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Method for preparing mesoporous molecular sieve with high hydrothermal stability by taking ionic liquid as template agent

A mesoporous molecular sieve, ionic liquid technology, applied in molecular sieve compounds, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc. The problem of low polarity of the active agent can achieve the effects of high hydrothermal stability, avoiding environmental pollution and simple preparation process.

Inactive Publication Date: 2011-01-19
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, fluorocarbon surfactants have low polarity, strong hydrophobicity, and weak interaction between fluorocarbon chains, so they are not suitable for use as templates alone, and fluorocarbon surfactants are harmful to the environment

Method used

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  • Method for preparing mesoporous molecular sieve with high hydrothermal stability by taking ionic liquid as template agent
  • Method for preparing mesoporous molecular sieve with high hydrothermal stability by taking ionic liquid as template agent
  • Method for preparing mesoporous molecular sieve with high hydrothermal stability by taking ionic liquid as template agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Preparation of the first step reaction mixture

[0025] Dissolve 3.12g TEOS in deionized water, stir magnetically at 40°C for 30min, then add 1.94g ionic liquid [C 16 mim] + Br - Aqueous solution, adjust pH to 9 with ammonia water, continue to stir 1h, obtain reaction mixture, the molar ratio of reaction mixture is Si:[C 16 mim] + Br - :H 2 O=1:0.33:100.

[0026] The second step of hydrothermal crystallization

[0027] The reaction mixture was placed in a polytetrafluoroethylene-lined stainless steel reactor, and hydrothermally crystallized at 170°C for 3 days. The crystallized product was filtered, washed with water, and dried at 50°C for 24h, and finally placed in a muffle furnace at Calcined at 550°C for 6h to obtain SiO 2 mesoporous molecular sieves.

[0028] N 2 Adsorption-desorption and TEM results show that the sample has a typical worm-like mesoporous structure, see figure 1 and figure 2 . The average pore diameter, BET specific surface area and po...

Embodiment 2

[0030] Preparation of the first step reaction mixture

[0031] Operation process is except following difference, all the other are with embodiment 1.

[0032] Added inorganic salt NaF in the preparation of reaction mixture, raw material molar ratio is Si: [C 16 mim] + Br - :NaF:H 2 O=1:0.33:0.05:100.

[0033] The second step of hydrothermal crystallization

[0034] With embodiment 1.

[0035] The structural parameters of the obtained mesoporous molecular sieves are shown in Table 1. After the sample was boiled in boiling water at 100°C for 8 days, its structure did not change significantly. Compared with Example 1, after adding NaF during the synthesis process, the hydrothermal stability of the mesoporous molecular sieve is further improved.

Embodiment 3

[0037] Preparation of the first step reaction mixture

[0038] Operation process is with embodiment 1.

[0039] The second step of hydrothermal crystallization

[0040] The reaction mixture was crystallized at 190°C for 3 days. All the other are with embodiment 1.

[0041] The structural parameters of the obtained mesoporous molecular sieves are shown in Table 1. After the sample was boiled in boiling water at 100°C for 7 days, its structure did not change significantly. Compared with Example 1, the increase in the crystallization temperature of the mesoporous molecular sieve increases the polymerization degree of the silicon wall of the mesoporous molecular sieve, and the hydrothermal stability of the obtained mesoporous molecular sieve is also improved.

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Abstract

The invention relates to a method for preparing a mesoporous molecular sieve with high hydrothermal stability by taking an ionic liquid as a template agent. The method comprises the following steps: taking the ionic liquid 1-hexadecyl-3-methyl bromoimidazole C16mim<+>Br<-> as the template agent, tetraethoxysilane (TEOS) or tetramethoxysilane (TMOS) as a silicon source, and NaF as an additive, andpreparing the mesoporous molecular sieve through the preparation of a reaction mixture and high-temperature hydrothermal crystallization and filtration, washing, drying and roasting. The method utilizes a plurality of characteristics of the ionic liquid and has simple preparation technology, and the prepared mesoporous molecular sieve has high hydrothermal stability. Moreover, the method avoids using an organic template agent which is harmful to the environment, so that the method is environment-friendly.

Description

technical field [0001] The invention relates to a method for preparing mesoporous molecular sieves by using ionic liquid as a template, in particular to a method for preparing mesoporous molecular sieves with high hydrothermal stability, and belongs to the technical field of inorganic chemical synthesis. Background technique [0002] Mesoporous molecular sieves have uniform and adjustable pore structure, high specific surface area and large adsorption capacity, and have broad application prospects in many fields such as catalysis, adsorption and assembly of macromolecular substances. However, because the pore walls of mesoporous molecular sieves are in an amorphous state, the condensation of silicon species in the framework is incomplete, and there are a large number of non-polymerized surface silanol groups, the hydrothermal stability of mesoporous molecular sieves is extremely poor, which seriously hinders its industrial application. process. Therefore, improving and enha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/10C01B37/00C01B39/00
Inventor 刘红梁玉广汪孟阳
Owner SHANGHAI UNIV
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