IP Library Granted Patent US 9,023,204
Granted Patent B2
US 9,023,204 · App. 13/510,676 · Granted May 5, 2015

Purifier for removing hydrogen fluoride from electrolytic solution

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Quick Facts
Patent No.
US 9,023,204
App. No.
13/510,676
Granted
May 5, 2015
Kind
B2
Abstract

The present invention is a purification system for removing hydrogen fluoride and water from an electrolytic solution for lithium-ion secondary batteries in which [1] a purifier for removing hydrogen fluoride containing a hydrogen fluoride adsorbent selected from among carbonate hydrotalcites and calcined hydrotalcites and [2] a purifier for removing water containing an adsorbent for trapping water are connected in this order from upstream to downstream.

Claims (18)

1. A purification system for removing hydrogen fluoride and water from a non-aqueous electrolytic solution for a lithium ion secondary battery, comprising:

a purifier for removing hydrogen fluoride containing an adsorbent selected from carbonate hydrotalcites or calcined hydrotalcites; and

a purifier for removing water connected downstream from the purifier for removing hydrogen fluoride, the purifier for removing water containing a water adsorbent,

each purifier comprising a housing, an electrolytic solution inlet member, an electrolytic solution outlet member and mesh for preventing outflow of the adsorbent at the inlet and outlet of the housing,

wherein the non-aqueous electrolytic solution flows into the purifier for removing hydrogen fluoride via the electrolytic solution inlet member of the purifier for removing hydrogen fluoride, whereby the non-aqueous electrolytic solution is supplied to the adsorbent selected from carbonate hydrotalcites or calcined hydrotalcites; out of the purifier for removing hydrogen fluoride via the electrolytic solution outlet member of the purifier for removing hydrogen fluoride; into the purifier for removing water via the electrolytic solution inlet member of the purifier for removing water, whereby the non-aqueous electrolytic solution is supplied to the water adsorbent; and out of the purifier for removing water via the electrolytic solution outlet member of the purifier for removing water.

2. The purification system according to claim 1 , wherein the purifier for removing hydrogen fluoride reduces a concentration of hydrogen fluoride contained in a non-aqueous electrolytic solution for a lithium ion secondary battery to less than 10 ppmw.

3. The purification system according to claim 1 , wherein the purifier for removing hydrogen fluoride attains a removal rate of the hydrogen fluoride of 90% or more.

4. The purification system according to claim 1 , wherein the purifier for removing water reduces a concentration of water contained in a non-aqueous electrolytic solution for a lithium ion secondary battery to 10 ppmw or less.

5. The purification system according to claim 1 , wherein the adsorbent contained in the purifier for removing hydrogen fluoride is a carbonate hydrotalcite which has a formula, [M 2+ 1−x M 3+ x (OH) 2 ] x+ [(CO 3 ) X/2 .mH 2 O] x− (m≧0) where 0<x≦0.33, M 2+ are divalent Mg, Mn, Fe, Co, Ni, Cu and Zn metal ions, and M 3+ are trivalent Al, Fe, Cr, Co and In metal ions.

6. The purification system according to claim 1 , wherein the adsorbent contained in the purifier for removing hydrogen fluoride is a calcined hydrotalcite which has a formula M 2+ 1−x M 3+ x O 1+x/2 , where 0<x≦0.33, M 2+ are divalent Mg, Mn, Fe, Co, Ni, Cu and Zn metal ions, and M 3+ are trivalent Al, Fe, Cr, Co and In metal ions.

7. The purification system according to claim 1 , wherein the water adsorbent is synthetic zeolite or activated alumina.

8. A purification system for removing hydrogen fluoride and water from a non-aqueous electrolytic solution for a lithium ion secondary battery, comprising:

a preliminary purifier for removing water containing an adsorbent for trapping water;

a purifier for removing hydrogen fluoride connected downstream from the preliminary purifier, the purifier for removing hydrogen fluoride containing an adsorbent selected from carbonate hydrotalcites or calcined hydrotalcites; and

a purifier for removing water connected downstream from the purifier for removing hydrogen fluoride, the purifier for removing water containing a water adsorbent,

each purifier comprising a housing, an electrolytic solution inlet member, an electrolytic solution outlet member and mesh for preventing outflow of the adsorbent at the inlet and outlet of the housing,

wherein the non-aqueous electrolytic solution flows into the preliminary purifier via the electrolytic solution inlet member of the preliminary purifier, whereby the non-aqueous electrolytic solution is supplied to the adsorbent for trapping water; out of the preliminary purifier via the electrolytic solution outlet member of the preliminary purifier; into the purifier for removing hydrogen fluoride via the electrolytic solution inlet member of the purifier for removing hydrogen fluoride, whereby the non-aqueous electrolytic solution is supplied to the adsorbent selected from carbonate hydrotalcites or calcined hydrotalcites; out of the purifier for removing hydrogen fluoride via the electrolytic solution outlet member of the purifier for removing hydrogen fluoride; into the purifier for removing water via the electrolytic solution inlet member of the purifier for removing water, whereby the non-aqueous electrolytic solution is supplied to the water adsorbent; and out of the purifier for removing water via the electrolytic solution outlet member of the purifier for removing water.

9. The purification system according to claim 8 , wherein the preliminary purifier reduces a concentration of water contained in a non-aqeuous electrolytic solution for a lithium ion secondary battery to 100 ppmw or less.

Assignments (8)
SECURITY INTEREST Recorded Jul 8, 2022
From: ENTEGRIS, INC.; ENTEGRIS GP, INC.; POCO GRAPHITE, INC.; CMC MATERIALS, INC.; INTERNATIONAL TEST SOLUTIONS, LLC; QED TECHNOLOGIES INTERNATIONAL, INC.
To: TRUIST BANK, AS NOTES COLLATERAL AGENT
Reel/Frame 060613/0072 →
ASSIGNMENT OF PATENT SECURITY INTEREST RECORDED AT REEL/FRAME 048811/0679 Recorded Nov 5, 2019
From: GOLDMAN SACHS BANK USA
To: MORGAN STANLEY SENIOR FUNDING, INC.
Reel/Frame 050965/0035 →
SECURITY INTEREST Recorded Nov 13, 2018
From: ENTEGRIS, INC.; SAES PURE GAS, INC.
To: GOLDMAN SACHS BANK USA
Reel/Frame 048811/0679 →
RELEASE OF SECURITY INTEREST Recorded Nov 8, 2018
From: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
To: ENTEGRIS, INC.; POCO GRAPHITE, INC.; ATMI, INC.; ATMI PACKAGING, INC.; ADVANCED TECHNOLOGY MATERIALS, INC.
Reel/Frame 047477/0151 →
RELEASE OF SECURITY INTEREST Recorded Nov 8, 2018
From: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
To: ENTEGRIS, INC.; POCO GRAPHITE, INC.; ATMI, INC.; ATMI PACKAGING, INC.; ADVANCED TECHNOLOGY MATERIALS, INC.
Reel/Frame 047477/0032 →
SECURITY INTEREST Recorded May 2, 2014
From: ENTEGRIS, INC.; POCO GRAPHITE, INC.; ATMI, INC.; ADVANCED TECHNOLOGY MATERIALS, INC.; ATMI PACKAGING, INC.
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 032812/0192 →
SECURITY INTEREST Recorded May 1, 2014
From: ENTEGRIS, INC.; POCO GRAPHITE, INC.; ATMI, INC.; ADVANCED TECHNOLOGY MATERIALS, INC.; ATMI PACKAGING, INC.
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 032815/0852 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 29, 2012
From: SHIMADA, YUTAKA; OHYASHIKI, YASUSHI
To: ENTEGRIS, INC.
Reel/Frame 028471/0801 →