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A kind of flame-retardant phase change microcapsule and preparation method thereof

A phase-change microcapsule, flame-retardant technology, applied in the directions of microcapsule preparation, microsphere preparation, chemical instruments and methods, etc., can solve the problem of low mechanical strength of the polymer capsule wall of phase change microcapsules, phosphonate monomers, etc. The reaction process is difficult to control, and the cross-linking density of the phase change microcapsule wall is low.

Inactive Publication Date: 2020-07-31
SICHUAN UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent CN 105542721A discloses a method for preparing flame-retardant phase-change microcapsules. The flame-retardant phase-change microcapsules are prepared by mixing flame retardant chlorinated paraffin into organic phase-change materials, but the flame-retardant and organic phase-change materials Physical blending reduces the content of phase-change substances in the microcapsules, thereby reducing the energy storage density of the phase-change microcapsules
[0006] Chinese patent CN 105112020A discloses another method for preparing flame-retardant phase-change microcapsules. A polymer capsule wall with certain flame-retardant properties is obtained by co-polymerizing reactive phosphonate monomers and acrylic acid monomers. However, phosphonate The monomer reaction process is difficult to control, and the polymer wall of phase change microcapsules has low mechanical strength
[0007] Chinese patent CN 103740337A prepares a phosphonate functional monomer, and prepares another flame-retardant microcapsule material by radical polymerization with acrylic acid monomer, but the preparation process of the microcapsule is cumbersome and the free radical polymerization The process is difficult to control, and the prepared phase change microcapsules have low cross-linking density

Method used

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  • A kind of flame-retardant phase change microcapsule and preparation method thereof
  • A kind of flame-retardant phase change microcapsule and preparation method thereof
  • A kind of flame-retardant phase change microcapsule and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0039] A preparation method of flame-retardant phase-change microcapsules, comprising the steps of:

[0040] S1. Mix 5mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 1mol 4,4'-diaminobenzophenone evenly and add them to the round bottom flask, heat up to Stir at 170°C for 5 hours;

[0041] S2. Cool down to 100°C, add 4kg of toluene to the round bottom flask and stir evenly, filter the reaction solution to obtain a filter cake and wash it with toluene;

[0042] S3. Dissolving the filter cake prepared in S2 in tetrahydrofuran and recrystallizing at -20°C, after filtering, drying the filter cake in a vacuum oven to obtain a phosphorus-containing diamine monomer;

[0043] S4. Mix 0.3kg of phosphorus-containing diamine monomer prepared in S3 with 1kg of melamine, 1.7kg of formaldehyde solution, and 3kg of deionized water, and adjust the pH value to 8.5 with triethanolamine, and stir and react at 70°C for 2h to obtain the prepared Polymer solution; wherein, in terms of w...

Embodiment 2

[0057] A preparation method of flame-retardant phase-change microcapsules, comprising the steps of:

[0058] S1. Mix 2mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 1mol 4,4'-diaminobenzophenone evenly and add to the round bottom flask, heat up to Stir at 150°C for 12 hours;

[0059] S2. Cool down to 80°C, add 1.3kg of toluene into the round bottom flask and stir evenly, filter the reaction solution to obtain a filter cake and wash it with toluene;

[0060] S3. Dissolving the filter cake prepared in S2 in tetrahydrofuran and recrystallizing at -20°C, after filtering, drying the filter cake in a vacuum oven to obtain a phosphorus-containing diamine monomer;

[0061] S4. Mix 0.1 kg of phosphorus-containing diamine monomer prepared in S3 with 1 kg of melamine, 1.5 kg of formaldehyde solution, and 1.5 kg of deionized water, adjust the pH value to 8.0 with triethanolamine, and stir and react at 60° C. for 4 hours to obtain Prepolymer solution; wherein, in terms of wei...

Embodiment 3

[0066] A preparation method of flame-retardant phase-change microcapsules, comprising the steps of:

[0067] S1. Mix 10mol 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 1mol 4,4'-diaminobenzophenone evenly and add them to the round bottom flask, heat up to Stir at 180°C for 1 hour;

[0068] S2. Cool down to 120°C, add 11.5kg of toluene to the round bottom flask and stir evenly, filter the reaction solution to obtain a filter cake and wash it with toluene;

[0069] S3. Dissolving the filter cake prepared in S2 in tetrahydrofuran and recrystallizing at -20°C, after filtering, drying the filter cake in a vacuum oven to obtain a phosphorus-containing diamine monomer;

[0070] S4. Mix 0.8 kg of phosphorus-containing diamine monomer prepared in S3 with 1 kg of melamine, 1.8 kg of formaldehyde solution, and 5 kg of deionized water, and adjust the pH value to 9.0 with triethanolamine, and stir and react at 80° C. for 1 hour to obtain the prepared Polymer solution; wherein, ...

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Abstract

The invention discloses a flame-retardant phase-change microcapsule and a preparation method thereof, and relates to the technical field of energy-saving materials. The capsule contains an organic phase-change material and a capsule wall wrapping the organic phase-change material; the general formula of the organic phase-change material is C n h 2n+2 straight-chain or branched-chain alkanes, the general formula is C n h 2n The higher fatty acid of COOH, the general formula is C n h 2n One or more of the higher fatty alcohols of OH, wherein, n=12-32; the capsule wall is made of phosphorus-containing diamine monomer, melamine, formaldehyde solution, emulsifier and deionized water. The flame-retardant phase-change microcapsules of the present invention use phosphorus-containing melamine-formaldehyde resin as the capsule wall material, which greatly improves the flame-retardant performance of the phase-change microcapsules, makes up for the flammability defects of organic phase-change materials, and can also avoid The direct mixing of flame retardants and organic phase change materials ensures that the phase change microcapsules have a high energy storage density.

Description

technical field [0001] The invention relates to the technical field of energy-saving materials, in particular to a flame-retardant phase-change microcapsule and a preparation method thereof. Background technique [0002] Energy is the basis for the survival and development of human society. With the increasing energy demand of human society and the increasing shortage of traditional energy, how to develop new energy and improve energy utilization has become an urgent task for scientists at home and abroad. Phase change materials (PCMs) are a class of functional materials that use the phase change process to absorb and release heat, and realize energy storage and temperature regulation during the phase change process. Phase-change energy storage materials can store unnecessary heat and release it when needed, thereby improving energy utilization. Therefore, phase-change energy storage materials are widely used in energy-saving buildings, solar energy storage, textile chemical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/18C09K5/06
CPCB01J13/18C09K5/06
Inventor 成煦杜晓声杜宗良王海波王双
Owner SICHUAN UNIV
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