Crystalline aluminophosphate composition

Claim 2

Microporous crystalline aluminophosphates having a framework structure whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table I TABLE I ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 VS 13.0-13.1 6.83-6.74 VW-W 14.1-14.2 6.28-6.22 VW-W 16.0-16.2 5.55-5.47 VW-M 17.9-18.3 4.94-4.84 VW-W 20.8-21.0 4.34-4.23 M 25.1-25.6 3.54-3.48 VW-W 30.8-31.0 2.903-2.887 W-M ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak, and Very Weak, respectively.

Claim 3

Microporous crystalline aluminophosphate composition according to claim 1 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth in Table II TABLE II ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 100 13.0-13.1 6.83-6.74 4-17 14.1-14.2 6.28-6.22 8-15 15.5-15.8 5.70-5.65 5-8 16.0-16.2 5.55-5.47 10-23 16.6-16.9 5.34-5.25 0-7 17.9-18.3 4.94-4.84 0-17 19.1-19.2 4.64-4.63 0-4 20.8-21.0 4.34-4.23 20-48 22.1-22.2 4.02-4.00 0-4 22.6-22.7 3.94-3.92 0-3 23.1-23.3 3.85-3.81 0-4 25.1-25.6 3.54-3.48 8-16 26.1-26.3 3.41-3.38 0-13 28.3-28.5 3.16-3.14 0-3 30.2-30.5 2.959-2.935 0-9 30.8-31.0 2.903-2.887 14-22 32.1-32.5 2.785-2.753 0-4 33.6-33.9 2.669-2.647 0-3 34.9-35.1 2.571-2.560 0-4 36.3-36.5 2.477-2.465 0-2 39.9-40.3 2.261-2.239 0-3 43.2-43.3 2.094-2.087 0-3 49.5-49.9 1.842-1.826 0-3 51.1-51.3 1.789-1.780 0-3. ______________________________________

Claim 4

A microporous crystalline aluminophosphate composition prepared by calcining a composition of claim 1.

Claim 5

Microporous crystalline aluminophosphate composition which results from the calcination of the composition of claim 1 at a temperature of at least 300° C.

Claim 6

Microporous crystalline aluminophosphate composition having a framework structure whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth in Table III TABLE III ______________________________________ Relative 2θ d (Å) Intensity ______________________________________ 9.7 9.10 VS 12.9 6.88 W 19.5 4.55 M 24.4 3.65 W 29.3 3.05 W 31.0 2.883 W ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively.

Claim 7

Microporous crystalline aluminophosphate composition having a framework structure whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth in Table III TABLE III ______________________________________ Relative 2θ d (Å) Intensity ______________________________________ 9.7 9.10 VS 12.9 6.88 W 19.5 4.55 M 24.4 3.65 W 29.3 3.05 W 31.0 2.883 W ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively.

Claim 8

Microporous crystalline aluminophosphate composition having a framework structure whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacing as set forth in Table IV TABLE IV ______________________________________ Relative 2θ d (Å) Intensity ______________________________________ 9.4 9.37 VS 12.9 6.87 W-M 16.0 5.53 W-M 17.8 4.97 W-M 20.7 4.30 M-S 25.0 3.56 W-M 30.7 2.910 W-S ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively.

Claim 9

Microporous crystalline aluminophosphate composition having a framework structure whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacing as set forth in Table IV TABLE IV ______________________________________ Relative 2θ d (Å) Intensity ______________________________________ 9.4 9.37 VS 12.9 6.87 W-M 16.0 5.53 W-M 17.8 4.97 W-M 20.7 4.30 M-S 25.0 3.56 W-M 30.7 2.910 W-S ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively.

Claim 10

Process for preparing a microporous crystalline aluminophosphate composition having framework structures formed of AlO 2 and PO 2 units whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth in Tables I TABLE I ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 VS 13.0-13.1 6.83-6.74 VW-W 14.1-14.2 6.28-6.22 VW-W 16.0-16.2 5.55-5.47 VW-M 17.9-18.3 4.94-4.84 VW-W 20.8-21.0 4.34-4.23 M 25.1-25.6 3.54-3.48 VW-W 30.8-31.0 2.903-2.887 W-M ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively, which process comprises, using an AlPO 4 -34 seed and forming a reaction mixture having a composition expressed in terms of mole ratios of oxides of Al.sub.2 O.sub.3 : 1-6 P.sub.2 O.sub.5 : 7-300 H.sub.2 O and containing from about 2 to about 12 moles of at least one organic templating agent, and heating the reaction mixture thus formed at a temperature of at least about 75° C. to about 200° C. under autogenous pressure until crystals of said aluminophosphate are formed.

Claim 11

Process for preparing a microporous crystalline aluminophosphate composition having framework structures formed of AlO 2 and PO 2 units whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern containing at least the d-spacings as set forth in Tables I TABLE I ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 VS 13.0-13.1 6.83-6.74 VW-W 14.1-14.2 6.28-6.22 VW-W 16.0-16.2 5.55-5.47 VW-M 17.9-18.3 4.94-4.84 VW-W 20.8-21.0 4.34-4.23 M 25.1-25.6 3.54-3.48 VW-W 30.8-31.0 2.903-2.887 W-M ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively, which process comprises, using an AlPO 4 -34 seed and forming a reaction mixture having a composition expressed in terms of mole ratios of oxides of Al.sub.2 O.sub.3 : 1-6 P.sub.2 O.sub.5 : 7-300 H.sub.2 O and containing from about 2 to about 12 moles of at least one organic templating agent, and heating the reaction mixture thus formed at a temperature of at least about 75° C. to about 200° C. under autogenous pressure until crystals of said aluminophosphate are formed.

Claim 12

Process for preparing a microporous crystalline aluminophosphate composition having framework structures formed of AlO 2 and PO 2 units whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in the following Table I TABLE I ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 VS 13.0-13.1 6.83-6.74 VW-W 14.1-14.2 6.28-6.22 VW-W 16.0-16.2 5.55-5.47 VW-M 17.9-18.3 4.94-4.84 VW-W 20.8-21.0 4.34-4.23 M 25.1-25.6 3.54-3.48 VW-W 30.8-31.0 2.903-2.887 W-M ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively, which process comprises forming a reaction mixture having a composition comprising Al 2 O 3 , and 4-6 moles of phosphorus source (calculated as P 2 O 5 ) per mole of Al 2 O 3 , and sufficient organic templating agent to provide the microporous crystalline aluminophosphate composition in the presence of sufficient water to form a solution, and taking the mixture to an elevated temperature sufficient to form crystals of said aluminophosphate composition.

Claim 13

Process for preparing a microporous crystalline aluminophosphate composition having framework structures formed of AlO 2 and PO 2 units whose chemical composition expressed in terms of mole ratios of oxides is Al.sub.2 O.sub.3 : 1.0±0.2 P.sub.2 O.sub.5 and having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in the following Table I TABLE I ______________________________________ Relative 2θ d, (Å) Intensity ______________________________________ 9.6-9.8 9.24-9.06 VS 13.0-13.1 6.83-6.74 VW-W 14.1-14.2 6.28-6.22 VW-W 16.0-16.2 5.55-5.47 VW-M 17.9-18.3 4.94-4.84 VW-W 20.8-21.0 4.34-4.23 M 25.1-25.6 3.54-3.48 VW-W 30.8-31.0 2.903-2.887 W-M ______________________________________ where the notations VS, M, W and VW represent Very Strong, Medium, Weak and Very Weak, respectively, which process comprises forming a reaction mixture having a composition comprising Al 2 O 3 , and 4-6 moles of phosphorus source (calculated as P 2 O 5 ) per mole of Al 2 O 3 , and sufficient organic templating agent to provide the microporous crystalline aluminophosphate composition in the presence of sufficient water to form a solution, and taking the mixture to an elevated temperature sufficient to form crystals of said aluminophosphate composition.

Claim 14

Process for preparing a microporous crystalline aluminophosphate composition of claim 7 wherein the templating agent is tetraethylammonium hydroxide.

Claim 15

Process for preparing a microporous crystalline aluminophosphate composition according to claim 7 wherein an additional step comprises mixing AlPO 4 -5 in a mixture to form AlPO 4 -34.

Claim 16

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table A TABLE A ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.6 9.24 100 13.0 6.80 12 14.1 6.27 11 15.6 5.69 7 16.2 5.48 23 16.8 5.27 3 17.9 4.94 14 19.1 4.64 3 20.9 4.25 41 22.1 4.02 4 22.6 3.94 3 23.3 3.81 3 25.1 3.54 15 26.3 3.39 9 28.3 3.16 3 30.2 2.959 4 30.9 2.896 22 32.5 2.753 3 33.9 2.647 3 34.9 2.570 3 36.5 2.465 2 39.9 2.258 2 43.3 2.090 2 49.5 1.842 2 51.3 1.782 3. ______________________________________

Claim 17

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table B TABLE B ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.7 9.10 100 10.2 8.65 34 12.1 7.30 3 12.9 6.88 19 15.5 5.73 4 17.2 5.15 4 19.5 4.55 29 19.8 4.48 26 20.7 4.30 23 21.5 4.13 5 22.8 3.91 7 24.4 3.65 14 24.9 3.58 7 25.9 3.44 5 27.0 3.30 5 27.4 3.25 3 28.2 3.17 8 29.3 3.05 17 31.0 2.883 15 32.0 2.799 10 33.0 2.714 7 38.4 2.347 3 40.1 2.250 3 43.1 2.097 2 49.6 1.838 3 53.0 1.726 3. ______________________________________

Claim 18

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table C TABLE C ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.6 9.19 100 13.1 6.77 10 14.1 6.26 10 15.5 5.70 6 16.2 5.47 23 16.9 5.25 2 18.0 4.93 14 19.2 4.63 4 20.9 4.25 40 22.2 4.00 4 22.7 3.92 3 23.3 3.81 2 25.2 3.54 16 26.3 3.38 8 28.4 3.14 3 30.5 2.935 4 30.9 2.893 22 32.1 2.785 2 33.8 2.653 2 35.0 2.566 3 36.3 2.475 2 40.1 2.248 2 43.3 2.089 2 49.5 1.842 2 51.2 1.784 3. ______________________________________

Claim 19

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table D TABLE D ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.4 9.37 100 12.9 6.87 34 14.0 6.34 5 16.0 5.53 25 17.8 4.97 27 19.1 4.66 4 20.7 4.30 87 22.1 4.02 7 22.5 3.96 5 23.1 3.85 10 23.9 3.73 2 25.0 3.56 40 26.0 3.43 33 27.7 3.22 7 28.2 3.16 5 29.7 3.01 5 30.7 2.910 74 31.2 2.871 39 32.5 2.759 4 33.5 2.673 6 34.6 2.590 16 36.1 2.485 13 38.8 2.321 3 39.7 2.270 62. ______________________________________

Claim 20

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table E TABLE E ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.6 9.23 100 13.0 6.83 10 14.1 6.28 11 16.1 5.51 18 16.7 5.32 5 18.1 4.91 14 20.9 4.25 48 23.1 3.85 4 25.2 3.53 11 26.1 3.41 11 28.4 3.14 3 30.3 2.954 9 30.9 2.898 16 43.2 2.093 3. ______________________________________

Claim 21

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table F TABLE F ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.7 9.15 100 13.1 6.75 8 14.2 6.24 11 16.1 5.50 15 18.3 4.84 16 21.0 4.23 35 23.3 3.81 3 25.5 3.49 11 26.2 3.40 10 28.5 3.14 2 30.4 2.945 7 30.9 2.889 16 32.2 2.783 3 33.6 2.669 2 34.9 2.571 3 40.3 2.239 3 49.7 1.834 2 51.1 1.789 2. ______________________________________

Claim 22

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table G TABLE G ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.6 9.18 100 13.1 6.74 5 14.1 6.28 10 16.1 5.51 14 18.3 4.86 16 20.9 4.25 26 22.1 4.02 2 22.6 3.93 3 23.1 3.85 3 25.5 3.50 11 26.2 3.40 6 28.3 3.15 2 30.9 2.897 16 32.3 2.773 4 34.9 2.571 2 40.0 2.252 2 49.9 1.826 3 51.1 1.786 2. ______________________________________

Claim 23

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table H TABLE H ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.6 9.17 100 13.1 6.74 4 14.2 6.26 9 16.0 5.53 10 18.3 4.84 16 20.9 4.26 22 22.1 4.02 3 23.2 3.83 3 25.6 3.48 11 28.4 3.15 2 30.9 2.897 14 32.4 2.767 4 34.4 2.610 2 40.1 2.251 2. ______________________________________

Claim 24

Crystalline aluminophosphates according to claim 1 having a characteristic X-ray powder diffraction pattern which contains at least the d-spacings set forth in Table J TABLE J ______________________________________ 2θ d (Å) 100I/Io ______________________________________ 9.8 9.06 100 13.0 6.79 17 14.2 6.22 15 16.1 5.50 12 21.0 4.24 28 25.6 3.48 9 30.3 2.948 6 31.0 2.887 21 35.1 2.560 4 36.3 2.477 2. ______________________________________