In situ determination for polymer conformation and crystal-form variation in supercritical fluid infrared spectrum

A technology of supercritical fluid and infrared spectroscopy, which is used in the field of conformation and crystal form changes of high-molecular polymers, and can solve the problems of inability to obtain changes and trends.

Inactive Publication Date: 2006-08-16
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
  • Application Information

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Problems solved by technology

Therefore, the changes and trends during the act

Method used

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  • In situ determination for polymer conformation and crystal-form variation in supercritical fluid infrared spectrum
  • In situ determination for polymer conformation and crystal-form variation in supercritical fluid infrared spectrum
  • In situ determination for polymer conformation and crystal-form variation in supercritical fluid infrared spectrum

Examples

Experimental program
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Effect test

Embodiment 1

[0039] An isotactic polypropylene membrane with a diameter of 0.5 cm and a thickness of 0.1 mm was placed in an in-situ Fourier transform infrared spectrometer equipped with a high-pressure infrared cell, and then carbon dioxide was charged into the system through a high-pressure syringe pump to maintain its temperature at 100 °C. The pressure is 10MPa, making it reach the supercritical state, and keep it for 48 hours. Use infrared spectroscopy to scan the infrared spectrum every 20min. Through the analysis of the infrared spectrum, it is found that the intensity of the absorption peak corresponding to the crystallization gradually increases with time, and reaches equilibrium in about 3 hours, that is to say, supercritical carbon dioxide has an induced crystallization effect on isotactic polypropylene.

[0040] Differential scanning calorimetry (DSC) analysis of isotactic polypropylene membranes before and after the experiment showed a significant increase in crystallinity, co...

Embodiment 2

[0042]A polyethylene diaphragm with a diameter of 0.5 cm and a thickness of 0.5 mm was placed in an in-situ Fourier transform infrared spectrometer equipped with a high-pressure infrared cell, and then propane was charged into the system through a high-pressure syringe pump to maintain its temperature at 150 °C and pressure It is 15MPa, making it reach the supercritical state and keep it for 48 hours. Use infrared spectroscopy to scan the infrared spectrum every 10min. By analyzing the infrared spectrum, it is found that the intensity of the absorption peak corresponding to the crystal does not change significantly with time, that is to say, the interaction between supercritical propane and polyethylene is very weak. This phenomenon was confirmed by differential scanning calorimetry (DSC) analysis of polyethylene membranes before and after the experiment. See Figure 4 and Figure 5 .

Embodiment 3

[0044] A syndiotactic polypropylene diaphragm with a diameter of 0.5 cm and a thickness of 0.2 mm was placed in an in-situ Fourier transform infrared spectrometer equipped with a high-pressure infrared cell, and then ethylene was charged into the system through a high-pressure syringe pump to maintain its temperature at 60 °C. The pressure is 20MPa, making it reach the supercritical state, and keep it for 48 hours. Use infrared spectroscopy to scan the infrared spectrum every 5min. Through the analysis of the infrared spectrum, it is found that the intensity of the absorption peak corresponding to the unstable crystal form gradually weakens with time, and the intensity of the absorption peak corresponding to the stable crystal form gradually increases with time, and reaches equilibrium in about 2 hours, that is, Supercritical ethylene promotes the transformation of the crystal form of syndiotactic polypropylene from an unstable state to a stable state. Differential scanning c...

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Abstract

A method for analyzing conformation and crystal-form of polymer in supercritical environment at home position includes setting said polymer in home position Fourier transform infrared spectrum with high pressure infrared pool, injecting supercritical fluid into said pool to carry out home position measurement of infrared spectrogram for polymer, measuring out conformation and crystal-form variation in acting to each other procedure of polymer with supercritical carbon dioxide by carrying out analysis on infrared spectrogram.

Description

technical field [0001] The invention relates to a method for measuring conformation and crystal form changes of high molecular polymers in a supercritical fluid environment by using in-situ infrared spectroscopy. Background technique [0002] Supercritical fluid refers to a fluid whose temperature and pressure are above the critical point. It is a fluid state between gas and liquid, with a density close to that of liquid and a viscosity close to that of gas. Supercritical fluids have unmatched solvency, fluidity and transfer properties that traditional solvents cannot match. In recent years, supercritical fluids have been widely used in chemical reactions, extraction and separation, and polymer processing. In the process of polymer processing using supercritical fluids, supercritical fluids such as supercritical carbon dioxide can swell and plasticize polymers. When carbon dioxide molecules interact with polymers, they can change the polymer Polymer conformation and crysta...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N21/25
Inventor 赵玲李斌曹贵平刘涛许志美袁渭康
Owner CHINA PETROLEUM & CHEM CORP
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