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A self-circulating crystallizer and multi-stage continuous crystallization method

A crystallizer and crystallization technology, which is applied in the fields of medicine and chemical industry, can solve the problems of small product particle size, short operation cycle, equipment fouling, etc., achieve large product particle size and improve the effect of small product particle size

Active Publication Date: 2020-12-08
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problems existing in the existing continuous crystallization technology and equipment, the present invention provides a high-efficiency self-circulation crystallizer and a multi-stage continuous crystallization method, through the specific configuration of the crystallizer and process material flow and operation control, the crystallization system can be stably regulated The degree of supersaturation can effectively control the nucleation and growth of crystals, and achieve the particle size classification of crystal particles, so as to improve the continuous crystallization process. Problems such as small product particle size, serious equipment fouling, pipeline blockage, short operating cycle, etc., improve the stability of the continuous crystallization process Operation cycle to ensure product quality

Method used

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  • A self-circulating crystallizer and multi-stage continuous crystallization method
  • A self-circulating crystallizer and multi-stage continuous crystallization method
  • A self-circulating crystallizer and multi-stage continuous crystallization method

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Embodiment 1

[0043] as attached figure 1 A typical crystallizer schematic diagram disclosed by the present invention shown, as shown in the figure, is provided with steam outlet and / or feeding port on the still head of the crystallizer, and the bottom of the still head is provided with annular spray pipe 2, toward the crystallizer inner wall direction Open the hole and wash the scale near the liquid level on the inner wall of the crystallizer. The diameter of the cylinder body 3 on the crystallizer is 1.2-1.3 times of the diameter of the middle straight barrel section 14, and the height is 0.7-1.4 times of the height of the middle straight barrel section 14, and the height of the middle straight barrel section 14 is 0.5-1.2 times of its own diameter. The cylinder and the middle straight barrel are connected with variable diameters. The diameter of the guide tube 5 is 0.6-0.8 times the diameter of the middle straight barrel section 14, and the height is 1.1-1.3 times the height of the middl...

Embodiment 2

[0047] For the system in which the solid mass in the final crystallization slurry feed liquid accounts for 10% to 25% of the total feed liquid mass, a two-stage continuous crystallization process can be used. like figure 2 Shown is a two-stage continuous reaction crystallization device and process for cephalexin, which consists of two-stage crystallizers connected in series. Brief technical process: under normal pressure, the cephalexin feed solution is dissolved and clarified when the pH is less than 1.5, and then crystals are precipitated by adding ammonia water. The temperature of the primary crystallizer is controlled at 25°C. Due to the exothermic reaction, the primary crystallizer needs an external cooling heat exchanger. In order to improve the process yield, the temperature of the secondary crystallizer is controlled at 15°C. The secondary crystallization requires an external cooling heat exchanger. device. Due to the fast reaction crystallization rate, in order to ...

Embodiment 3

[0053] For the system in which the solid mass in the final crystallization slurry feed liquid accounts for 25% to 40% of the total feed liquid mass, a three-stage continuous crystallization process can be used. like image 3 Shown is a three-stage continuous cooling crystallization device for continuous cooling and crystallization of vitamin C, which consists of three crystallizers connected in series. Brief technical process: under normal pressure, prepare a vitamin C aqueous solution with a concentration of 45-55%, heat up to 60°C to dissolve, cool down to 10°C and discharge. According to the solubility characteristics of vitamin C, the solid content and operating temperature of crystallizers at all levels are adjusted. The temperature of the primary crystallizer is controlled at 45°C, and its solid content is ~5%. The temperature of the secondary crystallizer is controlled at 33°C, and its solid content is ~20%. The temperature of the three-stage crystallizer is controlled...

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Abstract

The invention relates to a self-circulating crystallizer and a multistage continuous crystallization method. The crystallizer sequentially comprises a kettle head, an upper cylinder body, a middle cylinder body and a bottom hole-shrinkage cylinder body with a W-shaped bottom from top to bottom, wherein a steam outlet and / or a feeding hole are / is arranged on the kettle head, an annular spraying pipe is arranged at the lower part of the kettle head; a middle straight cylinder section is arranged in the middle cylinder body, a flow guiding cylinder is arranged in the middle straight cylinder section, and a stirrer is arranged in the flow guiding cylinder; the diameter of the middle cylinder body is larger than that of the upper cylinder body, and the diameter of the upper cylinder body is larger than that of the middle cylinder body; and the lower part of the upper cylinder body and the upper part of the middle cylinder body are respectively connected with the circumference of the top ofthe middle straight cylinder section via a hole-shrinkage transition section, and a discharging hole is formed in the W-shaped bottom. The invention provides the method for realizing multistage continuous evaporation, cooling or reaction crystallization through the series connection of the crystallizer, the prepared crystals are large in granularity and uniform in particle size, the problems thatthe product granularity is small, equipment is seriously scaled, a pipeline is blocked, and the like in the continuous crystallization process are improved, and the operation period of the continuouscrystallization process is prolonged.

Description

technical field [0001] The invention belongs to the technical fields of medicine and chemical industry, and relates to a self-circulating crystallizer and a multi-stage continuous crystallization method, which is applicable to various crystallization processes such as reaction crystallization, evaporation crystallization, and cooling crystallization. Background technique [0002] In the production of pharmaceutical and chemical industries, according to the operation mode, the crystallization process is divided into two modes: continuous crystallization and intermittent crystallization; according to the physical and chemical characteristics such as the solubility of the substance system, the crystallization process is divided into reaction crystallization, evaporation crystallization, cooling crystallization, and dissolution. Crystalline and other forms. The batch crystallization process is a crystallization process in which raw materials are added at one time, then different...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D9/02B01D1/30B01D1/26B01D1/00
CPCB01D1/0082B01D1/0088B01D1/26B01D1/30B01D9/0004B01D9/0018B01D9/0059B01D9/0063B01D2009/0086
Inventor 侯宝红龚俊波张美景李鸣晨尹秋响谢闯鲍颖王永莉王静康王玉德
Owner TIANJIN UNIV
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