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Study On Quantitative Characterization For Polarity Of Adsorption-Functional Polymers By Chromatography

Posted on:2012-02-13Degree:MasterType:Thesis
Country:ChinaCandidate:X J CaoFull Text:PDF
GTID:2131330332491253Subject:Chemical processes
Abstract/Summary:PDF Full Text Request
With the feature of absorption, adsorption-functional polymers play a role of concentration and separation in organic compounds. It is widely used in organic separation, wastewater treatment, pharmaceutical industry, petroleum industry, etc. Polarity is an important functional parameters for adsorption-functional polymers. At present, the technique conditions of Relative Polarities, McReynolds Constants, and Apparent Carbon Numbers, which characterize the polarity of the liquid materials by Gas Chromatography(GC) have already been very mature. While the characterization method of polarity of solid adsorption-functional polymers is studied less both at home and abroad. It still stays at the stage of qualitative expression of its polarity. The lassification of adsorption-functional polymers which divided qualitatively into non-polar, weakly polar and highly polar can not meet the needs of industrial production already. Therefore, through this project of researching the quantitative characterization of the polarity for adsorption-functional polymers, we aim to provide the basis for the application of adsorption-functional polymers.This thesis was based on researching the adsorption-functional polymers. The research started from the particle size of adsorption-functional polymers, which apply to the characterization of polarity by methods of chromatographic. Probe molecules, the column temperature, flow rate, and mobile phase were analysised for the effect to polarity characterization. Based on this, according to the models of Relative Polarities(P), McReynolds Constants(ΣΔI), and Apparent Carbon Numbers(△C ) calculated and characterizated the polarity of adsorption-functional polymers, we studied the characteriation rules of poarity and the accuracy of methods. Finally, through analyzing the advantages and disadvantages of the characterizaiton metheds and the mutual relationship, the better methods and operating conditions of characterizing adsorption-functional polymers were obtained. The main results were as follows:1. Research on quantitative characterization for polarity of adsorption-functional polymers by Gas Chromatography(GC):1) By studying the particle size of adsorption-functional polymers, which is appropriate for the characterization of polarity by chromatographic methods, we found that adsorption-functional polymers at 4090μm, which has the regular shape and small granule, would not plug the column, thus could be used as filler for GC column.2) By calculating the models of Relative Polarities(P), McReynolds Constants(ΣΔI), and Apparent Carbon Numbers(△C ), the column temperature was analysised for the effect to the retention time and polarity characterization. The column temperature which applying for the characterization of polarity for adsorption-functional polymers by chromatographic methods was studied. The results showed, the retention time of the probe molecules is shorten when the column temperature is rising through 100 to 160℃. The column temperature range influenced little on polarity characterization by Relative Polarities(P), McReynolds Constants(ΣΔI), and Apparent Carbon Numbers(△C ). Considering the low temperature help to extend the service life, 120℃was selected for the column temperature.3) According to the models of Relative Polarities(P), McReynolds Constants(ΣΔI), and Apparent Carbon Numbers(△C ) calculated the polarity of adsorption-functional polymers, we studied the characteriation rules of poarity and the accuracy of methods. The results showed,①The polarity of probe molecules influenced on the retention time. With the increasing polarity of the probe molecules, the retention time first increased and then decreased if the polar value <4.0, and reached a minimum at the polar value 4.3, the retained time first increased and then decreased if the polar value >4.3, and reached a maximum at the polar value 5.3. Using the benzene/hexane as the probe molecules, Relative Polarities(P) closely met with the perceive value, the relative average deviation was over 5% between the experimental values and the theoretic values, with low accuracy.②The relative average deviation of McReynolds Constants(ΣΔI) was over 5% between the experimental values and the theoretic values, with low accuracy.③The relative average deviation of Apparent Carbon Numbers(△C) was less than 5% between the experimental values and the theoretic values, with high accuracy.2. Research on quantitative characterization for polarity of adsorption-functional polymers by High Performance Liquid Chromatography (HPLC):1) The condition of HPLC methods for characterizing the polarity of adsorption-functional polymers had been researched, mainly includes particle size, column temperature and flow rate. The results showed that adsorption-functional polymers sized from 180 to 230μm with regulare shape, did not plug the column, thus was suitable as the filler for HPLC column. The retention time was influenced by the flow rate. 1.0mL/min was suitable for HPLC flow rate, for the retention time would be shorter and pump pressure was low. The column temperature from 30 to 60℃influenced a little on the retention time, taking the low temperature could prolong the useful time into account, 30℃is the better choice for column temperature.2) Single factor of the polarity of probe molecules and mobile phase influenced on polarity characterization and retention time had been studied through the methods Relative Polarities, and the rules of Relative Polarities(P) Characterization and accuracy were discussed. The results showed that the polarity of probe molecules influenced on the retention time, the materials with non-polar had longer retention time than the highly polar if the polar value<4.4; while the materials with highly polar had longer retention time than the non-polar if the polar value>4.4. Mobile phase polarity also influenced on the retention time. With the decreasing of mobile phase polarity, the retention time first decreased and then increased. When using the probe group of methanol/ethanol as the probe molecules and water as the mobile phase, the Relative Polarities(P) of functional polymer materials of adsorption closely met with the perceive value. Under these conditions, the relative average deviation of Relative Polarities was over 5% between the experimental values and the theoretic values, with low accuracy.3) Single factor of mobile phase which influenced on polarity characterization and retention time had been studied by the methods of McReynolds Constants(ΣΔI), and the rules of McReynolds Constants(ΣΔI) Characterization and accuracy were discussed. The results showed that single solvent of water, methanol, acetonitrile or mixed solvent of methanol:water = 3:7 were not suitable for mobile phase. Because McReynolds Constants(ΣΔI) could not be measured or the tested results did not match the prediction. Mixed solvent of methanol:water = 7:3 was coincided better with the prediction, so it was suitable as the mobile phase. Under this conditions, the relative average deviation of McReynolds Constants was over 5% between the experimental values and the theoretic values, with low accuracy.4) Single factor of mobile phase influencing on polarity characterization had been studied by the Apparent Carbon Numbers(△C ), and the rules of Apparent Carbon Numbers(△C ) Characterization and accuracy were discussed. The results showed that single solvent of water, methanol, acetonitrile or mixed solvent of methanol:water = 3:7, methanol:water = 7:3 were not suitable for mobile phase, for Apparent Carbon Numbers could not be measured or the tested results did not match the prediction.3. Several relationships of the characterization were obtained. The linear relationship of Relative Polarities was P2 = 1.0P1 +0.5; The linear relationship of McReynolds Constants wasΣΔI2 = 0.6ΣΔI1-28.5; The linear relationship between Relative Polarities and McReynolds Constants wereΣΔI1 = 13.7P1 +27.8,ΣΔI2 = 8.2P2-16.4; The linear relationship between Apparent Carbon Numbers and Relative Polarities was P1 = 25.4ΔC1-40.1; The linear relationship between Apparent Carbon Numbers and McReynolds Constants wasΣΔI1 = 349.4ΔC1-529.9. P = Relative Polarities,ΣΔI = McReynolds Constants,△C = Apparent Carbon Numbers, 1 = Gas Chromatography(GC), 2 = High Performance Liquid Chromatography (HPLC).4. Through analyzing the results of the study, the better methods and operating conditions of characterizing adsorption-functional polymers were obtained. We found that the better methods was Apparent Carbon Numbers(△C ), which is simple and with high accuracy. The separation was performed by Gas Chromatography(GC), the particle size of functional polymer materials of adsorption was 4090um, and nitrogen was used as the mobile phase at a pressure of 0.10MPa. The n-alkanes(C5C10) and n-alcohols(C2C8) were used as probe moleculars.
Keywords/Search Tags:Adsorption-functional polymers, Polarity, Chromatography, McReynolds constants, Apparent carbon numbers
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