Apparatus and method for continuous solvothermal synthesis of nanoparticles

Patent metadata

Field	Value
Publication number	US-11577966-B2
Application number	US-202117174233-A
Country	US
Kind code	B2
Filing date	Feb 11, 2021
Priority date	Feb 13, 2020
Publication date	Feb 14, 2023
Grant date	Feb 14, 2023

Abstract

An apparatus and a method for continuous solvothermal synthesis of nanoparticles, are provided. The apparatus includes an inlet section, a reactor section, a flexible quenching unit, and an outlet section. The inlet section separately receives reactants including the solvent and a precursor solution that are allowed to flow into the reactor section. The reactor section includes multiple spiral turns such that each of the spiral turns includes a helical channel followed by a counter-helical channel for enabling mixing of the reactants to cause solvothermal reactions between them. The counter-helical channel changes the direction of flow of reactants upon flow of said reactants from the helical channel to the counter-helical channel. The flexible quenching section enclosing a portion of the reactor section quenches a slurry formed as a result of the solvothermal reactions, wherein the slurry includes the nanoparticles of targeted characteristics. The outlet section facilitates withdrawal of the slurry.

First claim

What is claimed is:

1. An apparatus for continuous solvothermal synthesis of nanoparticles, comprising:
an inlet section comprising a plurality of inlet portions for separately receiving at least a metallic precursor solution and a solvent;
a reactor section extending from the inlet section, the reactor section enabling continuous mixing resulting in solvothermal reactions between the metallic precursor solution and the solvent, and further nanoparticles formation and nanoparticles growth, the reactor section comprising a spiral section having a plurality of spiral turns, each spiral turn of the plurality of spiral turns having a helical channel followed by a counter-helical channel, wherein the metallic precursor solution and the supercritical fluid interchanges the flow direction for enabling mixing between the metallic precursor solution and the solvent, and wherein the solvothermal reactions between the metallic precursor solution and the solvent yields a slurry comprising nanoparticles;
a flexible quenching unit enclosing a set of spiral turns from amongst the plurality of spiral turns, the set of spiral turns configured in proximity to an exit portion of the reactor section, the flexible quenching unit capable of holding a quenching fluid for rapidly reducing temperature of the reactor section to a set temperature, further wherein the flexible quenching unit capable of adjusting a number of the set of spiral turns based on targeted particle characteristics of the nanoparticles; and
an outlet section configured at an exit portion of the reactor section for collecting the slurry of nanoparticles.

2. The apparatus of claim 1 , wherein the solvent comprises one of an organic solvent, an inorganic solvent, and a supercritical fluid.

3. The apparatus of claim 1 , wherein the mixing section comprises a plurality of baffles configured within at least one of a helical channel of the plurality of helical channels and a counter-helical channel of the plurality of counter-helical channels for enhanced mixing of the metallic precursor solution and the solvent.

4. The apparatus of claim 1 , further comprising a first connector for coupling the inlet section with the reactor section.

5. The apparatus of claim 1 , wherein a number of the plurality of spiral turns is adjusted based on the targeted nanoparticle characteristics.

6. The apparatus of claim 4 , further comprising a plurality of second connectors, wherein each second connector from amongst the plurality of second connectors is capable of coupling and decoupling a helical channel to a corresponding counter-helical channel to adjust the number of the plurality of spiral turns.

7. The apparatus of claim 1 , wherein the flexible quenching unit comprises:
an enclosure around the set of spiral turns for holding the quenching fluid capable of reducing temperature of the reactor section to the set temperature;
an inlet configured on an outer portion of the enclosure for facilitating introduction of the quenching fluid to the enclosure; and
an outlet configured on the outer portion of the enclosure for facilitating removal of the quenching fluid from the enclosure.

8. The apparatus of claim 7 , further comprising a locking mechanism for holding the quenching unit with the set of spiral turns of the reactor section, the locking mechanism comprising a support structure for holding the quenching unit, and a plurality of screws mounted on the support structure for adjusting size of the enclosure.

9. A method for continuous solvothermal synthesis of nanoparticles, the method comprising:
introducing, in an apparatus for continuous solvothermal synthesis of nanoparticles, a metallic precursor solution and a solvent, the apparatus comprising:

an inlet section comprising a plurality of inlet portions for separately receiving at least the metallic precursor solution and the solvent;
a reactor section extending from the inlet section, the reactor section enabling continuous mixing resulting in solvothermal reactions between the metallic precursor solution and the solvent, and further nanoparticles formation and nanoparticles growth, the reactor section comprising a spiral section having a plurality of spiral turns, each spiral turn of the plurality of spiral turns having a helical channel followed by a counter-helical channel, wherein the metallic precursor solution and the supercritical fluid interchanges the flow direction for enabling mixing between the metallic precursor solution and the solvent, and wherein the solvothermal reactions between the metallic precursor solution and the solvent yields a slurry comprising nanoparticles;
a flexible quenching unit enclosing a set of spiral turns from amongst the plurality of spiral turns, the set of spiral turns configured in proximity to an exit portion of the reactor section, the flexible quenching unit capable of holding a quenching fluid for rapidly reducing temperature of the reactor section to a set temperature, further wherein the flexible quenching unit capable of adjusting a number of the set of spiral turns based on targeted particle characteristics of the nanoparticles; and
an outlet section configured at an exit portion of the reactor section for collecting the slurry of nanoparticles;
quenching the slurry, in the flexible quenching unit, to obtain the nanoparticles of targeted characteristics; and
collecting, at the outlet section, the slurry quenched in the quenching unit.

Assignees

• Tata Consultancy Services Ltd
• Tata Consultancy Services Limiteg

Inventors

• Pukkella Arjun Kumar
• Subramanian Sivakumar
• Nadimpalli Nagaravi Kumarvarma
• Vysyaraju Raviraju
• Runkana Venkataramana

Classifications

• B82Y40/00

  Manufacture or treatment of nanostructures · CPC title

• B22F2998/00

  Supplementary information concerning processes or compositions relating to powder metallurgy · CPC title

• B82B3/0004

  Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same · CPC title

• B01J2203/068

  Crystal growth · CPC title

• B01J2219/1944

  spiral · CPC title