# US 4,395,548 A · Process for production of an alkali metal dichloroisocyanurate and trichloroisocyanuric acid

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- Number: US 4,395,548 A
- Document ID: US4395548A
- Status: Granted
- Kind: A
- Application number: 06/365,060
- Filed: 1982-04-02
- Granted: 1983-07-26
- Earliest claimed: 1982-04-02
- Assignees: FMC Corporation
- Inventors: John F. Start
- Web page: https://patentgrep.com/patent/US4395548A

## CPC

- C07D 251/36: having halogen atoms directly attached to ring nitrogen atoms
- C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08)

## Abstract

A process to manufacture trichloroisocyanuric acid of commercially acceptable size and quality from a mother liquor used to produce an alkali metal salt of dichloroisocyanurate by monitoring and, if necessary, adjusting the mol ratio of available alkalinity to chlorine required to convert all of the triazine compounds in the mother liquor to trichloroisocyanuric acid to be between 1.0 and 1.3 with an alkali metal salt of carbonic acid.

## Claims

### Claim 1

A process for producing both an alkali metal dichloroisocyanurate and trichloroisocyanuric acid by a two-stage chlorination comprising:
(a) chlorinating an aqueous solution of a trialkali metal salt of cyanuric acid maintained at a temperature between 10.degree. C. and 30.degree. C. and at a pH between 5 and 9 thereby forming a slurry of alkali metal dichloroisocyanurate,
(b) separating the undissolved alkali metal dichloroisocyanurate from the aqueous medium constituting the mother liquor,
(c) whenever the mol ratio in the mother liquor of available alkalinity to chlorine required to convert any triazine compounds which are present to trichloroisocyanuric acid falls outside the range of 1.0 to 1.3, adding sufficient alkali metal salt of carbonic acid to the mother liquor to bring the mol ratio within the said range,
(d) chlorinating the mother liquor from step (c) while maintaining the temperature between 10.degree. C. and 30.degree. C. and the pH between 2.5 and 3.5, and
(e) recovering the resulting trichloroisocyanuric acid so produced.

### Claim 2 (depends on 1)

The process of claim 1 wherein the alkali metal dichloroisocyanurate is sodium dichloroisocyanurate.

### Claim 3 (depends on 1)

The process of claim 1 wherein the first chlorinator pH is maintained at 6.5 to 7.5.

### Claim 4 (depends on 1)

The process of claim 1 wherein the mol ratio of the mother liquor in step (c) is adjusted to be within the range of 1.0 to 1.15.

### Claim 5 (depends on 1)

The process of claim 1 wherein the temperature of the second chlorinator is maintained between 10.degree. C. to 20.degree. C.

### Claim 6 (depends on 1)

The process of claim 1 wherein the pH of the second chlorinator is maintained between 3.3 and 3.0.

### Claim 7 (depends on 1, 2, 3, 4, 5)

The process of claim 1, 2, 3, 4, 5, or 6 wherein the mol ratio of the mother liquor is adjusted to be within the range of 1.0 to 1.15.

### Claim 8 (depends on 7)

The process of claim 7 wherein the temperature of the second chlorinator is maintained between 10.degree. C. and 20.degree. C.

### Claim 9 (depends on 8)

The process of claim 8 wherein the pH of the second chlorinator is maintained between 3.3 and 3.0.

### Claim 10 (depends on 7)

The process of claim 7 wherein the alkali metal salt of carbonic acid comprises sodium bicarbonate.

### Claim 11 (depends on 7)

The process of claim 7 wherein the alkali metal salt carbonic acid comprises sodium carbonate.

### Claim 12 (depends on 7)

The process of claim 7 wherein the alkali metal salt of carbonic acid comprises sodium carbonate sesquicarbonate.

### Claim 13 (depends on 7)

The process of claim 7 wherein the alkali metal salt comprises potassium bicarbonate.

### Claim 14 (depends on 7)

The process of claim 7 wherein the alkali metal salt of carbonic acid comprises potassium carbonate.

### Claim 15

An improved two-stage chlorination process for making trichloroisocyanuric acid by chlorinating an aqueous slurry of a trialkali metal cyanurate in a first chlorinator maintained at a pH between 6.5 and 8.5, withdrawing an effluent from the first chlorinator and feeding it to a second chlorinator maintained at a pH between 2.5 to 3.5 and withdrawing an effluent from the second chlorinator and recovering trichloroisocyanuric acid from the effluent of the second chlorinator wherein the improvement comprises:
(a) monitoring the mol ratio of available alkalinity to chlorine required to convert any triazine compounds which are present to trichloroisocyanuric acid in the effluent from the first chlorinator,
(b) whenever the mol ratio of the effluent from the first chlorinator falls outside the range of 1.0 to 1.3, adjusting said mol ratio of the effluent of the first chlorinator to be within 1.0 to 1.3 by adding an alkali metal salt of carbonic acid,
(c) continuously adding the monitored and adjusted effluent to the second chlorinator.