Gradient pore HZSM-5 (hydrogen zeolite socony mobile-5) molecular sieve and preparation method thereof

A molecular sieve and stepped pore technology, applied in nanotechnology, crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of long hydrothermal crystallization time, increased process cost, material waste, etc. problems, to overcome poor accessibility, improve greenness, and reduce production costs

Active Publication Date: 2018-03-09
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101723403A discloses a method for synthesizing a stepped pore ZSM-5 molecular sieve compounded by mesopores and micropores. In the method, chemical reagents are used as silicon-aluminum sources, organic amines are used as microporous templates, and polysaccharide compounds and their derivatives are used as Mesoporous templates are used to synthesize step-pore ZSM-5 molecular sieves. The synthetic material includes micropores of 0.5-0.6nm and mesopores of 5-100nm (large), but the hydrothermal crystallization time of thi

Method used

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  • Gradient pore HZSM-5 (hydrogen zeolite socony mobile-5) molecular sieve and preparation method thereof
  • Gradient pore HZSM-5 (hydrogen zeolite socony mobile-5) molecular sieve and preparation method thereof
  • Gradient pore HZSM-5 (hydrogen zeolite socony mobile-5) molecular sieve and preparation method thereof

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Embodiment 1

[0036] This embodiment provides a kind of stepped pore HZSM-5 molecular sieve, which is prepared by the following steps:

[0037] (1) Synthesis of microporous NaZSM-5 molecular sieve: Weigh 20.00g of kaolin powder and roast at 800°C for 4h, take 0.48g of the above-mentioned roasted kaolin powder, add 30g of deionized water and 0.30g of concentrated sulfuric acid, mix and stir at 60°C 4h; then add 17.24g water glass, 0.05g seed crystal and 19.80g deionized water, stir vigorously for 30min, add sulfuric acid to adjust the pH to gel; age at 60°C for 4h; transfer the mixture into a polytetrafluoroethylene-lined In a stainless steel crystallization kettle, crystallize statically at 180°C for 48 hours. After the crystallization is completed, cool and filter to obtain the filter cake and crystallization mother liquor, wash the filter cake until neutral, and dry at 120°C to obtain a microporous NaZSM-5 molecular sieve ;

[0038] (2) Synthesis of step-pore NaZSM-5 molecular sieve: Mix...

Embodiment 2

[0045] This embodiment provides a kind of stepped pore HZSM-5 molecular sieve, which is prepared by the following steps:

[0046] (1) Synthesis of microporous NaZSM-5 molecular sieve: Weigh 20.00g of kaolin powder and roast at 600°C for 5h, take 0.64g of the above-mentioned roasted kaolin powder, add 30.00g of deionized water and 0.61g of concentrated hydrochloric acid, Mix and stir for 5 hours; then add 16.95g water glass, 0.15g seed crystal and 19.20g deionized water, stir vigorously for 30 minutes, add sulfuric acid to adjust the pH to gel; age at 60°C for 8 hours; transfer the mixture into a polytetrafluoroethylene In a lined stainless steel crystallization kettle, crystallize statically at 170°C for 36 hours; after the crystallization is completed, cool and filter to obtain a filter cake and crystallization mother liquor, wash the filter cake until neutral, and dry at 120°C to obtain a microporous NaZSM- 5 molecular sieves;

[0047] (2) Synthesis of step-pore NaZSM-5 mol...

Embodiment 3

[0051] This embodiment provides a step-pore HZSM-5 molecular sieve, which is prepared by the following steps:

[0052] (1) Synthesis of microporous NaZSM-5 molecular sieve: Weigh 20.00g rectorite powder and roast at 850°C for 4h, take 0.57g of the above-mentioned roasted rectorite powder, add 30.00g deionized water and 0.30g concentrated sulfuric acid, Mix and stir at 60°C for 4h; add 17.22g of water glass, 0.10g of seed crystal and 19.06g of deionized water, stir vigorously for 30min, then add sulfuric acid to adjust the pH to gel; age at 60°C for 4h; move the mixture into a belt In a stainless steel crystallization kettle lined with polytetrafluoroethylene, crystallize statically at 180°C for 36 hours; after the crystallization is complete, cool and filter to obtain the filter cake and crystallization mother liquor, wash the filter cake until neutral, and dry at 120°C to obtain Microporous NaZSM-5 molecular sieve;

[0053] (2) Synthesis of step-pore NaZSM-5 molecular sieve:...

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Abstract

The invention provides a gradient pore HZSM-5 molecular sieve and a preparation method thereof. The preparation method takes natural clay minerals as raw materials to synthesize a microporous NaZSM-5molecular sieve without application of template agent, performs alkali treatment on the microporous NaZSM-5 molecular sieve through crystallized mother liquid to prepare a gradient pore NaZSM-5 molecular sieve, and performs acid exchange on the gradient pore NaZSM-5 molecular sieve through acid liquor to obtain the gradient pore HZSM-5 molecular sieve. The invention also provides the gradient poreHZSM-5 molecular sieve prepared through the method. The preparation method of the gradient pore HZSM-5 molecular sieve does not require any template agent as well as additional alkali source during alkali treatment and has no discharge of acid liquor or alkali liquor during the whole process, thereby greatly reducing the production cost of molecular sieves and improving the environmental properties of the preparation process; the prepared gradient pore HZSM-5 molecular sieve is rich in micro-mesoporous composite gradient pore structures.

Description

technical field [0001] The invention relates to a molecular sieve and a preparation method thereof, in particular to a step-pore HZSM-5 molecular sieve and a preparation method thereof, belonging to the technical field of molecular sieve preparation. Background technique [0002] Mobil Corporation of the United States successfully synthesized ZSM-5 molecular sieve (US 3702886) for the first time in 1972. Because of its unique three-dimensional pore structure, shape-selective catalytic performance, excellent thermal and hydrothermal stability, and high catalytic activity, it is widely used It is used in many fields such as petrochemical industry, fine chemical industry and environmental protection. [0003] However, the smaller micropores of microporous ZSM-5 molecular sieves (micropores with a pore size of less than 2nm, macropores with a pore size of more than 50nm, and mesoporous pores with a pore size of 2-50nm) prevent larger molecules from entering the molecular sieve c...

Claims

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Application Information

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IPC IPC(8): C01B39/38B82Y40/00
CPCB82Y40/00C01B39/38C01P2002/72C01P2006/12C01P2006/16C01P2006/17
Inventor 岳源源康颖古立亮鲍晓军庞新梅
Owner PETROCHINA CO LTD
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