Continuous flow process for the synthesis of metal nanowires using bubble column reactor

Patent metadata

Field	Value
Publication number	US-12318844-B2
Application number	US-202017756037-A
Country	US
Kind code	B2
Filing date	Nov 12, 2020
Priority date	Nov 15, 2019
Publication date	Jun 3, 2025
Grant date	Jun 3, 2025

Abstract

A continuous flow process for the synthesis of metal nanowires using a bubble column reactor. Also disclosed are different types of multiphase bubble column reactors for synthesizing metal nanowires in high yields and purity through a continuous process. The continuous process provides tunability for the aspect ratio of the nanowires.

First claim

We claim:

1. A continuous flow process for the synthesis of metal nanowires, wherein the said process employs at least one unstirred bubble column reactor, and wherein the said process comprises the steps of:
a) dissolving a metal salt in ethylene glycol to obtain a solution A;
b) preheating ethylene glycol and dissolving poly (vinyl pyrrolidone) (PVP 40,000-360,000) to obtain a solution B;
c) continuously feeding a blend of the solution A, solution B and a solution of FeCl 3 in ethylene glycol to the at least one unstirred bubble column reactor from a bottom inlet;
d) maintaining the temperature in each reactor at 130-190° C., with a cumulative residence time of 25-80 min; and
e) allowing the growth of nanowires of the metal to the desired dimensions,
wherein the aspect ratio of said nanowire is tunable in the range of 300 to 1200 with 100% purity, and the conversion of metal salt is in the range of 85% to 95%.

2. The process as claimed in claim 1 , wherein the process employs at least two unstirred bubble column reactors.

3. The process as claimed in claim 1 , wherein a plurality of unstirred bubble column reactors are connected in series.

4. The process as claimed in claim 1 , wherein 2-10 unstirred bubble column reactors are connected in series.

5. The process as claimed in claim 1 , wherein the metal salt of step (a) is silver nitrate.

6. The process as claimed in claim 1 , wherein solution A is 0.25 to 0.65 M solution of silver nitrate in ethylene glycol.

7. The process as claimed in claim 1 , wherein solution B is 0.077 M solution of poly vinyl pyrrolidone in ethylene glycol.

8. The process as claimed in claim 1 , wherein the continuous flow process for the synthesis of metal nanowires comprises the steps of:
a) dissolving a metal salt into ethylene glycol to obtain 0.25 to 0.65 M solution of metal salt;
b) preheating ethylene glycol to 110° C. and dissolving poly (vinyl pyrrolidone) (PVP; 40,000-360,000) to obtain a 0.077 M solution of PVP;
c) continuously feeding a blend of the 0.25 to 0.65 M metal salt, the 0.077 M PVP, and 800 μM FeCl 3 in ethylene glycol solution to the at least one unstirred bubble column reactor;
d) maintaining the temperature in each reactor at 130-190° C., with a cumulative residence time of 25-80 min; and
e) allowing the growth of nanowires of the metal to the desired dimensions.

9. The process as claimed in claim 1 , wherein the at least one unstirred bubble column reactor comprises: a column alone or in series with at least one more column optionally comprising at least one external or one internal air loop or said column comprising one or at least two sections, the diameter of each section being same, the sections connected by a narrower section, wherein the ratio of diameter of narrow section:diameter of section is in the range 0.2 to 0.5 and the ratio of the length of section:diameter of section is always 1 to 2; a sintered plate sparger or a ring sparger wherein the diameter of the sparger is equal to or greater than the diameter of the narrow section, with a superficial air velocity of 0.01-0.06 m/s and at least two air jets of 1 mm diameter and a velocity >1 meter/second.

10. The process as claimed in claim 1 , wherein the at least one unstirred bubble column reactor further comprises one or more multiphase unstirred reactors wherein said reactor further comprises a simple unstirred bubble column reactor or an unstirred, sectionalized bubble column reactor with perforated plates or an unstirred sectionalized bubble column with plurality of compartments having no perforated plates or an internal air-lift loop reactor or external air-lift loop reactor with draft tube having diameter of 0.1-0.4 times the column diameter and the ratio of the reactor height to diameter in the range 6-20 and a sparger (ring sparger or sintered sparger) with at least one air jet periodically operated at 0.5 mm to 2 mm diameter with a jet air velocity >1 meter/second, wherein the diameter of the sparger is equal to the diameter of the column.

Assignees

• Council Scient Ind Res

Inventors

• Kulkarni Amol Arvind
• Kate Prachi
• Patil Suneha

Classifications

• B22F2301/255

  Silver or gold · CPC title

• B01J2204/002

  the feeding side being of particular interest · CPC title

• B01J19/1862

  placed in series · CPC title

• B01J10/002 Primary

  carried out in foam, aerosol or bubbles · CPC title

• B01J4/004

  Sparger-type elements · CPC title