162 results about "Titanium chloride" patented technology

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 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 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 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.

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 utility model provides a titanium tetrachloride refines with organic vanadium removal agent heating device, including the bucket body, the inside fixed mounting of bucket body has multilayer spiral type's steam heating tube, is provided with the heat preservation layer between steam heating tube and bucket body, the inside fixed connection of bucket body has vanadium removal agent storage tank seat, vanadium removal agent storage tank is located on vanadium removal agent storage tank seat, steam heating tube surrounds vanadium removal agent storage tank in. The both ends of steam heating tube are connected with steam inlet and steam outlet that extend to the outside of bucket body, are provided with steam gate valve and flowmeter on steam inlet, the top of bucket body is installed with sealed top cover, the below of bucket body is equipped with temperature sensor. The utility model discloses a steam heating tube to vanadium removal agent storage tank heating can realize the heating and heat preservation of vanadium removal agent storage tank, also can avoid the corrosion problem of steam overflow to the equipment of the scene, can realize the control of heating temperature simultaneously.

The application discloses a preparation method of rutile titanium oxide long fibers, and belongs to the field of titanium oxide preparation. The preparation steps comprise the following steps: mixing titanium chloride, ethylene glycol and ethanolamine, stirring and refluxing, filtering to obtain a clear and transparent solution, rotary evaporation of the clear and transparent solution to obtain a concentrated rectification product, mixing the rectification product with ethyl methyl ketone, adding deionized water into the mixture, stirring and refluxing to obtain an organic titanium solution; adding polyvinyl alcohol into the organic titanium solution, uniformly stirring to obtain a stable spinning solution, electrospinning, heat treating the fibers after spinning to obtain rutile titanium oxide long fibers. The titanium oxide fibers prepared by the method are of rutile structure, the fibers are continuous, not adhered to each other and smooth in surface, the preparation method is simple, suitable for industrialization, and has a wide application prospect.

The present invention relates to the preparation of carbon nanotubes. Disclosed is a catalyst for preparing carbon nanotubes. The catalyst comprises a molten halogen salt, wherein the halogen salt comprises a first halogen salt, a second halogen salt and a third halogen salt. The first halogen salt is calcium chloride; the second halogen salt is potassium chloride; and the third halogen salt is selected from one or more of zinc chloride, copper chloride, barium chloride, titanium chloride, chromium chloride, gallium chloride, cobalt chloride, nickel chloride, manganese chloride, ferric chloride, ferrous chloride and aluminum chloride. On the basis of the total molar weight of the catalyst, the content of the first halogen salt is 20-80 mol%, the content of the second halogen salt is 0-10 mol%, and the content of the third halogen salt is 20-80 mol%. In the present invention, using the molten salt as a catalyst for preparing carbon nanotubes can effectively reduce metal pollution in a carbon product, and is more environmentally friendly than acid pickling in a metal catalytic system

The invention discloses low-chlorine-content sponge titanium and a preparation method and device thereof. The preparation method comprises the steps that a titanium rod is placed in liquid magnesium, titanium tetrachloride is added, a reduction reaction is carried out, the titanium rod is moved out, and vacuum distillation is carried out; the vacuum distillation time is more than or equal to 10h / t-Ti, and the condensation temperature in vacuum distillation is less than or equal to 350 DEG C; when the condensate water is closed, the condensation temperature is in a decreasing trend and the temperature decreasing rate is greater than or equal to 3 DEG C / h, judging a distillation end point: stopping vacuum, calculating the H volatilization pressure rise rate after 10 minutes, and stopping vacuum distillation when the H volatilization pressure rise rate is less than or equal to 0.3 Pa / min; the volatilization pressure rise rate H is equal to L2 pressure rise rate minus L1 air leakage rate. According to the method, volatilization channels are additionally arranged in the liquid magnesium, so that the volatilization resistance of Mg / MgCl2 in pores of the sponge titanium is reduced; in addition, the vacuum distillation end point is judged by adopting a composite method, so that the production of the sponge titanium with low chlorine impurity content is realized.

The invention discloses a method for preparing high-purity titanium powder by taking titanium-aluminum waste as a raw material, which comprises the following steps: annealing a titanium-aluminum waste mixture at 400-600 DEG C in an inert atmosphere to remove organic waste in the titanium-aluminum mixed waste, and carrying out reduction deoxidation reconstruction on surface oxides of the titanium-aluminum waste by using reducing micromolecules generated by pyrolysis depolymerization of the organic waste, a clean titanium and aluminum mixture is obtained; the titanium and aluminum mixture is placed in the dense medium liquid, the aluminum material floats above the dense medium liquid, the titanium material sinks to the lower portion of the dense medium liquid, and separation is achieved; the method comprises the following steps: placing a titanium material in a closed reactor, reacting by using gaseous high-reactivity Lewis acid salt, and converting the titanium material into gaseous low-valence titanium chloride; the gaseous low-valence titanium chloride is guided into an inlet-outlet high-temperature-gradient high-temperature decomposition reactor in a high-frequency pulse mode, and is converted into high-purity titanium powder in the process of passing through the high-temperature decomposition reactor, and the high-purity titanium powder is deposited in a collection area of the reactor.

The invention relates to the technical field of metallurgical engineering, and provides a method for determining organic carbon impurities in titanium tetrachloride, which comprises the following steps: filtering a titanium tetrachloride sample to remove inorganic carbon impurities; reacting the filtered sample with an oxidizing agent under pressurizing and heating conditions, so that organic carbon impurities in the sample are converted into a carbon-containing gas-phase product and solid-phase residues; collecting and measuring the carbon content in the carbon-containing gas-phase product to obtain the gas-phase carbon content; carrying out distillation separation on the reacted liquid, collecting residues, and measuring the carbon content in the residues to obtain the solid-phase carbon content; and adding the gas-phase carbon content and the solid-phase carbon content to obtain the content of the organic carbon impurity in the titanium tetrachloride. According to the scheme, high-precision and high-specificity quantitative analysis on the organic carbon impurities in the titanium tetrachloride is realized.

The invention relates to the field of magnesia carbon bricks and discloses a novel magnesia carbon brick for a converter mouth and a preparation method thereof.The novel magnesia carbon brick for the converter mouth is prepared from, by weight, 73-80 parts of fused magnesia particles, 15-22 parts of fused magnesia fine powder, 3-5 parts of crystalline flake graphite, 4-6 parts of phenolic resin, 1-4 parts of modified carbon fibers, 0.5-3.5 parts of alpha-Al2O3 micro powder and 2-5 parts of additives; the modified carbon fiber is prepared by carrying out boron nitride coating on carbon fiber by adopting a boric acid and urea impregnation reaction process and then carrying out high-temperature carbonization and cracking by adopting phenolic resin to further carry out cracking carbon coating; the admixture is prepared by the following steps: preparing polyborosiloxane from octamethylcyclotetrasiloxane and boric acid as raw materials, preparing titanium dioxide sol from titanium tetrachloride and isopropyl ether as raw materials and dichloromethane as a solvent by adopting a non-hydrolytic sol-gel method, and then mixing the polyborosiloxane and the titanium dioxide sol. The magnesia carbon brick prepared by the method is high in overall strength and good in thermal shock resistance and oxidation resistance.

This invention relates to the field of titanium tetrachloride preparation technology, and proposes a method for preparing titanium tetrachloride products. The method includes: filtering titanium tetrachloride raw materials to remove insoluble solid impurities, obtaining a pre-filtered liquid; adding a reducing agent and a catalyst to the pre-filtered liquid to react, causing vanadium-containing impurities to be reduced and precipitated, then separating the precipitate to obtain a vanadium-removed clear liquid; subjecting the vanadium-removed clear liquid to countercurrent extraction, and separating the liquid to obtain a purified clear liquid; sequentially passing the purified clear liquid through a light-water removal tower to remove impurities with boiling points lower than titanium tetrachloride, and through a heavy-water removal tower to remove impurities with boiling points higher than titanium tetrachloride, and obtaining the purified titanium tetrachloride product from the top of the heavy-water removal tower. This invention achieves deep removal of multiple types of impurities from titanium tetrachloride raw materials, can stably obtain titanium tetrachloride products with purity meeting the requirements of high-end fields, and has the advantages of high operational safety, low energy consumption, and ease of industrial implementation.

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 invention relates to the technical field of chemical intermediates, and relates to C07F, in particular to a preparation method for co-production of acetyl chloride and phosphorous acid as well as a product and application thereof. The preparation method at least comprises the following steps: S1, stirring and cooling acetic acid and a catalyst, dropwise adding phosphorus trichloride, heating to 20-45 DEG C, and reacting for 0.5-6 hours; s2, after the reaction is finished, carrying out negative pressure desolvation to obtain a crude product acetyl chloride, and continuously heating to remove excessive phosphorus trichloride, so as to obtain a crude product phosphorous acid; s3, rectifying the crude product acetyl chloride to obtain an acetyl chloride product; recrystallizing the crude phosphorous acid to obtain a phosphorous acid product; the catalyst comprises at least one of aluminum trichloride, ferric trichloride, titanium tetrachloride, ytterbium trifluoromethanesulfonate and iodine; the mass ratio of the acetic acid to the catalyst is 1: (0-0.003). The method provided by the invention has the characteristics of high conversion rate, high yield, high content, small amount of three wastes, no solvent pollution, simple process, easy industrial preparation of acetyl chloride and the like.

This invention provides a method for preparing high-performance surface-modified titanium filters from recycled titanium waste, relating to the technical field of filter preparation. The method includes sequential steps of titanium raw material hydrogenation, preparation of micron-sized hydride titanium powder, preparation of a porous titanium filter cold forming mold, preparation of a titanium filter compact, preparation of the porous titanium filter, and surface modification of the high-performance surface-modified titanium filter. The filters prepared from the titanium waste of this invention have long service life, high filtration accuracy, short production process, and low production cost; they solve the problems of short life, easy perforation, easy breakage, insufficient filtration accuracy, and high cost associated with existing filters used for filtering titanium tetrachloride. The filter preparation technology of this invention has no special restrictions on raw material composition, can meet the needs of different production environments and conditions, and has wide applicability.