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Method for preparing coated crystals through microencapsulated crystallizing

A technology of microcapsules and internal crystallization, applied in the field of microcapsule preparation and crystallization, can solve the problems of low crystal coating rate, poor crystal protection effect, crystal morphology and property control, etc.

Inactive Publication Date: 2018-10-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned coating methods all cover the crystal after the crystal is formed, and separate the crystallization process from the coating process. After coating, the morphology and properties of the crystal can no longer be controlled. The coverage rate is low, and the protection effect on the crystal is also poor

Method used

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  • Method for preparing coated crystals through microencapsulated crystallizing
  • Method for preparing coated crystals through microencapsulated crystallizing
  • Method for preparing coated crystals through microencapsulated crystallizing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0045] The continuous phase uses water as a solvent, prepares two equal volumes, respectively adds 2% polyethylene glycol 20000 as a protective colloid to the two solvents, stirs thoroughly to completely dissolve the polyethylene glycol 20000, and adds 3% Tween 80 was used as a surfactant, and 10% of 0.5 mol / L 1,6-hexanediamine was added to the other part as a reactive monomer.

[0046] The dispersed phase uses a mixed solution of chloroform and cyclohexane as a solvent, and the volume ratio of chloroform and cyclohexane is 2:1. The volume ratio of dispersed phase and continuous phase is 1:2. The vanillin to be crystallized is dissolved in the dispersed phase, and 10% of 0.5 mol / L terephthaloyl chloride is added as a reaction monomer.

[0047] The microchannel used is composed of two focused flow microchannel modules coupled. The internal flow pattern of the first module is a cross type. A stainless steel pipe with an outer diameter of 0.31mm and an inner diameter of 0.16mm ...

Embodiment approach 2

[0052] For the continuous phase, a mixed solution of chloroform and cyclohexane with a volume ratio of 1:1 was used as a solvent, and two equal volumes were prepared, one was added with 2% Span 85 as a surfactant, and the other was dissolved with 20% of 1mol / L of terephthaloyl chloride as a reactive monomer. The dispersed phase uses water as a solvent, and 5% polyethylene glycol 20000 added to the water is used as a protective colloid, and 20% of 1mol / L 1,2-ethylenediamine and glycine to be crystallized are added, and the dispersed phase and the continuous phase The volume ratio is 1:3.

[0053] The microchannel used is composed of two focused flow microchannel modules coupled. The internal flow pattern of the first module is a cross type. A stainless steel pipe with an outer diameter of 0.31mm and an inner diameter of 0.16mm is inserted into the center of the PVC pipe. The outer diameter of the PVC pipe is 1.4mm and the inner diameter is 1.0mm. The internal flow type of th...

Embodiment approach 3

[0058] Prepare two equal volumes of continuous phase with water as solvent, add 5% polyethylene glycol 20000 as protective colloid to the two solvents respectively, stir well to dissolve polyethylene glycol 20000 completely, and add 2 % Tween 80 was used as a surfactant, and 10% of 1 mol / L 1,6-hexanediamine was added to the other part as a reactive monomer. The dispersed phase uses a mixed solution of chloroform and cyclohexane as a solvent, and the volume ratio of chloroform and cyclohexane is 2:1. The volume ratio of dispersed phase and continuous phase is 1:3. The vanillin to be crystallized is dissolved in the dispersed phase, and 10% of 1 mol / L terephthaloyl chloride is added as a reaction monomer.

[0059] Add the continuous phase solution without adding monomer to the dispersed phase solution into the three-necked flask, and stir at a constant speed of 8000r / min to form an emulsion. After the emulsion is stable, add the continuous phase solution dissolved in 1,6-hexan...

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Abstract

The invention relates to a method for preparing coated crystals through microencapsulated crystallizing. According to the method, firstly, a solution containing substances to be crystallized is microencapsulated by an interfacial polymerization method, namely, liquid droplets are formed firstly by using a microchannel interior shearing action or direct stirring action and then are coated by usinga polymerization reaction between interfaces of a dispersed phase and a continuous phase so as to form microcapsules. Then, by using the permeability of a microcapsule macromolecular wall material that the microcapsule macromolecular wall material has properties of a semi-permeable membrane and only water and other micromolecular substances can permeate, a solvent is evaporated under certain conditions to form crystals, and thus, encapsulated controllable crystallizing operation is achieved. Then, prepared microcapsules are introduced into an evaporating dish. In the evaporating dish, corresponding temperature and heating time are selected according to a boiling point of the selected solvent to achieve an encapsulated crystallization process, and the crystals meeting conditions are obtained. After the crystals are formed, the microcapsules are subjected to freeze-drying treatment to thoroughly remove the solvent, then, capsule walls of the microcapsules shrink, and thus, the coating ofthe crystals is achieved.

Description

technical field [0001] The invention relates to the field of microcapsule preparation and crystallization, in particular to a method for preparing film-coated crystals through microcapsule internal crystallization. Background technique [0002] As a traditional separation process, crystallization has the advantages of low energy consumption and high selectivity. With the development of crystal engineering, process crystallization technology and other related fields, the requirements for crystal quality are getting higher and higher. Crystal size distribution (CSD) and crystal morphology are very important quality indicators, which directly affect the purity of crystals, as well as follow-up operations such as filtration, washing, and drying. techniques and changing the anti-solvent addition rate, etc. In addition, it is necessary to determine the crystal form according to different application requirements. The formulation of a specific form of crystal mainly depends on ad...

Claims

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Application Information

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IPC IPC(8): B01J13/12B01J13/16B01D9/00
CPCB01D9/0018B01J13/12B01J13/16
Inventor 王靖涛黄炎孟子超
Owner TIANJIN UNIV
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