Preparation of synthetic zeolite molecular sieves

Claim 1

In a process for the manufacture of synthetic zeolites, comprising crystallizing the zeolite from a reaction mixture, the improvement comprising altering the reaction mixture by the addition thereto of an additive selected from the group consisting of crystal violet, methyl violet, nuclear fast red, methylene blue, toluidene blue, malachite green, magenta, acriflavine, and mixtures, salts and esters thereof.

Claim 6

A method of crystallizing zeolite AG5 having the composition 0.7 to 1.1 K 2 O . Al 2 O 3 . 2.5 to 6.0 SiO 2 . 0 to 8 H 2 O and the following X ray diffraction pattern: ______________________________________ dA 100I/I.sub.o ______________________________________ 16.0 100 7.8 22 6.25 22 6.00 15.5 4.79 62 4.60 67 4.15 78 3.87 37 3.66 37 3.42 70 3.25 53 3.17 50 3.10 80 2.80 61 2.68 14 2.60 11 2.57 9 2.32 27 2.17 30 ______________________________________ which comprises reacting together at 50°-120° C a silica source and an alumina source in a potassium-containing aqueous alkaline medium in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet and nuclear fast red, the molar ratio of the constituents of the mixture being represented by SiO 2 /Al 2 O 3 = 7 to 20 K 2 o/k.sub. 2 = 0.45 to 0.65 H 2 o/k.sub. 2 o = 80 to 140 (Basic dye)/Al.sub. 2 O 3 = 5 × 10 - 4 to 0.1

Claim 7

A method of crystallizing zeolite AG5 having the composition 0.7 to 1.1 K 2 O . Al 2 O 3 . 2.5 to 6.0 SiO 2 . 0 to 8 H 2 O and the following X ray diffraction pattern: ______________________________________ dA 100I/I.sub.o ______________________________________ 16.0 100 7.8 22 6.25 22 6.00 15.5 4.79 62 4.60 67 4.15 78 3.87 37 3.66 37 3.42 70 3.25 53 3.17 50 3.10 80 2.80 61 2.68 14 2.60 11 2.57 9 2.32 27 2.17 30 ______________________________________ which comprises reacting together at 50°-120° C a silica source and an alumina source in a potassium-containing aqueous alkaline medium in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet and nuclear fast red, the molar ratio of the constituents of the mixture being represented by SiO 2 /Al 2 O 3 = 7 to 20 K 2 o/k.sub. 2 = 0.45 to 0.65 H 2 o/k.sub. 2 o = 80 to 140 (Basic dye)/Al.sub. 2 O 3 = 5 × 10 - 4 to 0.1

Claim 8

A method of crystallizing zeolite Y or Y 1 which comprises reacting together at 75°-120° C. a silica source and an alumina source in an aqueous alkaline medium containing sodium ions or sodium ions and potassium ions in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet, nuclear fast red, toluidine blue and methylene blue, the molar ratio of basic dye to alumina being in the range of 5 × 10 - 4 to 0.1 and the molar composition of the mixture including SiO 2 /Al 2 O 3 and M 2 O/SiO 2 which are selected in combination from ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 M.sub.2 O/SiO.sub.2 ______________________________________ 4 to 6.9 0.25 to 0.4; 6.9 to 7.9 0.25 to 0.335; 7.9 to 10 0.25 to 0.34; 10 to 12 0.25 to 0.40; 12 to 14 0.25 to 0.45; 14 to 16 0.25 to 0.50; or 15 to 40 0.25 to 1.0, ______________________________________ and further including (b) Na 2 O/M.sub. 2 O = 0.7 to 1.0 H 2 o/m.sub. 2 o = 40 to 120 A 2/n /Al 2 O 3 = 0 to 3 to produce zeolite Y or Y 1 , where M 2 O = Na 2 O + K 2 O and A is an acid radical of valence n.

Claim 9

A method of crystallizing zeolite Y or Y 1 which comprises reacting together at 75°-120° C. a silica source and an alumina source in an aqueous alkaline medium containing sodium ions or sodium ions and potassium ions in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet, nuclear fast red, toluidine blue and methylene blue, the molar ratio of basic dye to alumina being in the range of 5 × 10 - 4 to 0.1 and the molar composition of the mixture including SiO 2 /Al 2 O 3 and M 2 O/SiO 2 which are selected in combination from ______________________________________ SiO.sub.2 /Al.sub.2 O.sub.3 M.sub.2 O/SiO.sub.2 ______________________________________ 4 to 6.9 0.25 to 0.4; 6.9 to 7.9 0.25 to 0.335; 7.9 to 10 0.25 to 0.34; 10 to 12 0.25 to 0.40; 12 to 14 0.25 to 0.45; 14 to 16 0.25 to 0.50; or 15 to 40 0.25 to 1.0, ______________________________________ and further including (b) Na 2 O/M.sub. 2 O = 0.7 to 1.0 H 2 o/m.sub. 2 o = 40 to 120 A 2/n /Al 2 O 3 = 0 to 3 to produce zeolite Y or Y 1 , where M 2 O = Na 2 O + K 2 O and A is an acid radical of valence n.

Claim 10

A method of crystallizing zeolite X which comprises reacting together at 50°-120° C a silica source and an alumina source in an aqueous alkaline medium containing sodium ions or sodium ions and potassium ions in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet, nuclear fast red, toluidine blue and methylene blue, the molar ratio of basic dye to alumina being in the range 5 × 10 - 4 to 0.1 and the molar composition of the mixture being represented by SiO 2 /Al.sub. 2 O 3 = 2.7 to 8 sodium metasilicate hydrate/Al.sub. 2 O 3 = 0.3 to 6.0 M 2 o/siO.sub. 2 = 0.3 to 6.0 Na 2 O/M.sub. 2 O = 0.7 to 1.0 N 2 o/m.sub. 2 o = 10 to 150 where M 2 O = Na 2 O + K 2 O to produce zeolite X.

Claim 11

A method of crystallizing zeolite X which comprises reacting together at 50°-120° C a silica source and an alumina source in an aqueous alkaline medium containing sodium ions or sodium ions and potassium ions in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet, nuclear fast red, toluidine blue and methylene blue, the molar ratio of basic dye to alumina being in the range 5 × 10 - 4 to 0.1 and the molar composition of the mixture being represented by SiO 2 /Al.sub. 2 O 3 = 2.7 to 8 sodium metasilicate hydrate/Al.sub. 2 O 3 = 0.3 to 6.0 M 2 o/siO.sub. 2 = 0.3 to 6.0 Na 2 O/M.sub. 2 O = 0.7 to 1.0 N 2 o/m.sub. 2 o = 10 to 150 where M 2 O = Na 2 O + K 2 O to produce zeolite X.

Claim 12

A method of crystallizing zeolite AG6 having the composition 0.7 to 1.1 (xK 2 O.(1-x)Na 2 O 3 .2.5 to 6.0 SiO 2 to 8 H 2 O wherein x is 0.2 to 0.8, and the following X-ray diffraction pattern: ______________________________________ dA 100I/I.sub.o ______________________________________ 9.36 100 7.05 20 6.24 35 5.42 25 3.116 30 2.978 70 2.618 20 ______________________________________ which comprises reacting together at 50°-120° C a silica source and an alumina in a potassium-containing aqueous alkaline medium in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet and nuclear fast red, the molar ratio of the constituents of the mixture being represented by SiO 2 /Al 2 O 3 = 1 to 10 K 2 o/na 2 O + K 2 O = 0.4 to 0.9 M 2 o/siO 2 = 0.4 to 4.0 H 2 o/m 2 o = 10 to 50 (basic dye)/Al.sub. 2 O 3 = 5 × 10 - 4 to 0.1 wherein M.sub. 2 O = K 2 O + Na 2 O, to produce zeolite AG6.

Claim 13

A method of crystallizing zeolite AG6 having the composition 0.7 to 1.1 (xK 2 O.(1-x)Na 2 O 3 .2.5 to 6.0 SiO 2 to 8 H 2 O wherein x is 0.2 to 0.8, and the following X-ray diffraction pattern: ______________________________________ dA 100I/I.sub.o ______________________________________ 9.36 100 7.05 20 6.24 35 5.42 25 3.116 30 2.978 70 2.618 20 ______________________________________ which comprises reacting together at 50°-120° C a silica source and an alumina in a potassium-containing aqueous alkaline medium in the presence of at least one basic dye selected from the group consisting of malachite green, magenta, crystal violet, methyl violet and nuclear fast red, the molar ratio of the constituents of the mixture being represented by SiO 2 /Al 2 O 3 = 1 to 10 K 2 o/na 2 O + K 2 O = 0.4 to 0.9 M 2 o/siO 2 = 0.4 to 4.0 H 2 o/m 2 o = 10 to 50 (basic dye)/Al.sub. 2 O 3 = 5 × 10 - 4 to 0.1 wherein M.sub. 2 O = K 2 O + Na 2 O, to produce zeolite AG6.