Nanoparticle Mass Purification System and Nanoparticle Mass Purification Method Using Same

Patent metadata

Field	Value
Publication number	US-2023173508-A1
Application number	US-202017995509-A
Country	US
Kind code	A1
Filing date	Apr 9, 2020
Priority date	Apr 7, 2020
Publication date	Jun 8, 2023
Grant date	—

Abstract

The present invention provides a nanoparticle mass purification system capable of purifying nanoparticles at high yield and high purify from a nanoparticle synthesis stock solution synthesized in large quantities, and reusing the used solvent by recovery, and a nanoparticle mass purification method using same.

First claim

1 . A system of purifying nanoparticles, the system comprising:
a first mix tank configured to prepare a first reaction mixture by mixing a crude solution for nanoparticle synthesis and a first mix solvent; a first continuous centrifuge configured to primarily separate nanoparticles and a first filtrate by centrifuging the first reaction mixture supplied from the first mix tank; a second mix tank configured to prepare a second reaction mixture by mixing the first filtrate supplied from the first continuous centrifuge and a second mix solvent; and a second continuous centrifuge configured to secondarily separate the nanoparticles and a second filtrate by centrifuging the second reaction mixture supplied from the second mix tank.

2 . The system of purifying nanoparticles of claim 1 , further comprising:
a third mix tank configured to prepare a third reaction mixture by mixing the second filtrate supplied from the second continuous centrifuge and a third mix solvent.

3 . The system of purifying nanoparticles of claim 2 , further comprising:
a distillation device configured to separate, in a distillation manner, a mix solvent and the nanoparticles from the third reaction mixture of the third mix tank or from the second filtrate separated by the second continuous centrifuge.

4 . The system of purifying nanoparticles of claim 3 , wherein the distillation device comprises:
a distillation heat exchanger into which the third reaction mixture or the second filtrate is supplied; and at least one heater disposed in contact with the distillation heat exchanger.

5 . The system of purifying nanoparticles of claim 3 , further comprising at least one solvent storage tank connected to the distillation device and configured to store a solvent recovered by distillation.

6 . The system of purifying nanoparticles of claim 5 , further comprising a plurality of solvent supply tanks,
wherein the solvent storage tank is connected to at least one of the plurality of solvent supply tanks and the first to third mix tanks such that the recovered solvent is reused.

7 . The system of purifying nanoparticles of claim 1 , further comprising a monitoring unit installed at a predetermined position in a pipe where the first continuous centrifuge and the second mix tank are connected.

8 . The system of purifying nanoparticles of claim 1 , wherein each of the first continuous centrifuge and the second continuous centrifuge includes an inert gas supply for supplying an inert gas into the first continuous centrifuge and the second continuous centrifuge.

9 . A method of purifying nanoparticles, the method comprising:
(i) preparing a first reaction mixture by mixing a crude solution for nanoparticle synthesis and a first mix solvent; (ii) primarily separating nanoparticles and a first filtrate from the first reaction mixture using a continuous centrifuge; (iii) preparing a second reaction mixture by mixing the first filtrate and a second mix solvent; and (iv) secondarily separating the nanoparticles and a second filtrate from the second reaction mixture using a continuous centrifuge.

10 . The method of claim 9 , wherein in step (i), the crude solution for nanoparticle synthesis comprises the nanoparticles and a high boiling point solvent.

11 . The method of claim 9 , wherein each of the first mix solvent and the second mix solvent is a mixture of a non-solvent in which the nanoparticles are not dispersible, or a mixture of a non-solvent and an organic solvent.

12 . The method of claim 9 , wherein each of the first mix solvent and the second mix solvent is a mixture of acetone and ethanol.

13 . The method of claim 12 , wherein in the first reaction mixture in step (i), a mixing ratio of the crude solution for nanoparticle synthesis, acetone and ethanol is in a range of 1 to 4 : 1 to 2 : 4 to 12 by volume.

14 . The method of claim 12 , wherein in the second reaction mixture in step (iii), a mixing ratio of the first filtrate, acetone and ethanol is in a range of 1 to 3 : 1 to 2 : 4 to 12 by volume.

15 . The method of claim 9 , wherein the first mix solvent in step (i) or the second mix solvent in step (iii) further comprises 1 to 10 percent by weight (wt%) of an inorganic material with respect to the total weight of ethanol in the corresponding mix solvent.

16 . The method of claim 15 , wherein the inorganic material is a metal halide comprising at least one of Zn, Mg, and Al, or an aqueous solution comprising the metal halide.

17 . The method of claim 9 , wherein the continuous centrifuges in steps (ii) and (iv) are operated under conditions of:
a reaction mixture input amount per minute in a range of 4 to 6 L/min; a G value in a range of 13,000 to 16,000 g; and a rotational speed in a range of 13,000 to 16,000 rpm.

18 . The method of claim 9 , wherein each of the first continuous centrifuge and the second continuous centrifuge centrifuges under an inert atmosphere by supplying a nitrogen gas into each of the first continuous centrifuge and the second continuous centrifuge.

19 . The method of claim 9 , further comprising, after step (iv):
(v) preparing a third reaction mixture by mixing the second filtrate and a third solvent; and (vi) tertiarily separating the nanoparticles and a solvent by distilling the third reaction mixture.

20 . The method of claim 19 , further comprising, after step (vi):
(vii) recovering the separated solvent and reusing the recovered solvent as a solvent of at least one of steps (i), (iii) and (v).

Assignees

• Hansol Chemical Co Ltd

Inventors

• Ha Sungmin
• Shin Jaewoo
• Lee Kwangdeok
• Nam Chunrae

Classifications

• B04B15/00

  Other accessories for centrifuges · CPC title

• B04B5/10 Primary

  Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges (B04B5/12 takes precedence; magnetic or electrostatic separators B03C; {amassing particles by electric fields, e.g. by agglomeration B03C3/0175}) · CPC title

• B01D3/00

  Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping ({evaporation in general, e.g. of liquids for gas phase reactions B01B1/005;} gas chromatography B01D15/08; destructive distillation C10B; preparation of alcoholic beverages by distillation C12H6/02) · CPC title

• B01D3/32

  Other features of fractionating columns {; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30} · CPC title

• B04B1/12

  with continuous discharge · CPC title