Solid particles having a silicate coating
View Patent ↗A method for producing solid particles having a silica coating, by: dispersing the solid particles to be coated in an aqueous medium to produce a solid particle dispersion, adjusting the pH of the solid particle dispersion by a buffer system to produce a buffered solid particle dispersion, and adding an alkaline silicate solution to the buffered solid particle dispersion to form the silica coating on the solid particles during a coating period. The amounts of buffer system and alkaline silicate solution are selected such that the pH of the buffered solid particle dispersion before the addition of the alkaline silicate solution is at least 7.0 and after completion of the addition of the alkaline silicate solution is at most 11.0.
1. A method for producing solid particles having a silica coating which are suitable as feature substances to increase the falsification security of documents of value, wherein the silica-coated solid particles have diameters in the range of 0.5 μm to 60 μm and the silica coating has a thickness in the range of 100 nm to 10 μm, the method comprising the steps:
producing a buffered solid-particle dispersion by:
dispersing acid-labile solid particles to be coated in an aqueous medium to produce a solid-particle dispersion, and setting the pH value of the solid-particle dispersion by a buffer system; or
dissolving a buffer system in an aqueous medium to produce a buffer solution having a pH value, and dispersing the acid-labile solid particles to be coated in the buffer solution; and
adding a basic silicate solution to the buffered solid-particle dispersion to form the silica coating on the solid particles during a coating time,
wherein the buffer system is selected from the group consisting of potassium hydrogen carbonate/potassium carbonate, sodium hydrogen carbonate/sodium carbonate, and mixtures thereof, the composition and the quantities of the buffer system and of the basic silicate solution are selected such that the pH value of the solid-particle dispersion, before the addition of the basic silicate solution, is at least 8.5, and after the completion of the addition of the basic silicate solution is at most 10.5.
2. The method according to claim 1 , wherein the addition of the basic silicate solution to the buffered solid-particle dispersion is carried out by mixing with the simultaneous presence of shearing forces of the buffered solid-particle dispersion.
3. The method according to claim 1 , wherein the temperature of the buffered solid-particle dispersion, before the addition of the basic silicate solution, is set to 60 to 90° C. and is maintained during the coating time of the solid particles.
4. The method according to claim 1 , wherein the basic silicate solution comprises potassium water glass or sodium water glass.
5. The method according to claim 1 , wherein the basic silicate solution contains:
10 g/L to 360 g/L SiO 2 ; and
5 g/L to 280 g/L, KOH or a quantity of NaOH or of a different base.
6. The method according to claim 1 , wherein the buffer system has a content of buffer acid corresponding to 1 to 4 molar equivalents, with respect to 1 equivalent hydroxide in the basic silicate solution.
7. The method according to claim 1 , wherein per 1 m 2 surface of the solid particles to be coated, the basic silicate solution contains 0.8 to 3.5 g SiO 2 .
8. The method according to claim 1 , wherein for producing the buffered solid-particle dispersion, for each 100 g of solid particles, 500 to 1000 ml water are used.
9. The method according to claim 1 , wherein the basic silicate solution is added to the buffered solid-particle dispersion at a rate which corresponds to 0.08 g to 1.6 g SiO 2 per m 2 solid-particle surface per hour (0.08 g to 1.6 g SiO 2 m −2 h −1 ).
10. The method according to claim 1 , wherein the acid-labile solid particles comprise acid-labile feature substances comprising one or more of:
one or more luminescent substances with characteristic luminescence properties;
one or more magnetic substances;
one or more electrically conductive substances; and
one or more substances absorbing specifically in the infrared wavelength range.
11. The method according to claim 1 , wherein after the end of the coating time, the silica-coated solid particles are separated from the buffered solid-particle dispersion, dried and annealed, said step of annealing being effected at a temperature in the range of 150° C. to 350° C., and for a period of at least 1 hour.
12. The method according to claim 11 , wherein the silica-coated solid particles are annealed at 150° C. for 12 hours or are annealed at 250° C. for 4 hours or are annealed at 300° C. for 2 hours, and wherein the heating is effected at a rate of 5° C./min up to 150° C. or 250° C. or 300° C.
13. The method according to claim 1 , wherein on the solid particles to be coated, there is formed a shell of silica nanoparticles, wherein the silica nanoparticles have diameters in the range of 1 nm to 100 nm.
14. The method according to claim 13 , further comprising at least partly condensing the silica nanoparticles so as to form a three-dimensional network which substantially gaplessly encloses the solid particles to be coated.