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Ordered mesoporous molecnlar sieve material with wltrahigh hydrothermal stability and synthesis method thereof

A mesoporous molecular sieve and thermally stable technology, applied in the chemical field, can solve problems such as structural damage, molecular sieves with no catalytic activity, incomplete condensation of silicon species, etc., and achieve good hydrothermal stability

Inactive Publication Date: 2004-03-24
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Just because the method for preparing mesoporous molecular sieve materials in the prior art only uses tri-block copolymer compounds as templates, which can only be synthesized at low temperature, the silicon species in the obtained product skeleton is incompletely condensed, and the hydrothermal stability is poor. SBA- 15 The structure is completely destroyed in boiling water for more than 50 hours; since there is no doping with species other than silicon, the molecular sieve has basically no catalytic activity

Method used

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  • Ordered mesoporous molecnlar sieve material with wltrahigh hydrothermal stability and synthesis method thereof
  • Ordered mesoporous molecnlar sieve material with wltrahigh hydrothermal stability and synthesis method thereof
  • Ordered mesoporous molecnlar sieve material with wltrahigh hydrothermal stability and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Regular hexagonal mesoporous molecular sieve JLU-20 and its high-temperature hydrothermal synthesis method

[0024] Using tetraethyl orthosilicate (TEOS) as the silicon source, a mixture of fluorocarbon surfactant (FC-4) and triblock copolymer compound (P123) as the template, hydrochloric acid (HCl) is used to adjust the pH value, and water is Solvent, the molar ratio of silicon source (TEOS), templating agent, solvent is as follows:

[0025] 1.0~1.6 FC-4 / 0.07~0.09 P123 / 8.5~11.2 TEOS / 0.5~2.0 HCl / 1000~2000H 2 o

[0026] The process is as follows: firstly dissolve fluorocarbon surfactant (FC-4) and triblock copolymer compound (P123) in water, add hydrochloric acid, stir until clear, then add silicon source (TEOS). The above solution was continued to be stirred at 40°C for 20 hours, then transferred to a reaction kettle, and crystallized at 180°C for 48 hours. The product was extracted and dried at room temperature for 24 hours to obtain the original powder. ...

Embodiment 2

[0028] Example 2: Regular hexagonal mesoporous molecular sieve Al-JLU-20 and its high-temperature hydrothermal synthesis method

[0029] First, dissolve the fluorocarbon surfactant (FC-4) and triblock copolymer compound (P123) in a certain amount of water, add an appropriate amount of hydrochloric acid, stir until clear, then add silicon source (TEOS) and aluminum source (NaAlO 2 ). Continue to stir the above solution at 40°C for 20 hours, then transfer it to the reaction kettle, take out the reaction kettle after crystallization at 180°C for 48 hours, adjust the pH value of the system to 8.0 with ammonia water, and then continue to crystallize at 180°C for 48 hours. The product was extracted and dried at room temperature for 24 hours to obtain the original powder of Al-JLU-20. Heating the raw powder to 650°C in the air and keeping it for 5 hours can completely remove the organic template agent and obtain open channels.

[0030] The molar ratio of raw materials is in the fol...

Embodiment 3

[0034] Example 3 Regular hexagonal mesoporous molecular sieve Ti-JLU-20 and its high-temperature hydrothermal synthesis method

[0035] To prepare regular hexagonal mesoporous molecular sieve Ti-JLU-20 doped with titanium, the precursor of titanium-silicon molecular sieve (TS-1) should be prepared at first. For the specific method, see Chinese invention patent CN1349929A, published on May 22, 2002; The obtained TS-1 precursor replaced TEOS as the silicon source to synthesize JLU-20, and the specific process was the same as in Example 1. The obtained product is Ti-JLU-20.

[0036] Uv-vis spectra showed that titanium species were effectively introduced into the framework of JLU-20, and its spectral peak appeared at around 210nm, and the four-coordination environment it was in was similar to that in TS-1 molecular sieve crystals. Ti-JLU-20 also exhibits ultra-high hydrothermal stability, similar to Al-JLU-20, its mesoporous structure can be stable in boiling water for more than ...

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Abstract

A ordered porous molecule sieve having a super high hydrothermal stability and a formula of SiO2-Al2O3-MxOy, wherein Al / Si=0-1.0, M / Si=0-0.05, M=Fe3+, B3+ and a completely condensation of siliceous species on the pore wall, Q4 / Q3 =3-7, can be synthesized according to the steps of 1) making a pattern plate reagent 2) preparing raw powder 3) getting rid of the pattern plate reagent. Particularly, making pattern plate reagent includes mixing the F-C surfactant with C-H surfactant, dissolving them in water, making the PH below 1 or 8-10. Crystallizing temperature is of 160-250 deg.C. to obtain the raw powder.

Description

technical field [0001] The invention belongs to the field of chemistry, including the fields of catalytic chemistry, chemical engineering, inorganic chemistry, physical chemistry and material chemistry, and particularly relates to a mesoporous molecular sieve material with ultrahigh hydrothermal stability and its preparation technology. Background technique [0002] In 1992, after Mobil Corporation of the United States first synthesized regular mesoporous molecular sieves, the synthesis of mesoporous molecular sieves has attracted increasing attention. However, unlike traditional microporous molecular sieve crystals, mesoporous molecular sieves have relatively low hydrothermal stability due to incomplete condensation of silicon species in the framework and a large number of hydroxyl groups on the surface and interior of the pore walls, which limits the mesoporous Molecular sieves are used in the fields of catalysis, adsorption and separation. [0003] It is an effective way...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/06
Inventor 肖丰收韩宇李得凤宋江伟吴硕阳晓宇砥岩
Owner JILIN UNIV
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