9results about How to "The crystallization process is easy to control" patented technology

This invention belongs to the technical field of medicinal chemistry and provides a milrinone-tartaric acid cocrystal. Using Cu-Kα radiation, its X-ray diffraction pattern (expressed as 2θ) exhibits characteristic peaks at at least 10.0±0.2°, 13.2±0.2°, 20.4±0.2°, 24.7±0.2°, 26.2±0.2°, 26.7±0.2°, and 34.3±0.2°. The cocrystal of this invention has high solubility and good stability. Using this cocrystal to prepare formulations avoids the use of large amounts of excipients and auxiliaries in existing technologies, reducing both production costs and clinical safety risks. The preparation method of the milrinone-tartaric acid cocrystal provided by this invention is simple to operate, the crystallization process is easy to control, and it has good reproducibility.

The invention provides a refining method of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid, which comprises the following steps: mixing a 3, 3 ', 4, 4'-biphenyltetracarboxylic acid crude product, acetic acid, a ketone solvent and water at 90-100 DEG C to obtain a biphenyltetracarboxylic acid crude product solution; and mixing the crude biphenyltetracarboxylic acid solution with the seed crystal at 80-90 DEG C, and then carrying out cooling crystallization to obtain a 3, 3 ', 4, 4'-biphenyltetracarboxylic acid refined product. The invention provides a refining method of 3, 3 ', 4, 4'-biphenyltetracarboxylic acid, which has the following advantages: (1) the total metal ions of the product are low and the purity is high, acetic acid is used as an ion exchanger in the refining method, the metal ion removal effect and the product purity can be effectively improved, and the total metal ions can be reduced to 0.2 ppm or below; (2) the yield and the whiteness of the product are high, and the whiteness can be increased to 98% or above; and (3) the refining method is simple and convenient in process.

The invention relates to the technical field of crystallization, and provides a crystallization method of psicose. The method comprises the following steps: separating a psicose crude product solution by adopting a simulated moving bed method to obtain a psicose purified solution; evaporating the psicose purified liquid to constant weight to obtain a psicose concentrate; mixing the psicose concentrate, water and a psicose seed crystal to obtain a mixture; and cooling and crystallizing the mixture, and carrying out solid-liquid separation to obtain the psicose crystal. The method provided by the invention has the advantages of high crystallization yield, proper crystallization rate, full crystal form, simple preparation process, no use of organic reagents, environmental friendliness, economy, high efficiency, improvement of production efficiency and product quality, and low production cost, and brings innovation and improvement for the production process of psicose.

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a new mirinol crystal form, and particularly to a mirinol-adipic acid co-crystal and a preparation method and application thereof. The co-crystal has an X-ray diffraction spectrum expressed by 2theta using Cu-Kalpha radiation, and has characteristic peaks at least at 9.0+ / -0.2°, 15.7+ / -0.2°, 18.0+ / -0.2°, 24.0+ / -0.2°, 31.4+ / -0.2°, 31.6+ / -0.2°. The preparation method of the mirinol-adipic acid co-crystal is simple in operation, easy to control in crystallization process, and good in reproducibility.

The utility model provides neutralization crystallization equipment capable of uniformly spraying at an inlet nozzle. The neutralization crystallization equipment comprises a shell, a steam condensate outlet, a tail gas ammonia input pipe and a sulfuric acid solution input pipe, wherein the steam condensate outlet is formed in the top of the shell; the tail gas ammonia input pipe and the sulfuric acid solution input pipe are arranged at the bottom of the shell; a nozzle is arranged at the inner end of the sulfuric acid solution input pipe, and a plurality of spraying holes are formed in the side face of the nozzle. The crystallizer has the beneficial effects that the nozzles capable of uniformly spraying are arranged, so that the liquid in the crystallizer can be uniformly distributed without dead angles or excessively concentrated areas, and the crystallization process can be uniformly carried out in the whole crystallizer. Competition and interference in the crystal growth process are reduced, the crystallization efficiency is improved, and crystals with uniform sizes and regular shapes can be formed. The liquid is uniformly distributed, so that the external influence on the crystal in the growth process is more consistent, the crystal form difference caused by different local conditions is reduced, and the phenomenon of local overheating or supercooling is avoided.

The present application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a crystal form of lamivudine salt of m-hydroxybenzoic acid and a preparation method thereof. The crystal form has an X-ray diffraction spectrum expressed by 2theta using Cu-Kalpha radiation, and has characteristic peaks at least at 9.26+ / -0.2, 12.56+ / -0.2, 13.05+ / -0.2, 14.59+ / -0.2, 17.45+ / -0.2, 20.30+ / -0.2, 21.76+ / -0.2, 23.37+ / -0.2, 25.05+ / -0.2 and 27.58+ / -0.2; the crystal form is composed of a molecule of lamivudine, a molecule of m-hydroxybenzoic acid and a molecule of n-butanol as a basic unit; meanwhile, the crystal form has good solubility, provides ideal raw material for preparing parenteral dosage forms which are convenient to administer and have rapid effect, and thus better meets the requirements of clinical application.

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a milrinone-citric acid dihydrate co-crystal. The application provides a new milrinone-citric acid dihydrate co-crystal and a preparation method thereof. The co-crystal has excellent properties, can significantly enhance the solubility and stability of milrinone, is helpful to improve the oral bioavailability, improve the clinical curative effect, has strong drug-making value, the preparation method is simple in operation and easy to control, and is suitable for industrial amplification.

The application belongs to the technical field of pharmaceutical chemistry, and particularly relates to a new crystal form of cabozantinib, a preparation method and application thereof. The new crystal form provided by the application is a cabozantinib-amino sulfonic acid-methanol co-crystal, wherein one molecule of cabozantinib, one molecule of amino sulfonic acid and one molecule of methanol form a basic unit of the crystal form, and great improvement is achieved in stability, solubility and the like, the preparation method is simple in operation, good in reproducibility and suitable for industrialized production.

The invention relates to the technical field of solar cells, in particular to a method for preparing a large-area tin-lead perovskite solar cell. The method is suitable for a perovskite solar cell with a p-i-n, n-i-p structure, and comprises the following steps: S1, spin-coating a hole transport layer precursor solution on a substrate, and annealing to obtain a hole transport layer; s2, spin-coating a perovskite light absorption layer precursor on the hole transport layer to obtain a perovskite light absorption layer wet film; s3, placing the perovskite light absorption layer wet film in a reduced pressure distillation device, and controlling the vacuum degree drop rate to realize nucleation control of the perovskite light absorption layer wet film; s4, moving out the perovskite light absorption layer wet film from which the solvent is removed, and annealing to obtain a perovskite light absorption layer; and S5, sequentially preparing a passivation layer, an electron transport layer, a hole blocking layer and an electrode layer on the perovskite light absorption layer. According to the method, the vacuum degrees of the fixed cavity at different moments are quantified, and the air exhaust time is in one-to-one correspondence with the vacuum degrees of the cavity, so that the air exhaust rate is clear, and the film nucleation crystallization is controllable.