Method of preparing diester-based material

Patent metadata

Field	Value
Publication number	US-12275698-B2
Application number	US-202117635925-A
Country	US
Kind code	B2
Filing date	Aug 20, 2021
Priority date	Nov 17, 2020
Publication date	Apr 15, 2025
Grant date	Apr 15, 2025

Abstract

A diester-based material can be prepared continuously including a reaction part in which a total of n reaction units from a first reaction unit to an nth reaction unit are connected in series, the reaction unit including a reactor which esterifies dicarboxylic acid and alcohol, includes: esterifying dicarboxylic acid and alcohol in a reactor of the first reaction unit to produce a reaction product, and supplying a lower discharge stream including the reaction product to a reaction unit at a rear end, wherein an operating pressure of the reactor of the first reaction unit is 0.4 kg/cm2G to 5.5 kg/cm2G, an operating pressure is reduced from a reactor of any one reaction unit of reaction units from a second reaction unit to the nth reaction unit, and an operating temperature is increased from the reactor of the first reaction unit to the reactor of the nth reaction unit.

First claim

The invention claimed is:

1. A method of preparing a diester-based material, which is carried out by a continuous preparation process of a diester-based material including a reaction part in which a total of n reaction units from a first reaction unit to an nth reaction unit are connected in series, the reaction unit including a reactor which esterifies dicarboxylic acid and alcohol in the presence of a catalyst, the method comprising:
esterifying dicarboxylic acid and alcohol in a reactor of the first reaction unit to produce a reaction product, and supplying a discharge stream from a lower portion of the reactor including the reaction product to a reaction unit at a rear end,
wherein an operating pressure of the reactor of the first reaction unit is 0.4 kg/cm 2 G to 5.5 kg/cm 2 G,
an operating pressure is reduced from a reactor of any one reaction unit of reaction units from a second reaction unit to the nth reaction unit to a reactor of the nth reaction unit,
an operating temperature is increased from the reactor of the first reaction unit to the reactor of the nth reaction unit, and
wherein the dicarboxylic acid includes terephthalic acid and the alcohol includes 2-ethylhexyl alcohol and the catalyst includes organic titanium compound.

2. The method of preparing a diester-based material of claim 1 , wherein an operating pressure of the reactor of the nth reaction unit is equal to or lower than an operating pressure of a reactor of an n−1th reaction unit.

3. The method of preparing a diester-based material of claim 2 , wherein the operating pressure of the reactor of the nth reaction unit is decreased by 0% to 90% as compared with the operating pressure of the reactor of the n−1th reaction unit.

4. The method of preparing a diester-based material of claim 1 , wherein the operating pressure of the reactor of the first reaction unit is 0.4 kg/cm 2 G to 4 kg/cm 2 G.

5. The method of preparing a diester-based material of claim 1 , wherein the operating temperature of the reactor of the first reaction unit is 160° C. to 210° C.

6. The method of preparing a diester-based material of claim 1 , wherein the operating temperature of the reactor of the nth reaction unit is increased by 0% to 20% as compared with the operating temperature of the reactor of the n−1th reaction unit.

7. The method of preparing a diester-based material of claim 1 , wherein the operating pressure of the reactor of the nth reaction unit is −1 kg/cm 2 G to 1 kg/cm 2 G, and the operating temperature thereof is 200° C. to 250° C.

8. The method of preparing a diester-based material of claim 1 , wherein a water content in the reactor of the nth reaction unit is decreased by 20% to 95% as compared with a water content in the reactor of the n−1th reaction unit.

9. The method of preparing a diester-based material of claim 1 , wherein n is 2 to 8.

10. The method of preparing a diester-based material of claim 1 , wherein a mole ratio between an amount of the dicarboxylic acid introduced and a total amount of alcohol introduced to the reactor of the first reaction unit is 1:2 to 1:5.

11. The method of preparing a diester-based material of claim 1 , wherein the reaction unit further includes:
a column which is supplied with an upper discharge stream from the reactor including alcohol and water vaporized during esterification from the reactor to perform gas-liquid separation, passes a gas phase through a condenser as the upper discharge stream to be supplied to a layer separator, and supplies a liquid phase to the reactor as a lower discharge stream; and
a separator which performs a separation into a water layer and an alcohol layer and refluxes only alcohol to the column while removing water.

Assignees

• Lg Chemical Ltd

Inventors

• Jeong Jae Hun
• Lee Sung Kyu
• Choo Yeon Uk
• Lee Song Hoon
• Jun Hyoung
• Heo Yun Gon

Classifications

• C07C69/82

  Terephthalic acid esters · CPC title

• C07C67/58

  by liquid-liquid treatment · CPC title

• C07C67/08 Primary

  by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds · CPC title