Abstract
The polyethylene glycol allyl glycidyl ether (PGAGE) is an important intermediate for preparing silicone softener that can be synthesized from allyl alcohol polyoxyethylene ether and epichlorohydrin (ECH). The performance parameters including the concentration of ECH, initial boron trifluoride diethyl etherate (BFEE) as well as CaCl2 quality were investigated respectively. The optimum process parameters which can get high capping and low by-product rate are as follows: the ECH concentration is 2.0 M, the initial BFEE concentration is 1.65mM, and the CaCl2 dosage is 1.65g/L. Under these conditions, the maximal yield can be improved to 91.36%, the percent of capping rate is higher than 98.16%, the residual concentration of F-is only 0.63 mg/L.
Highlights
Polyethylene glycol allyl glycidyl ether (PGAGE) and the allyl polyoxyethylene ether (APEG), tethering with both alkene and epoxy groups, are widely used as fabric finishing agent [1,2], reactive diluent [3], cross-linking agent, chemical fixation of carbon dioxide [4,5], and nonionic surfactants for detergents.[6]
The maximal yield can be improved achieved to be 91.36%, the percent of capping rate is higher than 98.16%, the residual concentration of Fis only 0.63 mg/L
NMR was used to confirm the structure of PGAGE. 1H NMR spectra of APEG and PGAGE are shown in Figure1 and Figure 2, The average degree of polymerization ( DP )
Summary
Polyethylene glycol allyl glycidyl ether (PGAGE) and the allyl polyoxyethylene ether (APEG), tethering with both alkene and epoxy groups, are widely used as fabric finishing agent [1,2] , reactive diluent [3] , cross-linking agent, chemical fixation of carbon dioxide [4,5], and nonionic surfactants for detergents.[6]. Allyl alcohol α -mono-chlorohydrin ether can convert to the APEG via the action occurring in concentrated basic solution, in which the total yield was between 90%~91% by Matsuoka et al [10] use the two-step reaction to synthesize AGE based on the reaction of allyl alcohol with ECH using BFEE as the catalyst. Their results demonstrated that the yield reaches 82% under the following condition: n (ECH) : n (allyl alcohol): (catalysis) = 1: (1~3) : (0.01~0.002). The maximal yield can be improved achieved to be 91.36%, the percent of capping rate is higher than 98.16%, the residual concentration of Fis only 0.63 mg/L
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