Process for preparing chromium(III) oxide

Patent metadata

Field	Value
Publication number	US-9663383-B2
Application number	US-201113635963-A
Country	US
Kind code	B2
Filing date	Mar 23, 2011
Priority date	Mar 23, 2010
Publication date	May 30, 2017
Grant date	May 30, 2017

Abstract

The present invention relates to a process for preparing chromium(III) oxide by reaction of alkali metal chromate with gaseous ammonia, subsequent hydrolysis, isolation of the hydrolysis product and calcination.

First claim

What is claimed is:

1. A process for preparing chromium(III) oxide, the process comprising:
a) reacting an alkali metal chromate with gaseous ammonia at a temperature of 200 to 600° C., thereby forming a reaction product,
b) hydrolysing the reaction product, wherein the hydrolysing comprises one of:
reducing the pH of water used for the hydrolysing before hydrolysing, or
reducing the pH of a resultant alkaline mother liquor during or after hydrolysing,
to a pH value of from 4 to 11, by adding an acid to the water or resultant mother liquor, whereby a hydrolysis product is formed,

c) isolating the hydrolysis product formed in step b), and
d) calcinating the hydrolysis product of step c) at a temperature of 700 to 1400° C. to produce a calcined chromium(III) oxide product.

2. The process according to claim 1 , wherein reacting the alkali metal chromate with gaseous ammonia comprises reacting the alkali metal chromate with gaseous ammonia in an indirectly heated reactor.

3. The process according to claim 1 , wherein the alkali metal chromate is sodium dichromate, sodium dichromate dihydrate or potassium dichromate.

4. The process according to claim 1 , wherein the acid is an inorganic acid or an organic acid.

5. The process according to claim 1 , further comprising:
suspending the calcined product obtained from step d) in water, and
subsequently drying the calcined product.

6. The process according to claim 1 , further comprising:
suspending the calcined product obtained from step d) in water,
washing the calcined product with water one or more times,
subsequently drying the calcined product, and
thereafter milling the calcined product.

7. The process according to claim 1 , further comprising adding before calcinating, in an amount of 0.01% by weight to 3.0% by weight, based on a product used for the calcinating, a compound selected from the group consisting of alkali metal halides, ammonium halides, alkaline earth metal halides, fluorides, chlorides, bromides, iodides of sodium or potassium or ammonium, alkali metal hydroxides, sodium hydroxide, potassium hydroxide, and chromic acid.

8. The process according to claim 1 , wherein hydrolyzing the reaction product comprises reducing the pH to a pH value of 5 to 10.

9. The process according to claim 1 , wherein calcining the hydrolysis product comprises calcinating the hydrolysis product at a temperature of 800 to 1300° C.

10. The process according to claim 1 , wherein reacting the alkali metal chromate with gaseous ammonia comprises reacting the alkali metal chromate with gaseous ammonia in a rotary tube furnace or in a fluidized bed.

11. The process according to claim 1 , wherein the acid is carbon dioxide.

12. The process according to claim 1 , further comprising adding before calcinating, in an amount of 0.02% by weight to 1.0% by weight, based on a product used for the calcinating, a compound selected from the group consisting of alkali metal halides, ammonium halides, alkaline earth metal halides, fluorides, chlorides, bromides, iodides of sodium or potassium or ammonium, alkali metal hydroxides, sodium hydroxide, potassium hydroxide, and chromic acid.

13. The process according to claim 1 , wherein:
the alkali metal chromate has a particle size of less than 1000 μm, and
the temperature for reacting the alkali metal chromate with the gaseous ammonia is 200 to 500° C.

14. The process according to claim 1 , wherein:
the alkali metal chromate has a particle size of less than 300 μm,
the reaction of the alkali metal chromate with the gaseous ammonia is started at a temperature of 200 to 300° C. and is increased continuously or step wise, and
the process further comprises removing samples of the reaction product during the reaction of the alkali metal chromate with the gaseous ammonia, forming a suspension of the sampled product in water, checking the pH of the suspension, and ending the reaction of the alkali metal chromate with the gaseous ammonia when the pH of a resulting suspension of the reaction product reaches at least 11.

15. The process according to claim 14 , wherein the reaction is ended when the pH of a resulting suspension of the reaction product reaches at least 13.

16. The process according to claim 14 , wherein:
the alkali metal chromate is sodium dichromate, sodium dichromate dihydrate or potassium dichromate,
the temperature for reacting the alkali metal chromate with the gaseous ammonia is 200 to 500° C.,
the acid is carbon dioxide,
after isolating the hydrolysis product, the hydrolysis product is further washed with water mixed with an acid to reduce the pH, and
after calcining, the method further comprises:
suspending the calcined product in water,
washing the calcined product with water one or more times,
subsequently drying the calcined product, and
thereafter milling the calcined product.

Assignees

• Ortmann Rainer
• Stenger Matthias
• Boll Matthias
• Friedrich Holger
• Lanxess Deutschland Gmbh

Inventors

• Ortmann Rainer
• Stenger Matthias
• Boll Matthias
• Friedrich Holger

Classifications

• C01G37/00

  Compounds of chromium · CPC title

• C01G37/033 Primary

  Chromium trioxide; Chromic acid · CPC title

• C09C1/346

  Chromium oxides · CPC title

• C01P2006/80

  Compositional purity · CPC title