Method for production of polymer-encapsulated pigments
View Patent ↗The invention relates to a method for production of an aqueous dispersion of polymer-encapsulated pigments characterized in that (a) an aqueous pigment dispersion, containing at least one organic pigment (P) at least one surfactant (T), and water is prepared,(b) a monomer miniemulsion stabilized by a hydrophobic organic compound with a water solubility at 20° C. of not more than 5×10 −5 g/l, is prepared from a polymerizable monomer (M) and at least one surfactant (T), in water, (c) a monomer pigment emulsion is prepared, whereby the aqueous pigment dispersion from (a) and the monomer miniemulsion from (b) are mixed and homogenized, and (d) the pigment-containing monomer miniemulsion from (c) is polymerized in the presence of a polymerization initiator and/or by heat, whereupon an encapsulation of the pigment with the polymer thus formed occurs.
1. A method of producing an aqueous dispersion of polymer-encapsulated pigment, comprising the steps of:
(a) preparing an aqueous pigment dispersion comprising at least one organic pigment P selected from the group consisting of azo, isoindolinone, isoindoline, anthanthrone, thioindigo, thiazineindigo, triarylcarbonium, quinophthalone, anthraquinone, dioxazine, phthalocyanine, quinacridone, quinacridonequinone, indanthrone, perylene, perinone, pyranthrone, diketopyrrolopyrrole, isoviolanthrone, and azomethine pigments, at least one surfactant T, and water;
(b) providing a monomer miniemulsion stabilized by a hydrophobic organic compound having a water solubility at 20° C. of not more than 5×10 −5 g/l and and wherein the monomer miniemulsion includes at least one polymerizable monomer M, at least one surfactant T1 and water, wherein the miniemulsion is in the form of droplets and wherein the droplets have a size of less than or equal to 1000 nm by a homogenization step;
(c) producing a pigment-containing monomer miniemulsion by combining and homogenizing the aqueous pigment dispersion from step (a) and the monomer miniemulsion from step (b), and
(d) polymerizing the pigment-containing monomer miniemulsion from step (c) in the presence of a polymerization initiator by heat or both to form the polymer-encapsulated pigment, wherein the polymer-encapsulated pigment has a homopolymer content of less than 5% by weight based on the total weight of the encapsulated pigment particles.
2. The method as claimed in claim 1 , wherein in step (a) the pigment P is pasted together with the surfactant T in water and the paste is dispersed with the aid of a grinding or dispersing assembly.
3. The method as claimed in claim 1 , wherein in step (a) the surfactant T is used in an amount of 0.1% to 50% by weight, based on the total weight of the aqueous pigment dispersion.
4. The method as claimed in claim 1 , wherein the surfactant T and T1 are the same or different and are selected from the group consisting of phosphates, carboxylates, polymeric ethoxylates, fatty amines, fatty amine ethoxylates, fatty alcohol ethoxylates, fatty acid salts, alkylsulfonates, alkyl sulfates, alkylammonium salts, and sugar ethoxylates.
5. The method as claimed in claim 1 , wherein in step (a) the at least one pigment P is used in an amount of 0.1% to 50% by weight, based on the total weight of the aqueous pigment dispersion.
6. The method as claimed in claim 1 , wherein in step (b) the at least one polymerizable monomer M is incorporated by stirring into an aqueous solution of the surfactant T1, and the hydrophobic organic compound having a water solubility at 20° C. of not more than 5×10 −5 g/l is added to form a mixture, and the mixture is homogenized to form the monomer miniemulsion.
7. The method as claimed in claim 1 , wherein the at least one polymerizable monomer M is a free-radically polymerizable compound selected from the group consisting of acrylic acid, acrylic esters, acrylonitrile, acrylamides, methacrylic acid, methacrylic esters, vinyl alcohols, vinyl ethers, vinylamines, vinyl acetates, vinyl esters, styrenes, maleic esters, maleic anhydride, and maleic acid.
8. The method as claimed in claim 1 , wherein the polymer of the polymer-encapsulated pigment is selected from the group consisting of polyhydroxycarboxylic acids, polyamino acids, polyamides, polyesters, polyimides, polycarbonates, amino resins, phenolic resins, polysulfides, polyepoxides, and urea resins.
9. The method as claimed in claim 1 , wherein the polymer of the polymer-encapsulated pigment is selected from the group consisting of polyurethanes, polyureas, and polyepoxides.
10. The method as claimed in claim 1 , wherein in step (b) the at least one polymerizable monomer M is added in an amount of 0.1% to 80% by weight, based on the total weight of the polymerizable monomer miniemulsion.
11. The method as claimed in claim 1 , wherein in step (b) the surfactant T1 is added in an amount of 0.1% to 50% by weight, based on the total weight of the at least one polymerizable monomer M.
12. The method as claimed in claim 1 , wherein in step (b) the hydrophobic organic compound is added in an amount of 1% to 50% by weight, based on the total weight of the at least one polymerizable monomer M.
13. The method as claimed in claim 1 , wherein in step (c) the aqueous pigment dispersion from (a) and the monomer miniemulsion from (b) are combined in a weight ratio of 5:95 to 95:5, based on the weight of the at least one polymerizable monomer M and the weight of the at least one organic pigment P.
14. The method as claimed in claim 1 , where in step (c) the homogenization is accomplished by exposure to ultrasound.