12results about How to "High crystal purity" patented technology

The invention belongs to the field of pharmaceutical chemical industry, and particularly relates to a crystal form of acetylated empagliflozin and a preparation method thereof, the synthesis route is # imgabs0 #, and the preparation method comprises the following steps: (1) stirring and dissolving a compound II, a solvent, triethylamine and DMAP, then dropwise adding acetic anhydride into the system, reacting after dropwise adding, controlling the compound II to be less than or equal to 1.0% by HPLC (High Performance Liquid Chromatography), and performing post-treatment to obtain a crude product; (2) adding the crude product into an alcohol solvent, heating to 60-90 DEG C, dissolving until clarification, slowly cooling to 15-40 DEG C, keeping the temperature, stirring, and centrifuging to obtain a primary refined product; and repeating the operation once by using the alcohol solvent, and carrying out vacuum drying to obtain the compound I. The method has the advantages of simple and controllable process operation, good reproducibility, easy realization of industrial production, efficiency improvement and production cost reduction. The acetylated empagliflozin crystal form obtained by the invention is high in purity and good in stability, and has important significance for ensuring that the quality of acetylated empagliflozin meets the medicinal requirements.

The invention discloses a crystal form of a compound as well as a preparation method and application thereof, the compound has a structure as shown in a formula I. The crystal form has higher crystal purity, lower hygroscopicity, better solid stability and better solubility, is beneficial to preparation and storage of pharmaceutical preparations, and has very good application value and patent medicine prospect. Besides, clinical test results show that the crystal form B of the compound as shown in the formula I has very good pharmacokinetic characteristics, low clinical toxicity, better safety and high oral bioavailability, and has a good treatment effect on various diseases.

The invention relates to the technical field of aluminum chloride, in particular to an anhydrous aluminum trichloride production system which comprises a reaction unit, a feeding unit, a heat exchange unit, a buffer unit and a crystallization unit, the heat exchange unit comprises a heat exchange shell and a plurality of heat exchange pipes, and the bottom wall of the heat exchange shell gradually inclines upwards in the direction away from a chlorination furnace; the buffer unit is used for buffering the aluminum trichloride and the fused salt carried by the aluminum trichloride so as to separate the fused salt from the aluminum trichloride; the feeding unit is used for feeding the chlorination furnace, generated aluminum trichloride sequentially passes through the heat exchange unit and the buffer unit and then enters the crystallization unit to form crystals, so that a set of complete and continuous production system is formed, and meanwhile, most fused salt can flow back to the chlorination furnace along the obliquely arranged heat exchange shell in the cooling process of the aluminum trichloride; and the residual molten salt is left in the buffer unit after being buffered and cooled by the buffer unit, so that most or even all of the molten salt carried in the aluminum trichloride gas can be removed, and the crystallization purity of aluminum trichloride is improved.

The invention provides a sludge total reduction and resourceful treatment process based on an ultrasonic technology. The method comprises the following steps: wastewater enters a secondary sedimentation tank after biological treatment, part of sludge flows back, and the rest of sludge is concentrated; 30% of concentrated sludge is taken out from the gravity concentration tank, nano bubbles with the volume ratio of 10% are introduced, ultrasonic cell dissolving treatment is conducted, the treated sludge flows back to the biological treatment device, and in-situ reduction is achieved; carrying out ultrasonic pretreatment and low-frequency pulse micro-current disintegration treatment on the residual 70% of concentrated sludge, enabling the treated sludge to enter an aerated grit chamber, discharging clean sand, and carrying out advection precipitation on the sludge to generate carbon-rich sludge; mgO2 is added into the supernate to form struvite crystals, the struvite crystals are recycled, and the carbon-rich supernate and the carbon-rich sludge are combined to serve as endogenous carbon. According to the method, in-situ reduction of the sludge is efficiently realized; comprehensive resource utilization is realized, nitrogen and phosphorus are recycled to generate struvite, and meanwhile, carbon-rich supernate and carbon-rich sludge are combined to serve as endogenous carbon.

The invention relates to a preparation method of an electronic grade caustic alkali solution, the mass fraction of the caustic alkali solution is 40-50%, and the content of transition metal ions is less than 5 ppb. The invention aims to provide the preparation method of the caustic alkali solution suitable for cleaning / etching the silicon wafer, the problem that transition metal ion impurities are easy to remain after the silicon wafer is cleaned / etched is solved, and the transition metal impurities in the caustic alkali solution are deeply removed mainly through a cooling crystallization process controlled by an additive. Compared with a mode of directly carrying out cooling crystallization and directly adding a chelating agent into the caustic alkali solution, the method provided by the invention fundamentally solves the problem that the content of transition metal impurities in the caustic alkali solution for cleaning the silicon wafer is too high, so that the silicon wafer is polluted.

The invention discloses a triazole iron-based spin cross complex, which has the following chemical expression: [FeL2]X2; the invention also discloses a method for preparing the triazole iron-based spin cross complex: step 1, synthesizing ligand L by 2-cyano-6-(1-pyrazole)pyridine or 6-cyano-2,2'-bipyridine and hydrazide; step 2, reacting ligand L with ferrous salt in acetonitrile to obtain a reaction solution; step 3, placing the reaction solution in a closed container with ether and standing to precipitate crystals. The complex of the invention has a clear crystal structure and variable temperature magnetic susceptibility data, and the ligand field of the spin center can be adjusted by adjusting the terminal coordination point of the ligand L, and then the spin state of Fe(II) can be adjusted; by changing the substituent and counter anion on the ligand L to adjust the spin cross property of the complex, it has potential application value in the technical fields of high-density information storage and molecular switch devices.

The invention discloses an electronic-grade hydrofluoric acid in-situ recycling device, and belongs to the field of wet electronic chemicals. The device comprises a reactor body, and a rotational flow liquid mixer and a circulating guide cylinder are arranged in the reactor body; a backflow cavity is formed in the lower end of the reactor body, a returned material screening device is arranged on the upper portion of the backflow cavity, a circulating pump is arranged on the outer side of the reactor body and located at the backflow cavity, a first connecting pipe and a second connecting pipe are connected to the circulating pump, the first connecting pipe is communicated with the backflow cavity, and the second connecting pipe is communicated with the rotational flow liquid mixer. Two materials are mixed in a diagonal rotational flow mode through the rotational flow liquid mixer, the problem of local supersaturation is avoided, the returned material screener is arranged at the bottom of the reactor body, crystals and fluid mixed liquid are distributed in an umbrella shape at an inlet of a circulating fluidization area due to the arrangement of a returned material cone, and the crystallization effect is improved. And meanwhile, pores formed in the screening plate can be used for carrying out particle screening on the seed crystals, so that the sizes of the seed crystals entering the circulating fluidization area are homogenized.

The invention discloses a triazole iron-based spin crossover complex. The triazole iron-based spin crossover complex has the following chemical expression formula: [FeL2] X2, the invention also discloses a preparation method of the triazole iron-based spin crossover complex, which comprises the following steps: step 1, synthesizing a ligand L from 2-cyano-6-(1-pyrazole) pyridine or 6-cyano-2, 2 '-bipyridine and hydrazide; 2, reacting the ligand L with ferrite in acetonitrile to obtain a reaction solution; and 3, placing the reaction liquid in a closed container with diethyl ether, standing, and separating out crystals. The complex disclosed by the invention has a clear crystal structure and variable temperature magnetic susceptibility data, and a ligand field of a spin center can be adjusted by adjusting a coordination site at an L end position of a ligand, so that the spin state of Fe (II) can be adjusted; the spin crossover property of the complex is adjusted by changing substituent groups and counter anions on the ligand L. The complex has potential application value in the technical field of high-density information storage and molecular switch devices.

The invention discloses a method for improving the crystal purity of struvite in the process of treating landfill leachate, and belongs to the field of environmental engineering technology. The steps of the method for improving the crystal purity of struvite in the process of treating landfill leachate include: homogenizing the landfill leachate and performing anaerobic digestion pretreatment, injecting the gas generated during the anaerobic digestion pretreatment into the landfill leachate after the anaerobic digestion pretreatment to perform a metal passivation reaction, adjusting the pH of the landfill leachate after the metal passivation reaction to 9-11, adding a magnesium source to perform a struvite crystallization reaction, and generating struvite crystals. Through the method provided by the invention, the crystal purity of the recovered struvite can reach more than 90%.

The utility model relates to sodium sulfate processing technical field, concretely is a kind of sodium sulfate evaporation crystallization environmental protection type separator, including main separator, the inside of main separator is equipped with shunt component, shunt component includes the multiple shunt pipes of being set in the inside of main separator, the upper and lower ends of multiple shunt pipes are fixedly installed with baffle, the inner wall of multiple shunt pipes is equipped with the guide component for prompting liquid to form cyclone in shunt pipe inside, and the adjusting component for controlling multiple guide components is arranged on main separator in shunt pipe inside deformation and cleaning its inner wall;By setting guide component and adjusting component, reached the effect that can let sodium sulfate solution form cyclone in shunt pipe, cyclone motion increases the contact area of sodium sulfate solution and pipe wall, while centrifugal force promotes crystallization particle to gather and settle to pipe wall, improves crystallization purity, and can control the effect that helical elastic piece realizes automatic cleaning dirt, maintains heat transfer efficiency.

The invention discloses a crystal form of a compound as well as a preparation method and application thereof, the compound has a structure as shown in a formula I. The crystal form has higher crystal purity, lower hygroscopicity, better solid stability and better solubility, is beneficial to preparation and storage of pharmaceutical preparations, and has very good application value and patent medicine prospect. Besides, clinical test results show that the crystal form A of the compound as shown in the formula I has very good pharmacokinetic characteristics, low clinical toxicity, better safety and high oral bioavailability, and has a good treatment effect on various diseases.

The invention provides a preparation method of a germanium triphosphide nanosheet, and belongs to the technical field of electrode material preparation. The preparation method comprises the following steps: step 1), pre-pressing mixed powder formed by red phosphorus powder and germanium powder to obtain a pre-pressed body; (2) carrying out high-temperature and high-pressure sintering on the pre-pressed body prepared in the step (1) to obtain bulk-phase germanium triphosphide; (3) taking the bulk-phase germanium triphosphide prepared in the step (2) as an electrode, and putting the bulk-phase germanium triphosphide into an electrolytic tank; 4) applying voltage or current to the electrode in the step 3) to perform intercalation dissociation on the germanium triphosphide; and (5) centrifuging the electrolyte subjected to electrochemical dissociation in the step (4), and collecting supernate to obtain the germanium triphosphide nanosheet. A large number of high-purity micron-sized germanium triphosphide nanosheets are prepared by combining a high-temperature and high-pressure technology with an electrochemical dissociation technology.