# US 10,865,177 B2 · Process for making high purity salts

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- Number: US 10,865,177 B2
- Document ID: US10865177B2
- Status: Granted
- Kind: B2
- Application number: 16/437,698
- Filed: 2019-06-11
- Published: 2020-10-01
- Granted: 2020-12-15
- Earliest claimed: 2018-07-02
- Assignees: Milliken & Company
- Applicants: Milliken & Company
- Inventors: Darin L. Dotson; Xiaoying Wang; Rui Liu
- Web page: https://patentgrep.com/patent/US10865177B2

## CPC

- C07C 51/412: {by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part}
- C07C 51/42: Separation; Purification; Stabilisation; Use of additives
- C07C 2601/14: The ring being saturated
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## 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.

## Claims

### Claim 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 9.9×104 GHz to about 3×105 GHz to reduce the moisture content of the organic salt to about 7% or less.

### Claim 2 (depends on 1)

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

### Claim 3 (depends on 1)

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.

### Claim 4 (depends on 1)

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

### Claim 5 (depends on 1)

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

### Claim 6 (depends on 5)

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

### Claim 7 (depends on 6)

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

### Claim 8 (depends on 1)

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

### Claim 9 (depends on 1)

The process of claim 1, wherein the energy flux of the microwave radiation is about 2×107 J·m−2·s−1 to about 4.5×107 J·m−2·s−1.

### Claim 10 (depends on 1)

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.