Granted Patent B2

US 12,448,348 · App. 17/416,742 · Granted Oct 21, 2025

Inventors: Thirumalaiswamy Raja (Maharashtra, IN); Nikitra Nihal Chand Gupta (Maharashtra, IN); Vipul Subhash Patil (Maharashtra, IN); Amrin Sattarkhan Punekar (Maharashtra, IN)

Assignee: Council of Scientific & Industrial Research

C07C231/065B01J19/008B01J23/63B01J37/0045B01J37/0063B01J37/04B01J37/082

Abstract

Claims (35)

1. A metal oxide-catalyzed process for hydration of nitrile using a catalyst of formula (I), under the influence of ultrasonic cavitation of Frequency 16-28 khz to achieve the maximum conversion and selectivity at lower temperature (35° C.) comprising:

heating a reaction mixture of nitrile, solvent, catalyst of formula (I), with or without cavitation influence, at a temperature range of 30 to 140° C. for a time period in the range of 5 to 10 hours (without cavitation and 1 hr with cavitation), to form a respective amide, wherein said nitrile is selected from aliphatic or aromatic nitrile,

wherein the catalyst of formula (I) is represented as:

A X B Y C Z    Formula (I)

wherein:

A is a promoter, wherein said promoter is a lanthanide, wherein said lanthanide is selected from the group consisting of divalent metals, trivalent metals and mixtures of oxides of said metals;

x is the weight % of the promoter in the range of 0.01-99;

B is a support, wherein said support is a transition element or an inner transition element;

y is the weight % of catalyst support in the range of 0.01-99;

C is a co-promoter, wherein said co-promoter is selected from oxides of transition elements having variable oxidation states ranging from 1 to 8 from group number VIII;

z is the weight % of the co-promoter in the range of 0.01-25; and

x+y≥75 weight %.

2. The metal oxide-catalyzed process as claimed in claim 1 , wherein said nitrile is selected from the group consisting of 2-Cyanopyridine, 3-Cyanopyridine, 4-Cyanopyridine, Benzonitrile, Acetonitrile, O-tolunitrile and methoxyacetonitrile.

3. The metal oxide-catalyzed process as claimed in claim 1 , wherein said solvent is selected from the group consisting of water, methanol, ethanol and mixture thereof.

4. The metal oxide-catalyzed process as claimed in claim 1 , wherein said amide is selected from the group consisting of 2-Picolinamide, 3-Picolinamide, 4-Picolinamide, Benzamide, Acetamide, O-toluamide and methoxyacetamide.

5. A catalyst of formula (I) represented as:

A X B Y C Z    Formula (I)

wherein:

A is a promoter, wherein said promoter is a lanthanide, wherein said lanthanide is selected from the group consisting of divalent metals, trivalent metals and mixtures of oxides of said metals;

x is the weight % of the promoter in the range of 0.01-99;

B is a support, wherein said support is a transition element or an inner transition element;

y is the weight % of catalyst support in the range of 0.01-99;

C is a co-promoter, wherein said co-promoter is selected from oxides of transition elements having variable oxidation states ranging from 1 to 8 from group number VIII;

z is the weight % of the co-promoter in the range of 0.01-25; and

x+y≥75 weight %;

wherein A is not praseodymium; and

wherein B is not praseodymium.

6. A process for the preparation of the catalyst of formula (I) as claimed in claim 5 , comprising the steps of:

a) dissolving metal nitrate hexahydrate in a solvent followed by vigorous stirring, wherein the addition of precursor started at 5° C. by keeping beaker in the chiller and continued until solution temperature reaches 25° C. to 30° C. to form a solution A;

b) mixing a metal precursor 1 into a metal precursor 2 solution by adding an excess of solvent to form a solution B;

c) adding solution B of step (b) into solution A of step (a) with constant stirring at a temperature in the range of 25° C. to 30° C. to form slurry and;

d) aging the slurry of step (c) at the temperature in the range of 70° C. to 200° C. for a time period in the range of 24 to 30 hours followed by drying and calcination with ramp rate of 1-5° C./min to 150-220° C. for period in the range of 1-30 hrs to obtain a material; and

e) cooling and fine crushing the material and further calcinations at 450-550° C. with ramp rate of 1-5° C./min for 1-30 hrs then finally heated to 900° C. and keeping constant for 5-50 h to form the catalyst of formula (I).

7. The process for the preparation of the catalyst of formula (I) as claimed in claim 6 , wherein said metal nitrate hexahydrate of step (a) is cerium nitrate hexahydrate and said solvent of step (a) is selected from the group consisting of water, methanol, ethanol, and a mixture thereof.

8. The process for the preparation of the catalyst of formula (I) as claimed in claim 6 , wherein said metal precursor 1 of step (b) is selected from lanthanum or samarium salt and said metal precursor 2 of step (b) is ruthenium salt.

Assignments (1)

Priority Claims (1)

Continuity (1)

References Cited (30)