56results about How to "Easy to refine and purify" patented technology

The invention relates to a pyrro-quinoline quinine (PQQ) sodium salt derivative and a preparation method thereof, belonging to the field of pharmacy. In the preparation method, PQQ is used as a raw material, and an acid-base neutralization reaction with PQQ is carried out in a basic solvent of sodium hydroxide to prepare the PQQ sodium salt derivative represented in the structural formula (I), wherein R1, R2 and R3 can be identical or different and respectively represents H, ammonium ion (NH3), potassium ion, sodium ion, magnesium ion, calcium ion or zinc ion, and at least one of R1, R2 and R3 is sodium ion. The invention has mild reaction conditions, easy product refining and purification, simple preparation steps and high yield more than 80%. The PQQ sodium salt derivative has the functions of inhibiting GSK-3 activity, reducing senile pigment formation in a transgenic mouse brain, reducing tau protein phosphorylation and the like. Thus, the PQQ sodium salt derivative can be medically used for treating senile dementia and other diseases.

The invention discloses a method for preparing high pure gold and enriching silver, platinum and palladium from silver anode mud. The process of separating silver with nitric acid, recycling silver, platinum and palladium with silver-enriched liquid, decomposing silver separating slag with aqua regia and preparing high pure gold with a one-time unsaturation reduction method is adopted and comprises the steps: leaching the silver anode mud with nitric acid to obtain separated silver, adding sodium chloride into the silver separating liquid to deposit the silver to obtain silver chloride sediment and silver depositing liquid, adding iron powder into the silver chloride sediment for replacement, returning the crude silver back to a Kaldo furnace for melting, and adding sodium hydrogen sulfite into the silver depositing liquid to reduce, deposit and recycle platinum and palladium; performing gold separating on the silver separating slag with aqua regia to obtain gold separating liquid and gold separating slag, performing the iron powder replacement step on the gold separating slag, adding the sodium hydrogen sulfite into the gold separating liquid to perform unsaturation reduction to obtain gold powder and gold depositing liquid, washing, drying and ingotting the gold powder to obtain a product gold ingot, and adding the sodium hydrogen sulfite into the gold depositing liquid to reduce and recycle the platinum and palladium for the second time to obtain the crude gold powder, and returning back to the previous steps. The method solves the problems of long leaching flow, high agent cost, complex operation, more devices and low recycle rate of the silver anode mud.

The invention discloses a preparation process of perfluoro-2-methyl-3-pentanone, belonging to the technical field of preparation methods of perfluoroketone compounds in the field of organofluorine chemistry. The perfluoro-2-methyl-3-pentanone is obtained by performing an epoxidation reaction and a catalytic isomerization reaction on perfluoro-2-methyl-pentene serving as a raw material in sequence. The preparation process comprises the following steps: I, in a continuous liquid phase epoxidation reaction, mixing a corresponding proportion of aprotic polar solvent into a sodium hypochlorite solution to promote the reaction, increase the raw material conversion ratio and increase the reaction rate at least by 2-3 percent, wherein the step is characterized by easiness and convenience in operation, low equipment requirement and high reaction equipment efficiency; II, performing a continuous gas phase catalytic reaction, wherein the application of a solvent is effectively avoided, the cost and environmental pollution are lowered, the problems of the need of separating the solvent from a product in post-treatment, difficulty in recycling and treating the solvent and a catalyst, and the like are solved, and the product can be refined and purified more easily. The preparation process has the advantages of high process automation degree, easiness and convenience in operation, high product purity and high reaction equipment efficiency, and is suitable for industrial application.

The invention relates to a kind of preparation method of tungsten hexafluoride gas, mix (F2) and high purity nitrogen(N2 ) with proportion of 1:0.5-20 and add them into pyrolysis device, warm-up temperature is 10-100 degree C, pressure is 0-0.6 MPa, time used is for 1min-20min,then add them into reactor where there is raw material of wolframium (W)of 5-15Kg, the reaction temperature of fluorine gas and raw material of wolframium is between 20 degree C and 400 degree C, the reaction time is for1min-20min, fluidify and collect tungsten hexafluoride gas made in the reaction by wipe low-boiling impurity such as fluorine gas, nitrogen and nitrogen trifluoride off, after collect WF6 gas of 10kg-50kg in the low temperature collector, stop collecting it and heat up to press WF6 into carboy for keeping, using pipe to connect pyrolysis device, reactor and low temperature collector. Purity of tungsten hexafluoride gas is up to more than 99.5%.

The invention relates to a method and a device for preparing sorbitol through continuous hydrogenation of glucose, and belongs to the technical field of hydrogenated production of sorbitol. A new process for producing the sorbitol through continuous flowing hydrogenation is provided, the key problems in continuity and upsizing of large-scale sorbitol production equipment are effectively solved, and the hydrogenation reaction is more safe, reliable and thorough; the method and the device are widely applied to production of biomass chemical alcohols, the method is superior to intermittent and semi-continuous methods in conventional processes, and the reaction efficiency is improved greatly; the method and the device are applied to production of the biomass chemical alcohols such as sorbitol,xylitol and mannitol.

The invention provides a continuous production process of perfluor-2-methyl-3-pentanone. The method specifically comprises the step of carrying out contact with reactants successively by taking hexafluoropropylene as a raw material to obtain a product, wherein the contact means that different materials in a reactor coexist with a time shorter than or equal to 600s. The continuous production process provided by the invention has the advantages of being cheap and easily available in raw material, simple to operate, high in degree of automation, high in synthetic yield, few in byproduct, short inreaction time and the like.

The invention relates to a method for producing ethylene and ethane and a catalytic reactor, belonging to the technical field of lower hydrocarbon. The method comprises the following steps of: carrying out first methane catalytic conversion reaction on a methane-rich feed gas and an oxidizing gas by using a first section of granular catalytic agent, carrying out second methane catalytic conversion reaction on the gas mixture entering a second integrated type catalytic agent reaction section after supplementing the oxidizing gas in a reaction gas mixture, and finally collecting a reaction product. A premixing chamber which is provided with a feed gas inlet and an oxidizing gas inlet is arranged at the top of the catalytic reactor; a first reactor in which a granular catalytic agent is placed is communicated with the lower end of the premixing chamber; an oxidizing gas replenisher is communicated with the first reactor; a second reactor in which an integral catalytic agent is placed is communicated with the oxidizing gas replenisher; and a product outlet is arranged at the lower end of the second reactor. The catalytic reactor has the advantages that the single-pass methane conversion rate of the methane catalytic conversion reaction is increased, the technological process is short, the operation is stable, and the equipment investment is few.

The invention relates to the technical field of 9, 9-bis(4-(2-hydroxyethoxy)phenyl)fluorene synthesis and especially relates to a method for preparing 9, 9-bis(4-(2-hydroxyethoxy)phenyl)fluorene from ethylene oxide. The method comprises that in the presence of a base, at a temperature of 30-80 DEG C, ethylene oxide and 9, 9-bis(4-hydroxyphenyl)fluorene undergo a reaction according to a mass ratio of 0.25: 1 to 0.35: 1 in a polar organic solvent. The preparation method adopts ethylene oxide and 9, 9-bis(4-hydroxyphenyl)fluorene as raw materials and a base as catalyst, and the reaction occurs at the normal temperature under the normal pressure so that a raw material cost is low. The preparation method does not produce waste gas and waste residues and has small pollution on the environment. The preparation method has the advantages of simple processes and low cost and is suitable for industrial production.

The invention relates to the technical field of medicine, in particular to a preparation method of Beraprost and its salt. The preparation method includes the steps of d), oxidizing a compound as shown in formula I-3 to prepare a compound as shown in formula IV, wherein the reaction equation is shown in the specification; e), and using IV compound as raw material to prepare the Beraprost or the salt of the Beraprost. The preparation method has the advantages that each reaction of the preparation process generates a single product, and the method is stable and controllable, environmentally friendly, good in yield, safe in process, and the like; the method is suitable for new drug research and development, capable of avoiding patent concentration, easy in refining and purification, easy in preparation and related impurity control, capable of optimizing a preparation process route and convenient to amplify.

The invention discloses preparation methods for acotiamide and hydrochloride thereof; 2[(2-hydroxy-4,5-dimethoxybenzoyl)amino]-1,3-thiazole-4-carboxylic acid methyl ester and N,N-diisoprylamino ethylamine are subjected to a reaction in a molten state to obtain N-[2-(diisopropylamino)ethyl]-2-(2-hydroxy-4,5-dimethoxybenzoyl)amino]-1,3-thiazole-4-carboxamide, and hydrochloric acid is dropwise added to N-[2-(diisopropylamino)ethyl]-2-(2-hydroxy-4,5-dimethoxybenzoyl)amino]-1,3-thiazole-4-carboxamide in methanol to prepare acotiamide hydrochloride trihydrate. The preparation methods reduce the use of toluene, and are economical and convenient, complete in reaction, and safe in process; at the same time, toluene residues in the final products and the amount of an impurity 2[(2-hydroxy-4,5-dimethoxybenzoyl)amino]-4-carboxyl-1,3-thiazole are reduced, and the product quality is improved; and the crude products are easy to refine and purify, and the reaction yield is high.

The invention discloses a preparation method of (2'R)-2'-deoxidation-2'-fluorine-2'-methylurea glucoside. According to the method, the (2'R)-2'-deoxidation-2'-fluorine-2'-methylurea glucoside is prepared by using 2-C-methyl-D ribotide-1,4-lactone as a starting material through the steps of silanization, fluorination, reduction, etherification, butt joint and hydrolysis reaction. The preparation method has the advantages that the route is simple and short; the use of highly toxic and harmful substances of barium chloride is avoided; the generation of a large number of solid wastes such as triphenylphosphine oxide is avoided; the acid of the catalytic amount is subjected to deprotection reaction; the use of a large amount of ammonia gas methyl alcohol for protecting group degreasing is avoided; the usage amount of dissolvent and the generation quantity of industrial wastes are reduced; the target product of alpha isomers can be recovered and used; the generation of solid wastes is reduced to the greatest degree. The total yield of the route is high; the intermediate is easily refined and purified; the preparation method is suitable for large-scale industrial production.

The invention discloses a dehydration control method for synthesis of bisphenol S, which is implemented by calculating a theoretical amount of dehydrated water according to a synthetic reaction equation of the bisphenol S and the feeding molar ratio of phenols and sulfuric acid; and controlling the early stage of the reaction to be in a rapid dehydration state and the late stage of the reaction to be in a slow dehydration state, wherein preferably, in one third of the dehydration process, 75-85% of water is dehydrated, and in the rest two thirds of the dehydration process, 25-15% of water is further dehydrated. The purity of the bisphenol S after being refined is 99.5% or over, and the chromaticity is less than 20 (platinum-cobalt colorimetric method). By controlling the dehydration speed in the process of bisphenol S synthesis, the excessive oxidation of phenols and phenolsulfonic acid can be avoided, and the purity of bisphenol S in a crude product can be improved. A synthetic bisphenol S crude-product is shallow in appearance color and low in chromaticity; and the purity of the bisphenol S crude-product is relatively high, so that the bisphenol S crude-product is easily further decolored, refined and purified.

The invention belongs to the technical field of organic matter preparation, and relates to a preparation method of high-light pure lactide. The high-light pure lactide is prepared by a one-stage or two-stage catalytic reaction, and the method comprises the following specific steps: with L-lactic acid as a raw material, adding 1,3-dimethyl-2-imidazolinone as a catalyst to prepare a lactic acid oligomer; and then directly adding sulfonylurea as a depolymerization catalyst, depolymerizing under high temperature and vacuum conditions, preparing crude lactide, and purifying the crude lactide to obtain high-light pure lactide. The total yield of lactide of the method reaches 86% or more, the melting point is 96.5 DEG C or more, and the optical purity of an isomer is 99.5% or more.

The invention discloses a treatment method for extracting gold from high-impurity silver anode slime. The treatment method mainly comprises the following steps: high-impurity silver anode slime is washed to remove soluble compounds; then base metals are removed through acid digestion; and after that, alkaline oxidation leaching, gold dissolution, reduction and washing are performed to obtain 99.99% gold dust. The treatment method is high in impurity removal rate, can comprehensively recover valuable metals and is reliable in process.

The invention relates to the technical field of organic chemistry and medicine, particularly to a gefitinib preparation method, and provides a gefitinib preparation method, wherein gefitinib is obtained from a compound represented by a formula I, and the preparation method of the compound represented by the formula I comprises: a nitration reaction, an oxidation reaction, a selective demethylationreaction, a reduction reaction, a cyclization reaction and a phenolic hydroxyl acetylation reaction. According to the present invention, the preparation method can simultaneously reduce the cost, easily achieve refining purification and easily prepare and control various related impurities, substantially optimizes the overall preparation process route, and is suitable for industrial scale production.

The invention discloses a removal method for purifying ethelene glycol monophenyl ether. A synthesized adsorption separation material is dispersed in ethelene glycol monophenyl ether, a content control technology of diethelene glycol monophenyl ether during the refining process in the conventional ethelene glycol monophenyl ether refining production process is improved, the technical problem of control of a trace of diethelene glycol monophenyl ether is solved, and the refining and purifying processes, through which the content of diethelene glycol monophenyl ether is lower than 800 ppm being difficult to achieve through common rectificating, become simple, convenient and easy. During the production and processing processes, the cost is low, the refining energy consumption is low, the removal method is suitable for ethelene glycol monophenyl ether production enterprises to use traditional equipment and traditional technical conditions, and a high-quality ethelene glycol monophenyl ether product is obtained.

This invention relates to technique of extract capsicine crystal from chili. The process as follows: use NaCl, NaHCO3, NaOH water solution and ethanol to compose modified ethanol solution; spray and leach capsicum stick layer from rotary infuser, the leaching solution contraflow to leach capsicum stick layer, transit spray - drip dry - spray - drip dry continuous countercurrent leaching, gain lixivium; condense the lixivium, use mobilizing agent composed by NaCl, sodium acetate and hydrochloric acid solution to blend, then use six number solvent oil to take circumfluence extraction, obtain capsicine crystal mother liquor, then takes controlled crystallization, gain high-purity capsicine crystal.

The invention relates to a new preparation method of 4-(1-piperazinyl)benzo[b]thiophene compound shown by a formula (2) or salt thereof, wherein R1 is a hydrogen atom or a protecting group. The method is realized in a way that the compound expressed by a formula (3) in which X1 is a leaving group reacts with the compound expressed by a formula (4) in which R1 is defined above or salt thereof to generate the compound expressed by the formula (2) or salt thereof in an inert solvent and under the effect of a certain amount of alkaline compounds. The method provided by the invention is safer and more environment-friendly since the use of usually adopted expensive palladium catalyst and complex is avoided.

The invention relates to a method for resolving curcumenol epoxy chirality isomer by ionic liquid. Quaternary ammonium salt type ionic liquid containing boron tetrafluoride or phosphorus hexafluoride anion is taken as resolving agent, the principle that complexes formed by two optically pure curcumenol epoxidation enantiomers with ionic liquid has obviously different solubility properties in the ionic liquid is utilized, the two complexes are conveniently separated, decomposition and purification are respectively carried out on the complexes, so as to respectively obtain two high quality and high enantiomeric excess (e. e%) optically pure curcumenol epoxidation enantiomers. The invention has simple post treatment, requires no conventional optically pure chirality compound to be taken as resolving agent, has low ionic liquid consumption, can recycle the ionic liquid and is applicable to mass production.

The invention relates to a method for preparing glycollic acid by glycol, which comprises a step of performing a reaction of glycol in the oxygen atmosphere under the condition of existence of solvent and catalysts, so as to prepare glycollic acid, wherein water is used as the solvent; V2O5 and Al2O3 are used as the catalysts; the adding weight ratio of glycol to water is 1.0:(4.0-8.0); the usingamounts of the catalysts take the amount of glycol as the reference; the using amount of V2O5 is in the range of 0.01 to 0.18 weight percent; the using amount of Al2O3 is in the range of 0.03 to 0.21weight percent; the reaction pressure is in the range of 0.20 to 0.50MPa; the reaction temperature is in the range of 120 to 155 DEG C; and the reaction time is in the range of 2.0 to 5.0 hours. The method has short process flow. The preparation of glycollic acid by glycol can be realized in one step. The used catalysts have low price and good effect. Both the conversion rate of glycol and the selectivity of glycollic acid are ideal. A reaction product is also easy to refine and purify, so that the high-purity glycollic acid product with high quality can be obtained.

The invention belongs to the field of zinc hydrometallurgy, and particularly discloses a method for efficiently recycling copper and cadmium from copper and cadmium slag. The method comprises the following step (1) of ball milling; the step (2) of thickener solid-liquid separation, the step (3) of leaching, the step (4) of removal of iron and germanium, the step (5) of preparation of metal copper,and the step (6) of replacement of metal cadmium. The method for efficiently recycling the copper and the cadmium from the copper and cadmium slag is short in process period and high in efficiency, and the purity of enriched copper and cadmium metal is very high.

The invention relates to a method for preparing chemical reference substances of niga-ichigoside F1 and suavissimoside R1 simultaneously. The method comprises the following steps of extracting crude extract from a rubus parvifolius L. medicinal material or adopting directly rubus parvifolius L. extract as a raw material, and carrying out high-efficiency purification through two processes of resin column separation and high speed counter current chromatography to obtain the chemical reference substances of niga-ichigoside F1 and suavissimoside R1, wherein purities of the chemical reference substances are above 98%. The method has the advantages of simple processes, high product purity and good adaptability for mass production.