Process for the manufacture of organosilicon compound-treated pigments
View Patent ↗An improved process for making an organosilicon compound surface-treated titanium dioxide material, comprising (a) forming a mixture of the titanium dioxide material in water, (b) wet milling the mixture, (c) adjusting the pH of the slurry resulting from step (b) to between about 5.0 and about 8.5, (d) after step (c), removing the titanium dioxide material from the mixture by vacuum or pressure filtration, (e) after step (d), washing the titanium dioxide material so removed, (f) after step (e), converting the washed titanium dioxide material to a fluid dispersion having a pH of from about 3.5 to less than about 7 via addition of a fluidizing agent comprising a water-soluble monoprotic acid, (g) after, or concurrently with, step (f), adding to the resulting dispersion of titanium dioxide material an organosilicon compound, with mixing, and (h) spray drying the dispersion of the washed titanium dioxide material resulting from step (g) to yield a dry titanium dioxide pigment powder.
1. An improved process for making an organosilicon compound surface-treated titanium dioxide material, comprising the steps of:
(a) forming a mixture comprising a titanium dioxide material in water;
(b) wet milling said mixture;
(c) adjusting the pH of a slurry resulting from step (b) to between about 5.0 and about 8.5;
(d) after step (c), removing said titanium dioxide material from said mixture by vacuum or pressure filtration;
(e) after step (d), washing said titanium dioxide material;
(f) after step (e), converting said washed titanium dioxide material to a fluid dispersion having a pH value of about 3.5 to less than about 7 via addition of a fluidizing agent comprising a water-soluble monoprotic acid;
(g) after, or concurrently with, step (f), adding to the resulting dispersion of titanium dioxide material an organosilicon compound as a organic surface treatment, with mixing; and
(h) after step (g), spray drying the dispersion of the washed titanium dioxide material resulting from step (g) to yield a dry titanium dioxide pigment powder.
2. A process as defined in claim 1 , comprising the further step after step (b) and before step (c) of depositing on the wet milled titanium dioxide material one or more inorganic oxides selected from the group consisting of the oxides of aluminum, boron, cerium, phosphorus, silicon, tin, titanium and zirconium.
3. A process as defined in claim 2 , wherein in step (g), the addition of an organosilicon compound is accomplished without substantial dilution of the titanium dioxide material.
4. A process as defined in claim 1 , wherein in step (g), the addition of an organosilicon compound is accomplished without substantial dilution of the titanium dioxide material.
5. A process as defined in claim 4 , wherein the washed titanium dioxide material is characterized by a titanium dioxide solids content of from about 40 percent by weight to about 70 percent by weight and a Brookfield viscosity of more than 10,000 cps, and further wherein the addition of the fluidizing agent provides a fluid dispersion for spray drying having a Brookfield viscosity of less than about 1000 cps.
6. A process as defined in claim 5 , wherein the fluid dispersion is characterized by a Brookfield viscosity of less than about 500 cps.
7. A process as defined in claim 6 , wherein the fluid dispersion is characterized by a Brookfield viscosity of less than about 100 cps.
8. A process as defined in claim 3 , wherein apart from any organosilicon compound added for providing an organic surface treatment of the titanium dioxide material, essentially only the fluidizing agent is added to the washed titanium dioxide material before a dispersion is formed and then spray dried in step h), and further wherein the fluidizing agent after the addition comprises between about 0.025% by weight and about 2% by weight of the titanium dioxide material.
9. A process as defined in claim 8 , wherein the fluidizing agent after the addition comprises between about 0.05% by weight and about 1% by weight of the titanium dioxide material.
10. A process as defined in claim 8 , wherein the fluidizing agent after the addition comprises between about 0.10% by weight and about 0.5% by weight of the titanium dioxide material.
11. A process as defined in claim 1 , wherein the fluidizing agent is an aqueous solution of one or more water-soluble monoprotic acids selected from the group consisting of nitric acid, hydrochloric acid, and carboxylic acids, sulfonic acids, phosphoric acid diesters and phosphinic acids containing less than about eight carbon atoms.
12. A process as defined in claim 11 , wherein the fluidizing agent is an aqueous solution of one or more of formic acid, acetic acid, propionic acid, lactic acid, glycolic acid, methanesulfonic acid, p-toluenesulfonic acid, phosphoric acid dimethyl ester, methylphosphonic acid monomethyl ester, dimethylphosphinic acid, hydrochloric acid and nitric acid.
13. A process as defined in claim 1 , wherein an alkyltrialkoxysilane or a dialkyldialkoxysilane is added for the organic surface treatment of the titanium dioxide material in step (g).
14. A process as defined in claim 1 , further comprising the step of processing the dry titanium dioxide pigment powder produced in step (h) in a fluid energy mill.