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Hard template synthetic composite hole zeolite molecular sieve and its preparing method

A zeolite molecular sieve and composite pore technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of large specific surface area, high preparation cost, and low acidity, and achieve high catalytic activity, simple method, and high quality.

Inactive Publication Date: 2006-03-22
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since zeolite molecular sieves have a smaller specific surface and narrower pores, the diffusion rate of catalytic reactions and the application of catalytic reactions involving macromolecules are greatly limited [see Corma, A.Chem.Rev.97, (1997) , 2373.]
For this reason, Mobil Company has invented MCM-41 series mesoporous molecular sieves [see Kresge, C.T., Leonowicz, M.E., Roth, W.J., Vartuli, J.C. & Beck, J.S.Nature 352, (1992), 710.], this kind of molecular sieve ratio The large surface area and large pore size overcome the shortcomings of zeolite molecular sieves to a certain extent, but due to the amorphous walls of mesoporous molecular sieves, their stability is low, their acidity is low, and their preparation costs are high. These factors limit the Further application of mesoporous molecular sieves [see Corma, A.Chem.Rev.97, (1997), 2373.]

Method used

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  • Hard template synthetic composite hole zeolite molecular sieve and its preparing method
  • Hard template synthetic composite hole zeolite molecular sieve and its preparing method
  • Hard template synthetic composite hole zeolite molecular sieve and its preparing method

Examples

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Comparison scheme
Effect test

Embodiment 1

[0020] Example 1: Using rice husk and TPABr as a template, and using silicon oxide in rice husk as a silicon source to synthesize a Silicalite-I zeolite molecular sieve with a composite pore structure

[0021] Synthetic raw materials: dry rice husk as silicon source, rice husk and TPABr as template, NH 4 F as a mineralizer. After determination, SiO in the rice husk used in this embodiment 2 The mass percentage accounted for is 20%, for example, if 20 grams of SiO 2 , you will add 100 grams of rice husk.

[0022] Synthetic ratio: SiO 2 / 40H 2 O / (0.1~0.35)TPABr / NH 4 F.

[0023] Synthetic steps: First, the NH 4 Dissolve F and TPABr in an appropriate amount of water, then stir evenly, add rice husk, stir vigorously for 10 hours, and crystallize the obtained mother liquor.

[0024] Crystallization conditions: the reactant is crystallized at 140-180°C for 20-192 hours, and the obtained product is filtered, washed, and dried at room temperature. Finally, the sample is first ...

Embodiment 2

[0028] Example 2: Using rice husk and TPABr as a template, and using silicon oxide in rice husk as a silicon source to synthesize a ZSM-5 zeolite molecular sieve with a composite pore structure

[0029] Synthetic raw materials: washed and dried rice husk as silicon source, TPABr as template, NH 4 F as a mineralizer, Al 2 (SO 4 ) 3 as a source of aluminum.

[0030] Synthetic ratio: SiO 2 / (0.002-0.04)Al 2 o 3 / 40H 2 O / (0.1~0.35)TPABr / NH 4 F.

[0031] Synthetic steps: First, the NH 4 F. Al 2 (SO 4 ) 3 Dissolve TPABr and TPABr in appropriate amount of water, then stir evenly, add rice husk, stir vigorously for 12 hours, and put the obtained mother liquor into a reactor for crystallization.

[0032] The crystallization conditions and calcination conditions are the same as in Example 1, and ZSM-5 zeolite molecular sieves are prepared.

[0033] Preparation of HZSM-5 catalyst: First, the original powder of ZSM-5 molecular sieve that has removed the template agent was mi...

Embodiment 3

[0034] Example 3: Using rice husk and TPAOH as a template, using silicon oxide and tetraethyl orthosilicate in rice husk as a silicon source to synthesize a ZSM-5 zeolite molecular sieve with a composite pore structure

[0035] Synthetic raw materials: washed and dried rice husk, TPAOH, sodium metaaluminate, tetraethyl orthosilicate (in this embodiment, silicon oxide in rice husk is used as silicon source).

[0036] Synthetic ratio: (0.01~0.1) Al 2 o 3 / SiO 2 / (0.01~0.1)Na 2 O / (0.04~1.8)TPAOH / (10~60)H 2 O. SiO here 2 The ratio is the ratio of ethyl orthosilicate and silicon oxide in rice husk as a silicon source; SiO provided by orthosilicate 2 It accounts for 0-80% of the total silicon source.

[0037] Synthesis steps: first dissolve TPAOH and sodium metaaluminate in an appropriate amount of water, stir evenly, add tetraethyl orthosilicate, stir well, then age at 80-110°C for 1-6 hours, add rice husk to the obtained solution, Continue to stir until uniform, and then c...

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Abstract

The present invention relates to inorganic chemistry, physical chemistry and catalytic chemistry technology. The present invention prepares composite pore zeolite molecular sieve with common silicon source and metal atom with doped skeleton as material, and water as solvent, and through hydrothermal treatment and calcinations process to obtain opened channels. In the hydrothermal treatment, material powder is prepared with hard template of rice hull, alkali styrene ion exchange resin or inorganic carbon, or composite template of mixture comprising hard template and organic amine or organic quaternary ammonium salt. The prepared molecular sieve has composite pore structure comprising micro pores and meso pores and pore walls of MFI, BEA, NaY or MOR crystal structure. The prepared molecular sieve may be used widely as adsorbent, catalyst and catalyst carrier in chemical field.

Description

technical field [0001] The invention belongs to the fields of inorganic chemistry, physical chemistry, material chemistry, catalytic chemistry and chemical engineering, and in particular relates to the synthesis of zeolite molecular sieve by template method and its preparation technology. Background technique [0002] As an important part of inorganic microporous crystal materials, molecular sieves are increasingly becoming the starting point for the research of new inorganic materials due to their unique pore structure and exchangeable cation positions. High-quality carrier of new materials such as electricity). In 1961, Barrer and Denny introduced tetramethyl cation into molecular sieve synthesis system and successfully synthesized Na-A molecular sieve with Si / Al>1 [see D.W.Breck, W.G.Eversole, and R.M.Milson, J.Chem.Soc. , 78, (1956), 2338. and D.W.Breck, and J.Y.Smith., Scienct.Am.200, 85, 1959], created the era of organic template synthesis of molecular sieves. Thu...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 肖丰收王利丰单志超林凯峰马淑杰
Owner JILIN UNIV
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