Process of preparation of an aqueous gel ink with fixed color comprising gold nanoparticles

Patent metadata

Field	Value
Publication number	US-12497525-B2
Application number	US-202017630814-A
Country	US
Kind code	B2
Filing date	Aug 28, 2020
Priority date	Aug 29, 2019
Publication date	Dec 16, 2025
Grant date	Dec 16, 2025

Abstract

The present invention concerns a process for preparing in situ an aqueous gel ink with fixed color comprising the following steps: (i) preparing a gel-based matrix of aqueous ink comprising reducing agent chosen in the group consisting of citric acid and/or derivatives of citric acid, (ii) adding a solution of gold salts, (iii) adding iron powder, (iv) adding polyvinylpyrrolidone to obtain an aqueous gel ink with fixed color, wherein the steps (ii) and (iii) can be interchanged. The present invention also relates to an aqueous gel ink with fixed color obtained according to the process of the invention, comprising citric acid and derivatives, gold nanoparticles, and iron powder. The invention finally concerns a writing instrument comprising an aqueous gel ink with fixed color according to the invention.

First claim

The invention claimed is:

1 . A process for preparing in situ an aqueous gel ink with fixed color comprising the following steps:
(i) preparing a gel-based matrix of aqueous ink comprising a reducing agent selected from the group consisting of citric acid, derivatives of citric acid including esters, amides, and thioesters of citric acid, salts of citric acid, salts of said derivatives of citric acid, solvates of citric acid including hydrates, solvates of said derivatives of citric acid including hydrates, and mixtures thereof, (ii) adding a solution of gold (III) salts, (iii) adding iron powder, and (iv) adding polyvinylpyrrolidone to obtain an aqueous gel ink with fixed color, wherein the steps (ii) and (iii) can be interchanged.

2 . The process according to claim 1 , wherein said reducing agent is selected from the group consisting of citric acid, said esters of citric acid, said salts of citric acid, said solvates of citric acid, solvates of said esters of citric acid, and mixtures thereof.

3 . The process according to claim 1 , wherein the gel-based matrix of aqueous ink includes citric acid and said derivatives of citric acid, and wherein a concentration of citric acid and said derivatives of citric acid in the gel-based matrix of aqueous ink of step (i) ranges from 0.10 to 0.50 mol·L −1 .

4 . The process according to claim 1 , wherein a concentration of said gold (III) salts in the gel-based matrix of aqueous ink of step (ii) ranges from 0.001 to 0.1 mol·L −1 .

5 . The process according to claim 1 , wherein a concentration of said iron powder in the gel-based matrix of aqueous ink of step (iii) ranges from 0.01 to 0.05 mol·L −1 .

6 . The process according to claim 1 , wherein a concentration of said polyvinylpyrrolidone in the aqueous gel ink of step (iv) ranges from 0.005 to 0.1%.

7 . An aqueous gel ink with fixed color obtained according to the process of claim 1 , comprising citric acid and said derivatives of citric acid, said gold (III) salts, wherein said gold (III) salts are to produce gold nanoparticles, and said iron powder.

8 . The aqueous gel ink according to claim 7 , wherein a total amount of citric acid and of said derivatives of citric acid in said aqueous gel ink ranges from 5 to 15% by weight relative to a total weight of the aqueous gel ink.

9 . The aqueous gel ink according to claim 7 , wherein the gold nanoparticles have an average particle size ranging from 10 to 200 nm.

10 . The aqueous gel ink according to claim 7 , wherein the gold nanoparticles have a shape of urchins.

11 . The aqueous gel ink according to claim 7 , wherein an amount of said gold nanoparticles in the aqueous gel ink ranges from 0.05 to 0.5% by weight relative to total weight of the aqueous gel ink.

12 . The aqueous gel ink according to claim 7 , wherein an amount of said iron powder in the aqueous gel ink ranges from 0.01 to 0.1% by weight relative to a total weight of the aqueous gel ink.

13 . The aqueous gel ink according to claim 7 , further comprising water, wherein an amount of said water in the aqueous gel ink ranges from 50 to 95% by weight relative to a total weight of the aqueous gel ink.

14 . The aqueous gel ink according to claim 7 , further comprising:
a solvent; and/or a corrosion inhibitor, in an amount ranging from 0.05 to 1% by weight relative to a total weight of the aqueous gel ink; and/or an antifoam agent, in an amount ranging from 0.05 to 1% by weight relative to the total weight of the aqueous gel ink; and/or a rheology modifier, in an amount ranging from 0.1 to 2% by weight relative to the total weight of the aqueous gel ink; and/or an antimicrobial agent, in an amount ranging from 0.01 to 0.5% by weight relative to the total weight of the aqueous gel ink.

15 . A writing instrument comprising:
an axial barrel containing the aqueous gel ink with fixed color according to claim 7 , and a pen body which delivers the aqueous gel ink stored in the axial barrel, wherein the writing instrument is selected from the group consisting of gel pens, felt pens, correction fluid, and markers.

Assignees

• SOCIéTé BIC
• Univ Haute Alsace
• Centre Nat Rech Scient

Inventors

• Albenge Olivier
• Metillon Romain
• Mougin Karine
• Ghellal Feriel
• Spangenberg Arnaud

Classifications

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C09D11/17 Primary

  characterised by colouring agents · CPC title

• C09D11/16 Primary

  Writing inks · CPC title