Process for the production of finely divided silicic acid by spray drying

Claim 2

A process for preparing a finely divided silicic acid having little grit, comprising: (a) preparing a sprayable aqueous suspension of a precipitated silicic acid containing at least about 12% by weight solids by: (1) continuously feeding a silicic acid filter cake and a suspension agent into a dissolver container provided with stirring means; (2) stirring said filter cake and suspension agent while maintaining a maximum pH value of about 4 in the suspension, said stirring means having a peripheral speed of about 20-30 m/sec; and (3) continuously removing a portion of the resulting suspension from a zone of highest turbulence of the suspension in said container; wherein said container and said stirring means each have a diameter and the ratio of container diameter to the diameter of the stirring means is about 3:1 and the ratio of container diameter to level of filling of said container is maintained at a maximum of about 1:2; and further wherein the silicic acid suspension in said container is maintained in an amount of at least 1.5 to about 2 kg for each 1 kg of silicic acid filter cake which is added to the container; and thereafter (b) spray drying said resulting suspension in the presence of a base or basic-reacting substance selected from the group consisting of alkali metal hydroxides, alkaline earth metal hydroxides, alkali metal carbonates or bicarbonates, alkaline earth metal carbonates or bicarbonates, ammonia or a compound capable of liberating ammonia in an amount at least sufficient to yield a dried, finely divided silicic acid having a pH value of >6 in a 5% by weight aqueous suspension.

Claim 3

Process according to claim 1 wherein said suspension agent is a dilute, aqueous acid.

Claim 4

Process according to claim 2 wherein said dilute, aqueous acid is an aqueous solution containing 20-30 weight percent H 2 SO 4 .

Claim 5

Process according to claim 1 whereby part of said portion of said resulting suspension removed from said zone of highest turbulence is returned to said dissolver to provide a shearing action on said filter cake.

Claim 6

Process according to claim 1 wherein the amount of base or basic-reacting substance is in excess of the amount required to yield said dried silicic acid.

Claim 7

Process according to claim 1 wherein said suspension contains an acid as suspension agent, and said acid is completely or partially neutralized with said base or basic-reacting substance.

Claim 8

Process according to claim 6 wherein said base is an alkali metal hydroxide or alkaline earth metal hydroxide.

Claim 9

Process according to claim 6 wherein said basic-reacting substance is an alkali metal carbonate or bicarbonate or an alkaline earth metal carbonate or bicarbonate.

Claim 10

Process according to claim 6 wherein said basic-reacting substance is ammonia or a compound capable of liberating ammonia.

Claim 11

Process according to claim 6 wherein the amount of base or basic-reacting substance is in excess of the amount required to yield said dried silicic acid.

Claim 12

Process according to claim 1 comprising adding said base or basic-reacting substance and said suspension in liquefied form simultaneously to a spray dryer.

Claim 13

Process according to claim 11 wherein said base is an alkali metal hydroxide or alkaline earth metal hydroxide.

Claim 14

Process according to claim 11 wherein said basic-reacting substance is an alkali metal carbonate or bicarbonate or an alkaline earth metal carbonate or bicarbonate.

Claim 15

Process according to claim 11 wherein said basic-reacting substance is ammonia or a compound capable of liberating ammonia.

Claim 16

Process according to claim 11 wherein the amount of base or basic-reacting substance is in excess of the amount required to yield said dried silicic acid.

Claim 17

Process according to claim 11 in which said base is an aqueous solution of sodium hydroxide.

Claim 18

Process according to claim 1 comprising adding said base or basic-reacting substance and said suspension in liquefied form separately but simultaneously to a spray dryer.

Claim 19

Process according to claim 17 in which said base is an aqueous solution of sodium hydroxide.

Claim 20

Process according to claim 1 comprising adding said suspension to a spray dryer and then adding said base or basic-reacting substances during spray drying of said suspension.

Claim 21

Process according to claim 19 wherein said base is an alkali metal hydroxide or alkaline earth metal hydroxide.

Claim 22

Process according to claim 19 wherein said basic-reacting substance is an alkali metal carbonate or bicarbonate or an alkaline earth metal carbonate or bicarbonate.

Claim 23

Process according to claim 19 wherein the amount of base or basic-reacting substance is in excess of the amount required to yield said dried silicic acid.

Claim 24

Process according to claim 19 in which said base is an aqueous solution of sodium hydroxide.

Claim 25

Process according to claim 1 comprising reacting said base or basic-reacting substance with said suspension in liquified form, and then spray drying the resulting mixture.

Claim 26

Process according to claim 24 in which said base is an aqueous solution of NaOH.

Claim 27

Process according to claim 1 in which said base is an aqueous solution of NaOH.

Claim 28

Process according to claim 1 wherein said silic acid suspension contains at least about 18% by weight solids.

Claim 29

A process for preparing a finely divided silicic acid having little grit, said process comprising adding an acidic silicic acid suspension containing at least about 12% by weight solids to a spray dryer, spray drying said suspension, and then contacting the resulting dried silicic acid in a conveying air stream therefor with a base or basic-reacting substance selected from the group consisting of alkali metal hydroxides, alkaline earth metal hydroxides, alkali metal carbonates or bicarbonates, alkaline earth metal carbonates or bicarbonates, ammonia or a compound capable of liberating ammonia in an amount at least sufficient to yield a dried, finely divided silicic acid having a pH value of >6 in a 5% by weight aqueous suspension, said silicic acid suspension having been prepared by (a) preparing a sprayable aqueous suspension of a precipitated silicic acid containing at least about 12% by weight solids by: (1) continuously feeding a silicic acid filter cake and a suspension agent into a dissolver container provided with stirring means; (2) stirring said filter cake and suspension agent while maintaining a maximum pH value of about 4 in the suspension, said stirring means having a peripheral speed of about 20-30 m/sec; and (3) continuously removing a portion of the resulting suspension from a zone of highest turbulence of the suspension in said container; wherein said container and said stirring means each have a diameter and the ratio of container diameter to the diameter of the stirring means is about 3:1 and the ratio of container diameter to level of filling of said container is maintained at a maximum of about 1:2; and further wherein the silicic acid suspension in said container is maintained in an amount of at least 1.5 to about 2 kg for each 1 kg of silicic acid filter cake which is added to the container.

Claim 30

A process for preparing a finely divided silicic acid having little grit, said process comprising adding an acidic silicic acid suspension containing at least about 12% by weight solids to a spray dryer, spray drying said suspension, and then contacting the resulting dried silicic acid in a conveying air stream therefor with a base or basic-reacting substance selected from the group consisting of alkali metal hydroxides, alkaline earth metal hydroxides, alkali metal carbonates or bicarbonates, alkaline earth metal carbonates or bicarbonates, ammonia or a compound capable of liberating ammonia in an amount at least sufficient to yield a dried, finely divided silicic acid having a pH value of >6 in a 5% by weight aqueous suspension, said silicic acid suspension having been prepared by (a) preparing a sprayable aqueous suspension of a precipitated silicic acid containing at least about 12% by weight solids by: (1) continuously feeding a silicic acid filter cake and a suspension agent into a dissolver container provided with stirring means; (2) stirring said filter cake and suspension agent while maintaining a maximum pH value of about 4 in the suspension, said stirring means having a peripheral speed of about 20-30 m/sec; and (3) continuously removing a portion of the resulting suspension from a zone of highest turbulence of the suspension in said container; wherein said container and said stirring means each have a diameter and the ratio of container diameter to the diameter of the stirring means is about 3:1 and the ratio of container diameter to level of filling of said container is maintained at a maximum of about 1:2; and further wherein the silicic acid suspension in said container is maintained in an amount of at least 1.5 to about 2 kg for each 1 kg of silicic acid filter cake which is added to the container.

Claim 31

Process according to claim 28 in which said base is an aqueous solution of sodium hydroxide.

Claim 32

Process according to claim 28 wherein said basic-reacting substance is an alkali metal carbonate or bicarbonate or an alkaline earth metal carbonate or bicarbonate.

Claim 33

Process according to claim 28 wherein said basic-reacting substance is ammonia or a compound capable of liberating ammona.

Claim 34

Process according to claim 28 wherein the amount of base or basic-reacting substance is in excess of the amount required to yield said dried silicic acid.

Claim 35

Process according to claim 28 wherein said base is an alkali metal hydroxide or alkaline earth metal hydroxide.