53results about How to "Short synthesis process" patented technology

The present invention relates to a method for preparing N, N-diethylamino ethanethiol, belonging to a chemical technical field. The method includes steps of a. heating rhodanides and ethylene carbonate to react under ordinary pressure, distilling to obtain Thiirane after the reaction, the general formula of the rhodanides is M-SCN, wherein M is alkali metal of Na or K; b. mixing and stirring the Thiirane and diethylamine in a toluene dissolvant, heating under an ordinary pressure to implement a backflow reaction and distilling to obtain the N, N-diethylamino ethanethiol after the backflow reaction. The method has a short synthesis technical process, the kind of the raw materials is few and source is wide, the used toluene dissolvant may be recovered, and there will generate little waste water, waste gas and waste which may reduce environmental pollution.

The invention discloses a preparation method of a single-crystal-morphology lithium ion battery positive electrode material. The preparation method comprises the following steps: (1) adding a metal salt solution and a sodium hydroxide solution into a reaction kettle, and carrying out a co-precipitation reaction to prepare precursor slurry; (2) mixing a precursor slurry with a lithium source and a doping agent by a wet method, and performing spray drying to obtain a precursor mixture; (3) performing primary sintering on the precursor mixture to obtain a primary sintering product; and (4) washing the primary sintering product with water, mixing the washed product with a coating agent, and carrying out secondary sintering to obtain the single-crystal-morphology lithium ion battery positive electrode material. In the preparation method, the precursor slurry is prepared by adopting an ammonia-free process, particles formed by stacking a plurality of fine particles are formed, the specific surface area of the precursor is very large and is greater than 100m < 2 >/g, and the precursor with an ultrahigh specific surface area is easier to form a single-crystal positive electrode material with uniformly dispersed primary particles after being sintered, so that development of the capacity is facilitated.

The invention discloses a preparation method of an Mg2Si/SiOx/C composite cathode material membrane electrode of a lithium ion secondary battery. The preparation method comprises the steps of evenly dispersing silicon oxides or silicon powder into slurry of an organic carbon source in a mixing way; enabling a foam magnesium substrate to be evenly coated with the dispersed slurry by a blade coating machine, and drying; carrying out roll-tensioning treatment on the dried membrane electrode precursor; sintering under the protection of inert atmosphere, partly reducing the silicon oxides by utilizing the reducing property of metal and generating alloy to obtain the Mg2Si/SiOx/C composite cathode material membrane electrode, wherein all components in the composition have lithium-ion inserting activities under different potentials. The Mg2Si/SiOx/C composite cathode material membrane electrode prepared by the method is higher in capacity and good in cycle performance; the traditional crushing classification technology and electrode manufacturing technology of the solid phase synthesis material are omitted, a conductive metal foil substrate of a pole piece is omitted, and the sintered membrane can be directly taken as the electrode, so that the cost is lowered, and the synthetic process is simple and suitable for industrial production.

The invention discloses a preparation method for a lithium titanate material membrane electrode and belongs to the technical field of lithium ion batteries. The preparation method for the lithium titanate material membrane electrode comprises the following steps: taking a nano-grade titanium source and a nano-grade lithium source as base bodies; adding an organic solvent, a dispersant, an adhesive, a plasticizer and a conductive agent, and carrying out wet-method ball-milling; coating ball-milled slurry by using a scraping knife coating machine; slightly drying to obtain a precursor membrane; taking off a piece by using a piece taking machine; putting a plurality of layers of membrane pieces into a mould; pressurizing and drying in vacuum; and sintering under an inert atmosphere to obtain the lithium titanate material membrane electrode. According to the lithium titanate membrane electrode synthesized by the method, a crushing grading and electrode manufacturing process of a traditional solid-phase synthesized material is saved; meanwhile, a conductive metal foil base body of a pole piece is also saved; the sintered membrane piece can be directly used as an electrode and the cost is reduced. Sheeting and sintering are adopted so that the contact degree between precursor grains is increased, the sintering temperature is reduced and the sintering time is shortened. The synthesis process is simple so that the preparation method is suitable for industrial production.

The invention discloses a preparation method of a laminated porous nitride micro-sheet/S composite positive electrode material. The preparation method comprises the following steps: S1, dissolving a metal salt in an alcoholic solution, regulating the mixed solution to be acidic by using a strong acid, fully stirring, adding a template, and obtaining a laminated oxide micro-sheet by using a hydrothermal method; S2, nitriding the laminated oxide micro-sheet obtained in step S1 in a tubular furnace; and S3, mixing the nitride obtained by nitriding in step S2 with sulfur to carry out sulfur fixation, thereby preparing the laminated porous nitride micro-sheet/S composite positive electrode material. Abundant intercommunicated pore structures of the laminated porous nitride micro-sheet are utilized, so a large amount of sulfur storage space is provided, excellent electrical conductivity, strong sulfur fixation capacity and efficient catalytic activity of the nitride are also provided, cooperation of high sulfur loading capacity and high sulfur utilization rate is achieved, and a sulfur positive electrode with high stacking density, high sulfur surface loading capacity and high energy density is constructed.

The invention discloses a preparation method of an SnO2/graphene/PPy ternary composite material. The composite material is prepared by wrapping the surfaces of hollow SnO2 particles with PPy and graphene at the same time through a hydrothermal-in-situ polymerization method; by utilizing the synergistic effect of hollow SnO2 and PPy layers on the buffer volume change, the two-dimensional graphene is introduced, so that the strength of an electrode is enhanced, and meanwhile, the migration rate of electrons and lithium ions in the electrode is effectively improved; excellent cycling stability and rate performance are presented; the SnO2/graphene/PPy ternary composite material has the advantages that the structure is novel, the preparation is simple, and the raw materials are cheap and easilyavailable; and therefore, the composite material has huge industrial application values.

The invention discloses a nano solid-core iron phosphate-carbon source-graphene composite material; the surfaces of nano solid-core iron phosphate particles are coated with a carbon source, the particles are connected through graphene, and the nano solid-core iron phosphate-carbon source-graphene composite material is formed. The invention also discloses a preparation method of the material. The process flow is simple, the cost is low, at the same time, nitrate radicals are adopted, and the disadvantages in a traditional process that sulfate radicals in an FeSO4 raw material are difficult to wash cleanly and chloride ions in an FeCl3 raw material have a corrosion effect on equipment are overcome. The prepared lithium iron phosphate positive electrode material has the tap density reaching up to 1.68 g/cm<3>, has large volume specific capacity, is beneficial for preparation of a positive electrode material slurry and coating of an electrode slice, and improves the quality of the electrode slice.

The invention discloses a biosynthesis method and an application of environment-friendly nanometer silver ions. The synthesis method comprises the steps of collecting glochidion eriocarpum champ freshleaves to be washed and aired; cutting up the glochidion eriocarpum champ leaves, performing heating, extracting and filtering, then, enabling the leaves and a silver nitrate solution to have a reaction under the dark condition until the solution becomes the brownness, and obtaining the nano-silver. Through the reaction, the synthetic method is low in environment requirement, and the nanometer silver ions which are good in dispersion property, moderate in particle diameter, narrow in particle diameter distribution range, free of hurt to the plant growth and being in spherical or near-spherical shape are prepared. Through the experiment, it is found that the nano-silver produced through the method has the repellant effect on termite, and the silver ions have the wide application to the termite prevention and treatment in the wood industry.

The invention provides a method for preparing carbon-coated nitride porous ceramic through arc discharge plasma magnetic filtration vapor deposition , belonging to the technical field of preparation of lithium-sulfur battery electrode materials. The method comprises the following steps: ball-milling and mixing titanium oxide powder, nanometer carbon black, a binder, a pore-forming agent and other powder with a ball mill; preparing a green body of an oxide porous ceramic by using a powder tabletting method via a tablet press; placing the green body in a tubular furnace for high-temperature-atmosphere sintering to obtain nitride porous ceramic; placing the nitride porous ceramic in a chemical vapor co-deposition device, and depositing S in a pore structure of the nitride porous ceramic to obtain a nitride porous ceramic sulfur-containing electrode; and finally, combining arc discharge plasma magnetic filtering vapor deposition with a solid source, coating the surface of the sulfur-containing nitride porous ceramic sulfur-containing electrode with a layer of carbon so as to prepare the carbon-coated nitride porous ceramic sulfur-containing electrode. According to the invention, nitride in the structure serves as a conductive framework, so the structural stability and the conductivity of a sulfur-containing carrier can be improved, and the nitride has excellent conversion and adsorption performance on polysulfide. Particularly, carbon coating is carried out on the surface of the nitride porous ceramic sulfur-containing electrode, so the shuttle effect of polysulfide can be further inhibited, and remarkable effects on improving the S content of a lithium-sulfur battery, prolonging the cycle life of the battery and the like are achieved.

The invention relates to a synthesis method for an important active ingredient /-borneol-alpha-D-glucopyranoside of an herb ophiopogon japonicas, wherein the synthesis method comprises two steps such as an addition reaction and a decarboxylation protection reaction. According to the present invention, borneol and D-glucose are adopted as the starting raw materials and the simple two-step reaction is performed to successfully synthesize the /-borneol-alpha-D-glucopyranoside, and the technical difficulties of raw material refining, low reaction yield, and the like are successfully overcome.

The invention discloses a preparation method of synthetic 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl propioric acid. S1: 3,5-bis(trifluoromethyl)bromobenzene is dissolved in an organic solvent, the solution is added dropwisely into isopropylmagnesium chloride, and a Grignard reagent is obtained; mafosfamide is dissolved in an organic solvent, the solution is added dropwisely into the Grignard reagent, in order to obtain 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl propyl-1-ketone; S2: 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl propyl-1-ketone obtained in the step S1 is dissolved in an organicsolvent, and 2-(3,5-bis(trifluoromethyl)phenyl)-2-bromo-methyl propyl-1-ketone is obtained; S3: 2-(3,5-bis(trifluoromethyl)phenyl)-2-bromo-2-methyl propyl-1-ketone obtained in the step S2 is dissolved in an organic solvent, zinc bromide is added, in order to obtain 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl methacrylate; S4: 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl methacrylate obtained in the step S3 is dissolved in an organic solvent, the solution is added into an aqueous solution of alkali, and 2-(3,5-bis(trifluoromethyl)phenyl)-2-methyl propioric acid is obtained.

The invention provides a preparation method for a carbon nanotube-coated thermoelectric nanometer capsule. The preparation method comprises the following steps: 1) dispersing functionalized multi-walled carbon nanotubes in a solvent and adjusting a pH value to 10 to 14; 2) dissolving a compound containing elemental Sb or Bi in a solvent; 3) dissolving a compound containing elemental Se or Te or elemental Se or Te in a solvent; 4) uniformly mixing a mixed solution obtained in the step 2) with a mixed solution obtained in the step 3) according to a stoichiometric ratio; and 5) adding a mixed solution obtained in the step 4) into a solution obtained in the step 1) step by step according to a mass ratio of the functionalized multi-walled carbon nanotubes to the product in the step 4) of 0.3: 1 to 3: 1, carrying out a reaction at 185 DEG C for 0.5 to 2 h, and then carrying out treatment so as to obtain the carbon nanotube-coated thermoelectric nanometer capsule. The preparation method is simple in process flow and rapid in synthesis; and the prepared carbon nanotube-coated thermoelectric nanometer capsule is extensively applicable to development of micro-nano devices and nano-materials and research in subject areas like mechanics, electromagnetism, catalysis and heat transport.

The invention relates to binderless A-type molecular sieve particles and a preparation method thereof. Specifically, the preparation method comprises the following steps: (1) adding a surfactant aqueous solution and an oil phase into an aqueous phase to form a system containing the oil phase, a surfactant phase and the aqueous phase, wherein the aqueous phase is an alkali solution containing an aluminum source; and (2) adding a silicon solution containing a gelling agent and an optional hierarchical porous organic templating agent into the system containing the oil phase, the surfactant phaseand the aqueous phase, removing the oil phase and the surfactant phase, and performing crystallization treatment on the aqueous phase to form the binderless A-type molecular sieve. The invention alsoprovides the binderless A-type molecular sieve particles having hierarchical pores and an application of the particles. The preparation method provided by the invention is simple and convenient to operate and suitable for industrialization.

The invention belongs to the field of composite catalytic material preparation, and specifically relates to a carbon ferrite-titanium oxide multifunctional water purification material and a preparation method thereof. A mixed alkali composed of sodium hydroxide and potassium hydroxide is taken as the solvent; agricultural and forestry wastes such as fern leaves, banyan leaves, leaf powder, and thelike, ferric trichloride, and titanium dioxide are taken as the raw materials; a hydrochloric acid with a pH value of 1 is taken as the extracting agent; deionized water is taken as the washing agentand detergent, and anhydrous ethanol is taken as the detergent and drying carrier. Under a normal pressure, at a low temperature of 180 DEG C, a carbon precursor-ferric hydroxide-titanate composite material is synthesized; and the composite material is burned in the air at a temperature of 300 DEG C to obtain the carbon ferrite-titanium oxide composite material with a porous structure. The carbonferrite-titanium oxide composite material has stable physical-chemical properties, can respond to visible light of sunlight, is hydrophilic, and has visible light catalytic activity, an adsorption function, and a magnetic separation function.

The invention discloses a preparation method of phthaloyl azo dye, which comprises the following steps of: mixing N-alkyl-4-nitrol-phthalimide with nitrobenzene compounds according to equal molar ratio, adding the mixture into alkali-containing solvent, feeding hydrogen into the solvent under the existence of catalyst, and conducting reaction for 4-24h at room temperature being approximately 98DEG C under low pressure or normal pressure to directly prepare the phthaloyl azo dye. Compared with the existing disclosed technique, the method provided by the invention has the advantages that the synthesis process flow is short and the defects of classic synthesis method of diazotization-coupling are avoided; the safety is high and only low-pressure or normal-pressure catalytic hydrogenation for coupling is needed; the energy consumption is low and the reaction is conducted at room temperature being approximately 98DEG C; the separation and the purification are simple to conduct and the intermediates are not needed to be purified or separated by using a great quantity of solvent; the quantity of the discharged sewage is less and the secondary environmental pollution is avoided.

The invention discloses a novel method for synthesizing 6-bromine-3,4-dihydro-1H-[1,8] naphthyridine-2-ketone and relates to the field of chemical synthesis. The method comprises the following steps:by using a four-step synthesis method, performing hydrogen substitution on a benzene ring on 2-amino-3-hydroxymethylpyridine by using bromine so as to generate 2-amino-3-hydroxymethyl-5-bromopyridine;substituting hydroxyl in the 2-amino-3-hydroxymethyl-5-bromopyridine by using chlorine in thionyl chloride so as to generate 2-amino-3-methyl chloride-5-bromopyridine hydrochloride; carrying out an annulation reaction of the 2-amino-3-methyl chloride-5-bromopyridine hydrochloride by using diethyl malonate so as to generate 6-bromine-3-nonanoic acid-ethyl ester-1,2,3,5-tetrahydro-1,8-naphthyridine-2-ketone; finally, under an alkali condition, removing carboxylic acid carbethoxy from the 6-bromine-3-nonanoic acid-ethyl ester-1,2,3,5-tetrahydro-1,8-naphthyridine-2-ketone, thereby obtaining a final product, namely 6-bromine-3,4-dihydro-1H-[1,8] naphthyridine-2-ketone. The method is low in raw material cost, simple in synthesis process, not harsh in reaction condition, safe and convenient to operate, high in final product yield, and applicable to large-scale industrial production.

The invention discloses a pyridyl-containing calix[4]arene derivative, a preparation method thereof and application of the derivative as a manganese ion extraction agent. The pyridyl-containing calix[4]arene derivative is obtained by carrying out nucleophilic substitution reaction on alkyl calix[4]arene and 2-(halogenated methyl)pyridine hydrochloride under base catalysis; the pyridyl-containing calix[4]arene derivative is high in physical and chemical stability, relatively good in oil solubility, insoluble in water and relatively good in metal ion recognition and complexation capability, and when the pyridyl-containing calix[4]arene derivative and P204 form a synergistic extraction system, the pyridyl-containing calix[4]arene derivative has a very strong positive synergistic extraction effect on manganese ions in a sulfate solution system; and the derivative has an obvious anti-synergistic extraction effect on metal ions such as nickel, cobalt, magnesium and lithium, is very suitable for selective extraction and separation of manganese ions in a complex metal ion system, and has a good industrial application prospect.

The invention discloses a method for preparing 3, 7-diethyl nonane-4, 6-diketone, and belongs to the field of chemical synthesis. The 'method for preparing the 3, 7-diethyl nonane-4, 6-diketone' has the advantages that dimethyl isophthalate which is low in cost is used as a raw material for the 3, 7-diethyl nonane-4, 6-diketone, the 3, 7-diethyl nonane-4, 6-diketone can be prepared by the aid of four-step reaction including elimination and addition, catalytic hydrogenation reaction, Birch reduction and ozone oxidation, the method is low in cost, convenient to operate, high in yield and suitable for large-scale industrial production, includes short synthesis processes and is safe, and reaction conditions are mild.

The invention provides a novel method for synthesizing ethenzamide. In the method, salicylamide and ethylsulfate serve as raw materials and are subjected to reaction to synthesize the ethenzamide in a sodium hydroxide solution. Accordingly, organic solvents are not adopted, synthesizing steps are simple, the yield is high, the index of ethenzamide products reaches 'national drug standard' of 2006 edition, and the method is suitable for drug production.