Synthesis of functionalized carbon microspheres and their catalyst activity in C—O and C—N bond formation reactions

Patent metadata

Field	Value
Publication number	US-10029240-B2
Application number	US-201414901456-A
Country	US
Kind code	B2
Filing date	Jun 25, 2014
Priority date	Jun 25, 2013
Publication date	Jul 24, 2018
Grant date	Jul 24, 2018

Abstract

Disclosed herein is a simple process for functionalization/grafting of carbon microspheres obtained from bagasse with various active functional groups onto it and use of the same as catalyst for various organic reactions, having very high selectivity and conversion rate.

First claim

The invention claimed is:

1. A process for preparation of functionalized carbon microspheres by grafting catalytically active functional groups on to carbon microspheres obtained from bagasse to generate an acidic or basic surface wherein said process comprises the steps of:
a) heating bagasse, water and oxalic acid at a temperature ranging between 150 to 180 ° C. for a time period ranging between 6 to 12 hours to obtain carbon microspheres; and
b) refluxing of carbon microspheres as obtained in step (a) and an organic solvent selected from the group consisting of n-pentane, n-hexane, toluene, and lower alcohols in the presence of a functional group grafting agent at a temperature ranging between 80-120 ° C. for a time period in the range of 8 to 12 hours to obtain functionalized carbon microspheres,
wherein the functionalized carbon microspheres catalyze C—O and C—N bond formation reactions in high selectivity of 90% to 100% and conversion rate of 45 to 95% or 10 to 98%.

2. A process for preparation of functionalized carbon microspheres by grafting catalytically active functional groups on to carbon microspheres obtained from bagasse to generate an acidic or basic surface, the process comprising:
heating bagasse, water and oxalic acid at a temperature of 150 to 180 ° C. for a time period of 6 to 12 hours to obtain carbon microspheres; and
refluxing the carbon microspheres and an organic solvent selected from the group consisting of n-pentane, n-hexane, toluene, and lower alcohols in the presence of a functional group grafting agent at a temperature of 80-120 ° C. for a time period of 8 to 12 hours to obtain functionalized carbon microspheres,
wherein the functional group grafting agent is selected from the group consisting of 3-aminopropyltrimethoxysilane (APTMS), (3-(2aminoethylamino) propyl)-trimethoxysilane, (3-mercaptopropyl)-trimethoxysilane, and 3-cyanopropyltriethoxysilane.

3. The process as claimed in claim 1 , wherein the active functional groups are selected from the group consisting of silylated acid, amine, and SO 3 H groups to obtain acidic, or basic functional characteristics.

4. The process as claimed in claim 1 , wherein the diameter or the particle size of the functionalized carbon microspheres (CMS) is 1 to 5 μm.

Assignees

• Council Scient Ind Res

Inventors

• Biradar Ankush Venkatrao
• Umbarkar Shubhangi Bhalchandra
• Dongare Mohan Keraba

Classifications

• B01J2231/4205

  C-C cross-coupling, e.g. metal catalyzed or Friedel-Crafts type · CPC title

• B01J31/08

  Ion-exchange resins · CPC title

• B01J31/0237 Primary

  Amines · CPC title

• B01J37/0209

  involving a reaction between the support and a fluid · CPC title

• C07C201/14

  by formation of nitro groups together with reactions not involving the formation of nitro groups · CPC title