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Method for synthesizing nano-HMS mesoporous molecular sieve in ion liquid

A technology of mesoporous molecular sieve and ionic liquid, applied in the field of preparation of HMS mesoporous molecular sieve, can solve the problems of difficult synthesis, few studies on the synthesis of nano-mesoporous molecular sieve, and no report on the synthesis of nano-HMS mesoporous molecular sieve, etc. The preparation process is simple and the effect of avoiding environmental pollution

Active Publication Date: 2008-09-24
海安市联发制衣有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Molecular sieves synthesized by conventional methods generally have a grain size larger than 1 μm, while molecular sieves with a grain size smaller than 0.1 μm are difficult to synthesize
Although the size of molecular sieve crystals can be reduced to a certain extent by changing the process conditions of hydrothermal synthesis, adding seeds, dielectrics, organic solvents or surfactants during the synthesis process, using microwave heating, and limited space synthesis, but still Satisfactory nano-molecular sieves cannot be synthesized, and some of the above-mentioned methods still have some shortcomings
So far, there have been many studies on the synthesis of nano-microporous molecular sieves, but few studies on the synthesis of nano-mesoporous molecular sieves. There has been no report on the synthesis of nano-HMS mesoporous molecular sieves.

Method used

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  • Method for synthesizing nano-HMS mesoporous molecular sieve in ion liquid
  • Method for synthesizing nano-HMS mesoporous molecular sieve in ion liquid
  • Method for synthesizing nano-HMS mesoporous molecular sieve in ion liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Example 1: 2.4023g DDA was mixed with 57.6ml deionized water, 18.2ml ethanol and 10.8g [BMIM][BF 4 ] mixed, stirred at room temperature for 30min, and then added dropwise 10g TEOS under stirring. The molar ratio of raw material liquid is TEOS: DDA: EtOH: H 2 O: [BMIM][BF 4 ]=1.0:0.27:6.5:66.7:1.0. After continuing to react at room temperature for 18 hours, perform suction filtration, wash with water, dry at 50°C for 24 hours, and finally bake at 550°C for 6 hours to remove template agent and ionic liquid to obtain HMS mesoporous molecular sieve. The analysis results show that the sample has a typical HMS mesoporous structure, see figure 1 and 2 , the synthesized molecular sieves are spherical particles with a diameter of about 60-100nm, uniform particle size and no agglomeration, see image 3 , the physical properties of the HMS mesoporous molecular sieve synthesized in this example are shown in Table 1.

Embodiment 2

[0023] Embodiment 2: This embodiment is basically the same as Embodiment 1, the difference is: the mol ratio of raw material liquid is TEOS: DDA: EtOH: H 2 O: [BMIM][BF 4 ]=1.0:0.27:6.5:4.0:2.5. In this example, due to the small amount of water used, the ionic liquid is equivalent to the role of the solvent. The results show that nano-HMS mesoporous molecular sieves can also be synthesized at this time, see Figure 4 , its XRD pattern is also similar to Example 1. The particle size of the molecular sieve is about 50-80nm and does not agglomerate. The physical properties of the molecular sieve are shown in Table 1.

Embodiment 3

[0024] Example 3: 3.1294g HDA was mixed with 62.2ml deionized water, 18.2ml ethanol and 5.4g [BMIM][BF 4 ] mixed, stirred at room temperature for 30min, and then added dropwise 10g TEOS under stirring. The molar ratio of the raw material solution is TEOS: HDA: EtOH: H 2 O: [BMIM][BF 4 ]=1.0:0.27:6.5:72:0.5. After continuing to react at room temperature for 24 hours, suction filtration, washing with water, drying at 50°C for 24 hours, and finally calcination at 550°C for 6 hours to remove the template agent and ionic liquid, the XRD spectrum and pore size distribution curve of the prepared molecular sieve are the same as in Example 1 , 2 similar, the particle size is about 70 ~ 100nm, its physical properties are shown in Table 1.

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Abstract

The invention relates to a method for synthesizing a nanometer HMS mesopore molecular sieve. The method has the concrete steps that template, water, ethanol (EtOH) and 1-butyl-3-methyl ionic liquid imidazole tetrafluoroborate ionic liquid are mixed for 5 to 60 min, and a silica source is dropped under the mixing to get a reaction precursor glue solution; the reaction precursor glue solution is continuously mixed to react for 12 to 36 hours to get a sol gelation reaction product; the sol gelation reaction product is filtered or centrifugalized and washed, dried at 50 DEG C for 24 hours, at last roasted at 500 to 650 DEG C of air for 4 to 10 hours, and the template and the ionic liquid are eliminated to get the nanometer HMS mesopore molecular sieve. Because the ionic liquid of the method relates to a nonvolatile green good solvent, the method has the advantages of green environmental protection, environmental pollution prevention and simple preparation technology, and uniform and separated particles of the prepared nanometer HMS mesopore molecular sieve.

Description

technical field [0001] The present invention relates to a kind of preparation method of HMS mesoporous molecular sieve, especially a kind of in ionic liquid [BMIM][BF 4 ] (1-butyl-3-methylimidazolium tetrafluoroborate) in the synthesis method of nanometer HMS mesoporous molecular sieve. Background technique [0002] Since the 1990s, research on the synthesis of mesoporous molecular sieves such as MCM-41, MCM-48, HMS, and MSU using surfactants as templates has been very active. Due to their uniform and regular pore structure, high specific surface area, large adsorption capacity, and high thermal stability, mesoporous molecular sieves have shown broad application prospects in the catalysis, adsorption, and separation of macromolecular organic compounds. Compared with mesoporous molecular sieves such as MCM-41 synthesized mainly by electrostatic interaction, HMS mesoporous molecular sieves synthesized mainly by hydrogen bonding have mild synthesis conditions, thicker pore wal...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 刘红胡宏玖李浩何世强
Owner 海安市联发制衣有限公司
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