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Preparation method of mannitol-silica core-shell structured PCM (phase-change material) microcapsule

A technology of silica and core-shell structure, which is applied in the direction of microcapsule preparation, microsphere preparation, chemical instruments and methods, etc., can solve the problems of thin shell layer and inability to prevent core material leakage, and achieve economical preparation process, high phase Enthalpy change and thermal cycle stability and controllability

Active Publication Date: 2014-09-17
ZHEJIANG UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

Philippe Poulin of France and Weihong Tan of the University of Florida in the United States prepared nanoparticles or microspheres with silica as the shell through W / O microemulsions, but the common disadvantage is that the shell is too thin to prevent the core during use. material leakage; recently British professor Mark R. Sambrook pointed out that a single tetraethoxysilane was used to prepare a thicker and structurally stable shell; but at the same time, Professor O'Sullivan of the University of Bristol The combination of silane and dimethyldiethoxysilane is easier to obtain a silica shell with better thickness and strength than tetraethoxysilane alone

Method used

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  • Preparation method of mannitol-silica core-shell structured PCM (phase-change material) microcapsule
  • Preparation method of mannitol-silica core-shell structured PCM (phase-change material) microcapsule

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preparation example Construction

[0020] The preparation method of mannitol-silica core-shell structure phase change material microcapsules includes the following steps:

[0021] 1) Mix surfactant A and organic solvent as a continuous phase at a mixing temperature of 40-80 o C, the concentration of surfactant A in the continuous phase is 0.5-3.0wt%;

[0022] 2) at 35-60 o Prepare a mannitol solution containing surfactant B as the dispersed phase under C, the concentration of the mannitol solution is 15-50wt%, and the concentration of surfactant B is 0.5-1.5wt%;

[0023] 3) Add the dispersed phase of step 2) to the continuous phase of step 1), stir and disperse for 1-100 minutes to form a stable W / O emulsion, and the volume ratio of the continuous phase to the dispersed phase is 1-100:1;

[0024] 4) Slowly add silicon source precursor C and silicon source precursor D to step 3) W / O emulsion and react for more than 5 hours to obtain silica-coated mannitol aqueous microcapsules. Silicon source precursor C and The volume ...

Embodiment 1

[0033] 1) Stir and mix Span80 with 130mL cyclohexane as the continuous phase, and keep the temperature of the mixture at 40 o C, the concentration of Span80 in the continuous phase is 0.5wt%;

[0034] 2) At 35 o Prepare 30 mL of mannitol solution containing sodium lauryl sulfate at C as the dispersed phase, the concentration of mannitol is 15 wt%, and the concentration of sodium lauryl sulfate is 0.5 wt%;

[0035] 3) Add the dispersed phase of step 2) to the continuous phase of step 1) and stir at high speed for 3.5 minutes to form a stable W / O emulsion;

[0036] 4) Put 18mL Si(OC 2 H 5 ) 4 And 7.0mL H 2 N(CH 2 ) 3 Si(OC 2 H 5 ) 3 Slowly and sequentially drip into step 3) W / O emulsion, react for 5 hours to obtain silica-coated mannitol aqueous microcapsules;

[0037] 5) Use 40 o Cyclohexane of C fully washes the silica-coated mannitol aqueous microcapsules obtained in step 4), and quickly reduces its temperature to below zero;

[0038] 6) Vacuum freeze-drying for 12 hours to obtain mann...

Embodiment 2

[0040] 1) Stir and mix Span80 with 130mL n-hexane as the continuous phase and keep the temperature of the mixture at 80 o C, the concentration of Span80 in the continuous phase is 3.0wt%;

[0041] 2) At 60 o Prepare 13 mL of mannitol solution containing sodium lauryl sulfate at C as the dispersed phase, the concentration of mannitol is 50 wt%, and the concentration of sodium lauryl sulfate is 1.5 wt%;

[0042] 3) Add the dispersed phase of step 2) to the continuous phase of step 1) and stir at high speed for 1 minute to form a stable W / O emulsion;

[0043] 4) Add 3.9mL SiCl 4 And 26mL H 2 N(CH 2 ) 3 Si(OCH 3 ) 3 Slowly and sequentially drip into step 3) W / O emulsion, react for 6 hours to obtain silica-coated mannitol aqueous microcapsules;

[0044] 5) Use 80 o Fully wash the silica-coated mannitol aqueous microcapsules obtained in step 4) with n-hexane in C, and quickly reduce its temperature to below zero;

[0045] 6) Vacuum freeze-drying for 12 hours to obtain mannitol-silica core-she...

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Abstract

The invention discloses a preparation method of a mannitol-silica core-shell structured PCM (phase-change material) microcapsule. The method comprises the following steps: preparing a mannitol solution serving as a dispersed phase and preparing an organic solution serving as a continuous phase to prepare a stable water-in-oil emulsion system; adding two kinds of silicon source precursors into the continuous phase in certain proportion so that the precursors are subjected to hydrolytic polycondensation at an oil-water interface to form a thickness-controllable silica capsule wall, thereby realizing the coating to the mannitol aqueous solution; and carrying out water removal so as to obtain a silica coated mannitol PCM microcapsule. The method disclosed by the invention firstly solves the microencapsulation problem of phase-change materials (used at a temperature of above 80 DEG C) under an approximate room temperature condition, and secondly solves the technical problems of the preparation of thick-walled silica microspheres. Through an appropriate raw material ratio and an appropriate process, a PCM microcapsule which has stable and good coating capacity is prepared, and the prepared PCM microcapsule can be applied to the fields of high-temperature thermal storage, protection and the like and has a high application potential.

Description

Technical field [0001] The invention relates to a preparation method of silicon oxide-coated sugar alcohol phase change material microcapsules, in particular to a preparation method of mannitol-silica core-shell structure phase change material microcapsules. It belongs to the field of preparation process of heat absorption and release energy storage materials. technical background [0002] Microencapsulation technology refers to the use of natural or synthetic polymer compounds to encapsulate solid, liquid or gas materials in a specific space. Due to its huge application prospects, it has attracted many scholars to conduct in-depth research. Since the first carbon paper was prepared using microencapsulation technology in the early 1950s, the technology has been widely used in various fields, such as cosmetics, pesticides, food, biology, medicine, and energy conservation. [0003] Because silica has many advantages such as good chemical stability, environmental friendliness, low to...

Claims

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Application Information

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IPC IPC(8): C09K5/06B01J13/02
Inventor 吴刚吴长波陈红征汪茫
Owner ZHEJIANG UNIV
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