66 results about "Solvothermal synthesis" patented technology

The application discloses a supercritical hydrothermal and solvothermal synthesis nanometer composite zirconia system and quality control method, belongs to the technical field of energy chemical industry, and sets material composite deployment and delivery unit, heat reuse unit, reaction post-processing unit and additional product recovery unit to constitute the whole preparation system. The supercritical hydrothermal and solvothermal synthesis nanometer composite zirconia system integrates energy reuse, additional product recovery and quality control and the like into one, can realize heat energy efficient utilization, additional product recovery and quality efficient control system, can realize energy level matching in the heat energy utilization process, can realize resource utilization in the post-processing link, can realize nanometer zirconia particle size control, purity control, crystal form stability and anti-agglomeration in the whole system operation, improves system thermal efficiency, reduces operation cost, saves energy, and simultaneously obtains high-quality nanometer zirconia particles, and lays a foundation for the industrialization process of continuous supercritical hydrothermal / solvothermal synthesis.

The invention discloses a process for preparing a V2O3 / ZnV2O3 total battery by simultaneously using vanadium oxide in a zinc ion battery as a positive electrode material and a negative electrode material, which comprises the following steps: reacting ammonium metavanadate with absolute ethyl alcohol by adopting a solvothermal synthesis method, washing, drying, and calcining in a tubular furnace to obtain V2O3; in the preparation process of the V2O3 positive electrode material, only V2O3, acetylene black serving as a conductive agent and PVDF serving as a binder are mixed in proportion and then are coated on graphite paper, other coating protection materials do not need to be introduced into a V2O3 / Zn negative electrode, and V2O3 is used as a protection layer to inhibit growth of zinc dendrites, relieve hydrogen evolution side reaction of the zinc negative electrode and reduce corrosion of zinc. Vanadium oxide V2O3 is directly used as a core positive electrode material, the zinc negative electrode coating is developed by utilizing the characteristics of the vanadium oxide V2O3, a material is formed, meanwhile, the performance optimization of the positive electrode and the negative electrode is realized, the used raw materials are simple and easy to obtain, the process is simple and easy to implement, and the preparation process is simple and easy to implement from V2O3 raw material synthesis to positive and negative electrode piece preparation to V2O3 / ZnV2O3 total battery assembly. And comprehensive improvement of positive and negative electrode performances of zinc ions is simultaneously realized by a single material.

In the production of an MOF membrane complex, seed crystals of a CAU-10 MOF are deposited on a support, an Al source solution that is an aqueous solution containing an Al ion source is prepared, and a ligand solution is prepared in which an organic ligand used for synthesis of the CAU-10 MOS dissolves in a solvent. Then, a starting material solution is prepared by mixing the Al source solution and the ligand solution at a rate that does not cause the starting material solution to become cloudy. The support is immersed in the starting material solution to form an MOF membrane that is the CAU-10 MOF on the support by Solvothermal synthesis.

This invention discloses a method for preparing interface-reinforced niobium pentoxide / porous graphene and its energy storage application. The method involves adding porous graphene oxide during the solvothermal synthesis of a niobium pentoxide precursor to obtain a composite precursor of niobium pentoxide and porous graphene oxide. This precursor is then annealed under a protective atmosphere to obtain the interface-reinforced niobium pentoxide / porous graphene composite material. The composite material obtained by this invention exhibits excellent performance as an electrochemical energy storage material. Furthermore, the preparation method of this invention is simple to operate, requires no complex equipment, and is easily controlled, making it suitable for mass production.

The invention discloses a Fe / Ce bimetal-based organic framework and a preparation method and application thereof.The Fe / Ce bimetal-based organic framework is obtained through an acid-base neutralization reaction of a Ce-based metal organic framework material and alkaline ferric hydroxide, and the preparation method specifically comprises the following steps that 1, Ce (NO3) 2.6 H2O solution and a 1, 3, 5-benzene tricarboxylic acid solution are mixed and subjected to a stirring reaction, synthesis is conducted through a solvothermal synthesis method, and the Fe / Ce bimetal-based organic framework is obtained; washing the precipitate obtained by the reaction, and drying in vacuum to obtain the Ce-based metal organic framework material (Ce-MOFs); and (2) Ce-MOFs and Fe (OH) 3 are subjected to in-situ acid-base neutralization, Fe enters an uncoordinated carboxyl skeleton, and Fe / Ce bimetallic doping is achieved. The preparation method is simple and easy to operate, and the prepared bimetal-based organic framework has a cluster overlapping structure, is large in specific surface area, shows sensitive detection characteristics on aflatoxin, and can be used as an electrode modification material to quickly, sensitively and accurately detect low-concentration aflatoxin in a detection environment and a food sample.

This invention discloses a hydrazone-linked fluorine-substituted covalent organic framework material, its preparation method, and its applications, belonging to the field of semiconductor photocatalysis technology. The material is synthesized by hydrazone condensation of 1,3,5-trifluoro-2,4,6-tris(4-formylphenyl)benzene and terephthalohydrazide, denoted as F-TPDH-COF. A one-step solvothermal synthesis is employed, resulting in a mild, environmentally friendly, low-cost, and easily scalable process. The material obtained by this invention utilizes hydrazone bonds to achieve proton enrichment in acidic media, and fluorine atoms regulate the electronic structure to improve charge separation efficiency. Under pH=2 conditions, the photocatalytic hydrogen peroxide production rate reaches as high as 5825.2 μmolg. ‑1 h ‑1 Its activity and stability are significantly better than most existing COF photocatalytic materials, and it can be used for efficient photocatalytic preparation of hydrogen peroxide in acidic systems, showing good prospects for industrialization.

The application provides a kind of copper sulfide@nickel disulfide positive electrode material based on two-dimensional nanosheet wrapping three-dimensional cube and its preparation method and lithium-magnesium dual-ion battery, first using copper salt, alkaline solution and D (+) -glucose in the water bath condition of 70 DEG C, directional formation Cu2O cube.And then, Cu2O and nickel source, sulfur source and surfactant are synthesized by solvothermal synthesis, forming the structure of two-dimensional and three-dimensional combination of NiS2 nanosheet wrapping Cu2S cube.The two-dimensional and three-dimensional combination structure can shorten the particle transmission path, achieve the effect of fast charging and discharging, at the same time, provide more active sites, increase the specific surface area, fully contact with electrolyte, improve the cycle stability of battery.

The invention relates to a preparation method of a Co-based MOF material constructed based on H3BTTC. The preparation method comprises the following steps: adding a ligand and a metal salt into N, N-dimethylacetamide through a conventional solvothermal synthesis method, adding a tetrafluoroboric acid aqueous solution to adjust the pH value and polarity of the solution, heating and crystallizing in a drying oven, washing a product with a solvent for multiple times, and carrying out vacuum drying to obtain a target material. The method can accurately regulate and control pore channels, conditions are mild and efficient, the performance of the material in the fields of gas adsorption and separation, catalysis, sensing and the like is effectively improved, and the remarkable advantages are enhanced.

A biphenylthiourea carboxylic acid metal organic framework crystal material and a preparation method and application thereof.The material has the following chemical formula: {[Zn4O(L)3]·DMF·H2O} n , wherein L is a 6-thio-6,7-dihydro-5H-dibenzo[d,f][1,3]diazepine-3,9-dicarboxylate divalent anion, and n is a degree of polymerization.The metal organic framework crystal material of the present application is synthesized by a solvothermal method, is simple to operate, has low cost, high yield, and is easy to mass industrial production.The prepared metal organic framework crystal material has a high specific surface area (a BET specific surface area of 594 m 2 / g), and an adsorption amount of CO2 of 46.0 cm 3 / g at 1 atm and 273 K.The biphenylthiourea carboxylic acid metal organic framework crystal material of the present application can efficiently catalyze a Friedel-Crafts alkylation reaction of substituted indole and substituted trans-nitrostyrene to generate an indole 3-substituted derivative, and can also efficiently catalyze a Michael addition reaction of diethyl malonate and substituted trans-nitrostyrene, both of which have mild conditions, and the catalyst can be recycled with almost no activity loss, and are good heterogeneous catalysts.

This invention provides a porous transparent Ga2O3 nanoceramic material and its preparation method. 0.5 g of Ga(NO3)3·9H2O was poured into 15 ml of anhydrous ethanol and stirred until a clear precursor solution was formed. This solution was then transferred to a polytetrafluoroethylene (PTFE) liner, and a solvothermal synthesis reactor was assembled and placed in a constant-temperature drying oven at 180 °C for 15 h. After the reaction, the reactor liner was opened, revealing a gel-like product. This product was washed three times with anhydrous ethanol by centrifugation, resulting in a white gel-like product. It was then dried in a constant-temperature drying oven at 80 °C for 10 h. The dried precursor was then placed in a muffle furnace and calcined at 500 °C for 5 h. The resulting ceramic material exhibited a maximum transparency of 79.64%. This invention yields a porous, transparent Ga2O3 nanoceramic material under normal pressure. The material is sintered from γ-Ga2O3 nanoparticles, exhibiting an irregular, near-spherical morphology with an average particle size of 5.86 nm. The nanoparticles form a nanoporous structure with pore diameters ranging from approximately 2 to 20 nm, showing a significant peak at 4.74 nm. The specific surface area is 159.3 m². 2 / g.

The present application belongs to the technical field of fuel cell science and technology, and particularly relates to an oxygen reduction catalyst of carbon nanotube / covalent organic framework compound coupled polyaniline conductive polymer and a preparation method and application thereof. The present application takes thionine and 1,3,5-tri(p-formylphenyl)benzene as raw materials, prepares a covalent organic framework compound through a solvothermal synthesis method, combines the covalent organic framework compound with carbon nanotubes, and uses an in-situ chemical oxidation polymerization method to prepare a polyaniline-coated carbon nanotube / covalent organic framework compound material, so as to form a carbon nanotube / covalent organic framework compound coupled polyaniline conductive polymer functional material modified fuel cell cathode which has high conductivity and porosity. The method of the present application has low cost and strong operability. The prepared oxygen reduction catalyst has superior oxygen reduction catalytic performance, exhibits good electrochemical activity and stability, and can be used as a fuel cell cathode catalyst to improve the electrochemical performance in actual application.

The invention relates to a synthesis method of a polyacrylamide modified Ni-Pt bimetallic nano-enzyme and application of the polyacrylamide modified Ni-Pt bimetallic nano-enzyme in detection of penicillin residues. Nickel acetate, platinum acetylacetonate (II), sodium acetate and polyacrylamide (PAM) are used as basic raw materials, a solvothermal synthesis method is adopted, the Ni-Pt bimetallic nano-enzyme which is simple in process, excellent in catalytic performance and stable in material property is synthesized, and the Ni-Pt bimetallic nano-enzyme is successfully applied to construction of a penicillin direct detection method system. The system has the characteristics of high sensitivity, good selectivity, low cost, convenience and rapidness, and penicillin in a water sample can be efficiently and directly detected. According to the invention, not only is the prospect of the high-activity bimetallic nano-enzyme shown, but also an expected way is provided for environmental antibiotic monitoring.

The application provides a bimetallic sulfide modified cadmium selenide photocatalyst and a preparation method and application thereof, and belongs to the technical field of photocatalytic hydrogen production. The application prepares cadmium selenide / copper molybdenum sulfide by hydrothermal reaction of copper molybdenum sulfide and cadmium selenide. The application successfully prepares cadmium selenide / copper molybdenum sulfide (CdSe / Cu2MoS4) with high purity and good crystallization by adopting a solvothermal synthesis method (hydrothermal reaction); the cadmium selenide (CdSe) is successfully modified by a method of constructing a heterojunction, and the photocatalytic hydrogen production performance is greatly improved, a new path is provided for modifying existing photocatalysts, and new impetus is injected into the development of photocatalytic hydrogen production technology.

The invention relates to an electro-catalysis electrode, a preparation method thereof and a method for preparing formic acid through electro-catalysis carbon dioxide reduction, and the preparation method of the electro-catalysis electrode comprises the following steps: carrying out two-phase solvent thermal synthesis reaction on a raw material mixture containing a bismuth source, an indium source, a first organic solvent and water to obtain a catalyst precursor; mixing the catalyst precursor, a binder and a second organic solvent to obtain a catalyst dispersion liquid; coating the catalyst dispersion liquid on the surface of an electrode substrate and drying to obtain a catalyst-loaded electrode; and carrying out constant-current activation treatment on the electrode loaded with the catalyst to obtain the electro-catalysis electrode. The electrocatalytic electrode disclosed by the invention has improved catalytic activity and catalytic stability, can effectively improve selectivity and Faraday efficiency when being used for preparing a formic acid product through electrocatalytic carbon dioxide reduction reaction, and has a good industrial application prospect.

The invention belongs to the technical field of material chemistry, and discloses a cobalt-doped ferric oxide material and a preparation method and application thereof.The preparation method comprises the following steps that 1, ferric chloride hexahydrate and cobalt nitrate hexahydrate are dissolved in deionized water, absolute ethyl alcohol and sodium acetate trihydrate are added, and stirring is conducted under the room temperature condition till solute is completely dissolved; 2, the precursor solution prepared in the step 1 is placed in an air atmosphere for magnetic stirring, then solvothermal synthesis is carried out, centrifugation, cleaning and drying are carried out after the reaction is finished, and the cobalt-doped ferric oxide material is obtained and comprises a framework formed by ferric oxide nano cubic crystals and a cobalt element, the cobalt element enters the framework to replace part of the iron element to form chemical bonds with the oxygen element, and the degradation rate of bisphenol A within 20 minutes is as high as 100%.

The application discloses a kind of based on sulfhydryl-UiO-66 high permeability composite nanofiltration membrane and preparation method thereof, steps are as follows: (1) using solvent hot synthesis method to prepare the suspension containing sulfhydryl-UiO-66;(2) the suspension of step (1) is centrifuged, after washing and drying, obtain sulfhydryl-UiO-66 nanomaterial;(3) preparation PIP aqueous solution and TMC n-hexane solution;(4) a certain concentration sulfhydryl-UiO-66 is ultrasonically dispersed in PIP aqueous solution or TMC n-hexane solution, obtain corresponding phase suspension;(5) PIP aqueous solution or PIP aqueous phase suspension is immersed PSF ultrafiltration membrane surface, subsequently n-hexane solution or n-hexane organic phase suspension is soaked PSF ultrafiltration membrane surface;(6) the membrane obtained in step (5) is heat treated and cleaned, obtain sulfhydryl-UiO-66 high permeability composite nanofiltration membrane.The composite nanofiltration membrane of the application has high permeability, high pore structure uniformity, and the effective separation of ion size similar cation.

The invention discloses a preparation method and application of a coordination polymer nanowire for catalyzing C-H bond functionalization, and belongs to the technical field of photocatalytic materials. According to the preparation method, a Cu-Cl chromophore is taken as a node, L is taken as a ligand, a three-dimensional chain-shaped coordination polymer material is constructed through a solvothermal synthesis strategy, and then the superfine coordination polymer nanowire with high catalytic activity is effectively prepared by adopting a solvent-assisted ultrasonic stripping technology. The prepared nanowire material is stable in chemical property and easy to put into practical application, and the accessibility of active sites can be greatly improved and the influence of the diffusion effect can be effectively inhibited in the catalysis process. A large number of Cu-Cl chromophores are uniformly distributed on the superfine one-dimensional nanowire, and the Cu-Cl chromophores and the photosensitive ligand L can activate inert C-H bonds and a green oxidant oxygen under light excitation so as to complete the functionalization process of the inert C-H bonds with high efficiency and high selectivity.

This invention discloses a highly uniform copper-based alloy powder for metal additive manufacturing and its production process, belonging to the field of alloy powder technology. First, zirconium oxychloride octahydrate, yttrium nitrate hexahydrate, and terephthalic acid are used as raw materials to obtain Zr-Y-MOF powder via solvothermal synthesis. Then, this powder is composited with nano-silicon carbide and pyrolyzed to obtain zirconium yttrium oxide-silicon carbide composite powder. Copper-coated composite refining agent is obtained through chemical copper plating. Finally, a double-crucible vacuum induction gas atomization process is used to in-situ alloy Cu-Cr and Cu-Nb master alloys, which are then instantaneously mixed and atomized with the composite agent to obtain highly uniform copper-based alloy powder. This invention solves the problems of high oxygen content, component segregation, and coarse grains in traditional copper-based additive manufacturing powders through the synergistic effect of double-crucible in-situ alloying and copper-coated composite refining agent. The resulting powder has uniform particle size, low oxygen content, and dense structure, making it suitable for the preparation of general copper alloy components in the field of metal additive manufacturing.

This invention belongs to the field of pharmaceutical technology, specifically relating to the application of a Co single-atom nanozyme in the prevention of radiation-induced intestinal injury. The invention first prepares a ZnCo-MOF material by coordinating zinc and cobalt metal ions with a 2-methylimidazole organic ligand via a solvothermal synthesis method. Subsequently, this MOF precursor is pyrolyzed at high temperature to convert it into a Co single-atom nanozyme, ultimately constructing a nanozyme material that combines multi-enzyme mimicry characteristics with oral pH responsiveness. This material achieves a dual core effect in the treatment of abdominal / pelvic tumors: enhancing the efficacy of radiotherapy and protecting the intestine from radiation damage. Its intestinal radiation protection mechanism is achieved by downregulating the PI3K / AKT pathway, reducing the formation of the extracellular neutrophil network (NETs), and scavenging reactive oxygen species in the intestine, thereby protecting the intestine from radiation damage. This invention provides a novel technical approach and implementation path for the clinical prevention and treatment of acute intestinal radiation injury.

The application provides a Co@ZrC catalyst and a preparation method and application thereof in furfural compound hydrogenation deoxygenation, the preparation method is as follows: using fumaric acid and zirconium salt as raw materials, a catalyst precursor Zr-MOF is prepared by a solvothermal synthesis method, then the precursor is impregnated with a cobalt salt, and in-situ high-temperature pyrolysis carbonization reduction is carried out to prepare the Co@ZrC catalyst. The catalyst is used in selective hydrogenation deoxygenation of furfural to prepare 2-methyl furan and selective hydrogenation deoxygenation of 5-hydroxymethyl furfural to prepare 2,5-dimethyl furan, and the target products are obtained in high yield. The catalyst preparation method is simple, the catalyst has high activity and selectivity and good stability, the furfural selective hydrogenation deoxygenation reaction condition is mild, the product yield is high, and obvious industrial production advantages are obtained.

Disclosed is an application of a magnetic carboxyl-functionalized covalent organic framework composite as a magnetic solid-phase extraction adsorbent. The preparation method for this composite comprises the following steps: (1) firstly, taking dopamine hydrochloride as a coordinating stabilizer, and synthesizing surface-aminated magnetic iron oxide particles by coprecipitating iron (III) chloride and iron (II) chloride; and (2) then activating the surface-aminated magnetic iron oxide particles, and performing covalent cross-linking on the surfaces of the aminated magnetic iron oxide particles by taking 1, 3, 5-triformylphloroglucinol (Tp) and 4, 4′-diamino-biphenyl-2, 2′-dicarboxylic acid as building blocks, acting under the reversible catalytic action of acetic acid and using a solvothermal synthesis method, so as to prepare the magnetic carboxyl-functionalized covalent organic framework composite. The carboxyl-functionalized covalent organic framework prepared has a large specific surface area, a good mesoporous structure, a stable structure, large adsorption capacity, a short balance time and multiple adsorption forces, thereby significantly simplifying the sample pretreatment steps and shortening the sample processing time.

This invention discloses a method for preparing and applying a carbon-supported platinum group metal-based high-entropy alloy, relating to the field of high-entropy alloy synthesis technology. The method includes the following steps: S1: Taking several transition metal precursor salts and one platinum group metal salt in a certain proportion, and dissolving the transition metal precursor salt and the platinum group metal salt in a mixed solvent to obtain a dispersion; S2: Transferring the dispersion into a reaction vessel for reaction, and then washing it by ultrasonic centrifugation after the reaction; S3: Drying the washed raw material in a vacuum oven to obtain a carbon-supported platinum group metal-based high-entropy alloy. This invention uses transition metals such as copper, iron, nickel, lead, zinc, vanadium, cobalt, molybdenum, and bismuth, which promote reduction reactions, to impregnate palladium metal, and uses a solvothermal synthesis method to prepare the platinum group metal-based high-entropy alloy. This preparation process allows the amorphous carbon generated simultaneously during the reduction of the metal precursor to act as a carrier, controlling both the flower-like alloy morphology and the dispersibility of the alloy particles in solution.

The invention belongs to the technical field of pervaporation membranes, and relates to a carbon nanotube-induced covalent organic framework membrane as well as a preparation method and application thereof. Comprising a covalent organic framework and a substrate, the substrate is a carbon nanotube modified porous polymer substrate, and the substrate is prepared by a suction filtration method; the covalent organic framework is prepared from an amino monomer and an aldehyde monomer by an in-situ solvothermal synthesis method; the covalent organic framework comprises a separation layer, the thickness of the separation layer is 30-50nm, and the aperture of the separation layer is 1.0-2nm. The carbon nanotube-induced covalent organic framework membrane prepared by the invention has high permeability and high salt rejection rate, and still keeps stable high performance under the conditions of high temperature, feeding with different salt concentrations and the like.

The application belongs to the technical field of optoelectronic materials, and particularly relates to a halogen-modified Schiff base zinc complex and a preparation method and application thereof. The Schiff base zinc complex is obtained by coordination of a halogen-substituted thiohemisemicarbazone Schiff base as a ligand with zinc ions; the chemical expression of the Schiff base zinc complex is C 11 H 13 RN4OSZn, wherein R is any one of Cl, Br and I. The Schiff base zinc complex has enhanced thermal stability and adjustable luminescence performance, and the luminescence wavelength can be adjusted by a halogen substituent, and the Schiff base zinc complex has application potential in optoelectronic devices such as light-emitting diodes. The application further provides a solvothermal synthesis method of the complex, which is simple to operate and has a high yield.

The invention discloses an IrCo-based nano-particle catalyst and a preparation method and application thereof.The preparation method comprises the following steps that Ir salt, Co salt, M salt and a surfactant are dissolved in polyhydric alcohol, a reflux reaction is conducted in an oil bath pan, grinding is conducted after drying, and secondary annealing treatment is conducted: heat preservation is conducted at the temperature of 200-300 DEG C for pre-alloying to form Ir-Co-M alloy nano-particles, carrying out heat preservation at 200-400 DEG C, and carrying out oxidizing annealing to form an oxide layer; and putting into an acid solution, and stirring to obtain the IrCo-based nano-particle catalyst. According to the preparation method, an Ir-Co-M ternary synergistic system is constructed, controllable solvothermal synthesis is adopted, air annealing is performed after pre-alloying, a stable metal oxide surface is formed, meanwhile, an alloy core is reserved, and therefore the optimal balance between activity and stability is achieved; the process is simple, the repeatability is good, and the prepared catalyst has high catalytic activity and excellent stability.

The invention discloses a preparation method of a GO (at) MOF-199 composite material for phenol-containing wastewater treatment, the preparation method comprises the main steps of preparing graphene oxide and GO (at) MOF-199, compounding, adopting a high-speed mechanical crushing and high-temperature chemical stripping method, preparing thin-layer graphene oxide in a mode of matching chemical solvent expansion with mechanical stirring stripping, and preparing the GO (at) MOF-199 composite material for phenol-containing wastewater treatment. Solvothermal synthesis and ultrasonic treatment are adopted for preparation and compounding of the GO-coated MOF-199, and the GO-coated MOF-199 composite material is used for characterization analysis and adsorption performance test of phenolic wastewater treatment when the GO-coated MOF-199 composite material is used for phenolic wastewater treatment. A certain proportion of graphene oxide is added in the preparation process of a metal organic framework compound, process conditions are adjusted to compound GO and MOF-199, the prepared GO-MOF-199 composite material is applied to phenol-containing wastewater treatment, adsorbent regeneration and phenol recovery are carried out, and the prepared GO-MOF-199 composite material has the advantages of environmental protection, environmental protection and the like. And the method has important significance on increasing sewage treatment, especially organic wastewater treatment of high-water-consumption enterprises such as coal chemical industry and the like.

This invention belongs to the field of wastewater treatment, and specifically discloses a copper-cobalt doped graphene MOF composite material, its preparation method and application. The graphene-doped bimetallic copper-cobalt MOF composite material was successfully prepared by solvothermal synthesis, exhibiting an octahedral porous structure with a very large specific surface area and pore volume, which can efficiently adsorb and photocatalytically degrade organic wastewater.

PMMAxPBMA1-x modified light diffusion particles containing nanoscale inorganic particle components are prepared through a simple solvothermal synthesis method, and the nanoscale inorganic particles are cross-linked to the surfaces of the light diffusion particles through the action of a coupling agent. The modified light diffusion particle has a high refractive index, and is beneficial to widening the visual angle range and maintaining the brightness at a high level.