20 results about "Hydrothermal reaction" patented technology

This invention relates to the synthesis of large pore composite molecular sieves and to the synthetic large pore composite molecular sieves so produced. The molecular sieves of the invention have the same general utilities of the comparable molecular sieves of the prior art but have been found to be superior catalysts and absorbents. This invention relates to a hydrothermal synthesis of large pore molecular sieves from nutrients, at least one of which contains an amorphous framework-structure, and which framework-structure is essentially retained in the synthetic molecular sieve. This invention stems from a discovery that the intrinsic porosity characteristics of a nutrient that possesses an amorphous cation oxide-framework can be substantially retained in the final molecular sieve containing product formed by a hydrothermal process by carefully controlling the conditions under which the hydrothermal process is conducted. For example, the invention contemplates retention of the particle size in a final molecular sieve-containing product that corresponds with that of an amorphous cation oxide-framework nutrient used in its manufacture. This invention drives the selection of process conditions to achieve one or more of macro and meso porosity ("large pore composite porosity") in the final molecular sieve product as a direct product of the hydrothermal reaction producing the molecular sieve. The invention allows the production of a molecular sieve that is in situ incorporated in the framework morphology of a solid cation oxide-framework used in the molecular sieve's manufacture.

The invention discloses a method for preparing a ZnWO4 nanorod photocatalysis material. The method includes preparing a tungstic acid solution A, a zinc chloride solution B and a sodium citrate solution C; dropwise adding the solution A and the solution C into the solution B to form a solution D; regulating potential of hydrogen (pH) of the solution D to 6-8, and uniformly stirring to obtain a solution E; adding the solution E into a microwave hydrothermal reaction kettle, performing a heating reaction, naturally cooling the solution E to the room temperature after the reaction is finished, and taking out the reaction kettle; and opening the reaction kettle, washing a product for 4-6 times by deionized water and absolute ethyl alcohol, and drying to obtain the ZnWO4 nanorod photocatalysis material. According to the method, the microwave hydrothermal method is utilized to rapidly synthesize the ZnWO4 nanorod with the photocatalysis property, the later crystallization heat treatment is not required, the obtained product is high in purity, and the shape is controllable. The ZnWO4 nanorod with the photocatalysis effect can be synthesized in 10 minutes, and the degradation rate of the prepared ZnWO4 nanorod to rhodamine B in 50-60 minutes can reach to 97%-99%.

The invention relates to a method and equipment for producing potassium manganate. The method comprises that: at a high temperature, by utilizing oxygen containing gas, mixed materials of enriched silicon-manganese mineral powder and a solution of caustic potash are subjected to gas-liquid parallel flow oxidation treatment; the 60 to 79 percent solution of caustic potash is heated up to the temperature of between 230 and 260 DEG C and sent into a three-phase circulation type bubbling reactor; the enriched silicon-manganese mineral powder is added into 5 to 18 percent solution of caustic potash and prepared into manganese pulp, and the manganese pulp is preheated up to the temperature of between 80 and 90 DEG C and sent into a reactor; compressed air preheated up to the temperature of between 140 and 200 DEG C is continuously filled in the reactor; the upper pressure of the reactor is maintained to be 0.2 to 0.5MPa, and the temperature of the suspension in the reactor is maintained to be between 230 and 250 DEG C; and the gas and liquid in the reactor jointly flow upward to perform contact reaction, the reaction time is 2 to 4 hours, and the coarse product of the potassium manganate is obtained. In the method, except the oxidation of the manganese powder, the dynamic hydrothermal reaction of calcium silicate is also performed, thereby reducing the consumption of alkali and fully utilizing natural resources and enriched silicon-manganese mineral resources.

The invention relates to the technical field of inorganic materials, and discloses a preparation method for a ferrous carbonate/graphene composite material. The preparation method comprises the steps of: I. mixing graphene materials, water-soluble ferrite, urea and water to form a suspension, wherein the mass ratio of the graphene materials to the water-soluble ferrite is (0.02-0.2):1, and the amount-of-substance concentration ratio of the urea to the water-soluble ferrite is (20-100):1; II. putting the suspension into a reaction kettle, controlling the temperature to be 100-180DEG C, and carrying out hydrothermal reaction for 4-12h to obtain the ferrous carbonate/graphene composite material. The invention further provides a lithium ion battery prepared by taking the ferrous carbonate/graphene composite material as a negative electrode material. By being synthesized through low-temperature hydrothermal reaction, the ferrous carbonate/graphene composite material is high in specific capacity and good in cycling performance, and has excellent development prospects after being applied to the negative electrode materials of the lithium ion battery.

The invention relates to a preparation method of perovskite structure lead titanate single crystal nanoparticles. The method adopts hydrothermal reaction and subsequent high-temperature calcination, a mixed precipitate of titanium and lead ions introduces reactant material of hydrothermal reaction, a potassium hydroxide mineralizer promotes partial crystallization of a product to form precursor powder, then the precursor powder is completely crystallized in a subsequent high-temperature calcination process, therefore, synthesis of perovskite structure lead titanate single crystal nanoparticles is realized. The method provided by the invention has characteristics of simple process, easy control, no pollution and low cost, and is easy for large-scale production. The prepared perovskite structure lead titanate single crystal nanoparticles have high purity, good dispersity, and uniform size.

The invention discloses a preparation method of nano-magnesium hydroxide. The preparation method comprises the following steps: carrying out ultrasonic dispersion on ammonia water and a sodium hydroxide solution so as to obtain a mixed alkali solution, and adding the mixed alkali solution into a reactor; putting the reactor in an ultrasonic field, dropwise adding a polyethylene glycol 6000 water solution into the reactor in a constant speed, and further carrying out ultrasonic dispersion for 0.5-1 hour; dropwise adding a magnesium chloride water solution into the reactor in a constant speed; after the dropwise adding of the magnesium chloride water solution, further carrying out ultrasonic dispersion for 0.5 hour; adding turbid liquid obtained in the reaction into a hydrothermal reaction kettle for treatment, so as to obtain Mg(OH)2 precipitates; and carrying out suction filtration, washing, drying and grinding on the precipitates, so as to obtain nano-Mg(OH)2. Nano-magnesium hydroxide is prepared by virtue of an ultrasonic-hydrothermal coupling method, and reaction conditions are easily controlled, so that the problems that nano-Mg(OH)2 particles easily form colloid in a solution and are unlikely to be filtered are solved; and the particle size of the prepared nano-Mg(OH)2 particles is small, the particle size distribution is uniform, the crystallization degree is high, the technical flow of the preparation method is simplified, the energy consumption is reduced, and the production cost is saved.

The invention discloses a preparation method of a SnS2 nanosheet loaded graphene-based nano composite material, which comprises the following steps: step 1, dispersing graphene oxide nanosheets in deionized water to prepare a graphene oxide solution; 2, dissolving tin tetrachloride in deionized water, and adding thiourea as a sulfur source and a reducing agent; 3, adding the graphene oxide solution in the step 1 into the solution obtained in the step 2, and carrying out mixing treatment through ultrasonic waves and transferring a mixture of the two solutions subjected to ultrasonic treatment into a hydrothermal reaction kettle for reaction to obtain a precipitate; and 4, centrifuging, washing, drying and grinding the precipitate obtained by the reaction in the step 3 to obtain the graphene nanosheet/tin disulfide composite nanomaterial. The graphene nanosheet/tin disulfide composite nanomaterial prepared by the method has higher capacity and stability when being used as a sodium storage electrode material.

The invention relates to a PbS nano-sheet preparation method. According to the method, analytically pure lead nitrate and L-cystine are adopted as reaction raw materials; deionized water is adopted as a solvent; analytically pure potassium hydroxide and sodium hexadecylbenzenesulfonate are adopted as reaction auxiliary agents; when lead nitrate and L-cystine are mixed in the solution, L-cystine is subjected to a reaction with Pb<2+>, such that a Cys-Pb<2+>-Cys complex is formed; under a high-temperature high-pressure hydrothermal reaction condition, the Cys-Pb<2+>-Cys complex is decomposed, such that a Pb<2+>-Cys complex is formed; with the extension of reaction time, under the hydrothermal condition, C-S bonds are broken, such that agglomerated PbS nano-ions are formed; during the decomposition process, under cystine obstruction and SDBS soft template restriction, PbS crystals extend with a trend of growing along a two-dimensional direction, such that large-area two-dimensional PbS nano-sheets are formed.

A preparing method of a Ag3PO4@Ag/carbon sphere ternary heterojunction composite material capable of selectively removing cationic dye is disclosed. The method includes subjecting a glucose solution having a mole concentration of 0.5 mol/L to a hydrothermal reaction in a hydrothermal reaction kettle at 180 DEG C for 5-8 h to obtain carbon spheres having an average diameter of 0.3-0.7 [mu]m; addingdropwise ammonia water having a concentration of 10-25 wt% into a AgNO3 solution having a concentration of 0.05-0.2 mol/L to prepare a transparent Tollens' reagent; adding the carbon spheres into theTollens' reagent with the mass ratio of the carbon spheres to the AgNO3 being 0.01-0.1:1 and stirring the mixture for 2-10 h; adding dropwise a Na2HPO4 solution into the mixture with the mole ratio of Ag<+> to PO<4><3-> being 3:1-10; reacting the mixture for 1-3 h; then performing centrifugation, filtration and washing; and drying a product in a vacuum drying oven at 50 DEG C to obtain the composite material. The composite material can rapidly and efficiently remove cationic dye and the synthesized composite material has good stability.

The invention discloses a method for preparing a vanadium-doped gallium antimonate visible light photocatalyst. The method comprises the following steps: (1) stirring and mixing gallium nitrate, antimony pentoxide, ammonium metavanadate and deionized water at room temperature, regulating the pH value to 1-5 through 2-6mol/L of nitric acid, and obtaining a nano powder precursor solution; (2) arranging the nano powder precursor solution in a high pressure reactor, raising the temperature to 100-200 DEG C at a speed of 1-5 DEG C per minute, preserving the temperature for 6-48 hours, carrying out hydrothermal reaction, naturally cooling to room temperature, taking the product out, washing by using deionized water and absolute ethyl alcohol, drying in a drying box at the temperature of 60-80 DEG C, and obtaining the vanadium-doped gallium antimonate visible light photocatalyst. The preparation of gallium antimonite nanoparticles and a vanadium doping process are synchronously realized, and the method is simple in process, easy to control and suitable for industrial production and application. The prepared vanadium-doped gallium antimonate visible light photocatalyst is high in visible light utilization rate and high in catalytic efficiency and can be used for treating wastewater containing organic pollutants.

The invention discloses a preparation method of a super-hydrophilic-super-hydrophobic controllable ZIS nano-grading material and an application thereof, and the preparation method comprises the following steps: taking InCl3.4H2O, ZnSO4.7H2O and CH3CSNH2 as raw materials, and carrying out a one-step hydrothermal reaction to obtain a Zn3In2S6 nano-grading material; and by regulating and controllingthe addition amount of CH3CSNH2 in the raw materials, realizing the regulation and control of the surface hydrophilic or hydrophobic characteristics of the obtained Zn3In2S6 (ZIS) nano-grading material. Under visible light, the obtained surface super-hydrophilic ZIS shows excellent removal activity of organic/inorganic pollutants in a water body, and the obtained surface super-hydrophobic ZIS shows excellent conversion activity of pollutants in the atmosphere.

The invention provides a reduced graphene/alpha-Fe2O3 supercapacitor material and a preparation method and application thereof. The preparation method of the reduced graphene/alpha-Fe2O3 supercapacitor material comprises the following steps: (1) dissolving Fe (NO3) 3.9H2O, CTAB, urea and graphene oxide dispersion in a methanol solution and performing hydrothermal reaction at 160-200 DEG C for 8-24h; (2) pumping and filtering the reaction product obtained in the step (1), adding the obtained solid and thiourea into water, uniformly mixing and transferring to a reaction kettle and performing hydrothermal reaction at 160-200 DEG C for 8-24 hours; and (3) pumping and filtering the product obtained in the step (2), freezing and drying and then performing heat treatment. The supercapacitor material is simple in preparation of the working electrode, and the electrochemical working window in the alkaline electrolyte is from -1.05 V to -0.3 V and the maximum specific capacity can be 1296 F/g so as to be an ideal negative electrode material. The shortcoming of low specific capacity of the negative electrode material of the supercapacitor can be overcome, the problem of mismatch between thepositive electrode and negative electrode specific capacity of the supercapacitor can be solved and thus the material has high research value.

The invention discloses a preparation method of Bi4Ti3O12 micron sheets. The preparation method comprises the following steps: mixing tetrabutyl titanate, bismuth nitrate pentahydrate and water so as to obtain suspension, mixing KOH with the suspension, further dripping a PVA solution into the suspension so as to obtain a precursor solution, and performing hydrothermal reaction for 22-24 hours at 220-240 DEG C, thereby obtaining the Bi4Ti3O12 micron sheets, wherein the mole ratio of bismuth nitrate pentahydrate to tetrabutyl titanate is (3.75-4.25) to (2.75-3.25), the concentration of KOH in the precursor solution is 0.8-1.2mol/L, the concentration of Bi<3+> is 0.1-0.2mol/L, and the concentration of PVA is 0.02-0.03mol/L. By precisely regulating and controlling the use amount of the above raw materials and the conditions of the hydrothermal reaction, the Bi4Ti3O12 micron sheets are prepared, and the preparation process is simple, can be easily controlled and can be applied to large-scale industrialized production.

The invention relates to the field of plastic masterbatch, and discloses a graphene magnetic injection molding masterbatch for nylon electrical appliance plastics, and a preparation method thereof. The preparation process comprises: (1) adding sulfonated graphene, an iron salt and a ferrous salt to deionized water, and carrying out a hydrothermal reaction to obtain graphene-Fe3O4 nanometer composite magnetic micro-particles; (2) carrying out surface treatment on the composite magnetic micro-particles, adding nylon 6 and a dispersant, and carrying out melt extrusion to obtain a nylon 6 melt; and (3) mixing melt, polyamide-amine, adipic acid and hexanediamine, carrying out a condensation polymerization, carrying out pressure relief, drying, and crushing to prepare the graphene magnetic injection molding masterbatch. According to the present invention, the nanometer composite magnetic micro-particles are coated with the hyperbranched nylon 6 with characteristics of good compatibility withthe nylon injection molding matrix and high fluidity, such that the dispersibility of the magnetic powder in the nylon is substantially improved, the melt has good fluidity, the processing performance is excellent, and the method is suitable for popularization and application.

The invention discloses a preparation method of a special-morphology micro nano structural lithium-rich manganese-based cathode material, and belongs to the technical field of novel energy material energy storage material preparation processes. The method comprises the following steps: dissolving a manganese salt and a nickel salt into distilled water according to a ratio to obtain an A liquid; dissolving a homogeneous precipitant weighed according to a ratio into distilled water to obtain a B liquid, introducing a certain ratio of an ionic liquid into the B liquid, performing full stirring, and performing uniform mixing; mixing the A liquid and the mixed B liquid, and performing full stirring; transferring the mixed liquid to a hydrothermal reaction kettle, performing a hydrothermal reaction, performing cooling to room temperature, performing centrifugal separation, performing washing, and performing drying to obtain a manganese-based precursor material; and finally grinding the precursor and a certain ratio of lithium carbonate, performing uniform mixing, performing pre-sintering, and performing calcination to obtain the lithium-rich manganese-based cathode material. The method provided by the invention solves the problems of high energy consumption, long consumed time and difficulty in control of product topography characteristics in the preparation process in the prior art.

The invention discloses a preparation method of nanometer strontium-doped hydroxyapatite powder. The preparation method comprises the following steps of: dissolving prepared Ca(NO3)2.4H2O and Sr(NO3)2.4H2O in water to form a 1# solution, dissolving Na2HPO4.12H2O in water to form a 2# solution and adjusting the pH values of the 1# solution and the 2# solution to 9-11; slowly adding the 2# solutionto the 1# solution and adjusting the pH value of the mixed liquid to 9-11; heating the mixed liquid to 60-80 DEG C, stirring for 1-3h, and adjusting the pH value to 9-11; then heating to 130-170 DEG C, preserving the temperature for 4-8h and carrying out a hydrothermal reaction; carrying out cooling, extraction filtering, washing and drying in sequence after the hydrothermal reaction is ended to obtain the nanometer strontium-doped hydroxyapatite powder. The preparation method disclosed by the invention is simple, economic and controllable; experiment conditions are looser; purer strontium-doped HA (hydroxyapatite) powder with very even grain diameter can be obtained in the larger Ca/Sr rate and temperature range; and the preparation method disclosed by the invention is applied to industrial large-scale production.

The invention relates to a method for preparing blue-shifting TiO2 microspheres. The method comprises the following steps: adding titanium sulfate in deionized water to obtain a solution A; adding urea in deionized water to obtain a solution B; slowly dripping the solution B in the solution A to obtain a solution C; mixing a dimethylformamide solution D and the solution C to obtain a solution E; transferring the solution E to a hydrothermal reaction kettle lined with Teflon, sealing the hydrothermal reaction kettle and then putting the sealed hydrothermal reaction kettle in a temperature-pressure-controlled microwave hydrothermal reaction instrument for preparation reaction in a temperature control mode, and carrying out natural cooling after the completion of reaction; and allowing the obtained white turbid liquid to stand, alternately washing the white turbid liquid with ethanol and deionized water, then carrying out centrifugal collection by taking absolute alcohol as the solvent, and drying to obtain the products, namely TiO2 microspheres. The microwave radiation heating method is adopted, the regular spherical blue-shifting TiO2 microspheres are further prepared in the high-temperature and high-pressure hydrothermal environment, and the blue-shifting TiO2 microspheres are 1-2 mum in diameter, 3.35 ev in forbidden bandwidth and better in dispersivity.

The invention relates to the technical field of material preparation, in particular to a preparation method of anhydrous barium carbonate crystals with special morphology. The preparation method comprises the following steps: respectively preparing a barium chloride solution with a concentration of 0.01-1 mol/L and a sodium carbonate solution with a concentration of 0.01 mol/L; adding a crystal form control agent into the barium chloride solution, and conducting stirring to prepare a primary solution; adding a sodium carbonate solution into the primary solution, carrying out stirring and heating to 30-70 DEG C, and carrying out a hydrothermal reaction to obtain reaction slurry; and filtering the reaction slurry, washing a white precipitate with deionized water to remove chloride ions, performing drying with an electrothermal blowing dryer to prepare spherical and petal-shaped anhydrous barium carbonate crystals, and distilling a filtrate to obtain sodium chloride crystals. The method disclosed by the invention is short in reaction time, simple in production process and equipment, high in product yield, low in cost, free of environmental pollution and easy to realize industrial production.