Method of making zeolite

Patent metadata

Field	Value
Publication number	US-12459828-B2
Application number	US-202217881173-A
Country	US
Kind code	B2
Filing date	Aug 4, 2022
Priority date	Aug 4, 2022
Publication date	Nov 4, 2025
Grant date	Nov 4, 2025

Abstract

The present disclosure relates to a method of making a zeolite. The method includes mixing an aluminum nitrate with an aqueous solution of NaOH to form a first mixture followed by mixing silica gel with the first mixture to form a second mixture. The second mixture is heated with microwave irradiation to form a first sample. The method further includes washing, drying, and ion exchanging the first sample with ammonium nitrate to form a second sample. The method includes calcining the second sample to form the zeolite, wherein the method does not use a seed or a structural directing agent.

First claim

The invention claimed is:

1 . A method of making a zeolite, the method comprising:
mixing an aluminum nitrate with an aqueous solution of NaOH to form a first mixture; mixing silica gel with the first mixture to form a second mixture; heating the second mixture with microwave irradiation to form a first sample; washing, drying, and ion exchanging the first sample with ammonium nitrate to form a second sample; and calcining the second sample to form the zeolite, wherein the method does not use a seed or a structural directing agent, wherein the zeolite has a molar ratio of Al 2 O 3 :xSiO 2 :yH 2 O:zNaOH, and x is in the range of 30 to 100, y is in the range of 10000 to 35000, and z is in the range of 8 to 30.

2 . The method of claim 1 , wherein the mixing, heating, washing, drying and ion exchanging are carried out in the same reaction vessel.

3 . The method of claim 2 , further comprising:
decanting a supernatant fluid from the first sample then drying the first sample in the same reaction vessel with microwave radiation at a temperature of at least 110° C., then contacting the dried first sample with an ion exchange fluid and heating with microwave radiation to a temperature of from 40 to 85° C.

4 . The method of claim 1 , wherein the second mixture is first heated at 50 to 60° C. for 30 to 90 minutes and then second heated at 150 to 200° C. for 6 to 12 hours.

5 . The method of claim 1 , wherein the second sample is calcined at 500 to 800° C.

6 . The method of claim 1 , wherein the second sample is calcined at 550 to 700° C.

7 . The method of claim 1 , wherein the zeolite is ZSM-5 zeolite.

8 . The method of claim 1 , wherein the zeolite has a substantially similar XRD pattern and acidity as a ZSM-5 zeolite prepared by hydrothermal heating.

9 . The method of claim 1 , wherein the microwave irradiation has a frequency of 300 MHz to 300 GHz.

10 . The method of claim 1 , wherein the microwave irradiation has a wavelength of 0.01 to 1 m.

11 . The method of claim 1 , wherein the microwave irradiation has a power of 5 to 300 W per gram of the second mixture.

12 . The method of claim 1 , wherein the zeolite is in the form of cube-shape particles.

13 . The method of claim 12 , wherein the cube-shape particles have a length, width, and height of 0.5 μm to 5 μm.

14 . The method of claim 1 , wherein the SiO 2 /Al 2 O 3 has a molar ratio of 25 to 35.

15 . The method of claim 1 , wherein the SiO 2 /Al 2 O 3 has a molar ratio of 45 to 55.

16 . The method of claim 1 , wherein the SiO 2 /Al 2 O 3 has a molar ratio of 65 to 75.

17 . The method of claim 1 , wherein the second mixture does not contain tetra propyl ammonium hydroxide, tetra propyl ammonium bromide, or isopropyl amine.

18 . The method of claim 1 , wherein the zeolite has a substantially similar XRD pattern to a zeolite precursor formed after the drying and before the ion exchanging.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Bakare Akolade Idris
• Naseer Galal A
• Sanhoob Mohammed Ahmed
• Yamani Zain Hassan

Classifications

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01P2004/03

  obtained by SEM · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2002/88

  by thermal analysis data, e.g. TGA, DTA, DSC · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title