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Synthetic method of molecular sieve ZSM-5 (zeolite socony mobil-5) with heteroatom-containing frame

A ZSM-5, synthesis method technology, applied in the directions of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of complex synthesis of molecular sieves and low yield, etc. Good technical effect, easy to synthesize effect

Active Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention mainly solves the problems in the prior art that the synthesis of ZSM-5 molecular sieves containing heteroatoms in the framework is complicated and the yield is low

Method used

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  • Synthetic method of molecular sieve ZSM-5 (zeolite socony mobil-5) with heteroatom-containing frame
  • Synthetic method of molecular sieve ZSM-5 (zeolite socony mobil-5) with heteroatom-containing frame

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Effect test

Embodiment 1

[0021] Dissolve 9.0 g of aluminum sulfate octadecahydrate, 2.0 g of ferric sulfate, 20.0 g of water, and 1.0 g of sulfuric acid to form a solution. 120.0 grams of water glass (containing 21% silicon dioxide, 6.5%) will be weighed. The above two materials are strongly stirred to form a gel. Dry at 50° C. for 150 hours to obtain a solid dry glue. Take 10.0 g of dry glue and put it into the upper part of the crystallization kettle, add 500.0 g of water to the lower part of the crystallization kettle, and add 1.5 g of tetrapropylammonium bromide to the top of the dry glue. Crystallize under airtight conditions at 140°C for 90 hours to obtain Fe-AlZSM-5 molecular sieves. For XRD and IR characterization results see figure 1 , figure 2 .

Embodiment 2

[0023] Dissolve 6.0 g of aluminum sulfate octadecahydrate, 1.0 g of ammonium vanadate, and 20.0 g of water to form a solution. Mix 50.0 g of silica sol (containing 40% silicon dioxide) and 5.0 g of sodium hydroxide. The above two materials were vigorously stirred to form a gel, and the pH of the mixture was 9. Spin-dry at 200° C. for 0.5 hour to obtain a solid dried gel. Take 20.0 g of dry glue and put it into the upper part of the crystallization kettle, add 10.0 grams of water in the crystallization kettle, and add 4.0 grams of tetrapropylammonium hydroxide aqueous solution (containing 30%) on the dry glue. Crystallize at 150°C for 60 hours under airtight conditions. Obtained V-AlZSM-5 molecular sieve.

Embodiment 3

[0025] Dissolve 0.6 g of germanium nitrate, 20.0 g of water, and 0.5 g of nitric acid to prepare a solution. 120.0 g of silica sol (containing 40% silicon dioxide by weight concentration) and 7.0 g of potassium hydroxide will be weighed. The above two materials are strongly stirred to form a gel. The pH value of the mixture was 9, and it was dried at 50°C for 2 hours and then at 120°C for 6 hours to obtain a solid dry gel. Take 20.0 g of dry glue and put it into the upper part of the crystallization kettle, add 600.0 grams of water in the crystallization kettle, and add 2.0 grams of tetrapropylammonium hydroxide aqueous solution (containing 30%) on the dry glue. Crystallize at 150°C for 90 hours under airtight conditions. Ge-ZSM-5 molecular sieves were obtained.

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Abstract

The invention relates to a synthetic method of a molecular sieve ZSM-5 (zeolite socony mobil-5) with a heteroatom-containing frame and mainly solves the problem that the molecular sieve ZSM-5 with the heteroatom-containing frame is hard to synthetize and low in yield in the prior art. Silicon source, aluminum source, heteroatom metal salt and water are mixed well and are dried at 50-200 DEG C for 0.5-150h to obtain dry glue; the dry glue is placed on the inner upper portion of a crystallization furnace, water or template is added into the lower portion of the crystallization furnace, crystallization is allowed at 100-250 DEG C for 4-150h after closing; after crystallization, crystallization product is washed, dried and roasted to obtain the molecular sieve ZSM-5 with the heteroatom-containing frame. The problem is solved well by the application of the technical scheme. The synthetic method is applied to industrial production of the molecular sieve with the heteroatom-containing frame.

Description

technical field [0001] The invention relates to a method for synthesizing ZSM-5 molecular sieves containing heteroatoms in the framework. Background technique [0002] Microporous zeolite molecular sieve is an inorganic silicon-containing crystal. Its skeleton has regular and orderly arranged pores with similar molecular size. It is widely used in the fields of catalysis, ion exchange and separation, especially ZSM-5 molecular sieve. ZSM-5 zeolite has a channel system composed of 10-membered rings and has three-dimensional channels. In the early 1970s, US Patent USP3702866 disclosed the synthesis method of ZSM-5 molecular sieve. Since then, ZSM-5 molecular sieves have been widely used in reactions such as alkylation, isomerization, disproportionation, selective cracking, and synthesis of gasoline from methanol. [0003] The traditional synthesis method of heteroatom ZSM-5 molecular sieve is to adopt complex synthesis method, under alkaline condition, the compound containin...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 李为孔德金陈秉祁晓岚
Owner CHINA PETROLEUM & CHEM CORP
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