Multi-section feeding type anti-solvent spraying crystallizer and spraying crystallization method thereof

A tubular crystallizer and anti-solvent technology, applied in solution crystallization, alkali metal chloride, organic chemistry, etc., can solve the problems of slow crystallization process, wide particle size distribution, uneven supersaturation distribution, etc. The effect of small diameter, rapid nucleation, and narrow particle size distribution

Active Publication Date: 2018-01-09
SOUTHEAST UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Technical problem: The purpose of this invention is to provide a multi-stage feed anti-solvent spray crystallizer and its spray crystallization method, which is mainly used to solve the slow crystallization process and uneven distribution of supersaturation in the existing commonly used anti-solvent crystallization technology , Uncontrollable particle size of crystallized products, wide particle size distribution, etc.

Method used

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  • Multi-section feeding type anti-solvent spraying crystallizer and spraying crystallization method thereof
  • Multi-section feeding type anti-solvent spraying crystallizer and spraying crystallization method thereof
  • Multi-section feeding type anti-solvent spraying crystallizer and spraying crystallization method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Sodium chloride crystal particles are prepared by using a jet crystallizer with double-stage feeding. The central tube of the jet crystallizer is a round tube with an inner diameter of 10mm. There are four tubes with a diameter of 2mm evenly distributed on the two tube walls at a distance of 50mm and 100mm from the entrance of the round tube. The small hole, the total length of the spray crystallizer tube is 300mm.

[0027] Ethanol is used as anti-solvent at normal temperature, and the flow rate is 500L / h, and it enters the spray crystallizer from the feed port of the central tube of the spray crystallizer. The sodium chloride aqueous solution fed into the first stage has a concentration of 200g / L. After entering the buffer chamber from the feed side hole of the first stage of the spray crystallizer, it is sprayed into the central circular pipe through the small hole, and the flow rate is 100L / h. The sodium chloride aqueous solution fed in the second stage has a concent...

Embodiment 2

[0029] The spray crystallizer with three-stage feed is used to prepare urapidil crystal particles. The central tube of the spray crystallizer is a round tube with an inner diameter of 15mm, and there are two symmetrically distributed tube walls at 40mm, 80mm, and 120mm from the entrance of the round tube. A slit with a length of 4mm and a width of 2mm, the total length of the spray crystallizer tube is 350mm.

[0030] Petroleum ether is used as an anti-solvent at normal temperature, with a flow rate of 700L / h, and enters the jet crystallizer from the feed port of the central tube of the jet crystallizer. The urapidil chloroform solution concentration of the first stage feed is 250g / L, after entering the buffer chamber from the first stage feed side hole of the jet crystallizer, it is sprayed into the central circular pipe by the slit, and the flow rate is 100L / h. The urapidil chloroform solution concentration of the second stage feed is 300g / L, after entering the buffer chambe...

Embodiment 3

[0032] Hexanitrohexaazaisowurtzitane (CL-20) crystal particles were prepared by using a three-stage feeding jet crystallizer. The center tube of the jet crystallizer was a circular tube with an inner diameter of 20mm, and the distance from the entrance of the circular tube was 50mm, 100mm, and 150mm. There are 4 circular holes with a diameter of 3mm distributed symmetrically on the three pipe walls, and the total length of the spray crystallizer circular pipe is 450mm.

[0033]At room temperature, n-heptane is used as an anti-solvent with a flow rate of 700L / h, and it enters the jet crystallizer from the feed port of the central tube of the jet crystallizer. The concentration of CL-20 ethyl acetate solution fed into the first stage is 300g / L. After entering the buffer chamber from the feed side hole of the first stage of the jet crystallizer, it is sprayed into the central circular pipe through the small hole, and the flow rate is 100L / h. The concentration of the CL-20 ethyl a...

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Abstract

The invention provides a multi-section feeding type anti-solvent spraying crystallizer and a spraying crystallization method thereof. The crystallizer is a tubular crystallizer which is vertically arranged, wherein a main pipe inlet (1) is formed in the upper part of the tubular crystallizer; small holes or slits (2) which are symmetrically distributed are formed in positions with different heights of a main pipe wall from top to bottom; buffering chambers (3) are arranged around the small holes or the slits (2) in the positions with the same height; a side feeding opening (4) is formed in each buffering chamber; a main pipe outlet (5) is formed in the lower part of the tubular crystallizer. According to the multi-section feeding type anti-solvent spraying crystallizer provided by the invention, a solution system A with a certain concentration is prepared by dissolving heterocyclic organic medicine particles, inorganic salt or oxide and particles P of a nitryl energy-containing material into a good solvent S; crude particles P are recrystallized by adopting the tubular crystallizer; the solution system A and a bad solvent are rapidly mixed to continually form a crystal nucleus andthe crystal nucleus grows continually; finally, a suspension solution containing fine particles P is obtained at an outlet of the spraying crystallizer. The particle products obtained by the method have the advantages of controllable grain diameter sizes and distribution, narrow grain diameter distribution and the like.

Description

technical field [0001] The invention relates to a technology for preparing powder products through anti-solvent spray crystallization, which belongs to the technical field of industrial crystallization. Background technique [0002] The methods of crystallization from solution mainly include cooling crystallization method, solvent evaporation crystallization method and anti-solvent method, among which anti-solvent crystallization method has the characteristics of simple operation and easy realization, and has been widely used in industrial production. Anti-solvent crystallization operations mainly include drop crystallization and spray crystallization. [0003] The dropwise crystallization method is usually carried out in a stirred tank, and the solvent with crystals dissolved is added dropwise to the antisolvent, and stirred while adding to promote mixing. For example, the patent CN 106188071 A discloses that a solvent containing HNIW is first added dropwise to the antisolv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02C07D487/22C07D239/545C01D3/04
Inventor 骆培成邬斌葛裕华吕龙史良伟
Owner SOUTHEAST UNIV
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