IP Library Granted Patent US 11,084,951
Granted Patent B2
US 11,084,951 · App. 16/605,700 · Granted Aug 10, 2021

Process for preparing an aqueous dispersion of pigment containing particles

Inventors: Marion Winkelmann (Ludwigshafen, DE); Yannick Fuchs (Ludwigshafen, DE); Murat Cetinkaya (Rijswijk, NL); Aaron Wagner (Ludwigshafen, DE); Paul Brown (Basel, CH); Steffen Onclin (Ludwigshafen, DE); Christof Kujat (Ludwigshafen, DE)
Assignee: BASF Colors & Effects GmbH
C09D17/003B01J13/18C09B67/0002C09B67/0013C09D7/45C09D7/65C09D17/001C09D161/24C09D161/32
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Quick Facts
Patent No.
US 11,084,951
App. No.
16/605,700
Granted
Aug 10, 2021
Kind
B2
Abstract

A process for preparing an aqueous dispersion of pigment particles is described. The pigment particle contains a pigment and an aminoplast resin which surrounds or embeds the pigment. The process includes (i) a step of subjecting an aqueous suspension of a pigment in the form of coarse particles to milling so that the coarse particles are comminuted in the presence of a polymeric dispersant to a particle diameter d(v 0.9) of below 1500 nm, as determined by laser diffraction; and (ii) a step of polycondensation of an aminoplast pre-condensate in the aqueous suspension of the comminuted particles of the pigment obtained in step (i) or during the milling of step (i). The polycondensation is performed in the presence of an acid catalyst at pH of below 5.5. The aqueous dispersion obtained by the process and the use of the aqueous dispersion for tinting waterborne liquid coating composition are also described.

Claims (30)

1. A process for preparing an aqueous dispersion of pigment-polymer particles containing an organic pigment and an aminoplast resin which surrounds or embeds the organic pigment, the process comprising:

i) subjecting an aqueous suspension of an organic pigment in the form of coarse particles to milling in order to comminute the coarse particles in the presence of a polymer dispersant to a particle diameter d(v 0.9) of below 1500 nm, as determined by laser scattering;

ii) performing a polycondensation of an aminoplast pre-condensate in the aqueous suspension obtained in i) or during the milling of i), thereby obtaining the aqueous dispersion of pigment-polymer particles;

wherein the polycondensation is performed in the presence of an acid catalyst at pH of below 5.5.

2. The process of claim 1 , wherein the aminoplast pre-condensate is selected from the group consisting of a melamine formaldehyde pre-condensate, a urea formaldehyde pre-condensate, and a mixture thereof.

3. The process of claim 2 , wherein the aminoplast pre-condensate comprises an etherified melamine formaldehyde pre-condensate.

4. The process of claim 1 , wherein the dispersant is a nonionic polymer containing a plurality of poly(oxy-C 2 -C 4 -alkylene) groups.

5. The process of claim 4 , wherein the dispersant is a comb polymer containing both repeating units bearing a poly(oxy-C 2 -C 4 -alkylene) group and repeating units derived from vinyl pyridine units.

6. The process of claim 1 , where an amount of the dispersant is from 0.1 to 4.0 parts by weight, per 1 part of the pigment.

7. The process of claim 1 , wherein the milling of i) is performed in the presence of at least a portion of the aminoplast pre-condensate subjected to the polycondensation of ii).

8. The process of claim 1 , wherein no aminoplast pre-condensate subjected to the polycondensation of ii) is present in the aqueous suspension during the milling of i).

9. The process of claim 1 , which satisfies at least one of the following a.1 to a.6:

a.1 the milling in i) is performed in a stirred media mill;

a.2 a concentration of the pigment in the aqueous suspension of i) is from 5 to 60% by weight;

a.3 an amount of the aminoplast pre-condensate is from 1 to 60% by weight, based on the organic pigment to be encapsulated;

a.4 the polycondensation of the aminoplast pre-condensate in the aqueous suspension obtained in i) is performed at a pH ranging from 1 to 4;

a.5 the acid catalyst is selected from the group consisting of formic acid, sulfuric acid, methane sulfonic acid, and hydrochloric acid; and

a.6 the aqueous dispersion of pigment-polymer particles obtained in ii) is neutralized by adding a base.

10. The process of claim 1 , wherein the polycondensation is performed at a temperature of at most 60° C.

11. The process of claim 1 , wherein the aqueous suspension is milled during the polycondensation of ii).

12. The process of claim 1 , wherein the organic pigment is selected from the group consisting of a monoazo pigment, a disazo pigment, a disazo condensation pigment, an anthanthrone pigment, an anthraquinone pigment, an anthrapyrimidine pigment, a quinacridone pigment, a quinophthalone pigment, a diketopyrrolopyrrole pigment, a dithioketopyrrolopyrrol pigment, a dioxazine pigment, a flavanthrone pigment, an indanthrone pigment, an isoindoline pigment, an isoindolinone pigment, an isoviolanthrone pigment, a metal complex pigment of an azo metal complex pigment and an azomethine metal complex pigment, a perinone pigment, a perylene pigment, a phthalocyanine pigment, a pyranthrone pigment, a pyrazoloquinazolone pigment, an indigo pigment, a thioindigo pigment, a triarylcarbonium pigment, and a combination thereof.

13. An aqueous dispersion of pigment-polymer particles, obtained by the process of claim 1 , wherein the pigment-polymer particles have a particle diameter d(v 0.9) of below 2.0 μm, as determined by laser scattering.

14. The aqueous dispersion of claim 13 , wherein the pigment-polymer particles have a volume average particle diameter d(v 0.5) of from 10 to 1000 nm, as determined by laser scattering.

15. The aqueous dispersion of claim 13 , which satisfies at least one of the following x.1 to x.4:

x.1: the dispersant is a nonionic polymer containing a plurality of poly(oxy-C 2 -C 4 -alkylene) groups;

x.2: an amount of the dispersant is from 0.1 to 4 parts by weight per 1 part of the pigment-polymer particles;

x.3: an amount of the dispersant is from 0.2 to 2.0 parts per 1 part of the pigment-polymer particles; and

x.4: an amount of the dispersant is from 0.25 to 1.3 parts per 1 part of the pigment-polymer particles.

16. A tinting waterborne coating composition, comprising:

the aqueous dispersion of claim 13 .

Assignments (5)
CHANGE OF NAME Recorded Aug 12, 2023
From: BASF COLORS & EFFECTS GMBH
To: SUN CHEMICAL COLORS & EFFECTS GMBH
Reel/Frame 064573/0082 →
NUNC PRO TUNC ASSIGNMENT Recorded Feb 8, 2023
From: SUN CHEMICAL COLORS & EFFECTS GMBH
To: SUN CHEMICAL GROUP COÖPERATIEF U.A.
Reel/Frame 062630/0554 →
NUNC PRO TUNC ASSIGNMENT Recorded Feb 8, 2023
From: SUN CHEMICAL GROUP COÖPERATIEF U.A.
To: SUN CHEMICAL B.V.
Reel/Frame 062630/0810 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 17, 2020
From: WINKELMANN, MARION; FUCHS, YANNICK; CETINKAYA, MURAT; WAGNER, AARON; ONCLIN, STEFFEN; KUJAT, CHRISTOF
To: BASF SE
Reel/Frame 056708/0123 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 17, 2020
From: BROWN, PAUL
To: BASF SCHWEIZ AG
Reel/Frame 053242/0590 →
Priority Claims (1)
EP 17167560 · Apr 21, 2017 · regional
Continuity (1)
Related Publication 20200123405A1 · Apr 23, 2020