Process for preparing aqueous colloidal silica sols of high purity from alkali metal silicate solutions
View Patent ↗The present invention relates to a process for preparing aqueous colloidal silica sols of high purity from silicate solutions, to aqueous colloidal silica sols with a specific profile of impurities, and to the use thereof. The invention further encompasses high-purity aqueous silica obtained as an intermediate in the course of the purification process, high-purity silicon dioxide obtainable by dewatering, and the use thereof.
1. A process for preparing an aqueous colloidal silica sol, the process comprising the following steps:
a. Preparing an acidic aqueous alkali metal silicate solution with a pH of less than 2 by mixing a water-soluble alkali metal silicate or an aqueous alkali metal silicate solution with an acidifier, wherein the concentration of the alkali metal silicate in the acidic aqueous alkali metal silicate solution is 1 to 8% by weight (based on the SiO 2 content), and wherein the weight ratio between the alkali metal silicate (based on the SiO 2 content) and the acidifier in the acidic aqueous metal silicate solution is within a range from 0.4 to 40, and contacting the acidic aqueous alkali metal silicate solution with a resin containing one or more chelate-forming functional groups selected from the group consisting of phosphonic acid groups, substituted or unsubstituted amino phosphonic acid groups, sulphonic acid groups, and carboxyl groups, wherein the chelate-forming functional groups have binding affinity to divalent or higher-valency metal ions;
b. Contacting the acidic alkali metal silicate solution from process step a) with a basic anion exchange resin of the hydroxyl type and an acidic cation exchange resin of the hydrogen type in any sequence, the anion exchange resin and the cation exchange resin being used in spatial separation or in a mixture; and
c. Forming a stable colloidal silica sol by establishing a temperature, concentration and pH suitable for nucleation and particle growth in the aqueous silica solution obtained from step b).
2. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the acidic alkali metal silicate solution obtained from process step a) is aged at a temperature in the range from 10 to 100° C. for a period of 0 to 48 h.
3. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the acidifier is initially charged in step a) and the water-soluble alkali metal silicate or the aqueous alkali metal silicate solution is added.
4. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the mixing in step a) is effected by means of a static or dynamic mixer.
5. The process for preparing an aqueous colloidal silica sol according to claim 1 , in which the water-soluble alkali metal silicate is a sodium waterglass or potassium waterglass with a molar ratio of SiO 2 /A 2 O (A: Na or K) of 4.5 to 1.5.
6. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the acidifier comprises one or more acids selected from the group consisting of hydrochloric acid, phosphoric acid, nitric acid, sulphuric acid, chlorosulphonic acid, sulphuryl chloride and perchloric acid.
7. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the acidic aqueous solution of a water-soluble alkali metal silicate comprises hydrogen peroxide.
8. The process for preparing an aqueous colloidal silica sol according to claim 1 , wherein the aqueous silica solution obtained after step b) has a pH of 1 to 5.