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

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 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 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 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 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 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 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 present invention relates to the field of pharmaceutical technology, in particular to a sevelamer carbonate analogue and its preparation method and application, wherein the preparation method of the sevelamer carbonate analogue is: firstly prepare allylamine hydrochloride into allylamine carbonate Salt; Allylamine carbonate and diallylamine-epichlorohydrin conjugates are polymerized under the conditions of a polymerization initiator to generate carbonic acid sevelamer analogues. The prepared sevelamer carbonate analogue can be used to prepare phosphate ion adsorbent. The present invention solves the problem of many wastes and high waste rate in the synthesis process of sevelamer carbonate in the prior art, and the structure of the sevelamer carbonate analog provided is similar to that of sevelamer carbonate, retaining Vilam has the property of adsorbing phosphorus, and the preparation process is simple and environmentally friendly.

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 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 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 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 light-colored catechol lignosulfonate sunscreen microcapsule and its preparation and application. The invention adopts vulcanization method to modify lignosulfonate to prepare catechol lignosulfonate, and then carries out ultrasonic cavitation to catechol lignosulfonate, sunscreen agent and surfactant to prepare catechol lignosulfonate Diphenol lignosulfonate / chemical sunscreen microencapsulated emulsion. The preparation process of the lignin / chemical sunscreen microcapsules in the present invention is green and environmentally friendly, with low cost and excellent ultraviolet absorption performance. Traditional sunscreens have problems such as poor water resistance, high pollution in the preparation process, and easy penetration into the skin to harm the human body.

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 discloses a method for deeply removing antimony-copper impurities in regenerated crude tin. The antimony-copper removing agent mainly adopts borax and tin sulfide, is easy to operate, reduces the removal temperature at the same time, has low energy consumption, good impurity separation effect, and is safe. It is environmentally friendly, and removes antimony copper at the same time, and the quality of coarse tin reaches AA grade Sn99.90, which meets the requirements of GB / T728‑2010. The impurity Sb content is less than 0.02wt%, and the impurity Cu content is less than 0.008wt%. The problem of environmental pollution existing in the existing technology of adding aluminum to remove antimony and adding sulfur to remove copper solves the problems of cumbersome steps and high energy consumption for removing antimony and copper in the prior art.

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%.