Phyllosilicate compositions designated CIT-13P and methods of preparing the same
The present disclosure is directed to novel phyllosilicate compositions designated CIT-13P and methods of producing and using the same.
1. A crystalline phyllosilicate designated CIT-13P, comprising delaminated cfi-layers and having a Si:Ge ratio in a range of from about 40 to infinity.
2. The crystalline phyllosilicate of claim 1 that exhibits one or more of:
(a) a major peak in the powder X-ray diffraction (PXRD) pattern in a range of from 6.9 to 9 degrees 2-θ;
(b) a 29 Si and/or an 1 H- 29 Si CP MAS NMR spectrum, as shown in FIGS. 26 (A-B); or
(c) a 29 Si and/or an 1 H- 29 Si CP MAS NMR spectrum with chemical, δ, at −113 ppm, −105 ppm, and −94 ppm, relative to tetramethylsilane (TMS);
or that is prepared by:
(d) treating a germania-rich microporous crystalline germanosilicate of CIT-13 topology having a Si/Ge ratio in a range of from 3.8 to 5.68 with dilute mineral acid at an elevated temperature; or
(e) treating a crystalline microporous germanosilicate of CIT-5 topology having an Si:Ge ratio in a range of from 3.8 to 5.68, with dilute mineral acid at an elevated temperature.
3. A method of preparing the crystalline phyllosilicate of claim 2 , the method comprising treating a crystalline microporous germanosilicate of CIT-13 topology having a Si/Ge ratio in a range of from about 3.8 to about 6.4, with a dilute mineral acid under conditions sufficient to delaminate at least a portion of the CIT-13 germanosilicate.
4. The method of claim 3 , wherein the dilute mineral acid comprises hydrochloric acid, nitric acid, phosphoric acid, and/or sulfuric acid.
5. A method of preparing the crystalline phyllosilicate of claim 2 , the method comprising treating a crystalline microporous germanosilicate of CIT-5 topology having an Si:Ge ratio in a range of from 3.8 to 5.68, with a dilute mineral acid under conditions sufficient to delaminate at least a portion of the CIT-5 germanosilicate.
6. The crystalline phyllosilicate of claim 1 , having a Si:Ge ratio in a range of from about 40 to about 200.
7. The crystalline phyllosilicate of claim 1 that exhibits a major peak in the powder X-ray diffraction (PXRD) pattern in a range of from 6.9 to 9 degrees 2-θ.
8. The crystalline phyllosilicate of claim 1 , that exhibits a major peak in the PXRD pattern either at about 7.2 (±0.2) degrees 2-θ or about 8.2 (±0.2) degrees 2-θ.
9. The crystalline phyllosilicate of claim 1 that exhibits and 29 Si and/or an 1 H- 29 Si CP MAS NMR spectrum as shown in FIGS. 26 (A-B).
10. The crystalline phyllosilicate of claim 1 that exhibits an 29 Si and/or an 1 H- 29 Si CP MAS NMR spectrum with chemical shifts, δ, at −113 ppm, −105 ppm, and −94 ppm, relative to tetramethylsilane (TMS).
11. The crystalline phyllosilicate of claim 1 , prepared by treating a germania-rich microporous crystalline germanosilicate of CIT-13 topology having a Si/Ge ratio in a range of from 3.8 to 5.68 with dilute mineral acid at an elevated temperature, the treating resulting in delamination of the germania-rich microporous crystalline germanosilicate of CIT-13 topology to form the crystalline phyllosilicate designated CIT-13P.
12. The crystalline phyllosilicate CIT-13P of claim 11 , wherein the dilute mineral acid comprises hydrochloric acid, nitric acid, phosphoric acid, and/or sulfuric acid.
13. The crystalline phyllosilicate of claim 1 , prepared by treating a crystalline microporous germanosilicate of CIT-5 topology having an Si:Ge ratio in a range of from 3.8 to 5.68, with dilute mineral acid at an elevated temperature, the treating resulting in the delamination of the microporous germanosilicate composition of CIT-5 topology to form the crystalline phyllosilicate designated CIT-13P.