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3502 results about "Hydrothermal synthesis" patented technology
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Hydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures; also termed "hydrothermal method". The term "hydrothermal" is of geologic origin. Geochemists and mineralogists have studied hydrothermal phase equilibria since the beginning of the twentieth century. George W. Morey at the Carnegie Institution and later, Percy W. Bridgman at Harvard University did much of the work to lay the foundations necessary to containment of reactive media in the temperature and pressure range where most of the hydrothermal work is conducted.
The invention discloses a method for preparing aerogel materials by combining hydrothermal synthesis technology and sol-gel technology. The prepared aerogel comprises one or more of aluminaaerogel, silica aerogel, zirconia aerogel and titania aerogel. The method comprises the following steps: mixing a reactant and a structure-directing agent according to certain proportion, and adding a pH value control agent to adjust the pH value; sealing hydrothermal reaction equipment, heating the mixture to be between 50 and 280 DEG C, making the mixture stand for 0 to 72 hours, raising the temperature to be between 60 and 300 DEG C, and continuously reacting for 0.1 to 72 hours; and cooling gel, taking out the gel, drying the gel and obtaining the aerogel. Compared with the prior art, the method has low reaction temperature and pressure, small equipment investment and simple and controllable technology, reduces potential safety hazards, greatly improves the preparation speed of the aerogel, saves the production cost, and is favorable to realize commercial mass production.
The invention discloses a hydrothermal synthesis method of lithium-ion battery anode material of lithiumiron phosphate, relating two kinds of metalphosphate. The steps are as follows: lithium source and phosphorus source are dissolved in water or mixed with water, and added into the reaction autoclave, the quaternary cationic surfactants and the alkylphenols polyoxyethylene ethers nonionic surfactant is also added into the reaction autoclave, the air in the dead volume of the autoclave inside is purged by the inert gas, the autoclave is sealed and heated to 40-50 DEG C with stirring, a feed valve and an exhaust valve are opened, pure ferroussalting liquid is added into the autoclave, and then the autoclave is sealed for the reaction of the material at 140 to 180 DEG C for 30 to 480 minutes; the mixture ratio of the invention is set as follows: the molar ratio of Li, Fe and P is 3.0-3.15:1:1.0-1.15, and then the resultant is filtered, washed, dried and carbon-coated, thus the lithium iron phosphate is obtained. The lithium iron phosphate which is produced by the invention has the advantages that: the electrochemical performance is excellent, the particle size distribution of which the D50 is between 1.5 um to 2 um is even, the phase purity is above 99 percent and the electronic conductivity of the material is improved.
The invention discloses a graphene nano sheet / MoS2 composite nano material and a synthesis method thereof. The method comprises the following steps of: preparing a graphiteoxide nano sheet from graphite by using a chemical oxidation method, then dissolving molybdate into deionized water to form a solution of 0.02 to 0.07M, and adding thioacetamide or thiourea serving as a sulfur source and a reducer, wherein the mass ratio of the thioacetamide or the thiourea to the molybdate is 5:1-12:1; and adding the graphiteoxide nano sheet into the solution, performing ultrasonic treatment for 1 to 2 hours so that the graphite oxide nano sheet is fully dispersed in a hydrothermal reaction solution, transferring the mixture into a hydrothermal reaction kettle, sealing, reacting for 20 to 36 hours at the temperature of between 220 and 260 DEG C, and obtaining the graphene nano sheet / molybdenum disulfide composite nano material by one-step hydrothermal synthesis, wherein the mass ratio of the graphene nano sheet to the molybdenum disulfide in the composite material is 1:2-4:1. The method has the characteristics of mild reaction condition and simple process. The synthesized graphene nano sheet / molybdenum disulfide composite nano material serving as an electrochemical lithium storage and electrochemical magnesium storage electrode material has wide application.
The present invention relates to a hydrothermal synthesis preparation method of a lithiumiron phosphate of an anode material used by a lithiumion battery, concerning a phosphate containing two metals. The step is that a lithium source and a phosphor source are solubilized into the water or mixed with the water and then put into a high pressure kettle. After the air in the kettle is blown out by an inert gas, the high pressure kettle is sealed and heated to a temperature between 40 DEG C and 50 DEG C from a room temperature after being stirred. An inlet valve and a vent valve are opened and then a prepared divalentferric salt liquor is added in. The high pressure kettle is sealed and the reaction time lasts from 200 minutes to 480minutes at the temperature between 140 DEG C and 170 DEG C. At the time, the inner pressure corresponding to the system is from 0.36 MPa to 0.85 MPa. The mixture rate of the added substance is Li: Fe: P and the mol ratio is 3.0-3.15: 1: 1.0-1.15. When the reaction starts, the reactant concentration is from mol / L 0.2 to 1.0mol / L, computed according to the concentration of the ferrousion and then the resultant is filtrated, cleaned, dried and coated with the carbon. Finally the lithium iron phosphate product can be obtained. The present invention has the advantages of simple technology, good batch stability, good electrochemical performance and even distribution. The purity quotient can be more than 99 percent and the grain diameter D50 is between1.5Mu m and 2Mum.
The invention provides a method for preparing a high-performance molybdenum-based hydrogen evolution electrode by phosphatizing a molybdate precursor and belongs to the fields of water electrolysis and electric catalytic hydrogen evolution in the chlor-alkali industry. The method comprises the steps of pre-processing foamed nickel, growing the molybdate precursor in situ on the surface of a pre-processed foamed nickel base with the hydrothermal synthesis method, and finally placing the prepared precursor and a phosphorus source into a rube furnace together for phosphating of the molybdate precursor so that the high-performance molybdenum-based hydrogen evolution electrode can be prepared. The method is novel, the technology adopted is simple, production cost is low, the requirement for equipment is low, and the method is suitable for industrial production. Furthermore, the electrode is large in specific area, can be combined with the base firmly, has excellent hydrogen evolution activity and stability, and can be widely applied to the fields of water electrolysis and hydrogen evolution in the chlor-alkali industry.
The invention provides a controllable synthetic method of graphitized carbon spheres with a hollow structure. The controllable synthetic method comprises the following steps of: (1) dissolving a carbon source, soluble metal salts and a catalyst in deionized water according to proportioning, stirring till completely dissolving, transferring to a hydrothermal reaction kettle for hydro-thermal synthesis, and washing, filtering and drying precipitates to obtain primary products; (2) reducing the primary products at a high temperature in a high-temperature reaction furnace under the production of gas; and (3) placing the products obtained through reduction in an acid solution for soaking, and washing, filtering and drying to obtain the graphitizing carbon spheres with the hollow structure. The graphitizing carbon spheres with the hollow structure have the advantages that the morphology is uniform, the carbon shells are of microcellular structures, the interiors of the carbon spheres are of mesoporous support structures, the graphitization degree is good, and the like. The graphitizing carbon spheres can be used in numerous fields of high-efficiency catalytic conversion, energy source storage and transition, medicine release control, matter adsorption and separation and the like. An invented formwork-free hydrothermal synthesis technology is simple and controlled and can be used for large-scale production.
The present invention relates to a preparation method of carbon quantum dots with adjustable fluorescence colors, and belongs to the technical field of nanometer materials. According to method, citric acid or a citrate is adopted as a carbon source, a nitrogen-containing compound is adopted as a nitridation agent, hydrogenperoxide is adopted as an oxidant, a hydrothermal synthesis method is adopted to obtain an aqueous solution of carbon quantum dots emitting blue or green fluorescence under ultravioletlight excitation, reaction conditions are easily controlled, and the method is suitable for scale production. The prepared carbon quantum dots have advantages of adjustable fluorescence color, high yield, high quantum efficiency, good result reproducibility and the like, wherein the product can be directly used for tumor cell labeling and live cell imaging labeling. According to the present invention, only the one reactant is required, the raw materials are easily-available and non-toxic, the production process does not require special protection, the reaction condition is easily controlled, and the obtained carbon quantum dots have advantages of high yield, high quantum efficiency, good result reproducibility and the like; and the method has characteristics of high yield, simple preparation process, low cost, easy scale production and the like.
The invention discloses a controllable synthesizing method of an N-doped graphitized carbon ball with hollow structures. The method comprises the following steps: (1) dissolving silicon source, soluble metal salt and a catalyst to the solvent according to the molar ratio, transferring the solvent to the thermal water kettle to conduct hydro-thermal synthesis after being stirred until being thoroughly dissolved, and cleaning, filtering and drying the sediment to obtain a primary commodity; (2) reducing the primary commodity at high temperature under the protection of gas in a high-temperature reaction furnace; and (3) soaking the product obtained by high-temperature reducing in acidic solution, and obtaining the graphitized carbon ball nitrogendoping with the hollow structure after cleaning, filtering and drying. The graphitized carbon ball with the hollow structures provided by the invention has the advantages that the carbon sphere has a uniform appearance, the carbon shell has millipore structures, a mesoporous carbon support structure is formed inside the carbon sphere and a better graphitize degree is provided, and can be used in the field of high-efficient catalyzing and transforming, energy storage and transforming, medicine releasing, substance adsorptive separation and the like. The non-template hydrothermal synthesis technique provided by the invention is simple and controllable, and can be used in large scale production.
Disclosed is a method for preparing a lithium-metalcomposite oxide, the method comprising the steps of: (a) mixing an aqueous solution of one or more transition metal-containing precursor compounds with an alkalifying agent and a lithium precursor compound to precipitate hydroxides of the transition metals; (b) mixing the mixture of step (a) with water under supercritical or subcritical conditions to synthesize a lithium-metalcomposite oxide, and drying the lithium-metalcomposite oxide; and (c) subjecting the dried lithium-metal composite oxide either to calcination or to granulation and then calcination. Also disclosed are an electrode comprising the lithium-metal composite oxide, and an electrochemical device comprising the electrode. In the disclosed invention, a lithium-metal composite oxide synthesized based on the prior supercritical hydrothermal synthesis method is subjected either to calcination or to granulation and then calcination. Thus, unlike the prior dry calcination method or wet precipitation method, a uniform solid solution can be formed and the ordering of metals in the composite oxide can be improved. Accordingly, the lithium-metal composite oxide can show crystal stability and excellent electrochemical properties.
The invention discloses a hydrothermal synthesis method of molybdenum disulfide nano flowers. The hydrothermal synthesis method mainly comprises the following steps: adding an inorganic molybdenum source, an organic sulfur source and a proper amount of reducing agent into deionized water, uniformly mixing the ingredients, transferring the mixture into a high pressure reaction kettle, and then heating the mixture at a high temperature for 24 hours; washing and centrifugally separating the obtained solution for multiple times, and finally drying the solution to obtain black solidpowder, namely, the molybdenum disulfide nano flowers. The hydrothermal synthesis method disclosed by the invention has the beneficial effects that the whole reaction and drying process is carried out in a sealed environment to avoid direct air exposure so as to ensure the product purity; since the reducing agent adopted by the hydrothermal synthesis method disclosed by the invention can be both used as the sulfur source and as a catalyst, no impurity is generated, and thus, the product purity is further improved.
The invention provides a method of partial vulcanization to improve oxygen evolution electrode performance of metalhydroxide and belongs to the field of oxygen evolution catalyzation of electrolysis of water. The method comprises the following steps: firstly, pretreatment is carried out on nickel foam, then, special nano floriform metalhydroxide is formed on the surface of the nickel base after the pretreatment in an in-situ growth manner through the hydrothermal synthesis method, and finally, the prepared metalhydroxide and a sulphur source have hydrothermal reaction to prepare a hydroxyl metal sulfideoxygen evolution electrode. According to the invention, the method is novel, the demanded technology is simple, the production cost is low, requirements to equipment are lower, and industrial production is suitable; in addition, the prepared electrode has excellent oxygen evolution activity and stability, is large in specific surface area, firmly combines with a base, and can be applied to the field of oxygen evolution through industrial electrolysis of water.
A synthetic method of a novel visible light photocatalyst Bi2MoO6 (bismuthmolybdate) is provided. The method includes the following steps: weighing Bi(NO3)3*5H2O and (NH4)6Mo7O24*4H2O solids at the theoretical ratio by mass of 14:1, dispersing the weighed solids into an appropriate amount of deionized water, stirring to obtain white curdy precipitates, placing the precipitates in a magnetic stirrer and stirring at normal temperature for 30 minutes, subjecting to ultrasonic treatment with a ultrasonic generator for 30 minutes to allow intensively mixing, allowing reactions of the treated white precipitates at 150-200 DEG C under sealed conditions, filtering the reaction product to collect flavescent precipitates, washing, drying, and grinding to obtain Bi2MoO6 (bismuthmolybdate) photocatalyst. The photocatalyst has good photodegradation effect on target pollutants; and when the temperature of hydrothermal synthesis is 160 DEG C, the removal rate of target pollutant 4BS after photodegradation for 90 minutes reaches 99.5%. The inventive synthetic method has the advantages of simple process and low requirement for equipment, and is suitable for the synthesis of highly-active visible light photocatalyst Bi2MoO6 (bismuthmolybdate).
The invention relates to a method for preparing water-soluble fluorescent carbon dots. The method comprises the following steps: by adopting a citric acid as a carbon source, urea as a passivator and a dopant and deionized water as solvents aiming at the conditions that the fluorescent carbon dots are high in accuracy and difficult to synthesize, preparing a carbon dot water solution by adopting a hydrothermal synthesis method; and preparing the carbon dots by the following processes of preparing the solution, air-tight reaction, filtering, dialyzing, freezing and drying, and grinding. The technology is advanced in process, rapid and efficient, accurate and specific in data, and good in product shape; the product is green powder particles; and the diameters of the particles are smaller than or equal to 5.5nm; the product is high in purity which can be up to 99%, and good in water-solubility which can be up to 99.5%. The method is an ideal method for preparing the fluorescent carbon dots. The product can be applied to the fields such as ion detection, bioimaging, photoelectric devices and composite materials.
The invention discloses a visible light responsive pucherite-graphene composite photocatalyst and a preparation method thereof. The composite photocatalyst is prepared by compositing pucherite and graphene according to the mass ratio of (1:2)-(1:5). The preparation method comprises the following steps of: putting graphiteoxide into a mixed solution of water and ethanol for ultrasonic dispersion,respectively adding bismuthnitrate and ammonium metavanadate into ethanol for stirring, and finally mixing the three systems and regulating the pH to be greater than 7; then, transferring the mixed system into a hydrothermal kettle for reacting; and after the reaction is finished, centrifugally separating, washing and drying the product to obtain a leaf-shaped pucherite-graphene composite photocatalyst. In the invention, by using graphene as a template, the leaf-shaped pucherite-graphene composite photocatalyst is prepared by a hydrothermal synthesis method. The pucherite-graphene composite photocatalyst prepared by the method disclosed by the invention has better application prospect and economic benefit in the aspect of sewage treatment.
The invention discloses a method for synthesizing an ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve TS-1 by using a hard template. The method comprises the following steps: with a three-dimensional ordered macroporous-mesoporous hierarchical carbon material as a hard template, performing limited-range growth of TS-1 nanocrystals in a three-dimensional ordered cage type mesoporous canal of the hard template by adjusting and controlling hydrothermal synthesis conditions according to a hydrothermal synthesis method of the TS-1 nanocrystals, and removing the hard template to obtain the ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve TS-1. The method disclosed by the invention is simple and feasible, synthetic conditions are easy to control, and the cycle is short; the molecular sieve TS-1 prepared by adopting the method has a novel ordered macroporous-mesoporous-microporous hierarchical pore structure, mesopores are uniform and controllable in diameter, and the method has an important promotion effect on expansion of application of the molecular sieve TS-1 in the field of catalysis.
The invention relates to a synthetic method for a magnetic metal organic framework composite material coated by [Cu2(btc)2] on surfaces of ferroferric oxide microspheres and application of the composite material. The method comprises the following steps of: firstly synthesizing ferroferric oxide microspheres by a hydrothermal synthesis method; dispersing magnetic spheres in an ethanol liquid of mercaptoacetic acid, wherein hydroxyls are formed on the surface of the spheres; dispersing mercaptoacetic acid modified magnetic spheres to an ethanol liquid of copper acetate, reacting for 15 minutes at 70 DEG C, and then dispersing the product in an ethanol liquid of trimesic acid and reacting for 30 minutes at 70 DEG C; and performing alternate reaction of magnetic spheres with copper acetate and the ethanol liquid of trimesic acid to finally, obtain the magnetic metal organic framework composite material with a core-shell structure. The material has a metal organic framework shell layer and can be coordinated with peptide fragments with amino groups and carboxylic group so as to enrich low concentration peptide. Meanwhile, the enriching and separating process is fast, simple and convenient due to high paramagnetism of ferroferric oxide. The synthetic method is simple and low in cost, and can be used for enrichment and separation of low abundance peptide fragments less than 1nM and MALDI-TOFMS (Matrix-Assisted LaserDesorptionIonization-Time Of FlightMassSpectrometer) detection.
The invention discloses a method for hydrothermally synthesizing a porous metal-organic framework under low temperature and normal pressure, which comprises the following steps: 1) bivalent transition metal salt is put into proper amount of distilled water to be dissolved; 2) a multidentate organic ligand is put into proper amount of distilled water, and ammonia (30 percent, W / W) is added into the solution until the organic ligand is dissolved; 3) solutions obtained in step 1) and step 2) are mixed, and diluted by the distilled water; 4) the solution obtained in step 3) reacts for 4 to 24h at a temperature of between 80 and 100 DEG C, and is naturally cooled to room temperature at an environmental temperature to obtain an MOF crystal product; and 5) the MOF crystal product obtained in step 4) is filtered, MOF crystals are colleted and washed by the distilled water and absolute ethyl alcohol respectively, and the product is obtained after the natural drying. By performing a hydrothermal reaction in an ammonia solution, the method has mild conditions needed by the synthesis, less energy consumption and time consumption, and does not need a voltage resistant reactor. Therefore, the method is simpler and has lower cost; and a porous crystal material obtained by the synthesis has potential application value in the fields of gas separation, gas storage and heterogeneous catalysis.