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A kind of large particle diameter polyurethane phase change microcapsule and preparation method thereof

A phase change microcapsule, polyurethane technology, applied in the directions of microcapsule preparation, microsphere preparation, chemical instruments and methods, etc., can solve the problems of fast reaction rate, difficulty in microcapsule washing, purification, depending on preparation conditions, etc., and achieve violent reaction. The degree of reduction is beneficial to the exchange of heat energy, and the effect of optimizing the preparation process

Active Publication Date: 2021-08-10
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent application CN110215885A discloses "a preparation method of kaolinite polyurea phase-change microcapsules". This patent application uses kaolinite as a stabilizer for Pickering emulsion, and utilizes the condensation polymerization of IPDI and water at the interface of Pickering emulsion A kind of kaolinite polyurea phase change microcapsules was obtained by reaction coating paraffin, but the prepared microcapsules could only withstand the centrifugal washing at 4000 rpm, and the mechanical strength was poor
[0009] (1) When polyurea / polyurethane urea is used as the wall material to prepare microcapsules, the reaction rate between diamine monomers and isocyanate groups is extremely fast, which is difficult to control, and the resulting microcapsules have poor compactness and the core material is easy to leak; polyurea The wall material of microcapsules is brittle and has poor mechanical strength
[0010] (2) When ionic polyurethane is used as the wall material, although no emulsifier is used in the preparation process, there are hydrophilic anion or cationic groups in the molecular chain, which makes it difficult to wash and purify the microcapsules, and the prepared microcapsules are acid-resistant Alkaline and electrolyte resistance will also be poor
[0011] (3) The particle size of the phase change microcapsules prepared by the above patent application is less than 100 μm, the microcapsule wall is thin, and the thermal stability and compactness are poor
However, due to the instability of the emulsion, the traditional interfacial polymerization technology has certain limitations in increasing the wall thickness and diameter of the microcapsules, but these limitations depend on the preparation conditions

Method used

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  • A kind of large particle diameter polyurethane phase change microcapsule and preparation method thereof
  • A kind of large particle diameter polyurethane phase change microcapsule and preparation method thereof
  • A kind of large particle diameter polyurethane phase change microcapsule and preparation method thereof

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Effect test

Embodiment 1

[0040] A preparation method for large-diameter polyurethane phase-change microcapsules, comprising the following steps:

[0041] (1) Dissolve 25.00 g of isophorone diisocyanate and 5.00 g of polyethylene glycol (molecular weight 400) in 25.00 g of ethyl acetate, drop into 0.4 mL of dibutyltin dilaurate, under nitrogen protection, 50°C Under the condition of reaction 1 h, then add 110.40 g methyl laurate, obtain oily phase.

[0042] (2) Add 3 g of 20 wt% nano-titanium dioxide aqueous dispersion to 997 g of water to obtain 1000 g of nano-titanium dioxide aqueous dispersion with a concentration of 0.06 wt%, then add 5.00 g of pentaerythritol and stir well.

[0043] (3) Slowly add the oil phase prepared in step (1) into the dispersion prepared in step (2) under stirring at 300 rpm, continue stirring, and raise the temperature to 60 °C for 2.5 h.

[0044] (4) After the reaction is completed, the solid powder of polyurethane phase change microcapsules is obtained by suction filtrat...

Embodiment 2

[0046] A preparation method for large-diameter polyurethane phase-change microcapsules, comprising the following steps:

[0047](1) Dissolve 11.00 g of 2,4-toluene diisocyanate and 14.00 g of polytetrahydrofuran (molecular weight: 1000) in 25.00 g of toluene, drop into 0.2 mL of dibutyltin dilaurate, and react under nitrogen protection at 50 °C 1 h, and then add 128.80 g of n-octadecane to obtain an oily phase.

[0048] (2) Add 50.00 g of rutile nano-titanium dioxide to 1000.00 g of water, then add 27.50 g of glycerin, and stir well.

[0049] (3) Slowly add the oil phase prepared in step (1) into the dispersion prepared in step (2) under stirring at 400 rpm, continue stirring, and raise the temperature to 50 °C for 4 h.

[0050] (4) After the reaction is completed, filter with suction, wash with distilled water, and dry to obtain a solid powder of polyurethane phase change microcapsules. The average particle size is 103 μm, which can withstand 8000 rpm centrifugal washing and...

Embodiment 3

[0052] A preparation method for large-diameter polyurethane phase-change microcapsules, comprising the following steps:

[0053] (1) Dissolve 18.90 g of hexamethylene diisocyanate, 28.14 g of diphenylmethane diisocyanate and 50.00 g of polypropylene glycol (molecular weight 1000) in 48.53 g of ethyl acetate, drop into 0.3 mL of dibutyltin dilaurate, in Under nitrogen protection, the reaction was carried out at 50°C for 1 h, and then 147.2 g of butyl stearate was added to obtain an oil phase.

[0054] (2) Add 20.00 g of anatase nano-titanium dioxide to 1000.00 g of water, then add 50.00 g of trimethylolpropane, and stir well.

[0055] (3) Take the oil phase prepared in step (1) and slowly add it to the dispersion liquid prepared in step (2) under stirring at 250 rpm, continue stirring, and raise the temperature to 70 °C for 2 h.

[0056] (4) After the reaction is completed, filter with suction, wash with distilled water, and dry to obtain a solid powder of polyurethane phase c...

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Abstract

The invention discloses a large-diameter polyurethane phase-change microcapsule and a preparation method thereof. In this method, diisocyanate and diol are reacted to prepare polyurethane prepolymer, and then phase-change material is added and stirred evenly to obtain an oil phase; then, a nano-titanium dioxide aqueous dispersion is prepared, and water-soluble polyol is added to obtain a water phase; finally, the The prepared oil phase is added dropwise to the water phase under stirring to form a Pickering emulsion, and a condensation polymerization reaction occurs at the interface of the Pickering emulsion to form a polyurethane phase change microcapsule. After the reaction is completed, it is filtered by suction, washed with distilled water, and dried to obtain Polyurethane phase change microcapsule solid powder. The preparation method of the present invention does not require high-speed shear emulsification, does not need to use an emulsifier, and the reaction rate is controllable. The average particle size of the prepared phase change microcapsules is greater than 100 μm, and the thermal stability is good, the compactness is good, the mechanical strength is good, and the enthalpy is relatively high. high.

Description

technical field [0001] The invention belongs to the field of phase-change microcapsules, and in particular relates to a large-diameter polyurethane phase-change microcapsule and a preparation method thereof. Background technique [0002] In recent years, due to the continuous consumption of fossil fuels, environmental problems such as smog, global warming and ocean acidification have become increasingly serious. Adding to the concern, fossil fuel resources are finite and non-renewable. Therefore, researchers have begun to work on the efficient use of clean and sustainable energy. Especially in order to overcome the intermittency problem of most renewable energy sources, energy storage technology has received great attention, for example, thermal energy storage can be successfully realized by utilizing phase change materials as working media. [0003] Phase change material is a new type of energy storage material. It has the ability to absorb or release a large amount of la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/16C09K5/06
CPCB01J13/16C09K5/063
Inventor 马文石王志强
Owner SOUTH CHINA UNIV OF TECH