A kind of preparation method of heat-resistant bio-based block copolyester
A block copolyester and bio-based technology, which is applied in the field of polyester preparation, can solve the problems of low heat resistance and poor polyester degradation of degradable polyester, and achieve good hue, high degradability and heat resistance , The process method is simple and easy to implement
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Embodiment 1
[0028] Embodiment 1: A kind of preparation method of heat-resistant bio-based block copolyester comprises the following preparation steps:
[0029] 1) Mix 100g of 2,5-furandicarboxylic acid, 64g of ethylene glycol, 0.1g of catalyst, and 0.1g of stabilizer, and carry out esterification reaction at 195°C to prepare esterified product A;
[0030] 2) Mix 100g of 2,3-dibromo-1,4-butanediol, 109g of phenylboronic acid, 27mg of tetrakistriphenylphosphine palladium, 10g of 1mol / L sodium carbonate solution, and 50ml of toluene at 90°C under a nitrogen atmosphere Insulated reaction for 2 hours, diol A was obtained after precipitation by a poor solvent n-hexane;
[0031] 3) Put 100g of diol A, 40g of 1,4-succinic acid, 0.1g of n-butyl titanate and 0.1g of thermal stabilizer 1010 in a reaction kettle, and carry out esterification reaction at 220°C to prepare an esterified product B;
[0032] 4) Insulate the esterified product B at 245°C and 200pa for 0.5h for precondensation reaction to...
Embodiment 2
[0034] Embodiment 2: A kind of preparation method of heat-resistant bio-based block copolyester comprises the following preparation steps:
[0035] 1) Mix 100g of 2,5-furandicarboxylic acid, 64g of ethylene glycol, 0.1g of catalyst, and 0.1g of stabilizer, and carry out esterification reaction at 195°C to prepare esterified product A;
[0036] 2) Mix 100g of 2,3-diiodo-1,4-butanediol, 82g of phenylboronic acid, 10mg of palladium acetate, 10g of 1mol / L potassium carbonate solution, and 50ml of chloroform, and keep the reaction at 70°C under a nitrogen atmosphere 4h, after being precipitated by a poor solvent n-heptane, diol A was obtained;
[0037] 3) Put 100g of diol A, 52g of 2,5-furan dibasic acid, 0.1g of stannous octoate and 0.1g of heat stabilizer 1076 in a reaction kettle, and carry out esterification reaction at 200°C to prepare esterified product B ;
[0038] 4) Insulate the esterified product B at 235° C. and 200 Pa for 1 hour for precondensation reaction to prepare...
Embodiment 3
[0040] Embodiment 3: A kind of preparation method of heat-resistant bio-based block copolyester comprises the following preparation steps:
[0041] 1) Mix 100g of 2,5-furandicarboxylic acid, 64g of ethylene glycol, 0.1g of catalyst, and 0.1g of stabilizer, and carry out esterification reaction at 195°C to prepare esterified product A;
[0042] 2) Add 100g of 2-iodo-3-methoxybutane-1,4-diol, 148g of phenyl borate, 20mg of [1,1'-bis(diphenylphosphino)ferrocene]dichloro Palladium chloride, 10 g of 1 mol / L cesium carbonate solution, and 50 ml of acetonitrile were mixed, kept at 80 ° C and reacted for 3 hours under a nitrogen atmosphere, and diol A was obtained after ethanol precipitation in a poor solvent;
[0043] 2) Put 100g of dihydric alcohol A, 50g of 1,6-adipic acid, 0.1g of potassium acetate and 0.1g of heat stabilizer 425 in a reaction kettle, and carry out esterification reaction at 210°C to prepare esterified product B;
[0044] 3) Insulate the esterified product B at 2...
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