Apparatus for preparing inorganic compound and method of preparing inorganic compound using the same

Patent metadata

Field	Value
Publication number	US-9865874-B2
Application number	US-201314432350-A
Country	US
Kind code	B2
Filing date	Nov 27, 2013
Priority date	Nov 27, 2012
Publication date	Jan 9, 2018
Grant date	Jan 9, 2018

Abstract

Disclosed is a hydrothermal synthesis device for continuously preparing an inorganic slurry using a hydrothermal method. The hydrothermal synthesis device includes a mixer to mix at least one precursor solution for preparing an inorganic material, injected via at least one supply tube, to prepare an intermediate slurry, a connection tube provided at a side of the mixer, continuously discharging the prepared intermediate slurry to a reactor, and having an inner surface contacting a precursor solution mixture on which abrasive polishing has been performed, and the reactor performing hydrothermal reaction of the intermediate slurry supplied from the connection tube by receiving a liquid stream heated to supercritical or subcritical conditions using a heat exchanger and connected to the connection tube into which the intermediate slurry prepared from the mixer is introduced and to at least one injection tube into which the heated liquid stream is injected.

First claim

The invention claimed is:

1. A hydrothermal synthesis device for continuously preparing an inorganic slurry using a hydrothermal method, the hydrothermal synthesis device comprising:
a mixer to mix at least one precursor solution for preparing an inorganic material, injected via at least one supply tube, to prepare an intermediate slurry;
a connection tube provided at a side of the mixer, continuously discharging the prepared intermediate slurry via the connection tube to a reactor, and having an inner surface contacting a precursor solution mixture on which abrasive polishing has been performed; and
the reactor performing hydrothermal reaction of the intermediate slurry supplied from the connection tube by receiving a liquid stream heated to supercritical or subcritical conditions using a heat exchanger and connected to the connection tube into which the intermediate slurry prepared from the mixer is introduced and to at least one injection tube into which the heated liquid stream is injected; and

wherein the connection tube is provided at an outer portion thereof with a cooling member to dissipate heat transferred from the heated liquid stream in order to maximize the effects of the abrasive polishing with respect to the prevention of clogging in the connection tube.

2. The hydrothermal synthesis device according to claim 1 , wherein the supply tube comprises a first supply tube disposed at a central portion of an upper surface of the mixer, a second supply tube disposed at a side part of the mixer so as to form an internal angle of 10° to 90° with respect to the first supply tube, and a third supply tube disposed at another side of the mixer so as to face the second supply tube.

3. The hydrothermal synthesis device according to claim 1 , wherein the connection tube comprises an austenite-based stainless steel material.

4. The hydrothermal synthesis device according to claim 3 , wherein the austenite-based stainless steel material is selected from STAINLESS STEEL 304, STAINLESS STEEL 316, STAINLESS STEEL 304L, or STAINLESS STEEL 316L.

5. The hydrothermal synthesis device according to claim 1 , wherein the abrasive polishing is performed by at least one method selected from mechanical polishing, chemical polishing, chemical mechanical polishing, or electropolishing.

6. The hydrothermal synthesis device according to claim 1 , wherein the abrasive polishing is performed by electropolishing.

7. The hydrothermal synthesis device according to claim 6 , wherein the electropolishing is performed by a process comprising:
pre-treatment comprising acid treatment and water cleaning of an inner surface of the connection tube;
electropolishing of the inner surface of the connection tube; and
post-treatment comprising neutralization of an electropolishing solution and water cleaning.

8. The hydrothermal synthesis device according to claim 7 , wherein the electropolishing solution comprises sulfuric acid and phosphoric acid.

9. The hydrothermal synthesis device according to claim 1 , wherein an entire inner surface of the connection tube is abrasively polished.

10. The hydrothermal synthesis device according to claim 1 , wherein an amount of an inorganic material in the inorganic slurry is 0.05 wt % to 5 wt %.

11. The hydrothermal synthesis device according to claim 1 , wherein a hydrophobic coating is formed on an inner surface of at least one of the mixer, the reactor, and the injection tube.

12. The hydrothermal synthesis device according to claim 1 , wherein the liquid stream is supercritical water heated under conditions of a temperature of 350° C. to 800° C. and a pressure of 180 bar to 550 bar.

13. The hydrothermal synthesis device according to claim 1 , wherein the injection tube comprises two injection tubes positioned at outer sides of the reactor.

14. A method of preparing an inorganic slurry by using the hydrothermal synthesis device according to claim 1 , the method comprising:
injecting, into a mixer, a first precursor solution for preparation of an inorganic material via a first supply tube and a second precursor solution for preparation of an inorganic material via each of second and third supply tubes;
introducing, into a reactor, an intermediate slurry prepared through mixing of the injected first and second precursor solutions via a connection tube;
injecting supercritical water containing high-temperature and high-pressure water into the reactor via an injection tube;
dissipating heat, transferred from the heated liquid stream to the connection tube, by the cooling member provided at an outer portion of the connection tube; and
preparing an inorganic slurry by hydrothermal reaction in the reactor and continuously discharging the prepared inorganic slurry therefrom.

Assignees

• Lg Chemical Ltd

Inventors

• Noh Hyun Kuk
• Ryu Ji Hoon
• Jung Wang Mo
• Park Hong Kyu
• Oh Sang Seung
• Jo Chi Ho

Classifications

• Y02P20/54

  using solvents, e.g. supercritical solvents or ionic liquids · CPC title

• B01J2219/02

  Apparatus characterised by their chemically-resistant properties · CPC title

• H01M4/5825 Primary

  Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines · CPC title

• B01J2219/0286

  Steel · CPC title

• B01J4/002

  Nozzle-type elements (nozzle-type reactors B01J19/26) · CPC title