Preparation method of polyether ester random copolymer based on polyethylene furandicarboxylate
A technology for ethylene furandicarboxylate and diester furandicarboxylate is applied in the field of preparation of polyetherester random copolymers, and can solve the problems of narrow adjustable range of ether bond content, large amount of catalyst, expensive catalyst and the like, Achieve the effects of low cost, high activity, excellent gas barrier properties and mechanical strength
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[0033] A preparation method of polyether ester random copolymer based on polyethylene furandicarboxylate: comprising:
[0034] 1) With 2,5-furandicarboxylic acid and / or 2,5-furandicarboxylic acid diester and ethylene glycol as polymerized monomers with a molar ratio of 1:1.1-1:5, in the catalysis of multi-component organic sulfonic acid catalyst The esterification-etherification reaction is carried out at a temperature of 160-210°C, the reaction time is 2-5h, and the reaction pressure is normal pressure or positive pressure, and the polyether ester oligomer is obtained after the reaction.
[0035] 2) Add an organometallic catalyst to the polyether ester oligomer obtained in step 1) to carry out polycondensation reaction, the reaction temperature is 210-260°C, the reaction time is 1-6h, and the reaction pressure is less than 50Pa; after the reaction, the polyether ester is obtained Random copolymer, polyethylene furandicarboxylate-co-diethylene glycol ester.
[0036] Wherein, ...
Embodiment 1
[0048] Add 30.00g of 2,5-furandicarboxylic acid, 23.85g of ethylene glycol, and 0.072g of propanedisulfonic acid into a reactor protected by nitrogen, and react at 180°C for 1h, at 190°C for 1h, and at 200°C until No more water distilled out to obtain a polyether ester oligomer, then add 0.06g of dibutyltin oxide to the polyether ester oligomer, and react at 230°C for 1h under high vacuum conditions (figure 1 For the sample prepared in Example 1 1 H NMR spectrum; figure 2 DSC curve of the sample prepared for Example 1.
Embodiment 2
[0050] Add 30.00g of 2,5-furandicarboxylic acid, 23.85g of ethylene glycol, and 0.015g of propanedisulfonic acid into a reactor protected by nitrogen, and react at 180°C for 1h, at 190°C for 1h, and at 200°C until No more water distilled out to obtain a polyetherester oligomer; then add 0.06g of dibutyltin oxide to the polyetherester oligomer, and react at 230°C for 1h under high vacuum conditions (<50Pa), 240°C The reaction was carried out for 3 hours to obtain polyethylene furandicarboxylate-co-diethylene glycol ester, whose performance parameters are shown in Table 1.
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