Process for producing a percarbonate

• US 20010014306A1
• Filed: 02/28/2001
• Published: 08/16/2001
• Est. Priority Date: 03/27/1996
• Status: Active Grant

• Current Assignee: Solvay Chemicals Incorporated (Solvac SA)
• Original Assignee: Alun P. James, Graham R. Horne, Lido Signorini, Manfred Mathes, Pier-Luigi Deli, Richard Roesler, Robert Owen, Romano Pardini, Soraya Parvaneh, Stefano Bigini, Uwe Droste
• Inventors: Mathes, Manfred, Horne, Graham R., Roesler, Richard, James, Alun P., Owen, Robert, Bigini, Stefano, Pardini, Romano, Deli, Pier-Luigi, Parvaneh, Soraya, Signorini, Lido, Droste, Uwe
• Granted Patent: US 6,482,385 B2
• Time in Patent Office: Days
• US Class Current: 423/415.2
• CPC Class Codes: C01B 15/103 containing only alkali metals as metals
• CPC Class Codes: C11D 3/128 Aluminium silicates, e.g. zeolites C11D3/1253 takes precedence
• CPC Class Codes: C11D 3/3942 Inorganic per-compounds C11D3/3902 takes precedence

Abstract

Sodium percarbonate is traditionally made in a crystallization process from aqueous hydrogen peroxide and sodium carbonate with recycle of mother liquor in the presence of a substantial concentration of a salting out agent, conventionally sodium chloride.

The invention provides a process intended to be conducted without addition of chloride salting-out agent in which the dissolution step is controlled to restrict the sodium carbonate concentration to below 95%, preferably 60 to 90% of its saturated concentration at a temperature preferably controlled to at most 35C. and the mole ratio of hydrogen peroxide:sodium carbonate in the reaction vessel is controlled to between 0.7 to 1.2:1, and preferably about 1:1.

In some embodiments at least a fraction of the mother liquor introduced into the dissolution tank is obtained by extraction from the reaction vessel and in other embodiments a fraction of the sodium percarbonate is introduced in solution in the mother liquor and a fraction is introduced in particulate form directly into the reaction vessel.

Large particle sodium percarbonate is provided which has a 7 day aged heat emission at 40C. of not more than 3 μW/g measured in a microcalorimeter over 16 hours that is lower than the heat emission from conventionally produced sodium percarbonate employing a chloride salting-out agent.

Claims

1. Dry particulate sodium percarbonate having:

(a) a mean particle size of 500 μ

m to 1200 μ

m; and

(b) a seven day aged heat emission in 16 hours at 40°

C. of below 3 μ

W/g.

2. The sodium percarbonate according to

claim 1

having a moisture pick-up over 24 hours storage at 80% relative humidity and at 32°

C. of not more than 30 g/kg.

3. The sodium percarbonate according to

claim 2

having a moisture pick-up over 24 hours storage at 80% relative humidity and at 32°

C. of not more than 15 g/kg.

4. The sodium percarbonate according to

claim 1

having an apparent bulk density of 800 to 1100 g/kg.

5. The sodium percarbonate according to

claim 4

having an apparent bulk density of 850 to 1000 g/kg.

6. The sodium percarbonate according to

claim 1

having an Avox of at least 14.5% by weight.

7. The sodium percarbonate according to

claim 6

having an Avox of at least 14.8% by weight.

8. The sodium percarbonate according to

claim 1

having a mean particle size of 600 to 650 microns.

9. The sodium percarbonate according to

claim 1

having a mean particle size of about 750 microns.

10. The sodium percarbonate according to

claim 1

containing at least one phosphonate stabiliser and at least one crystal habit modifier selected from sodium silicate and a polyacrylate in a total amount of from 1 to 8 g/kg.

11. The sodium percarbonate according to

claim 1

produced in a process free from chloride.

12. The sodium percarbonate according to

claim 1

produced in a process free from any salting-out agent.

13. The sodium percarbonate according to

claim 1

produced by crystallisation from a bulk solution containing hydrogen peroxide and sodium carbonate.

14. The sodium percarbonate according to

claim 13

obtained using a crystalliser-classifier.

15. The sodium percarbonate according to

claim 1

comprising a core material which is coated with at least one inorganic or organic agent.

16. The sodium percarbonate according to

claim 15

coated with 1 to 10% by weight of coating agent.

17. The sodium percarbonate according to

claim 16

coated with 2 to 5% by weight of coating agent.

18. The sodium percarbonate according to

claim 15

wherein the coating agent is selected from the group consisting of sodium sulphate, sodium silicate, sodium carbonate and binary and ternary mixtures thereof.