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Method for measuring dissolvability of CO2-micromolecule-polymer system and quartz crystal microbalance

A technology of quartz crystals and small molecules, applied in measuring devices, analytical materials, instruments, etc., can solve the problem of inaccurate saturation solubility of small molecules and carbon dioxide.

Inactive Publication Date: 2012-08-01
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The technical problem to be solved by the present invention is to overcome the inaccurate defects of the saturated solubility of small molecules in the carbon dioxide-small molecule-polymer system measured in the prior art, and the common saturated solubility of small molecules and carbon dioxide, and provide a measurement Equipment and method for saturated solubility of carbon dioxide-small molecule-polymer system

Method used

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  • Method for measuring dissolvability of CO2-micromolecule-polymer system and quartz crystal microbalance
  • Method for measuring dissolvability of CO2-micromolecule-polymer system and quartz crystal microbalance
  • Method for measuring dissolvability of CO2-micromolecule-polymer system and quartz crystal microbalance

Examples

Experimental program
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Effect test

Embodiment 1

[0074] Example 1 Quartz crystal microbalance

[0075] like figure 1 As shown, a kind of quartz crystal microbalance provided by the present invention mainly includes a high pressure cell 1, a small molecule cell 2, a frequency feedback device 3, a gas supply device 4, a vacuum pump 5, a gas circulation pump 6 and A filtering device 9 . Wherein, the polymer pool 1 is used for placing quartz wafers and can be completely closed. The polymer pool 1 has a first temperature control device (not shown in the figure), a first pressure testing device (not shown in the figure) and a first vent valve (not shown in the figure). The small molecule pool 2 is used to store small molecule substances and can be completely closed. The small molecule pool 2 has a second temperature control device (not shown in the figure) and a second pressure testing device (not shown in the figure). The frequency feedback device 3 can detect and record the feedback frequency of the quartz wafer under differ...

Embodiment 2

[0084] (1) Place the quartz wafer with a clean base frequency of 5MHz in the high pressure pool 1, open the second valve 802 and the fourth valve 804, close the fifth valve 805 and the seventh valve 807, and use vacuum pump 5 to Evacuate the high pressure cell 1 and measure the actual fundamental frequency F at 60°C and under vacuum conditions 0 =5001847.12Hz;

[0085] (2) PMMA and chloroform are made into a solution with a concentration of 3wt%, and the solvent evaporation method is used to coat the quartz wafer. After vacuum drying, the quartz wafer is placed in the high-pressure pool 1, and the second valve 802 and the fourth valve are opened. 804, close the fifth valve 805 and the seventh valve 807, measure the frequency of the coated quartz wafer at 60°C and vacuum conditions, repeat the steps of vacuum drying and measurement until a stable frequency F is obtained p =5001001.12Hz; by Saurbrey formula, by F p -F 0 =-846.0Hz Calculate the quality Δm of the PMMA film on t...

Embodiment 3

[0098] The specific operation steps are the same as in Example 2. The quartz wafer with a clean base frequency of 6MHz is placed in the No. 1 pool to measure the actual base frequency. At the same time, PAA and ethanol are made into a solution with a concentration of 4wt%. After the quartz wafer is coated, the The PAA film thickness was measured, and the PAA film thickness was measured to be 0.07 μm. Place the coated quartz wafer and dimethyl sulfoxide in pool No. 1 and pool No. 2, respectively, and measure the pressure at 70°C in sequence: vacuum, 2MPa, 4MPa, 6MPa, 7MPa, 7.5MPa, 8MPa, 9MPa, 11MPa , 13MPa, 15MPa, 20MPa, 25MPa and 30MPa, CO 2 Solubility in PAA and CO 2 and DMSO in PAA co-solubility. The results show that under the test temperature and pressure, CO 2 The solubility in PAA increases with the increase of pressure, and the highest value reaches 0.198g (CO 2 ) / g(PAA); CO 2 The co-solubility of dimethyl sulfoxide and dimethyl sulfoxide in PAA increases with the ...

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Abstract

The invention discloses a quartz crystal microbalance, comprising a high pressure tank and a frequency feedback device connected with the high pressure tank as well as a micromolecule tank, a gas supply device, a vacuum pump, a filtering device and at least one gas circulation pump, wherein a macromolecule tank can be communicated with the micromolecule tank; the gas circulation pump is used for forming a double-tank circulation in the macromolecule tank, the micromolecule tank and the gas circulation pump or causing gas to form a single-tank circulation in the macromolecule tank and the gas circulation pump; the filtering device can be communicated with the micromolecule tank and a gas circulation device; and the gas supply device is used for supplying gas to the high pressure tank and / or micromolecule tank and causing a pressure in the high pressure tank and / or micromolecule tank to reach a test pressure, and the vacuum pump is used for vacuumizing the high pressure tank and / or the micromolecule tank. The invention also discloses a method for measuring dissolvability of a CO2-micromolecule-polymer system by utilizing the quartz crystal microbalance. The method disclosed by the invention is simple to operate, and the measured micromolecule saturated dissolvability and common saturated dissolvability of the micromolecule and CO2 are accurate.

Description

technical field [0001] The invention relates to a quartz crystal microbalance and a method for measuring the saturation solubility of a carbon dioxide-small molecule-polymer system by using the quartz crystal microbalance. Background technique [0002] High-pressure carbon dioxide refers to carbon dioxide when the pressure of the carbon dioxide system is higher than 5MPa. When the system temperature is higher than 31°C and the pressure is higher than 7.3MPa, carbon dioxide is called supercritical carbon dioxide. in supercritical CO 2 -In the polymer binary system, supercritical CO 2 The modification of polymers can be summarized as: supercritical CO 2 Plasticize the polymer, change the microenvironment of the polymer molecular chain, significantly increase the free volume of the polymer, improve the movement capacity of the polymer chain, and then change the CO 2 - Thermodynamic properties of polymers. These thermodynamic properties include: supercritical CO 2 Solubili...

Claims

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Application Information

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IPC IPC(8): G01N5/00
Inventor 曹贵平李雪坤朱正航
Owner EAST CHINA UNIV OF SCI & TECH
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