Preparation method of spherical meso-porous molecular sieve

A mesoporous molecular sieve, spherical technology, applied in the direction of silica, silica, etc., can solve the problems of high cost, complicated synthesis steps, harsh synthesis conditions, etc., to achieve rapid synthesis, shorten synthesis time, and reduce production costs. Effect

Inactive Publication Date: 2016-06-22
LIAONING OXIRANCHEM INC
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Problems solved by technology

[0012] The purpose of the present invention is to overcome the disadvantages of cumbersome synthesis steps, harsh synthesis conditions and high cost when preparing spherical mesoporous molecular sieve MCM-41 in the prior art, and introduce methyl ethyl ketone with low boiling point, low polarity and low surface tension as a co- Solvent, to obtain spherical mesoporous molecular sieves with smaller particle size conveniently and quickly

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  • Preparation method of spherical meso-porous molecular sieve
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[0032] The invention provides a preparation method of a spherical mesoporous molecular sieve, comprising: mixing a cationic surfactant, ammonia water, methyl ethyl ketone and water to obtain a mixed solution; adding tetraethyl orthosilicate (TEOS) to the mixed solution, and stirring to obtain a reaction solution; filtering the reaction solution to obtain a filtrate; and calcining the filtrate to obtain a spherical mesoporous molecular sieve.

[0033] The cationic surfactant, ammonia water, methyl ethyl ketone and water can be mixed by adding cationic surfactant to deionized water, and then adding ammonia water and methyl ethyl ketone after it is completely dissolved, or adding ammonia water and methyl ethyl ketone to water first, Afterwards, the cationic surfactant is added, as long as the components are completely dissolved to obtain a mixed solution. The concentration of ammonia water used is preferably 25-28% (volume fraction).

[0034] In order to obtain a mesoporous mole...

Embodiment 1

[0049] Weigh 0.62g CTAB and dissolve it in 30g deionized water. After it is completely dissolved, add 2.6mL ammonia water and 8.8g butanone to the solution.

[0050] Stir at room temperature for about 20 minutes, then add 2.6mLTEOS, the molar ratio of each component in the final sol is TEOS / CTAB / NH 3 / H 2 O / butanone=1:0.14:1.4:150:10.

[0051] Continue to stir at room temperature for about 2 hours, then filter with suction, rinse with deionized water, dry the white precipitate in an oven at 60°C for 1 day, and bake the final powder at 500°C in a muffle furnace for 6 hours. Remove template agent, obtain the spherical MCM-41 mesoporous molecular sieve with smooth surface, its scanning electron micrograph (SEM) such as figure 1 As shown, the characteristic small-angle X-ray diffraction pattern (XRD) is as figure 2 shown.

[0052] After measurement, the total surface area of ​​the obtained spherical MCM-41 mesoporous molecular sieve is 1055m 2 / g, the total pore volume is 0....

Embodiment 2

[0054] Weigh 0.62g CTAB and dissolve it in 30g deionized water. After it is completely dissolved, add 2.6mL ammonia water and 8.8g butanone to the solution.

[0055] Stir at room temperature for about 20 minutes, then add 2.6mLTEOS, the molar ratio of each component in the final sol is TEOS / CTAB / NH 3 / H 2 O / butanone=1:0.14:1.4:150:10.

[0056] After adding TEOS and reacting for 4 hours, transfer the obtained solution to a crystallization kettle, conduct hydrothermal treatment at 85°C for 1 day, then perform suction filtration, rinse with deionized water, dry, and finally roast at 600°C , to obtain spherical MCM-41 mesoporous molecular sieves with a slightly rough surface.

[0057] After measurement, the total surface area of ​​the obtained spherical MCM-41 mesoporous molecular sieve is 919m 2 / g, the total pore volume is 0.79cm 3 / g, the pore diameter is about 3.1nm, and the average diameter of solid spheres is about 300-400nm.

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Abstract

The invention provides a preparation method of spherical meso-porous molecular sieve. The method comprises the following steps: mixing a cationic surfactant, ammonia water, butanone and water to obtain a mixed solution; adding tetraethyl orthosilicate, and stirring to obtain a reaction solution; filtering the reaction solution to obtain a filtered product; and calcining the filtered product to obtain the spherical meso-porous molecular sieve. The preparation method solves the defect of only synthesis of solid spheres with large particle sizes under simple synthesis step and mild synthesis conditions; butanone with a low boiling point, low polarity and low surface tension is used as a cosolvent, so the spherical meso-porous molecular sieve with small particles sizes can be conveniently and fast obtained, the synthesis time is greatly shortened, the rapid synthesis purpose is reached, and the production cost is reduced; and the spherical meso-porous molecular sieve prepared in the invention has wide practical application values in the fields of carriers in catalyst preparation, and chromatographic column filling in chromatographic separation.

Description

technical field [0001] The invention belongs to the field of molecular sieve inorganic materials, in particular to a preparation method of spherical mesoporous molecular sieves. Background technique [0002] MCM-41 molecular sieve has regular pore structure (two-dimensional hexagonal structure), narrow pore size distribution (2-10nm), large pore volume (>0.3cm 3 / g), high specific surface area (800~1200m 2 / g) and other characteristics. The large and uniform pore size is conducive to the effective diffusion of macromolecules in its channels. MCM-41 modified with metal ions is effective in alkylation reactions, alkane isomerization reactions, oxidation reactions of aromatic compounds, esterification reactions, It has good activity in acylation reaction and polymerization reaction, and has attracted great attention in the field of macromolecular catalytic reactions. [0003] The higher specific surface area and larger pore volume are conducive to its use as an adsorbent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12
Inventor 朱建民刘兆滨董振鹏周立明张金昌
Owner LIAONING OXIRANCHEM INC
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