Method for preparing DD3R molecular sieve
A molecular sieve and seed crystal technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long synthesis time, difficult DD3R synthesis, and poor repeatability.
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Embodiment 1
[0048] In this example, DD3R molecular sieve seed crystals were synthesized by microwave at 160° C. for 3 days.
[0049] After mixing 4.88 g of ethylenediamine with 1.51 g of amantadine, 34.2 g of H 2 O stirred for about 0.5 hour, then slowly added dropwise 3 grams of silica sol (SiO in silica sol 2 The content is 40wt%), stirred for 24 hours. Microwave synthesis at 160°C for 3 days. After the product is taken out, it is washed with deionized water, centrifuged, and dried to obtain DD3R molecular sieve crystals. SiO in the silicon source described in this embodiment 2 The molar ratio of water, amantadine and ethylenediamine is 1:95:0.5:4.065.
[0050] figure 1 It is a scanning electron micrograph of DD3R molecular sieve crystals. The DD3R molecular sieve crystals are rhombohedral crystals of about 5 microns, and the crystal size is relatively uniform. Compared with the traditional DD3R synthesis method, the microwave synthesis time is shortened from 25 to 48 days to 3 da...
Embodiment 2
[0053] In this example, DD3R molecular sieves were synthesized by adding 0.046wt% molecular sieve crystals as in Example 1 as seed crystals and microwaved at 160° C. for 3 hours.
[0054] Step 1: Grind the DD3R molecular sieve crystal synthesized in Example 1 with a ball mill, the ball milling speed is 300 rpm, and the ball milling time is 6 hours; grind the DD3R molecular sieve crystal until the molecular sieve crystal particle size is 2-8 microns .
[0055] Step 2: 4.88 grams of ethylenediamine, 1.51 grams of amantadine and 34.2 grams of water were mixed and stirred for 0.5 hour, and 3 grams of silica sol (SiO in silica sol) were added. 2 content of 40wt%), stirred and aged for 24 hours, then added 20 mg of ground DD3R seed crystals obtained in step 1, stirred for 5 minutes, synthesized by microwave at 160° C. for 3 hours, centrifuged and washed to obtain DD3R molecular sieves.
[0056] image 3 and Figure 4 are the scanning electron microscope and XRD patterns of the gr...
Embodiment 3
[0060] In this example, DD3R molecular sieves were synthesized by adding 0.046 wt% molecular sieve crystals in Example 1 as seed crystals and microwaved at 160° C. for 6 hours.
[0061] The difference from Example 2 is that in step 2, microwave synthesis was performed at 160° C. for 6 hours. All the other steps are the same as in Example 2.
[0062] Figure 7 Scanning electron micrographs of DD3R molecular sieves synthesized by this method. It can be seen from the figure that the particle size of DD3R molecular sieve is uniform, and the particle size is about 1 μm. At the same time, the crystallinity is good, and compared with 3 hours of synthesis, the crystallinity is greatly improved. The yield is calculated based on the silicon dioxide added to the mother liquor, which is close to 100%.
[0063] Figure 8 The XRD spectrum of the DD3R molecular sieve synthesized by this method is consistent with the standard spectrum.
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