95 results about "Borohydride" patented technology

The invention discloses a catalytic system for preparing amine compounds through nitro reduction and application of the catalytic system. The catalytic system comprises an alkaline aqueous solution, a reducing agent and a catalyst, the alkaline aqueous solution is an alkali metal hydroxide aqueous solution; the reducing agent is alkali metal hydroboron and / or alkaline earth metal hydroboron; the catalyst is copper salt lewis acid and / or other lewis acid; the other Lewis acid is selected from one or a combination of more of cobalt salt, ferric salt, zinc salt, manganese salt and palladium salt. When the catalytic system is used for reducing the aromatic nitro-compound, the using amount of a reducing agent is small, meanwhile, the using amount of an organic solvent is reduced, the reaction yield is high, the reaction is milder, and amplified production of the process is facilitated.

The invention relates to a method for preparing norambrox ether from sclareolide. The method comprises the following steps: 1) preparing a red aluminum toluene solution; 2) dissolving sclareolide with toluene to obtain a sclareolide toluene solution, adding the sclareolide toluene solution into the red aluminum toluene solution for complete reaction, and quenching with a NaCl solution to obtain a reactant containing sclarediol; 3) carrying out oil-water separation on the reactant to obtain a primary organic phase and a water phase, so as to obtain an organic phase containing sclarediol; 4) carrying out a dehydration reaction on the organic phase containing sclarediol by using a molecular sieve, and after the reaction is completed, separating out an organic phase containing norambrox ether; 5, the organic phase containing the norambergyl ether is subjected to distillation concentration and crystallization separation, and a norambergyl ether product is obtained.According to the method, sclareolide is reduced through the red aluminum, and compared with lithium aluminum hydride, hydroboron and red aluminum, the red aluminum has the advantages of being good in stability, beneficial to industrialization, low in reaction temperature and safe.

The application discloses a catalyst for isocyanate borohydration reaction and a preparation and application method thereof. When the catalyst is used for catalyzing the borohydration reaction of isocyanate and borane to synthesize borate, the catalyst has high catalytic activity, mild reaction conditions (the reaction can be carried out at room temperature), short reaction time, high product yield (≥99%), and the reaction is simple, controllable, and simple in post-treatment.

The subject of the invention is N-substituted derivatives of l-(l-phenyl-3-aryl)-lH-pyrazol-4-yl)methanamine with the general formula 1, where ¥ represents CH or N, R1 represents hydrogen, R2 represents no substituent, R3 represents hydrogen, while R4 represents N-propylbenzamide, benzo[b]furan, dihydrobenzo [b] furan, methylenedioxybenzene, ethyl benzoate, or propyl benzoate, substituted accordingly, their method of production and application, and the method of obtaining and application of N-substituted derivatives of l-(l-phenyl-3-aryl)-IH-pyrazol-4-yl)methanamine with the general formula 1, where Y represents C, CH, or N, R1 represents hydrogen or a methyl group, R2 represents a methyl group or no substituent, R3 represents hydrogen or a methyl group, while R4 represents dimethylpyrazole, methylpyrazole, dimethylimidazo[l,2-a]pyrimidine, or isopropoxybenzene, substituted accordingly. The compounds that are the subject of the invention are obtained through reductive amination using borohydride derivatives as the reducing agent, advantageously sodium triacetoxyborohydride, in the amount of 1.4-2.0 eq, amine in the amount of 1.0-1.1 eq, advantageously in slight excess, base, advantageously triethylamine in the amount of 1.0-1.1 eq (in the case of using amine in the form of hydrochloride), and the starting aldehyde. The reaction is conducted in a nonpolar solvent environment, advantageously dichloroethane at a concentration of about 0.1 M. The crude product is purified by column chromatography on silica gel using a methanol in dichloromethane mixture as the eluent, in concentration ranges from 2% to 5%. In order to obtain a solid form and improve the physicochemical parameters, the free bases are converted into hydrochloride form, and then crystallized from a polar solvent, advantageously ethanol or propanol.

A full continuous-flow preparation method of (+)-biotin, including: subjecting a cyclic anhydride and a chiral biphenyl propylene glycol to asymmetric ring-opening reaction to produce a first intermediate, which undergoes selective reduction with a borohydride and cyclization with an inorganic mineral acid to produce (3aS, 6aR)-lactone; subjecting the (3aS, 6aR)-lactone and a sulfenylating reagent to sulfenylation to produce (3aS, 6aR)-thiolactone, which undergoes Fukuyama coupling with a zinc reagent in the presence of a palladium catalyst and elimination reaction in the presence of an inorganic mineral acid to produce an alkenyl valerate compound; subjecting the alkenyl valerate compound to reduction in the presence of a Pd / C catalyst to produce a valerate ester, which undergoes hydrolysis to produce a valeric acid salt; and subjecting the valeric acid salt to debenzylation in the presence of an inorganic mineral acid to produce the target product (+)-biotin.

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 of the metal borohydride composite material comprises the following steps: preparing the boron-doped carbon-based carrier; the boron-doped carbon-based carrier is mixed with a metal source, a first boron source and a first solvent, hydrogen is added for a thermal reaction, metal borohydride is generated on the surface of the boron-doped carbon-based carrier in situ, and the metal borohydride composite material is obtained. According to the method, a boron-doped carbon-based carrier is prepared, boron and carbon in the boron-doped carbon-based carrier are inert elements, a chemically inert electron-deficient carrier is constructed, and metal cations in metal borohydride are induced to generate charge transfer to the carrier in the in-situ preparation process of the metal borohydride on the surface of the boron-doped carbon-based carrier. Molecular internal electron interaction of metal cations and borohydride anions is weakened, so that the thermodynamic stability of the metal borohydride is reduced.

The invention discloses a method for preparing azithromycin by using a microchannel reactor. The method uses erythromycin as a starting material and prepares azithromycin through oximation, rearrangement, reduction and methylation reactions. During the oximation reaction, the contact time of the feed liquid in the microchannel reactor is very short, which greatly reduces the safety risk of the oximation reaction. The reduction reaction is carried out in the microchannel reactor, and neither explosive sodium (potassium) borohydride nor a high-pressure reactor is used, which reduces the safety risk. A tray layer of palladium carbon is laid on the reaction bed to achieve the hydrogenation target, while greatly improving the utilization efficiency of palladium carbon. In the rearrangement reaction, a milder leaving group, sodium 2-naphthalenesulfonate, is used to replace the existing leaving group. Water is used as a solvent and the reaction is carried out at room temperature. The method is green, safe, and has a high yield, and is suitable for industrial production.

The invention discloses a method for recovering polycarbonate plastic to obtain an amine high-temperature antioxidant, and belongs to the technical field of plastic recovery. Aromatic amine is used as a nitrogen source, hydroboron and formate are used as in-situ hydrogen donors, and in an inert atmosphere and a heating environment, under the synergistic catalysis of a catalyst and a molecular sieve, the amine high-temperature antioxidant is prepared from polycarbonate based on a one-step method. The reaction path is simple, the selectivity is high, the amine high-temperature antioxidant taking diphenylamine and alkyl diphenylamine as main components can be directly obtained without multi-stage separation and intermediate preparation, and the requirements of simple process flow, low energy consumption and the like are met. The invention provides a high-valued way for polycarbonate recovery, also provides a large-scale raw material source for the field of high-temperature-resistant antioxidants for lubricating oil / fuel / rubber and high polymer materials, and has a wide application prospect.

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 particularly relates to 4 '-thiosugar and a preparation method thereof. The preparation method comprises the following steps: taking D-ribose as a raw material, firstly carrying out methylation protection on C1-site hydroxyl, and then carrying out benzylation protection on other hydroxyl; the preparation method comprises the following steps: firstly, carrying out hydrolysis on a glucosidic bond at a C1 site, carrying out reduction through hydroboron to obtain open-loop ribitol (formula V), carrying out sulfonic acid esterification and bromination substitution on hydroxyl of the ribitol, forming a sulfur bridge bond by taking sodium sulfide as a nucleophilic reagent to obtain benzyl-protected thiosugar, oxidizing a thioether bond into sulfoxide, rearranging to obtain acetoxy thioether, and carrying out debenzylation reaction and hydroxybenzoylation reaction to obtain the high-purity acetoxy thioether. According to the present invention, the multi-step intermediate reaction only needs simple purification, the key intermediate can be obtained through recrystallization, the method is simple, the yield is high, the amplification production is convenient, and the obtained 4 '-thiosugar as the basic sugar can participate in the reaction with a variety of basic groups to form the sulfur-containing nucleoside so as to provide the good foundation for the subsequent drug development or activity screening.

The invention relates to a process for preparing a star copolymer of 1,3-diene and ethylene, the copolymer containing more than 50 mole percent ethylene units. The process comprises the polymerization of a monomeric mixture of 1,3-diene and ethylene in the presence of a catalytic system based on at least one neodymocene borohydride metallocene and an organomagnesium cocatalyst, followed by the reaction of tin tetrachloride with the polymerization reaction product, and then a chain-terminating reaction. The invention also relates to a star copolymer obtainable by the process according to the invention.

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.

The present invention belongs to the field of degradation of aromatic hydrocarbon organic matter in saline-alkali environments, and relates to a preparation method and application of sulfide nano-zero-valent iron-doped biochar. The method includes the selection of a carbon-based material modifier, the preparation of a surface chemically modified carbon-based material, and the degradation process of a target pollutant. The preparation steps of the modified carbon-based material are as follows: first, (1) preparing biochar by carbonizing lotus leaf stems and facility agricultural crop straw at high temperature; (2) preparing sulfide nano-zero-valent iron particles by a modified borohydride reduction method under inert atmosphere conditions; and (3) preparing sulfide nano-zero-valent iron-doped biochar particles. The sulfide nano-zero-valent iron-doped biochar particles are subjected to solid-liquid separation, vacuum drying, and high-temperature calcination under a reducing atmosphere to obtain metal-modified biochar nanoparticles. The above-mentioned material is used to activate persulfate to degrade aromatic hydrocarbon organic matter, degrading the target PAHs to generate non-condensed ring organic small molecule compounds. The operation is simple, the strengthening effect is significant, the degradation effect is obvious, and the material is salt-alkali resistant.

A method for removing halogen ions adsorbed on the surface of a metal nanocrystal is characterized in that the halogen ions adsorbed on the surface of the metal are removed through strong adsorption of [BH4] <-> and H <-> released by hydroboron and the metal, and surface modification and effective dispersion of the metal nanocrystal are realized by introducing proper molecules (or groups) to be adsorbed on the surface. Therefore, removal of halogen ions on the metal surface, adsorption of specific molecules (or groups) and dispersion of metal nanocrystals are realized. According to the method, halogen ions on the metal surface can be removed and replaced, and then characteristic modification and effective dispersion on the surface of the metal nanocrystal are achieved.

The application discloses a borohydride / graphyne composite hydrogen storage material, a preparation method thereof and application of the borohydride / graphyne composite hydrogen storage material in the field of hydrogen storage. The borohydride / graphyne composite hydrogen storage material comprises a graphyne carrier and borohydride loaded on the carrier. The preparation method comprises the following steps: adding the graphyne into a homogeneous solution of the borohydride and performing ultrasonic dispersion, then removing part of the solvent in a state of keeping the graphyne suspended to form a paste, and finally removing the solvent by vacuumizing to obtain the borohydride / graphyne composite hydrogen storage material. The graphyne is used as the carrier, so that the stability of the borohydride in the hydrogen absorption and release cycle can be ensured. The borohydride / graphyne composite hydrogen storage material has low hydrogen release initial and peak temperatures, good hydrogen absorption and release kinetic performance and high hydrogen absorption and release reversibility.

The application belongs to the technical field of luminescent materials, and particularly relates to a cerium ion doped borohydride-based cesium halide anti-perovskite and a preparation method and application thereof. The cerium ion doped borohydride-based cesium halide anti-perovskite provided by the application has a structure of Cs3Cl[B 12 H 12 ]:Ce 3+ . The cerium ion doped borohydride-based cesium halide anti-perovskite is non-toxic, stable and has high luminous efficiency.

The present specification relates to a flying body provided with a fuel cell for generating hydrogen using sodium borohydride, which is one kind of tetrahydroborate, and generating power using the hydrogen, and provides a technique for reducing the weight of a power generation device. A flying object disclosed in the present specification is provided with: an SBH container for storing sodium borohydride (SBH) that generates hydrogen when mixed with water; a water container for storing water mixed with the SBH; and a fuel cell stack that generates power using the hydrogen generated by the SBH. The outer wall of the flying body is also used as a part of the SBH container and a part of the water container. The water container is arranged above the SBH container, a bottom plate of the water container also serves as a top plate of the SBH container, and a valve is arranged on the bottom plate. In the technology disclosed in the present specification, the outer wall of the flying body also serves as part of an SBH container and part of a water container. With this configuration, a part of the power generation device can be reduced in weight.

The invention relates to a catalytic system based on at least one neodymocene borohydride, a co-catalyst which is a dialkylmagnesium compound of formula RB-Mg-RL, in which RB is a secondary alkyl of formula R2CH and RL is a primary alkyl of formula RCH2, the Rs, identical or different, being alkyls. The catalytic system addresses the objective of improved macrostructure control in a polymerization process of ethylene or a monomer mixture containing ethylene and a 1,3-diene.

The invention provides a gold shell coated long-afterglow nano material for imaging photo-thermal and preparation and application of the gold shell coated long-afterglow nano material. The nano material comprises a Cr-doped zinc-gallium-germanium oxide long afterglow nano core, a mesoporous silica shell layer coated on the surface of the nano core and a gold shell layer coated on the outer surface of the mesoporous silica shell layer. The preparation method comprises the following steps: performing hydrothermal reaction and calcining to prepare a long afterglow nano core; the preparation method comprises the following steps: carrying out hydrolytic polycondensation on tetraethoxysilane (TEOS) under a cetyl trimethyl ammonium bromide (CTAB) template and an alkaline condition to form a mesoporous silica shell layer, removing the template and carrying out amination; adsorbing gold ions on the aminated surface, reducing the gold ions by using hydroboron to form gold seeds, and promoting growth by using hydroxylamine salt in a gold precursor solution containing carbonate to form a gold shell layer; the obtained nano material has near-infrared long-afterglow luminescence capability, generates photo-thermal temperature rise under 808 nm laser irradiation, and can be used for bacterial imaging and photo-thermal treatment of bacterial samples.

The invention relates to the technical field of batteries, in particular to a composite solid-state electrolyte membrane which comprises a halide solid-state electrolyte layer, a first solid-state electrolyte layer and a sulfide solid-state electrolyte layer arranged between the halide solid-state electrolyte layer and the first solid-state electrolyte layer. The first solid electrolyte layer comprises a first solid electrolyte, and the first solid electrolyte comprises a borohydride solid electrolyte and / or a carbon borohydride solid electrolyte. The electrochemical stability and the ionic conductivity of the composite solid electrolyte membrane can be improved, and the cycle performance and the rate capability of the battery can be improved.

The application discloses a method for predicting catalytic strength of transition metal on borohydride, comprising: constructing a model of metal and a model of BH4 group, setting parameters related to the model, performing structure optimization calculation on the constructed model, obtaining work functions (W f ) of surfaces of nine transition metals as indexes of inherent properties of the transition metals, marking catalytic strength of different 4d transition metals on BH4, and obtaining predicted catalytic strength by using a data analysis method. The method can realize efficient prediction and selection of a suitable borohydride metal catalyst, reduce prediction cost, has good practicability, and provides a new insight into catalytic performance of transition metal on borohydride.

The invention discloses a preparation method of a nucleotide monomer, which comprises the following steps: taking methyl-D-ribofuranoside as an initial raw material, and finally realizing the synthesis of a compound monomer as shown in a formula P through the steps of selective protection, selective deprotection, C-C bond construction, acylating chlorination reaction, basic group introduction through glycosylation, deprotection, hydroboration oxidation and ring closing in sequence. By providing a brand new synthesis method, the reaction yield is improved, the cost of the whole synthesis molecule is reduced, the binding affinity of the prepared target nucleoside monomer serving as a reported drug applied to HCV resistance to RNA can be improved so as to further improve nuclease resistance, and the method has great significance for subsequent nucleic acid drug research.

The application provides a kind of imaging photothermal gold shell coated long afterglow nanomaterial and its preparation and application.The nanomaterial includes Cr doped zinc-gallium-germanium oxide long afterglow nanometer core, mesoporous silica shell layer coated on the surface of the nanometer core and gold shell layer coated on the outer surface of the mesoporous silica shell layer.The preparation method includes: hydrothermal reaction and calcination to prepare long afterglow nanometer core;Under the condition of alkali, make tetraethyl orthosilicate (TEOS) hydrolysis and condensation to form mesoporous silica shell layer, remove template and carry out amination under cetyltrimethylammonium bromide (CTAB) template;Gold ions are adsorbed on the aminated surface and reduced to form gold seeds using borohydride, and gold shell layer is formed by promoting growth using hydroxylamine salt in a gold precursor solution containing carbonate.The obtained nanomaterial has near-infrared long afterglow luminescence capability, and generates photothermal heating under 808 nm laser irradiation, which can be used for bacterial imaging and photothermal treatment of bacterial samples.

The invention belongs to the technical field of molecular sieve preparation, and provides a boron-doped MFI type hierarchical pore molecular sieve and a preparation method thereof. The preparation method comprises the following steps: mixing an organic template agent solution, a silicon source and a boron source to obtain reaction precursor gel; and sequentially carrying out hydrothermal crystallization and roasting on the reaction precursor gel to obtain the boron-doped MFI type hierarchical pore molecular sieve, the boron source is hydroboron. According to the method, borate released by slow hydrolysis of hydroboron is used as a boron source, hydrogen released in the hydrolysis process is used as a soft template, modulation of the pore channel structure of the molecular sieve is realized, and the molecular sieve with a micro-mesoporous structure is constructed, so that the mass transfer efficiency of the MFI type molecular sieve is improved, and limitation of steric hindrance and diffusion resistance is reduced.

A method of producing hydrogen gas that includes contacting a catalytic MnO2 / MgO / CuO / g-C3N4 nanocomposite with a solution including water and a borohydride source. The catalytic MnO2 / MgO / CuO / g-C3N4 nanocomposite includes 5 to 15 wt. % MgO nanoparticles, 5 to 15 wt. % MnO2 nanoparticles, 15 to 25 wt. % CuO nanoparticles, and 55 to 65 wt. % g-C3N4 nanosheets. The MgO nanoparticles, MnO2 nanoparticles, and CuO nanoparticles are disposed on the g-C3N4 nanosheets.

The invention discloses a high-efficiency rotigotine preparation process which comprises the following steps: dissolving sodium triacetoxyborohydride in a reaction solvent, adding 2-thiopheneethylamine while stirring, dropwise adding a dichloromethane solution of 5-methoxy-2-tetralone, continuously reacting, and carrying out post-treatment to obtain N-(1, 2, 3, 4-tetramethyl-4-piperidine)-1, 2, 3, 4-tetramethyl-4-piperidine. The preparation method comprises the following steps: adding 2, 2, 4-tetrahydro-5-methoxy-2-naphthyl)-2-thiophene ethylamine; dissolving L-DTTA and L-DBTA in ethanol and a water solvent, adding into the product, carrying out a reflux reaction, and recrystallizing to obtain a single-configuration resolution salt; the preparation method comprises the following steps: adding sodium triacetoxyborohydride into a reaction kettle, carrying out product alkalization, carrying out methyl tertiary ether extraction, concentrating an organic layer until the organic layer is dry, dissolving with dichloromethane, adding sodium triacetoxyborohydride, dropwise adding propionaldehyde, continuously carrying out stirring reaction after dropwise adding, after the reaction is finished, concentrating until no liquid drop exists, and carrying out post-treatment to obtain (S)-5-methoxyrotigotine; and dropwise adding HBr, and recrystallizing with n-hexane to obtain rotigotine. According to the present invention, the STAB-mediated continuous reductive amination is adopted to replace the high pressure hydrogenation, and the L-DTTA / L-DBTA composite resolution system is designed to improve the chiral selectivity, such that the process is simplified, and the cost is reduced.

The invention discloses a synthesis method of a borohydride anion B11H14 <->. According to the synthesis method, hydroboron and halogenated hydrocarbon are taken as raw materials and are fully pyrolyzed in an organic solvent to prepare precursor salt, the precursor salt and quaternary ammonium salt are subjected to an ion exchange reaction, so that inorganic hydroboron is converted into organic quaternary ammonium salt, and then a poor solvent is adopted to achieve the purpose of crystallization and purification. According to the method, B11H14-can be efficiently synthesized, the yield can reach 70% or above, and the purity of B11H14-can reach 99.5% or above after repeated crystallization. The method is suitable for preparing the quaternary ammonium salt compound corresponding to high-purity B11H14-on a hectogram scale.

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 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.