Precipitated silicas with a particular pore size distribution
View Patent ↗Precipitated silicas which have a broad pore size distribution of the pores with a pore diameter smaller than that of the maximum of the derivative of the pore volume distribution function are useful, for example, for tires.
1. A precipitated silica, having the following physicochemical parameters:
a relative breadth γ of pore size distribution of
4.0-10.0 (g nm)/ml,
a sears number V 2 of
28-40 ml/(5 g),
a sears number V 2 /CTAB ratio of
0.18-0.28 ml/(5 m 2 ), and
CTAB of
100-200 m 2 /g.
2. The precipitated silica according to claim 1 , wherein a BET/CTAB ratio is greater than 1.3.
3. The precipitated silica according to claim 1 , wherein a zeta potential at pH 5 is from −12 to −30 mV.
4. The precipitated silica according to claim 1 , wherein an oil adsorbency expressed as DBP number is from 200 to 330 g/(100 g).
5. The precipitated silica according to claim 1 , wherein an Al 2 O 3 content is from 0.001 to 5% by weight.
6. The granular precipitated silica according to claim 1 , wherein a (Ro-Tap) sieve residue on a 300 μm sieve is at least 80% by weight.
7. The granular precipitated silica according to claim 1 , wherein a <75 μm (Ro-Tap) sieve fraction is at most 10% by weight.
8. The precipitated silica according to claim 1 , wherein the silica has a carbon content of from 0.1 to 20.0% by weight.
9. An elastomer mixture, comprising:
the precipitated silica of claim 1 .
10. The vulcanizable rubber mixture or vulcanizate, comprising:
at least one precipitated silica according to claim 1 as a filler.
11. A tire, comprising:
at least one precipitated silica according to claim 1 .
12. A process for production of precipitated silica, comprising:
in succession,
a) using, as an initial charge, an aqueous solution of at least one member selected from the group consisting of an alkali metal silicate, an alkaline earth metal silicate, an organic base, an inorganic base and mixtures thereof, the alkali number of the initial charge being from 20 to 40,
b) simultaneously metering alkali metal silicate and/or alkaline earth metal silicate and acidifier into said initial charge with intensive stirring at from 55 to 85° C. until the viscosity rises in the reaction mixture,
c) stopping the feed for from 35 to 85 minutes,
d) simultaneously feeding alkali metal silicate and/or alkaline earth metal silicate and an acidifier with stirring at from 55 to 85° C., until a solids content of from 90 to 140 g/l has been reached in the reaction mixture,
e) acidifying said reaction mixture of step d) to a pH of from about 2.5 to 5.0 with an acidifier, and
f) filtering and drying said acidified reaction mixture, thereby obtaining dried precipitated silica.
13. The process according to claim 12 , wherein in at least one of the steps a) to e), the reaction mixture is sheared with a shear assembly.
14. The process according to claim 13 , wherein, in the steps b) and d), sulfuric acid is metered directly onto a shear head of the shear assembly, to immediately achieve intensive incorporation of the acid by mixing into the reaction mixture.
15. The process according to claim 12 , wherein the inflow rate of the components in step d) is greater than in step b).
16. The process according to claim 15 , wherein the inflow rate of the components in step d) is from 125 to 140% of the inflow rate in step b).
17. The process according to claims 12 , wherein in step b) and/or d), alkali metal silicate and/or alkaline earth metal silicate and acidifier are metered in such a way that the alkali number remains constant during the respective step.
18. The process according to claim 12 , wherein an alkali metal silicate and/or alkaline earth metal silicate and/or an alkali metal hydroxide and/or an alkaline earth metal hydroxide is used as base.
19. The process according to claim 12 , wherein, during steps a) to e), an organic or inorganic salt is added.
20. The process according to claim 12 , wherein a pneumatic dryer, spray dryer, staged dryer, belt dryer, rotating-tube dryer, flash dryer, spin-flash dryer or spray nozzle dryer is used for the drying process.
21. The process according to claim 12 , wherein, after the drying process, a granulation process is carried out with a roll-press.
22. The process according to claim 12 , wherein the precipitated silica is modified with linear, cyclic and/or branched silanes, silazanes, siloxane compounds and/or organosilicon compounds.
23. The process according to claim 22 , wherein bis(3-triethoxysilylpropyl)tetrasulfane or bis(3-triethoxysilylpropyl)disulfane is used for modification of the precipitated silica.