Rapid mercury-free photochemical microencapsulation/nanoencapsulation at ambient conditions

Inventors

Kurdi, JamalFarid, Mohammed

Assignees

Auckland In New Zealand, University ofDoha For Science & Technology, University ofAuckland Uniservices LtdDoha For Science And Technology, University of

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Publication Number

US-12233434-B2

Patent

Publication Date

2025-02-25

Expiration Date


Abstract

A method of mercury-free photochemical micro-/nano-encapsulation of an active material is a process for obtaining micro-/nano-capsules by means of curing by UV LED radiation at ambient or even cold temperatures. A stirrer photo-reactor made from glass or transparent plastics can be used but mixed flow reactor could be also employed. Appropriate mixing is sufficient to expose all droplets, which contain an active material surrounded by curable-shell materials in the emulsion to the LED radiation. Using the optimum light intensities and reactions' times is critical for encapsulating the active material with a high efficiency and producing a high quality micro-/nano-capsules, Solar monochromator device can also be used as long as it generate the same radiation with a narrow/single wavelengths as the LED device. Light emitted diode (LED) is a mercury-free UV radiation source with a long operating life time and an instant ON-Off. it has a high efficiency, a very low cooling requirements and cost-efficient in photochemical encapsulation. It reduces the time of microencapsulation from 6 hours to a less than 5 minutes. It has a significant decrease in manufacturing cost, waste-water, unconverted monomers, and leftover active phase change material (PCM) compared to other methods. Conversion of more than 90% of monomers can be achieved, and encapsulation efficiency can reach 100% at optimum conditions. This is in addition to the ability of this invented technology for encapsulate volatile and heat sensitive active materials at ambient as well as low temperatures. Normal glass or transparent plastics can be used as a reactor material. Only the matched useful wavelength radiation is emitted by LED without having other wavelengths which might have a bad impact on the encapsulation process.

Core Innovation

The invention relates to mercury-free UV or UV/Visible LED photochemical microencapsulation or nanoencapsulation of a phase change active material with a curable material at ambient or cold temperature for five minutes or less. The curable material comprises a mono-functional monomer, and the photochemical encapsulation uses LED radiation with narrow or single wavelength, including a solar monochromator.

The photoreactor includes a transparent tube equipped with a helix stirrer that can be fit inside the tube, and at least one LED lamp with adjustable light intensities. The microencapsulation or nanoencapsulation is carried out with discontinuous droplets phase formed by emulsion preparation including the active material, the curable shell material, and a photo-initiator, together with sufficient mixing exposure of droplets to irradiation.

The transparent photoreactor is configured for photochemical curing under LED wavelength and irradiation conditions that achieve high monomer conversion and high encapsulation efficiency while reducing process time compared to mercury lamps and thermal encapsulation. Documented outcomes include monomer conversion greater than 90% and encapsulation efficiency up to about 100%, with efficiency strongly dependent on radiation intensity and irradiation time.

The disclosed approach is described in the context of reducing energy and waste compared to mercury lamps, and addressing oxygen or wavelength selectivity effects associated with photochemical encapsulation. The use of narrow or single wavelength LED radiation, or a solar monochromator, is presented as enabling selection of irradiation conditions while maintaining encapsulation performance at ambient or cold temperature in minutes or less.

Claims Coverage

Independent claim clm-00001 defines an LED stirrer photoreactor for photochemical microencapsulation or nanoencapsulation at ambient or cold temperature for five minutes or less, with a curable material that comprises a mono-functional monomer. The independent claim is refined by seven inventive features specifying reactor structure, lighting configurations, timing, and curable material composition.

LED stirrer photoreactor for photochemical microencapsulation or nanoencapsulation

An LED stirrer photoreactor for photochemical microencapsulation or nanoencapsulation of a phase change active material at ambient or cold temperature for five minutes or less, wherein the curable material comprises a mono-functional monomer.

Transparent tube with helix stirrer

A transparent tube equipped with a helix stirrer that can be fit inside the tube.

Adjustable-intensity LED lamp(s)

At least one LED lamp with adjustable light intensities.

Transparent tube made of glass with a specified diameter

The photoreactor includes a transparent tube made of glass with a diameter of 3.5 cm.

Two LED lamps at 365 nm and specified intensity

The photoreactor includes two LED lamps, each emitting radiation at a wavelength of 365 nm with an intensity of 0.6 W/cm2.

Encapsulation at ambient or cold temperature for less than five

The photoreactor is used for microencapsulation or nanoencapsulation at ambient or cold temperature for less than five.

Multiple LEDs configuration

The photoreactor includes more than one LED light.

Curable material with additional monomers beyond mono-functional monomer

The photoreactor is configured so that the curable material includes an additional mono-functional monomer or a di-, tri-, or poly-functional monomer.

Overall claim coverage centers on an LED stirrer photoreactor that enables photochemical microencapsulation or nanoencapsulation of a phase change active material at ambient or cold temperature for five minutes or less, using a curable material comprising a mono-functional monomer. The inventive features further specify a transparent tube with a helix stirrer, glass tube dimensions, LED wavelength and intensity arrangements, a less-than-five timing constraint, multi-LED configurations, and inclusion of additional mono-functional or di-, tri-, or poly-functional monomers in the curable material.

Stated Advantages

Mercury-free UV or UV/Visible LED photochemical encapsulation is presented as reducing process time compared to hours and as enabling five minutes or less at ambient or cold temperature.

Achieves high monomer conversion greater than 90%.

Achieves encapsulation efficiency up to about 100%.

Reduces energy and waste compared to mercury lamps and thermal encapsulation.

Uses narrow or single wavelength LED radiation, or a solar monochromator, to address oxygen or wavelength selectivity effects associated with photochemical encapsulation.

Documented Applications

Photochemical microencapsulation or nanoencapsulation of a phase change active material using mercury-free UV or UV/Visible LED radiation at ambient or cold temperature for five minutes or less.

Encapsulation performance comparison context versus mercury lamps and thermal encapsulation, including reported outcomes tied to monomer conversion and encapsulation efficiency.

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