low-boiling-point substances, and feeding a liquid phase into a rectifying tower II; high-boiling residues at the bottom of the rectifying tower II are removed from a residual liquid tank, a tower top gas phase part supplies heat to a rectifying tower I reboiler, a residual gas phase enters a first-stage adsorption column and a second-stage adsorption column after passing through a superheater, and a condensed liquid phase enters a rectifying tower III after passing through a third-stage adsorption column; discharging low-boiling-point substances at the top of the rectifying tower III, feeding a liquid phase part into a rectifying tower IV, supplying heat to a reboiler of the rectifying tower III by a gas phase of the tower IV, and feeding high-boiling-point substances at the bottom into a residual liquid tank; the other part of the liquid phase in the third rectifying tower enters a product evaporation tower, and the electronic-grade high-purity TiCl4 is obtained through a finished product filter after tower top condensation. According to the process, multi-tower rectification and three-stage adsorption are combined, cyclic utilization of heat energy is achieved through the differential pressure coupling technology, and the process has the advantages of being low in energy consumption, high in purity and stable in operation and is suitable for industrial production of electronic-grade titanium tetrachloride.

To provide a manufacturing method of titanium tetrachloride efficiently for an extended period.SOLUTION: In a titanium tetrachloride manufacturing device 1 assembled with a container 10, a bottom plate 11 partitioning the container to a lower side space S1 and an upperside space S2 and having a plurality of vent holes 11a, a gas introduction hole 12 for introducing a chlorine gas to the lower side space, and a dispersion layer 18 arranged on the upper side of the bottom plate and constituted of an initial non-active solid particle, provided herein is a titanium tetrachloride manufacturing method for manufacturing titanium tetrachloride by chemical reaction of chlorine gas to a fluid bed 19 arranged on the upper side of the dispersion layer and constituted of an initial titanium raw material 19a and an initial coke 19b. The titanium tetrachloride manufacturing method includes introducing chlorine gas to a gas introduction hole, supplying an additional titanium raw material and an additional coke to the fluid bed, and supplying additional non-active solid particles to the fluid bed in response to a decrease in the dispersion layer.SELECTED DRAWING: Figure 1