507 results about "ALUMINUM HYDRIDE" patented technology

The present invention is a method for manufacturing a negative electrode material for a secondary battery with a non-aqueous electrolyte comprising at least: coating a surface of powder with carbon at a coating amount of 1 to 40 mass % with respect to an amount of the powder by heat CVD treatment under an organic gas and/or vapor atmosphere at a temperature between 800° C. and 1300° C., the powder being composed of at least one of silicon oxide represented by a general formula of SiO_x (x=0.5 to 1.6) and a silicon-silicon oxide composite having a structure that silicon particles having a size of 50 nm or less are dispersed to silicon oxide in an atomic order and/or a crystallite state, the silicon-silicon oxide composite having a Si/O molar ratio of 1/0.5 to 1/1.6; blending lithium hydride and/or lithium aluminum hydride with the powder coated with carbon; and thereafter heating the powder coated with carbon at a temperature between 200° C. and 800° C. to be doped with lithium at a doping amount of 0.1 to 20 mass % with respect to an amount of the powder. As a result, there is provided a method for manufacturing a negative electrode material for a secondary battery with a non-aqueous electrolyte that enables a silicon oxide negative electrode material superior in first efficiency and cycle durability to conventional ones to be mass-produced (manufactured) readily and safely even in an industrial scale.

In one aspect, the invention relates to activated aluminum hydride hydrogen storage compositions containing aluminum hydride in the presence of, or absence of, hydrogen desorption stimulants. The invention particularly relates to such compositions having one or more hydrogen desorption stimulants selected from metal hydrides and metal aluminum hydrides. In another aspect, the invention relates to methods for generating hydrogen from such hydrogen storage compositions.

The invention discloses a method for reducing 8-benzyl-2,8-diazabicyclo[4,3,0]nonane and a chiral isomer thereof. The method comprises the steps of: taking 8-benzyl-7,9-dioxo2,8-diazabicyclo[4,3,0]nonane or (1S,6R)-8-benzyl-7,9-dioxo2,8-diazabicyclo[4,3,0]nonane as a raw material, and adopting a metal borohydride/BF3 reduction system for reduction to obtain a corresponding product, namely the 8-benzyl-2,8-diazabicyclo[4,3,0]nonane or (S,S)-8-benzyl-2,8-diazabicyclo[4,3,0]nonane. The method adopts the metal borohydride/BF3 reduction system for reduction, avoids the use of an expensive and dangerous reagent, namely lithium aluminum hydride, reduces production cost, improves the safety of the operation, and provides a safe and economical production method for industrial mass production of a moxifloxacin intermediate, namely the (S,S)-8-benzyl-2,8-diazabicyclo[4,3,0]nonane.

The invention belongs to the technical field of medicament synthesis, and in particular relates to a chemical synthetic method of hydroxytyrosol. The chemical synthetic method comprises the steps of (1) protecting two phenolic hydroxyl groups of catechol by using dichloromethane, and enabling catechol to react with dichloromethane to prepare 1,2-methylenedioxybenzene; (2) enabling 1,2-methylenedioxybenzene to react with various monoesters of oxalyl chloride to prepare 3,4-methylenedioxy phenylglyoxylic acid ester; (3) preparing 3,4-methylenedioxy phenylacetic acid by using 3,4-methylenedioxy phenylglyoxylic acid ester through a Wollff-kishner-Huang Minglong reduction reaction; and (4) reducing the 3,4-methylenedioxy phenylacetic acid by using lithium aluminum hydride, lithium borohydride or sodium borohydride to prepare 3,4-methylenedioxy phenethyl alcohol, and then removing methylene protection of the 3,4-methylenedioxy phenethyl alcohol by using boron tribromide or palladium on activated carbon to prepare hydroxytyrosol. A reactive reagent used in the synthetic method disclosed by the invention is easy to obtain and low in price, the reaction condition is mild, and the final yield of the whole reaction is 23%.

The invention discloses a method for synthesizing low-chloride polyphenylene sulfide resin, comprising the following steps: taking sodium sulfide and p-dichlorobenzene with the molar ratio of 1:1 as raw materials, N-methyl-2-pyrrolidone as a solvent, and carrying out polycondensation to generate the polyphenylene sulfide resin under the action of alkali metal cosolvent. The synthesizing process mainly comprises the following steps: adding adjuvant lithium aluminum hydride in the dewatering phase of sodium sulfide; adding molecular weight regulator and deionizer in the polycondensation stage; and adopting an extraction process in the resin recovery stage. The product obtained in the invention has low content of halogen element, relative low polydispersion coefficient, very narrow molecularweight distribution, high oxygen index and other excellent performance indexes, can be used as products such as injection moulds, extrusion moulds, fibers, films and the like, can be widely used in the fields such as machinery, chemical industry, electrical and electronic products, military project, aerospace and the like, and is particularly applied to electrical and electronic field with very excellent electrical insulation property.

The present invention publicly discloses a synthetic method and intermediates of rosuvastatin calcium and synthetic methods of the intermediates. The synthetic method uses 4-4′-fluorophenyl-6-isopropyl-2-(N-methyl-N-methylsulfonylamino)pyridine-5-formaldehyde as the raw material, includes 4-4′-fluorophenyl-6-isopropyl-2-(N-methyl-N-methylsulfonylamino)pyridine-5-acrylonitrile (intermediate I) from a nitrilized reaction, and 4-4′-fluorophenyl-6-isopropyl-2-(N-methyl-N-methylsulfonylamino)pyridine-5-acraldehyde (intermediate II) from an aldehydized reaction of the intermediate I, and further goes through such unit processes as side-chain extension, ketone-group reduction, ethyl-group hydrolysis and neutralization reaction or decomposition reaction to obtain rosuvastatin calcium. The nitrilized reagent can be phosphate diethylacetonitrile, acetonitrile, etc.; the aldehyde reductant can be diisobutyl aluminum hydride, red aluminum, etc.; and the ketone-group reductant can be diethylmethoxyborane, NaBH₄, KBH₄, etc.

The invention discloses an aluminum hydride surface coating modification method. A metal oxide or a metal substance with a nanometer thickness is deposited on the aluminum hydride powder surface to clad the aluminum hydride powder surface by adopting an atomic layer deposition technology, so as to improve the heat stability of the aluminum hydride powder. The method comprises the following steps: S1, putting aluminum hydride powder into a cavity and vacuumizing; S2, introducing a fluidized gas after the cavity is heated to the set temperature and the temperature is even and stable, so that aluminum hydride is pre-dispersed; S3, atomic layer deposition reaction, carrying out the atomic layer deposition reaction when the temperature inside the cavity achieves 50-130 DEG C; S4, repeating the atomic layer deposition reaction for a plurality of times, so that the powder surface deposition thickness is continuously increased, and controlling the thickness of the metal oxide or the metal deposited on the surface of the aluminum hydride powder by controlling the circulating times of the deposition reaction. Thus, a cladding layer of which the cladding thickness is 1-1,000nm is cladded on the surface of the aluminum hydride powder, so as to achieve stabilization of powder.

Methods of controlled hydrolysis/alcoholysis and regeneration of a borohydride are disclosed. Examples of the present invention show that hydrolysis of sodium borohydride or lithium borohydride with dilute acid provides simultaneous generation of H₂ and boric acid for recycling. Other examples of the present invention show methods for regenerating a borohydride by reacting an aluminum hydride to a borate compound to provide a regenerated borohydride.

There are provided a conductive film forming composition capable of forming wiring or an electrode which can be suitably used in a variety of electronic devices, easily and inexpensively, a method for forming a film using the composition, a conductive film formed by the method, and wiring or an electrode which comprises the film.

A conductive film forming composition comprising a complex of an amine compound and aluminum hydride and an organic solvent is applied on a substrate and then subjected to a heat treatment and/or irradiation with light, whereby a conductive film such as an electrode or wiring is produced.

The invention provides an Mg-based composite hydrogen storage material containing alkaline earth metals-aluminum hydride and a preparation method thereof, which belongs to the technical field of hydrogen storage material. The chemical general formula of the hydrogen storage material is MgH2+x wt.%(Sr1-yCay)2AlH7+z wt.%TiF3, wherein x is more than or equal to 30 and less than or equal to 50, y is more than or equal to 0 and less than or equal to 0.5, and z is more than or equal to 2 and less than or equal to 10. The hydrogen storage material is gained by mechanically ball milling three materials powder of MgH2, (Sr, Ca)2AlH7 and TiF3, a planetary ball mill is adopted when ball milling, the ball material ratio is 15:1 to 20:1, the rotational speed is 350 to 400rpm, the ball milling time is 10 to 20h, the ball milling protecting atmosphere is argon gas or hydrogen gas, and the atmosphere pressure is 1 to 5atm. The invention has the advantages that: the preparation technique is simple, the provided composite hydrogen storage materials do not need to be activated, and have high hydrogen storage capacity, simultaneously have good low temperature hydrogen absorption dynamic performance and high hydrogen absorption and desorption cycling stability. The invention is applicable to the safe and efficient storage and transportation of the hydrogen, especially the hydrogen fuel cells and other fields.

The present invention relates to diarylphenoxyaluminum compounds which are obtainable by reacting a bis(diarylphenol) ligand of the formula (I)

with an alkylaluminum compound and/or a complex aluminum hydride.

The invention moreover relates to the use of such diarylphenoxyaluminum compounds as catalysts.

Moreover, the invention relates to a method of producing isopulegol by cyclization of citronellal in the presence of diarylphenoxyaluminum compounds as catalysts.

The invention also relates to a method of producing menthol by cyclization of citronellal in the presence of diarylphenoxyaluminum compounds as catalysts and subsequent hydrogenation.

A complex aluminum hydride doped with a catalytic material adapted to increase the kinetics of hydrogen absorption/desorption of the aluminum hydride without reducing the hydrogen storage capacity of the aluminum hydride.

The invention discloses a reduction method of graphene oxide. According to the reduction method, with metal hydride as a reducing agent and lewis acid as a catalyst, graphene oxide is reduced at room temperature. The reduction method comprises the following steps: dispersing the graphene oxide in a solvent according to the dispersing concentration of 0.2mg/ml-4mg/ml by virtue of a magnetic stirring, high-shearing mixing or ultrasonic dispersing method; adding lewis acid, stirring and dispersing, wherein the adding concentration of the lewis acid is 1mM-30mM; adding metal hydride and stirring, wherein the dispersing concentration of the metal hydride is 10mM-300mM, and carrying out reduction reaction for 30 minutes to 12 hours at room temperature; filtering and washing by using a cleaning agent until the pH value is neutral, wherein the cleaning agent is pure water, and the metal hydride is one of lithium aluminum hydride, sodium borohydride and sodium hydride. The reduction method of the graphene oxide is efficient, cheap, non-toxic and pollution-free and capable of efficiently removing oxygen-containing functional groups out of graphene oxide, so that a hexatomic ring structure of the graphene oxide is recovered.

The invention relates to a preparation method for PBO fiber, in particular to a preparation method for binary grafted modified PBO fiber, and aims to solve the problem that the conventional PBO fiber has poor infiltration with matrix resin as the surface is inert and the fiber mechanical property is reduced as PBO fiber molecular chains break due to elemental oxygen. The preparation method comprises the following steps: 1, functionally processing graphene oxide; 2, performing activating treatment on PBO fiber; adding the PBO fiber into a lithium aluminum hydride-diethyl ether saturated solution to be subjected to hydroxyl functional processing; 4, grafting APTMS on the surface of the PBO fiber; 5, binarily grafting the graphene oxide on the surface of the PBO fiber. According to the invention, both the APTMS and the graphene oxide are grafted on the surface of the PBO fiber through a chemical grafting method, so that the infiltration of the PBO fiber is improved, and the binary grafted PBO fiber can keep higher tensile strength under the impact of elemental oxygen. The preparation method is mainly applied to the preparation of PBO fiber.

A method for directly preparing alkali metal aluminum hydrides such as NaAlH4 and Na3AlH6 from either the alkali metal or its hydride, and aluminum. The hydride thus prepared is doped with a small portion of TiAl3, in order to improve the reaction kinetics of the hydride compound thus formed. The process provides for mechanically mixing the dry reagents under an inert atmosphere followed by charging the mixed materials with high pressure hydrogen while heating the mixture to about 125° C.

A primary aluminum hydride cell and a battery formed with a plurality of the cells is described herein.. In some embodiments, the cells are constructed of:

(a) an anode comprising aluminum hydride and a conductive material;

(b) a cathode; and

(c) an aqueous electrolyte.

The invention belongs to the field of medicinal synthesis, and particularly relates to a method for preparing hydroxytyrosol, which comprises the following steps of: (1) protecting free hydroxyl groups at 3 and 4 positions, on 3,4-dihydroxy benzaldehyde with benzyl, namely, reacting the 3,4-dihydroxy benzaldehyde with benzyl bromide to prepare 3,4-dibenzyloxybenzaldehyde; (2) reacting N-methylaniline acetonitrile with the 3,4-dibenzyloxybenzaldehyde to prepare 3-(3,4-dibenzyloxyphenyl)-2-(methylphenylamino) acrylonitrile, and hydrolyzing the 3-(3,4-dibenzyloxyphenyl)-2-(methylphenylamino) acrylonitrile under acidic condition to prepare a 3,4-dibenzylosyphenylacetic acid; (3) reducing a carboxyl group of the 3,4-dibenzylosyphenylacetic acid with lithium borohydride, lithium aluminum hydride or sodium borohydride to prepare 3,4-dibenzyloxyphenethyl alcohol; and (4) catalyzing the 3,4-dibenzyloxyphenethyl alcohol with a catalyst palladium/carbon to prepare the hydroxytyrosol. The reagents used in the method are easily obtainable and low in cost, reaction conditions are mild, and the final overall yield of the whole reaction reaches 50 to 60 percent.

The invention relates to a sulfoacid rare earth catalyst for polymerizing high-cis-isoprene rubber and a preparation method thereof. The catalyst comprises benzenesulfonic acid neodymium rare earth complex and alkyl aluminum; the molar ratio of the alkyl aluminum to the rare earth neodymium in the benzenesulfonic acid neodymium rare earth complex is 15 to 40:1, wherein the benzenesulfonic acid neodymium rare earth complex comprises benzenesulfonic acid neodymium alcohol complex, benzenesulfonic acid neodymium sulphoxide complex, benzenesulfonic acid neodymium furan complex, benzenesulfonic acid neodymium amine complex, benzenesulfonic acid neodymium ether complex and benzenesulfonic acid neodymium ester complex; ligand comprises: alcohol compound, sulfoxide compound, furan compound, amine compound, ether compound and ester compound; and the alkyl aluminum comprises: 3-isobutyl aluminum, triethyl aluminum, diisobutyl aluminum hydride, or diethyl aluminum hydride. The sulfoacid rare earth complex catalyst is used for polymerizing isoprene, and can obtain the high-cis rare earth polyisoprene rubber with the cis 1,4 structure content more than 96.0 percent and the weight-average molecular weight more than 2.2 million.

The invention provides a composition used for a rare earth catalyst. The composition contains alkyl aluminum and/or alkyl aluminum hydride, a rare earth compound and conjugated diene. The rare earth compound is a compound having a general formula as MR3.nL, wherein M is a rare earth metal, R is halogen, L is an electron-donating ligand, and the value of n is 1-3. Also, the alkyl aluminum and/or alkyl aluminum hydride, the rare earth compound and the conjugated diene are in a molar ratio of 0.05-1.5:0.01-0.05:1. The invention provides a rare earth catalyst, which is obtained by enabling the composition provided in the invention to contact an inert organic solvent mutually under the protection of an inert gas. Specifically, the contact condition enables the conjugated diene in the composition to polymerize so as to obtain a conjugated diene polymer with a polymerization degree of not less than 150. The invention also provides application of the catalyst in the polymerization of conjugated diene. The rare earth catalyst provided in the invention has good stability, and is in favor of synthesizing polymer products with stable quality and uniformity when it is used for conjugated diene polymerization.

The present invention provides methods and materials for the formation of hydrogen storage alanes, AlH_x, where x is greater than 0 and less than or equal to 6 at reduced H₂ pressures and temperatures. The methods rely upon reduction of the change in free energy of the reaction between aluminum and molecular H₂. The change in free energy is reduced by lowering the entropy change during the reaction by providing aluminum in a state of high entropy, by increasing the magnitude of the change in enthalpy of the reaction or combinations thereof.

The present invention discloses a synthetic method of heteroaromatics polyphenyl sulfur ether. The present invention adopts sodium sulfide and paradichlorobenzene and 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole as raw materials and N-methyl-2 pyrrolidone as solvent for condensation and polymerization under the role of alkali metal lacquer solvent, so as to produce the polyphenyl sulfur ether resin. The mol ratio between sodium sulfide and paradichlorobenzene and 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole is 1:0.6-0.9:0.4-0.1. The sequential process mainly includes: in the process of sodium sulfide dehydration stage, assistant lithium aluminum hydride is added; in the condensation and polymerization stage, 2-(4-chlorine phenyl group)-5-chlorine phenyl benzimidazole is added. The product provided by the present invention with excellent indexes of relatively low dispersion coefficient and narrow molecular weight distribution and oxygen index can be made into paint, injection mold, fiber and membrane and be widely applied to the fields of machinery, chemicals, oil, electronic apparatus, war industry and airspace.

The invention discloses an aluminum catalyst for polyester synthesis, a preparation method thereof and a usage method thereof. The catalyst which is aluminum glycol and is special for a polycondensation reaction in a polyester synthesis process of terephthalic acid and glycol is prepared through reacting aluminum/aluminum alcoholates/lithium aluminum hydride with glycol. The catalyst, which has less toxicity, allows the molecular weight of PET catalyzed by the catalyst to achieve more than 30,000, can coexist with polycondensation products, has no influence on the quality of the PET, allows requirements of environmental protection to be satisfied and requirements of activity to be guaranteed, has a high activity on the PET synthesizing reaction, and has low cost, is a novel catalyst for the condensation polymerization of PET synthesis.