Silica gel comprising guanidine carbonate
View Patent ↗A process of preparing a silica sol is described. The process involves reacting a fresh sol with guanidine carbonate. The reaction may be conducted in the presence of a base (e. g. , sodium water glass), and at a pH of from 8 to 12. The process of the present invention may also include concentrating steps. The silica sol prepared by the method of the present invention has a BET surface area of greater than or equal to 100 m 2 /g, and contains from 0.05 to 15% by weight of gaunidinium ions, based on the total weight of the silica gel.
1. A process for the preparation of a silica sol comprising reacting a fresh sol with guanidine carbonate, wherein the fresh sol comprises an aqueous system having an SiO 2 content of 4 to 8% by weight and a pH of 2 to 4, wherein the prepared silica sol has a BET surface area of 100 to 1200 m 2 /g, comprises from 0.05 to 15% by weight of guanidinium ions, based on the total weight of the prepared silica sol, and wherein the prepared silica sol is free of amine.
2. The process of claim 1 , wherein the reaction with guanidine carbonate is conducted in the presence of a base.
3. The process of claim 2 , wherein the base is selected from the group consisting of sodium water glass, potassium water glass, potassium hydroxide, sodium hydroxide and combinations thereof.
4. The process of claim 2 , wherein the reaction is carried out at a reaction temperature and at a pH of from 8 to 12, the pH being measured at the reaction temperature.
5. The process of claim 1 , wherein said process is conducted continuously.
6. The process of claim 2 , wherein the fresh sol and an aqueous solution of guanidine carbonate are fed continuously into a reactor, said reaction being conducted at,
a pH of from 8 to 12, and
a reaction temperature of from 25C to 100C, further wherein an average residence time is selected such that the silica sol prepared has a BET surface area of ≧100 m 2 /g.
7. The process of claim 6 , wherein said reaction temperature is from 80to 100C.
8. The process of claim 6 , wherein an additional base is added into the reactor.
9. The process of claim 6 , wherein the reactor is a multistage reactor cascade having a first reactor, said fresh sol and an aqueous solution of guanidine carbonate being fed to the first reactor.
10. The process of claim 9 , wherein the pH, measured at the reaction temperature, is from 8 to 12 in all reactors of the multistage reactor cascade, and the reaction temperature in the first reactor is kept at from 25C to 100C, and the reaction temperature in each further reactor is kept at from 60C to 100 C.
11. The process of claim 1 , wherein the reaction is conducted batchwise, the guanidine carbonate being in the form of an aqueous solution of guanidine carbonate, said process comprising,
introducing initially a part of the fresh sol and the aqueous solution of guanidine carbonate into a reactor, resulting in the formation of a remainder comprising said fresh sol and said aqueous solution of guanidine carbonate, said remainder not being initially introduced into said reactor, and
metering subsequently said remainder into the reactor, and the holding said reactor at a temperature such that an amount of solvent which corresponds to the amount of said remainder evaporates from said reactor, thereby concentrating said silica sol.
12. The process of claim 1 , further comprising concentrating said silica sol by a method selected from the group consisting of evaporation of solvent and by ultrafiltration, wherein the concentration step is conducted during or after the reaction of fresh sol with guanidine carbonate.
13. The process as claimed in claim 1 , wherein said silica sol is not stabilized with aluminum and is free of amine.