43results about How to "The reaction process is safe and environmentally friendly" patented technology

The invention relates to a preparation method of a multilevel-structured hollow nano-sphere of negative electrode material of a high-performance lithium ion secondary battery. The preparation method comprises the following steps: with a zinc source, a tin source and weak base as raw materials as well as surfactant polyacrylic acid (PAA) as a template, synthesizing a multilevel-structured hollow zinc hydroxystannate nano-sphere by virtue of a one-step hydrothermal method, wherein the diameter of the nano-sphere is 400-600nm; calcining in an air atmosphere, so as to obtain a morphology-maintained multilevel-structured zinc stannate nano-sphere structure. According to the preparation method, when the multilevel-structured hollow zinc hydroxystannate nano-sphere and a multilevel-structured zinc stannate nano-sphere are utilized as the negative electrode materials of the lithium ion secondary battery, both the two compounds show excellent electrochemical performance, high specific discharge capacity, good cycling stability and excellent rate capability; due to a specific multilevel structure, the hollow nano-sphere can provide a large surface area and a stable structure and can be widely applied to the fields of catalysis, the lithium ion secondary battery, solar cells and the like.

The invention discloses a method for preparing a lithium ion battery cathode material in-situ carbon coated lithium manganese borate composite material. The method comprises the following steps of: grinding a lithium source, a manganese source, a boron source and a carbon source in a dispersed solvent in a ratio and uniformly mixing; drying slurry to obtain powder; and sintering the powder in a tube furnace to obtain a hexagonal or monocline composite material of lithium manganese borate and the carbon. A lithium ion battery pole piece which is made of the obtained composite material is used for assembling a battery and the obtained battery material has relatively higher discharge capacity and good cycle stability. In the invention, a solid phase method is adopted, the method is easy to operate, the energy consumption is low, the composite material can be manufactured in bulk and industrialization can be easily realized.

The invention discloses a method of preparing a super-capacitor electrode material. The method comprises: step S1: preparing a nanorod precursor powder: uniformly fixing transition metal salt and carbamide or sodium hydroxide solution, and after heating in a hydrothermal reaction kettle, keeping temperature until the reaction is finished, after cooling, cleaning and drying, obtaining the nanorod precursor powder; and step S2: preparing the electrode material; taking deionized water as a solvent, uniformly mixing the nanorod precursor powder and a sulfur source, after heating in the hydrothermal reaction kettle, keeping temperature until the reaction is finished, after cooling, cleaning and drying, obtaining the nanotube electrode material. According to the method of preparing the super-capacitor electrode material, the nanorod precursor is prepared by hydrothermal method; then, the electrode material is obtained by mixing precursor and the sulfur source and performing the hydrothermal reaction; the reaction process is safe and environment-friendly and the process is simple; in addition, the calibers of the nanotubes are uniform and can be controlled, the production rate of the nanotube is high and the nanotube has excellent electrochemical performances, so that the nanotube has broad application prospects.

The invention discloses a one-step method for in-situ preparation of carbon coated manganese carbonate for the negative electrode of a lithium ion battery .The method specifically comprises the steps of 1, preparing potassium permanganate solution of certain concentration and carbon source solution of certain concentration respectively, wherein the molar concentration ratio of the carbon source solution to the potassium permanganate solution is 1:(2-2.5); 2, adding the carbon source solution to the potassium permanganate solution, and conducting stirring dispersion and ultrasonic treatment in sequence; 3, adding dispersed solution into a reaction still to be heated for 3-24 h at the temperature of 120-180 DEG C; 4, naturally cooling the reaction still to room temperature, and conducting cleaning and drying to obtain powder, namely the in-situ carbon coated manganese carbonate for the negative electrode of a lithium ion battery .Raw materials for preparation are cheap and easy to obtain, operation is easy, energy consumption is low, pollution is avoided, carbon coating of the obtained manganese carbonate is uniform, size distribution is uniform, purity is high, particle collapse during charging and discharging of manganese carbonate can be effectively prevented, and the cycling stability of the lithium ion battery is improved.

The invention relates to an electron transport material for organic electroluminescent devices and a preparation method of the electron transport material. The preparation method comprises the following steps of taking 4,7-dihalogen-1,10-phenanthroline as a starting material, and carrying out a Suzuki reaction on the starting material and arylboronic acid or arylboronate to obtain 4,7-diaryl-1,10-phenanthroline and derivates thereof as the electron transport material. The method provided by the invention has shorter synthetic route, simpler technology and higher reaction yield, obtains end-products with various types of different substituent groups, and has more easiness in material structure design and performance optimization in comparison with the conventional Skraup preparation method; meanwhile, no highly toxic materials such as arsenic acid and the like are in the reaction process, so that the reaction condition is milder, and the reaction process is safer and more environment-friendly. The preparation method provided by the invention is suitable for laboratorial preparation in gram scale and kilogram scale as well as industrial mass production in ton scale.

The invention provides a high-performance polycarboxylate superplasticizer, a preparation method thereof and concrete. The polycarboxylate is prepared from the following components: ethylene glycol monovinyl polyethylene glycol ether macromonomer, unsaturated carboxylic acid micromonomer, alkali, an oxidizing agent, a reducing agent, a chain transfer agent and a catalyst. Compared with the prior art, the polycarboxylate superplasticizer is synthesized at normal temperature, the reaction time is short, the synthesis process is simple, the investment is low, and the economic benefit is relatively good. The polycarboxylate superplasticizer prepared according to the preparation method not only has a better water reducing effect, but also is excellent in collapse resistance.

The invention provides a method for synthesizing 8-(nitro methyl) quinoline compounds. 8-methylquinoline compounds are taken as a raw material and are added into an organic solvent together with a catalyst and a nitration reagent, the mixture is sealed and heated to 80-130 DEG C for a reaction, the reaction is traced with TLC (thin-layer chromatography) until the reaction ends, a reaction liquid is subjected to aftertreatment, and the 8-(nitro methyl) quinoline compounds shown in the formula II are obtained. The nitration method has the advantage of specifity of the nitration position, nitration is only performed on methyl, no nitration products are generated on a benzene ring, the reaction process is safe and environment-friendly, the substrate adaptability is good, and methyl nitration of all substituent groups can be realized; 8-methylquinoline is directly taken as a raw material, the reaction steps are simple, and the method is a new way for synthesizing 8-(nitro methyl) quinoline compounds containing substituent groups.

The invention provides a preparation method of a pregabalin chiral intermediate. The pregabalin chiral intermediate is (S)-4-isobutyl-dihydro-3H-furan-2-one. The preparation method comprises following steps: S1, a chiral hydroxyl compound 3 is obtained from an S-epoxypropane compound 2 via ring-opening reaction under Grignard reagent conditions; S2, sulfonylation protection of hydroxy groups in the chiral hydroxyl compound 3 is carried out so as to obtain a compound 4 with chiral leaving groups; and S3, the compound 4 and an acetate compound or malonic ester are subjected to substitution reaction, and a compound 1 is obtained via hydrolysis, decarboxylation, and ring closing reaction under acidic conditions. The raw materials used in preparation of the pregabalin chiral intermediate are cheap and easily available; reaction route is short; operation is simple; reaction process is safe and is friendly to the environment; the entire yield is high; the preparation method is convenient for large scale production; and an economical feasible route is provided for production of high purity pregabalin.

The invention discloses a synthesis method of morpholine compounds, belonging to the field of organic synthesis. The invention aims to solve the problem of poor environment friendliness of the traditional synthesis method of morpholine compounds. The method comprises the steps of firstly, adding heterocyclic nitrogen compounds, persulfate and 2-chlorohydrin into a reaction vessel, and reacting at room temperature; secondly, adding a diluent, then, adding KOH, carrying out cyclization reaction at room temperature, next, filtering, and concentrating to be dry to obtain a solid; and thirdly, carrying out silica gel column chromatographic purification and separation on the solid obtained in the second step by taking a mixed solution composed of petroleum ether and ethyl acetate as an eluant to obtain the morpholine compounds. The synthesis method is capable of realizing reaction at normal temperature and normal temperature, mild in reaction condition, free of inert gas protection and simple in operation; and the persulfate serving as an oxidizing agent is cheap, easy to obtain, free of pollution, safe, environment-friendly and low in cost.

The invention provides a method for synthesizing (nitroalkynyl)benzene compounds shown in formula II, comprising: adding phenylacetylene compounds shown in formula I as materials, along with a nitrifying agent, into an organic solvent, hermetically reacting at 20-50 DEG C, performing TLC (thin layer chromatography) tracing until the reaction is over, and post-treating the reacted liquid to obtain (nitroalkynyl)benzene compounds shown in the formula II. The nitrifying method of the invention has the advantage of good nitrifying site specificity, nitrifying is carried out only on alkynyl, no nitrification products are produced on benzene rings, the reaction process is good in safety, environment-friendly and good in substrate adaptability, and it is possible to provide alkynyl nitrifying for various substituents.

The invention discloses a preparation method of crystal form I atorvastatin calcium. The method includes the steps of: preparation of atorvastatin ester; preparation of an atorvastatin salt; preparation of atorvastatin calcium; refining an atorvastatin calcium crude product; and crystal transformation of the atorvastatin calcium refined product. The method provided by the invention adopts one-potprocess to simplify the synthesis process of the crystal form I atorvastatin calcium, optimizes the reaction conditions, adopts cheap, easily available and environment-friendly materials, directly reduces the industrial cost, and realizes safe and environment-friendly production.

The invention discloses a method for preparing and purifying hexaalkylguanidine chloride, which includes steps that tetraalkylurea first reacts with triphosgene under the effect of catalyst, then dialkyl amine is added to continue reacting, pH is adjusted through alkali liquor after reaction, then liquid is separated, and finally recrystallization is conducted in mixed organic solvent and the like. The method adopts molecular sieve catalyst, improves conversion rate of triphosgene, and greatly increases product yield. The triphosgene is non-toxic, and safe and reliable to use. The mixed organic solvent is used to recrystallize, not only product purity is improved, but also solid ion phase transfer catalyst is obtained. The method is convenient to operate, does not require special equipment, and is suitable for industrial production, high in product purity and especially suitable for high temperature polymerization.

The invention discloses a method for deeply removing antimony and copper impurities from regenerated crude tin. Borax and tin sulfide are mainly used as antimony and copper removing agents, the operation is easy, additionally, the removing temperature is reduced, the energy consumption is low, the impurity separation effect is good, the effects of safety and environmental friendliness are achieved, antimony and copper are simultaneously removed at one time, the quality of the crude tin reaches Sn99.90 of the AA grade, the requirements of GB / T728-2010 are met, the content of the impurity Sb islower than 0.02 wt%, the content of the impurity Cu is lower than 0.008 wt%, the problem of environmental pollution caused by adding aluminum to remove antimony and adding sulfur to remove copper in the prior art is solved, and the problems of complex antimony and copper removing steps and high energy consumption in the prior art are solved.

The invention discloses a preparation method of crystal form I atorvastatin calcium. The method includes the steps of: preparation of atorvastatin ester; preparation of an atorvastatin salt; preparation of atorvastatin calcium; refining an atorvastatin calcium crude product; and crystal transformation of the atorvastatin calcium refined product. The method provided by the invention adopts one-potprocess to simplify the synthesis process of the crystal form I atorvastatin calcium, optimizes the reaction conditions, adopts cheap, easily available and environment-friendly materials, directly reduces the industrial cost, and realizes safe and environment-friendly production.

The invention discloses a preparation method of a clopidogrel hydrogen sulfate crystal form II. The method includes: preparation of (+)o-chlorophenylglycine methyl ester; preparation of (+)alpha-(2-thiophene ethylamino)-alpha-(2-chlorphenyl)methyl acetate hydrochloride; preparation of (+)clopidogrel free alkali; preparation of (+)clopidogrel camphorsulfonic acid double salt; hydrolysis of (+)clopidogrel camphorsulfonic acid double salt; and preparation of clopidogrel hydrogen sulfate. The preparation method of the clopidogrel hydrogen sulfate crystal form II provided by the invention optimizesthe synthesis process of clopidogrel hydrogen sulfate, selects cheap and easily available materials, adopts mild reaction conditions, and can achieve safe and environment-friendly production of a high-purity product.

The invention provides a method for synthesizing 2, 6-dibromo-4-cyanophenol. The method includes a particular operation step of carrying out reaction on 4-cyanol phenol and bromine such as sodium bromine and potassium bromine in air or nitrogen atmosphere in the presence of persulfate and solvents under heating or illumination conditions. The method has the advantages that the method is safe and reliable, is high in yield, free of pollution and easy to implement, is an environment-friendly chemical process and can be used for preparing the 2, 6-dibromo-4-cyanophenol, and reaction conditions are mild.

The invention relates to a preparation method of a multilevel-structured hollow nano-sphere of negative electrode material of a high-performance lithium ion secondary battery. The preparation method comprises the following steps: with a zinc source, a tin source and weak base as raw materials as well as surfactant polyacrylic acid (PAA) as a template, synthesizing a multilevel-structured hollow zinc hydroxystannate nano-sphere by virtue of a one-step hydrothermal method, wherein the diameter of the nano-sphere is 400-600nm; calcining in an air atmosphere, so as to obtain a morphology-maintained multilevel-structured zinc stannate nano-sphere structure. According to the preparation method, when the multilevel-structured hollow zinc hydroxystannate nano-sphere and a multilevel-structured zinc stannate nano-sphere are utilized as the negative electrode materials of the lithium ion secondary battery, both the two compounds show excellent electrochemical performance, high specific discharge capacity, good cycling stability and excellent rate capability; due to a specific multilevel structure, the hollow nano-sphere can provide a large surface area and a stable structure and can be widely applied to the fields of catalysis, the lithium ion secondary battery, solar cells and the like.

The invention discloses a method for synthesizing tris(trihydrocarbylsiliconyl)phosphite. Phosphorous acid and trihydrocarbylsiliconyl amine are added to a dry reaction bottle, and then reacted and evaporated under the conditions of heating, stirring and reflux condensation. The generated amine, the reaction liquid is subjected to precision filtration and rectification under reduced pressure to obtain high-purity tris(trihydrocarbylsilyl)phosphite. The present invention adopts phosphorous acid to react with trihydrocarbyl silyl amine, and the selectivity of tris (trihydrocarbyl silyl) phosphite product is high, and the obtained tris (trihydrocarbyl silyl) phosphite crude product can be easily purified to more than 99.9%. , to meet the requirements of lithium ion electrolyte additives; and the raw materials of the present invention are easy to obtain, the process route is simple, the reaction process is safer and more environmentally friendly, the energy consumption is low, and the amount of waste discharge is small, and it is suitable for industrial production.

The invention discloses a synthesis method of 1-hydroxy-pyrrolo[2,3-c]piperidine, which adopts the following steps: (1) 1-nitro-5-chloro- 1-pentene is the starting material, reacts with TosMIC shown in formula (Ⅴ) under alkaline conditions to obtain compound (VI); (2) compound (VI) generates compound (VII) through catalytic hydrogenation; (3) Compound (VII) generates compound (III) under the action of a base. The synthesis method of 1-hydroxy-pyrrolo[2,3-c]piperidine of the present invention reduces the process cost and production risk.

The invention discloses a hydrogenation treatment method for high-acid crude oil, which is characterized in that the high-acid crude oil is conveyed to a fixed bed reactor with heat accumulation bodies after being mixed with hydrogen gas for hydrogenation reaction, and reaction products flow out of the reactor to obtain products with qualified acid values. When the operation is started, a hot mixture of clean oil and hydrogen gas is firstly introduced for heating the heat accumulation bodies, after the heat accumulation bodies reach the reaction temperature, the materials are switched into acid-containing crude oil, reaction effluents accumulate heat for the other heat accumulation body, and the two heat accumulation bodies are alternately switched for being used. The method has the advantages that the heat released by high-acid crude oil hydrogenation and the accumulated heat of the heat accumulation bodies can be used for maintaining the temperature required by the hydrogenation reaction, an external heat source is not needed, a heating furnace is omitted, the corrosion of the high-acid crude oil on high-temperature equipment is avoided, the equipment investment and the operation cost are saved, and simultaneously, the heat sources are also reasonably utilized.

The invention discloses a synthesis method of pharmaceutical-grade potassium antimony tartrate. Newly prepared metantimonic acid sol is used instead of insoluble antimony trioxide to perform liquid-phase reaction with potassium bitartrate in a water solution to prepare the high-purity potassium antimony tartrate. The method comprises the following steps: dispersing metantimonic acid sol in deionized water, adding ground potassium bitartrate crystal, heating and stirring for 0.5-1 hour to form a potassium antimony tartrate solution, carrying out vacuum concentration at 70-80 DEG C until a crystal precipitates, regulating the pH value of the solution to 5-7 with a potassium bitartrate solution, cooling to room temperature, precipitating the crystal, washing with anhydrous ethanol, and drying to obtain the high-purity white crystal product with the purity of 99.5%.

The invention discloses a synthesis method of 6-(4-methylpiperazine-1-yl)-4-o-tolyl nicotinamide, which comprises the following steps: (1) taking 6-chloronicotinonitrile as an initial raw material, carrying out nucleophilic addition reaction on the initial raw material and a reagent A in the presence of a boron trifluoride reagent, and after the reaction is completed, adding an oxidizing agent to carry out oxidation reaction to obtain a compound (II); the reagent A is o-tolyl magnesium halide or a combination of o-tolyl magnesium halide and lithium chloride; (2) condensing the compound (II) and N-methyl piperazine to generate a compound (III); (3) carrying out hydrolysis reaction on the compound (III) and hydrogen peroxide under the action of alkali to generate a compound (IV); the method is simple in reaction route, mild in reaction condition, high in product yield and suitable for industrial production.

The invention discloses a coumarin compound and a synthesis method thereof, relates to the field of organic compounds, and aims to provide a coumarin compound and a synthesis method thereof. The synthesis method disclosed by the invention is simple to operate, high in yield and mild in reaction condition, and according to the reaction, 7-hydroxycoumarin, 4-hydroxycoumarin and 7-hydroxy-4-methylcoumarin are respectively obtained by utilizing aldol condensation reaction of aldehyde, ketone and active methylene or active hydrogen compounds. The whole reaction process is safe and environment-friendly, low in cost and high in economic benefit, and belongs to a green chemical process. The method is applied to the field of coumarin synthesis.