Mesoporous silicon dioxide molecular sieve and preparation method thereof

A mesoporous silica and molecular sieve technology, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve problems such as limiting industrial scale production

Inactive Publication Date: 2012-01-11
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This greatly limits the industrial-scale production of such materials

Method used

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  • Mesoporous silicon dioxide molecular sieve and preparation method thereof
  • Mesoporous silicon dioxide molecular sieve and preparation method thereof
  • Mesoporous silicon dioxide molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Add 3g of PEO-PPO-PEO (F127, molecular weight 12600) into 120ml of water, 2 SO 4 The pH of the solution was adjusted to 1.0, 5 g of methyl orthosilicate was added, and stirred at 25° C. for 1 hour. to obtain a homogeneous colloidal solution

[0024] (2) Add 25 mM carbonate buffer solution (pH 9.23) to the sol mixture obtained in step 1 under stirring at room temperature, adjust the pH value of the solution to 5.0, and obtain white silica precipitate.

[0025] (3) Calcining the precipitated product in step 2 at a high temperature of 600° C. at a rate of 2° C. / min for 5 hours to obtain a white mesoporous silica mesoporous molecular sieve.

[0026] The main physical and chemical properties of the product: the specific surface area is 665m 2 / g, the mesopore diameter is 4.0nm~4.2nm, and the pore volume is 0.75cm 3 / g.

[0027] image 3 The TEM pattern of the product is shown. It can be seen from the graph that the product obtained in Example 1 is a TJU-1 worm-lik...

Embodiment 2

[0029] (1) 1.5g of EO 20 po 70 EO 20 (P123, molecular weight 5700-5800) was added into 100ml of water, the pH of the solution was adjusted to 2.0 with 1M HCl, 3.3g of tetraethyl orthosilicate was added, and stirred at 45°C for 1 hour. to obtain a homogeneous colloidal solution

[0030] (2) The sol mixture obtained in step 1 was stirred at room temperature, and 250 mM carbonate buffer solution (pH. 10.56) was added to adjust the pH value of the solution to 6.4 to obtain a white silica precipitate.

[0031] (3) Calcining the precipitated product in step 2 at a high temperature of 550° C. at a rate of 1.5° C. / min for 5 hours to obtain a white mesoporous silica mesoporous molecular sieve.

[0032] The main physical and chemical properties of the product: the specific surface area is 750m 2 / g, the mesopore diameter is about 4.0nm, and the pore volume is 0.70cm 3 / g.

[0033] Figure 4 The TEM spectrum of the embodiment product shown. The structural information shown in the...

Embodiment 3

[0035] (1) 1.5g of EO 20 po 70 EO 20 (P123, molecular weight 5700-5800) was added into 100ml of water, with 3M H 3 PO 4 The pH of the solution was adjusted to 3.0, 3.3 g of ethyl orthosilicate was added, and stirred at 40° C. for 3 hours. to obtain a homogeneous colloidal solution

[0036] (2) The sol mixture obtained in step 1 was stirred at room temperature, and added with 100 mM phosphate buffer solution (pH 7.9) to adjust the pH value of the solution to 6.7 to obtain a white silica precipitate.

[0037](3) Calcining the precipitated product in step 2 at a high temperature of 550° C. at a rate of 1.5° C. / min for 4 hours to obtain a white mesoporous silica mesoporous molecular sieve.

[0038] The main physical and chemical properties of the product: the specific surface area is 495m 2 / g, the mesopore diameter is about 5.6nm, and the pore volume is 0.88cm 3 / g. The TEM pattern of this embodiment product shown in Fig. 54. The structural information shown in the spect...

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Abstract

The invention relates to a mesoporous silicon dioxide molecular sieve and a preparation method thereof. The method comprises the following synthesis steps: 1), mixing a nonionic surfactant, a silicon source and water in a molar ratio of (0.01-0.1): (300-500): (1-3), regulating the pH value of the solution to 1.0 to 3.0 with an acid, and stirring the solution at 20 to 80 DEG C for 1 to 3 hours to form a sol mixture; 2) stirring the sol mixture obtained by the step 1 at room temperature, adding an alkaline buffer solution and regulating the pH value of the solution to 5 to 7.5 to obtain a whitesilicon dioxide precipitate; and 3) roasting the precipitate obtained by the step 2 at 500 to 600 DEG C for 3 to 5 hours to obtain a white mesoporous silicon dioxide material. The white mesoporous silicon dioxide material has an order hexagonal phase structure, a local short range order hexagonal phase structure, a multilayer onion-like structure, a worm-like structure or a foam-like hollow vesica structure. The method for synthesizing the mesoporous silicon dioxide molecular sieve of the invention is a real green biomimic synthesis method. The application of the method can promote the industrial production of like materials.

Description

technical field [0001] The invention belongs to the technical field of inorganic porous materials, and in particular relates to a mesoporous silica molecular sieve and a preparation method thereof. Background of the invention [0002] Mesoporous molecular sieve refers to a kind of inorganic porous material with a pore size between 2 and 50 nm and a regular structure assembled by the sol=gel process of inorganic substances under certain conditions using surfactants as supramolecular templates. From 1990 to 1992, after applying for a series of patents (US5057296, US5098684, US5102643, US5108725, WO1991011390 and WO1992011934), Mobil Corporation of the United States published the successful synthesis of MCM family mesoporous silica molecular sieves in Nature, which opened the A milestone in the study of porous molecular sieves. Due to the characteristics of uniform pore size distribution, precise tunable pore size, long-range pore order, high specific surface area, and relativ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48B01J20/10B01J20/30B01J32/00
Inventor 董伟兵杨志民谭小月龚俊波
Owner TIANJIN UNIV
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