A method of crystallizing a crystalline molecular sieve having a pore size in the range of from about 2 to about 19 Å, said method comprising the steps of (a) providing a mixture comprising at least one source of ions of tetravalent element (Y), at least one hydroxide source (OH−), and water, said mixture having a solid-content in the range of from about 15 wt. % to about 50 wt. %; and (b) treating said mixture to form the desired crystalline molecular sieve with stirring at crystallization conditions sufficient to obtain a weight hourly throughput from about 0.005 to about 1 hr−1, wherein said crystallization conditions comprise a temperature in the range of from about 200° C. to about 500° C. and a crystallization time less than 100 hr.
Description
DESCRIPTION OF THE FIGURE
FIG. 1 is X-ray diffraction pattern of the crystalline material product of example 2.
FIG. 2 is SEM image of the crystalline material product of example 2.
Claims
1. A method of making a crystalline molecular sieve having a pore size in the range of from about 2 to about 19 Å, said method comprising the steps of:
(a) providing a mixture comprising at least one source of ions of tetravalent element (Y), at least one hydroxide source (OH−), and water, said mixture having a solid-content in the range of from about 15 wt. % to about 50 wt. %; and(b) treating said mixture to form the desired crystalline molecular sieve with stirring at crystallization conditions sufficient to obtain a weight hourly throughput from about 0.005 to about 1 hr−1, wherein said crystallization conditions comprise a temperature in the range of from about 200° C. to about 500° C. and a crystallization time less than 100 hr.
2. The method recited in claim 1, wherein said solid-content range is from about 20 wt. % to about 30 wt. %.
3. The method recited in claim 1, wherein said crystalline molecular sieve formed in step (b) is substantially free of non-crystalline material.
4. The method recited in claim 1, wherein said weight hourly throughput is in the range of from about 0.008 to about 1 hr−1.
5. The method recited in claim 1 wherein the mixture comprises a structure—directing agent (template) for the molecular sieve.
6. The method recited in claim 5, further having a weight hourly template efficiency in the range of from about 0.01 to about 0.5 hr−1.
7. The method recited in claim 1, wherein said temperature range is from about 225° C. to about 250° C.
8. The method recited in claim 1, wherein said mixture further comprises from about 0.01 to 20 wt. % based on the total weight of said mixture of at least one seed source (Seed).
9. The method recited in claim 1, wherein said mixture further comprises from about 0.01 to 10 wt. % based on the total weight of said mixture of at least one seed source (Seed).
10. The method recited in claim 1, wherein said mixture further comprises at least one source of ions of trivalent element.
11. The method recited in claim 10, wherein said trivalent element is aluminum.
12. The method recited in claim 1, wherein said crystallization temperature is in the range of from about 200° C. to about 300° C., and crystallization time is less than 72 hr.
13. The method recited in claim 1, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 48 hr.
14. The method recited in claim 1, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 10 hr.
15. The method recited in claim 1, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 5 hr.
16. The method recited in claim 1, wherein said crystalline molecular sieve has a zeolite framework type comprising at least one of ABW, AEI, AEL, AET, AFI, AFO, CHA, EMT, FAU, FER, LEV, LTA, LTL, MAZ, MEL, MTT, NES, OFF, TON, VFI, MWW, MTW, MFI, MOR, EUO, *BEA, and MFS.
17. The method recited in claim 1, wherein said crystalline molecular sieve comprises at least one of mordenite, MCM-22, MCM-49, MCM-56, ZSM-57, ZSM-5, ZSM-11, ZSM-12, ZSM-22, ZSM-23, ZSM-30, ZSM-48, ZSM-50, ZSM-48, ETS-10, ETAS-10, and ETGS-10.
18. The method recited in claim 1, wherein said tetravalent element is silicon.
19. A process of manufacturing a crystalline molecular sieve having a pore size in the range of from about 2 to about 19 Å, said method comprising the steps of:
(a) providing a mixture comprising at least one source of ions of tetravalent element (Y), at least one hydroxide source (OH−), and water, said mixture having a solid-content in the range of from about 15 wt. % to about 50 wt. %;(b) treating said mixture to form the desired crystalline molecular sieve with stirring at crystallization conditions sufficient to obtain a weight hourly throughput from about 0.005 to about 1 hr−1, wherein said crystallization conditions comprise a temperature in the range of from about 200° C. to about 500° C. and a crystallization time less than 100 hr; and(c) separating said crystalline molecular sieve from said product.
20. The process recited in claim 19, wherein said solid-content range is from about 20 wt. % to about 30 wt. %.
21. The process recited in claim 19, wherein said crystalline molecular sieve formed in step (b) is substantially free of non-crystalline material.
22. The process recited in claim 19, wherein said weight hourly throughput is in the range of from about 0.008 to about 1 hr−1.
23. The process recited in claim 19 wherein the mixture comprises a structure-directing agent (template) for the molecular sieve.
24. The process recited in claim 23, further having a weight hourly template efficiency in the range of from about 0.01 to about 0.5 hr−1.
25. The process recited in claim 19, wherein said mixture further comprises at least one source of ions of trivalent element.
26. The process recited in claim 25, wherein said trivalent element is aluminum.
27. The process recited in claim 19, wherein said temperature range is from about 225° C. to about 250° C.
28. The process recited in claim 19, wherein said mixture further comprises from about 0.01 to 20 wt. % based on the total weight of said mixture of at least one seed source (Seed).
29. The process recited in claim 19, wherein said mixture further comprises from about 0.01 to 10 wt. % based on the total weight of said mixture of at least one seed source (Seed).
30. The process recited in claim 19, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 72 hr.
31. The process recited in claim 19, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 48 hr.
32. The process recited in claim 19, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 10 hr.
33. The process recited in claim 19, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 5 hr.
34. The process recited in claim 19, wherein said crystalline molecular sieve has a zeolite framework type comprising at least one of ABW, AEI, AEL, AET, AFI, AFO, CHA, EMT, FAU, FER, LEV, LTA, LTL, MAZ, MEL, MTT, NES, OFF, TON, VFI, MWW, MTW, MFI, MOR, EUO, *BEA, and MFS.
35. The process recited in claim 19, wherein said crystalline molecular sieve comprises at least one of mordenite, MCM-22, MCM-49, MCM-56, ZSM-57, ZSM-5, ZSM-11, ZSM-12, ZSM-22, ZSM-23, ZSM-30, ZSM-48, ZSM-50, ZSM-48, ETS-10, ETAS-10, and ETGS-10.
36. The process recited in claim 19, wherein said tetravalent element is silicon.
37. A crystalline molecular sieve composition having a pore size in the range of from about 2 to about 19 Å, said crystalline molecular sieve composition made by a process comprising the steps of:
(a) providing a mixture comprising at least one source of ions of tetravalent element (Y), at least one hydroxide source (OH−), and water, said mixture having a solid-content in the range of from about 15 wt. % to about 50 wt. %; and(b) treating said mixture to form the desired crystalline molecular sieve with stirring at crystallization conditions sufficient to obtain a weight hourly throughput from about 0.005 to about 1 hr−1, wherein said crystallization conditions comprise a temperature in the range of from about 200° C. to about 500° C. and a crystallization time less than 100 hr.
38. The crystalline molecular sieve composition recited in claim 37, wherein said solid-content range is from about 20 wt. % to about 30 wt. %.
39. The crystalline molecular sieve composition recited in claim 37, wherein said crystalline molecular sieve is substantially free of non-crystalline material.
40. The crystalline molecular sieve composition recited in claim 37, wherein said weight hourly throughput is in the range of from about 0.008 to about 1 hr−1.
41. The crystalline molecular sieve composition recited in claim 37, further having a weight hourly template efficiency in the range of from about 0.01 to about 0.5 hr−1.
42. The crystalline molecular sieve composition recited in claim 37, wherein said temperature range is from about 225° C. to about 250° C.
43. The crystalline molecular sieve composition recited in claim 37, wherein said mixture further comprises from about 0.01 to 20 wt. % based on the total weight of said mixture at least one seed source (Seed).
44. The crystalline molecular sieve composition recited in claim 37, wherein said mixture further comprises from about 0.01 to 10 wt. % based on the total weight of said mixture at least one seed source (Seed).
45. The crystalline molecular sieve composition recited in claim 37, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 72 hr.
46. The crystalline molecular sieve composition recited in claim 37, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 48 hr.
47. The crystalline molecular sieve composition recited in claim 37, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 10 hr.
48. The crystalline molecular sieve composition recited in claim 37, wherein said crystallization temperature is in the range of from about 200° C. to about 250° C., and crystallization time is less than 5 hr.
49. The crystalline molecular sieve composition recited in claim 37, wherein said crystalline molecular sieve has a zeolite framework type comprising at least one of ABW, AEI, AEL, AET, AFI, AFO, CHA, EMT, FAU, FER, LEV, LTA, LTL, MAZ, MEL, MTT, NES, OFF, TON, VFI, MWW, MTW, MFI, MOR, EUO, *BEA, and MFS.
50. The crystalline molecular sieve composition recited in claim 37, wherein said crystalline molecular sieve comprises at least one of mordenite, MCM-22, MCM-49, MCM-56, ZSM-57, ZSM-5, ZSM-11, ZSM-12, ZSM-22, ZSM-23, ZSM-30, ZSM-48, ZSM-50, ZSM-48, ETS-10, ETAS-10, and ETGS-10.
51. The crystalline molecular sieve composition recited in claim 37 wherein said crystalline molecular sieve comprises at least one trivalent element.
52. The crystalline molecular sieve composition recited in claim 51 wherein the trivalent element is aluminum.
53. The crystalline molecular sieve composition recited in claim 37 wherein said tetravalent element is silicon.
54. A process for converting hydrocarbons comprising the step of contacting said hydrocarbons under conversion conditions with crystalline molecular sieve made by the process of claim 19 or method of claim 21, or the crystalline molecular sieve of claim 37.
Patent Application
20070191660
