Page 56 - 《橡塑技术与装备》英文版2026年2期

HINA R&P TECHNOLOGY AND EQUIPMENT

The sample adhering to the inner wall of the rotary evaporation absorption peak of C-H stretching vibration of methyl groups
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flask was transferred to a beaker using a spatula to obtain the on the benzene ring; 1607 cm and 1481 cm represent the
test sample. characteristic absorption peaks of C=C stretching vibration
Synthesis of thermally crosslinked polyphenylene ether: in the toluene skeleton; 1 305 cm and 1 204 cm represent
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The PPO content of the three samples was 20%, 40%, and the characteristic absorption peaks of C-O vibration on the
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60%, respectively. The content of 2E4MZ was always 2% of benzene ring; 853 cm represents the characteristic absorption
the total mass of the blend. The required PPO, BNE-200, and peak of C-H bending vibration of methyl groups on the
2E4MZ for the three samples were added to three beakers, benzene ring. From the infrared spectrum, it can be seen that
and then an appropriate amount of tetrahydrofuran (about 50 the participation of benzoyl peroxide with different masses
ml for each sample) was added to the beakers and stirred to in the redistribution reaction does not change the molecular
dissolve the samples. After the tetrahydrofuran had completely structure of polyphenyl ether. After the reaction, the product
evaporated, the resulting solids were placed in a mortar only changes its molecular chain length, resulting in different
and ground into fine powder. The powders from different molecular weights.
beakers were then used to make different samples in different
proportions.
2.4 Polymer performance testing
Fourier Transform Infrared Spectrometer (FTIR) analysis
of sample chemical structure: Prepare the sample, using pure
potassium bromide sample for comparison. Mix the sample
with potassium bromide and pour into a crucible, grind them
thoroughly, and press them into a pellet.
Measurement of intrinsic viscosity using the Ubbelohde
viscometer: Prepare the sample by weighing 1.2 g of the
sample and dissolving it in 30 mL of xylene to obtain a test
sample with a concentration of 0.04 g/mL. Measure the efflux
Figure 3 Infrared spectrum of the redistribution reaction
time of a series of solutions using the dilution method (with
product PPO-2OH
pure solvent and at ½, ⅓, and ¼ of the initial concentration).
Differential scanning calorimetry (DSC) test: The 3.2 Determination and analysis of intrinsic
obtained samples were subjected to DSC analysis. First, a viscosity
blank control crucible was set up for blank control. For samples Dissolve the polyphenylene ether (PPE) sample from each
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1 , 2 , and 3 : The differential scanning calorimeter was set up redistribution reaction in xylene to form a solution with a mass
to operate in a nitrogen atmosphere, with the temperature range concentration of 0.04 g/ml, and measure it at room temperature
controlled between 50~280℃. 3~5 mg of sample was weighed, using an Ubbelohde viscometer. After calculating the intrinsic
and the heating rates were set to 5℃/min, 10℃/min, 15℃/min, 2(η sp −ln ηr )
viscosity according to the formula[[η]= , the
and 20℃/min, respectively. Finally, data statistics and analysis C
average molecular weight M1 of the BPO reaction product
were performed based on the obtained DSC test line graphs.
of PPO-10%PPO is calculated using the two-parameter
Mark-Houwink empirical formula:η=ΚΜ (According to the
α
3 Results and Discussion handbook of intrinsic viscosity-molecular weight relationship
3.1 Infrared spectroscopy analysis
parameters for polymers, in the PPE (polymer)-xylene (solvent)
The results are shown in Figure 3. In the figure, 3504 -2
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cm represents the characteristic absorption peak of O-H system, K=2.6×10 mL/g, α=0.69). Similarly, the average
molecular weight M2 of the BPO reaction product of PPO-
stretching vibration; 2950 cm represents the characteristic
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