25 results about "Lithium borohydride" patented technology

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.

The application discloses a preparation method of an important intermediate of a pyrimidine-4(3H)-ketone heterocyclic compound shown in formula h, namely a preparation method of (3S,4S)-tert-butyl 4-((R)-1,1-dimethylethylsulfinamido)-3-methyl-2-oxa-8-azaspiro[4.5]decane-8-carboxylate, which is synthesized through a series of reactions such as substitution, reduction, nucleophilic addition, reduction and deprotection, ring closure, oxidation and reductive amination and the like by taking L-methyl lactate as a raw material. In the application, red aluminum is used to replace lithium borohydride and tetrabutylammonium fluoride in the prior art, so that the problems of the risk caused by the use of lithium borohydride and the difficulty in post-treatment caused by the use of tetrabutylammonium fluoride in the prior art are overcome, the reaction steps are shortened, and the post-treatment operation is simplified.

The invention provides a preparation method of buracametacin hydrochloride and an intermediate compound shown as a formula II thereof. The preparation method of the compound as shown in the formula II comprises the following steps: in the presence of a reducing agent, a compound as shown in the formula I is subjected to a reduction reaction to generate the compound as shown in the formula II. The reducing agent is selected from sodium borohydride and / or lithium borohydride, lewis acid also exists in the reaction system, and the lewis acid is also selected from zinc bromide, zinc chloride, boron trifluoride, aluminum chloride, ferric chloride or a combination thereof. The preparation method disclosed by the invention is low in reducing agent price, mild in reaction, relatively high in product yield and purity, and suitable for industrial large-scale production. # imgabs0 #

A fiber-reinforced lithium borohydride-based all-solid-state electrolyte for suppressing dendrite formation, its preparation method, and its application are disclosed. The method employs a reverse micelle precipitation method to prepare a precursor solution by dissolving lithium borohydride and lithium iodide in an ether solvent solution. Aluminum oxalate and vapor-grown carbon fibers are then added, followed by dropwise addition to an isopentane solution containing a surfactant. After reverse micelles form, the solution is allowed to settle and react completely, and the solvent is thoroughly removed. The product from the settled reaction is dried and then subjected to partial hydrogen release treatment. The partially hydrogen-released product is dispersed in a benzene solution containing polymethyl methacrylate, freeze-dried, and then melt-reacted in situ in a universal mold. This process is simple and highly controllable, significantly improving the mechanical stability and dendrite resistance of the lithium borohydride-based all-solid-state electrolyte, and enabling long lifespan of all-solid-state lithium batteries under fast-charging conditions, thus facilitating commercial applications.

The application discloses a preparation method of 3-methyl mercaptopropionate, and belongs to the technical field of pesticide intermediate preparation. The application takes di-tert-butyl disulfide and methyl acrylate as raw materials, generates 3-tert-butyl mercaptopropionate under the action of lithium borohydride, then generates 3-methyl mercaptopropionate and 5-tert-butyl-1,3-dimethoxybenzene under the action of tri (pentafluorophenyl) boron while isobutene is removed and isobutene reacts with m-dimethoxybenzene, and 3-methyl mercaptopropionate is obtained after rectification. In the method, the route is good in operability, low in three wastes and cost, and provides a reference for the preparation of the compound.

The application discloses a preparation method of a metal-catalyzed lithium borohydride composite hydrogen storage material, which comprises the following steps: mixing raw materials including lithium borohydride and a ferrocene salt, and performing ball milling to obtain the metal-catalyzed lithium borohydride composite hydrogen storage material; the ferrocene salt is selected from one or more of nickelocene, chromocene and manganocene. The preparation method disclosed by the application is simple and controllable, is suitable for large-scale industrial production, and more importantly, the prepared composite hydrogen storage material has the advantages of low hydrogen absorption and desorption temperature, good hydrogen absorption and desorption kinetics, high cycle stability and the like without reducing the high theoretical capacity of lithium borohydride.

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 present invention discloses a 1,4,7,10-tetraazadodecane derivative, a preparation method, and its use in the synthesis of gadolinium complexes, belonging to the field of organic synthesis. The method uses compound 1 as a substrate and reacts it with lithium borohydride to produce compound 2. By utilizing a specific selective reduction reaction route and specific intermediates, this method eliminates the need for overprotection / deprotection steps, reduces reaction steps, and improves preparation efficiency.

The invention belongs to the field of hydrogen storage materials, and provides a hydride hydrogen storage material and a preparation method thereof. According to the preparation method, a block material is prepared through discharge plasma sintering forming by adopting a multi-level collaborative design of a reactive composite hydride phase formed by magnesium hydride and lithium borohydride, an ordered mesoporous carbon and hexagonal boron nitride composite carrier structure, an atomic layer deposition oxide coating layer, a niobium pentoxide and titanium hydride catalyst and a heat-conducting outer coating; the comprehensive performance that the reversible hydrogen storage mass fraction is 5.5-7.0 wt%, the capacity retention ratio after 50 times of circulation is larger than or equal to 90%, and the temperature gradient in the block is smaller than or equal to 10 DEG C / cm is achieved, and the multiple contradictions between the high hydrogen storage capacity and the block mechanical strength, between the oxide coating layer stability and the hydrogen diffusion rate and between the heat conduction uniformity and the structural integrity are solved. The method has a wide application value in a solid hydrogen storage system.

This invention relates to the field of lithium-ion battery technology, and discloses a solid electrolyte for lithium-ion batteries, its preparation method, and its application. The solid electrolyte is lithium borohydride modified with MX2 doping; in MX2, M is one or more of Fe, Co, and Ni, and X is Cl and / or Br; MX2 includes at least CoBr2. This invention, by using specific dopants to modify lithium borohydride, can significantly improve the ionic conductivity of the lithium borohydride-based solid electrolyte.

This invention discloses a high-purity lithium borohydride and its preparation method, belonging to the field of inorganic synthesis technology. The method includes: surface activation of lithium hydride with an aminosilane activator, reaction with a borane-tetrahydrofuran complex at 30-80℃, followed by impurity removal through a combination of lithium bromide and alkaline alumina, negative pressure decomposition, crystallization, washing, and drying to obtain high-purity lithium borohydride. The obtained product is a white crystalline powder with a purity ≥99.90%, chloride ions ≤15ppm, free alkali ≤50ppm, and metallic impurity Na. + / K + / Al 3+ ≤5 / 5 / 1ppm, particle size D50=5-15μm, ionic conductivity at 25℃≥3.0×10 ‑5 S / cm, moisture absorption rate ≤0.1% / 24h. This invention has wide raw material adaptability, mild process, and high product purity, and is suitable for solid electrolytes, pharmaceutical synthesis and other fields.

The invention provides an alkyl uracil derivative and a preparation method and application thereof, and relates to the technical field of organic synthesis.The preparation method comprises the following steps that a uracil analogue and olefin are subjected to a hydrogenation alkylation reaction under the action of an iron catalyst and a hydrogen source, and the alkyl uracil derivative is obtained; the iron catalyst comprises at least one of iron nitrate nonahydrate, ferrous nitrate, ferric chloride, ferrous chloride, ferric sulfate and ferric oxalate; the hydrogen source comprises at least one of sodium borohydride, lithium borohydride, lithium aluminum hydride, triphenyl silicon, triethyl silicon and borane. According to the present invention, the olefin is adopted as the alkyl raw material, the pre-functionalization is not required, the specific catalyst and the specific hydrogen source are combined, the hydrogenation alkylation reaction of the olefin and the uracil analogue is successfully achieved, and the technical effect of constructing a series of alkyl uracil derivatives is achieved. According to the invention, the reaction can be carried out at room temperature without light and heat conditions, the reaction time is short, and the functional group tolerance is better.

Alkali-containing apparatuses and methods for making alkali-containing apparatuses are provided. In one aspect, an anode electrode structure is provided. The anode electrode structure includes a current collector comprising copper and / or stainless steel, a lithium metal film formed over the current collector, and a protective film stack formed on the lithium metal film. The protective film stack includes a metal film formed over the lithium metal film and a lithium salt film formed on the metal film. The metal film is selected from a bismuth film, a tin film, a silver film or a combination thereof. And a lithium salt film formed on the metal film, the lithium salt film being selected from the group consisting of lithium sulfide, lithium oxide, lithium halide, lithium chalcogenide, lithium borohydride, or a combination thereof.

The invention relates to a calcium iodide-based organic electrolyte, a secondary battery and a preparation method of the calcium iodide-based organic electrolyte, the electrolyte is composed of calcium salt, an organic solvent and an additive, the calcium salt is calcium iodide or a combination of calcium iodide and other calcium salt, the organic solvent is one or a combination of more of ether organic solvent, sulfone organic solvent, ester organic solvent, amide organic solvent, ionic liquid organic solvent and amine organic solvent; the additive is selected from one or more of lithium borohydride, sodium borohydride, potassium borohydride, zinc borohydride, magnesium borohydride, lithium iodide, sodium iodide, magnesium iodide, potassium iodide, tetraethyl ammonium borohydride, tetramethyl ammonium borohydride, benzyltriethyl ammonium borohydride and tetra-n-butylammonium borohydride. Compared with the prior art, the fluoride-free, thermodynamically stable and low-passivation-effect calcium iodide-based electrolyte provided by the invention can improve the interface property of a calcium metal negative electrode-electrolyte and increase the stability of the electrolyte, so that the cycle life of a calcium metal battery is prolonged, and the stability of the calcium metal battery is improved.

Method for the production of a core-shell-shell FeCo / SiO2 / MnBi nanoparticle comprising: a) Joint reduction of an iron ion and a cobalt ion from a common solution; and joint precipitation of an FeCo alloy nanoparticle; Isolating the FeCo nanoparticle from the reduction mixture; b) Forming a silicon dioxide coating on the FeCo nanoparticle to obtain a core-shell nanoparticle, wherein the nanoparticles are treated with tetraethyl orthosilicate in a water-ethanol mixture using triethylamine as a basic catalyst; and c) Forming a MnBi alloy nanocoating on the core-jacket nanoparticle by reducing Bi ions through a Mn-lithium borohydride complex by precipitation from a solution as a MnBi alloy onto the silicon dioxide jacket; the formation of the MnBi alloy nanocoating c) is carried out in a magnetic field of 0.005 T (50 Gauss) to 0.08 T (800 Gauss).

Provided are a composite electrolyte with a wide working voltage range for an all-solid-state lithium-ion battery, and a preparation method and use thereof. The composite electrolyte includes a lithium borohydride-based solid-state electrolyte and a polymer coating layer coated on a surface of the lithium borohydride-based solid-state electrolyte. A voltage window of the composite electrolyte with the wide working voltage range is not less than 6 V and up to 10 V. The lithium borohydride-based solid-state electrolyte comprises lithium borohydride, alumina, and lithium iodide. The polymer coating layer is poly(methyl methacrylate). A mass percentage of the lithium borohydride-based solid-state electrolyte in the composite electrolyte with the wide working voltage range is in a range of 70 wt. % to 99 wt. %; and a mass percentage of the polymer coating layer in the composite electrolyte with the wide working voltage range is in a range of 1 wt. % to 30 wt. %.

The invention discloses a synthesis method of 1, 1, 3, 3-tetramethyl butyl peroxypivalate, which comprises the following steps: sequentially adding soft water, isoparaffin and TOHP into a reaction kettle, cooling, dropwise adding inorganic base, keeping for 15 minutes, and cooling to 10 DEG C; after alkalization is finished, pivaloyl chloride is dropwise added, the rotating speed is increased, the temperature is kept for 120 min, water is added after the temperature is kept for 15 min, stirring is stopped after the temperature is kept for 15 min, standing is conducted for 30 min, a separating funnel is used for material separation, and a crude product is obtained; adding glacial acetic acid into the crude product, then adding triisobutyl lithium borohydride, separating by using a separating funnel, then adding a sodium hydroxide solution and soft water, and finally separating to obtain a fine sample; and drying the high-quality sample to obtain the 1, 1, 3, 3-tetramethyl butyl peroxypivalate. The 1, 1, 3, 3-tetramethyl butyl peroxypivalate provided by the invention is simple, safe and environment-friendly to synthesize, and the produced refined product is high in purity and low in water content.

The invention discloses a method for improving hydrogen desorption performance of lithium borohydride, and belongs to the technical field of hydrogen energy. The method comprises the following steps: firstly, carrying out corrosion treatment on Al85Ni10Co5 alloy powder by adopting a sodium hydroxide solution; then carrying out oxidation treatment on the corrosion product in an air atmosphere; putting the obtained oxidation product and potassium fluotitanate into hot water according to a certain mass ratio, stirring, and freeze-drying; and finally, pouring a certain mass of the dried product into anhydrous tetrahydrofuran containing lithium borohydride, stirring, and carrying out vacuumizing treatment, so that the hydrogen desorption performance of lithium borohydride can be improved. The method has the advantages that the method for improving the hydrogen desorption performance of the lithium borohydride is wide in raw material source, low in price, simple in process, safe and reliable; the lithium borohydride modified by the technology provided by the invention has low hydrogen desorption temperature and high hydrogen desorption amount.

The application discloses a lithium borohydride-ammonium halide composite solid electrolyte and a preparation method and application thereof, and belongs to the technical field of solid-state battery electrolyte preparation. The application comprises the following steps: mixing lithium borohydride and ammonium halide to obtain a mixture; under a protective atmosphere, the mixture is heated to 90-180 DEG C and is subjected to heat preservation treatment; and under vacuum conditions, the heat preservation treated material is subjected to heat treatment, thereby obtaining the lithium borohydride-ammonium halide composite solid electrolyte. The application induces lithium borohydride crystal phase transition through ammonium halide decomposition, and effectively removes gaseous by-products through vacuum heat treatment, thereby significantly improving the ionic conductivity and electrochemical stability of the electrolyte, and the preparation process is simple and suitable for large-scale production.

The invention discloses a preparation method of (S)-2-aminopropanol. The preparation method comprises the following steps: S1, inputting L-2-aminopropionic acid and an organic solvent tetrahydrofuran into a reaction device; s2, dropwise adding the lithium borohydride tetrahydrofuran solution into the reaction device through a dropwise adding device; s3, inputting an ammonium chloride aqueous solution into the reaction device for quenching excessive lithium borohydride which is not completely reacted; s4, inputting the lower-layer water phase in the reaction device into an extraction device, and inputting an extraction solvent into the extraction device to extract the lower-layer water phase in the extraction device; s5, inputting the organic materials in the reaction device and the extraction device into a first distillation device for distillation; and S6, inputting the residual material distilled by the first distillation device into a second distillation device for rectification to obtain (S)-2-aminopropanol. The preparation time of the product is shortened, and the yield of the prepared product is improved.

The application discloses a method and a reaction device for preparing nanofibrillar lithium borohydride. The reaction device comprises a material tank with a valve and placed in a freeze-drying chamber, a condensing machine for adjusting the temperature of the material in the material tank to freeze-dry and normal-temperature dry the material, a vacuum pump connected with one end of the freeze-drying chamber for vacuumizing to form negative pressure in the freeze-drying chamber, and an inert gas supply device connected with the freeze-drying chamber for providing inert gas to the freeze-drying chamber. The method comprises the following steps: mixing a mixed solution containing lithium borohydride and a polar organic solvent with a refrigerant to obtain a solution, transferring the solution to a reaction kettle, filling hydrogen into the reaction kettle, freezing to condense the solution in the reaction kettle, and sequentially performing vacuumizing, low-temperature freeze-drying and vacuumizing normal-temperature drying on the material in the reaction kettle in a water-free and oxygen-free environment to remove the polar organic solvent and the refrigerant, so as to obtain nanofibrillar lithium borohydride.

This invention relates to the field of lithium-ion battery technology, and discloses a multi-component composite lithium borohydride-based solid electrolyte, its preparation method, and its applications. The multi-component composite lithium borohydride-based solid electrolyte includes a core layer and a shell layer covering the core layer; the core layer comprises lithium borohydride modified with nickel iodide doping; the shell layer comprises zirconium dioxide. In the multi-component composite lithium borohydride-based solid electrolyte of this invention, by doping LiBH4 with NiI2 and providing a shell layer containing ZrO2, the bidirectional promoting effect between NiI2 and ZrO2 can be utilized to impart higher ionic conductivity to the solid electrolyte.

The invention relates to a method for improving hydrogen desorption performance of lithium borohydride by co-doping fluoride and MXene. The provided composite hydrogen storage material comprises the following raw material components in parts by weight: 50-80 wt% of LiBH4, 10-25 wt% of Ti3C2 MXene and 10-25 wt% of metal fluoride. Compared with the prior art, the metal fluoride and the Ti3C2 MXene material are introduced into the LiBH4 hydrogen storage material through a simple and efficient ball milling process, the hydrogen desorption temperature of LiBH4 is effectively reduced through the synergistic effect of the metal fluoride and the Ti3C2 MXene material, meanwhile, the hydrogen desorption capacity of LiBH4 is improved, the prepared compound can achieve hydrogen desorption at about 78.70 DEG C, the peak hydrogen desorption temperature of the compound is about 344.25 DEG C, and the hydrogen desorption efficiency is greatly improved. And finally, 11.46 wt% of hydrogen and the like are released at the temperature of 400 DEG C.

This invention discloses a method for regenerating lithium borohydride using aluminum-based materials. The method involves simultaneously adding rare-earth-aluminum intermetallic compounds and lithium oxide, followed by solid-phase ball milling of aluminum and lithium metaborate dihydrate in a ball mill jar under non-oxidizing atmosphere or vacuum conditions to regenerate lithium borohydride. The addition of rare-earth-aluminum intermetallic compounds and lithium oxide additives improves ball milling efficiency, removes the aluminum oxide passivation layer, improves positive and negative hydrogen conversion, promotes lithium borohydride formation, and increases the yield of lithium borohydride. The rare-earth-aluminum intermetallic compound additives include inexpensive Al2Ce, Al3Ce, and Al... 11 One or more of Ce3, Al2La, and Al3La. This invention has the advantages of simple process, low cost, and easy industrialization.

The invention relates to the technical field of silicon-based negative electrode plates, in particular to a silicon-based negative electrode plate capable of stabilizing an interface, a preparation method of the silicon-based negative electrode plate and an all-solid-state lithium ion battery. The invention provides a preparation method of a silicon-based negative electrode plate capable of stabilizing an interface, which comprises the following steps: dripping a lithium borohydride solution on the surface of the silicon-based negative electrode plate, and drying to obtain the silicon-based negative electrode plate capable of stabilizing the interface. According to the preparation method of the silicon-based negative electrode plate capable of stabilizing the interface, the lithium borohydride solution is dripped on the silicon-based negative electrode plate, and the high-stability lithium borohydride interface layer formed on the surface of the silicon-based negative electrode plate can reduce the contact area between the silicon-based negative electrode plate and the sulfide solid electrolyte; insulation products generated by side reaction between the two are effectively reduced, and rapid increase of interface impedance and continuous consumption of active substances are avoided.