Method for synthesizing bimodal silicon-aluminum mesoporous material

A technology of mesoporous materials and synthesis methods, applied in the direction of crystalline aluminosilicate zeolites, etc., can solve the problems of single pore size distribution, high price, and difficulty in reducing the cost of organosilanes, and achieve unique properties and reduced synthesis costs.

Inactive Publication Date: 2009-09-16
SHANDONG UNIV OF SCI & TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0006] However, the raw materials for the synthesis of SBA series mesoporous materials and the structure-directing agent are still expensive. Although the structure-directing agent can be recycled, which can reduce its synthesis cost to a certain extent, the cost of organosilane as a raw material is difficult to reduce
Some people also use inorganic raw material sodium metasilicate (Na 2 SiO 3 ·H 2 O) The mesoporous material FDU-7 (Wang Limin, 2002: ZL 02 1 36298.x) with a structure close to SBA-15 was successfully synthesized from a silicon source, but the mesoporous mat

Method used

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  • Method for synthesizing bimodal silicon-aluminum mesoporous material
  • Method for synthesizing bimodal silicon-aluminum mesoporous material
  • Method for synthesizing bimodal silicon-aluminum mesoporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] ①Weigh 5.0g of fly ash, add 4.0g of NaOH solid, add water to dissolve NaOH, mix thoroughly, dry in an oven, calcinate in a muffle furnace at 700°C for 15min, add distilled water to dissolve, ultrasonically oscillate for 10min, then filter, and filtrate in a water bath at 70°C Volatile to 93mL, this is silicon source;

[0037] ② Dissolve 1.10g of P123 in a small amount of distilled water, stir magnetically for 60min, add the above silicon source dropwise at a rate of 8 seconds per drop, add 30mL concentrated HCl after the drop, stir evenly, and react with magnetic stirring at 40°C for 24 hours;

[0038] ③Put the above reactant into a polytetrafluoroethylene bottle, seal and crystallize at 100°C for 48 hours, cool, wash and filter, and dry at room temperature.

[0039] ④The above-mentioned dry matter was transferred to a Soxhlet extractor, and extracted continuously for 42 hours with absolute ethanol to obtain 1.97 g of mesoporous material product,

[0040] ⑤ The product...

Embodiment 2

[0042] ① Weigh 3.0g of fly ash, add 15.0g of 32°Bé grass pulp black liquor, dry in an oven, calcinate in a muffle furnace at 700°C for 15min, add distilled water and 5mL of 1mol / L NaOH, oscillate ultrasonically for 10min and then filter. The filtrate was evaporated to 42mL in a water bath at 70°C, which was the source of silicon.

[0043] ② Dissolve 1.05g P123 in a small amount of distilled water, stir magnetically for 60min, add the above silicon source dropwise at a speed of 9 seconds per drop, add 15mL concentrated HCl after dripping, stir evenly, stir magnetically at 40°C for 24 hours,

[0044] ③Put the above reactant into a polytetrafluoroethylene bottle, seal and crystallize at 100°C for 48 hours, cool, wash and filter, and dry at room temperature.

[0045] ④The above dry matter was transferred to a Soxhlet extractor, and extracted continuously with absolute ethanol for 36 hours to obtain 1.24 g of mesoporous material product

[0046] ⑤ The product name is MSPS-160, whi...

Embodiment 3

[0048] ①Weigh 3.0g of fly ash, add 3.0g of NaOH solid, add water to dissolve NaOH, mix thoroughly, dry in oven, calcinate in muffle furnace at 850°C for 15min, add distilled water to dissolve, ultrasonically oscillate for 10min and filter, filtrate in water bath at 70°C Volatile to 48mL, this is silicon source;

[0049] ② Dissolve 1.10g of P123 in a small amount of distilled water, stir magnetically for 60min, add the above silicon source dropwise at a rate of 10 seconds per drop, add 2.15g concentrated HCl after dripping, stir evenly, and react with magnetic stirring at 40°C for 24 hours;

[0050] ③Put the above reactant into a polytetrafluoroethylene bottle, seal and crystallize at 100°C for 48 hours, cool, wash and filter, and dry at room temperature.

[0051] ④The above-mentioned dry matter was transferred to a Soxhlet extractor, and extracted continuously for 42 hours with absolute ethanol to obtain 1.44 g of mesoporous material product,

[0052] ⑤ The product name is MS...

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Abstract

The invention relates to a method for synthesizing a bimodal silicon-aluminum mesoporous material. The method comprises that: pulverized coal ash/black liquid for papermaking or strong alkali is used as a raw material; firstly, the raw material is evenly mixed in a solution, dried and roasted in a muffle furnace; a roasted product is dissolved by water or acid; an insoluble substance is filtered and removed; and the solution is condensed to obtain a raw material solution for synthesizing the mesoporous material. A surfactant, namely a triblock copolymer (P123) of three block polymers of polyoxyethylene, polyoxypropylene and polyoxyethylene used as a structure guiding agent is dissolved in water, and the mixture is stirred at a constant temperature for more than 1 hour, and slowly dripped with the raw material solution; after the dripping, hydrochloric acid is added into the solution, continuously stirred for more than 24 hours, crystallized at the temperature of 100 DEG C, cooled and filtered to obtain a coarse product; after the coarse product is naturally dried at room temperature, the coarse product can be roasted at the temperature of 550 DEG C or extracted by ethanol to remove the structure guiding agent; and after the coarse product is dried, the mesoporous material of which aperture is in bimodal distribution, namely bimodal SBA-15 is obtained. The mesoporous material contains two kinds of mesopores, wherein the small mesopore is within the range between 3 and 4 nm; the large mesopore is within the range between 5 and 7 nm; an SEM image also shows two different pores; BET nitrogen adsorption proves that the specific surface area of the pore is between 500 and 700m<2>/g; and the size of the pore is between 0.4 and 0.6 cm<3>/g.

Description

(1) Technical field [0001] The present invention relates to a method for synthesizing mesoporous materials, in particular to a method for synthesizing bimodal mesoporous materials using fly ash / coal gangue and papermaking black liquor or fly ash / coal gangue and alkali as raw materials; bimodal is It means that there are two high-intensity peaks at different pore sizes on the pore size distribution curve. (2) Background technology [0002] Inorganic porous materials, due to their large specific surface area and adsorption capacity, have a wide range of applications in the fields of adsorption, separation, and catalysis. According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), porous materials can be divided into the following three types according to the pore size: Microporous, Mesoporous and Macroporous materials. The pore diameter of inorganic microporous materials is generally <2nm, including wollastonite, activated carbon, zeolite,...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 刘振学杜立功崔家强付宇平徐怀浩贺龙
Owner SHANDONG UNIV OF SCI & TECH
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