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Halide-free process for the synthesis of ETS-10
| Details |
Inventors: Blosser, Patrick W.; Kuznicki, Steven M.;
Assignee: Engelhard Corporation (Iselin, NJ)
Primary Examiner: Bell; Mark L.
Assistant Examiner: Samae; David
Attorney, Agent or Firm:
A novel process for the preparation of a crystalline titanium molecular sieve zeolite identified as ETS-10 characterized by crystals of uniform morphology which is free from halide-containing reactants is disclosed. |
|
DETAILED DESCRIPTION OF THE INVENTION The present invention is directed towards crystalline titanium molecular sieve zeolites which have a pore size of approximately 8 Angstrom units and have a titania-to-silica mole ratio in the range of from 2.
5 to 25.
ETS-10 molecular sieves are disclosed and claimed in U.
S.
Pat.
No.
4,853,202, the entire disclosure of which is incorporated herein by reference, and have a crystalline structure and an X-ray powder diffraction pattern having the following significant lines:
TABLE 1
______________________________________
XRD Powder Pattern of ETS-10 (0-40.
degree.
theta)
Significant d-Spacing (Angs.
)
I/I.
sub.
o
______________________________________
14.
7 .
+-.
.
35 W-M
7.
20 .
+-.
.
15 W-M
4.
41 .
+-.
.
10 W-M
3.
60 .
+-.
.
05 VS
3.
28 .
+-.
.
05 W-M
______________________________________
In the above table: VS=60-100 S=40-60 M=20-40 W=5-20 The above values were determined by standard techniques.
The radiation was the K-alpha doublet of copper, and a scintillation counter spectrometer was used.
The peak heights, I, and the positions as a function of 2 times theta, where theta is the Bragg angle, were read from the spectrometer chart.
From these, the relative intensities, 100 I/I.
sub.
o, where I.
sub.
o is the intensity of the strongest line or peak, and d (obs.
), the interplanar spacing in A, corresponding to the recorded lines, were calculated.
It should be understood that this X-ray diffraction pattern is characteristic of all the species of ETS compositions.
Ion exchange of the sodium ions and potassium ions with cations reveals substantially the same pattern with some minor shifts in interplanar spacing and variation in relative intensity.
Other minor variations can occur depending on the silicon to titanium ratio of the particular sample, as well as if it had been subjected to thermal treatment.
Various cation exchanged forms of ETS have been prepared and their X-ray powder diffraction patterns contain the most significant lines set forth in Table 1
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