40 results about "Niobium(V) chloride" patented technology

The invention relates to a preparation method of stable water-soluble niobium precursor. Niobium pentoxide is dissolved in hydrofluoric acid solution to obtain niobium pentafluori solution. Niobium is precipitated in the form of niobic acid hydrate by alkali liquor. Precipitation is dissolved in tartaric acid solution to obtain stable soluble-niobium tartrate precursor solution which is faintly acid. The concentration of the niobium tartrate solution can be controlled according to the amount of the niobium pentoxide added in early regulation. The stable niobium tartrate solution can be used to synthesize mesoporous niobium oxide, mesoporous niobium phosphate and mesoporous niobium-silicon materials, and the materials are as excellent as commercial niobium chloride soluble salt in property. The highly stable water-soluble niobium tartrate precursor is obtained from low-cost materials in a simple and feasible synthesis path.

The invention relates to a preparation method of a solid acid catalyst for preparing 5-hydroxymethylfurfural from biomass. The solid acid catalyst is a compound of charcoal and niobium pentoxide and has an amorphous structure. The preparation method comprises the steps that with carbohydrate compounds as a carbon source, tartaric acid, niobium oxalate, niobium citrate, niobium pentachloride or other niobium salts as a niobium source as well as inorganic or organic acid as a catalyst, the compound is prepared by virtue of a hydrothermal or solvothermal method, and high temperature carbonization is implemented under nitrogen, so as to obtain the niobium-charcoal solid acid catalyst. The solid acid catalyst is applied to dehydration reaction of saccharides and cellulose, the yield of the product 5-hydroxymethylfurfural is high, and the cycle use performance of the catalyst is good; and the solid acid catalyst is a very good catalyst for preparing 5-hydroxymethylfurfural through biomass catalytic conversion.

The invention relates to a graphene / niobium pentoxide composite electrode material and a manufacturing method thereof. The manufacturing method comprises the following steps of 1) mixing and stirringa graphene oxide dispersion liquid and a carbodiimide type compound, and carrying out heating reflux reaction; 2) dissolving niobium pentachloride in absolute ethyl alcohol, then adding into a reaction liquid obtained in the step 1), and carrying out heating reflux reaction; 3) adding a reducing agent to the reaction liquid obtained in the step 2) to carry out a reduction reaction; 4) carrying outa solvothermal reaction on the reaction liquid obtained in the step 3), and collecting solid products, washing and drying; and 5) annealing the dried solid products in the step 4) under inert gas shielding so as to obtain the graphene / niobium pentoxide composite electrode material. The graphene / niobium pentoxide composite electrode material acquired through the above manufacturing method can havea high specific capacity and high cycle performance during high-speed charge and discharge processes.

The invention discloses a niobium pentoxide (at) reduced graphene oxide catalyst and a preparation method and application thereof. The preparation method of the niobium pentoxide (at) reduced grapheneoxide catalyst comprises the following steps of: 1) mixing a graphene oxide dispersion liquid with N-N'-dicyclohexylcarbodiimide, and reacting to obtain modified graphene oxide; and 2) adding the modified graphene oxide into a niobium pentachloride organic solution, and carrying out a hydrothermal reaction to obtain the niobium pentoxide (at) reduced graphene oxide catalyst. The graphene oxide ismodified by using N, N'-dicyclohexylcarbodiimide; then, the modified graphene oxide is combined with hydrolyzed niobium pentachloride through rich oxygen-containing groups on the surface of the graphene oxide; and finally the catalyst containing reduced graphene oxide and niobium pentoxide is obtained through a hydrothermal method. The catalyst has excellent catalytic selectivity on oxidation ofthioether into sulfoxide, and the sulfoxide selectivity is 85% or above.

The invention discloses a preparation method and application of a Mo-doped HNb3O8 nanosheet, and the preparation method comprises the following steps: dissolving niobium pentachloride in ethanol, adding a certain amount of molybdenum pentachloride powder into the solution, completely dissolving the mixed solution by ultrasonic treatment and oscillation, dropwise adding an aqueous solution of tetraalkylammonium into the mixed solution, and stirring at a constant speed to completely dissolve; then putting the obtained solution into a high-pressure reaction kettle for heating reaction; and cooling, washing and drying to obtain the Mo-doped HNb3O8 nanosheet. The Mo-doped HNb3O8 nanosheet material prepared by the method is used as a photocatalyst, and has the advantages of proper forbidden bandwidth, strong visible light absorption, higher hydrogen production and good cycling stability.

The invention relates to a nanometer spectral long-acting catalyst capable of highly-efficiently decomposing organic pollutants under dark light and light-free conditions. The nanometer spectral long-acting catalyst is composed of, by weight, 100 parts of water and 3 to 20 parts of nanometer modified niobium oxide. The nanometer modified niobium oxide is prepared through the following steps: dissolving 3 to 10 parts by weight of niobium pentachloride in 100 parts by weight of absolute ethyl alcohol at room temperature so as to obtain an ethanol solution of niobium pentachloride, and carrying out standing for 5 to 30 min; adding 5 to 15 parts by weight of bismuth vanadate and 0.01 to 0.1 part by weight of blocked isocyanate into the ethanol solution of niobium pentachloride and carrying outuniform mixing so as to obtain a first mixed solution; dripping 100 parts by weight of an aqueous solution of ethanol into the first mixed solution at a speed of 3 to 10 ml / min while stirring the first mixed solution; adding N,N-dimethyl formamide, continuing stirring the first mixed solution for 30 min and carrying out standing at room temperature so as to obtain a second mixed solution; and carrying out soaking and drying, putting a dried substance into a muffle furnace and carrying out calcining at 400 to 500 DEG C so as to obtain the nanometer modified niobium oxide. The nanometer spectral long-acting catalyst has good catalysis effect under dark light and light-free conditions.

The invention discloses a preparation method of a sea urchin-shaped niobium pentoxide electrode material. The preparation method comprises the following steps: dissolving niobium pentoxide into deionized water to obtain a liquid; adding hydrofluoric acid in a certain proportion; adding the obtained liquid into a high-pressure reaction kettle, and carrying out heating reaction; and cooling, washing, drying, and roasting so as to obtain the sea urchin-shaped niobium pentoxide electrode material. The invention further discloses the sea urchin-shaped niobium pentoxide electrode material prepared by virtue of the preparation method. A sea urchin-shaped niobium pentoxide microsphere has a uniform and regular shape and relatively good dispersity, is formed by the assembly of one-dimensional nanowires and has the advantages of low-dimensional nano materials, lots of new physical and chemical properties generated through coupling as well as excellent electrochemical performance after being used as the cathode of a lithium ion battery; and by controlling the concentration of niobium chloride, the molar ratio of niobium ions to fluorine ions, the reaction temperature, the reaction time and the like, the shape and size of a product are controlled.

The invention discloses a preparation method of a porous niobium nitride powder microwave absorption material, and belongs to the technical field of material science. The method includes: taking niobium pentachloride as a niobium source, adopting anhydrous ethanol as an oxygen donor, using dichloromethane as a solvent, employing polyoxyethylene-polyoxypropylene-polyoxyethylene (P123) as a pore-forming agent, preparing a niobium oxide xerogel by a sol-gel method, performing presintering to obtain niobium oxide powder, then mixing the niobium oxide powder with a structure stabilizer cyanamide, and then carrying out reduction nitridation reaction in an ammonia atmosphere to obtain porous niobium nitride powder. The niobium nitride powder prepared by the method is good in crystallinity and high in purity, has Nb4N5 serving as the phase, is uniform in particle size distribution, and has an abundant porous structure, the pore size and quantity can be adjusted by simply changing the dosage ofthe pore-forming agent, and meanwhile, the niobium nitride powder has excellent microwave absorption characteristic.

The invention discloses a preparation method of 1, 3-dichloro-1, 1-difluoropropane, and belongs to the technical field of fluorine-containing chemicals. Under the action of a lewis acid catalyst, in the presence or absence of a solvent, 1, 1, 1, 3-tetrachloropropane reacts with antimony trifluoride to generate 1, 3-dichloro-1, 1-difluoropropane, and the lewis acid catalyst is niobium pentachloride, tantalum pentachloride or antimony pentachloride. According to the preparation method of the 1, 3-dichloro-1, 1-difluoropropane, the raw materials are easy to obtain, the conversion rate is high, the 1, 3-dichloro-1, 1-difluoropropane can be prepared with high selectivity, and the selectivity can reach 90% under better conditions.

The invention relates to nano powder material preparation and application and provides a niobium and indium co-doped nano tin oxide powder preparation and application method. The method includes: taking and adding niobium chloride, indium trichloride and chloride pentahydrate into deionized water, and well dissolving to form uniform mixed solution; adding a complexing agent to perform complexing reaction of metal cations; adopting ammonium hydroxide solution to adjust solution pH value to 7-12, and continuing reaction to form sol; adjusting rotary evaporation temperature, and continuing reaction to form wet gel; drying, and subjecting obtained powder to grinding, screening and sintering to obtain niobium and indium co-doped nano tin oxide powder. By effective modification of tin oxide surface structural characteristics, the foundation is provided for subsequent compounding with a silver substrate, and silver-based electrical contact composite materials can be further improved in density, electricity and hardness performance.

The invention discloses a method for preparing allantion by a titanium dioxide-based composite solid catalyst. The method comprises: 1) mixing tetrabutyl titanate, graphene, dimethyl formamide and ethanol to form a solution A; 2) mixing water, ethanol and acetic acid to form a solution B; 3) mixing copper salt, zinc salt, silver salt, water and ethanol to form a solution C; 4) simultaneously dropwise adding the solution B and the solution C to the solution A, then standing, drying and grinding to obtain a powder object; 5) calcining the powder object to obtain a solid catalyst; 6) soaking thesolid catalyst, zinc chloride and niobium pentachloride in hydrochloric acid, then drying to obtain a titanium dioxide-based composite / Lewis acid composition; and 7) performing oxidation reaction on glyoxal with nitric acid to produce glyoxylic acid, and performing condensation reaction on glyoxylic acid, urea and the composition to produce allantion. The method has an excellent yield.

The invention discloses a preparation method of a phosphorus-selenium co-doped niobium disulfide nano material, and belongs to the technical field of clean energy storage and conversion material preparation. The preparation method comprises the following steps: mixing niobium pentachloride and degassed oleylamine, performing magnetic stirring, performing heating to 300 DEG C under the protection of nitrogen, injecting a CS2 sulfur source, keeping for 2 hours at the temperature, performing natural cooling to 200 DEG C, injecting a TOP-Se solution prepared in advance, quickly heating the system to 320 DEG C, keeping for 1 hour, ending the reaction, and performing natural cooling, washing and freeze-drying to obtain the niobium-doped carbon quantum dot. The phosphorus and selenium co-doped niobium disulfide nanoflower is obtained. According to the invention, the synthesis of the phosphorus-selenium co-doped niobium disulfide nano material with controllable morphology is realized for the first time, the vacancy of the transition metal sulfide synthesis technology is filled, and conditions are provided for the research of the nano material in the field of catalytic materials.

The invention relates to the technical field of electrochemical energy source materials and provides a phosphorus niobium oxide preparation method. The method includes: dissolving columbium pentachloride into an alcohol solvent, and subjecting to reduction reaction under airtight conditions to obtain a niobium oxide precursor; putting red phosphorus and the niobium oxide precursor in an upstream area and a downstream area of a flowing protective atmosphere respectively; heating the upstream area into a first area temperature in a range of 425-550 DEG C, keeping the temperature for 1-10h, heating the downstream area to a second area temperature in a range of 650-950 DEG C, and performing combination reaction to obtain a phosphorus niobium oxide. The preparation method is simple, easy to operate and free of high-corrosiveness reagents, thereby being a green environmental-friendly process.

The invention relates to a synthetic method for preparing amide compounds through co-catalysis of niobium pentachloride and ionic liquid. The preparation method is characterized by comprising the following steps: weighing organic carboxylic acid, organic amine, niobium pentachloride, ionic liquid and a molecular sieve, adding the materials into a reactor, adding an organic solvent, and reacting for 6-24 hours at the reaction temperature of 70-110 DEG C to obtain a corresponding amide product. The molar ratio of the organic carboxylic acid to the organic amine to the niobium pentachloride to the ionic liquid is 1:(1-3):(0.01-1):(0.05-1); wherein the mass ratio of the organic carboxylic acid to the molecular sieve is 1: (0.2-1). According to the method, the substrate range is expanded, the reaction yield is high (95% or above), the catalyst dosage is small, the atom economy is high, the catalyst is cheap and easy to obtain, the production cost can be greatly reduced, and the method is suitable for industrial production.

The invention discloses a preparation method of a positive electrode material of a lithium manganate battery, which comprises the following steps: (1) weighing a certain amount of MnO2 and Al2O3 and mixing and dispersing in an aqueous solution of sodium pyrophosphate to obtain a suspension A; (2) adding lithium hydroxide, sodium dodecylbenzene sulfonate and N-methyl pyrrolidone to obtain a suspension B; (3), heating the suspension B to 170-180 DEG C for reaction for more than 10 hours, and filtering to obtain a solid phase A after the reaction; (4) soaking the solid phase A in an ethanol solution of chloroiridic acid, and then taking out and drying; (5), calcining the solid phase A to obtain a solid phase B; (6) immersing the solid phase B in the ethanol solution of niobium pentachloride and nickel nitrate, then filtering out, drying and calcining to obtain the positive electrode material of the lithium manganate battery. By improving the preparation method of the lithium manganate positive electrode material, the invention makes the obtained lithium manganate used in the production of the battery, the capacity retention rate of the battery at normal temperature or high temperatureis significantly improved, and the service performance of the battery is improved.

The invention relates to the technical field of electrochemical energy source materials and provides a phosphorus niobium oxide preparation method. The method includes: dissolving columbium pentachloride into an alcohol solvent, and subjecting to reduction reaction under airtight conditions to obtain a niobium oxide precursor; putting red phosphorus and the niobium oxide precursor in an upstream area and a downstream area of a flowing protective atmosphere respectively; heating the upstream area into a first area temperature in a range of 425-550 DEG C, keeping the temperature for 1-10h, heating the downstream area to a second area temperature in a range of 650-950 DEG C, and performing combination reaction to obtain a phosphorus niobium oxide. The preparation method is simple, easy to operate and free of high-corrosiveness reagents, thereby being a green environmental-friendly process.

The invention discloses a method for preparing fine niobium powder through calcium thermal reduction of niobium chloride in calcium chloride molten salt. The method for preparing the fine niobium powder through calcium thermal reduction of the niobium chloride in the calcium chloride molten salt comprises the following steps of: introducing niobium pentachloride gas into calcium chloride molten salt dissolved with metal calcium by adopting argon, leaching a reaction product by adopting diluted hydrochloric acid after the reaction is finished, washing with deionized water and absolute ethyl alcohol, and finally, performing vacuum drying to obtain fine niobium powder. The method for preparing the fine niobium powder through calcium thermal reduction of the niobium chloride in the calcium chloride molten salt has the advantages that the niobium powder prepared through the method is high in purity, the particle size is small, the sphericity degree is good, the preparation process can be carried out continuously, and the method can be popularized to preparation of other fine metal powder.

The invention relates to a kind of in-situ growth of potassium niobate on the surface of vermiculite and a preparation method thereof. The preparation method of in-situ growth of potassium niobate on the surface of vermiculite is to adopt a one-step hydrothermal method to place the vermiculite in a place containing potassium hydroxide and pentachloride. In the solution of niobium compound, the nucleation and growth of KNbO3 on vermiculite is controlled by controlling the reaction temperature and time. Potassium niobate grows in situ on the inner and outer surface of the two-dimensional layered vermiculite with a one-dimensional needle-like structure, forming a Three-dimensional structure of KNbO3 / VMT material, in which KNbO3 and vermiculite interact through chemical bonds and have greater adhesion. The preparation method has a simple process. This material can be used as a photocatalytic material. The invention solves the problems that in the past, KNbO3 powder could only be used as a catalyst, the reaction raw materials were easily lost, storage and separation were difficult, and the recycling cost was high.

The invention discloses a preparation method and application of a tin sulfide@niobium disulfide (SnS@NbS2) core-shell heterojunction, and belongs to the technical field of functional nano material preparation. In the method, niobium pentachloride, tin tetrachloride pentahydrate and carbon disulfide are used as raw materials, oleylamine is used as a solvent, a reducing agent and a surfactant through a solvothermal method, and the SnS@NbS2 core-shell heterojunction is synthesized; and dispensing an ethanol solution of the heterojunction on the interdigital electrode to prepare the corresponding photoelectric detector.

The invention provides a preparation method of a single-phase cobalt nitrate nanomaterial. The preparation method comprises the following steps: dissolving columbium pentachloride and cobaltous chloride into an alcohol solution in a stoichiometric ratio of 2 to 1, so as to obtain a solution A; dissolving ammonium carbonate into a water solution, so as to obtain a solution B; mutually mixing the solution A and the solution B, stirring at the room temperature for a period of time, so as to obtain suspension liquid; carrying out centrifugal treatment on the suspension liquid, so as to obtain powder; drying the powder; and calcining the dried powder at 700-1000 DEG C for 6-12 hours, so as to obtain the single-phase cobalt nitrate nanomaterial. The single-phase cobalt nitrate nanomaterial prepared by virtue of the preparation method does not have an impure phase.

The invention provides a titanium dioxide matrix composite / Lewis acid composition suitable for preparing allantoin and a preparation method thereof, wherein the preparation method comprises the following steps of: 1) mixing tetrabutyl titanate, graphene, dimethylformamide and ethanol to form solution A; 2) mixing water, ethanol and acetic acid to form solution B; 3) mixing copper salts, zinc salts, silver salts, water and ethanol to form solution C; 4) simultaneously dripping the solution B and the solution C into the solution A, standing, drying and grinding to obtain powder object; 5) calcining the powder object to prepare a titanium dioxide matrix composite solid catalyst; 6) soaking the titanium dioxide matrix composite solid catalyst, zinc chloride and niobium pentachloride in hydrochloric acid, and then drying to obtain the titanium dioxide matrix composite / Lewis acid composition. The composite / Lewis acid composition has excellent catalytic effect on the synthesis of allantoin.

The invention provides a method for preparing 2-furan formyl-3-aryl-4-ethoxycarbonyl-5-methyl-anti-form-2 and 3-dihydrofuran under the catalytic action of niobium chloride. According to the method for preparing the 2-furan formyl-3-aryl-4-ethoxycarbonyl-5-methyl-anti-form-2 and 3-dihydrofuran under the catalytic action of the niobium chloride, the niobium chloride is used to serve as a catalyzer, and reaction is carried out under the reaction condition with low requirements to prepare the 2-furan formyl-3-aryl-4-ethoxycarbonyl-5-methyl-anti-form-2 and 3-dihydrofuran. The method for preparing the 2-furan formyl-3-aryl-4-ethoxycarbonyl-5-methyl-anti-form-2 and 3-dihydrofuran under the catalytic action of the niobium chloride has the advantages that the prepared product is easy to separate, the technique is simple, and little industrial waste is generated.

The invention provides a method for preparing cis-1-methoxycarbonyl-2-substituted phenyl-3,3-dinitrile cyclopropane under the catalysis of niobium pentachloride. The niobium pentachloride is prepared in a solvent under the action of the catalyst niobium pentachloride by taking brominating methoxycarbonyl methyl triphenylarsine and aryl methylene malononitrile as raw materials. Compared with the traditional reaction system, the method provided by the invention has the characteristics of higher yield, more easiness for post processing, higher product purity, high yield, low energy consumption, and the like.

The invention relates to a long-acting nano-spectrum medium that can efficiently decompose organic pollutants under dark and no-light conditions. The long-acting nano-spectrum medium is composed of 100 parts by weight of water and 3-20 parts by weight of nano-modified niobium oxide. Modified niobium oxide is prepared by the following steps: Dissolve 3-10 parts by weight of niobium pentachloride in 100 parts by weight of absolute ethanol at room temperature to obtain an ethanol solution of niobium pentachloride, and let it stand for 5-30 minutes; Add 5-15 parts by weight of bismuth vanadate and 0.01-0.1 parts by weight of blocked isocyanate to the ethanol solution of niobium pentachloride, and mix evenly to obtain the first mixed solution; keep stirring the first mixed solution, and add 100 parts by weight of the ethanol aqueous solution Drop into the first mixed solution at a speed of 3-10ml / min; add N, N-dimethylformamide, keep stirring the first mixed solution for 30 minutes, and let stand at room temperature to obtain the second mixed solution; after soaking and drying, The dried material is calcined in a muffle furnace at a temperature of 400-500°C to obtain nano-modified niobium oxide. Nano-spectrum long-lasting media has good catalytic effect in dark light and no light conditions.

The preparation of oxygen-sensing sensor includes the steps of: preparation of titanium trichloride doped with certain amount of niobium or tantalum pentachloride as source matter; addition of hydrogen peroxide as strong oxidant and DBS surface cladding agent and stirring at 50-70 deg.c water bath for 3-5 hr to form gel; mixing obtained powder with terpineol and painting the mixture to ceramic tube with brush-type electrodes; sintering in a muffle furnace at 380-450 deg.c for 1 hr to prepare niobium or tantalum pentachloride doped TiO2 nanometer powder, addition of heating filament to prepare the thick-film oxygen-sensing element; and aging through electrical heating for 10 dyas. The present invention has low working temperature, high sensitivity, fast response and high stability.

The preparation method of a phosphorus-selenium co-doped niobium disulfide nanomaterial of the invention belongs to the technical field of preparation of clean energy storage and conversion materials. The niobium pentachloride and the degassed oleylamine were mixed and stirred magnetically, heated to 300 °C under the protection of nitrogen, and injected into CS 2 The sulfur source was kept at this temperature for 2 hours, and then naturally lowered to 200°C. The TOP-Se solution prepared in advance was injected. The temperature of the system was rapidly increased to 320°C and kept for 1 hour. , to obtain phosphorus-selenium co-doped niobium disulfide nanoflowers. The invention realizes for the first time the synthesis of niobium disulfide nanomaterials with controllable phosphorus and selenium co-doping morphology, fills the vacancy of such transition metal sulfide synthesis technology, and provides conditions for its research in the field of catalytic materials.

The invention belongs to the technical field of photocatalyst synthesis, and concretely relates to a niobium hydroxide visible-light-driven photocatalyst having a wide-spectral catalytic performance and grafting with aromatic alcohol on the surface, and preparation and application thereof. A preparation method of the niobium hydroxide visible-light-driven photocatalyst comprises the steps of adopting columbium pentachloride as a niobium source, and hydrolyzing the columbium pentachloride at a certain temperature so as to firstly prepare niobium hydroxide; then adopting the aromatic alcohol as an organic solvent, and carrying out condensation reaction on the niobium hydroxide and aromatic alcohol molecules under a solvent thermal condition; and centrifugally separating, washing and drying an obtained solid substance so as to obtain the niobium hydroxide grafting with the aromatic alcohol on the surface. The niobium hydroxide grafting with the aromatic alcohol on the surface prepared by the invention is yellow powder, can effectively absorb visible light, and degrades pollutant rhodamine B, methyl orange and phenol under the visible light radiation; and reactions such as preparation of benzaldehyde through selective oxidation of phenylcarbinol, reduction of heavy metal ion hexavalent chromium Cr (VI), and reductive dechlorination of chlorophenol pollutants show that the niobium hydroxide grafting with the aromatic alcohol on the surface has better catalytic activity, is non-toxic, high-efficient, not easy to inactivate, and wide in application range, and has a favorable application prospect in the photocatalysis field.

The invention discloses a solvothermal preparation method of NbS2 nanosheet self-assembled hollow microspheres. According to the preparation method, niobium pentachloride is used as a niobium source in an organic solvent environment, diethyl sulfide or other sulfur-containing compounds are used as a sulfur source, and the NbS2 nanosheet self-assembled hollow microspheres are prepared through a high-temperature reaction for a certain time. According to the preparation method, the NbS2 nano material is prepared by a simple one-step solvothermal method, the complex preparation process of the existing NbS2 nano material is greatly optimized, and meanwhile, the obtained NbS2 hollow nano microsphere is of a hollow open pore structure and is controllable in size and morphology. According to the invention, the problem of preparing the NbS2 nano material through a solvothermal method at a relatively low temperature is solved. The adopted raw materials are cheap, the preparation process is simpler, and the product NbS2 nanosheet self-assembled hollow microspheres are unique in morphology. The NbS2 nanosheet self-assembled hollow microspheres can be applied to the fields of electromagnetic wave absorption, catalysis, energy storage, biosensing and the like.