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A kind of method of synthesizing silicalite-1

A synthesis method, a technique for uniform mixing, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, silica, etc.

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 method of synthesizing silicalite-1
  • A kind of method of synthesizing silicalite-1
  • A kind of method of synthesizing silicalite-1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] At a stirring speed of 400r / min, after mixing ethyl orthosilicate, tetraethylammonium hydroxide, sodium hydroxide, sodium fluoride and deionized water evenly, the molar ratio of the mixture obtained is OH - : SiO 2 :R:F:H 2 O=0.5:1:0.2:0.8:15, then the resulting mixture was transferred to a closed pressure vessel.

[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 Silicalite-1 molecular sieve at a temperature of 550 °C for 4 hours to obtain Silicalite-1 molecular sieve powder. 1 molecular sieve, the crystal phase diagram of its X-ray diffraction (XRD) is ...

Embodiment 2

[0050] At a stirring speed of 400r / min, after mixing white carbon black, tetraethylammonium chloride, sodium hydroxide, sodium chloride and deionized water evenly, the molar ratio of the mixture obtained is OH - : SiO 2 :R:F:H 2 O=1.5:1:0.3:2:30, then the resulting mixture was transferred to a closed pressure vessel.

[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 molecular sieve at a temperature of 550 °C for 6 hours to obtain Silicalite-1 molecular sieve powder. 1 molecular sieve, the crystal phase diagram of its X-ray diffraction (XRD) and fi...

Embodiment 3

[0053] At a stirring speed of 400r / min, after mixing the silica sol, tetraethylammonium bromide, sodium hydroxide and deionized water evenly, the molar ratio of the mixture obtained is OH - : SiO 2 :R:F:H 2 O=3:1:0.35:3:50, then the resulting mixture was transferred to a closed pressure vessel.

[0054] Under the stirring condition of 200r / min, the temperature of the crystallization system was raised to 180°C, and the temperature was kept at autogenous pressure for 5 days to obtain a mixture of crystallized products; the mixture was filtered and washed with water for several times; at a temperature of 150°C Dry for 2 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 molecular sieve at a temperature of 650 °C for 8 hours to obtain Silicalite-1 molecular sieve powder. 1 molecular sieve, the crystal phase diagram of its X-ray diffraction (XRD) and figure 1 Similar (to prov...

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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, a mineralizer and water, to obtain a reaction mixture with the molar ratio of OH<->:SiO2:R:F:H2O=(0.05-5):1:(0.05-0.39):(0.05-5):(2-100), wherein R represents the mole number of the structure directing agent, F represents the mole number of the mineralizer, 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) transferring the reaction mixture obtained in the step (1) to a pressureproof airtight container, 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 uniform and perfect crystal grains 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 catalytic cracking, alkylation, isomerization and methanol to olefins and other petrochemical, coal chemical and fine chemical industries. Therefore, the synthesis and mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18C01B39/00
Inventor 林民王宝荣朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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