Method for continuously preparing biodegradable aliphatic/aromatic polyester copolymer
Provided is a method of continuous preparation of a biodegradable aliphatic/aromatic polyester copolymer, the method including: performing a first esterification reaction of an aliphatic dihydroxy compound and an aliphatic dicarboxylic acid at a temperature of 185° C. or less; continuously performing a second esterification reaction of a reaction product obtained by the first esterification reaction; obtaining a pre-polymer by continuously performing a first polycondensation reaction of a reaction product obtained by the second esterification reaction; and continuously performing polycondensation reaction of the pre-polymer, wherein an aromatic carboxylic acid is added to a reactor in which the first esterification reaction or the second esterification reaction is performed, to prepare the biodegradable aliphatic/aromatic polyester copolymer. According to the method of continuous preparation of the biodegradable aliphatic/aromatic polyester copolymer as described above, the amount of the aliphatic dihydroxy compound used, which is a starting material, is reduced and accordingly, manufacturing costs are reduced.
1. A method of continuously preparing a biodegradable aliphatic/aromatic polyester copolymer, the method comprising:
performing a first esterification reaction of an aliphatic dihydroxy compound with an aliphatic dicarboxylic acid at a temperature of 185° C. or less;
continuously performing a second esterification reaction of a reaction product obtained from the first esterification reaction;
obtaining a prepolymer by continuously performing a first polycondensation reaction of a product obtained from the second esterification reaction; and
continuously performing polycondensation reaction of the prepolymer,
wherein an aromatic carboxylic acid is added to the step of performing the first esterification reaction or the step of continuously performing the second esterification reaction to prepare the biodegradable aliphatic/aromatic polyester copolymer.
2. The method of claim 1 , wherein the first esterification reaction is performed at a temperature in a range of about 160 to about 185° C.
3. The method of claim 1 , wherein the second esterification reaction is performed at a temperature in a range of about 220 to about 250° C.
4. The method of claim 1 , wherein an amount of the aliphatic dihydroxy compound is in a range of about 1.1 to about 1.5 moles based on 1 mole of a total sum of the aliphatic dicarboxylic acid and the aromatic dicarboxylic acid.
5. The method of claim 1 , wherein the step of continuously performing the polycondensation of the prepolymer comprises:
continuously performing a second polycondensation reaction of the prepolymer; and
continuously performing a third polycondensation reaction of a reaction product obtained from the second polycondensation reaction.
6. The method of claim 5 , wherein the second polycondensation reaction is performed under conditions of a temperature in a range of 220 to about 250° C., a degree of vacuum in a range of 2 to about 7 torr, and a residence time of a reaction mixture in a range of 1 to 4 hours.
7. The method of claim 5 , wherein the third polycondensation reaction is performed under conditions of a temperature in a range of 220 to about 250° C., a degree of vacuum in a range of 0.5 to about 2 torr, and a residence time of a reaction mixture in a range of 1 to 3 hours.
8. The method of claim 1 , wherein the first polycondensation reaction is performed under the conditions of a temperature in a range of 220 to about 250° C., a degree of vacuum in a range of 10 to about 30 torr, and a residence time of a reaction mixture in a range of 1 to 4 hours.
9. The method of claim 1 , wherein the first esterification reaction is performed in a batch reactor or continuously performed in an esterification reactor.
10. The method of claim 1 , wherein at least one selected from a catalyst, a heat stabilizer, a branching agent, a color stabilizing agent, and a color control agent is further added to a reactor in which the first esterification reaction of the aliphatic dihydroxy compound and the aliphatic dicarboxylic acid is performed.
11. The method of claim 1 , wherein a catalyst is further added to a reactor in which the first polycondensation reaction is performed.
12. The method of claim 1 , wherein the aliphatic dihydroxy compound comprises at least one selected from a group consisting of ethanediol, 1,2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, 2,4-dimethyl-2-ethyl-1,3-hexanediol, 2,2-dimethyl-1,3-propanediol, 2-ethyl-2-butyl-1,3-propanediol, 2-ethyl-2-isobutyl-1,3-propanediol, 2,2,4-trimethyl-1,6-hexanediol, and a mixture thereof;
the aliphatic dicarboxylic acid comprises at least one selected from a group consisting of malonic acid, succinic acid, glutaric acid, 2-methylglutaric acid, 3-methylglutaric acid, adipic acid, pimellic acid, suberic acid, azelaic acid, sebacic acid, undecanedioic, dodecanedioic acid, brassylic acid, tetradecanedioic acid, fumaric acid, 2,2-dimethylglutaric acid, maleic acid, itaconic acid, 2,5-norbornene dicarboxylic acid, and a mixture thereof; and
the aromatic dicarboxylic acid comprises at least one selected from a group consisting of terephthalic acid, isophthalic acid, 2,6-naphthoic acid, 1,5-naphthoic acid, and a mixture thereof.