Method for treating an ammonium salt

Patent metadata

Field	Value
Publication number	US-12076708-B2
Application number	US-202318116666-A
Country	US
Kind code	B2
Filing date	Mar 2, 2023
Priority date	May 30, 2018
Publication date	Sep 3, 2024
Grant date	Sep 3, 2024

Abstract

A thermal method of forming ferric oxide nano/microparticles with predominant morphology is described using different solvents. Methods of using the Fe3O4 nano/microparticles as catalysts in the reduction of nitro compounds with sodium borohydride to the corresponding amines and decomposition of ammonium salts.

First claim

The invention claimed is:

1. A method, comprising:
heating a composition comprising a ferric halide and an alkali metal salt of a carboxylic acid in hexane at a temperature of 150-300° C. in a sealed container to form ferric oxide microparticles; and
contacting an ammonium salt with the ferric oxide microparticles,
wherein the ferric oxide microparticles have an octahedron morphology,
wherein on the contacting the ammonium salt is decomposed, and
wherein the ammonium salt has a final decomposition temperature of 420° C.

2. The method of claim 1 , wherein the ferric halide is ferric chloride.

3. The method of claim 1 , wherein the alkali metal salt of a carboxylic acid is sodium acetate.

4. The method of claim 1 , wherein the heating temperature is in the range of about 195 to 205° C.

5. The method of claim 1 , wherein the composition consists of a ferric halide and an alkali metal salt of a carboxylic acid in hexane.

6. The method of claim 1 , wherein a particle diameter of the ferric oxide microparticles catalyst is about 4.3 μm.

7. The method of claim 1 , wherein the ferric halide is selected from the group consisting of ferric fluoride, ferric chloride, ferric bromide, and ferric iodide.

8. The method of claim 1 , wherein the carboxylic acid of the alkali metal salt of a carboxylic acid is selected from the group consisting of formic acid, acetic acid, propionic acid, butyric acid, citric acid, oxalic acid, and tartaric acid.

9. The method of claim 1 , wherein the composition is heated for 8 to 36 hours.

10. The method of claim 1 , wherein the composition is heated for 12 to 24 hours.

11. The method of claim 1 , wherein the composition does not comprise a templating agent.

12. The method of claim 1 , wherein the ferric oxide microparticles are aggregated.

13. The method of claim 12 , wherein aggregates of the aggregated ferric oxide microparticles are in a form of a cylinder.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Janjua Muhammad Ramzan Saeed Ashraf
• Jamil Saba
• Khan Shanza Rauf

Classifications

• B01J35/77

  Compounds characterised by their crystallite size · CPC title

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J35/55

  Cylinders or rings · CPC title