Material ITQ-55, method for preparation and use
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C01B-039/48
C01B-037/02
B01J-020/18
B01J-029/70
B01D-071/02
B01D-053/04
B01D-053/047
C01B-003/50
B01D-053/02
B01D-053/22
C01B-017/16
C01B-021/04
C01C-001/12
B01J-020/30
C07C-001/20
C07C-001/32
C07C-002/76
C07C-029/00
C07C-041/01
C01B-039/06
C01B-039/08
C01B-037/00
C01B-039/12
B01J-029/89
B01J-029/86
출원번호
US-0744169
(2015-06-19)
등록번호
US-9856145
(2018-01-02)
발명자
/ 주소
Corma Canos, Avelino
Rey Garcia, Fernando
Valencia Valencia, Susana
Cantin Sanz, Angel
Jordá Moret, Jose Luis
출원인 / 주소
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
대리인 / 주소
Ward, Andrew T.
인용정보
피인용 횟수 :
0인용 특허 :
17
초록▼
This invention refers to a microporous crystalline material of zeolitic nature that has, in its calcined state and in the absence of defects in its crystalline matrix manifested by the presence of silanols, the empirical formula x(M1/nXO2):yYO2:gGeO2:(1-g)SiO2in whichM is selected between H+, at lea
This invention refers to a microporous crystalline material of zeolitic nature that has, in its calcined state and in the absence of defects in its crystalline matrix manifested by the presence of silanols, the empirical formula x(M1/nXO2):yYO2:gGeO2:(1-g)SiO2in whichM is selected between H+, at least one inorganic cation of charge +n, and a mixture of both,X is at least one chemical element of oxidation state +3,Y is at least one chemical element with oxidation state +4 different from Si,x takes a value between 0 and 0.2, both included,y takes a value between 0 and 0.1, both included,g takes a value between 0 and 0.5, both includedthat has been denoted ITQ-55, a method for its preparation and its use.
대표청구항▼
1. A microporous crystalline material of zeolitic nature having, in calcined state and in absence of defects in its crystalline matrix manifested by the presence of silanols, the empiric formula x(M1/nXO2):yYO2:gGeO2:(1-g)SiO2 in whichM is selected between H+, at least one inorganic cation of charge
1. A microporous crystalline material of zeolitic nature having, in calcined state and in absence of defects in its crystalline matrix manifested by the presence of silanols, the empiric formula x(M1/nXO2):yYO2:gGeO2:(1-g)SiO2 in whichM is selected between H+, at least one inorganic cation of charge +n, and a mixture of both,X is at least one chemical element of oxidation state +3,Y is at least one chemical element with oxidation state +4 different from Si,x takes a value between 0 and 0.2, both included,y takes a value between 0 and 0.1, both included,g takes a value between 0 and 0.5, both included,and wherein the material, as synthesized, has an X-ray diffraction pattern with, at least, the angle values 2θ (degrees) and relative intensities (I/I0): 2θ (degrees) ± 0.5Intensity (I/I0)5.8w7.7w8.9w9.3mf9.9w10.1w13.2m13.4w14.7w15.1m15.4w15.5w17.4m17.7m19.9m20.6m21.2f21.6f22.0f23.1mf24.4m27.0mwhere I0 is the intensity from the most intense peak to which is assigned a value of 100w is a weak relative intensity between 0 and 20%,m is an average relative intensity between 20 and 40%,f is a strong relative intensity between 40 and 60%,and mf is a very strong relative intensity between 60 and 100%. 2. A microporous crystalline material of zeolitic nature according to claim 1, wherein X is selected from the group consisting of Al, Ga, B, Fe, Cr and mixtures thereof. 3. A microporous crystalline material of zeolitic nature according to claim 1, wherein Y is selected from the group consisting of Zr, Ti, Sn, V and mixtures thereof. 4. A microporous crystalline material of zeolitic nature according to claim 1, wherein M is selected among H+, at least one inorganic cation of charge +n selected from the group consisting of alkaline, alkaline-earth metals and combinations thereof. 5. A microporous crystalline material of zeolitic nature according to claim 1, wherein “x” is 0, “y” is 0, and “g” is 0. 6. A microporous crystalline material of zeolitic nature according to claim 1, wherein “x” is 0, “y” is 0 and “g” is different from 0. 7. A microporous crystalline material of zeolitic nature according to claim 1, wherein: X is selected from the group consisting of Al, Ga, B, Fe, Cr, and combinations of the same,y takes the value 0, andg takes the value 0. 8. A microporous crystalline material of zeolitic nature according to claim 1, wherein: Y is selected from the group consisting of Ti, Zr, Sn and combinations thereofx takes the value 0, andg takes the value 0. 9. A microporous crystalline material of zeolitic nature according to claim 1, wherein: X is selected from the group consisting of Al, Ga, B, Fe, Cr, and combinations thereof,Y is selected from the group consisting of Ti, Zr, Sn, and combinations thereof andg takes the value 0. 10. A microporous crystalline material of zeolitic nature according to claim 1, wherein: Y is selected from the group consisting of Ti, Zr, Sn, and combinations thereof,x takes the value 0, andg takes a value different from 0 and less than 0.33. 11. A microporous crystalline material of zeolitic nature according to claim 1, wherein, in calcined state, it has an X-ray diffraction pattern with, at least, the angle values 2θ (degrees) and relative intensities (I/I0): 2θ (degrees) ± 0.5Intensity (I/I0)6.2w7.8w8.0w9.8mf10.0m10.3w12.3w13.4w13.7w15.0w15.2w16.8w18.1w20.1w21.3w23.5w23.9w26.8wwherew is a weak relative intensity between 0 and 20%,m is an medium relative intensity between 20 and 40%,f is a strong relative intensity between 40 and 60%, andmf it is a very strong relative intensity between 60 and 100%. 12. A microporous crystalline material of zeolitic nature according to claim 1 or 11, wherein: X is selected from the group consisting of Al, Ga, B, Fe, Cr, and combinations thereof,y takes the value 0, andg takes a value different from 0 and less than 0.33. 13. A microporous crystalline material of zeolitic nature according to claim 1 or 11, wherein: X is selected from the group consisting of Al, Ga, B, Fe, Cr, and combinations thereof,Y is selected from the group consisting of Ti, Zr Sn, and combinations thereofg takes a value different from 0 and less than 0.33. 14. A microporous crystalline material of zeolitic nature according to claim 1 or 11 having a framework of tetrahedral (T) atoms connected by bridging atoms, wherein the tetrahedral atom is defined by connecting the nearest T atoms in the manner described in the following Table: ITQ-55 tetrahedral atom interconnectionsT atomConnected to:T1T6, T7, T55, T73T2T3, T5, T9, T56T3T2, T7, T21, T27T4T8, T9, T58, T73T5T2, T8, T52, T59T6T1, T8, T53, T60T7T1, T3, T50, T61T8T4, T5, T6, T51T9T2, T4, T21, T63T10T15, T16, T64, T74T11T12, T14, T18, T65T12T11, T16, T30, T36T13T17, T18, T67, T74T14T11, T17, T43, T68T15T10, T17, T44, T69T16T10, T12, T41, T70T17T13, T14, T15, T42T18T11, T13, T30, T72T19T24, T25, T37, T73T20T21, T23, T27, T38T21T3, T9, T20, T25T22T26, T27, T40, T73T23T20, T26, T41, T70T24T19, T26, T42, T71T25T19, T21, T43, T68T26T22, T23, T24, T69T27T3, T20, T22, T45T28T33, T34, T46, T74T29T30, T32, T36, T47T30T12, T18, T29, T34T31T35, T36, T49, T74T32T29, T35, T50, T61T33T28, T35, T51, T62T34T28, T30, T52, T59T35T31, T32, T33, T60T36T12, T29, T31, T54T37T19, T42, T43, T75T38T20, T39, T41, T45T39T38, T43, T57, T63T40T22, T44, T45, T75T41T16, T23, T38, T44T42T17, T24, T37, T44T43T14, T25, T37, T39T44T15, T40, T41, T42T45T27, T38, T40, T57T46T28, T51, T52, T76T47T29, T48, T50, T54T48T47, T52, T66, T72T49T31, T53, T54, T76T50T7, T32, T47, T53T51T8, T33, T46, T53T52T5, T34, T46, T48T53T6, T49, T50, T51T54T36, T47, T49, T66T55T1, T60, T61, T75T56T2, T57, T59, T63T57T39, T45, T56, T61T58T4, T62, T63, T75T59T5, T34, T56, T62T60T6, T35, T55, T62T61T7, T32, T55, T57T62T33, T58, T59, T60T63T9, T39, T56, T58T64T10, T69, T70, T76T65T11, T66, T68, T72T66T48, T54, T65, T70T67T13, T71, T72, T76T68T14, T25, T65, T71T69T15, T26, T64, T71T70T16, T23, T64, T66T71T24, T67, T68, T69T72T18, T48, T65, T67T73T1, T4, T19, T22T74T10, T13, T28, T31T75T37, T40, T55, T58T76T46, T49, T64, T67. 15. A method to synthesize the microporous crystalline material of claim 1 by forming a reaction mixture comprising: one or several sources of SiO2 one or several sources of organic cation R,at least one source of anions selected from the group consisting of hydroxide anions, fluoride anions and the combinations thereof, and waterheating to a temperature between 80 and 200° C., and the reaction mixture having a composition, in terms of molar ratios, comprised between the intervalsR+/SiO2=0.01-1.0OH−/SiO2=0-3.0F−/SiO2=0-3.0(F−+OH−)/SiO2=0.01-3.0,H2O/SiO2=1-50. 16. A method according to claim 15, wherein the reaction mixture also includes, at least, one source of one or more trivalent X elements. 17. A method according to claim 15, wherein the reaction mixture also includes, at least one source of other tetravalent elements Y, different from Si and Ge. 18. A method according to claim 15, wherein the source of organic cation R is N2,N2,N2,N5,N5,N5,3a,6a-octamethyloctahydropentalene-2,5-diammonium. 19. A method according to claim 18, wherein the organic cation R is added in selected form the group consisting of hydroxide, another salt and a hydroxide mixture and another salt. 20. A method according to claim 15, wherein a quantity is added to the reaction mixture of the microporous crystalline material as promoter of the crystallization, in a quantity between 0.01 and 20% by weight with regard to the total of inorganic oxides added. 21. A method according to claim 15, wherein the reaction mixture includes one or more sources of GeO2 and having a composition, in terms of molar ratios, between the intervals GeO2/SiO2=0 and 0.5R+/(SiO2+GeO2)=0.01-1.0,F−/(SiO2+GeO2)=0.0-3.0,OH−/(SiO2+GeO2)=0.0-3.0,(F−+OH−)/(SiO2+GeO2)=0.01-3.0H2O/(SiO2+GeO2)=1-50. 22. A method according to the claim 15 or 21, wherein the anion is fluoride and having a composition, in terms of molar ratios, between the intervals GeO2/SiO2=0 and 0.5R+/(SiO2+GeO2)=0.01-1.0,F−/(SiO2+GeO2)=0.01-3.0,H2O/(SiO2+GeO2)=1-50. 23. A method according to the claim 15 or 21, wherein the anion is hydroxide and having a composition, in terms of molar ratios, between the intervals GeO2/SiO2=0 and 0.5,R+/(SiO2+GeO2)=0.01-1.0,OH−/(SiO2+GeO2)=0.01-3.0,H2O/(SiO2+GeO2)=1-50. 24. A microporous crystalline material of zeolitic nature having a framework of tetrahedral (T) atoms connected by bridging atoms, wherein the tetrahedral atom is defined by connecting the nearest T atoms in the manner described in the following Table: ITQ-55 tetrahedral atom interconnectionsT atomConnected to:T1T6, T7, T55, T73T2T3, T5, T9, T56T3T2, T7, T21, T27T4T8, T9, T58, T73T5T2, T8, T52, T59T6T1, T8, T53, T60T7T1, T3, T50, T61T8T4, T5, T6, T51T9T2, T4, T21, T63T10T15, T16, T64, T74T11T12, T14, T18, T65T12T11, T16, T30, T36T13T17, T18, T67, T74T14T11, T17, T43, T68T15T10, T17, T44, T69T16T10, T12, T41, T70T17T13, T14, T15, T42T18T11, T13, T30, T72T19T24, T25, T37, T73T20T21, T23, T27, T38T21T3, T9, T20, T25T22T26, T27, T40, T73T23T20, T26, T41, T70T24T19, T26, T42, T71T25T19, T21, T43, T68T26T22, T23, T24, T69T27T3, T20, T22, T45T28T33, T34, T46, T74T29T30, T32, T36, T47T30T12, T18, T29, T34T31T35, T36, T49, T74T32T29, T35, T50, T61T33T28, T35, T51, T62T34T28, T30, T52, T59T35T31, T32, T33, T60T36T12, T29, T31, T54T37T19, T42, T43, T75T38T20, T39, T41, T45T39T38, T43, T57, T63T40T22, T44, T45, T75T41T16, T23, T38, T44T42T17, T24, T37, T44T43T14, T25, T37, T39T44T15, T40, T41, T42T45T27, T38, T40, T57T46T28, T51, T52, T76T47T29, T48, T50, T54T48T47, T52, T66, T72T49T31, T53, T54, T76T50T7, T32, T47, T53T51T8, T33, T46, T53T52T5, T34, T46, T48T53T6, T49, T50, T51T54T36, T47, T49, T66T55T1, T60, T61, T75T56T2, T57, T59, T63T57T39, T45, T56, T61T58T4, T62, T63, T75T59T5, T34, T56, T62T60T6, T35, T55, T62T61T7, T32, T55, T57T62T33, T58, T59, T60T63T9, T39, T56, T58T64T10, T69, T70, T76T65T11, T66, T68, T72T66T48, T54, T65, T70T67T13, T71, T72, T76T68T14, T25, T65, T71T69T15, T26, T64, T71T70T16, T23, T64, T66T71T24, T67, T68, T69T72T18, T48, T65, T67T73T1, T4, T19, T22T74T10, T13, T28, T31T75T37, T40, T55, T58T76T46, T49, T64, T67. 25. A microporous crystalline material of zeolitic nature according to claim 24, wherein the material, as synthesized, has an X-ray diffraction pattern with, at least, the angle values 2θ (degrees) and relative intensities (I/I0): 2θ (degrees) ± 0.5Intensity (I/I0)5.8w7.7w8.9w9.3mf9.9w10.1w13.2m13.4w14.7w15.1m15.4w15.5w17.4m17.7m19.9m20.6m21.2f21.6f22.0f23.1mf24.4m27.0mwhere I0 is the intensity from the most intense peak to which is assigned a value of 100w is a weak relative intensity between 0 and 20%,m is an average relative intensity between 20 and 40%,f is a strong relative intensity between 40 and 60%,and mf is a very strong relative intensity between 60 and 100%.
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