31 results about "Crystal habit" patented technology

The invention provides an ultrasonic-assisted gamma-aminobutyric acid crystallization particle size regulation and control method, which comprises the following steps: removing impurities and decolorizing gamma-aminobutyric acid-containing feed liquid, heating, stirring and concentrating to a nearly saturated state, then carrying out ultrasonic-assisted crystallization, cooling, aging and suction filtration to obtain coarse crystals, and finally washing and drying to obtain target crystals. According to the method, a synergistic process of raw material liquid pretreatment, evaporation concentration-ultrasonic-cooling coupling crystallization, aging and post-treatment is adopted, an ultrasonic cavitation effect is utilized to reduce a nucleation barrier, and a supersaturation degree precise control and gradient cooling strategy is combined, so that grain size refinement, obvious narrowing of distribution and effective inhibition of agglomeration of crystals are realized; the median particle size of the crystal can be controlled to be smaller than or equal to 200 microns, the particle size distribution span is smaller than or equal to 1.5, the agglomeration phenomenon is remarkably inhibited, the crystal form is kept stable, the crystal habit is complete and smooth, the crystal product quality and the process efficiency are remarkably improved, and the method has important industrial application value.

This application discloses a method for preparing ultra-high purity citric acid monohydrate based on supercritical CO2, belonging to the field of citric acid preparation technology. The method includes the following steps: dissolving citric acid monohydrate in an organic solvent to prepare a citric acid solution; spraying the citric acid solution into a supercritical CO2 environment to crystallize the citric acid using the supercritical anti-solvent effect; performing dynamic washing with pure supercritical CO2; and obtaining ultra-high purity citric acid monohydrate crystals after depressurization and drying. The citric acid monohydrate product prepared by this method has high purity, high light transmittance, low total metal ion content, controllable crystal habit, and low organic solvent residue, meeting the stringent requirements of high-end applications such as electronic and pharmaceutical grades.

The invention relates to the technical field of pesticide crystal form molecules, and discloses a dodine crystal form as well as a preparation method and application thereof. The dodine crystal form has characteristic absorption peaks when 2theta is 6.40 + / -0.2 degrees and 19.20 + / -0.2 degrees in an X-ray powder diffraction pattern of the dodine crystal form under Cu-K alpha radiation at the temperature of 25 DEG C; the crystal form has a block-shaped or sheet-shaped crystal habit. According to the invention, the crystal form singleness of the product in the production, storage and transportation processes can be ensured, and the stability of the product is ensured; and the crystal habit is qualitatively characterized by PXRD, so that the quality standard of the original medicine and the preparation can be more effectively controlled, and the standard is provided for the practical application process.

Conventional progesterone formulations often rely on carriers, limiting drug load. This invention presents engineered progesterone microcrystals functioning as carrier-free controlled-release systems, where crystal structure dictates drug release. Distinct microcrystal forms were selectively developed using solvent / antisolvent methods, notably hollow Habit A (from IPA / DDW system) and dense Habit B (from ACN / DDW system). Both Habits A and B are confirmed stable Form 1 polymorphs. Additional habits (e.g., C and D) with diverse morphologies and crystallographic parameters were also produced using other solvent systems (e.g., involving DMSO, acetone, ethanol), demonstrating method versatility. These carrier- free microcrystals exhibit controlled, elongated progesterone release (≥14 days under tested conditions). Crucially, release profiles are tunable based on crystal habit (Habit A releasing faster than Habit B at similar sizes) and particle size, demonstrating suitability for tailored long-term controlled release applications.

The invention relates to the technical field of rebaudioside A crystals, in particular to a preparation process of a high-fluidity rebaudioside A crystal, which comprises the following steps: (1) taking a rebaudioside A raw material with the purity not lower than 60%, adding a composite solvent, heating and stirring, filtering the obtained saturated solution, and collecting the filtrate for later use; the composite solvent comprises a good solvent, a poor solvent and a crystal habit modifier; and (2) taking the filtrate obtained in the step (1), carrying out programmed cooling treatment, and then carrying out crystal growing, separation and drying to obtain rebaudioside A crystals. By utilizing the preparation process, a rebaudioside A crystal product with high flowability, uniform particle size distribution and high dissolution speed can be obtained.

The invention provides a preparation method of submicron narrow-distribution spheroidic alpha alumina for heat conduction, and belongs to the field of heat conduction filler materials. The method comprises the following steps: mixing boehmite and a crystal appearance control agent to obtain composite powder; calcining the composite powder at low temperature to obtain primary calcined powder; performing wet grinding on the primary calcined powder to obtain ground slurry; carrying out spray drying on the grinding slurry to obtain precursor powder; calcining the precursor powder at high temperature to obtain secondary calcined powder; carrying out wet depolymerization on the secondary calcined powder to obtain depolymerized slurry; carrying out spray drying on the depolymerized slurry to obtain submicron sphere-like alpha alumina spray-dried powder; and carrying out airflow scattering on the submicron sphere-like alpha alumina spray-dried powder to obtain the submicron sphere-like alpha alumina micro powder. The preparation method not only can improve the morphology of crystal grains to be spherical-like, but also has low impurity content and low specific surface area, and has good formability and good thermal conductivity after being applied to heat-conducting products.

The application discloses a method for simultaneously regulating a new crystal form and crystal habit of aripiprazole; in the technical scheme, proteins are added in the crystallization process of aripiprazole to prepare aripiprazole with different crystal habits, and new crystal forms APZ-H1 and APZ-H2 of aripiprazole are found; the application creatively applies the protein, which is harmless to human bodies, to regulate the crystal habit of drugs, so as to replace other toxic and harmful crystal habit additives and guarantee the safety of the drugs; the method has the characteristics of simplicity, high efficiency and no pollution, is harmless to human bodies, is more green and environmental protection, and is easy to realize green industrial production.

The application discloses small-granularity meropenem crystals and a preparation method thereof. Through a further reaction-dissolution coupling crystallization process after dissolving a raw material crude product by adding a lye, uniform small-granularity meropenem crystal products can be obtained. The obtained crystal products are white block or flaky shuttle-shaped crystal habits, have high content (≥99.5%), low total residual solvent (≤0.2%), and high process yield (≥90%); the aqueous solution is colorless, clear and transparent, and has an acidity of 4.84-5.12; the granularity is uniform, the fluidity is good (the angle of repose is ≤35°), the granularity distribution is small (D50 is ≤25 μm, and D90 is ≤70 μm), and the product redissolution time is fast (≤75 s); after the obtained products are placed under the condition of 30 ± 2 ℃ and 60 ± 5% RH for three months, no obvious changes are found in various indexes, and the products have good stability. The required equipment is simple, the processing scale is large, the operation is simple, industrial production can be carried out, and the method has good technical economy and high industrial application value.

The present application relates to the field of biotechnology, in particular to a method for regulating the crystal habit of dipeptide-containing crystals. The present application provides a method for regulating the crystal habit of dipeptide-containing crystals. Compared with the traditional crystallization method, after using inorganic salt as a crystal agent to change the crystal habit, the bulk density of the product is improved, and the fluidity is improved. The improvement of the bulk density of the product can reduce the storage and transportation cost of the enterprise. The improvement of the fluidity of the product can reduce the processing difficulty and health management difficulty of the downstream enterprise in the processing process. This has very important significance for promoting the application of carnosine, SH, GH and related products in health care and beauty.

The application provides a method for continuous crystallization of large-particle D-psicose crystal, based on the growth kinetics characteristics of D-psicose crystal, through the mode of "single stimulation nucleation + constant temperature crystal growth + circulating seed reservation + mother liquor recovery", the synergism of continuous production and accurate regulation of crystal habit is realized, and high-purity, large-particle and regular rod-shaped D-psicose crystal is prepared, which is a continuous preparation process for realizing large-particle, high-purity and easy-to-filter D-psicose crystal through "circulating seed reservation and crystal growth + mother liquor recovery cycle". Meanwhile, the process is simple, the degree of automation is high, the product quality is stable, there is no batch difference, the raw material utilization rate is high, there is no organic solvent addition in the whole process, the energy consumption is low, the cost is controllable, and the process is suitable for industrialized large-scale continuous production.

The application relates to the technical field of fine chemical production, and particularly discloses a crystallization process of short-rod-shaped ivermectin, which comprises the following steps: dissolving ivermectin crude product in a crystallization solvent, heating to 50-55 DEG C, adding a crystallization agent, uniformly mixing, then cooling to 35-40 DEG C at a rate of 0.1-0.3 DEG C / min, adding ivermectin crystal seeds, continuously cooling to 5-15 DEG C, and incubating and crystallizing to obtain ivermectin products. The crystallization process of ivermectin provided by the application realizes effective control of the particle size and crystal habit of ivermectin products in the crystallization process by adopting a combination strategy of selecting a specific crystallization solvent, adding a crystallization agent and crystal seeds at specific stages, controlling the cooling rate and the incubation time, obtaining short-rod-shaped ivermectin products with uniform particle size distribution, and the products have good fluidity, are convenient for subsequent preparation application, do not need repeated crystallization for multiple times, effectively reduce the cost of the crystallization process, and have extremely high practical application value.

The present application relates to the field of pharmaceutical preparations, in particular to a rilugolimab long-acting microcrystalline pharmaceutical composition and a preparation method thereof, wherein a specific recrystallization process is used for rilugolimab raw materials, and the obtained crystals have uniform relative particle size and good crystal habit morphology. The rilugolimab long-acting microcrystalline pharmaceutical composition is administered by intramuscular injection, and can be sustained in vivo for at least more than 1 month, or more than 2 months, more than 3 months, or even more than 4 months, thereby effectively reducing the administration frequency, maintaining stable blood drug concentration, improving clinical efficacy, and better meeting the clinical needs.

The application discloses a preparation method of penicillin V potassium, which mainly aims at improving the crystal habit of penicillin V potassium and reducing the content of a key impurity, 4-hydroxy penicillin V potassium. The application also relates to a penicillin V heavy crystal and a method for preparing a potassium salt from penicillin V, which comprises the following operation steps: dissolving raw materials, reacting with alkali to form a salt, solvus crystallization, suction filtration and drying. The method is simple and easy to operate and can be used for preparing penicillin V potassium by using a low-toxicity solvent, and the content of the key impurity, 4-hydroxy penicillin V potassium, can be reduced by more than 50%. The process is low in cost, low in energy consumption, high in efficiency and suitable for industrial production.

The application provides a particle size control method for ultrasonic-assisted gamma-aminobutyric acid crystallization. After impurity removal and decolorization of a gamma-aminobutyric acid feed liquid, the feed liquid is concentrated to a near-saturated state through heating and stirring, then ultrasonic-assisted crystallization is performed, cooling and temperature reduction are performed, aging is performed, and crude crystals are obtained through suction filtration, and finally, the target crystals are obtained through washing and drying. The method is a synergistic process of raw material liquid pretreatment, evaporation concentration-ultrasonic-cooling coupled crystallization, aging and post-treatment, uses ultrasonic cavitation effect to reduce nucleation potential barrier, and combines supersaturation precision control and gradient cooling strategies to realize crystal particle size refinement, obvious narrowing of particle size distribution and effective inhibition of agglomeration, so that the median particle size of the crystals can be controlled to be less than or equal to 200 microns, the particle size distribution span is less than or equal to 1.5, the agglomeration phenomenon is significantly inhibited, the crystal form remains stable, the crystal habit is complete and smooth, the crystal product quality and process efficiency are significantly improved, and the method has important industrial application value.

The invention provides a crystal form I of 2-nitro dimethyl terephthalate as well as a preparation method and application thereof. The crystal form I is characterized in that by using Cu-K alpha radiation, X-ray powder diffraction represented by a 2 theta angle has characteristic peaks at diffraction angles of 10.2 + / -0.2 degrees, 14.3 + / -0.2 degrees, 14.9 + / -0.2 degrees, 15.8 + / -0.2 degrees, 16.3 + / -0.2 degrees, 17.3 + / -0.2 degrees, 19.3 + / -0.2 degrees, 20.1 + / -0.2 degrees, 20.5 + / -0.2 degrees, 22.1 + / -0.2 degrees, 22.5 + / -0.2 degrees, 23.4 + / -0.2 degrees, 24.4 + / -0.2 degrees, 25.0 + / -0.2 degrees, 25.5 + / -0.2 degrees, 26.4 + / -0.2 degrees, 26.7 + / -0.2 degrees, 27.2 + / -0.2 degrees, 27.5 + / -0.2 degrees and The crystal product of the crystal form I of 2-nitro dimethyl terephthalate is a bulk crystal, and has the advantages of complete crystal habit, smooth surface, high product crystallinity and good stability.

The invention discloses a process for producing potassium sulfate and sodium sulfate from glaserite. The process comprises the five steps of concentration evaporation, sodium sulfate evaporative crystallization, glaserite cooling crystallization, conversion and mother liquor circulation. A crystal nucleus inhibition auxiliary agent (a compound of carboxymethyl chitosan and sodium alginate) is continuously added in the concentration and evaporation stage to prevent equipment from scaling; a crystal habit modification auxiliary agent (a compound of sulfonated polyaspartic acid and trisodium citrate) is added in a pulse mode in the sodium sulfate crystallization stage to control the crystal morphology; in the cooling crystallization stage, potassium sulfate seed crystals and a selective nucleation promoting aid are added, and a staged cooling strategy is adopted. Compared with a traditional process, the method has the advantages that the particle size distribution Span value of sodium sulfate is reduced to 1.15-1.48, the purity of potassium sulfate reaches 99.0% or above, and the comprehensive utilization rate of raw materials reaches 93-95%. And the auxiliary agent is recycled along with the mother liquor, the wastewater discharge is reduced by more than 60%, and the production period is 7.5-10.0 hours.

The application discloses a preparation method of ranitidine hydrochloride small rod-like crystal habit, and the preparation method comprises the following steps: directly crystallizing ranitidine hydrochloride in 95% ethanol to obtain ranitidine hydrochloride small rod-like crystal habit powder. The preparation method is beneficial to controlling the growth of NDMA impurities in ranitidine hydrochloride, and the growth speed of the NDMA impurities in the prepared ranitidine hydrochloride small rod-like crystal habit powder is 40 times slower than that in the ranitidine hydrochloride agglomerated crystal habit powder on the market, and the stability is obviously improved.

Object of the present invention is an improved process for the preparation of Trenbolone Acetate of formula (I) having irregular hexagon plates crystal habit and / or a median value (D50) of the particle size distribution comprised in the range from 50 μm to 80 μm, or from 60 μm to 90 μm, or from 90 μm to 250 μm, by means of a crystallization wherein an addition of a seed having a median value (D50) of the particle size distribution comprised respectively in the range from 8 μm to 15 μm, or from 15 μm to 20 μm, or from 20 μm to 90 μm, to a solution of Trenbolone Acetate in a solvent, wherein the solvent is a C2-C5 alkyl alcohol or mixture thereof.

The invention discloses a method for regulating and controlling a fluorescent silver nanocluster crystal habit through a cellulose template and application of the method in fluorescent ink. The preparation method comprises the following steps: by taking hydroxypropyl methyl cellulose as a raw material, carrying out dissolution and formylation treatment to obtain formyl modified cellulose; and uniformly mixing a silver source and a protective ligand, adding aldehyde modified cellulose (used as a stabilizer and a structure-directing agent), and standing at room temperature to regulate and control the fluorescent silver nanocluster crystal habit. On the basis, a proper volume of ethyl alcohol is added, and the obtained composite material can emit obvious yellow fluorescence under excitation of 365 nm ultraviolet light and can be applied to the fields of novel fluorescent ink, anti-counterfeit printing, biological imaging and the like.

The invention provides a method for accurately regulating and controlling empagliflozin crystal habit based on a deep eutectic solvent, and belongs to the technical field of medicine. The preparation method of empagliflozin with the controllable crystal habit comprises the following steps: step S100: mixing tetrabutylammonium chloride and maleic acid according to a molar ratio of 1: 2-1: 5, and stirring and reacting at 50-60 DEG C for 2-4 hours to prepare a eutectic solvent; s200, adding an empagliflozin raw material into the eutectic solvent, controlling the concentration to be 5-15 mg / mL, stirring and dissolving at 40-50 DEG C, and slowly cooling the solution to 30-35 DEG C at the cooling rate of 0.5-2 DEG C / min, so that the empagliflozin forms a cubic or flaky crystal habit; and S300, after the crystallization is completed, separating crystals and the eutectic solvent by adopting reduced pressure filtration, washing the crystals with ethanol, and carrying out vacuum drying under the conditions of 45-55 DEG C and 1-3 kPa until the weight is constant. The preparation method of the empagliflozin with the controllable crystal habit is simple in process, the eutectic solvent can be recycled, and the preparation method is green and low in cost.

The object of the present invention is an improved process for the preparation of Trenbolone Acetate of formula (I) by means of crystallization, having irregular hexagonal plate-like crystal habit and / or being comprised in a particle size distribution median value (D50) ranging from 50 pm to 80 pm, or from 60 pm to 90 pm, or from 90 pm to 250 pm, wherein seed crystals having a particle size distribution median value (D50) comprised in the range from 8 pm to 15 pm, or from 15 pm to 20 pm, or from 20 pm to 90 pm, respectively, are added to a solution of Trenbolone Acetate in a solvent, wherein the solvent is a C2-C5 alkyl alcohol or a mixture thereof.

This invention discloses a eutectic compound of dimethyl 5-aminoisophthalate and tetracyanophenylene, its preparation method, and its applications. The chemical formula of the invented eutectic compound is C5. 30 H 24 N6O8 has a monoclinic crystal system, space group P21 / n, with cell parameters α = 90°, β = 101.461(3)°, γ = 90°, and cell volume. This invention uses a solvent evaporation method for preparation, which features simple processing, mild conditions, good crystal quality, and complete crystal habit. The eutectic compound provided by this invention can serve as a potential luminescent material.

The application provides a method for preparing alpha-hemihydrate calcium sulfate whiskers by in-situ induced crystallization of chemical high-salinity wastewater, and belongs to the technical field of comprehensive utilization of water resources and salt resources. The method uses chemical high-salinity wastewater as raw material, concentrates the wastewater to a proper ion concentration after impurity removal treatment, and then performs slurry preparation. NaCl in the high-salinity wastewater is used as a crystallization induction medium, and in-situ normal-pressure induced crystallization is performed to obtain a crystal slurry. Then, solid-liquid separation is performed on the crystal slurry to obtain a whisker filter cake. After washing and drying, the whisker filter cake is used to obtain finished alpha-hemihydrate calcium sulfate whiskers. The whole process is operated at normal pressure and low temperature, and high-pressure special equipment is not needed, so that investment and energy consumption are saved. NaCl in the high-salinity wastewater is directly used as the crystallization induction medium, ion balance and efficient cooperation in the system are realized, the mother liquor is recycled in a closed loop, and no salt-containing wastewater is discharged. Through precise regulation and control of the external morphology of the crystals by using a compounded crystal habit modifier, uniform needle-shaped whiskers with a length-diameter ratio of more than 60 are produced, and liquid-phase disposal and high-value utilization of the chemical high-salinity wastewater are realized.

The application provides a composite adsorption crystallization aid, a preparation method thereof and application in ODA purification, wherein the aid is composed of three types of functional components: a porous adsorption matrix, which is biomass activated carbon; a crystal habit regulating component selected from an organic compound or a salt thereof containing two or more carboxyl groups and / or hydroxyl groups; and a coordination chelation component selected from an organic ligand containing nitrogen and / or oxygen coordination atoms; the porous adsorption matrix is loaded with metal organic framework or covalent organic framework nanoparticles on the surface, and the surface is modified by oxidation to introduce oxygen-containing functional groups; the crystal habit regulating component and the coordination chelation component are grafted on the surface of the porous adsorption matrix through chemical bonds; through the broad-spectrum adsorption and molecular sieving effect of the porous adsorption matrix, and the efficient capture of metal ions by the coordination chelation component, the simultaneous deep removal of pigments, macromolecular organic matters, organic isomers and trace metal ions in the ODA solution is realized.

The application discloses a baloxavir ester crystal form B1 and a preparation method thereof. Using Cu-Kα radiation, the X-ray powder diffraction pattern expressed by a 2θ angle has characteristic peaks at positions of 8.24°±0.2°, 9.80°±0.2°, 11.24°±0.2°, 11.76°±0.2°, 13.50°±0.2°, 14.80°±0.2°, 18.08°±0.2°, 19.44°±0.2°, 20.60°±0.2°, 21.18°±0.2°, 21.46°±0.2°, 22.58°±0.2°, 24.38°±0.2°, 25.28°±0.2°, 27.18°±0.2° and 33.42°±0.2°. The crystal habit is blocky, the filtration resistance is smaller than that of Form I with a fine needle-like crystal habit, the particle sample after grinding has a smaller angle of repose, has better particle flowability, and is more beneficial to subsequent preparation process treatment.

The present invention relates to crystal forms A and B of a compound (HS378) of formula (I) and a preparation method therefor. The crystal forms A and B have a good physiochemical stability, a regular crystal habit, a good particle size uniformity, and a good fluidity; the preparation method for the crystal forms A and B is simple; moreover, a good impurity removal effect, easiness in filtration and a high yield are achieved, and samples with few impurities and a high purity can be obtained; and the purification problem of difficulties during impurity removal can be fully solved.

The present invention provides a method for precisely controlling the crystal habit of empagliflozin based on a deep eutectic solvent, belonging to the field of pharmaceutical technology. The method for preparing empagliflozin with controlled crystal habit comprises: step S100: mixing tetrabutylammonium chloride and maleic acid in a molar ratio of 1:2-1:5, stirring and reacting at 50-60°C for 2-4 hours to prepare a deep eutectic solvent; step S200: adding empagliflozin raw material to the deep eutectic solvent to control the concentration to 5-15 mg / mL, stirring and dissolving at 40-50°C, and slowly cooling the solution to 30-35°C at a cooling rate of 0.5-2°C / min to form cubic or lamellar crystals of empagliflozin; step S300: after crystallization is completed, separating the crystals from the deep eutectic solvent by vacuum filtration, washing the crystals with ethanol, and vacuum drying at 45-55°C and 1-3kPa to constant weight. The method for preparing empagliflozin with controlled crystal habit applied by the present invention is simple in process, the deep eutectic solvent can be reused, and it is green and low-cost.

The application discloses a method for improving L-alanine crystal habit, relates to the technical field of L-alanine preparation, and comprises the following steps: adding an organic sodium salt ionic compound into an aqueous solution containing L-alanine, and crystallizing to obtain rod-shaped L-alanine crystals; the organic sodium salt ionic compound comprises one or more of sodium acetate, sodium stearate and sodium oxalate. According to the application, the water molecule hydrogen bond network in the solution is rearranged into a sodium salt-containing hydrogen bond network by adding the organic sodium salt into the aqueous solution containing L-alanine, so that the ionic compound can better interact with L-alanine molecules, the morphology of the L-alanine crystals is effectively improved, and the obtained L-alanine product has good flowability and high tap density.

The invention discloses a preparation method of daunorubicin hydrochloride rod-like crystal habits, and belongs to the technical field of medicines. The method comprises the following steps: dissolving daunorubicin hydrochloride in a benign solvent, and heating and stirring until the daunorubicin hydrochloride is completely dissolved; and then adding a certain amount of poor solvent at a certain rate, then adding seed crystal, then adding a certain amount of poor solvent, controlling the stirring speed and cooling at a certain cooling rate after the addition is completed, continuing to maintain the stirring speed to grow the crystal, and filtering, washing and drying the product to obtain the daunorubicin hydrochloride rod-like crystal habit. The product crystal habit has the advantages of uniform particle size distribution, good product stability, good fluidity, large bulk density, high yield and the like. The method is high in experiment repeatability, is less interfered by external factors, and is suitable for industrial production.