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A technology of SAPO-34 and molecular sieve, which is applied in the field of preparation of SAPO-34 molecular sieve to achieve obvious effect of mineralization
Active Publication Date: 2010-07-07
CHNA ENERGY INVESTMENT CORP LTD +1
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For the technology of preparing SAPO-34 molecular sieves using sodium fluoride and potassium fluoride with low toxicity and more obvious mineralization effect as auxiliary templating agent, there is no report yet
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Embodiment 1
[0026] The 85% phosphoric acid of 13.84g, the pseudo-boehmite of 9.86g, the triethylamine of 18.18g, the deionized water of 55.73g, the 40% silica sol of 5.35g and the NaF of 0.152g according to figure 1 The process shown is for preparation, wherein the aging temperature is room temperature, and the aging time is 6 hours; the crystallization temperature is 200°C, and the crystallization time is 48 hours; the calcination temperature is 550°C, and the calcination time is 7 hours. The molar ratio of each component in the resulting mixed solution is: 3.0Et 3 N: 0.06NaF: 0.6SiO 2 : Al 2 O 3 :P 2 O 5 : 60H 2 O.
Embodiment 2
[0028] The 85% phosphoric acid of 17.77g, the pseudo-boehmite of 9.0g, the triethylamine of 25.0g, the deionized water of 36.58g, the 40% silica sol of 11.56g and 0.24gNaF according to figure 1 The process shown is for preparation, wherein the aging temperature is 50°C, and the aging time is 10 hours; the crystallization temperature is 180°C, and the crystallization time is 50 hours; the calcination temperature is 500°C, and the calcination time is 5 hours. The molar ratio of each component in the resulting mixed solution is: 4.5Et 3 N: 0.1NaF: 1.4SiO 2 : Al 2 O 3 : 1.4P2 O 5 : 50H 2 O.
Embodiment 3
[0030] 15.38g of 85% phosphoric acid, 10.96g of pseudo-boehmite, 16.34g of tetraethylammonium hydroxide (30wt%), 13.46g of triethylamine, 74.46g of deionized water, 4.95g of 40 % silica sol and 0.84g NaF according to figure 1 prepared according to the procedures shown. The aging temperature is 80°C, and the aging time is 10 hours; the crystallization temperature is 200°C, and the crystallization time is 72 hours; the calcination temperature is 600°C, and the calcination time is 5 hours. The molar ratio of each component in the obtained mixed solution is: 0.5TEAOH:0.3NaF:2.0Et 3 N: 0.5SiO 2 : Al 2 O 3 :P 2 O 5 : 80H 2 O.
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Abstract
The invention provides a method for preparing a SAPO-34 molecular sieve. The method comprises the following steps of: 1, uniformly mixing a proper amount of phosphorus source, aluminum source, silicon source, template, auxiliary template and water at a proper temperature and under a stirring condition to obtain mixed solution, of which a molar ratio of all components, namely, the molar ratio of R to F- to SiO2 to Al2O3 to P2O5 to H2O, is a:b:c:1:d:e, wherein R represents the template, a is 0.2 to 5.0, b is 0 to 1.0, c is 0.2 to 1.5, d is 0.2 to 2.0 and e is 20 to 200; 2, ageing the mixed solution; and putting the aged mixed solution in a crystallization kettle, sealing the crystallization kettle, heating the mixed solution to a crystallization temperature, and crystallizing the mixed solution at the constant crystallization temperature; 3, performing centrifugal separation of the crystallized mixed solution, filtering, washing the mixed solution until a pH value of the mixed solution is 7 to 8, and drying a solid sample to obtain the SAPO-34 raw powder; and 4, baking the SAPO-34 raw powder at the temperature of between 450 and 650 DEG C for 4 to 8 hours to obtain the SAPO-34 molecular sieve. The SAPO-34 molecular sieve prepared by the method is characterized by high crystallinity and can show better low carbon olefin selectivity in an MTO reaction.
Description
technical field [0001] The invention relates to a preparation method of SAPO-34 molecular sieve, more specifically, relates to a method for preparing SAPO-34 molecular sieve by using fluoride as an auxiliary template agent. Background technique [0002] SAPO-n molecular sieve is a new series of silicoaluminophosphate molecular sieves (USP 4440871, USP 4499327) researched and developed by Union Carbide Corporation (UCC) in 1984. The sol is an aluminum source, a phosphorus source and a silicon source, and is obtained by first obtaining an organic amine / aluminum phosphate / silicon complex with a microporous phase by hydrothermal crystallization, and then removing the template (organic amine) by roasting. At present, SAPO molecular sieves have been reported to have 13 three-dimensional microporous framework structures, and SAPO-34 is one of them. Its structure is similar to chabazite, with three-dimensional intersecting channels, and the pore diameter is about 0.38nm. It belongs ...
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