Methods for preparing amorphous zirconium phosphosilicate

Claim 2

A process for producing an amorphous zirconium phosphosilicate represented by the formula Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 10.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and a SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; and (vii) optionally heating the dried cake at about 250° to about 950° C.

Claim 3

A process as defined in claim 1 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 4

A process as defined in claim 2 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 5

A process as defined in claim 1 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammonium salts of these acids.

Claim 6

A process as defined in claim 4 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 7

A process as defined in claim 1 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 8

A process as defined in claim 6 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 9

A process as defined in claim 1 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 10

A process as defined in claim 1 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 11

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorous compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and a SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00, with at least one kind of cation incorporated in at least one of said aqueous solutions; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; and (vii) optionally heating the dried cake at about 250° to about 950° C.

Claim 12

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorous compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and a SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00, with at least one kind of cation incorporated in at least one of said aqueous solutions; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; and (vii) optionally heating the dried cake at about 250° to about 950° C.

Claim 13

A process as defined in claim 10 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 14

A process as defined in claim 11 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 15

A process as defined in claim 10 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammonium salts of these acids.

Claim 16

A process as defined in claim 13 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 17

A process as defined in claim 10 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 18

A process as defined in claim 15 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 19

A process as defined in claim 10 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 20

A process as defined in claim 10 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 21

A process as defined in claim 10 wherein the cation is at least one ion chosen from the group consisting of NH 4 + and ions formed from metals of Group 1A, Group 1B, Group 2A, Group 2B, Group 3A, Group 3B, Group 5A, Group 6A, Group 7A and Group 8 of the Periodic Table.

Claim 22

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00 and a solution containing at least one kind of cation; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; and (vii) optionally heating the dried cake at about 250° to about 950° C.

Claim 23

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00 and a solution containing at least one kind of cation; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; and (vii) optionally heating the dried cake at about 250° to about 950° C.

Claim 24

A process as defined in claim 20 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 25

A process as defined in claim 21 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 26

A process as defined in claim 20 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammcnium salts of these acids.

Claim 27

A process as defined in claim 23 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 28

A process as defined in claim 20 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 29

A process as defined in claim 25 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 30

A process as defined in claim 20 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 31

A process as defined in claim 20 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 32

A process as defined in claim 20 wherein the cation is at least one ion chosen from the group consisting of NH4+ and ions formed from metals of Group 1A, Group 1B, Group 2A, Group 2B, Group 3A, Group 3B, Group 5A, Group 6A, Group 7A and Group 8 of the Periodic Table.

Claim 33

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) admixing at least one kind of cation with the resulting slurry containing the reaction product; (iv) aging the resulting mixture containing the reaction product of about 5° to about 100° C. for about 1 to 240 hours; (v) washing the resulting precipitate; (vi) subjecting the precipitate to solid-liquid separation; (vii) drying the wet cake obtained at a temperature of up to about 250° C.; and (viii) optionally heating the dried cake at about 250° to about 950° C.

Claim 34

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) admixing at least one kind of cation with the resulting slurry containing the reaction product; (iv) aging the resulting mixture containing the reaction product of about 5° to about 100° C. for about 1 to 240 hours; (v) washing the resulting precipitate; (vi) subjecting the precipitate to solid-liquid separation; (vii) drying the wet cake obtained at a temperature of up to about 250° C.; and (viii) optionally heating the dried cake at about 250° to about 950° C.

Claim 35

A process as defined in claim 30 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 36

A process as defined in claim 31 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 37

A process as defined in claim 30 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammonium salts of these acids.

Claim 38

A process as defined in claim 33 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 39

A process as defined in claim 30 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 40

A process as defined in claim 35 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 41

A process as defined in claim 30 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 42

A process as defined in claim 30 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 43

A process as defined in claim 30 wherein the cation is at least on ion chosen from the group consisting of NH 4 + and ions formed from metals of Group 1A, Group 1B, Group 2A, Group 2B, Group 3A, Group 3B, Group 5A, Group 6A, Group 7A and Group 8 of the Periodic Table.

Claim 44

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O) wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) admixing at least one kind of cation with the wet cake obtained; (vii) drying the wet cake at a temperature of up to about 250° C.; and (viii) optionally heating the dried cake at about 250° to about 950° C.

Claim 45

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O) wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) admixing at least one kind of cation with the wet cake obtained; (vii) drying the wet cake at a temperature of up to about 250° C.; and (viii) optionally heating the dried cake at about 250° to about 950° C.

Claim 46

A process as defined in claim 40 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 47

A process as defined in claim 41 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 48

A process as defined in claim 40 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammonium salts of these acids.

Claim 49

A process as defined in claim 43 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 50

A process as defined in claim 40 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 51

A process as defined in claim 45 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 52

A process as defined in claim 40 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 53

A process as defined in claim 40 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 54

A process as defined in claim 40 wherein the cation is at least one ion chosen from the group consisting of NH 4 + and ions formed from metals of Group 1A, Group 1B, Group 2A, Group 2B, Group 3A, Group 3B, Group 5A, Group 6A, Group 7A and Group 8 of the Periodic Table.

Claim 55

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and a SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; (vii) optionally heating the dried cake at about 250° to about 950° C.; (viii) dispersing the resulting powder in water; (ix) admixing at least one kind of cation with the resulting dispersion; (x) subjecting the resulting mixture to solid-liquid separation; and (xi) drying the resulting solids.

Claim 56

A process for producing an amorphous zirconium phosphosilicate represented by the formula M 2/l Zr(PO 4 ) 2y (SiO 2 ) z .n'H 2 O wherein M is a cation, l is the valence of the cation, y is 0.02 to 2.00, z is 0.05 to 16.00 and n' is 0 to 9.00 comprising: (i) preparing respective aqueous solutions of a zirconium compound, a phosphorus compound and a silicon compound in a P 2 O 5 /ZrO 2 mole ratio of 0.02 to 2.50 and a SiO 2 /ZrO 2 mole ratio of 0.05 to 20.00; (ii) mixing together said aqueous solutions so that the resulting slurry contains an end product in an amount of up to 20% by weight; (iii) aging the resulting slurry containing the reaction product at about 5° to about 100° C. for about 1 to 240 hours; (iv) washing the resulting precipitate; (v) subjecting the precipitate to solid-liquid separation; (vi) drying the wet cake obtained at a temperature of up to about 250° C.; (vii) optionally heating the dried cake at about 250° to about 950° C.; (viii) dispersing the resulting powder in water; (ix) admixing at least one kind of cation with the resulting dispersion; (x) subjecting the resulting mixture to solid-liquid separation; and (xi) drying the resulting solids.

Claim 57

A process as defined in claim 50 wherein the zirconium compound is at least one salt chosen from the group consisting of mineral acid salts, organic acid salts and complex salts.

Claim 58

A process as defined in claim 51 wherein the zirconium compound is at least one of zirconium oxychloride, zirconium hydroxychloride, zirconyl sulfate and zirconyl nitrate.

Claim 59

A process as defined in claim 50 wherein the phosphorus compound is at least one of phosphoric acid, pyrophosphoric acid, condensation phosphoric acid and alkali metal salts and ammonium salts of these acids.

Claim 60

A process as defined in claim 53 wherein the phosphorus compound is phosphoric acid and/or sodium phosphate.

Claim 61

A process as defined in claim 50 wherein the silicon compound is at least one of silicic acid, alkali silicates, water glass silicate and colloidal silica.

Claim 62

A process as defined in claim 55 wherein the silicon compound is at least one of sodium silicate, sodium metasilicate and water glass silicate.

Claim 63

A process as defined in claim 50 wherein the reaction is conducted at a temperature of about 5° to about 70° C.

Claim 64

A process as defined in claim 50 wherein the drying is conducted at a temperature of about 40° to about 150° C.

Claim 65

A process as defined in claim 50 wherein the cation is at least one ion chosen from the group consisting of NH 4 + and ions formed from metals of Group 1A, Group 1B, Group 2A, Group 2B, Group 3A, Group 3B, Group 5A, Group 6A, Group 7A and Group 8 of the Periodic Table.