53results about "Monoborane/diborane hydrides" patented technology

A method of producing a chemical hydride is described and which includes selecting a composition having chemical bonds and which is capable of forming a chemical hydride; providing a source of a hydrocarbon; and reacting the composition with the source of the hydrocarbon to generate a chemical hydride.

The invention discloses lithium borohydride and a preparation method thereof, and belongs to the technical field of hydrogen storage material preparation. The preparation method provided by the invention comprises the following steps: in a hydrogen atmosphere of 50bar, mixing lithium hydride, triethylamine borane and an organic solvent, and performing mechanical ball milling to obtain a mixture; and evaporating the solvent in the mixture, and carrying out heat treatment to obtain the lithium borohydride. Lithium borohydride is prepared through mechanical ball milling, the preparation process is high in safety coefficient, low in energy consumption, simple in process, mild in condition, adjustable in reaction process and easy to implement; the optimal yield is 80%, and the method is originally superior to other similar processes, has technical conditions for efficient mass production, and has a wide application prospect in hydrogen storage materials.

A sodium borate, aluminum powder and fluoride powder are mixed together in a hermetic vessel filled with hydrogen gas, and the mixture is reacted at not less than 410° C. and not more than 560° C. to produce sodium borohydride.

The invention relates to preparation and application of a metal hydride serving as a lithium ion battery negative electrode material. The lithium ion battery negative electrode material is obtained by mixing Ti3C2 and MgH2 serving as raw materials and then carrying out dehydrogenation-hydrogenation treatment. Compared with the prior art, the lithium ion negative electrode material provided by the invention is simple in preparation method, and the obtained product is high in purity, uniform in size distribution and good in electrochemical performance, and can be further applied to the fields of battery materials, supercapacitors and the like.

The present disclosure relates to hydrogen storage mediums comprising sodium borohydride, magnesium oxide, and magnesium which release hydrogen when contacted with a proton source. The present disclosure also relates to methods of producing hydrogen storage mediums.

The invention belongs to the technical field of hydrogen storage materials, and particularly relates to a metal borohydride composite material, a preparation method thereof and a hydrogen storage material. The preparation method comprises the following steps: activating the carbon-based carrier by adopting an alkaline substance; performing gas-phase fluorination treatment on the activated carbon-based carrier; the carbon fluoride-based carrier is mixed with a metal source, a boron source and a solvent, a solvothermal reaction is driven by hydrogen, metal borohydride is synthesized in situ on the surface of the carbon fluoride-based carrier, metal atoms in the generated metal borohydride react with F atoms in the carbon fluoride-based carrier to form a metal-F bridging phase, and meanwhile, the metal borohydride generates metal vacancies. The metal affinity of fluorine in the carbon fluoride-based carrier is utilized to induce nucleation loading of the metal borohydride in the synthesis process of the metal borohydride, and meanwhile, an interface chemical reaction is carried out to generate vacancies and bridging phases. Vacancies weaken B-H bonds, the hydrogen absorption and desorption heat / dynamics of the material are improved, and the bridging phase improves the structural stability and hydrogen absorption and desorption cycle performance of the material.

The invention discloses a method for preparing magnesium borohydride by a solution method, and relates to the technical field of hydrogen storage materials. The method comprises the following steps: dissolving MgCl2 in tetrahydrofuran to form a magnesium source solution, dissolving NaBH4 in isopropylamine to form a boron-hydrogen source solution, mixing the two solutions, and stirring to react; carrying out centrifugation and microfiltration membrane suction filtration separation on the reacted mixture to remove solid impurities so as to obtain a clarified filtrate; and carrying out vacuum desolventizing treatment on the filtrate to finally obtain solid magnesium borohydride. The method is simple in process flow, can be completed under mild conditions, and has the advantages of low raw material cost and high operation safety; the prepared magnesium borohydride product has excellent performance of lower initial hydrogen desorption temperature, and the temperature is only 115.8 DEG C. The method is especially suitable for large-scale industrial production.

A sodium borate, aluminum powder and fluoride powder are mixed together in a hermetic vessel filled with hydrogen gas, and the mixture is reacted at not less than 410°C and not more than 560°C to produce sodium borohydride.

The invention discloses a preparation method of magnesium borohydride based on solvothermal reaction, and relates to the technical field of hydrogen storage materials, and the preparation method specifically comprises the following steps: S1, carrying out ball milling pretreatment on magnesium hydride according to a certain ball-to-material ratio; s2, adding the pretreated magnesium hydride and triethylamine borane into a self-made hydrothermal reaction kettle, then adding a solvent, starting heating and stirring procedures, carrying out a reaction for a certain time, and carrying out centrifugal separation to obtain a solid product; and S3, transferring the solid product into a tubular furnace, and carrying out vacuum drying to obtain magnesium borohydride. The method provided by the invention has the advantages of simple process, low price, one-step reaction, high safety, high yield and high purity.

The invention provides a biomass carbon / CoF2 composite material as well as a preparation method and application thereof. The preparation method of the biomass carbon / CoF2 composite material comprises the following steps: calcining a carbon source to obtain biomass carbon; biomass carbon, fluoride salt, cobalt salt, urea and ethylene glycol are fully mixed and dispersed uniformly, and the biomass carbon / CoF2 composite material is obtained through solvothermal reaction, centrifugation, washing and drying. The preparation method is simple, and the obtained biomass carbon / CoF2 composite material is formed by loading spherical CoF2 on the surface of a biomass carbon material; the biomass carbon / CoF2 composite material is applied to the field of magnesium hydride-sodium borohydride solid hydrogen storage, biomass carbon and CoF2 can generate a synergistic effect, and excellent magnesium hydride-sodium borohydride solid hydrogen storage catalytic modification performance is shown.

The invention relates to the technical field of sodium borohydride preparation, in particular to a sodium borohydride preparation method based on concentration and crystallization treatment. Comprising the following steps: adding crude sodium borohydride and deionized water into a high-pressure kettle according to a mass ratio, stirring, and filtering to obtain extract liquor; pumping the extract liquor into a reverse osmosis system, and carrying out membrane concentration; the concentrated solution is transferred to a crystallization kettle, polyethylene glycol-4000 is added, gradient cooling is executed for crystallization, and in the second stage of gradient cooling, sodium borohydride seed crystals are added, and meanwhile ultrasonic waves are applied for auxiliary crystallization; pumping the crystallized slurry into a horizontal centrifugal machine, separating crystals, putting the obtained crystals into a double-cone rotary drying machine, and drying to obtain concentrated sodium borohydride crystals; a traditional evaporation process is replaced by reverse osmosis membrane low-temperature concentration, by-product sodium metaborate impurity pollution is eradicated, the source of the phenomenon that metal ions induce dendritic crystal growth is eliminated, high-purity sodium borohydride crystals can be obtained through single crystallization, and the product yield is increased.

The invention discloses high-purity lithium borohydride and a preparation method thereof, and belongs to the technical field of inorganic synthesis.The preparation method comprises the steps that firstly, surface coordination activation is conducted on micron-sized lithium hydride through amino silane, and the reaction activity of the micron-sized lithium hydride is remarkably improved; and then, in a uniform ionic liquid organic solvent composite medium, efficiently synthesizing lithium borohydride with a purified borane complex at a mild temperature. For key impurity chloride ions, trimethylchlorosilane is innovatively introduced to carry out targeted precipitation conversion, and effective removal is carried out before crystallization. And finally, directly separating out a high-purity product from a reaction system through a directional crystallization technology. According to the high-purity lithium borohydride and the preparation method thereof disclosed by the invention, high-efficiency preparation of high-purity and low-chloride-ion lithium borohydride under a mild condition is realized, a key reagent can be recycled, and the problems of high energy consumption and insufficient purity in a traditional method are perfectly solved.

The application discloses a kind of multilayer nanostructure metal hydride and preparation method thereof, the preparation method includes that transition metal ion salt and carbon material are added to polar solvent mixture, heating stirring and obtain solid powder, hydrogen hot reduction reaction is carried out to solid powder and obtains functionalized carbon material;Metal hydride raw material, functionalized carbon material are added to organic solvent, ultrasonic, and mixed and obtain mixed solution, the metal hydride raw material is alkyl metal Mg compound or alkyl metal Li compound and mixture of borane compound;Under hydrogen atmosphere, the mixed solution is carried out solvothermal reaction, then centrifugation, washing, filtration, drying and obtain multilayer nanostructure metal hydride.The preparation method prepared multilayer nanostructure metal hydride has higher hydrogen absorption and hydrogen storage capacity.

The application discloses a mechanical-chemical preparation method of potassium borohydride, and belongs to the technical field of potassium borohydride preparation. The method is characterized in that magnesium-based reducing agent, hydrogen supplementing agent and potassium borate hydrate are used to prepare potassium borohydride through a mechanical-chemical method under a protective atmosphere, and the prepared potassium borohydride is subjected to yield testing and purification under an air atmosphere. The method can realize solid-phase mechanical-chemical reaction under a vibration or low-energy planetary ball milling condition, breaks through the limitation that the reaction must be driven by high-energy ball milling equipment in the prior art, and can realize synthesis of potassium borohydride with a yield of more than 90% through low-energy planetary ball milling, so that the method has large-scale production application potential. In addition, the method has the advantages of simple process, convenient operation and low cost.

In a method of producing metal borohydride, M(BH4)n, from metal metaborate, M(BO2)n, in which M is a metal, such as a metallic metal, an alkali metal, an alkaline earth metal, a transition metal or a chemical compound behaving as a metal, and n is a valence value of the metal, metal borohydride is formed through a reaction of metal hydride, MHn, with trimethyl borate, B(OMe)3, and metal trimethyl borate is formed through a reaction of boric acid, H3BO3, with methanol, MeOH, under removal of water, H2O. An electrochemical cell is used for the conversion of metal metaborate and water, H2O, to boric acid, in the electrochemical cell. The electrochemical cell has an anodic half-cell and a cathodic half-cell separated by a cation exchange membrane, and a solvent and water is provided to both the anodic half-cell and the cathodic half-cell. Metal metaborate is provided to the anodic half-cell, where acid ions, H+, and electrons, e−, are generated at the anode from electrolysis of water, and H reacts with metal metaborate and water. The cation exchange membrane passes metal ions, Mn+, from the anodic half-cell to the cathodic half-cell, and metal hydroxide, M(OH)n, is formed in the cathodic half-cell.

This invention relates to the field of sodium borohydride preparation technology, specifically to a method for preparing sodium borohydride based on concentration and crystallization. The method includes: adding crude sodium borohydride and deionized water to a high-pressure reactor in a specific mass ratio, stirring, and filtering to obtain an extract; pumping the extract into a reverse osmosis system for membrane concentration; transferring the concentrate to a crystallization reactor, adding polyethylene glycol-4000, and performing gradient cooling for crystallization, wherein sodium borohydride seed crystals are added in the second stage of gradient cooling while ultrasound is applied to assist crystallization; pumping the crystallized slurry into a horizontal centrifuge to separate the crystals, and placing the obtained crystals in a double-cone rotary dryer for drying to obtain concentrated sodium borohydride crystals; replacing the traditional evaporation process with low-temperature concentration via reverse osmosis membranes eliminates the byproduct sodium metaborate impurity contamination, removes the root cause of metal ion-induced dendrite growth, and allows for the acquisition of high-purity sodium borohydride crystals in a single crystallization, thus improving product yield.

To produce potassium borohydride by a simple process.SOLUTION: A production method of potassium borohydride comprises a reaction process in which solid raw materials, including an alkali metal compound, fluoride, and at least one or more materials selected from aluminum compounds and aluminum, are mixed and heat-treated at a temperature greater than 560°C.SELECTED DRAWING: Figure 5

A method of regenerating sodium borohydride includes: pretreating reactants including sodium tetraborate hydrate (Na2B4O7·xH2O, 0<x≤10), a metal salt, and a reducing agent; and reacting the pretreated reactants by a ball-milling method, wherein the metal salt includes NaHCO2, KHCO2, LiHCO2, NaHCO3, Na2CO3, NaOH, KHCO3, K2CO3, LiHCO3, Li2CO3, Na2O2, NaH, or a combination thereof.

The application discloses a kind of core-shell nanostructure magnesium hydride-magnesium borohydride hydrolysis hydrogen production materials and preparation method thereof.A kind of core-shell nanostructure magnesium hydride-magnesium borohydride hydrolysis hydrogen production material preparation method, comprising the following steps: magnesium hydride is loaded into ball mill jar vacuum, then borane gas is filled in ball mill jar, ball milling treatment is carried out, and the core-shell nanostructure magnesium hydride-magnesium borohydride hydrolysis hydrogen production material is obtained.The application uses solvent-free gas-solid reaction, ball milling method, simple, low cost;This composite method not only avoids the direct use of expensive magnesium borohydride, but also overcomes the shortcomings of other composite systems, and even improves the theoretical hydrogen release capacity;The in-situ formed magnesium borohydride nanoshell plays a key role in improving the hydrolysis kinetics of magnesium hydride by releasing heat and forming a local magnesium ion and metaborate ion solution environment.

The invention relates to the field of solid hydrogen storage materials, in particular to a preparation method and application of oxalate modified metal hydride.The preparation method comprises the steps that metal oxalate and metal hydride serve as starting raw materials, and the metal oxalate and the metal hydride are mixed in an argon glove box according to a certain mass ratio; and adding a certain proportion of ball-milling beads into the mixed sample, and selecting different rotating speeds and ball-milling time to obtain the oxalate composite metal hydride. The preparation process is simple, large-scale and low in cost, the hydrogen absorption and desorption performance and the thermal / dynamic performance of the metal hydride are greatly improved, and the preparation method has a good application prospect. Taking vanadyl oxalate and magnesium hydride as examples, the prepared vanadyl oxalate composite magnesium hydride hydrogen storage system shows excellent hydrogen absorption and desorption characteristics, the mass hydrogen storage density reaches 6.35 wt%, the initial hydrogen desorption temperature is as low as 182.4 DEG C, the peak hydrogen desorption temperature is 220.4 DEG C, and the performance is remarkably improved compared with that of original magnesium hydride.

The invention discloses a room-temperature rapid preparation method of light metal hydroboron, and relates to the technical field of hydrogen storage materials. The method specifically comprises the following steps that S1, metal hydride is subjected to ball milling pretreatment according to a certain ball-to-material ratio; s2, mixing the pretreated metal hydride and dimethyl sulfide borane in a flask, then adding a solvent, and carrying out ultrasonic-assisted reaction; and S3, transferring the solid product into a tubular furnace, and carrying out vacuum drying to obtain the metal borohydride. The method has the advantages of simple process, low price, one-step reaction and high safety; the yield is obviously improved, the reaction conditions are obviously reduced, the production efficiency is greatly improved, and the method has an industrialization prospect.

Provided is a method for producing sodium borohydride. At a time when a sodium borate, an aluminum powder, and a fluoride powder are mixed and caused to react in a tightly sealed vessel filled with a hydrogen gas at a temperature of 560°C or lower, stirring using a stirrer is carried out in the tightly sealed vessel, and a stirring height ratio (X) expressed by a following formula (I) is 75% or more, in which (a) is a minimum clearance between the stirrer and the lowest part of the tightly sealed vessel in a gravity direction, and (b) is a raw material charged height when a raw material is charged into the tightly sealed vessel: X=b−a / b×100

To provide a solid electrolyte for an electrochemical device with high ionic conductivity.SOLUTION: An ultra-high closo-borate concentration solid state electrolyte is provided that is a combined salt of an alkali metal or alkaline earth metal closo-borate and a conductivity-increasing SISE. The combined salts allow significantly higher conductivity in the solid state than the contained alkali metal or alkaline earth metal closo-borate. The combined salts can be prepared by mechanical combination or combination in solution. This salt can be used in a solid state electrochemical device.SELECTED DRAWING: Figure 1

The invention relates to the field of magnesium hydride production, in particular to a continuous magnesium hydride production system and method. Through optimized process design, a tubular main reaction kettle controls constant temperature and pressure, a double-helix mechanism is arranged in the tubular main reaction kettle to stir and push powder to move directionally, hydrogen and magnesium powder mixed with a catalyst are injected from a top decompression chamber at the inlet end of the reaction kettle, and synthesized magnesium hydride powder is discharged from an outlet at the tail end of the reaction kettle and is output. According to the system for continuously producing magnesium hydride, solid magnesium hydride can be continuously and stably synthesized, the hydrogen content of magnesium hydride can reach 7.6 wt.% at most, compared with a magnesium vapor-hydrogen reaction, the magnesium hydride production method provided by the invention is lower in reaction temperature and controllable in pressure, the conversion efficiency can reach 99.5% at most, and the production cost is low. And industrial large-scale synthesis of magnesium hydride is realized.

Methods of synthesizing orthorhombic-structure closo-hydroborate include mixing orthorhombic-structure closo-hydroborate precursors with low shear mixing to form a precursor mixture, placing the precursor mixture in a reaction vessel with an inert environment, heating the precursor mixture to a reaction temperature for the precursor mixture, and quenching the reaction vessel from the reaction temperature. The resulting orthorhombic-structure closo-hydroborate has ionic conductive stability at 25°C. Cathode composites that include the orthorhombic- structure closo-hydroborate therein are disclosed as well as solid-state batteries or all-solid-state batteries that have the orthorhombic-structure closo-hydroborate made according to the methods as a solid electrolyte and / or as part of the cathode composite.

Provided is a method for producing sodium borohydride. When sodium borates, aluminum powder, and fluoride powder are mixed in an airtight container filled with hydrogen gas and reacted at 560ºC or less, stirring is performed using a stirrer in the airtight container, a stirring height ratio (X) expressed by equation (I) based on the minimum gap (a) between the stirrer and a bottommost section of the airtight container in the gravity direction, and a raw material insertion height (b) at which raw materials are inserted into the airtight container is 75% or greater.　(I): X = [(b-a) / b] × 100

Provided is a method for producing sodium borohydride. An aluminum powder and a fluoride powder are mixed, and a pretreatment thereof is carried out at 100°C or higher and 330°C or lower; and after the pretreatment, a fluoride powder and a sodium borate are added and mixed, and the resulting mixture is charged into a tightly sealed vessel; and then after a hydrogen gas is introduced thereto, a heat treatment is carried out by heating the tightly sealed vessel at 490°C or higher and 560°C or lower.

A method for producing a tetrahydroborate includes a hydrogenating step (step S14) of exposing a borate to a hydrogen plasma while grinding the borate.