Method for reducing a nitro compound to an amine compound

Patent metadata

Field	Value
Publication number	US-12090470-B2
Application number	US-202418616331-A
Country	US
Kind code	B2
Filing date	Mar 26, 2024
Priority date	May 30, 2018
Publication date	Sep 17, 2024
Grant date	Sep 17, 2024

Abstract

A thermal method of forming ferric oxide nano/microparticles with predominant morphology is described using different solvents. Methods of using the Fe 3 O 4 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 for reducing a nitro compound to an amine compound with an iron oxide catalyst, comprising:
contacting a solution comprising the nitro compound and sodium borohydride with a ferric oxide octahedral particles catalyst, wherein the ferric oxide octahedral particles catalyst has an octahedron morphology in an amount that is more than any other morphology or combination of morphologies;
wherein the ferric oxide octahedral particles catalyst is formed by:
heating a composition comprising a ferric halide and an alkali metal salt of a carboxylic acid in a solvent at a temperature of 150-300° C. in a sealed container,
wherein the solvent consists of hexane.

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 to form the ferric oxide octahedral particles catalyst 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 ferric oxide octahedral particles 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 to form the ferric oxide octahedral particles catalyst.

10. The method of claim 1 , wherein the composition is heated for 12 to 24 hours to form the ferric oxide octahedral particles catalyst.

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 octahedral particles catalyst comprises aggregated ferric oxide nano particles.

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