System and method for manufacturing diester-based composition

Patent metadata

Field	Value
Publication number	US-12186729-B2
Application number	US-202017600889-A
Country	US
Kind code	B2
Filing date	Jul 2, 2020
Priority date	Jul 4, 2019
Publication date	Jan 7, 2025
Grant date	Jan 7, 2025

Abstract

The present disclosure relates to a preparation system and a preparation method of a diester-based composition. A first alcohol which is a reaction raw material is added to waste water as an extracting agent, and layer separation is performed to separate a second alcohol which is another reaction raw material in the waste water. Accordingly, the amount of alcohol discharged as waste water can be reduced, and an eco-friendly process operation is possible. In addition, it is economical and efficiency to use the alcohol separated again as a reaction raw material.

First claim

The invention claimed is:

1. A preparation system of a diester-based composition, the system comprising:
a first purification part comprising a purification space for separating a reaction product of esterification reaction of a dicarboxylic acid and a first alcohol into a purified product and the first alcohol which is an unreacted reactant, and a purified product line and an unreacted reactant recovering line for discharging the purified product and the unreacted reactant;
a trans reaction unit comprising an interior space for performing trans esterification reaction of the purified product injected from the purified product line of the first purification part and a second alcohol injected from a separate alcohol injection part, and a trans reaction product line discharging a produced trans reaction product;
a neutralized water separating apparatus comprising a partition wall separating an interior part into a neutralization space and a water separation space and forming a passage capable of moving a fluid, and an organic layer line and a waste water line for separately discharging an ester-rich organic layer and a water-rich waste water layer from the water separation space, the trans reaction product line being connected with the neutralization space;
a second purification part comprising an unreacted reactant recovering line, a second waste water line and a product line for separately discharging the ester-rich organic layer injected from the organic layer line of the neutralized water separating apparatus into three streams of a mixed alcohol of the unreacted first alcohol and the second alcohol, a mixed waste water comprising water, the first alcohol and the second alcohol, and a diester-based composition; and
a waste water treating unit comprising a waste water injecting line which is connected with the waste water line of the neutralized water separating apparatus and the second waste water line of the second purification part, an extracting agent injecting line injecting the first alcohol which is an extracting agent, a layer separating space for layer separating a mixed waste liquid of water, the first alcohol and the second alcohol into a mixed alcohol layer and a waste water layer, and a mixed alcohol recovering line and a final waste water line, separately discharging the mixed alcohol layer and the waste water layer.

2. The preparation system of a diester-based composition according to claim 1 , wherein the unreacted reactant recovering line of the second purification part and the mixed alcohol recovering line of the waste water treating unit further comprise a mixed alcohol tank connected with an interior mixed alcohol storing space.

3. The preparation system of a diester-based composition according to claim 2 , wherein the preparation system further comprises an ester reaction unit performing esterification reaction of the dicarboxylic acid and the first alcohol, and
wherein the unreacted reactant recovering line of the first purification part is connected with one or more of the ester reaction unit and the mixed alcohol tank.

4. The preparation system of a diester-based composition according to claim 2 , wherein the mixed alcohol tank comprises a mixed alcohol discharging line discharging the mixed alcohol stored, and
wherein the preparation system further comprises an alcohol recovering part comprising a mixed alcohol injecting line connected with the mixed alcohol discharging line, a purification space separating the mixed alcohol into the first alcohol and the second alcohol, and a first alcohol recovering line and a second alcohol recovering line respectively discharging the first alcohol and the second alcohol separated.

5. The preparation system of a diester-based composition according to claim 1 , wherein the waste water treating unit further comprises a temperature controlling part controlling a temperature of the layer separating space.

6. The preparation system of a diester-based composition according to claim 1 , wherein the waste water treating unit further comprises a flowing amount controlling part controlling a flowing amount of the first alcohol injected as the extracting agent.

7. The preparation system of a diester-based composition according to claim 1 , wherein a stream in the waste water line of the neutralized water separating apparatus comprises water and the second alcohol, and a concentration of the second alcohol in the stream is 0.01 to 10 wt %.

8. The preparation system of a diester-based composition according to claim 1 , wherein a stream in the second waste water line of the second purification part comprises water, the first alcohol and the second alcohol, and a concentration of the second alcohol in the stream is 0.01 to 10 wt %.

9. The preparation system of a diester-based composition according to claim 1 , wherein the preparation system is operated by a continuous type.

10. A preparation method of a diester-based composition, the method comprising:
a step of removing an unreacted first alcohol from a reaction product produced by esterification reaction of a dicarboxylic acid and a first alcohol to obtain a purified product (S 1 );
a step of performing trans esterification reaction of the purified product and a second alcohol to obtain a trans reaction product (S 2 );
a step of separating a water-rich waste water layer and an ester-rich organic layer by neutralizing the trans reaction product and separating water, and transporting the waste water layer to a waste water treating unit (S 3 );
a step of separating the ester-rich organic layer into three streams of a diester-based composition, a mixed alcohol of an unreacted first alcohol and the second alcohol, and a second waste water comprising water, the first alcohol and the second alcohol, and transporting the second waste water to the waste water treating unit (S 4 ); and
a step of injecting an extracting agent to the waste water treating unit for layer separating the mixed waste water into a final waste water layer and a mixed alcohol layer (S 5 ),
wherein the extracting agent comprises the first alcohol.

11. The preparation method of a diester-based composition according to claim 10 , wherein the mixed alcohol stream separated in step S 4 and the mixed alcohol layer separated in step S 5 are transported to a mixed alcohol tank, and
wherein the method further comprises a step of separating the mixed alcohol in the mixed alcohol tank into the first alcohol and the second alcohol (S 6 ).

12. The preparation method of a diester-based composition according to claim 11 , wherein the first alcohol separated in step S 6 is used for the esterification reaction in step S 1 , and the separated second alcohol is used for the trans esterification reaction in step S 2 .

13. The preparation method of a diester-based composition according to claim 10 , wherein a temperature of the waste water treating unit in step S 5 is 50 to 100° C.

14. The preparation method of a diester-based composition according to claim 10 , wherein an injection ratio of the first alcohol injected into the waste water treating unit as the extracting agent in step S 5 is 5 to 60%.

15. The preparation method of a diester-based composition according to claim 10 , wherein the dicarboxylic acid is selected from the group consisting of phthalic acid, terephthalic acid, isophthalic acid and cyclohexane dicarboxylic acid.

16. The preparation method of a diester-based composition according to claim 10 , wherein the first alcohol is an alcohol having a carbon number of 7 to 12, and the second alcohol is an alcohol having a carbon number

Assignees

• Lg Chemical Ltd

Inventors

• Choo Yeon Uk
• Lee Sung Kyu
• Shin Joon Ho
• Jun Hyoung
• Jin Chan Hyu

Classifications

• B01J2219/00164

  controlling the flow · CPC title

• B01J2219/00051

  Controlling the temperature · CPC title

• C02F1/26

  by extraction · CPC title

• B01D17/12

  Auxiliary equipment particularly adapted for use with liquid-separating apparatus, e.g. control circuits · CPC title

• B01J19/0046

  Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays (synthesis methods per se C40B50/00) · CPC title