Process for preparation of highly coordinated sulfated mixed metal oxide catalyst having high crushing strength

Patent metadata

Field	Value
Publication number	US-11731121-B2
Application number	US-202117178619-A
Country	US
Kind code	B2
Filing date	Feb 18, 2021
Priority date	Feb 19, 2020
Publication date	Aug 22, 2023
Grant date	Aug 22, 2023

Abstract

The present invention provides a process of preparing a high coordination sulfated mixed metal oxide catalyst. The process comprises mixing specific ratios of alumina and zirconia mixtures at specific particle size limits which do not exceed 37 μm, in the presence of a combination of α-amino acids, i.e., non-polar side chains and basic side chains having molecular weight less than 250, nitric acid (HNO3) and sulfuric acid (H2SO4) at a pH range of 1.5 to 3.8 at temperatures below 30° C. The catalysts have a high conversion towards hydrocarbon isomerization reaction while concurrently having crushing strength in range of 2.0 daN and 5.0 daN, allowing for efficient commercial application.

First claim

What is claimed is:

1. A process for synthesis of high coordination sulfated mixed metal oxide catalyst, the process comprising:
a) dissolving Zirconium nitrate or acetate in distilled water;
b) precipitating Zirconium hydroxide using diethylamine, washing with double distilled water, and drying;
c) loading sulfate ions on the dried Zirconium hydroxide using Ammonium sulfate or Ammonium persulfate with ammonia as a competing ion;
d) reducing particle size of the sulfate ions loaded Zirconium hydroxide obtained in step (c) from 310 μm to 44 μm by milling;
e) reducing particle size of high surface area acidified alumina from 90 μm to 44 μm by milling, and further mixing with the sulfate ions loaded Zirconium hydroxide obtained in step (c) in a ball mill to obtain a joint particle size of less than 37 μm;
f) adding the mixture obtained in step (e) to a binder liquid comprising α-amino acids, HNO 3 and H 2 SO 4 and mixing to maintain a pH in a range of 1.5 to 3.8, wherein the α-amino acids are a combination of α-amino acid with a non-polar side chain and α-amino acid with a basic side chain;
g) peptizing followed by extruding after settling the mixture obtained in step f) for 30 minutes;
h) drying the extrudates obtained in step g) at 100-200° C. for 6 hours followed by calcination; and
i) adding a hydrogenating component.

2. The process as claimed in claim 1 , wherein α-amino acids, H 2 SO 4 , and HNO 3 are in a weight ratio of 1:1:1 to 2.5:2.4:1.

3. The process as claimed in claim 1 , wherein pH of the Zirconium hydroxide obtained in step (b) is in a range of 9.0-11.0.

4. The process as claimed in claim 1 , wherein drying in step (c) is carried out at a temperature of 100 to 130° C. for 6 hours.

5. The process as claimed in claim 1 , wherein an extruder in step (g) is a single screw axial extruder having a thickness of 1-2 mm.

6. The process as claimed in claim 1 , wherein the calcination in step (h) is carried out at a temperature range of 550 to 800° C. for 3 hours.

7. The process as claimed in claim 1 , wherein the hydrogenating component is selected from Platinum, Palladium, and a combination thereof.

8. The process as claimed in claim 1 , wherein the α-amino acid with the non-polar side chain is selected from Glycine, Alanine, Valine, Leucine, Isoleucine, Methionine, Proline and Phenylalanine; with molar concentration in a range of 1 to 2M.

9. The process as claimed in claim 1 , wherein, the α-amino acid with the basic side chain is selected from Lysine, Arginine and Histidine, with molar concentration in a range of 2 to 3M.

Assignees

• Viridis Chemicals Private Ltd
• Indian Oil Corp Ltd

Inventors

• Sampara Chaitanya
• Varshney Pushkar
• Manna Reshmi
• Subramani Saravanan
• Sau Madhusudan
• Bhattacharyya Debasis
• RAMAKUMAR Sankara Sri Venkata

Classifications

• B01J35/40

  characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) · CPC title

• B01J35/391 Primary

  Physical properties of the active metal ingredient · CPC title

• B01J35/0046 Primary

  Operations & Transport · mapped topic

• B01J21/066

  Zirconium or hafnium; Oxides or hydroxides thereof · CPC title

• B01J23/42

  Platinum · CPC title