Silicic acid for the filtration of beverages particularly beer

Abstract

A finely divided silicic acid simultaneously suitable as a filtering auxiliary and as a beer stabilizing agent in the filtration of beer. The acid is particulate, and the particles are of an essentially spherical or spheroidal shape with SiO 2 content of at least 95% and an Na 2 O content of less than 0.25%.

What is claimed is: 
     
       1. Process for the preparation of finely divided silicic acid particles, which are simultaneously suitable as a filtering auxiliary and as a stabilizing agent for beer in the filtration thereof, said silicic acid particles being of an essentially spherical or spheroidal shape and having an SiO 2  content of at least 95% by weight, said content being based upon said particles after drying at about 110° C., an Na 2  O content of less than 0.25% by weight, and wherein the pH value of said particles comprising a 10% suspension in water is from about 4 to 7, said particles further having a surface according to Carman no greater than 100 m 2  /g. and said particles having a standard test filtration time t o  of 20 seconds to 6 minutes and a ratio of ##EQU16## of about 0.7 to 6.5, with ##EQU17## being the test filtration time after a stirring stress of 120 minutes at 1000 rpm, comprising forming an aqueous charge containing 0.4 to 2.0% dissolved common salt by weight, said charge being between 33% and 70% by volume of the final volume of said charge and said silicic acid after precipitation of particles of said silicic acid, and wherein said aqueous charge has added uniformly and separately thereto a sodium silicate solution and an acid to form a silicic acid suspension that contains said silicic acid, said sodium silicate solution being metered into said charge whereby the pH value in the charge is about 3 to 10 during the addition, the temperature of said charge being maintained between about 50° C. and 95° C. during said addition, adjusting the pH value of said silicic acid suspension to about 7 to 4 after termination of the addition, filtering said silicic acid, washing said silicic acid with water and immediately drying said silicic acid while avoiding elevated shear stresses, followed by screening said acid in the absence of grinding with the aid of a sieving device. 
     
     
       2. Process for the preparation of finely divided silicic acid particles, which are suitable simultaneously as a filtering auxiliary and as a stabilizing agent for beer in the filtration thereof, said silicic acid particles being of an essentially spherical or spheroidal shape and having an SiO 2  content of at least 99% by weight, said content being based upon said particles after drying at about 110° C. an Na 2  O content less than 0.25% by weight and wherein the pH value of said particles comprising a 10% suspension in water is from about 4 to 7, said particles further having a surface according to Carman no greater than 80 m 2  /g, and said particles having a standard test filtration time t o  of 20 seconds to 6 minutes and a ratio of ##EQU18## of about 1.0 to 4.0, with ##EQU19## being the test filtration time after a stirring stress of 120 minutes at 1000 rpm, ##EQU20## having a value no greater than 10 minutes, wherein said particles are prepared by precipitation to form a dried mass and in the absence of grinding of said dried mass, comprising adding, uniformly and separately, to an aqueous charge containing 0.4 to 2.0% dissolved common salt by weight, said charge being between 33% to 70% by volume of the final volume of said charge and said silicic acid after precipitation of said silicic acid, a sodium silicate solution and an acid to form a silicic acid suspension that contains said silicic acid particles, said sodium silicate solution being metered into said charge whereby the pH value in the charge is about 3 to 10 during the addition, the temperature of said charge being maintained between about 50° C. and 95° C. during said addition, adjusting the pH value of said silicic acid suspension to about 7 to 4 after termination of the addition, filtering said silicic acid, washing said silicic acid with water and immediately drying said silicic acid while avoiding elevated shear stresses, followed by screening said acid in the absence of grinding with the aid of a sieving device. 
     
     
       3. Process pursuant to claim 2, wherein the volume of said charge is at least 50% by volume of the final volume of said charge and said silicic acid after precipitation of said silicic acid. 
     
     
       4. Process pursuant to claim 3, wherein said acid is sulfuric acid. 
     
     
       5. Process pursuant to claim 4, wherein said screening is accomplished with brush passing screens. .Iadd. 
     
     
       6.  Finely divided non-crystalline silicic acid particles, which are simultaneously suitable as a filtering auxiliary and as a stabilizing agent for beer in the filtration thereof, said silicic acid particles being of an essentially spherical or spheroidal shape and having an SiO 2  content of at least 95% by weight, said content being based upon said particles after drying at about 100° C., an Na 2  O content of less than 0.25% by weight, and wherein the pH value of said particles comprising a 10% suspension in water is from about 4 to 7, said particles further having a surface according to Carman no greater than 100 m 2  /g., said particles having a particle size distribution determined according to the method of screen analysis with a set of ultrasound wet screens pursuant to Seitz, with a residue of at least 60% with a hole size of 40μ, a residue of about 1 to 5% with a hole size of 5μ, and an ultra-fine constituent below 5μ no greater than 5%, said particles being made from an aqueous charge containing 0.4 to 2.0 weight percent dissolved common salt and having a volume of 33-70% of the final volume of the silicic acid suspension, said aqueous charge having added uniformly and separately thereto a sodium silicate solution and an acid to form said silicic acid suspension, said particles having a standard test filtration time t o  of 20 seconds to 6 minutes and a ratio of ##EQU21## of about 0.7 to 6.5 with ##EQU22## being the test filtration time stress of 120 minutes at 1000 rpm, said particles being prepared by wet precipitation and drying while avoiding elevated shear stresses to form a dried mass and in the absence of grinding of said dried mass. .Iaddend. 
     
     
       7.  Finely divided silicic acid pursuant to claim 6, wherein said SiO 2  content is at least 99% by weight.  8. Finely divided silicic acid pursuant to claim 6, characterized by a ratio ##EQU23## 
     
     
        of about 1.0 to 4.0.  9.  Finely divided silicic acid pursuant to claim 7, characterized by a ratio ##EQU24## 
     
     
        of about 1.0 to 4.0.  10.  Finely divided silicic acid pursuant to claim 6, wherein said test filtration time ##EQU25## 
     
     
        is 10 minutes or less.  11.  Finely divided silicic acid pursuant to claim 7, wherein said test filtration time ##EQU26## 
     
     
        is 10 minutes or less.  12.  Finely divided silicic acid pursuant to claim 8, wherein said test filtration time ##EQU27## 
     
     
        is 10 minutes or less.  13.  Finely divided silicic acid pursuant to claim 9, wherein said test filtration time ##EQU28## 
     
     
        is 10 minutes or less.  14.  Finely divided silicic acid, containing no lung harmful crystalline silicic acid particles and which is suitable simultaneously as a filtering auxiliary and as a stabilizing agent for beer in the filtration thereof, said silicic acid particles being of an essentially spherical or spheroidal shape and having an SiO 2  content of at least 99% by weight, said content being based upon said particles after drying at about 110° C., an Na 2  O content less than 0.25% by weight, and wherein the pH value of said particles comprising a 10% suspension in water is from about 4 to 7, said particles further having a surface according to Carman no greater than 80 m 2  /g, and said suspension having a standard test filtration time t o  of 20 seconds to 6 minutes and a ratio of ##EQU29## of about 1.0 to 4.0, with ##EQU30## being the test filtration time after a stirring stress of 120 minutes at 1000 rpm, ##EQU31## having a value no greater than 10 minutes, said particles having a particle size distribution determined according to the method of screen analysis with a set ultrasound wet screens pursuant to Seitz, with a residue of at least 60% with a hole size of 40μ, a residue of about 15 to 30% with a hole size of 15μ, a residue of about 1 to 5% with a hole size of 5μ, and an ultra-fine constituent below 5μ of not greater than 5%, said particles being made from an aqueous charge containing common salt to which is added uniformly and separately, a sodium silicate 
     
     
        solution and an acid to form a suspension of said particles.  15.  Finely divided silicic acid pursuant to claim 14, wherein said standard test filtration time t o  is from 30 to 150 seconds.  16. Finely divided silicic acid pursuant to claim 14, characterized by a BET surface of 15 to 350 m 2  /g.  17. Finely divided silicic acid pursuant to claim 15, characterized by a BET surface of 15 to 350 m 2  /g.  18. Finely divided silicic acid pursuant to claim 14, characterized by a BET surface from 40 to 60 m 2  /g.  19. Finely divided silicic acid pursuant to claim 15, characterized by a BET surface from 40 to 60 m 2  /g.  20. Finely divided silicic acid pursuant to claim 17, characterized by a BET surface from 40 to 60 m 2  /g.