Process for producing encapsulated metal colloids as inorganic coloured pigments

Patent metadata

Field	Value
Publication number	US-9399206-B2
Application number	US-201013514484-A
Country	US
Kind code	B2
Filing date	Dec 15, 2010
Priority date	Dec 18, 2009
Publication date	Jul 26, 2016
Grant date	Jul 26, 2016

Abstract

A process for producing encapsulated metal colloids useful as inorganic colored pigments, including, reacting one or more glass-forming components according to the sol-gel process to obtain a sol dispersing a metal salt in the resulting sol in the presence of an additional reducing agent to form metal colloids, converting the resulting dispersion into xerogel-encapsulated metal colloids by spray drying, heating the resulting xerogel-encapsulated metal colloids to density them. The present invention relates, furthermore, to inorganic colored pigments, in particular producible by the process of the invention, including metal colloids produced from metal salts and encapsulated in an encapsulation, the encapsulation being produced from glass-forming components according to the sol-gel process and being densified to a xerogel or glass, the proportion of metal colloid in the capsules being at least 80%.

First claim

The invention claimed is:

1. A process for producing encapsulated metal colloids useful as inorganic colored pigments comprising:
a) reacting one or more glass-forming components according to a sol-gel process to obtain a sol;
b) dispersing a metal salt in the resulting sol in the presence of a reducing agent to form metal colloids;
c) converting the resulting dispersion into xerogel-encapsulated metal colloids by spray drying; and
d) heating the resulting xerogel-encapsulated metal colloids to densify them,
wherein the reducing agent used in step b) is at least one from the group consisting of glucose, ascorbic acid, formaldehyde, glycerol, hexamethylenetetraamine, methoxy polyethylene glycol, hydroquinone and urea, wherein the sol in step a) is obtained by hydrolysis and polycondensation of
(A) at least one hydrolysable silane of the general formula (I)
SiX 4   (I)

where the X radicals are the same or different and represent hydrolysable groups or hydroxyl groups, or an oligomer derived therefrom, and
(B) at least one organosilane of the general formula (II)
R 1 a R 2 b SiX (4−a−b)   (II)

where R 1 is a non-hydrolysable group, R 2 is a radical bearing a functional group, X is as defined above and a and b are each 0, 1, 2 or 3 provided the sum (a+b) is 1, 2 or 3, or an oligomer derived therefrom in an amount of substance ratio for (A):(B) of 5-50:50-95,
and wherein tetraalkoxysilanes are used as hydrolysable silanes (A),
and wherein epoxysilanes or aminosilanes are used as organosilanes (B), and wherein the metal salts are selected from the group consisting of salts of silver, of gold, of copper, of iron, of lead, of palladium and of platinum.

2. The process according to claim 1 , wherein the dispersion obtained in step b) is subjected to a UV treatment.

3. The process according to claim 1 , wherein the hydrolysis and polycondensation is carried out in the presence of a complexing agent.

4. The process according to claim 1 , wherein the refractive index of the sol obtainable in step a) is altered using B 2 O 3 .

5. The process according to claim 1 , wherein the metal salts are selected from the group consisting of metal nitrates, metal halides, metal carbides, metal nitrides, metal arsenides, metal phosphides and metal chalcogenides.

6. The process according to claim 1 , wherein the xerogel-encapsulated metal colloids obtained are heated to 775° C.

7. The process according to claim 1 , wherein the uncoated metal colloid cores have a diameter of 5-25 nm.

8. The process according to claim 1 , wherein the encapsulated metal colloids have a particle size between 50 nm and 2 μm.

Assignees

• Fink-Straube Claudia
• Fries Kira
• Mennig Martin
• Anschutz Dieter
• Schumacher Sarah
• De Oliveira Peter William
• Ishii Masahiko
• Murata Wataru
• Vandenberghe Veronique
• Toyota Motor Corp

Inventors

• Fink-Straube Claudia
• Fries Kira
• Mennig Martin
• Anschutz Dieter
• Schumacher Sarah
• De Oliveira Peter William
• Ishii Masahiko
• Murata Wataru
• Vandenberghe Veronique

Classifications

• B01J13/0091

  Preparation of aerogels, e.g. xerogels · CPC title

• B01J13/0043 Primary

  containing elemental metal (for medical or diagnostical purposes A61K, G01N) · CPC title