46results about "Titanium tetrachloride" patented technology

The present invention relates to a porous composite feedstock for metal chloride preparation, comprising a metal oxide containing material,; and / or a first additive; and a binder; wherein the porous composite feedstock is in particulate form; wherein the water content of the porous composite feedstock is in the range of from 0.01 to 5 wt.% based on the weight of the porous composite feedstock; and wherein the porous composite feedstock has a poured bulk density in the range of from 0.2 g / cm3 and 2.0 g / cm3.

The invention discloses a method for preparing titanium tetrachloride through gas-based reduction carbonization and fused salt chlorination of melt separation titanium slag. The method comprises the steps that titanium slag obtained through hydrogen reduction and electric furnace melt separation of vanadium-titanium magnetite concentrate is ground to a certain particle size; the titanium slag obtained in the first step is placed in a tubular furnace, the temperature is increased to 1100-1300 DEG C, meanwhile, mixed gas of methane and hydrogen is introduced for a reaction, and a carbonized product is obtained; and mixing the carbonized product obtained in the second step with chlorine salt, and carrying out chlorination reaction at a certain temperature to produce crude titanium tetrachloride. According to the method, gas-based reduction and carbonization of the melt separation titanium slag are achieved, compared with a traditional high-temperature carbonization process, the reaction temperature is greatly reduced, the carbonization rate is remarkably increased, and a new thought is provided for comprehensive utilization of the melt separation titanium slag.

The invention belongs to the field of separation, and particularly relates to a method for extracting and separating niobium and titanium from niobium concentrate. The method comprises the following steps: (1) crushing a niobium concentrate raw material, and then adding a carbonaceous reducing agent and a binder to prepare a spherical material; (2) heating the spherical material in an inert atmosphere for carbonization treatment to obtain pretreated powder; (3) heating and roasting the pretreated powder, and then continuously introducing chlorine until the reaction is finished; and (4) performing fractional condensation on a volatile gas-phase product in the roasting process to obtain NbCl5 and TiCl4, thereby completing the separation. The method is efficient in reaction, short in process, low in cost and free of secondary pollution, product purity exceeds 99%, traditional technical problems are solved, and industrialization is easy.

The invention relates to a method for treating a residue obtained from the chloride process, wherein the residue comprises the components titanium dioxide, coke, an inert metal oxide, and an iron-containing component. Further, the invention refers to the use of this method to separate the components contained in said residue, and to the use of the separated components in the chloride process for obtaining titanium dioxide.

A long-term operation method that effectively increases the amount of material fed into a molten salt chlorination furnace in the later stage of operation. With the operation of the molten salt chlorination system, the inner wall of the chlorine gas pipeline in front of the furnace of the chlorine gas system in front of the molten salt chlorination furnace is scarred, and the pressure in the buffer tank gradually increases. When the pressure in the buffer tank affects the stable operation of the molten salt chlorination system, the molten salt chlorination furnace performs a salt return operation; ensure that the molten salt in the molten salt chlorination furnace is completely solidified after returning to the chlorine pipe outside the molten salt chlorination furnace, clean or replace the chlorine gas pipeline in front of the furnace, and after completion, remove the blind plate and reinstall the chlorine gas pipeline in front of the furnace, and restart the furnace production. The advantages are: the process is simple, the chlorine gas pipeline in front of the furnace that is blocked in the later stage of the chlorination furnace operation can be cleared online, and the docking pressure between the chlorination furnace and the oxidation can be reduced, thereby achieving the purpose of increasing the amount of material fed into the chlorination furnace, effectively avoiding the situation where the amount of material fed is reduced due to the increase in docking pressure, greatly increasing the output of crude titanium tetrachloride and titanium dioxide in the chlorination furnace, and ensuring the long-term operation of the molten salt chlorination.

The invention provides a process for purifying and refining industrial grade titanium tetrachloride, which comprises the following steps of: removing main impurities such as silicon tetrachloride, vanadium oxychloride, aluminum chloride, ferric chloride and titanium oxychloride in a titanium tetrachloride crude product by adopting a rectification method and a chemical method, and condensing into a titanium tetrachloride liquid; carrying out degassing treatment on the titanium tetrachloride liquid; filtering the titanium tetrachloride liquid by using an ultrafiltration membrane; filtering the titanium tetrachloride liquid by using a nanofiltration membrane; and crystallizing the titanium tetrachloride liquid to obtain a finished product of which the purity reaches 99.99% and the total content of metal impurities is less than 5ppb. Main impurities in a titanium tetrachloride crude product are removed through a rectification method and a chemical method, then titanium tetrachloride liquid is filtered through an ultrafiltration membrane and a nanofiltration membrane, and metal impurities are efficiently removed through surface negative charges of the nanofiltration membrane, so that a titanium tetrachloride finished product with the purity reaching 99.99% and the total content of the metal impurities being smaller than 5 ppb is obtained. The process steps are simplified, and the titanium tetrachloride purification efficiency is improved.

A novel circulating fluidized bed chlorination furnace system is disclosed. The outlet of the petroleum coke feed tank is connected in parallel to the lower inlet of the chlorination furnace via a discharge pipe. The bottom of the chlorination furnace also has multiple chlorine inlets and slag discharge ports. The chlorine inlets are connected to chlorine pipes, and the slag discharge ports are connected to slag discharge pipes. The top of the chlorination furnace has an outlet, which is connected to the side inlet of a high-temperature cyclone separator via a feed pipe. The top of the high-temperature cyclone separator also has a liquid discharge port, which is connected to the top of a low-temperature cyclone separator via a liquid discharge pipe. The top of the low-temperature cyclone separator also has a liquid outlet. This invention features a compact structure, convenient installation, stable operation, and is safe and environmentally friendly. The entire reaction system is fluidized, preventing slag discharge pipe blockage. The combined use of the high-temperature and low-temperature cyclone separators ensures multiple cycles, repeated combustion, and reaction of the titanium tetrachloride mixture.

A reactor has a double-wall inlet tube for supplying a gas that contains a chlorination agent and also providing a protective gas shrouding at the end of the inlet tube. The reactor includes a reactor vessel with a protective lining on the inside wall. The double-walled inlet tube extends into the reactor vessel through the protective lining. The double-walled chlorine inlet tube has an inner pipe, an outer pipe, and a peripheral space between the inner and outer pipes. The chlorination agent containing gas is injected into the reactor vessel through the inner pipe, and the protective gas is injected simultaneously into the reactor vessel through the outer pipe in the peripheral space between the inner pipe and the outer pipe to form a protective gas shroud around the end of the double-wall inlet tube. The protective gas may be recycled from other portions of the process to reuse various materials produced from carbochlorination process.

The present invention relates to a method for removing vanadium from crude titanium tetrachloride using a synergistic catalyst, belonging to the technical field of organic matter-based titanium tetrachloride purification. Organic matter and crude titanium tetrachloride are mixed and stirred at room temperature to obtain a mixed liquid; the synergistic catalyst is added to the mixed liquid, the temperature is raised to 100-130°C, and the mixture is stirred for 1-4 hours to fully react; the synergistic catalyst is composed of an oxide support, a metal chloride complexing agent, and an active metal; the temperature is further raised to 140-160°C, and the titanium tetrachloride is distilled to obtain refined titanium tetrachloride and an easily handled residue. By optimizing the selection of organic matter and adding the synergistic catalyst, the present invention can reduce the formation of agglomerated carbon-containing small molecules, lower the carbon content in the titanium sponge, and thus improve the rigidity and production quality of the titanium sponge.

The present invention relates to the technical field of chemical waste recycling, and in particular to a waste resource processing system and equipment. The waste resource processing system includes: a microwave low-temperature desorption furnace, suitable for heating the waste at a first temperature to obtain a first mixed gas and a first solid residue; a microwave cracking furnace, suitable for heating the first solid residue at a second temperature to obtain a second mixed gas and a second solid residue; a microwave gas-phase catalytic cracking furnace, suitable for heating the first mixed gas and / or the second mixed gas at a third temperature to obtain a third mixed gas; a secondary high-temperature gas-phase cracking furnace, suitable for heating the third mixed gas at a fourth temperature to obtain a fourth mixed gas; the fourth mixed gas is condensed and distilled twice to obtain a high-purity titanium tetrachloride solution. The waste resource processing system provided by the present invention can completely decompose organic matter to obtain high-purity titanium tetrachloride, thereby realizing resource processing of titanium tetrachloride.

A device and method for efficient clean utilization of fluor carbon cerium ore double chlorination method, relate to the field of rare earth comprehensive utilization and recovery, the device is composed of a first continuous packing bed, pipeline device; second continuous packing bed; third continuous packing bed; first screw propelling type condenser; second screw propelling type condenser. Rare earth concentrate is chlorinated with aluminum chloride, carbon monoxide and chlorine gas generated in the first and second continuous packing beds in the third continuous packing bed. Chlorinated rare earth, aluminum fluoride and alkaline earth metal chlorides generated by chlorination reaction remain in the chlorination slag in solid form, and titanium tetrachloride, silicon tetrachloride and iron chloride leave the chlorination furnace in gaseous form. The gaseous chlorination products are condensed and recovered by the screw propelling type condenser. The solid phase products are separated by water immersion to obtain single rare earth chloride. The present application realizes the comprehensive utilization of rare earth elements and associated elements such as titanium, fluorine, silicon and iron in fluor carbon cerium ore, and no acid and alkali waste liquid and wastewater are generated in the reaction process, which has good environmental benefits.

A metal chloride generator is provided. The metal chloride generator is a metal chloride centrifugal reactor that can be operated under conditions sufficient to cause metal particles and chlorine in the generator to be brought into contact with one another and react using centrifugal force to form metal chloride. A process for manufacturing titanium dioxide that utilizes the metal chloride generator is also provided.

The present invention discloses a method for producing titanium tetrachloride by large-scale molten salt chlorination, 1) a mixture of high titanium slag, sodium chloride and petroleum coke is delivered to a chlorination furnace through a spiral feeder; 2) chlorine is delivered to the bottom of the molten salt in the chlorination furnace through a chlorine spray gun; 3) the chlorination furnace is sprayed with leaching mud for temperature control; 4) the gas pipe of the chlorination furnace is connected to a gas-solid separation device at 14 to 16 m; 5) the direct condensation stage is to spray the dust-collected furnace gas with the crude titanium tetrachloride slurry sprayed by the leaching device; 6) the indirect condensation stage is to condense the furnace gas that has completed direct condensation through a condensation device; 7) refined titanium tetrachloride is obtained; the present invention increases the molten salt chlorination capacity by expanding the chlorination furnace, improves the process control conditions, and reduces its control difficulty. A method for controlling production and improving the chlorination rate is proposed for large-scale chlorination furnaces to meet the needs of the production of later-stage products and avoid the shortcomings of molten salt chlorination.

The invention relates to the field of comprehensive smelting of titanium metal and vanadium metal, in particular to a device and a method for extracting and converting vanadium oxytrichloride from crude titanium tetrachloride. The method comprises the following steps: adding organic matter naphthenic oil in a refining process of crude titanium tetrachloride, and reducing VOCl3 in crude titanium into VOCl2 to enter refined slurry; the method comprises the following steps: firstly recovering TiCl4 in the refined vanadium-containing slurry, and then introducing chlorine gas for heating, so that VOCl2 is converted into VOCl3 gas again; condensing the VOCl3 gas to obtain a VOCl3 liquid; and finally, evaporating the VOCl3, and condensing and recovering the gas VOCl3 to obtain pure liquid VOCl3. The method is continuous in production operation, high in production efficiency, large in capacity, safe, economical and environmentally friendly, two products are creatively produced in a joint mode, the products are diversified through rigorous reaction steps, and a production line does not need to be independently developed.

The invention provides a method for blowing a micro-fine particle grade titanium-rich material in a fluidizing chlorination furnace, which comprises the following steps: step S1, drying and screening the micro-fine particle grade titanium-rich material to obtain titanium-rich material fine powder; s2, conveying the titanium-rich material fine powder to a chlorine pipeline of a boiling chlorination furnace; s3, the titanium-rich material fine powder is fully mixed with chlorine while being conveyed in a chlorine pipeline; and S4, a mixture of the titanium-rich material fine powder and chlorine is blown into a boiling chlorination furnace reaction zone. According to the method for blowing the micro-fine particle-grade titanium-rich material by the fluidizing chlorination furnace, the problem of resource waste caused by the fact that the micro-fine particle-grade titanium-rich material cannot be directly used for production of the fluidizing chlorination furnace is solved, efficient utilization of the micro-fine particle-grade titanium-rich material is realized through the blowing technology, the production cost is reduced, the energy consumption is reduced, and the yield and the quality of titanium tetrachloride are improved.

The invention discloses a method for pre-judging abnormal quality of a titanium tetrachloride distillation system, which comprises the following steps: arranging a trial observation hole on a reflux pipeline of the titanium tetrachloride distillation system, and pre-judging the quality of distillation reflux according to the change of the trial color on the basis that the initial color of the trial color is colorless and transparent. And the work of the distillation system is regulated and controlled according to different colors presented by the trial mirror. According to the method, the trial mirror observation hole is formed in the reflux pipeline of the titanium tetrachloride distillation system, and whether the quality of distillate reflux is abnormal or not is pre-judged according to the color presented by the trial mirror; according to the method, the distillation system does not need to be sampled and detected, and whether the reaction quality in the distillation system is controlled or not can be quickly and accurately judged only by observing the color of the distillate on line in real time through the trial mirror, so that the detection time can be effectively saved, enough regulation and control time can be provided for workers when the quality of the distillation system is abnormal, and the detection efficiency is improved. And unqualified distillates can be prevented from entering the distillation system in time.

The application provides a titanium tetrachloride mother liquor treatment method and system. The method comprises the following steps: introducing the titanium tetrachloride mother liquor, TiO2 solid and HCl gas into a gas-solid-liquid three-phase reactor, and reacting TiO2 and HCl with TiCl4 and alkoxy titanium chloride in the mother liquor to generate titanium oxychloride; after separation, titanium oxychloride solid and gas-liquid phase materials are obtained; the titanium oxychloride solid is heated and decomposed to generate TiCl4 gas and TiO2 solid, and TiCl4 liquid is obtained after condensation of the TiCl4 gas. The system comprises a gas-solid-liquid three-phase reactor, a separation device, a thermal decomposition reactor and a condenser, etc. The method and system realize low-cost and efficient recovery of the titanium tetrachloride mother liquor.

The application provides a method for preparing titanium tetrachloride by using a fluidized bed, wherein the powder fluidization area and the cooling area are alternately arranged in the fluidized bed, the whole is in a rectangular structure, the powder material is added from one side of the fluidized bed, and is sequentially overflowed through several fluidization areas and cooling areas and then discharged from the outlet; the fluidization gas enters the fluidized bed through the distribution plate at the bottom of the fluidization area, and reacts with the added powder particles at a certain temperature to prepare titanium tetrachloride; and the cooling medium is sent from the bottom of the fluidized bed and discharged from the top outlet after heat exchange. The method uses the slag containing titanium carbide, titanium nitride or titanium carbonitride as the raw material, and reacts with chlorine gas, so that the reaction efficiency is high; the fluidized bed adopts the cross design of the fluidization area and the cooling area, so that the heat released by the chlorination reaction is discharged from the fluidized bed through the cooling medium in time, and the local heat release of the reaction is avoided, and the sintering of the material or even the dead furnace condition is avoided.

The invention relates to the technical field of chemical engineering, and discloses a denitration slag recycling method which comprises the following steps: 1) fully mixing a waste denitration slag catalyst with high-concentration strong alkali, leaching, and carrying out solid-liquid separation; (2) refining the leachate; (3) washing and roasting the leaching residues by using H2SO4; (4) mixing the denitration slag and the titanium slag according to the proportion, and conveying the mixture to a middle stock bin to be fully and uniformly mixed after matching; 5) conveying petroleum coke and sodium chloride to an intermediate bin; 6) a material consumption proportioning scheme; 7) chlorination reaction; and (8) waste fused salt and dust collection slag are recycled. Vanadium in the denitration catalyst is recycled and utilized in the early stage, the content of vanadium oxytrichloride generated by chlorination is low, the use amount of vanadium removal oil can be reduced in the refining process, the content of C in titanium tetrachloride can be reduced, then the content of C in titanium sponge is controlled, and the quality of the titanium sponge is improved; the production cost is reduced, the pollution to the environment is reduced, and the requirement of the green development concept is met.

The invention belongs to the technical field of chemical chlorination equipment, and particularly relates to equipment for preparing artificial rutile from titanium slag, which comprises a chlorination furnace and a chlorine spray gun mounted on the chlorination furnace, the device comprises a chlorine spray gun and a switching valve, the chlorine spray gun is arranged in the chlorine spray gun, the chlorine spray gun is internally provided with a backflow dredging mechanism, and the backflow dredging mechanism dredges the chlorine spray gun by controlling backflow of molten salt. On the other hand, due to the fact that the two states of the ventilation cavity and the backflow cavity of the cavity are alternately switched, molten salt backflow cleaning can be periodically conducted in the long-time using process of the cavity, and then an attached salt layer is removed; and long-term operation of titanium slag chlorination operation is maintained.

The invention relates to the technical field of titanium metallurgy, and discloses a method for preparing titanium tetrachloride from titanium-containing composite slag through low-temperature selective chlorination, which comprises the following steps: providing the titanium-containing composite slag which comprises a multiphase solid material of a TiCxOy phase and a melilite phase; the method comprises the following steps: putting titanium-containing composite slag into a reactor, and heating to 350-700 DEG C; introducing chlorine-containing gas into the reactor, and contacting the chlorine-containing gas with the titanium-containing composite slag to carry out selective chlorination reaction; and collecting and condensing gas generated in the reaction process to obtain a TiCl4 product, and discharging chlorination residues after the reaction. The method provided by the invention overcomes the dilemma in the traditional process, efficiently extracts titanium through a low-temperature selective chlorination technology, inhibits chlorination of impurities such as calcium and magnesium from the source, and realizes green production.

The invention relates to a method for recycling chlorine in the production of titanium tetrachloride. Further, the invention refers to the use of this method in the chloride process to produce titanium dioxide.

The invention discloses a method and a device for removing vanadium from crude titanium tetrachloride, and belongs to the technical field of impurity removal and refining of inorganic matters. The method comprises the following steps: (1) preheating crude titanium tetrachloride liquid, then introducing hydrogen into the crude titanium tetrachloride liquid, and irradiating the crude titanium tetrachloride liquid by adopting ultraviolet light with the wavelength not greater than 274 nm, so that the crude titanium tetrachloride reacts with the hydrogen; and (2) evaporating the reaction product to obtain refined titanium tetrachloride and vanadium-rich slag. According to the method, hydrogen is activated through ultraviolet light to generate H free radical ions, the problem that hydrogen cannot directly react with titanium tetrachloride and vanadium oxytrichloride is successfully solved, the efficient clean reducing agent hydrogen is used for removing vanadium from titanium tetrachloride, the safety and environmental friendliness of the vanadium removal process are effectively improved, the vanadium removal effect is improved, and the method is suitable for industrial production. The titanium tetrachloride with higher purity and the vanadium-rich slag with higher vanadium grade are obtained, an excellent foundation is laid for subsequent use of the titanium tetrachloride and the vanadium-rich slag, and a new thought is provided for vanadium removal of the titanium tetrachloride.

The present invention provides a method and system for purifying semiconductor-grade ultra-high-purity titanium tetrachloride. The purification system comprises at least a distillation tower, wherein the distillation column of the distillation tower comprises, from bottom to top, a stainless steel theta-ring packing section, a quartz packing section, an aluminum wire braided theta-ring packing section, and a quartz packing section. The aluminum section reacts with crude titanium tetrachloride to produce titanium trichloride, which reacts with difficult-to-remove impurities, raising the boiling point of the impurity compounds and significantly improving the purity of the product. The purification method comprises subjecting the crude titanium tetrachloride raw material to distillation in the purification system to obtain semiconductor-grade ultra-high-purity titanium tetrachloride. In the present invention, semiconductor-grade ultra-high-purity titanium tetrachloride is obtained through a single distillation through the synergistic action of each section. This process is simple, has low waste, and is easily scalable. The product purity reaches 99.99999999%, meeting the requirements for integrated circuit manufacturing.

The application discloses a chlorination furnace flue gas rinsing device, which comprises a feeding unit provided with a breathing pipe, a circulating unit for containing liquid-phase titanium tetrachloride, the breathing pipe being connected with the circulating unit and located above the liquid surface, a rinsing unit comprising a rinsing tower, and a recovery unit in communication with the circulating unit. The application also relates to a chlorination furnace comprising the chlorination furnace flue gas rinsing device. The application greatly reduces the flue gas temperature through heat exchange, effectively improves the recovery rate of titanium tetrachloride, reduces the production cost, and provides higher-quality crude titanium tetrachloride for a subsequent refining system.

A method of manufacturing a porous composite feedstock as well as a porous composite feedstock for use in the carbochlorination process of making TiCl4 in a fluidized bed reactor is provided. A homogeneous mixture of one or more particulate feedstock materials and a binder are extruded using a stiff vacuum extrusion process to form an extrudate. The extrudate can then be further processed to have a desired water content, particle sizes, and / or other characteristics for use as a porous composite particulate feedstock in the carbochlorination process. The method provides the ability to use a much wider variety and sources of feedstock for use in making TiO2 pigment particles according to the carbochlorination process.

The invention relates to the technical field of titanium metallurgy, and discloses a method for directionally converting titanium-containing slag into TiCxOy-containing composite slag, which comprises the following steps: putting titanium-containing slag containing perovskite phase and a carbonaceous reducing agent into a reactor; heating the materials in the reactor to carry out carbon thermal reduction reaction; cO-containing gas generated in the reaction process is discharged, converted slag is obtained, and the slag is multiphase composite slag comprising the TiCxOy phase and the melilite phase. According to the method, phase transformation is accurately controlled, the obtained product is the composite slag containing TiCxOy and melilite, the composite slag can be directly used as a downstream chlorination raw material without complex crushing and magnetic separation iron removal procedures, the technological process is greatly shortened, and the equipment investment and operation cost are reduced.

The present application belongs to the field of mixed metallurgy, and discloses a method for removing organic impurities in refined titanium tetrachloride, comprising the following steps: opening a titanium tetrachloride valve, and introducing refined titanium tetrachloride after vanadium removal into a mixing tank; opening a reagent valve, and introducing a reagent into the mixing tank, wherein the reagent comprises at least one of the following: alkali metal chlorides and their hydrated chlorides, alkaline earth metal chlorides and their hydrated chlorides, aluminum trichloride and its hydrated chloride, and iron trichloride and its hydrated chloride; opening a stirrer in the mixing tank to stir, so that the reagent and the refined titanium tetrachloride are fully mixed and reacted; and introducing the reaction liquid into a distillation device, and obtaining refined titanium tetrachloride with an organic impurity content of <0.0001% through distillation. The method of the present application has a high removal rate of organic impurities in refined titanium tetrachloride, reaching 99.99%, and the process of the present application is simple, the equipment investment is small, and the energy consumption is low.

The invention discloses a purification method, particularly discloses a purification method for high-purity titanium tetrachloride, and belongs to the technical field of metallurgical production processes. The purification method for the high-purity titanium tetrachloride is low in raw material purity requirement and high in production efficiency. The purification method comprises the following steps: firstly, converting metal impurities in a titanium tetrachloride raw material into heavy-component metal impurities of which the boiling point is different from that of titanium tetrachloride; and then heavy-component metal impurities, light-component organic impurities and particulate matter impurities are sequentially removed according to different boiling points of all the components and the molecular free path difference of substances of all the components, and finally a titanium tetrachloride product with the purity meeting the requirement is obtained.

The invention relates to the technical field of chemical production, and provides a method for dynamically controlling the temperature of fused salt in a fused salt chlorination furnace, which comprises the following steps: continuously adding chlorine, titanium slag, petroleum coke and chlorate into the fused salt chlorination furnace, carrying out fused salt chlorination reaction, and monitoring the temperature of the fused salt in real time; on the basis of the deviation between the real-time molten salt temperature and the preset reference temperature, the furnace returning flow of the liquid titanium tetrachloride slurry is adjusted according to a first dynamic proportion, main body excess heat is absorbed through gasification phase change of the liquid titanium tetrachloride slurry in the molten salt, and the discharge flow of the waste molten salt is adjusted according to a second dynamic proportion so that residual excess heat can be removed; and the real-time molten salt temperature is maintained to be stabilized in a process requirement interval. The scheme can guarantee continuous and efficient operation of the reaction and improve the raw material utilization rate.