Product comprising lithiated bayerite and method of making such a product

Patent metadata

Field	Value
Publication number	US-2025187985-A1
Application number	US-202318844836-A
Country	US
Kind code	A1
Filing date	Mar 6, 2023
Priority date	Mar 7, 2022
Publication date	Jun 12, 2025
Grant date	—

Abstract

A product includes water, and crystallites, at least a portion, preferably substantially all of the crystallites, including lithiated bayerite, the mean size of lithiated bayerite crystallites is 10 nm or more and 25 nm or less, and the product having a combined aluminum hydroxide and boehmite content of 10% or less, the product including at least the elements Li, Cl, Al, O and H, the elements Li, Cl and Al being present in the dry product in the following contents, determined by inductively coupled plasma spectrometry, in weight percentages: −2%<Li<5%, 10%<Cl<26%, 15%<Al<30%.

First claim

1 . A product comprising:
water, and crystallites, at least part of said crystallites consisting of lithiated bayerite, a mean size of lithiated bayerite crystallites is 10 nm or more and 25 nm or less, and said product having a combined aluminum hydroxide and boehmite content of 10% or less, said product comprising at least the elements Li, Cl, Al, O and H, the elements Li, Cl and Al being present in said dry product in the following contents, determined by inductively coupled plasma spectrometry and in weight percentages:

2
⁢
%

<
Li
<

5
⁢
%

,

10
⁢
%

<
Cl
<

26
⁢
%

,

15
⁢
%

<
Al
<

30
⁢

%
.

2 . The product according to claim 1 , having the following chemical analysis, determined on the dry product by inductively coupled plasma spectroscopy, in % by weight

2
⁢
%

<
Li
<

5
⁢
%

,

10
⁢
%

<
Cl
<

26
⁢
%

,

15
⁢
%

<
Al
<

30
⁢
%

,

elements other than Li, Cl, Al, O and H: <3%,
O and H: complement to 100%.

3 . The product according to claim 1 , wherein:
the water content is greater than 1% and less than 95%, and/or an average size of lithiated bayerite crystallites of less than 23 nm.

4 . The product according to claim 1 , wherein:
a cumulative content of aluminum hydroxide and boehmite is less than or equal to 8%, and/or the crystallized phases comprise lithiated bayerite, boehmite and/or an aluminum hydroxide chosen from gibbsite, bayerite, doyleite, nordstrandite and mixtures thereof.

5 . The product according to claim 3 wherein:
the water content is greater than 5%, and/or
the water content is less than 80%, and/or
the crystallized phases comprise lithiated bayerite and an aluminum hydroxide selected from gibbsite, bayerite, doyleite, nordstrandite and mixtures thereof.

6 . The product according to the preceding claim 5 , wherein:
the water content is greater than 10%, and/or the water content is less than 70%, and/or the only crystallized phase is lithiated bayerite.

7 . The product according to claim 1 , consisting of at least 80% by weight of water and crystallites of lithiated bayerite, aluminum hydroxide and/or boehmite, and LiCl, and a binder.

8 . The product according to claim 7 , consisting of at least 80%, by weight, of water, and crystallites of lithiated bayerite, and aluminum hydroxide, and LiCl, and a binder.

9 . The product according to claim 8 , consisting of at least 80% by weight in total of water, lithiated bayerite crystallites, LiCl and a binder.

10 . The product according to claim 7 , wherein the binder is a polysaccharide.

11 . The method of making a product according to claim 1 comprising:
a) providing an aqueous suspension of an aluminum source, selected from boehmite or aluminum hydroxide and mixtures thereof, grinding said aqueous suspension to a median size of 3 μm or less if the median size of the aluminum source is greater than 3 μm,
said suspension being maintained during this-step a) at a temperature of less than 50° C.;
b) increasing the pH by adding a base, such that a molar ratio between the OH supplied by said base and the Al present in the mixture is greater than 0.20, said mixture being kept stirring after introduction of said base, at a temperature below 50° C.;
c) of adding a chlorine salt, such that a molar ratio of Cl supplied by said chlorine salt to Al present in the mixture is greater than 0.25, said mixture being kept stirring after introduction of said chlorine salt at a temperature below 50° C.; the base in step b), the chlorine salt in step c) and their respective amounts being chosen so as to provide a quantity of lithium in the mixture such that the Li/Al molar ratio is greater than or equal to 1;
d) raising a temperature of the mixture to a temperature greater than or equal to 50° C. and less than or equal to 60° C., a time t 1 being the time during which said mixture is at a temperature greater than or equal to 50° C.;
e) maintaining the mixture at a temperature greater than or equal to 50° C. and less than or equal to 60° C. for a time t 2 ;
f) optionally, adding an acid to the mixture, with stirring, so as to reduce the pH of the mixture to 8 or less, the chlorine salt in step c), said acid and their respective quantities being chosen so that the Cl/Al molar ratio in the mixture is greater than or equal to 1, the mixture being maintained at a temperature less than or equal to 60° C., a time t 3 being the time during which the mixture is at a temperature greater than or equal to 50° C., the molar ratio between the Cl supplied by the chlorine salt and the Al present in the mixture being greater than or equal to 0.5 if the method does not include said step f);
g) optionally, filtration of the mixture so as to obtain a paste, the mixture being maintained at a temperature of less than or equal to 60° C., a time t 4 being the time during which the mixture is at a temperature of greater than or equal to 50° C.;
a cumulative time t 1 +t 2 +t 3 +t 4 =t 5 being greater than or equal to 45 minutes and less than 15 hours.

12 . The method of making a product according to claim 11 , wherein in step a) a grinding of the aqueous suspension of an aluminum source selected from a boehmite or aluminum hydroxide and mixtures thereof is carried out, so as to obtain a median size of ≤1 μm.

13 . The method according to claim 11 , wherein the time t 3 is such that the times t 1 , t 2 , t 3 a

Assignees

• Saint Gobain Ct Recherches

Inventors

• Nguyen Van Nuoi Patrick
• Giardella Lucas

Classifications

• H01M4/485

  of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy (H01M4/505, H01M4/525 take precedence) · CPC title

• C04B2235/781

  Nanograined materials, i.e. having grain sizes below 100 nm · CPC title

• C04B2235/6567

  Treatment time · CPC title

• C04B2235/444

  Halide containing anions, e.g. bromide, iodate, chlorite · CPC title

• C04B2235/3222

  Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4) · CPC title