213 results about "Titanium chloride" patented technology

The invention discloses a method for determining the content of total carbon, inorganic carbon and organic carbon in titanium tetrachloride, and belongs to the technical field of analytical chemistry. The determination method comprises the following steps: under inert atmosphere protection and a low-temperature environment, adding a titanium tetrachloride sample into an inorganic acid solution, fully hydrolyzing, and fixing the volume to obtain hydrolysate; analyzing the concentration of total carbon and inorganic carbon in the hydrolysate by using a TOC (Total Organic Carbon) analyzer; and calculating the contents of total carbon, inorganic carbon and organic carbon in the titanium tetrachloride sample according to the concentrations of total carbon and inorganic carbon in the hydrolysate. According to the method, inorganic carbon and total carbon in the hydrolysate can be directly measured, the content of organic carbon is calculated through a difference value method, and accurate typing of carbon forms is achieved. The method is simple to operate, short in detection period, high in efficiency and lower in cost. The method can effectively solve the problem that blind areas exist in impurity traceability and accurate control due to the fact that detection data of total carbon, inorganic carbon and organic carbon cannot be accurately separated through an existing method for measuring the carbon-containing compounds in titanium tetrachloride.

The invention discloses a halide electrolyte electrode material, a composite positive electrode, an all-solid-state battery and a preparation method of the all-solid-state battery. The chemical formula of the halide electrolyte electrode material is Li Zr T < c > Cl < d >, the preparation method of the halide electrolyte electrode material comprises the following steps: mixing titanium chloride, zirconium chloride and lithium chloride according to a stoichiometric ratio to obtain precursor powder, and placing the precursor powder in a first protective atmosphere for ball milling to obtain premixed amorphous precursor powder; and placing the premixed amorphous precursor powder in a second protective atmosphere, and calcining at 200-400 DEG C, thereby obtaining the product. And mixing the halide electrolyte with commercial lithium iron phosphate and conductive carbon to obtain the composite positive electrode. The all-solid-state battery assembled based on the positive electrode material shows higher energy density. The material provided by the invention has good structural stability and excellent charge-discharge cycle performance.

The invention discloses a high-temperature-resistant and salt-resistant fracturing fluid and a preparation method thereof, and relates to the technical field of oil field fracturing fluids. When the high-temperature-resistant and salt-resistant fracturing fluid is prepared, sodium 3-chloro-2-hydroxypropane sulfonate, N, N-dimethylacrylamide and ethylene glycol react to prepare a quaternized solid product, and then the quaternized solid product reacts with 1-bromooctadecane to prepare an amphoteric hydrophobic monomer; guar gum powder reacts with 3-(1-naphthyloxy)-1, 2-epoxypropane to prepare naphthyloxy functionalized guar gum, and then the naphthyloxy functionalized guar gum, acrylamide and an amphoteric hydrophobic monomer are subjected to initiated polymerization through ceric ammonium nitrate to prepare modified guar gum; enabling zirconium oxychloride octahydrate, titanium chloride, lactic acid, ethanediamine and glycerol to react to prepare an organic zirconium cross-linking agent; and finally, mixing the modified guar gum, an organic zirconium cross-linking agent, sodium thiosulfate, sodium bromate, a surfactant and water to prepare the high-temperature-resistant and salt-resistant fracturing fluid. The high-temperature-resistant and salt-resistant fracturing fluid prepared by the invention has excellent high-temperature resistance and salt resistance.

The invention discloses a high-selectivity pyridine alkylation method which comprises the following steps: taking anhydrous titanium chloride and an anhydrous ferric chloride solution as raw materials, adding a dispersing agent, heating and uniformly stirring, adding ammonia water to adjust the pH value to a fixed value, grinding and sieving to obtain a catalyst carrier; dipping the catalyst carrier into a rare earth metal oxide solution dissolved by dilute sulphuric acid in an equivalent volume manner, aging, grinding and sieving to obtain a rare earth metal modified solid superacid catalyst; the method comprises the following steps: activating a rare earth metal modified solid superacid catalyst, cooling to a reaction temperature, filling a fluidized bed reaction tube with the catalyst, mixing pyridine and dimethyl carbonate, starting feeding, opening an air inlet valve, introducing nitrogen, and carrying out a reaction on the raw material mixed nitrogen in a catalyst layer to realize high-selectivity pyridine alkylation. Pyridine and a green methylation reagent dimethyl carbonate are used as raw materials, and high-selectivity synthesis of 2-methylpyridine can be realized under the action of a rare earth metal modified solid superacid catalyst.

The invention relates to the technical field of stainless steel, in particular to a bamboo-like stainless steel guardrail production and processing technology which comprises the steps that a formed stainless steel guardrail is treated in a spraying mode, and a bamboo paint layer and a protective layer are sequentially constructed on the surface of the stainless steel guardrail by optimizing protective paint; composite zinc-titanium hydrotalcite and double-bond nano silicon dioxide are introduced into the protective coating to serve as filler, anhydrous zinc acetate, titanium tetrachloride and dopamine hydrochloride serve as raw materials, and polydopamine-coated zinc-titanium hydrotalcite is prepared through a hydrothermal method. Then depositing an antibacterial hydrophobic copolymer synthesized by taking 3-methacryloyl dopamine, styrene, dodecafluoroheptyl methacrylate, dimethylaminoethyl methacrylate and citronellyl methyl methacrylate as raw materials; the waterborne polyurethane emulsion is used as a photocurable protective coating base material.

The utility model relates to the technical field of titanium tetrachloride production, in particular to a material circulation device for a multi-stage fluidized bed. The utility model discloses a material circulation device for a multistage fluidized bed. The material circulation device comprises a U-shaped communicating vessel and a gate valve, one end of the U-shaped communicating vessel is communicated with a discharge port of one fluidized bed, the other end of the U-shaped communicating vessel is communicated with a feed port of the other fluidized bed, and an insertion plate groove is formed in the upper portion of the middle of the U-shaped communicating vessel. The gate valve is arranged on the U-shaped communicating vessel and comprises an insertion plate which is inserted into the insertion plate groove in an up-down movable mode. According to the utility model, the U-shaped communicating vessel and the gate valve are combined between the two fluidized beds, so that the adaptive adjustment of the material conveying quantity between the two adjacent fluidized beds is realized, the requirements of materials on flowing in different fluidized beds are met, and the overall reaction efficiency is improved.

The invention discloses a high-strength 6082 aluminum alloy, and relates to the technical field of alloys. When the high-strength 6082 aluminum alloy is prepared, firstly, aluminum chloride, titanium tetrachloride, chromium chloride, cerous nitrate and lanthanum nitrate serve as precursors, carbon fibers are doped, a reinforced phase A is prepared after heat treatment, secondly, aluminum powder, titanium powder, copper powder, chromium powder and manganese powder are prepared into high-entropy alloy to serve as a reinforced phase B, and finally, the high-strength 6082 aluminum alloy is prepared. And the reinforced phase A, the reinforced phase B and the aluminum alloy powder are mixed to prepare the aluminum alloy. The high-strength 6082 aluminum alloy prepared through the method has the good mechanical property.

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 discloses a method for preparing an impurity content test solution in titanium tetrachloride by a sulfuric acid method and a detection method, and belongs to the technical field of component detection and analysis. The preparation method and the detection method comprise the following steps: adding water into a titanium tetrachloride sample to react until a precipitate is dissolved and no thick white smoke is generated; heating and evaporating the obtained product to dryness under the condition that the temperature is not higher than 100 DEG C; then adding a sulfuric acid solution and a proper amount of water, heating under the condition that the temperature is not higher than 200 DEG C until the titanium matrix is completely dissolved to obtain a clear and transparent solution, and adding water to dilute and fix the volume to obtain a titanium tetrachloride impurity content test solution with the sulfuric acid concentration being less than 2%; and determining the impurity content in the solution by adopting ICP-MS or ICP-OES. The method disclosed by the invention is simple to operate, effectively avoids the pollution risk of external elements, and reduces the operation error, thereby greatly improving the accuracy and reliability of an analysis result.

The invention discloses a modified flocculant and equipment for rapidly removing microplastics in drinking water, and the modified flocculant is a polyaluminum sulfate-titanium tetrachloride-poly dimethyl diallyl ammonium chloride ternary composite flocculant. The pH application range value is increased by compounding with the poly dimethyl diallyl ammonium chloride, the charge neutralization bridging and netting capabilities are enhanced, and the adsorption bridging through a polymer chain is enhanced, so that the flocculant has the advantages of strong flocculation capability, quick demulsification, high settling velocity and small flocculant volume; and the water purifier has very strong purification capacity on fine suspended matters such as micro-plastics in water. Through the special flocculant adding, stirring and precipitation structure design, the removal rate of the micro-plastics is remarkably improved.

The invention discloses a coal-based solid waste-based ultrahigh water filling material and a preparation method thereof. The filling material can improve the utilization rate of coal-based solid wastes, reduce the material cost, improve the stability and strength of the material and enhance the environmental adaptability. The filling material is composed of a component A and a component B. The component A comprises the following components: sulphoaluminate clinker, citric acid and ethylenediamine tetra (methylene phosphonic acid) iron; the component B is prepared from the following components: desulfurized gypsum, fly ash, aluminum sulfate, N-(2-nitrophenyl) ethanolamine and a triisopropoxy titanium chloride complex.

The invention belongs to the field of preparation of a titanium-based material titanium tetrachloride for an integrated circuit, and relates to a method for removing trace impurities of electronic-grade chemicals, in particular to a method for preparing ultrapure titanium tetrachloride through membrane filtration and adsorption, which comprises the following steps: S1, performing ultrasonic treatment on a microfiltration membrane in ultrapure water to obtain an ultrapure microfiltration membrane; s2, flatly placing the ultra-pure micro-filtration membrane in a drying oven for drying, and removing internal moisture; and S3, enabling the titanium tetrachloride stock solution to penetrate through the dried ultra-pure micro-filtration membrane under pressure driving, so as to prepare the ultra-pure titanium tetrachloride. The method can efficiently adsorb trace metal impurities in titanium tetrachloride, and the whole filtration and adsorption process has the advantages of being simple and convenient to operate, mild in condition, high in removal efficiency, environmentally friendly and the like.

The invention relates to the technical field of chlorination process titanium dioxide production, and provides a preparation method and system of a titanium dioxide chloride finished product. The method comprises the following steps: uniformly mixing primary titanium dioxide chloride powder and desalted water in proportion to obtain titanium dioxide chloride slurry; conveying the titanium dioxide chloride slurry to a nano-particle separator, and obtaining oxidized primary slurry in different particle size ranges through the nano-particle separator; and respectively carrying out coating treatment on the oxidized primary product slurry in different particle size ranges, and then inputting the coated oxidized primary product slurry with different particle sizes into a gas-phase mixing tank according to a ratio for mixing to obtain a titanium dioxide chloride finished product meeting the target particle size requirement. According to the scheme, in the process of preparing the finished titanium dioxide chloride product meeting the target particle size requirement, the addition amount of the additive and reaction conditions in the preparation process do not need to be strictly controlled, the finished titanium dioxide chloride product particles with the good particle size distribution condition can also be obtained, and due to the fact that accurate control is not needed, the production cost is reduced, and the preparation efficiency is improved.

The invention discloses a preparation method and a detection method of a total carbon content test solution in titanium tetrachloride, and belongs to the technical field of component detection and analysis. The preparation method and the detection method comprise the following steps: adding water into a titanium tetrachloride sample to fully react, and heating and evaporating the obtained product to dryness at the temperature of not higher than 90 DEG C; then adding a hydrofluoric acid solution and a proper amount of water, heating and dissolving at the temperature of not higher than 80 DEG C to obtain a clear and transparent solution, and adding water to dilute and fix the volume to obtain the solution for testing the total carbon content in the titanium tetrachloride. And fully shaking up the test solution, and then immediately determining the total carbon content in the solution by adopting ICP-MS or ICP-OES (Inductively Coupled Plasma-Mass Spectrometry). The method disclosed by the invention is simple and rapid to operate, small in reagent dosage and low in test solution acidity, and can effectively solve the problems that coexisting components such as high-concentration Cl <-> and H < + > in the TiCl4 sample solution interfere a detection result and corrode an instrument.

The application provides a preparation method of a high-performance porous titanium-based intermetallic compound filter and relates to the technical field of filter preparation.The method comprises sequentially performing titanium raw material hydrogenation, micron-sized titanium hydride powder preparation, mixed powder preparation, mixed powder dehydrogenation alloying, micron-sized alloy powder preparation, cold isostatic forming mold preparation of the porous titanium-based intermetallic compound filter, titanium-based filter compact preparation and porous titanium-based intermetallic compound filter preparation.The application uses off-grade titanium as a matrix raw material, adds alloying elements such as aluminum and iron, combines the hydrogenation-dehydrogenation process with high-energy ball milling, and then realizes near forming of the porous titanium-based intermetallic compound filter through cold isostatic pressing and vacuum sintering.The prepared filter has high porosity, uniform pore size distribution and excellent corrosion resistance, can be used stably for a long time in a high-temperature and strong-corrosion environment, can realize efficient and high-precision purification of titanium tetrachloride, and is beneficial to industrial large-scale production and popularization.

The invention relates to the field of inorganic chemistry, electrochemistry and powder metallurgy science, in particular to a preparation device and a preparation method of metal Ti. The preparation device of the metal Ti comprises the reactor, the anode device and at least one group of cathode devices, preferably, the number of the cathode devices is multiple, so that cathode reactions can be carried out at the same time to improve the yield, different cathodes can also be carried out in turn to carry out the cathode reactions, continuous production is realized, and the production efficiency is improved. According to the preparation method of the metal Ti, the yield and quality of titanium are improved by improving the electrochemical performance of an electrolyte and the mass transfer rate of titanium tetrachloride, molten salt MgCl2 is used as the electrolyte, and the depth of a metal cathode immersed in the molten salt MgCl2 is continuously changed in the reaction process, so that the metal Ti is uniformly deposited on the surface of the metal cathode; and meanwhile, the cathode current density is controlled to be 0.1-10A / cm < 2 >, and the feeding rate of TiCl4 is 130-200g / A.h, so that the yield and the quality of a metallic titanium product are improved.

The application belongs to the technical field of metal surface treatment, and particularly relates to a passivation agent for a conversion film of die-cast aluminum and aluminum alloy and a preparation method thereof, which comprises gamma-aminopropyl triethoxysilane, cyclopentadienyl dibutoxy titanium chloride, fatty alcohol polyoxyethylene ether sodium carboxylate, zirconium isooctoate, aluminum coupling agent AL-M and water. The passivation agent for the conversion film of the die-cast aluminum provided by the application does not contain strong acid, strong base and phosphorus components, is friendly to the environment, is safe to operate in production and use, has a simple operation process, does not have obvious corrosion or discoloration on a metal substrate, and can reach 120 hours in neutral salt spray.

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.

This invention relates to the field of titanium chemical technology and discloses a refining process for crude titanium tetrachloride, comprising: feeding crude titanium tetrachloride and a vanadium removal agent into the bottom of a distillation column, mixing them in the bottom, and completing the vanadium removal reaction; the material in the bottom is extracted by a refining circulation pump and heated, then returned to the upper middle part of the bottom for in-situ flash evaporation, and the flash-evaporated liquid phase falls back to the bottom of the bottom; the titanium tetrachloride vapor generated by flash evaporation enters the purification section at the top of the distillation column for distillation separation, and the refined titanium tetrachloride gas generated at the top is condensed and enters a reflux tank, part of which is returned to the top of the distillation column to control the distillation purity, and the other part is output as qualified refined titanium tetrachloride product. This invention also provides a system for implementing this process. This invention solves the technical problem that traditional processes require multiple separate devices such as a circulation pump tank and a flash evaporation tank, making production operation and condition control difficult.

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 invention discloses a method for pyridine alkylation, comprising the following steps: using anhydrous titanium chloride and anhydrous ferric chloride solution as raw materials, adding a dispersant and then heating and stirring evenly, then adding ammonia to adjust the pH to a fixed value, grinding and sieving to obtain a catalyst support; immersing an equal volume of the catalyst support into a rare earth metal oxide solution dissolved in dilute sulfuric acid for aging, grinding and sieving to obtain a rare earth metal-modified solid superacid catalyst; after activation of the rare earth metal-modified solid superacid catalyst, the reaction temperature is lowered to be loaded into a fluidized bed reaction tube, pyridine and dimethyl carbonate are mixed and fed, and nitrogen is introduced into the air inlet valve at the same time. The raw material mixed nitrogen reacts in the catalyst layer to achieve high-selectivity pyridine alkylation. Using pyridine and green methylating agent dimethyl carbonate as raw materials, under the action of a rare earth metal-modified solid superacid catalyst, 2-methylpyridine can be synthesized with high selectivity.

The present invention discloses a coal-based solid waste-based ultra-high water filling material and a preparation method thereof. The filling material can improve the utilization rate of coal-based solid waste, reduce the material cost, and at the same time improve the stability and strength of the material, and enhance the environmental adaptability. The filling material consists of component A and component B. Among them, component A includes the following components: sulfoaluminate clinker, citric acid and iron ethylene diamine tetra(methylene phosphonic acid); component B includes the following components: desulfurized gypsum, fly ash, aluminum sulfate, N-(2-nitrophenyl) ethanolamine, and triisopropoxy titanium chloride complex.

The invention provides a coating method of high-silicon-content compact silicon-aluminum coated titanium dioxide, which comprises the following steps: S1) mixing titanium dioxide chloride, deionized water, a pH regulator and a dispersing agent to obtain oxidized slurry; the oxidized slurry is diluted and then heated, and then the pH of the slurry is adjusted; s2) adding sodium silicate and acid liquor into the slurry obtained in the step S1), and curing; s3) adding sodium silicate and acid liquor into the slurry obtained in the step S2), and curing; s4) adding sodium silicate and acid liquor into the slurry obtained in the step S3), and curing; s5) adding sodium silicate and acid liquor into the slurry obtained in the step S4) for curing; and S6) adding an aluminum source and an acid solution into the slurry obtained in the step S5), and curing to obtain the silicon-aluminum coated titanium dioxide. According to the coating method provided by the invention, by adopting a strategy of in-situ generation of nano seeds and layer-by-layer assembly, the bottleneck of coating densification of a titanium dioxide film layer with high silicon content is broken through, so that the silicon-aluminum coated titanium dioxide with low porosity and ultrahigh weather resistance is prepared.

The invention provides a medetomidine preparation method, which comprises: S1, taking 2, 3-dimethyl benzaldehyde as an initial raw material, and carrying out a reaction on the 2, 3-dimethyl benzaldehyde and methylmagnesium chloride to generate 1-(2, 3-dimethyl phenyl) ethanol; s2, excessive silyl group protected imidazole is added into a reaction system in the step S1, and an activated [1-(2, 3-dimethylphenyl) ethyoxyl] silyl ether intermediate is obtained; taking trimethylsilyl trifluoromethanesulfonate as a catalyst, carrying out a Friedel-Crafts reaction with silyl-protected imidazole, and after the reaction is finished, carrying out post-treatment on the reaction liquid to obtain a medetomidine crude product. 2, 3-dimethyl benzaldehyde is adopted as a starting raw material, medetomidine is prepared through a one-pot method, raw materials are cheap, reaction steps are short, the production cost is greatly reduced, TMSOTf is adopted as a catalyst in the Friedel-Crafts reaction, the reaction is efficient, it can be effectively avoided that in the aftertreatment process of a traditional catalyst titanium tetrachloride, a large number of titanic acid colloidal solid insoluble substances are formed, and the yield of medetomidine is increased. The problem that post-treatment layering is difficult is solved, and the yield is increased.

The invention provides a method for preparing a high-performance surface modified titanium filter through titanium waste recovery, and relates to the technical field of filter preparation. The method sequentially comprises the steps of titanium raw material hydrogenation, micron-sized titanium hydride powder preparation, porous titanium filter cold forming die preparation, titanium filter compact preparation, porous titanium filter preparation and high-performance surface modification titanium filter surface modification. The filter prepared from the titanium waste has the advantages of long service life, high filtering precision, short production flow and low production cost; the problems that an existing filter used for filtering titanium tetrachloride is short in service life, prone to perforation and breakage, insufficient in filtering precision and high in cost are solved. The preparation technology of the filter has no special limitation on raw material components, can meet the requirements under different production environments and conditions, and has wide applicability.

This invention relates to the field of titanium tetrachloride production technology, specifically a column-cooled, spray-type feeding process for titanium tetrachloride, comprising the following steps: S1, adding liquid magnesium to the reactor to a set amount; S2, after the temperature reaches the set temperature, starting the titanium tetrachloride feeding device; S3, simultaneously starting the cooling device while starting the titanium tetrachloride feeding; S4, installing a baffle above the outlet of titanium tetrachloride; S5, starting the discharge system; S6, after reduction, transferring to the distillation section. In this column-cooled, spray-type feeding process for titanium tetrachloride, the reactor is modified by adding a water-cooling structure for titanium tetrachloride, connecting cooling water to cool the titanium tetrachloride pipeline, thereby lowering the overall reaction temperature. Furthermore, this process avoids the formation of a hard core due to central overheating in the titanium agglomerate. The baffle above the titanium tetrachloride outlet ensures that the titanium tetrachloride is sprayed into the liquid magnesium, resulting in a more uniform reaction and guaranteeing product quality.

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.

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.

This invention discloses a method for preparing a test solution for impurity content in titanium tetrachloride using the sulfuric acid method, and a detection method thereof, belonging to the field of component detection and analysis technology. The preparation and detection methods are as follows: water is added to the titanium tetrachloride sample and reacted until the precipitate dissolves and no more dense white fumes are produced; the obtained product is heated to dryness at a temperature not exceeding 100°C; then sulfuric acid solution and an appropriate amount of water are added, and the mixture is heated at a temperature not exceeding 200°C until the titanium matrix is ​​completely dissolved, obtaining a clear and transparent solution. This solution is diluted with water to a final volume, yielding a test solution for impurity content in titanium tetrachloride with a sulfuric acid concentration of less than 2%; the impurity content in the solution is determined using ICP-MS or ICP-OES. This invention is simple to operate, effectively avoids the risk of contamination by foreign elements, reduces operational errors, and thus greatly improves the accuracy and reliability of the analytical results.

The invention provides a treatment method of a titanium dioxide primary product slurry in a chlorination process titanium dioxide process, which comprises the following steps: feeding a titanium dioxide primary product produced by a chlorination process into water in a beating tank, mixing to obtain a mixture, adding hydrogen peroxide, and continuously mixing to obtain a slurry; washing and filter-pressing the slurry obtained in the previous step to obtain a filter cake; and mixing the filter cake obtained in the previous step with water, and adding a pH regulator to obtain the pulped titanium dioxide slurry. The method can ensure that the viscosity of the slurry is relatively low, meets the requirements of a sanding process, does not need to additionally add a dispersing agent, reduces the consumption of hydrogen peroxide and caustic soda flakes, thoroughly cleans sodium and chloride ions in a titanium dioxide chloride primary product, reduces the ion concentration in the titanium dioxide slurry, solves the problems of high pulping viscosity and poor sanding effect, reduces the sanding cost, and improves the production efficiency. The product quality is improved to a certain extent, and the problem that the content of impurity elements in titanium dioxide is unstable can be avoided.