46results about How to "Uniform crystal form" patented technology

The invention discloses a preparation method of cefepime hydrochloride, comprising the following steps of: reacting oxalyl chloride with 2-methoxyimino-2-(2-aminothiazole-4-yl) acetic acid hydrochloride to obtain a midbody I, i.e. 2-methoxyimino-2-(2-aminothiazole-4-yl) acetyl chloride hydrochloride; mixing silanized 7-aminoce-phalosporanic acid and silanized N-methylpyrrolidine, and reacting to obtain a midbody II, i.e. hydriodic acidification (6R, 7R)-7-amino-3-[(1-methyl-1-tetrahydro pyrrolidine) methyl]-3-cephem-4-formic betaine, in the presence of trimethyl idodine silicon hydride, isopropanol and an aqueous solution of hydrogen iodide; dissolving the midbody II into dichloromethane, sequentially adding trimethylchlorosilane and hexamethyldisilazane for reaction, and then adding the midbody I and triethylamine to react to prepare the cefepime hydrochloride. The cefepime hydrochloride prepared by the method has the advantages of uniform crystal form, good flowability and simple process and is suitable for industrialized production.

The invention discloses a preparing method for cubic CaCO3 and SiO2 composite particles. The preparing method includes the steps that nano calcium carbonate prepared through a carbonization method is used as a raw material, while calcium hydroxide is carbonized into calcium carbonate, surface modification is carried out by using sulfuric acid as a crystal form control agent, polyethylene glycol as a dispersing agent and silica sol as a surface modifier, the surface of calcium carbonate is coated with nano silica sol, and the cubic CaCO3 and SiO2 composite particles are prepared through one step. Compared with a traditional method, the preparing method adopts the one-step method and has the advantages of being short in time, high in efficiency, easy to operate, low in cost and the like. The obtained cubic CaCO3 and SiO2 composite particle product is uniform in size and crystal form, pure and free of impurities and is coated completely.

The invention relates to a synthesis method of cefpiramide sodium, including reacting of cefpriamide free acid with triethylamine, diethylamine or diethylamine in the organic solvent in -10-40 deg c, then getting mixture after reaction, dripping 10-15wt% sodium sulfocyanate acetone solution, adjusting pH to 6-8, filtering, drying to obtain cefpiramide sodium. The synthesis cefpiramide sodium has an even polytype, a good color, a high purity, and a good product stability and a safe conservation.

The invention discloses a preparation method of cefminox sodium, which comprises the following steps: 7 beta-bromoacetamide-7 alpha-methoxy-3-(1-methyl-1H-5-tetrazyl)sulfur methyl-3- cephem-4-carboxylic acid and D-cysteine hydrochloride are dissolved in water, the pH value is regulated to 6.0-7.0 by sodium bicarbonate, condensation reaction is carried out, and reaction products are post-treated to obtain the cefminox sodium. In the method, cefminox sodium raw material can be prepared through low-temperature reaction, a nonpolar macroporous resin X5 chromatography column is used for purification, ethanol-aqueous solution or anhydrous alcohol recrystallization and other simple operations are adopted to obtain target products, the yield and the purity of the target products are high, the products have uniform crystal forms and good fluidity, no special equipment is needed for the production, and the method is suitable for industrial production.

The invention provides a method for preparing recombinant human insulin crystal, and belongs to the technical field of protein crystallization. According to the method, zinc ions are subjected to three times of crystallization, the obtained insulin crystal is large in particle size and good in homogeneity, phenols or organic solvents used in normal methods are not used in the method, so that residues of harmful substances in the product are avoided and the quality of the insulin crystal is improved; moreover, the method is stable in preparation process and beneficial to industrial production.

The invention relates to a method for electrochemical synthesis of Cu3 (BTC) 2 and belongs to the field of preparation technologies of catalytic material and nanometer material. The method comprises the following steps: preparing a mixed solution of 1-butyl-3 methylimidazole bromide, trimesic acid, methyl alcohol and ethyl alcohol, adopting a copper electrode as an anode and a platinum electrode as a cathode, and adjusting the impressed voltage through a mixed solution of EDTA and DETA for electrolysis to obtain the Cu3 (BTC) 2 material. According to the invention, the adopted raw materials are cheap and easy to obtain, the operation is simple and easy, the preparation method is simple and easy to control, the equipment requirements are low, the environmental friendliness is achieved, and the Cu3 (BTC) 2 material is of a regular octahedron structure and has a diameter of 10-20 nm and a specific area of 950 m<2>g<-1>; the test conditions of the reaction are as follows: 500 ppm of NO, 500 ppm of NH3, 5% of O2, N2 as balance gas, the total flow of exhaust gas being 100ml/min, and the denitration catalytic efficiency reaching 100% at 230-280 DEG C.

The invention relates to a medicine composition without any excipients and a preparation process thereof; the invention carries out deep and careful research to the composition of sodium vedproate for injection and the preparation process, finally, the medical prescription, only containing effective ingredients: sodium vedproate and water, is determined. By adopting a plurality of critical processes in the adjusting and freeze-dry process, namely, in the pre-freezing step, the medicine composition is kept for a long time at the eutectic point of -2 degrees, so as to ensure a crystal nucleus to be big enough; vacuum pressure is adjusted in the steps of a first drying and a second drying, the action is repeated in a large-range vacuum degree with mass transferring and heat transmission principles. Under the condition that any excipients are not used, the appearance of the freeze-dry products and the compound dissolubility are remarkably improved, the freeze-dry time is obviously shortened, and the energy source is saved.

The invention discloses a preparation method of low-moisture and high-stability sterile cefuroxime sodium, which comprises the steps of (a) dissolving cefuroxime acid in an anhydrous mixed solvent, decolorizing, conducting sterile filtration, collecting filter liquor to a crystallizing tank, (b) dissolving soda in an organic solvent, decolorizing, conducting the sterile filtration, collecting filter liquor to a sodium solution metering tank, (c) controlling temperature for 10-50min, adding a soda solution into the crystallizing tank dropwise, controlling a stirring rate at 20-60r/min, crystallizing, adding acetone after the sterile filtration to ensure full crystallizing; (d) pressing crystallized liquid in a three-in-one multifunctional tank for filtration, washing with the mixed solvent, drying at 30-60 DEG C, obtaining the sterile cefuroxime sodium, and (e) transferring materials in a sterile bicone at 30-70 DEG C, continuing to dry under reduced pressure for 2-5h, and obtaining the sterile cefuroxime sodium with better stability and the moisture less than 1%. The preparation method is short in drying time and simple and practicable, the sterile cefuroxime sodium is easy to smash, low in moisture, less in solvent residual and stable in quality, the color, clarity and color points of the sterile cefuroxime sodium are not affected, and the production cost is lowered.

The invention relates to a production technology and application of calcium hydrophosphate. The production technology comprises the following steps of: by using an ammonium dibasic phosphate and a calcium chloride solution as raw materials, carrying out double liquid phases to obtain hydryoxyapetite by stirring at a certain temperature and flow rate, then dewatering through a belt filter to separate and washing a mother liquid till chloride ions reach 500PPM, thus obtaining hydryoxyapetite; adding a certain amount of deionized water to hydryoxyapetite, adjusting a slurry ratio to be in line with technological requirements, adding a certain amount of acid, carrying out high-temperature digestion after adjusting a pH value, observing the state of the slurry after raising the temperature to 90 DEG C, stopping heating when the slurry is expanded and solidified, and removing two crystal water after settling for 30 minutes, thereby obtaining calcium phosphate dibasic anhydrous; carrying out washing chlorine, dewatering, drying and sieving, thus obtaining the calcium hydrophosphate finished product. The production technology has the advantages that the synthetic technology is simple, raw materials are easily obtained, by-products can be recycled, and the environmental pollution is little.

The invention discloses a preparation method of high-purity solid hydroxylamine sulphate. The preparation method of the high-purity solid hydroxylamine sulphate comprises the following steps: adding a 5-15% hydroxylamine sulphate aqueous solution into a first reactor, mixing the hydroxylamine sulphate aqueous solution with 18-23% ammonia water, controlling the temperature of the first reactor to 20-30 DEG C, and regulating the pH value of the solution to 5.8-6.5, so that a first reaction product is obtained; fully mixing an extracting agent, a diluter and a stabilizer in a volume ratio of 1:(3-3.5):(0.001-0.002), putting the obtained mixture into a second reactor, regulating the pH value to 7.0-7.8 by adopting 18-23% ammonia water, and controlling the temperature of the second reactor to 20-30 DEG C, so that a second reaction product is obtained; carrying out extraction, concentration, cold crystallization, centrifugation and vacuum drying on the first reaction product and the second reaction product, so that the target product high-purity solid hydroxylamine sulphate is obtained. The preparation method of the high-purity solid hydroxylamine sulphate has the advantages of simple temperature, mild reaction conditions, high yield and low cost.

The invention belongs to the field of iron phosphate preparation, and particularly relates to an iron phosphate continuous dehydration and crystal form controllable system and a control method thereof. The system comprises a flash steaming dryer, a cyclone dust collector, a rotary kiln, a second cyclone dust collector and a packaging machine, which are arranged in sequence along a logistical direction; a hot air blower which is used for supplying air to the flash steaming dryer is arranged at one side of the flash steaming dryer; the hot air blower is communicated with the bottom of the flashsteaming dryer; a beater which is used for beating the hot air and forming cyclone in the flash steaming dryer is arranged at the bottom of the flash steaming dryer; a second beater is arranged between the cyclone dust collector and the rotary kiln; the rotary kiln is an external electric heating type rotary calcining kiln; and a flash dry bag filter which is used for collecting free water tail gas not dehydrated by the cyclone dust collector is arranged between the flash steaming dryer and the rotary kiln. The iron phosphate continuous dehydration and crystal form controllable system and thecontrol method thereof are small in investment, low in energy consumption and suitable for large-scale popularization and application.

The invention provides a method for crystallizing psicose from an ethanol solution. The method comprises the steps that a purified psicose solution is taken, and decompression concentration is carriedout to obtain a solution I; the concentrated solution I is heated, absolute ethyl alcohol is added, decompression concentration is carried out again, so that ethyl alcohol takes away the moisture inthe psicose solution to become an ethanol solution II of the psicose; the absolute ethyl alcohol is added into the concentrated solution II, heating is carried out until the psicose is completely dissolved, slow cooling is carried out, after crystals are separated out, slow cooling is carried out until crystals are no longer added, and a mixed liquor III is obtained; solid-liquid separation is carried out to on the mixed liquor III to obtain a solid IV and a clear liquid V; decompression drying is carried out on the solid IV to obtain psicose crystals; the clear liquid V continues to be concentrated, the above steps are repeated, and crystallization is carried out to obtain remaining psicose crystals. The method for crystallizing psicose from the ethanol solution has the advantages that through the cooling crystallization of the psicose in the ethanol solution, one-time crystallization ratio is high, the crystal forms of crystallization are uniform, the drying preservation and transportation are easy, the preparation process is safe and reliable, the process is simplified, the conventional operability of equipment is strong, and the material consumption is low.

The invention relates to a method and a device for continuously and stably preparing an acesulfame potassium crystal. The device comprises a decompressing evaporator, a heat exchanger, a crystal kettle, a scraper-type centrifugal machine and a mother liquor tank, wherein the decompressing evaporator is provided with the heat exchanger. The decompressing evaporator is communicated with the crystalkettle. The crystal kettle is communicated with the scraper-type centrifugal machine. The scraper-type centrifugal machine is communicated with the mother liquor tank. The mother liquor tank is communicated with the decompressing evaporator. The device for continuously and stably preparing the acesulfame potassium crystal is capable of solving a series of technical problems existing in an acesulfame potassium crystallization process that the process is tedious, multiple device crossings are existed, crystallization time is long, the crystal is non-uniform, quality is unstable and the like, andproviding a crystallizing device which is continuous in crystallization, uniform in crystal form, stable in technology quality, efficient in production, and high in industrialization degree, and capable of realizing remote control.

The invention discloses a method for preparing apigenin by utilizing biological enzymolysis. The method comprises the following steps of: S1, enzymolysis: adding rhoifolin and water or a lower alcohol solution into a reaction container, uniformly mixing, heating to 70 DEG C or above, preserving heat, cooling to 60 DEG C or below, adding acid to adjust the pH value, adding a compound enzyme for an enzymolysis reaction, detecting whether the rhoifolin is completely reacted or not, and heating to extinguish the compound enzyme after the enzymolysis reaction is completed to obtain a reaction solution, wherein the compound enzyme comprises rhamnosidase and glucosidase; S2, separation: filtering the reaction solution to obtain apigenin coarse crystals, mixing the apigenin coarse crystals with an alcohol solution, and stirring until the apigenin coarse crystals are completely dissolved to obtain a complex solution; and S3, purification: cooling and crystallizing the complex solution, and filtering to obtain the apigenin. According to the method for preparing the apigenin by utilizing the biological enzymolysis, the rhoifolin is hydrolyzed into the apigenin by adopting biological enzyme catalysis, so that the method is easy and convenient to operate, green, pollution-free and suitable for large-scale production.

The invention discloses a preparation method of rifapentine, and the steps are as follows: rifamycin S is used as a starting material for reacting with dihydroxy methyl tert-butyl amine in a first organic solvent to convert into intermediate rifaoxazine; a catalyst and a reductant are added into a second organic solvent for hydrolysis ring opening of the intermediate rifaoxazine; a rifapentine solution is obtained by condensation of a rifaoxazine hydrolysis product and 1-amino-4-cyclopentyl piperazine; and a rifapentine finished product is obtained by filtration, segmented crystallization at multistage crystallization temperature, first separation, washing, second separation, drying, soaking, third separation, drip washing, spin drying, sieving, drying, and powder mixing refining processes of the rifapentine solution. The preparation method adopts the reductant which can play a role in anti oxidation; different crystallization temperature is adopted in the segmented crystallization process; and by combination with the adding of a crystallization solvent, the crystalline polymorph is uniform, the particles are uniform, the stability is good, and the defects of high impurity content and nonuniform particles of rifapentine processes in the prior art can be solved.

The invention relates to a chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide or its salt and a preparation method thereof. The chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide is an important intermediate for preparing a hepatitis C-resistant drug Telaprevir. The preparation method utilizes D-tartaric acid as a resolving agent to resolve 3-amino-N-cyclopropyl-2-hydroxyalkanamide so that the chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide or its salt is obtained.

The invention provides a preparation method of high-purity calcium oxide. Calcium hydroxide is produced by using raw materials with extremely high calcium oxide content, the dispersity of calcium ionsis improved by using stearic acid and polyvinyl alcohol 124, and the crystal form and the particle size of the calcium ions are controlled so that calcium hydroxide solids are high in fineness and good in dispersity, and finally, calcium oxide with high purity and good dispersity is prepared through high-temperature calcination. Calcium hydroxide with good dispersity can be better and more uniformly calcined at high temperature so that the production efficiency is improved, the yield of waste gas CO2 is reduced, and the cost of subsequent treatment is reduced. The method is simple in process,safe, environmentally friendly and high in production efficiency, and the prepared calcium oxide product is high in purity and good in dispersity.

The invention relates to a ferrite hot-rolling process, and in particular to a production process for controlling metallographic structure formation in the ferrite hot-rolling process. The raw materials comprises according to percentage by mass: less than or equal to 0.06 percent of C,less than or equal to 0.10 percent of Si, less than or equal to 0.30 percent of Mn, less than or equal to 0.025 percent of P, less than or equal to 0.020 percent of S, less than or equal to 0.03 percent of Al, less than or equal to 0.05 percent of Cu, less than or equal to 0.05 percent of Cr, less than or equal to 0.05 percent of Ni and the balance of iron. The materials are sequentially smelted by a converter, a RH furnace and an LF furnace; and the material hot-rolling process can be carried out by a CSP orESP production line. By optimizing the proportion of the materials, a suitable process window is set according to the proportion of the materials in order to eliminate mixed crystal and caky structures in ferrite rolling and optimize the mechanical performance index of rolling.

Embodiments of the invention disclose a preparation method for an ultrafine calcium zincate crystal applied to a zinc battery. The preparation method comprises the following steps: (a) dissolving zincoxide in an alkaline solution to prepare an alkaline saturated zinc oxide solution; (b) adding a calcium silicate seed crystal having a particle size of 2000-8000 meshes into the alkaline saturated zinc oxide solution under stirring to obtain a mixed solution; (c) separately adding calcium hydroxide and zinc oxide in a molar ratio of 1: 2 into the mixed solution for a reaction under the conditionof continuous stirring; and (d) after the reaction is completed, performing suction filtration, washing and drying to obtain the ultrafine calcium zincate crystal. The calcium zincate crystal prepared by using the preparation method of the invention has a small and uniform particle size, a complete crystal form and a high purity, and can effectively inhibit battery deformation and zinc dendrite formation when added to a zinc-nickel battery as a negative electrode material of the battery. The preparation method is short in reaction time, does not require long-time aging, saves energy consumption, and has high labor productivity.