Super-macroporous silicate molecular sieve NUD-1 and preparation method thereof

A technology of porous silicate and molecular sieve, which is applied in the direction of molecular sieve catalysts, molecular sieves and base exchange compounds, chemical instruments and methods, etc., and can solve the problems of difficult crystallization and limited number of sieves

Inactive Publication Date: 2015-02-25
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is well known that the crystallization of macroporous and ultra-large pore silicate molecular sieves is very difficult, and the number of silicate molecular sieve materials with ultra-large pore structures that have been synthesized is very limited. There are only five kinds of porous silicate molecular sieve materials, which are ITQ-37 with 30-membered rings [J.Sun, C.Bonneau, A.Cantin, A.Corma, M.J.Diaz-Cabanas, M.Moliner, D.Zhang, M.Li, X.Zou, Nature,

Method used

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  • Super-macroporous silicate molecular sieve NUD-1 and preparation method thereof
  • Super-macroporous silicate molecular sieve NUD-1 and preparation method thereof
  • Super-macroporous silicate molecular sieve NUD-1 and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: Taking the template agent 2 in Table 2 as an example, the synthesis process of the template agent is illustrated. Mix 16.997g of benzyl bromide and 75ml of tetrahydrofuran in a 250ml round-bottomed flask. Under reflux, add 1,2-dimethylimidazole in tetrahydrofuran (9.607g / 75ml) dropwise to the mixture. The system was reacted under stirring for two days, and the reaction mixture was rotovaped to remove the solvent to obtain a crude product, which was recrystallized from ethanol to obtain 25.274 g of the product, with a yield of 95%. The product was tested by liquid NMR (D 2 O) and electrospray mass spectrometry characterization, confirmed as the target compound.

[0035] The obtained product was dissolved in 100 ml of deionized water, and column exchange was carried out through 717 strong basic anion exchange resin to obtain an aqueous solution of the template agent 2 in the form of hydroxide. Weigh an appropriate amount of this solution, calibrate it with...

Embodiment 2

[0037] Embodiment 2: according to molar ratio 1SiO 2 : 1GeO 2 :0.8ROH:0.8HF:10H 2 The ratio of O to prepare the gel synthesized by molecular sieves, the general steps are as follows: Weigh an appropriate amount of template agent 7 solution after exchange, add 5mmol (0.523g) of germanium dioxide powder to it, stir for about half an hour to make the added germanium dioxide Dissolve completely, add 5mmol (1.042g) of tetraethyl orthosilicate later, stir at room temperature for about two hours to completely dissolve the tetraethyl orthosilicate, then add the designed amount of hydrofluoric acid solution, stir evenly, and mix the gel Place under an infrared lamp or in an oven at 80°C to remove excess solvent to a theoretical weight. The final reaction gel was transferred to a 15ml stainless steel reaction kettle with polytetrafluoroethylene lining, and reacted at 160°C for 30 days under sealed conditions. The product was washed twice with water and twice with ethanol, and dried fo...

Embodiment 3

[0038] Embodiment 3: according to molar ratio 1SiO 2 : 1GeO 2 : 0.5ROH: 0.5NH 4 F: 5H 2 The ratio of O to prepare the gel synthesized by molecular sieves, the general steps are as follows: Weigh an appropriate amount of template agent 4 solution after exchange, add 5mmol (0.523g) of germanium dioxide powder to it, stir for about half an hour to make the added germanium dioxide Dissolve completely, add 5mmol (1.042g) of tetraethyl orthosilicate later, stir at room temperature for about two hours to completely dissolve the tetraethyl orthosilicate, then add the designed amount of ammonium fluoride, stir evenly, and place the mixed gel Under infrared light or in an oven at 80°C, remove excess solvent to theoretical weight. The resulting reaction gel was transferred to a 15ml stainless steel reaction kettle with a polytetrafluoroethylene liner, and reacted at 150°C for 15 days under sealed conditions. The product was washed twice with water and twice with ethanol, and dried for...

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Abstract

The invention discloses a super-macroporous silicate molecular sieve material and a preparation method thereof, the molecular sieve has the X ray powder diffraction characteristic shown in Table 1, is obtained by hydrothermal synthesis method, has a three-dimensional pore structure of 18 * 12 * 10, good thermal stability, and larger specific surface area, can be incorporated into heteroatom, and has potential application values in petrochemistry, fine chemical engineering and life science and other fields.

Description

technical field [0001] The invention belongs to the field of crystalline microporous materials, and in particular relates to a novel structure ultra-large microporous silicate molecular sieve material and a preparation method thereof. Background technique [0002] Molecular sieve materials are a class of TO 4 (T stands for oxidation state atoms with +4 or +3 valence in general, such as Si, P, Al, B, Ge, Ga, etc.) A type of inorganic microporous solid material composed of tetrahedrons sharing vertices. Usually, the composition of molecular sieves can be represented by the following empirical chemical formula: x(M 1 / n XO 2 )·yYO 2 ·zR·qH 2 O, where M represents one or more +n-valent organic or inorganic cations; X represents one or more trivalent elements; Y represents one or more tetravalent elements, usually Si; R represents one or more an organic molecule. For a molecular sieve with a specific structure obtained by a specific synthesis method, whether it is a freshly ...

Claims

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Application Information

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IPC IPC(8): C01B39/48B01J29/70B01J29/86B01J29/04
CPCB01J29/04B01J29/70B01J29/86C01B33/20C01B39/48C01P2002/72C01P2006/12C01P2006/16
Inventor 杜红宾陈飞剑
Owner NANJING UNIV
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