447results about How to "Suitable for industrial scale-up production" patented technology

The invention belongs to the technical field of mesoporous composite materials, and particularly relates to a three-dimensional interconnected hierarchical-structured zeolite molecular sieve material and a preparation method thereof. The method comprises the following steps of: self-assembling anionic and cationic surfactants, serving as primary constitutional units, in solution phase to form a secondary constitutional unit; self-assembling in solution to be compounded into amphipathic block copolymer; then, self-assembling in the solution by taking the amphipathic block copolymer as a template agent and by using a structural guide agent and inorganic silicon to obtain a silicon dioxide/surfactant/template agent composite material; and finally, calcining to remove the surfactant and the template agent to obtain the hierarchical-structured mesoporous zeolite molecular sieve material consisting of interconnected mesopores, micropores and macropores. The material has higher specific surface area and stronger hydrothermal stability, and has a broad application prospect in the aspects of petrochemical industry, heavy oil catalysis cracking, biological separation, adsorption and the like. The material obtained in the invention has the advantages of superior performance, simple synthesis method and readily available raw material and is suitable for industrial production.

The invention discloses a method for preparing a high-performance Silicalite-1 molecular sieve membrane, which comprises the following steps: using cheap TPABr and silica sol as raw materials for preparing a high-activity Silicalite-1 molecular sieve crystal; using the crystal as a seed crystal to be loaded on the outer surface of a supporting body, and carrying out the high-temperature hydrothermal crystallization in the diluted synthetic liquid using TPABr as the template agent to obtain the high-performance Silicalite-1 molecular sieve membrane. The invention is characterized by adopting asecondary growth hydrothermal method and carrying out the high-temperature (180-210 DEG C) hydrothermal one-step synthesis of the diluted synthetic liquid using TPABr as the template agent (300-750 ofH2O/SiO2, 0.1-0.5 of TPABr/SiO2, and 0.1-0.5 of NaOH/SiO2) on the surface of a porous tubular mullite carrier to form the high-performance Silicalite-1 molecular sieve membrane. The method not only effectively uses the cheap TPABr to replace TPAOH to prepare the molecular sieve membrane, but also greatly reduces the demand quantity of the silicon source and the template agent in the membrane synthetic liquid, thereby greatly reducing the membrane preparing cost. By applying the prepared Silicalite-1 molecular sieve membrane to a pervaporation test in a 60 DEG C ethanol/water (5/95 wt %) mixedsystem, the permeation flux and the separation factor can reach 1.71kg/m<2>.h and 66 respectively. The invention obviously improves the permeation flux and the selectivity of the Silicalite-1 molecular sieve membrane, reduces the production cost and is suitable for industrial production.

The invention discloses a method for producing pyrroloquinoline quinine through microbial fermentation and a fermentation medium used in the method for producing the pyrroloquinoline quinine through the microbial fermentation. An oxygen control fermentation culture method is used for culturing methylotrophic bacteria, a carbon source contained in the fermentation medium is methyl alcohol, and a nitrogen source contained in the fermentation medium is ammonium sulfate, a dissolved oxygen level is controlled by stages to be 30%-50% of saturated dissolved oxygen in the fermentation process, pH is controlled to be 5.5-6.0 through fed-batch, the fed-batch is achieved through a pH-nitrogen source joint control technology, the methylotrophic bacteria are cultured for six days in a 7.5L fermentation tank, and eventually the cell density (OD 600) exceeds 10, yield of PQQ reaches 2g/L, and production intensity of the PQQ is 333.33mg/L/day. The method for producing the pyrroloquinoline quinine through the microbial fermentation is simple in operation, automatic control and continuous fermentation can be achieved easily, and a solid foundation for industrially producing the pyrroloquinoline quinine through the methylotrophic bacteria is laid.

The invention discloses a preparation method of LCZ696 intermediate and relates to the technical field of preparation of an aromatic nucleus compound containing 2 benzene rings and 1 chiral center. The preparation method includes the steps of S1, allowing benzyl magnesium bromide to react with methyl oxalyl chloride to obtain a compound as shown in formula I; S2, allowing the compound as shown in formula I to have a bromination reaction with a bromination reagent to generate a compound as shown in formula II; S3, coupling the compound as shown in formula II with phenylboronic acid to obtain a compound as shown in formula III; S4, performing reductive ammoniation on the compound as shown in formula III to obtain a compound as shown in formula IV; S5, applying Boc to the compound as shown in formula IV to obtain a compound as shown in formula V; S6, performing ester group reduction on the compound as shown in formula V to obtain a compound as shown in formula VI. The preparation method has the advantages that overall raw material consumption is lowered, and product productivity and market competiveness are increased; by the overall process optimization, the reaction of each step can be performed and controlled easily, the use of heavy metal catalysts is reduced and avoided, and accordingly the quality index of the final product is increased, and an economic and environment-friendly process route is developed.

The invention discloses a preparation method of carboxyl silicone oil. Undecylenic acid and methyl hydrogen dichlorosilane are taken as raw materials to be subjected to direct hydrosilylation in the presence of a platinum/carbon catalyst to obtain 11-carboxyl undecyl methyl dichlorosilane; and the carboxyl silane monomer 11-carboxyl undecyl methyl dichlorosilane and dimethyldichlorosilane are subjected to co-hydrolysis and equilibrium polycondensation to obtain 11-carboxyl undecyl methyl silicone oil. The preparation method has the following advantages: the preparation process of carboxyl silicone oil is simplified by adopting the method for preparing the carboxyl silane monomer by one step through the direct addition reaction; the raw materials adopted for synthesis are industrial raw materials and are suitable for industrial large-scale production; and after being prepared into emulsion and compounded with amino silicone oil emulsion, the prepared carboxyl silicone oil can provide very good softness and full hand feel when being applied to textile finishing.

The invention discloses a cerium zirconium aluminum composite oxide oxygen storage material and a preparation method thereof. According to the cerium zirconium aluminum composite oxide oxygen storage material, the particle size is 5 to 10 nm; the BET specific surface area is 200 to 240 m<2>/g; the pore volume is 0.50 to 0.70 cm<3>/g; the average pore size is 5 to 10 nm; a cerium zirconium solid solution has a stable cubic fluorite structure. The cerium zirconium aluminum composite oxide oxygen storage material provided by the invention has the characteristics of stable structure, large specific surface area, excellent oxygen storage performance and excellent anti-ageing performance. The preparation method provided by the invention has the advantages of easily accessible raw materials and low production cost, and is suitable for industrialized amplification production.

The invention relates to a preparation method and a refining method of medical hemostatic polysaccharide starch. With pretreated potato starch as a raw material and epichlorohydrin as a crosslinking agent, a microsphere adopting a three-dimensional network structure is synthesized by an emulsifying and crosslinking technology. The medical hemostatic polysaccharide starch is high in biocompatibility; the medical hemostatic polysaccharide starch is full with wrinkles on the surface, so that the particle surface area is increased, the water absorbing rate is significantly improved and the hemostatic time is greatly reduced; the medical hemostatic polysaccharide starch is especially applicable to large-area blood seepage, deep bleeding, and bleeding at a part difficult to reach by operative procedures.

The invention discloses a method for synthesizing mirabegron, relates to a method for preparing mirabegron, and aims at solving the problems that the existing method for synthesizing the mirabegron is not friendly to environment, more in reaction steps, low in yield, and complicated in post-treatment, and cannot be amplified to produce. The method disclosed by the invention comprises the following steps: 1, carrying out ring-opening reaction by taking p-nitrophenylethylamine and (R)-phenylethylene oxide as initial raw materials; 2, carrying out reduction reaction; 3 carrying out condensation reaction. The method disclosed by the invention is cheap and available in selected raw materials, high in yield, low in cost, friendly to environment and applicable to industrial amplifying production. The method is applied to synthesis of the mirabegron.

The invention relates to a zinc oxide based normal-temperature deep desulfurizing agent as well as a preparation method and application thereof. During preparation, a mixed solution of a zinc salt, an aluminum salt and an aid metallic salt is subjected to a one-step coprecipitation reaction to form a compound precipitate; the compound precipitate is subjected to aging, drying and roasting to obtain the zinc oxide based normal-temperature deep compound desulfurizing agent. The prepared zinc oxide based normal-temperature deep desulfurizing agent is used for the normal-temperature deep removal of H2S in various gaseous and liquid materials in the field of petroleum and coal chemical industries; that is, the fixed-bed operation is adopted; in conditions that a reaction temperature is 20 to 60 DEG C and operation pressure is 0.1MPa to 5MPa, the volume space velocity of liquid is controlled to be 1h<-1> to 12h<-1> or a gas-phase space velocity is controlled to be 1,000h<-1> to 30,000h<-1>; the H2s of which the content is 1ppm to 1,000ppm in a to-be-treated material is removed until the content is not more than 0.03ppm. Compared with the prior art, the desulfurizing agent prepared by the preparation method has breakthrough sulfur capacity, which reaches 26.1 percent, at a normal temperature and desulfurization precision which reaches 0.03ppm or below; the preparation method is simple, and can be used for large-scale industrialized production.

The invention provides an enzymatic pretreatment assisted curcumin extraction technology. The enzymatic pretreatment assisted curcumin extraction technology comprises steps as follows: after 1 part of curcuma powder is taken, ground, sieved, added with water and stirred uniformly, the mixture is subjected to water bath for 60 min and is cooled to the constant temperature of 52-58 DEG C, and curcuma pulp is obtained; compound enzyme comprising cellulase, amylase and papain is added to the curcuma pulp and reacts for 2-4 h, and enzymatic hydrolysate is obtained; the enzymatic hydrolysate is taken, added with an ethanol solution and homogenized for 1-2 min under the condition of 8,000-9,000 r/min, and a curcumin extracting solution is obtained; finally, a flocculant is added to the extracting solution, the mixture is stirred and filtered, a clear liquid flows through an activated carbon chromatographic column and is eluted with an alkaline solution, and a curcumin desorbed solution is obtained. The technology has the advantages of high extraction speed, low temperature, low energy consumption, high yield of the effective component curcumin, stable product quality and controllable reaction conditions, and is applicable to industrial large-scale production.

The invention provides a method for synthesizing a nano three-way catalyst and belongs to the technical field of a catalyst preparation process. The method takes a metal organic salt and a commercial carrier as raw materials and comprises the following steps: reacting in a solvent at 60-300 DEG C for 1-720 minutes; and controlling experimental parameters including a mol ratio of reactants, the concentration of the reactants, a reducing agent, a reaction temperature and the like to form the nano three-way catalyst which is formed in series and has controllable structure, shape and size. The method provided by the invention has the advantages that the raw materials are cheap and easy to obtain, time for a reaction is short, the solvent can be repeatedly utilized, the equipment is simple, and the method is easy to realize and control, has good process repeatability and stable product quality, is safe and reliable to operate, and is suitable for industrial large-scale production.

The invention relates to the technical field of small-molecule chemical drug, and particularly relates to a preparation method of a crizotinib intermediate. The preparation method comprises: (1) synthesizing a compound 3 from a compound 1 and a compound 2 by flow chemistry; (2) synthesizing the crizotinib intermediate I from the compound 3 obtained in the step (1) and a boric acid ester compound 4 by flow chemistry. The preparation method of the crizotinib intermediate, which is provided by the invention, is high in yield, can greatly reduce energy consumption and cost in the preparation process of crizotinib, is environmental-friendly, is high in safety and high in automation degree, and is suitable for industrial amplification production. A reaction route is as follows: (with reference to the specification), wherein Y represents a leaving group, Z represents an amino protection group, and X is selected from F, Cl, Br and I.

The invention belongs to the technical field of waste battery treatment, and particularly discloses a waste lithium ion battery recovery method. A to-be-recovered raw material containing a waste positive electrode active material and an auxiliary agent are roasted at 500-800 DEG C, and then water extraction treatment is performed; and the auxiliary agent is at least one of NaHSO4, KHSO4, CoSO4, NiSO4, MnSO4, NH4HSO4 and (NH4)2SO4. The method overcomes the disadvantages of a traditional recovery method, is simple, practical and economically feasible, realizes comprehensive utilization of wastelithium ion batteries, and is suitable for industrial production.

The invention discloses a method for synthesizing ultrathin molybdenum disulfide nanocrystals and belongs to the technical field of inorganic material preparation processes. According to the method, a molybdenum-containing inorganic salt and a sulfur-containing compound or sulfur powder are used as raw materials and have a reaction at the temperature of 160-300 DEG C for 30-120 min in a long-chain amine solvent and a long-chain fatty acid surfactant, experiment parameters such as the reactant molar ratio, the reactant concentration, the reaction temperature, the reaction time and the like are controlled, molybdenum disulfide nanocrystals which are well crystallized and have a few atomic layers (1-5 layers) are formed and can be well dispersed in a nonpolar solvent or base oil, and stable lubricating oil is formed. According to the method, raw materials are cheap and easy to obtain, the reaction time is short, the yield is high, instruments and equipment are simple, operation is convenient, safe and reliable, process repeatability is good, product quality is stable, and the method is suitable for industrial enlarged production.

The present invention discloses a preparation method and application of a fatty dioic acid derivative. The method is as below: first reacting long-chain fatty dioic acid with thionyl chloride to obtain acyl chloride; reacting acyl chloride with t-butanol and removing chlorine group to obtain long-chain tert-butyl fatty dioic acid; then reacting the tert-butyl fatty dioic acid with N-hydroxy succinimide to obtain long-chain fatty dioic acid succinimidyl tert-butyl ester; reacting long-chain fatty dioic acid succinimidyl tert-butyl ester with L- glutamic acid-1-t-butyl ester to obtain tert-butyl long-chain aliphatic diacyl-L-Glu-OtBu; then reacting tert-butyl long-chain aliphatic diacyl-L-Glu-OtBu with N-hydroxysuccinimide to obtain tert-butyl long-chain aliphatic diacyl-L-Glu(OSu)-OtBu; and finally, removing the fatty dioic acid derivative in the tert-butyl long-chain aliphatic diacyl-L-Glu(OSu)-OtBu to obtain long-chain fatty dioic acid derivative. The method has the advantages of simple route operation, controllable quality, suitability for industrial scale production, low cost, simple purification, and is applicable to the preparation of high purity insulin analogues.

The invention relates to a ruthenium carbene complex, a preparation method and an application thereof. The chemical formula of the ruthenium carbene complex is shown as formula (I), wherein X is selected from trifluoromethyl, nitryl, dimethylamino or cyanogroup. In a preparation process, firstly, chloromethyl benzene ligand reacts with zinc alkyls so as to synthesize a chloromethyl benzene-zinc alkyls compound, and then the chloromethyl benzene-zinc alkyls compound reacts with tris (triphenylphosphine) ruthenium chloride and tricyclohexylphosphine in turn so as to acquire a catalyst precursor, and lastly, the catalyst precursor and N-heterocyclic carbene are subjected to ligand replacement. The prepared ruthenium carbene complex is used as a catalyst for catalyzing the olefin metathesis. Compared with the prior art, the ruthenium carbene complex provided by the invention has the advantages of convenience in preparation, property stability and capability of effectively catalyzing the olefin metathesis. The preparation method is characterized by simple operation, technology stability, controllability, environment-friendly effect, high yield, suitability for industrial amplification production and wide application prospect.

The invention relates to a method for synthesizing organic compounds, in particular to a process method for synthesizing 4-site heteroatom-substituted cyclohexenyl halide. The method comprises the following steps of: performing refluxing reaction on 4-site heteroatom-substituted cyclohexanone (1) and 1 to 50 equivalents of anhydrous hydrazine or hydrazine hydrate in a solvent at the temperature of -20 DEG C; filtering or spin-drying the solvent to obtain corresponding hydrazone; reacting the hydrazone with a CuX2/alkali mixture in an alcohol solvent at the temperature of between -20 and 40 DEG C; adding aqueous alkali and a solvent after the reaction; performing separation to obtain mixed solution; adding organic alkali and performing the refluxing reaction; adding 1N acid to remove excessive alkali; adding saturated NaHSO3 to react; and removing the solvent to obtain the 4-site heteroatom-substituted cyclohexenyl halide (3). The method has the advantages of original and simple synthesis process and mild process condition, is easy and convenient to operate, avoids super-low temperature reaction and column chromatography purification involved in literatures, and is suitable for industrial scale-up production.

The present invention provides one kind of slow released dry azithromycin suspension and its preparation process. The medicine of the present invention has slow released azithromycin microsphere prepared through spray drying process, and capsule wall material for coating azithromycin medicine made of viscous medicinal polymer material or insoluble medicine polymer material, such as acrylic polymer, gelatin, Arabic gum, carboxymethyl cellulose salt, etc. and preferably of acrylic polymer. The slow released dry azithromycin suspension has improved administration compliance and convenience, and high bioavailability.

The invention belongs to the technical field of medicine, and relates to a preparation method of iron-protein succinylate with a high iron content. The preparation method comprises the following steps: (1) acylation: adding succinic anhydride into a casein solution to carry out reactions, continuously adding a sodium hydroxide solution into the reaction system to keep the pH value in a range of 6 to 9, after the reaction, adding acid into the reaction liquid to adjust the pH value to a range of 1 to 4, and filtering to obtain precipitate; (2) iron loading: dispersing the obtained precipitate into water, adding a proper amount of sodium hydroxide solution, stirring to dissolve the precipitate, then adding a ferric trichloride solution containing sodium bicarbonate into the obtained protein succinylate solution, adding a sodium hydroxide solution simultaneously to maintain the pH value of the reaction liquid in a range of 6 to 9, after the reaction filtering to remove the insoluble substances so as to obtain a iron-protein succinylate solution; refining the solution to remove the insoluble substance, adding acid to generate precipitate, filtering to obtain the precipitate, washing the precipitate by water, and finally drying the precipitate. In the recent literature, the reported iron content of iron-protein succinylate is in a range of 4.5 to 10%, while the iron content of iron-protein succinylate prepared by the provided method is as high as 15%. Moreover, the provided preparation method has the advantages of simple technology, good product solubility, and stable product quality.