Salt and crystal form of egfr inhibitor, and composition and use thereof
US-2024352053-A1 · Oct 24, 2024 · US
US10179758B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10179758-B2 |
| Application number | US-201715615890-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jun 7, 2017 |
| Priority date | Jun 15, 2016 |
| Publication date | Jan 15, 2019 |
| Grant date | Jan 15, 2019 |
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A method for crystallizing succinic acid includes agitating a succinic acid reaction solution with a jet-flow agitator that is rotated at low speed and has a low volume power density; compared with the conventional agitators, the jet-flow agitator helps increase the uniformity of succinic acid particles, shorten the time required for crystallizing succinic acid, and raise the yield of the crystallized succinic acid as well as purity of crystallized succinic acid having a purity of 99.8-99.9%.
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What is claimed is: 1. A method for enhancing uniformity of crystallized succinic acid, comprising the steps of: a) preparing a crystallization tank containing therein a jet-flow agitator composed of a rotating shaft and a plurality of inclined converging-tube blades driven by the rotating shaft into rotation; b) pouring a solvent into the crystallization tank of the step a), wherein the solvent is one selected from the group consisting of water, methanol and ethanol; c) adding succinic acid solids to the solvent of the step b) by weight ratio of the solvent to the succinic acid solids ranged from 2.0 to 10.0 to form a reaction solution; d) activating the jet-flow agitator of the step a) to have the inclined converging-tube blades thereof rotated at 50-500 rpm to cause the reaction solution of the step c) to undergo irregular fluctuations or mixing to disperse the succinic acid solids uniformly in the reaction solution; e) setting a cooling rate of the crystallization tank to 10-35° C. per hour, and allowing the succinic acid solids of the reaction solution to undergo a crystallization and purification reaction for 1-8 hours at a reaction pressure of 5-100 lbf/in 2 and a reaction temperature of 0-90° C.; and f) after the crystallization and purification reaction of step e) completed, filtering out and removing the solvent from the reaction solution of the step e) to obtain solid residues, and drying the solid residues to obtain final products of high-purity succinic acids having a purity of 99.8-99.9%. 2. The method of claim 1 , wherein the inclined converging-tube blades of the jet-flow agitator of the step a) are formed as inclined nozzle blades or inclined conical spring blades. 3. The method of claim 2 , wherein in the step b) the ethanol is used as the solvent. 4. The method of claim 2 , wherein in the step c), the weight ratio of the solvent to the succinic acid solids ranges from 2.3 to 7.0. 5. The method of claim 2 , wherein in the step c), the weight ratio of the solvent to the succinic acid solids ranges from 4.0 to 7.0. 6. The method of claim 2 , wherein in the step c), the weight ratio of the solvent to the succinic acid solids was equivalent to 4.
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