Purification process for hydrophilic organic solvent

Patent metadata

Field	Value
Publication number	US-11759774-B2
Application number	US-201616067031-A
Country	US
Kind code	B2
Filing date	Dec 16, 2016
Priority date	Dec 28, 2015
Publication date	Sep 19, 2023
Grant date	Sep 19, 2023

Abstract

Methods for the removal of ionic contaminants from a hydrophilic organic solvent by a mixed bed of ion exchange resins are described. A mixed bed of ion exchange resins with gel-type strong-acid cationic ion exchange resin with a specific moisture holding capacity and gel-type anionic ion exchange resin is used in some embodiments of such methods.

First claim

We claim:

1. A method for removing ionic contamination from a hydrophilic organic solvent, the method comprising:
contacting the hydrophilic organic solvent with a mixed bed of ion exchange resins comprising cationic ion exchange resins and anionic ion exchange resins, wherein:
(a) the cationic ion exchange resins are hydrogen (H) form strong-acid cationic ion exchange resins with a moisture holding capacity from 40 to 55 wt %, and
(b) both the cationic ion exchange resins and the anionic ion exchange resins have a porosity of 0.001 to 0.1 cm 3 /g, an average pore size of 0.001 to 1.7 nm, and a B.E.T. surface area of 0.001 to 10 m 2 /g,

wherein the hydrophilic organic solvent is a glycol ether or a mixture of glycol ethers and
wherein the concentration of Na, K, Ca, Al, Fe, Ni, Zn, Cu, Cr and Sn in the hydrophilic organic solvent after contacting with the mixed bed of ion exchange resins is each 0.1 ppb or less.

2. The method of claim 1 , wherein the mixed bed of ion exchange resins show 10 ppb or less of total organic carbon measured by the following method:
washing the mixed bed of ion exchange resins with 25 bed volumes (BV) of ultra pure water for 24 hours; and then analyzing total organic carbon of the ultra pure water.

3. The method of claim 1 , wherein the contents of Na, K, Ca, Al, Fe, Ni, Zn, Cu, Cr and Sn in the H form strong cationic ion exchange resins and the anionic ion exchange resins are each 10 mg/kg or less based on dry weight of the ion exchange resins.

4. A hydrophilic organic solvent obtained by the method of claim 1 , wherein the concentration of Na, K, Ca, Al, Fe, Ni, Zn, Cu, Cr and Sn in the hydrophilic organic solvent after contacting with the mixed bed of ion exchange resins is each 0.1 ppb or less.

5. The method of claim 1 , wherein the hydrophilic organic solvent comprises propylene glycol mono-methyl ether, dipropylene glycol mono-methy ether, diethylene glycol mono ethyl ether, diethylene glycol mono-butyl ether, or a mixture thereof.

6. A method for removing ionic contamination from a hydrophilic organic solvent, comprising the steps of
(i.) preparing a mixed bed ion of exchange resins comprising hydrogen (H) form strong cationic ion exchange resins and strong anionic ion exchange resins, wherein:
(a) the cationic ion exchange resins have a moisture holding capacity from 40 to 55 wt %, and
(b) both the cationic ion exchange resins and the anionic ion exchange resins have a porosity of 0.001 to 0.1 cm 3 /g, an average pore size of 0.001 to 1.7 nm, and a B.E.T. surface area of 0.001 to 10 m 2 /g; and

(ii.) contacting a hydrophilic organic solvent with the mixed bed of ion exchange resins, wherein the hydrophilic organic solvent is a glycol ether or a mixture of glycol ethers and wherein the concentration of Na, K, Ca, Al, Fe, Ni, Zn, Cu, Cr and Sn in the hydrophilic organic solvent after contacting with the mixed bed of ion exchange resins is each 0.1 ppb or less.

7. The method of claim 6 , wherein the method further comprises: (iii) rinsing the mixed bed of ion exchange resins by 30 to 50 bed volumes (BV) of the hydrophilic organic solvent under a flow rate of 1 to 50 BV/Hr, and step (iii) is conducted between steps (i) and (ii).

8. The method of claim 6 , wherein the hydrophilic organic solvent comprises propylene glycol mono-methyl ether, dipropylene glycol mono-methy ether, diethylene glycol mono ethyl ether, diethylene glycol mono-butyl ether, or a mixture thereof.

Assignees

• Dow Global Technologies Llc

Inventors

• Ohba Kaoru
• Takano Kenji
• Iida Masonori
• Abe Shinnosuke
• Masudo Takashi
• Kishizaki Osamu
• Ishibashi Ryo
• Yamashita Yusuke

Classifications

• B01J47/04 Primary

  Mixed-bed processes · CPC title

• B01J39/05

  in the strongly acidic form · CPC title

• B01J41/05

  in the strongly basic form · CPC title

• B01D15/362

  Cation-exchange · CPC title

• B01D15/363

  Anion-exchange · CPC title