Distillation method

Patent metadata

Field	Value
Publication number	US-10556191-B2
Application number	US-201615563772-A
Country	US
Kind code	B2
Filing date	Apr 1, 2016
Priority date	Apr 3, 2015
Publication date	Feb 11, 2020
Grant date	Feb 11, 2020

Abstract

By using the distillation device of the present application, energy loss occurring in a purification process of a solution including a waste stripper and a stripped photoresist resin used in a stripping process of a photoresist can be minimized and the installation cost of the distillation device can be reduced compared to the case in which dual distillation columns are used, thereby increasing the economic feasibility of a process.

First claim

The invention claimed is:

1. A distillation method, comprising a distillation device, comprising a reboiler, and a distillation column, a dividing wall being provided in an interior of the distillation column:
wherein an interior of the distillation column is divided into a column top zone; a column bottom zone; and a dividing wall zone that is present between the column top zone and the column bottom zone and contacts the column top zone and the column bottom zone, the dividing wall is located in the dividing wall zone, and the dividing wall zone is divided into a feed supply zone and a product discharge zone divided by the dividing wall,
a raw material of a waste stripper solution comprising a stripper and a stripped photoresist resin is introduced into a feed supply zone and the introduced raw material is respectively separated into and discharged as a product stream, a column bottom stream, and a column top stream,
the column bottom stream is discharged from the column bottom zone and a portion of the column bottom stream is refluxed into the column bottom zone via the reboiler,
the column top stream is discharged from the column top zone and a portion of the column top stream is refluxed into the column top zone via the condenser, and
the product stream is discharged from the product discharge zone,
wherein the stripper is a non-aqueous stripper and the temperature of the column top zone is adjusted to within a range of lower and upper temperatures respectively calculated according to Equations 1 and 2 below:
P= 0.00126× T top,lower 3 −0.07051× T top,lower 2 +3.17767× T top,lower −15.01040  [Equation 1]

P= 0.00150× T top,upper 3 −0.18493× T top,upper 2 +9.56742× T top,lower −176.07273  [Equation 2]

wherein T top,lower represents a lower temperature of the column top zone,
T top,upper represent an upper temperature of the column top zone, and
P represents the pressure of the column top zone.

2. The distillation device method according to claim 1 , wherein the column bottom stream comprises a stripped photoresist resin.

3. The distillation method according to claim 1 , wherein the column top stream comprises one or more selected from the group consisting of water and materials having a boiling point of less than 100° C. at atmospheric pressure.

4. The distillation method according to claim 1 , wherein the product stream comprises a prone organic solvent, an aprotic polar solvent, and an organic amine compound.

5. The distillation method according to claim 1 , wherein a temperature of the column bottom zone is 100° C. to 250° C.

6. The distillation method according to claim 1 , wherein a temperature of the column top zone is 14° C. to 92° C.

7. The distillation method according to claim 1 , wherein a pressure of the column bottom zone is 50 to 400 mmHg.

8. The distillation method according to claim 1 , wherein a pressure of the column top zone is 20 to 300 mmHg.

9. A distillation method using a distillation device, comprising a condenser, a reboiler, and a distillation column, a dividing wall being provided in an interior of the distillation column,
wherein an interior of the distillation column is divided into a column top zone; a column bottom zone; and a dividing wall zone that is present between the column top zone and the column bottom zone and contacts the column top zone and the column bottom zone, the dividing wall is located in the dividing wall zone, and the dividing wall zone is divided into a feed supply zone and a product discharge zone divided by the dividing wall,
a raw material of a waste stripper solution comprising a stripper and a stripped photoresist resin is introduced into the feed supply zone and the introduced raw material is respectively separated into and discharged as a product stream, a column bottom stream, and a column top stream,
the column bottom stream is discharged from the column bottom zone and a portion of the column bottom stream is refluxed into the column bottom zone via the reboiler,
the column top stream is discharged from the column top zone and a portion of the column top stream is refluxed into the column top zone via the condenser, and
the product stream is discharged from the product discharge zone,
wherein the stripper is an aqueous stripper and a temperature of the column top zone is adjusted to within a range of lower and upper temperatures respectively calculated according to Equations 3 and 4 below:
P= 0.00177× T top,lower 3 −0.01645× T top,lower 2 +2.13532× T top,lower −12.36272  [Equation 3]

P= 0.00144× T top,lower 3 −0.10028× T top,lower 2 +4.27752× T top,lower −44.49051  [Equation 4]

wherein T top,lower represents a lower temperature of the column top zone,
T top,lower represent an upper temperature of the column top zone, and
P represents the pressure of the column top zone.

10. The distillation method according, to claim 9 , wherein the column bottom stream comprises a stripped photoresist resin.

11. The distillation method according to claim 9 , wherein the column top stream comprises a material having a boiling point of less than 100° C. at atmospheric pressure.

12. The distillation method according to claim 9 , wherein the product stream comprises water, a protic organic solvent, an aprotic polar solvent, and an organic amine compound.

13. The distillation method according to claim 9 , wherein a temperature of the column bottom zone is 150° C. to 300° C.

14. The distillation method according to claim 9 , Wherein a temperature of the column top zone is 4° C. to 74° C.

15. The distillation method according to claim 9 , wherein a pressure of the column bottom zone is 50 to 400 mmHg.

Assignees

• Lg Chemical Ltd

Inventors

• Lee Si Nae
• Lee Sung Kyu
• Lee Sang Beom
• Lee Sung Ho
• Kim Jeong Seok
• Shin Joon Ho
• Jung Dae Chul
• Jang Yong Hee
• Park Tae Moon
• Yi Hyun Jik

Classifications

• B01D3/141 Primary

  where at least one distillation column contains at least one dividing wall · CPC title

• G03F7/425

  containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen · CPC title

• B01D3/32

  Other features of fractionating columns {; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30} · CPC title

• B01D3/02 Primary

  in boilers or stills · CPC title

• B01D5/0063

  Reflux condensation · CPC title