Method for synthesizing ZSM-48 zeolite through solvent-free solid-phase synthesis
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A ZSM-48, solid-phase synthesis technology, applied in chemical instruments and methods, inorganic chemistry, molecular sieves and alkali exchange compounds, etc., can solve problems such as low synthesis efficiency, limited application, safety hazards, etc. Crystallinity and purity, loss reduction effect
Active Publication Date: 2017-09-12
JIAXING UNIV
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[0003] However, the traditional ZSM-48 zeolite is synthesized in a hydrothermal system, which makes its synthesis efficiency low and there are certain safety hazards
On the other hand, the organic template for the synthesis of ZSM-48 zeolite is mainly hexamethylammonium bromide, which also greatly increases the cost of synthesis and limits its application.
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[0023] Grind 1.6g of solid silica gel, 0.8g of ammonium fluoride, and 1g of organic template (T) in a grinding mill, and then crystallize at 180°C for 4 days to complete the crystallization. The product is suction filtered and dried to obtain ZSM- 48 Zeolite products.
[0024] The molar ratio of the reaction raw materials is as follows: 1SiO 2 :0.8NH 4 F:0.3T
[0025] Through XRD analysis, its structure of the product that obtains is ZSM-48 zeolite ( figure 1 ), and find out by SEM photo, the ZSM-48 zeolite that this method obtains is the morphology of long rod ( figure 2 and image 3 ).
Embodiment 2
[0026] Embodiment 2: Solvent-free solid-phase rapid synthesis of ZSM-48 zeolite
[0027] Put 1.6g of white carbon black, 0.5g of ammonium fluoride, 0.33g of organic template and 0.1g of ZSM-48 seeds in a grinding mill, and then crystallize at 200°C for 1 day to completely crystallize, and the product is suction filtered. After drying, the ZSM-48 zeolite product can be obtained.
[0028] The molar ratio of the reaction raw materials is as follows: 1SiO 2 :0.5NH 4 F:0.1T
Embodiment 3
[0029] Embodiment 3: Solvent-free solid-phase synthesis of aluminum-containing ZSM-48 zeolite
[0030] Grind 1.6g of solid silica gel, 0.2g of boehmite, 1g of ammonium fluoride, and 0.5g of organic template in a grinding mill, and then crystallize at 160°C for 6 days to complete crystallization. The product is suction filtered and dried A ZSM-48 zeolite product is available.
[0031] The molar ratio of the reaction raw materials is as follows: 1SiO 2 :0.8NH 4 F:0.05Al 2 o 3 :0.15T
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Abstract
The invention relates to a molecular sieve preparation technology, and aims at providing a method for synthesizing ZSM-48 zeolite through solvent-free solid-phase synthesis. The method comprises the following steps of using a silicon source, an aluminum source, ammonium fluoride and 4-dimethylamiopryidine used as a template agent into a mortar; performing grinding for 5 min; putting a mixture obtained after the grinding into a reaction kettle; performing crystallization reaction for 1 to 8d at 140 to 200 DEG C; after the reaction is completed, performing suction filtration and drying on the products to obtain the ZSM-48 zeolite. Compared with the prior art, the product obtained through preparation has the advantages that the good crystallinity and purity are maintained; good catalytic reaction activity is realized. No solvent is used in the whole production process; unnecessary loss in the production process is reduced; the yield is greatly improved. The synthesis operation is simple; the implementation is easy; the cost of using the expensive organic template agents is reduced; the important significance is realized in the practical chemical production field.
Description
technical field [0001] The invention belongs to a molecular sieve preparation method, in particular to a solvent-free solid-phase synthesis method of ZSM-48 zeolite under the action of a novel template agent. Background technique [0002] Silica-based zeolite molecular sieve materials are widely used in petrochemical and fine chemical industries. One-dimensional ten-membered ring silica-based zeolite molecular sieves are an important family, and the common ones are ZSM-22, ZSM-48, EU-1 and so on. Among them, the pore size of ZSM-48 zeolite is 0.53nm×0.56nm, which has good thermal and hydrothermal stability and adjustable acidity. Therefore, ZSM-48 zeolite shows excellent catalytic performance in reactions such as shape-selective catalysis, alkylation, and hydroisomerization. [0003] However, the traditional ZSM-48 zeolite is synthesized in a hydrothermal system, which makes its synthesis efficiency low and has certain safety hazards. On the other hand, the organic templa...
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