Method for preparing biodegradable polyester resin
A method of preparing a biodegradable polyester resin is provided. The method of preparing a biodegradable polyester resin includes: (a) synthesizing the biodegradable polyester resin having a reheating crystallization initiation temperature (T ch1 ), a reheating crystallization peak temperature (T ch ), and a reheating crystallization end temperature (T ch2 ); and (b) crystallizing the biodegradable polyester resin synthesized in step (a) by cooling the resin from a temperature of T 1 to a temperature of T 2 and then maintaining the resin at a temperature of T 2 for a time of t c . Thus, the biodegradable polyester resin with improved solidification rate may be obtained.
1. A method of preparing a biodegradable polyester resin, the method comprising:
(a) synthesizing the biodegradable polyester resin having a reheating crystallization initiation temperature (T ch1 ), a reheating crystallization peak temperature (T ch ), and a reheating crystallization end temperature (T ch2 ); and
(b) crystallizing the biodegradable polyester resin synthesized in step (a) by cooling the biodegradable polyester resin from a temperature of T 1 to a temperature of T 2 and then maintaining the biodegradable polyester resin at a temperature of T 2 for a time of t c ,
wherein T ch1 , T ch , and T ch2 respectively denote an initial temperature, a peak temperature, and a final temperature of the crystallization peak that appears in a second step after a first step, wherein, in the first step, the molten biodegradable polyester resin synthesized in step (a) is cooled at a cooling rate of about 10° C./min from about 200° C. to about −50° C., and in the second step, the cooled biodegradable polyester resin is heated at a heating rate of about 10° C./min from about −50° C. to about 200° C., in a differential scanning calorimeter (DSC),
T 1 is a temperature between about 220° C. and about 280° C., and
T 2 satisfies the condition of T ch1 ≦T 2 ≦T ch2 .
2. The method of claim 1 , wherein T 2 is a temperature between about 15° C. and about 80° C.
3. The method of claim 1 , wherein t c is 5 minutes or less.
4. The method of claim 1 , wherein the biodegradable polyester resin is poly(ethylene succinate) (PES) or poly(ethylene succinate-co-adipate) (PESA).
5. The method of claim 4 , wherein the biodegradable polyester resin is synthesized by using ethylene glycol in an amount of from about 1 part by mole to about 2 parts by mole based on 1 part by mole of the total amount of succinic acid and adipic acid.
6. The method of claim 4 , wherein when the biodegradable polyester resin is PESA, the amount of the succinic acid used and the amount of the adipic acid used are from about 80 parts by mole to about 99.9 parts by mole and from about 0.1 part by mole to about 20 parts by mole, respectively, based on 100 parts by mole of the total amount of the succinic acid and the adipic acid used.
7. The method of claim 1 , wherein at least one nucleating agent selected from a polymer nucleating agent including polyethylene (PE), polypropylene (PP), polyethylene terephthalate (PET), or a combination thereof; an organic nucleating agent including sodium stearate, ethylene bis-stearamide (EBS), or a combination thereof; and an inorganic nucleating agent including TiO 2 , carbon black, clay, talc, mica, or a combination thereof is added in step (a).
8. The method of claim 7 , wherein the nucleating agent is added in an amount of about 0.1 wt % to about 5 wt % based on the total weight of the biodegradable polyester resin.