Quality Control of Columns for High-Temperature Gel-Permeation Chromatography

Author(s):  
A. Willem deGroot
2010 ◽  
Vol 139-141 ◽  
pp. 661-665
Author(s):  
Yu Zhou ◽  
Bo Wen Cheng ◽  
Zhen Huan Li ◽  
De Xin Shen ◽  
Sheng Zhang ◽  
...  

A linear and high molecular weight poly(phenylene sulfide) (PPS) was synthesized from P-dichlorobenzene (P-DCB) and anhydrous sodium sulfide in N-methyl pyrrolidone (NMP), and the High Temperature Gel Permeation Chromatography (HTGPC) technique was utilized to investigate the effects of reaction condition on PPS chain propagation. The experiment results indicated that the high pro-reaction temperature or high post-temperature would interfere with PPS chain propagation, and post-reaction time was another important factor to influence PPS molecular weight (Mw) extension. Furthermore, the optimized ratio of high Mw PPS polymer synthesis was typically at 3-6% molar excess of Na2S over p-dichlorobenzene, and N-methyl-2-pyrrolidone (NMP) were beneficial to the production of high Mw PPS due to the formation of sodium 4-(N-methylamino) butanoate (SMAB). The alkaline reagents such as Na3PO4 and K3PO4 et al could capture the H of -SH, which changed -SH into -SNa and promoted the chain growth of PPS to achieve extension.


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