207results about How to "High crystal purity" patented technology

The present invention relates to improved methods for the production, isolation and purification of epothilone B. These methods include, for example, a fermentation process for the production of epothilone B, isolation via adsorption onto a resin, and subsequent purification.

The invention discloses a method for extracting succinic acid from a broth. The method comprises the following steps: a sodium succinate broth generated from microbial fermentation goes through a microfiltration membrane to conduct cross-flow filtration so as to remove thallus and other relatively large impurity particles; cross-flow filtration is carried out through a nanofiltration membrane to remove residual protein and pigment in the broth so as to get a clean filtrate; after the electrolysis, electrodialysis and electrolysis of the clean filtrate through a bipolar membrane, a succinic acid solution and a sodium hydroxide solution are obtained respectively; and the succinic acid solution is decompress-vaporized, cooled and crystallized, and therefore white succinic acid crystals are obtained. All working procedures in the method are closely connected, feed liquid always recycles under sealed condition, conditions through the whole technique process are mild, no organic solvent and any other organic compounds are added, the technique flow is short, steps are simple, the requirements on equipment are not high, the final product has high purity and the content of succinic acid is more than 99.0 percent through test.

Belonging to the field of fluorescent solid materials, the invention in particular relates to a terpyridine zinc benzoate complex [Zn(tpb)2(Htpb)2] and its preparation condition. The terpyridine zinc benzoate complex prepared by the invention has a coordination structure shown as formula (1) in the specification, can emit yellow fluorescence under 365nm ultraviolet irradiation, and has high thermal stability, and the skeleton starts decomposition at a temperature above 300DEG C, so that the complex can be used as a zinc based fluorescent solid material in various fields, and specifically can be applied to ink anti-counterfeiting technology, like anti-counterfeiting of bills, currencies, securities and other high-end products. According to the preparation condition of the terpyridine zinc benzoate complex [Zn(tpb)2(Htpb)2] provided by the invention, the operation is simple, the crystallization purity is high, and the yield is up to 69%. (formula (1)).

The method relates to a method for purifying ceftazidime, more concretely relating to a method for preparing high quality ceftazidime pentahydrate by impure, high-polymer impurity content ceftazidime through crystallization. It prepares impure, high-polymer impurity content ceftazidime pentahydrate, ceftazidime Hclú¼ceftazidime hydrobromide or ceftazidime overdue or recovered from the market, into a ceftazidime water solution, then regulates the pH value of the ceftazidime water solution to 1.5-2.5 by alkali or acid, here the impurity ceftazidime polymer is separated out with a little ceftazidime, and the separated-out matter is filtered, and the pH value of the filtrate is regulated to 3.5-4.8 by alkali so that the ceftazidime pentahydrate crystals are separated out. The method is simple and convenient to operate, low-cost, good-safety and high-yield. The obtained ceftazidime pentahydrate crystals are high purity and the polymer is low-content, reaching pharmacopoeia specified requirements.

The invention provides a crystal form of sorafenib tosylate, and a preparation method thereof. The X-ray powder diffraction pattern of sorafenib tosylate of crystal form B has diffraction peaks when the values of 2theta are about 7.34DEG, 18.03DEG, 20.15DEG, 20.77DEG, 22.04DEG, 22.43DEG and 23.21DEG; and the X-ray powder diffraction pattern of sorafenib tosylate of crystal form C has diffraction peaks when the values of 2theta are about 7.61DEG and 13-33DEG. The sorafenib tosylate of crystal form C is prepared through reduced pressure heating of the sorafenib tosylate of crystal form B. The invention also provides a preparation method of amorphous crystals of sorafenib tosylate through reduced pressure heating of the sorafenib tosylate of crystal form B or C. The sorafenib tosylate crystals prepared in the invention have the advantages of good stability, high crystallization purity, simple preparation process, and suitableness for industrial production.

The invention discloses a method for preparing barium titanate monocrystal nano particles of six-pin structural perovskite, and a two-step hydrothermal method is adopted. The method comprises the following steps of: depositing tetrabutyl titanate which serves as a precursor by use of oxyhydroxide of titanium prepared from ethylene glycol monomethyl ether; performing hydrothermal reaction by utilizing potassium hydroxide a mineralizer, so as to obtain a K2Ti6O13 nano line; and performing secondary hydrothermal reaction on the prepared K2Ti6O13 nano line which serves as a titanium source, barium acetate which serves as a barium source and KOH which serves as the mineralizer, so as to obtain the barium titanate monocrystal nano particles of the six-pin structural perovskite. The process is simple and easy to control; pollution is avoided; the cost is low; large-scale production is realized; and the barium titanate monocrystal nano particle crystal of the six-pin structural perovskite is high in purity and high in dispersion.

The present invention relates to preparation process of hydrocarbon hydroprocessing catalyst, which has gamma-Al2O3 as carrier, VIB and VIII metal as the active component, and Ti, etc as the active assistant, with the assistant Ti being introduced in the pH swinging carbonization process for producing aluminum hydroxide. The process of preparing the catalyst is one complete mixing and kneading process including the steps of introducing Ti to aluminum hydroxide powder via adding Ti salt solution, adding Mo and/or W containing alkaline solution, mixing and kneading until the aluminum hydroxide powder is wetted completely by the alkaline solution, adding Co and/or Ni containing acid solution, mixing and kneading to obtain plastic material, extruding, drying, and roasting to obtain the catalyst. The catalyst has homogeneously distributed Ti component and obviously raised performance.

The invention discloses a crystallization-type Ilaprazole sodium and a preparation method thereof. The Ilaprazole sodium with a novel crystalline form provided by the invention is easy to prepare, high in purity and low in impurity content. The preparation method provided by the invention needs low solvent amount, has advantages of low production cost, simple operation and mild reaction condition, is easy to control, and can produce the target product crystalline form doubtlessly and well-repeatedly.

The invention discloses a preparation method of high-purity all-trans lycopene crystal, and comprises the following steps: filtering the ferment material liquid, thus obtaining mycelium; adding polar organic solvent to the mycelium to grind and break the wall, and then filtering and removing the organic solvent; taking the mixture of mycelium and low-boiling petroleum based organic solvent as degreaser to remove mycelium oily consistituent and the foreign matter such as little amount of Beta-carotene; taking the mixture of mycelium and low-boiling petroleum based organic solvent as extractingagent to liquid-solid extract the lycopene in mycelium; cooling down the extract liquor for crystallization; filtering and drying in vacuum, thus obtaining high-purity all-trans lycopene crystal. Thetechnique adopted by the method can avoid lycopene from retrogradation and isomerization owing to heat and oxidation. The lycopene crystal prepared by the method has high purity, the content of lycopene exceeds over 97 percent, and the content of the all-trans structure exceeds over 90 percent.

The invention relates to a synthetic method of (ethoxymethylene)-malononitril, which includes the following steps: (1) dropwise adding malononitrile into triethyl orthoformate in ice bath cooling condition, and adding catalyst anhydrous zinc chloride after dropwise adding for reaction for 2-4 hours, and (2) steaming and removing ethanol after the reaction is finished, cooling for dissolving out solids, and filtering and collecting the solids to obtain the (ethoxymethylene)-malononitrile. The synthetic method is easy to operate, high in yield, low in cost, environment-friendly, high in product crystallization purity, stable in quality and suitable for large-scale industrial production.

The invention discloses a method for preparing alpha-imatinib mesylate, and belongs to the field of medicines. The method comprises the following steps of: suspending imatinib base in a mixed solvent of water and an organic solvent, stirring, and adjusting the temperature to be 20-30DEG C; dissolving methanesulfonic acid, and dripping into reaction liquid; after the dripping is finished, standingfor clarifying the liquid, heating to the temperature of between 50 and 60DEG C, and keeping the temperature to react for 0.5 to 1 hour; and reducing the temperature to 32-40DEG C, adding alpha-imatinib mesylate seed crystals, dripping the organic solvent, continuously reducing the temperature to 20-30DEG C, separating out crystals, filtering, and drying to obtain a product. The preparation method has the advantages of simple operation, short reaction time, high yield, high purity of alpha-imatinib mesylate, low production cost, and suitability for industrial production.

The application discloses a zirconium carbide-silicon carbide composite powder material, wherein a molar ratio of components in the zirconium carbide-silicon carbide composite powder material satisfies ZrC:SiC=1:0.1-1:10; a preparation process is easy, the cost is low, and the process is easy to control; and the obtained zirconium carbide-silicon carbide composite powder material has the advantages of submicron level, uniform composition and high purity.

The invention belongs to the field of medicine and particularly relates to a new method for preparing a citric acid tofacitinib medicinal crystal form. The method has the advantages of being simple inoperation, good in reproducibility, high in yield, good in purifying effect for API related substances, high in crystal form purity, suitable for industrialized mass production and the like, and overcomes the problems of complicated operation, low reproducibility, low yield, poor purifying effect for API related substances, low crystal form purify, unsuitability for industrialized production andthe like.

The invention relates to a preparation method of sodium citrate crystal through solvent-out crystallization. The preparation method comprises the following steps: (A) carrying out salt-forming reactions: preparing critic acid and a salt forming agent according to a certain mole ratio, dissolving the salt forming agent into water at first, then slowly adding critic acid into the water, controlling the reaction temperature at a range of 20 to 30 DEG C, wherein the pH value of the solution is in a range of 7.5 to 9.0 when the reactions finish, and filtering the solution after the reactions so as to obtain a mixed solution, wherein the mixed solution concentration calculated by waterless sodium citrate is 285 g/L to 570 g/L; (B) carrying out solvent-out crystallization: adding a solvent-out agent into the mixed solution obtained in the step (A) according to a certain volume ratio to crystallize the sodium citrate crystals, and controlling the crystallization temperature at 20 to 75 DEG C; (C) filtering and drying so as to obtain the sodium citrate product; wherein the sodium citrate product comprises waterless sodium citrate, dihydrate sodium citrate, and pentahydrate sodium citrate. The provided preparation method is simple and convenient, the yield is high, the crystal is large, the purity is high, and the sodium citrate quality is largely improved.

The invention discloses a preparation method of I type clopidogrel hydrogen sulfate. The method comprises the following steps: (1) dissolving clopidogrel free base in tetrahydrofuran, and adding concentrated sulfuric acid at the temperature of minus 14-0 DEG C; (2) leading the mixture to react for 1-2 hours, then slowly increasing the reaction temperature to 20-40 DEG C, continuing the reaction for 10-12 hours, and fully precipitating crystals; and (3) filtering after obtaining the crystals, washing a filter cake with the tetrahydrofuran, draining, vacuum-drying and obtaining the I type clopidogrel hydrogen sulfate. The I type clopidogrel hydrogen sulfate prepared through the method is not doped with II type clopidogrel hydrogen sulfate and has high crystal phase purity, and the preparation process does not need the steps of nitrogen production and the like, thereby reducing the production cost, leading the operation method to be simple and easy, realizing high repeatability and being easy to realize mass production.