Preparation method of ITQ-13 molecular sieve in non-concentrated-gel system
A molecular sieve and non-condensing technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of increased synthesis cost, poor repeatability, high cost, etc., and achieve the effects of reduced loss, good crystallinity and purity, and low price
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[0033] Example 1:
[0034] First, pipette 1.5mL deionized water and 3.0mL TMHDA, mix them evenly, add 0.104g GeO to them 2 , 0.20mL ethyl orthosilicate (TEOS), add 0.12mL hydrofluoric acid (40wt%) under stirring, continue stirring until a uniform silicon germanium gel is formed, and then transfer to a polytetrafluoroethylene reactor at 180°C Under the conditions of static crystallization for 7 days. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA: 42H 2 O: 1.4HF. After the reaction kettle is cooled to room temperature, the product is suction filtered, washed with water 4 times, and dried at 85° C., product 1 can be obtained. The BET specific surface area of product 1 measured by nitrogen adsorption is 296.87m 2 / g, the pore volume of the micropore is 0.126mL / g, and the pore diameter is
[0035] The XRD spectrum of product 1 is as follows figure 1 . It can be seen that product 1 has a typical ITH molecular sieve structure and has a high degree of crystallinit...
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[0037] Example 2:
[0038] Mix 1.5mL deionized water and 3.0mL TMHDA evenly, add 0.104g GeO to it 2 , 0.22mL silica sol, add 0.12mL hydrofluoric acid (40wt%) under stirring, continue stirring until a uniform silicon-germanium gel is formed, then transfer it to a polytetrafluoroethylene reactor, and statically crystallize at 180℃. day. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA: 42H 2 O: 1.4HF. After the reaction kettle is cooled to room temperature, the product is suction filtered, washed with water 4 times, and dried at 85° C., product 2 can be obtained.
[0039] The XRD spectrum of product 2 is as follows image 3 . The baseline of product 2 is relatively flat, indicating that product 2 has high crystallinity.
[0040] SEM of product 2 such as Figure 4 . Product 2 has a typical bar-shaped crystal morphology, with a size of about 20-30 μm.
Example Embodiment
[0041] Example 3:
[0042] Measure 1.5mL deionized water and 3.0mL TMHDA, mix well and add 0.104g GeO 2 , 0.20mL TEOS, add 0.15g ammonium fluoride under stirring, continue stirring until a uniform silicon-germanium gel is formed, then transfer to a polytetrafluoroethylene reactor, and statically crystallize at 180°C for 7 days. The ratio of reaction raw materials is 0.5SiO 2 :0.5GeO 2 :7TMHDA:42H 2 O: 1.4NH 4 F. After the reaction kettle is cooled to room temperature, the product is filtered off with suction, washed with water 4 times, and dried at 85°C to obtain product 3.
[0043] The XRD spectrum of product 3 is as follows Figure 5 . The baseline of product 3 is relatively flat, indicating that product 3 has high crystallinity.
[0044] SEM of product 3 such as Image 6 . Product 3 has a bar-shaped crystal morphology with a size of about 20-30 μm.
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