Production method of aliphatic polyester
View Patent ↗An object of the present invention is to provide a method for efficient continuous production of aliphatic polyester having good quality. The invention relates to a continuous production method of aliphatic polyester, wherein the polyester is obtained through a preparation step of slurry containing aliphatic dicarboxylic acid and aliphatic diol, an esterification reaction step and a polycondensation reaction step, wherein temperature range of the slurry during the preparation step thereof is from the coagulation point of the aliphatic diol to 80° C., and moisture content in the slurry is from 0.01 to 10% by weight.
1. A continuous method of producing an aliphatic polyester, comprising, in the following order:
(I) mixing an aliphatic dicarboxylic acid and an aliphatic diol, to obtain a slurry;
(II) esterifying the dicarboxylic acid and aliphatic diol, to produce an esterification reaction product; and
(III) polycondensing the esterification reaction product, thereby obtaining the aliphatic polyester,
wherein, during (I), a temperature range of the slurry is from the coagulation point of the aliphatic diol to 80° C., and a moisture content in the slurry is from 0.01 to 10% by weight, based on a total weight of the slurry,
wherein the aliphatic diol comprises 70 mol % or more of 1,4-butanediol, and the aliphatic dicarboxylic acid comprises 70 mol % or more of succinic acid, and
wherein the aliphatic dicarboxylic acid in the slurry is in the form of particles having an average particle diameter D(50) and particle diameter D(90) in 90% of an accumulated volume percentage curve of particle diameter that satisfy formulae (1) and (2):
1 μm≦ D (50)≦500 μm (1)
D (90)/ D (50)≦2.5 (2).
2. The method of claim 1 , wherein a molar ratio of the aliphatic diol to the aliphatic dicarboxylic acid in the slurry is from 0.8 to 2.0.
3. The method of claim 1 , wherein the aliphatic diol comprises 90 mol % or more of 1,4-butanediol, and the aliphatic dicarboxylic acid comprises 90 mol % or more of succinic acid.
4. The method of claim 2 , wherein the aliphatic diol comprises 90 mol % or more of 1,4-butanediol, and the aliphatic dicarboxylic acid comprises 90 mol % or more of succinic acid.
5. The method of claim 1 , wherein the moisture content in the slurry is from 0.01 to 5% by weight, based on a total weight of the slurry.
6. The method of claim 1 , wherein the moisture content in the slurry is from 0.05 to 5% by weight, based on a total weight of the slurry.
7. The method of claim 1 , wherein the moisture content in the slurry is from 0.05 to 2% by weight, based on a total weight of the slurry.
8. The method of claim 1 , wherein the moisture content in the slurry is from 0.1 to 1.5% by weight, based on a total weight of the slurry.
9. The method of claim 1 , wherein the moisture content in the slurry is from 0.1 to 1% by weight, based on a total weight of the slurry.
10. The method of claim 1 , wherein the temperature range of the slurry is from the coagulation point of the aliphatic diol to 70° C.
11. The method of claim 1 , wherein the temperature range of the slurry is from the coagulation point of the aliphatic diol to 60° C.
12. The method of claim 1 , wherein the temperature range of the slurry is from the coagulation point of the aliphatic diol to 50° C.
13. The method of claim 8 , wherein the temperature range of the slurry is from the coagulation point of the aliphatic diol to 60° C.
14. The method of claim 8 , wherein the temperature range of the slurry is from the coagulation point of the aliphatic diol to 50° C.
15. The method of claim 13 , wherein the aliphatic diol comprises 90 mol % or more of 1,4-butanediol, and the aliphatic dicarboxylic acid comprises 90 mol % or more of succinic acid.
16. The method of claim 13 , wherein the aliphatic dicarboxylic acid particles have an average particle diameter D(50) and particle diameter D(90) in 90% of an accumulated volume percentage curve of particle diameter that satisfy formulae (1) and (2):
10 μm≦ D (50)≦400 μm (1)
1.2 ≦D (90)/ D (50)≦2.3 (2).
17. The method of claim 13 , wherein the aliphatic dicarboxylic acid particles have an average particle diameter D(50) and particle diameter D(90) in 90% of an accumulated volume percentage curve of particle diameter that satisfy formulae (1) and (2):
30 μm≦ D (50)≦200 μm (1)
1.2 ≦D (90)/ D (50)≦2.0 (2).
18. The method of claim 13 , wherein the aliphatic dicarboxylic acid particles have an average particle diameter D(50) and particle diameter D(90) in 90% of an accumulated volume percentage curve of particle diameter that satisfy formulae (1) and (2):
30 μm≦ D (50)≦100 μm (1)
1.2 ≦D (90)/ D (50)≦1.8 (2).
19. The method of claim 15 , wherein the aliphatic dicarboxylic acid particles have an average particle diameter D(50) and particle diameter D(90) in 90% of an accumulated volume percentage curve of particle diameter that satisfy formulae (1) and (2):
10 μm≦ D (50)≦400 (1)
1.2 ≦D (90)/ D (50)≦2.3 (2).