A kind of synthetic method of silicalite-1 molecular sieve

A synthesis method and technology of reaction mixture are applied in the direction of crystalline aluminosilicate zeolite to achieve the effect of complete crystal form and few framework defects

Active Publication Date: 2019-02-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the synthesis of molecular sieve Silicalite-1 reported in the current literature is actually carried out under the guidance of tetrapropylammonium, and no templates with other structures have been used for the synthesis of Silicalite-1.

Method used

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  • A kind of synthetic method of silicalite-1 molecular sieve
  • A kind of synthetic method of silicalite-1 molecular sieve
  • A kind of synthetic method of silicalite-1 molecular sieve

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preparation example Construction

[0026]The invention provides a kind of synthetic method of Silicalite-1 molecular sieve, comprises the following steps:

[0027] (1) Mix the silicon source, structure directing agent, water and optional alkali source evenly to obtain a molar ratio of SiO 2 :R:OH - :H 2 The reaction mixture of O=1: (0.05-0.39): (0.05-2): (2-100), wherein, R represents the molar number of the structure directing agent in the reaction mixture; the structure directing agent is selected from tetraethyl At least one of ammonium hydroxide, tetraethylammonium bromide, tetraethylammonium chloride, tetraethylammonium fluoride, tetraethylammonium iodide and triethylamine;

[0028] (2) By mineralizer: OH - =(1-5): 1 molar ratio, adding a halogen-containing acidic mineralizer or an acidic halogen-containing mineralizer after hydrolysis to the reaction mixture obtained in step (1), after stirring evenly, the mixture Transfer to a pressure-resistant airtight container, and crystallize at a temperature of...

Embodiment 1

[0047] At a stirring speed of 400r / min, according to SiO 2 :R:OH - :H 2 O=1:0.2:0.2:20 molar ratio, mix ethyl orthosilicate, tetraethylammonium hydroxide and deionized water evenly, and hydrolyze at 50°C for 18 hours to obtain clear orthosilicate Hydrolyzed solution of ethyl ester. Under the stirring condition of 600r / min, according to mineralizer: OH - =1:1 molar ratio, add hydrofluoric acid to the mixed solution, stir evenly, transfer the resulting mixture into a closed pressure-resistant container.

[0048] Under the stirring condition of 400r / min, the temperature of the crystallization system was raised to 150°C, and the temperature was kept at autogenous pressure for 6 days to obtain a mixture of crystallized products; the mixture was filtered and washed with water for several times; at a temperature of 110°C Dry for 6 hours, and grind the dried mixture evenly to obtain the raw powder of unroasted Silicalite-1 molecular sieve; finally, roast the raw powder of Silicali...

Embodiment 2

[0050] At a stirring speed of 400r / min, according to SiO 2 :R:OH - :H 2 O=1:0.3:1:30 molar ratio, mix silica gel, tetraethylammonium hydroxide, lithium hydroxide and deionized water uniformly, and hydrolyze at 30°C for 24 hours to obtain a hydrolysis solution of silica gel. Under the stirring condition of 400r / min, according to mineralizer: OH - =1.5:1 molar ratio, add hydrofluoric acid to the mixed solution, stir evenly, transfer the resulting mixture into a closed pressure-resistant container.

[0051] Under the condition of stirring at 300r / min, the temperature of the crystallization system was raised to 135°C, and the temperature was kept at autogenous pressure for 12 days to obtain a mixture of crystallized products; the mixture was filtered and washed with water several times; at a temperature of 130°C Dry for 4 hours, and grind the dried mixture evenly to obtain the raw powder of unroasted Silicalite-1 molecular sieve; finally, roast the raw powder of Silicalite-1 mo...

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Abstract

The invention discloses a synthesis method for a Silicalite-1 molecular sieve, wherein the method comprises the following steps: (1) mixing evenly a silicon source, a structure directing agent and water with an optionally alkali source, to obtain a reaction mixture with the molar ratio of SiO2 to R to OH<-> to H2O of 1 to (0.05-0.39) to (0.05-2) to (2-100), wherein R represents the mole number of the structure directing agent, and the structure directing agent is at least one selected from the group consisting of tetraethylammonium hydroxide, tetraethylammonium bromide, tetraethylammonium chloride, tetraethylammonium fluoride, tetraethylammonium iodide and triethylamine; (2) according to the molar ratio of a mineralization agent to OH<-> of (1-5) to 1, adding the mineralization agent to the reaction mixture obtained in the step (1), stirring evenly, crystallizing for 0.5-60 days at the temperature of 80-200 DEG C and at the self-generated pressure, to obtain a crystallized product; and (3) recycling the crystallized product obtained in the step (2). By the synthesis method, the Silicalite-1 molecular sieve with perfect and uniform crystal grains and fewer skeleton defects can be synthesized under the action of the novel structure directing agent.

Description

technical field [0001] The invention relates to a synthesis method of Silicalite-1 molecular sieve. Background technique [0002] ZSM-5 is a molecular sieve with MFI topology developed by Mobil Corporation in the 1970s. It has a two-dimensional ten-membered ring channel structure, in which the [100] direction is a straight channel with a pore size of 0.51×0.55 nm, and the [010] direction is a sinusoidal channel with a pore size of 0.53×0.56 nm. The Si / Al ratio of ZSM-5 can be changed in the range of silicon-rich and full-silicon, which has good adjustability. [0003] Due to its special two-dimensional ten-membered ring channel structure and acid catalytic performance, ZSM-5 has become one of the most important molecular sieve catalytic materials. At present, ZSM-5 molecular sieve has been widely used in petrochemical, coal chemical and fine chemical fields such as catalytic cracking, alkylation, isomerization and methanol to olefins. Therefore, the synthesis and modifica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 王宝荣朱斌林民彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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