Process for delamination of layered silicates

Patent metadata

Field	Value
Publication number	US-11905418-B2
Application number	US-201916966924-A
Country	US
Kind code	B2
Filing date	Feb 4, 2019
Priority date	Feb 8, 2018
Publication date	Feb 20, 2024
Grant date	Feb 20, 2024

Abstract

The invention relates to a process for delamination of a layered silicate in an aqueous medium, wherein in a first step a layered silicate is treated with a delamination agent, and in a second step the thus treated layered silicate is contacted with an aqueous medium, whereby the delamination agent is a compound having exactly one positively charged atom, the positively charged atom being selected from the group consisting of nitrogen and phosphorous; contains nf functional groups selected from the group consisting of hydroxyl groups, ether groups, sulfonic acid ester groups and carboxylic acid ester groups, nf being a number from 3 to 10; comprises a total number of carbon atoms nc being from 4 to 12; has a ratio nc/(1+nf) from 1 to 2, wherein nc is the total number of carbon atoms of the delamination agent and nf is the total number of functional groups in the delamination agent as defined under ii.; contains nt atoms selected from the group consisting of carbon, nitrogen, phosphorous, oxygen and sulfur, nt being ≥9; and wherein the delamination agent is used to treat the layered silicate in an amount of at least equal to the cation exchange capacity of the layered silicate. The invention further relates to the thus produced delaminated layered silicates, their use in the production of composite and coating material and as a barrier material. Moreover, the invention relates to compositions containing the thus produced delaminated layered silicates.

First claim

The invention claimed is:

1. A process for delamination of a layered silicate in an aqueous medium, the process comprising:
treating a layered silicate with an amount of a delamination agent, the amount of the delamination agent being at least equal to the cation exchange capacity of the layered silicate; and
contacting the treated layered silicate with an aqueous medium,
wherein the delamination agent
i. is a compound having exactly one positively charged atom, the positively charged atom being nitrogen or phosphorous;
ii. contains n f functional groups including any one or more of a hydroxyl group, an ether group, a sulfonic acid ester group, or a carboxylic acid ester group, n f being a number from 3 to 10;
iii. comprises a total number of carbon atoms n c being from 4 to 12;
iv. has a ratio n c /(1+n f ) from 1 to 2, and
v. including any one or more of carbon, nitrogen, phosphorous, oxygen, or sulfur, n t being greater than or equal to 9

wherein the layered silicate is represented by general formula (I)
[ M Lc/valency ] inter [M I m M II o ] octa [M III 4 ] tetra X 10 Y 2   (I)

wherein,
M represents metal cations of oxidation state 1 to 3;
M I represents metal cations of oxidation state 2 or 3;
M II represents metal cations of oxidation state 1 or 2;
M III represents atoms of oxidation state 4;
X represents di-anions;
Y represents mono-anions;
m is less than or equal to 2.0 for metal atoms M I of oxidation state 3;
m is less than or equal to 3.0 for metal atoms M I of oxidation state 2; and
o is less than or equal to 1.0.

2. The process according to claim 1 , wherein the layered silicate is a synthetic or naturally occurring 2:1 clay mineral.

3. The process according to claim 1 , wherein the layered silicate is a smectite or vermiculite.

4. The process according to claim 1 , wherein
M independently represent Li + , Na + ,or Mg 2+ ;
M I independently represent Mg 2+ , Al 3+ , Fe 2+ ,or Fe 3+ ;
M II independently represent Li + or Mg 2+ ;
M III is a tetravalent silicon cation;
X is O 2− ;
Y independently represent OH − , or F − .

5. The process according to claim 1 , wherein
the delamination agent
ii. contains 3 to 8 of the of functional groups; and/or
iii. comprises 4 to 10 of the total number of carbon atoms n c ; and/or
iv. has the ratio n c /(1+n f ) from 1 to 1.8; and/or
v. contains 10 or more of the n t atoms.

6. The process according to claim 1 , wherein
the delamination agent
i. is a compound having exactly one positively charged nitrogen atom; and/or
ii. contains 3 to 6 of the of functional groups, the of functional groups including any one or more of a hydroxyl group or an ether group; and/or
iii. comprises 5 to 9 of the total number of carbon atoms n c ; and/or
iv. has the ratio n c /(1+n f ) from 1 to 1.5; and/or
v. contains 11 or more of the n t atoms.

7. The process according to claim 1 , wherein treating the layered silicate with the amount of the delamination agent includes treating the layered silicate with an aqueous solution of the delamination agent, wherein the concentration of the delamination agent in the aqueous solution is high enough to prevent delamination of the layered silicate while treating the layered silicate with the amount of the delamination agent.

8. The process according to claim 7 , wherein the concentration of the delamination agent in the aqueous solution is from 0.2 to 2 mol/L.

9. The process according to claim 7 , wherein the concentration of the layered silicate in the aqueous solution containing the delamination agent is in the range from 1 to 50 g/L.

10. The process according to claim 1 , wherein when contacting the treated layered silicate with the aqueous medium, the aqueous medium has an ionic strength low enough to cause delamination of the treated layered silicate.

11. The process according to claim 1 , wherein the aqueous medium includes water.

12. The process according to claim 4 , wherein the layer charge L c is greater than or equal to 0.28 and less than or equal to 0.95.

13. The process according to claim 7 , wherein the concentration of the delamination agent in the aqueous solution is in the range of 0.5 to 1.5 mol/L.

14. The process according to claim 7 , wherein the concentration of the layered silicate in the aqueous solution containing the delamination agent is in the range from 5 to 40 g/L.

15. The process according to claim 7 , wherein the concentration of the layered silicate in the aqueous solution containing the delamination agent is in the range from 10 to 30 g/L.

16. The process according to claim 11 , wherein the water is purified water.

Assignees

• Byk Chemie Gmbh

Inventors

• Daab Matthias
• Breu Josef
• Edenharter Andreas

Classifications

• C09C1/3063 Primary

  Treatment with low-molecular organic compounds · CPC title

• C01B33/405

  not containing aluminium · CPC title

• C01B33/425

  not containing aluminium · CPC title

• C09C1/405 Primary

  containing combined silica, e.g. mica · CPC title

• C01B33/18

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title