One-step synthesizing method for hollow type multilevel-hole Fe-Silicalite-1

A multi-level porous and hollow technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of few, high cost, complicated process, etc., and achieve the effects of slowing down side reactions, large carbon capacity, and simple synthesis process.

Active Publication Date: 2014-10-15
CHAMBROAD CHEM IND RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are not many reports on the synthesis of hierarchically porous Fe-Silicalite-1 zeolite, and the alkali treatment method or soft and hard template method is mainly used, which is not only complicated in process, but also high in cost.
One-step synthesis of hollow hierarchically porous Fe-Silicalite-1 zeolites without the addition of soft templates such as organosilicon has not been reported yet

Method used

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  • One-step synthesizing method for hollow type multilevel-hole Fe-Silicalite-1
  • One-step synthesizing method for hollow type multilevel-hole Fe-Silicalite-1
  • One-step synthesizing method for hollow type multilevel-hole Fe-Silicalite-1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 15.4 mL of ethyl orthosilicate to 16.5 mL of tetrapropylammonium hydroxide aqueous solution (1.14 mol / L), stir at room temperature for 3 h, add 0.71 g of ferric citrate and 33 mL of water, continue stirring for 2 h, and then add crystal Crystallize at 170°C for 3 days in a furnace, centrifuge, wash, dry overnight at 100°C, and roast at 540°C for 6 hours to obtain Fe-Silicalite-1. Raw materials used, in terms of molar ratio of pure substances, SiO in silicon source 2 : Fe in iron source 2 o 3 : TPA in the templating agent + : OH in alkali source - :H 2 O=1:0.021:0.27:0.27:37;

[0032] figure 1 is the XRD pattern of the sample, it can be seen from the figure that the sample has an MFI structure;

[0033] figure 2 It is the SEM picture of the sample. It can be seen from the picture that the particle size of the sample is uniform, and it is a small grain aggregate of about 400nm;

[0034] image 3 It is the TEM picture of the sample. It can be seen from the f...

Embodiment 2

[0038] Add 15.4mL tetrapropylammonium hydroxide aqueous solution (1.14mol / L) to 15.4mL tetrapropylammonium hydroxide aqueous solution (1.14mol / L), stir at room temperature for 3h, add 1.01g ferric citrate and 33mL water, continue to stir for 2h, and then add crystal Crystallize at 80°C for 5 days in a furnace, centrifuge, wash, dry overnight at 100°C, and roast at 540°C for 6 hours to obtain Fe-Silicalite-1. Raw materials used, in terms of molar ratio of pure substances, SiO in silicon source 2 : Fe in iron source 2 o 3 : TPA in the templating agent + : OH in alkali source - :H 2 O=1:0.03:0.27:0.27:37.

Embodiment 3

[0040]Add 15.4 mL of ethyl orthosilicate to 16.5 mL of an aqueous solution of tetrapropylammonium hydroxide (1.14 mol / L), stir at room temperature for 3 h, add 0.10 g of ferric citrate and 33 mL of water, continue stirring for 2 h, and then add crystal Crystallize at 200°C for 1 day in a furnace, centrifuge, wash, dry overnight at 100°C, and roast at 540°C for 6 hours to obtain Fe-Silicalite-1. Raw materials used, in terms of molar ratio of pure substances, SiO in silicon source 2 : Fe in iron source 2 o 3 : TPA in the templating agent + : OH in alkali source - :H 2 O=1:0.003:0.27:0.27:37.

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Abstract

The invention provides a one-step synthesizing method for hollow type multilevel-hole Fe-Silicalite-1 zeolite and application thereof. The method adopts a silicon source, an organic iron source, an alkali source, a template agent and water as raw materials, and the raw materials are crystallized in a crystallization kettle, and then subjected to centrifugal separation, washing, drying and calcinating for preparing the hollow type Fe-Silicalite-1 zeolite with distributed micropores and mesoporouses . The synthesis technology is simple, and requires no multistep operation and no additional expensive additive; through adjusting the types of the iron source, the appearance and the pore size distribution of the Fe-Silicalite-1 zeolite are adjusted effectively; when used for catalyzing a methanol-to-propylene reaction, the Fe-Silicalite-1 zeolite synthesized through the invention is higher in propylene selectivity and methanol conversion rate, and longer in the service life of a catalyst.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical synthesis, and relates to a preparation method and application of an iron-silicon molecular sieve, in particular to a method and application of one-step synthesis of hollow multi-level porous Fe-Silicalite-1 zeolite. Background technique [0002] As an important chemical raw material, propylene is widely used in the production process of polypropylene, propylene oxide, acrylonitrile and other chemical products. At present, propylene is mainly obtained from petroleum raw materials through steam cracking or catalytic cracking. However, my country is a country with severe shortage of petroleum resources, which makes it necessary to develop new propylene production processes. Methanol to propylene (MTP) technology has attracted more and more attention because it can use abundant coal or natural gas to produce propylene through methanol. [0003] ZSM-5 zeolite molecular sieve has become the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 牟庆平郭新闻侯晓峰代成义栾波刘民张安峰姚刚
Owner CHAMBROAD CHEM IND RES INST CO LTD
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