研究目的
Investigating the synthesis, UV curing characteristics, and properties of a novel star-shaped, cardanol-based bio-prepolymer with inherent fire-retardancy.
研究成果
A novel star-shaped, cardanol-based bio-prepolymer with inherent fire-retardancy was successfully synthesized. The UV-cured films exhibited excellent thermal stability and fire-retardant properties, with LOI values over 24. The high Tg and crosslinking density of the films make them suitable for practical applications as surface coatings.
研究不足
The technical and application constraints include the need for long irradiation times for thick samples, which can lead to free radical degradation reactions of films. The thick samples were brittle and not suitable for LOI test.
1：Experimental Design and Method Selection:
The synthesis of a novel star-shaped, cardanol-based bio-prepolymer with a phosphazene core and six Cardanol arms. The chemical structures were characterized using NMR and FTIR. UV-curable mixtures were formulated and their photopolymerization dynamics were investigated using photo-DSC.
2：Sample Selection and Data Sources:
Cardanol (technical grade) was used as the starting material. Hexachlorocyclotriphosphazene (HCCP) was purified by recrystallization and vacuum-sublimation.
3：List of Experimental Equipment and Materials:
Bruker AV400 NMR spectrometer, Bruker Vertex 70 FTIR spectrometer, DSC Q2000 V
4：4 Build 116, Photo DSC Q2000, High Resolution STA 409PC thermogravimetric analyzer, PerkinElmer’s Diamond DMA, CMT4104 tensile testing machine, MCR302 SN81054732 rotational rheometer, Data physics instrument (OCA20), TC3000 instrument, Digital Abbe refractometer WAY-2S instrument. Experimental Procedures and Operational Workflow:
Synthesis of HCPP, EHCPP, and AEHCPP; preparation of UV crosslinked films; characterization of the chemical structure, thermal properties, and mechanical properties of the cured films.
5：Data Analysis Methods:
The conversion percentage of functional groups and polymerization rate were calculated from photo-DSC curves. The thermal stability and flame-retardant properties were analyzed using TGA and LOI calculations.
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Bruker AV400 NMR spectrometer
AV400
Bruker
Recording NMR spectrum at room temperature using deuterated solvents.
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Bruker Vertex 70 FTIR spectrometer
Vertex 70
Bruker
Measuring FTIR spectrum at 4 cm?1 resolution and a recording range of 4000–400 cm?1.
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PerkinElmer’s Diamond DMA
Diamond DMA
PerkinElmer
Collecting dynamic mechanical properties under tensile mode with a heating rate of 3 °C min?1 and at a fixed frequency of 1Hz.
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MCR302 SN81054732 rotational rheometer
MCR302 SN81054732
Anton Paar
Measuring the rheological behavior of UV-curable mixture with variable shear rates at 25 °C.
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DSC Q2000 V24.4 Build 116
Q2000 V24.4 Build 116
TA Instruments
Investigating the glass transition temperature (Tg) at a heating rate of 10 °C min?1 within a temperature range from -60 to 160 °C.
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Photo DSC Q2000
Q2000
TA Instruments
Studying the photopolymerization kinetics under nitrogen atmosphere with gas purging rate of 50 mL.min?1 during the test.
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High Resolution STA 409PC thermogravimetric analyzer
STA 409PC
Netzsch Instruments
Carrying out thermogravimetric analysis (TGA) with nitrogen flow rate of 60 mL.min?1 and a heating rate of 10 °C min?1 in the scanning range from 40°C to 850°C.
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CMT4104 tensile testing machine
CMT4104
Switzerland
Testing the tensile strength, elongation at breakage of the dumbbell-shaped sample under ambient condition.
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Data physics instrument (OCA20)
OCA20
Germany
Studying the surface properties of coatings by measuring static contact angles.
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TC3000 instrument
TC3000
Xiatech Electronics Co., Ltd
Measuring the thermal conductivity according to ASTM D5930-2001.
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Digital Abbe refractometer WAY-2S instrument
WAY-2S
Shanghai Changfang Optical Instrument Co., LTD
Measuring the refractive index at 25°C.
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