Process for making high purity salts

Patent metadata

Field	Value
Publication number	US-10865177-B2
Application number	US-201916437698-A
Country	US
Kind code	B2
Filing date	Jun 11, 2019
Priority date	Jul 2, 2018
Publication date	Dec 15, 2020
Grant date	Dec 15, 2020

Abstract

A process for making a high purity salt comprises the steps of providing an organic compound, providing a metal salt, adding the metal salt and organic compound to an aqueous medium, heating the reaction mixture to react the organic compound and the metal salt to form an organic salt, collecting the organic salt, exposing the collected organic salt to microwave radiation, and exposing the collected organic salt to infrared radiation.

First claim

What is claimed is:

1. A process for making a high purity salt, the process comprising the steps of:
(a) providing an organic compound selected from the group consisting of cis-cyclohexane-1,2-dicarboxylic acid anhydride, cis-cyclohexane-1,2-dicarboxylic acid, and mixtures thereof;
(b) providing a metal salt selected from the group consisting of metal hydroxides and metal carbonates, the metal salt comprising a metal selected from the group consisting of alkali metals and alkaline earth metals;
(c) adding the metal salt and the organic compound to an aqueous medium to produce a reaction mixture;
(d) heating the reaction mixture to a temperature of about 65° C. to about 80° C. to react the organic compound and the metal salt and form an organic salt;
(e) collecting the organic salt from the aqueous medium;
(f) exposing the collected organic salt to microwave radiation having a frequency of about 900 MHz to about 2,500 MHz to reduce the moisture content of the organic salt to about 20% or less; and
(g) exposing the organic salt from step (f) to infrared radiation having a frequency of about 9.9×10 4 GHz to about 3×10 5 GHz to reduce the moisture content of the organic salt to about 7% or less.

2. The process of claim 1 , wherein the organic compound is cis-cyclohexane-1,2-dicarboxylic acid anhydride.

3. The process of claim 1 , wherein the organic compound contains about 1.5 mol. % or less trans-cyclohexane-1,2-dicarboxylic acid anhydride or trans-cyclohexane-1,2-dicarboxylic acid.

4. The process of claim 1 , wherein the metal salt is calcium hydroxide.

5. The process of claim 1 , wherein the organic salt is calcium cis-cyclohexane-1,2-dicarboxylate.

6. The process of claim 5 , wherein the organic salt contains about 2.5 mol. % or less of trans-cyclohexane-1,2-dicarboxylate salts.

7. The process of claim 6 , wherein the organic salt contains about 1 mol. % or less of trans-cyclohexane-1,2-dicarboxylate salts.

8. The process of claim 1 , wherein the collected organic salt is granulated prior to exposure to the microwave radiation.

9. The process of claim 1 , wherein the energy flux of the microwave radiation is about 2×10 7 J·m −2 ·s −1 to about 4.5×10 7 J·m −2 ·s −1 .

10. The process of claim 1 , wherein the energy flux of the infrared radiation is about 1,900 J·m −2 ·s −1 to about 2,500 J·m −2 ·s −1 .

Assignees

• Milliken & Co

Inventors

• Dotson Darin L
• Wang Xiaoying
• Liu Rui

Classifications

• C07C2601/14

  The ring being saturated · CPC title

• C07C61/09

  Completely hydrogenated benzenedicarboxylic acids · CPC title

• C07C51/412 Primary

  by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part · CPC title

• C07C51/42

  Separation; Purification; Stabilisation; Use of additives · CPC title