Diplopore silica gel material, and preparation method

A technology of silica gel column and pore size, which is applied in the direction of silica, silica, etc., can solve the problems of application limitation, insufficient mechanical strength of silica gel integral column, etc., and achieve the effect of improving mechanical strength and good mechanical strength

Active Publication Date: 2006-12-06
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mechanical strength of the silica monolithic column prepared by this method is not enough, which greatly limits its application.

Method used

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  • Diplopore silica gel material, and preparation method
  • Diplopore silica gel material, and preparation method
  • Diplopore silica gel material, and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 4.97g of polyethylene glycol (molecular weight: 10,000) into 52mL of 0.01mol / L nitric acid, stir until completely dissolved, then add 28.4mL of tetramethoxysilane (TMOS), and stir vigorously at 0°C for 30 minutes , Pour the obtained sol into a polytetrafluoroethylene tube with a diameter of about 1.0 cm and seal it, and place it in a water bath at 40° C. for 2 hours to gel.

[0024] Secondly, take out the silica gel column in the polytetrafluoroethylene tube, wash it with deionized water, place it in a methanol solution with a volume ratio of 20% (water / methanol), and keep it at 55° C. for 24 hours. Then placed in a methanol solution of TMOS with a volume ratio of 65% (TMOS / methanol), aged at 65° C. for 60 hours. Then soak in methanol at 50°C for 24 hours. Finally, dry at 70°C for 24 hours, and bake at 700°C for 2 hours to obtain a silica gel column sample.

[0025] figure 1 is the SEM image of the obtained sample, figure 2 is the X-ray diffraction pattern of t...

Embodiment 2

[0028] Add 4.97g of polyethylene glycol (molecular weight: 100,000) into 52mL of 0.01mol / L acetic acid, stir until completely dissolved, then add 28.4mL of tetramethoxysilane (TMOS), and stir vigorously at 0°C for 30 minutes , Pour the obtained sol into a polytetrafluoroethylene tube with a diameter of about 1.0 cm, seal it, and place it in a water bath at 40° C. for 3 hours to gel.

[0029] Next, take out the silica gel column in the polytetrafluoroethylene tube, wash it with deionized water, put it in an ethanol solution with a volume ratio of 18% (water / ethanol), and keep it at 62.5° C. for 24 hours. Then placed in a TMOS ethanol solution with a volume ratio of 59% (TMOS / ethanol), aged at 65° C. for 96 hours. Then soak in ethanol at 50°C for 24 hours. Finally, dry at 60°C for 48 hours, and bake at 700°C for 2 hours to obtain a silica gel column.

[0030] image 3 It is a scanning electron microscope photo of the obtained sample. The macropore diameter of the sample is 1....

Embodiment 3

[0032] Add 4.37g of polyethylene glycol (molecular weight: 10,000) into 52mL of 0.044mol / L nitric acid, stir until completely dissolved, then add 28.4mL of tetramethoxysilane (TMOS), and stir vigorously at 0°C for 30 minutes , Pour the obtained sol into a polytetrafluoroethylene tube with a diameter of about 1.0 cm and seal it, and place it in a water bath at 40° C. for 2 hours to gel.

[0033] Next, take out the silica gel column in the polytetrafluoroethylene tube, wash it with deionized water, place it in a methanol solution with a volume ratio of 26% (water / methanol), and keep it at 70° C. for 24 hours. Then placed in a methanol solution of TMOS with a volume ratio of 50% (TMOS / methanol), aged at 57.5° C. for 24 hours. Then soak in an aqueous solution of Tween 80 at 50°C for 24 hours. Finally, dry at 70°C for 24 hours, and bake at 700°C for 2 hours to obtain a silica gel column.

[0034] Figure 4 It is a scanning electron microscope photo of the obtained sample. The ma...

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Abstract

This invention discloses a method for preparing porous silica gel column material. The macropore sizes are 0.5-3.0 mum, and the mesopore sizes are 3-10nm. The volume of the pores is 2.5-3.5 cu cm/g, and the specific surface area is 250-710 sq cm/g. The compressive strength of the particles is 180-220 N.

Description

technical field [0001] The invention relates to an inorganic porous material and a preparation method thereof, more specifically to a through-flow double-hole silica gel column material with high hardness and a preparation method thereof. Background technique [0002] In the field of porous materials, increasing the pore size is one of the goals of structure control. Ordered macroporous materials with pore sizes in the light wavelength range (hundreds of nanometers) will have unique optical properties and other properties, and may be used as photonic bandgap materials in important role in the information industry. Actual industrial catalysts cannot be powder materials, and require particles with a certain size (millimeter or submicron). The mesopores and macropores in these particles are conducive to the diffusion of reactants and products. pore to mesopore to macropore) will have a higher efficiency. [0003] In Anal.Chem.1996, 68 (9): 3498. re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/113C01B33/14
Inventor 赵天波宗保宁郑明芳徐文国雷骞
Owner CHINA PETROLEUM & CHEM CORP
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