Preparation method for super-macroporous silicate molecular sieve

A technology of porous silicate and molecular sieve, which is applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of cumbersome steps and molecular sieve application limitations, and achieve good thermal stability

Active Publication Date: 2018-04-10
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis of this molecular sieve requires the use of a very expensive substituted cobaltocene as a template. When the molecular sieve is roasted, the template is transformed into CoO. It needs to be washed with acid to remove CoO to obtain a pure molecular sieve. The steps are cumbersome, which severely limits the application of the obtained molecular sieve.

Method used

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  • Preparation method for super-macroporous silicate molecular sieve
  • Preparation method for super-macroporous silicate molecular sieve
  • Preparation method for super-macroporous silicate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: Taking the template agent 1 in Table 1 as an example, the synthesis process of the template agent is illustrated.

[0028] 39.648g of benzimidazole was dissolved in 750mL of tetrahydrofuran solution, and then 14.4g of sodium hydroxide was added, and the reaction was carried out under reflux for one day. After cooling down to room temperature, 60 mL of iodomethane was added. The system was reacted under stirring for two days, the reaction mixture was filtered with suction, and the filter residue was washed three times with acetone. The product was then dried with a yield of 97%. The product was subjected to liquid NMR (D 2 O) and electrospray mass spectrometry characterization, confirmed as the target compound.

[0029] The obtained product was dissolved in 100 mL of deionized water, and column exchange was performed through 717 strong basic anion exchange resin to obtain an aqueous solution of the template agent in the form of hydroxide. Weigh an appro...

Embodiment 2

[0031] Embodiment 2: according to molar ratio 1SiO 2 :0.5ROH:0.5HF:5H 2The ratio of O to prepare the gel synthesized by molecular sieves, the general steps are as follows: Weigh an appropriate amount of template agent 1 solution after exchange, add 5mmol (1.042g) of tetraethyl orthosilicate to it, stir at room temperature for about two hours to make orthosilicate Dissolve ethyl acetate completely, then add a designed amount of hydrofluoric acid solution, stir evenly, place the mixed gel under an infrared lamp or in an oven at 80°C, and 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 150°C for 30 days under sealed conditions. The product was washed twice with water and twice with ethanol, and dried to obtain the product. Take an appropriate amount of sample and calcinate it in a muffle furnace at 550°C for 2 hours in an air atmosphere to remove th...

Embodiment 3

[0032] Embodiment 3: according to molar ratio 1SiO 2 :0.5ROH:0.5HF:5H 2 Ratio of O Prepare molecular sieve-synthesized gels using the hydroxide form of 1-methyl-3-benzyl imidazolium salt similar to the templates in Table 1 It is a template agent, synthesized according to the method of Example 2, and the X-ray powder diffraction of the obtained product is identified as an amorphous substance.

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Abstract

The invention discloses a preparation method for a super-macroporous silicate molecular sieve material. The molecular sieve material is obtained by utilizing a low-cost template agent and adopting a hydrothermal synthesis method. The prepared super-macroporous silicate molecular sieve has a UTD-1 structure, 14-ring pore channels in the direction of a crystal axis c and good thermal stability, canbe doped with heteroatoms, and has potential application value in the fields of petrochemistry, fine chemical engineering, life sciences and the like.

Description

technical field [0001] The invention belongs to the field of crystalline microporous materials, and in particular relates to a preparation method of an ultra-large microporous silicate molecular sieve material. Background technique [0002] Molecular sieve materials are a class of TO 4 (T represents the oxidation state atom with +4 valence or +3 valence usually, such as Si, P, Al, B, Ge, Ga, etc.) A type of inorganic microporous solid material composed of tetrahedra sharing vertices. Generally, the composition of molecular sieves can be represented by the following empirical chemical formula: p(M 1 / n XO 2 )·qYO 2 ·rR·wH 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 synthesized prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48
Inventor 杜红宾陈飞剑高子豪刘代融訾文文
Owner NANJING UNIV
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