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Preparation method of monolithic microporous-macroporous Silicalite-1@SiO2

A monolithic, microporous technology used in chemical instruments and methods, other chemical processes, etc.

Inactive Publication Date: 2019-01-15
陈秋霞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been few reports on hierarchically porous monolithic Silicalite-1 materials with stable structures and different regular shapes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A monolithic microporous-macroporous Silicalite-1@SiO 2 The preparation method comprises the following steps: 20 parts of epoxy resin, 25 parts of polyethylene glycol 1000 and 7 parts of polyethylene glycol 20000 are placed in a beaker, mixed, heated and melted, and when the solution is uniform and transparent, quickly add 15 parts of Triethylenetetramine, maintain the system temperature at 65°C and continuously stir vigorously for 25min, transfer the liquid in the beaker to the mold, react at 65°C for 3.5h, the liquid in the mold turns into a white solid, put the white solid in distilled water Soak to remove polyethylene glycol, and finally dry naturally at room temperature to obtain a monolithic epoxy resin macroporous polymer with a three-dimensional skeleton structure; after vacuum drying the polymer template prepared above at 50 ° C for 3.5 h, in Soak in tetraethyl orthosilicate for 48h, then take out the material and place it in NH at 25°C 3 In the atmosphere for...

Embodiment 2

[0022] A monolithic microporous-macroporous Silicalite-1@SiO 2 The preparation method comprises the following steps: 15 parts of epoxy resin, 20 parts of polyethylene glycol 1000 and 5 parts of polyethylene glycol 20000 are placed in a beaker, mixed, heated and melted, and when the solution is uniform and transparent, quickly add 10 parts of Triethylenetetramine, maintain the system temperature at 64°C and continuously stir vigorously for 20 minutes, transfer the liquid in the beaker to the mold, react at 64°C for 3 hours, the liquid in the mold turns into a white solid, soak the white solid in distilled water to remove polyethylene glycol, and finally dry naturally at room temperature to obtain a monolithic epoxy resin macroporous polymer with a three-dimensional skeleton structure; after vacuum drying the polymer template prepared above at 45°C for 3 h, Soak in tetraethyl acetate for 47h, then take out the material and place it in NH at 20°C 3 In the atmosphere for 25h and ...

Embodiment 3

[0024] A monolithic microporous-macroporous Silicalite-1@SiO 2 The preparation method comprises the following steps: 25 parts of epoxy resin, 30 parts of polyethylene glycol 1000 and 9 parts of polyethylene glycol 20000 are placed in a beaker, mixed, heated and melted, and when the solution is uniform and transparent, quickly add 20 parts of Triethylenetetramine, maintain the system temperature at 66°C and continuously stir vigorously for 30 minutes, transfer the liquid in the beaker to the mold, react at 66°C for 4 hours, the liquid in the mold turns into a white solid, soak the white solid in distilled water to remove polyethylene glycol, and finally dry naturally at room temperature to obtain a monolithic epoxy resin macroporous polymer with a three-dimensional skeleton structure; the polymer template prepared above was vacuum-dried at 55°C for 4 hours, and then placed on orthosilicon Soak in tetraethyl acetate for 49h, then take out the material and place it in NH at 30°C ...

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PUM

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Abstract

The invention discloses a preparation method of monolithic microporous-macroporous Silicalite-1@SiO2. The preparation method comprises the following steps: mixing, heating and melting epoxy resin, polyethylene glycol 1000 and polyethylene glycol 20000, adding triethylenetetramine, stirring for 20-30 min, transferring to a mould, carrying out a reaction for 3-4 h, and transforming the liquid in themould into a white solid; soaking the white solid in distilled water, drying, soaking in tetraethyl orthosilicate, taking out the material, placing in NH3 for 25-27 h, drying and calcining to obtainmonolithic macroporous SiO2; and mixing and stirring a 40% tetrapropyl ammonium hydroxide solution, tetraethyl silicate and distilled water, soaking the macroporous SiO2 carrier in the solution for 3-4 h, then transferring into a pressure reaction kettle, carrying out a reaction, taking out the material, washing and drying, and then calcining to obtain the product. The material prepared by the method has good phenol adsorption performance and is easy to separate from an adsorption system.

Description

technical field [0001] The invention relates to an integral microporous-macroporous Silicalite-1@SiO 2 method of preparation. Background technique [0002] Zeolite molecular sieves have a unique pore structure and adjustable framework elements, and have the characteristics of large specific surface area, strong acidity, and high hydrothermal stability, so they have high application value in the fields of gas adsorption and separation, catalysis, and ion exchange. However, traditional powdered molecular sieves are not only difficult to recycle in application, but also increase the pressure drop in the fixed bed reactor and consume more power. Therefore, molecular sieve catalysts in industrial applications are usually made into monolithic spherical or strip to reduce the pressure drop in the reactor. The method for preparing monolithic molecular sieve materials is generally to add an inorganic binder (such as Al 2 o 3 , SiO 2 etc.), but the micropore channels and active c...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/30
CPCB01J20/18B01J20/103
Inventor 陈秋霞
Owner 陈秋霞
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