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Oxidized graphene/mesoporous silica compound ultrafiltration membrane preparation method and application thereof

A technology of mesoporous silica and ultrafiltration membrane, which is applied in the preparation method of peptides, chemical instruments and methods, ultrafiltration, etc., can solve the problems of increased flux and interception, side effects, and easy agglomeration, and achieve increased mechanical properties and thermal stability effects

Pending Publication Date: 2019-01-25
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, pure SBA-15 also has some shortcomings. It improves the flux and interception of the membrane, but the range is not particularly large, and the small amount of SBA-15 increases the hydrophilicity and also makes the membrane easy to be polluted. Large doses of SBA-15 tend to agglomerate inside the polymer and cause side effects

Method used

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  • Oxidized graphene/mesoporous silica compound ultrafiltration membrane preparation method and application thereof
  • Oxidized graphene/mesoporous silica compound ultrafiltration membrane preparation method and application thereof
  • Oxidized graphene/mesoporous silica compound ultrafiltration membrane preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] ①Activation of SBA-15: Take 1 g of dry SBA-15 and disperse it in 2mol / L HCl solution, reflux at 80°C for 24h, wash with distilled water three times, then vacuum dry at 80°C for 12h to obtain activated SBA-15.

[0034] ② Amination modification of SA-15: Disperse 1 g of dry activated SBA-15 in 40 mL of anhydrous toluene, and then add 0.9 mL of APTES dropwise to the solution. The mixed system was condensed and refluxed at 100° C. for 12 h under the protection of nitrogen. The product was washed three times with toluene and ethanol, and finally dried under vacuum at 50 °C for 12 h to obtain NH 2 -SBA-15.

[0035] ③ Preparation of GO-SBA-15: Graphene oxide was prepared by improving the Hummers method. Take 0.05g GO and disperse in 100mL DMF, and ultrasonicate vigorously for 30min. Subsequently, 0.2 g NH 2 -SBA-15 and 0.04g DCC, 40°C water bath for 24h. Finally, the product was washed three times with DMF and ethanol, and dried under vacuum at 50 °C for 12 h to obtain GO...

Embodiment 2

[0039] ①Activation of SBA-15: Take 1 g of dry SBA-15 and disperse it in 2mol / L HCl solution, reflux at 80°C for 24h, wash with distilled water three times, then vacuum dry at 80°C for 12h to obtain activated SBA-15.

[0040] ② Amination modification of SA-15: Disperse 1 g of dry activated SBA-15 in 40 mL of anhydrous toluene, and then add 1.4 mL of APTES dropwise to the solution. The mixed system was condensed and refluxed at 100° C. for 12 h under the protection of nitrogen. The product was washed three times with toluene and ethanol, and finally dried under vacuum at 50 °C for 12 h to obtain NH 2 -SBA-15.

[0041] ③ Preparation of GO-SBA-15: Graphene oxide was prepared by improving the Hummers method. Take 0.08g GO and disperse it in 100mL DMF, and intensify sonication for 30min. Subsequently, 0.2 g NH 2 -SBA-15 and 0.04g DCC, 40°C water bath for 24h. Finally, the product was washed three times with DMF and ethanol, and dried under vacuum at 50 °C for 12 h to obtain GO-...

Embodiment 3

[0045] ①Activation of SBA-15: Take 1 g of dry SBA-15 and disperse it in 2mol / L HCl solution, reflux at 80°C for 24h, wash with distilled water three times, then vacuum dry at 80°C for 12h to obtain activated SBA-15.

[0046] ② Amination modification of SA-15: Disperse 1 g of dry activated SBA-15 in 40 mL of anhydrous toluene, and then add 0.9 mL of APTES dropwise to the solution. The mixed system was condensed and refluxed at 100° C. for 12 h under the protection of nitrogen. The product was washed three times with toluene and ethanol, and finally dried under vacuum at 50 °C for 12 h to obtain NH 2 -SBA-15.

[0047] ③ Preparation of GO-SBA-15: Graphene oxide was prepared by improving the Hummers method. Take 0.05g GO and disperse in 100mL DMF, and ultrasonicate vigorously for 30min. Subsequently, 0.2 g NH 2 -SBA-15 and 0.04g DCC, 40°C water bath for 24h. Finally, the product was washed three times with DMF and ethanol, and dried under vacuum at 50 °C for 12 h to obtain GO...

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Abstract

The invention belongs to the technical field of material preparation and separation and relates to an oxidized graphene / mesoporous silica compound ultrafiltration membrane preparation method and application thereof. The preparation method disclosed by the invention comprises the following steps: firstly, utilizing oxidized graphene, SBA-15, 3-aminopropyl triethoxysilane and dicyclohexyl carbodiimide to prepare a GO-SBA-15 inorganic hybrid material; then mixing polysulfone PSF, polyvinyl pyrrolidone PVP and GO-SBA-15 into N,N-dimethyl formamide DMF to obtain a membrane casting solution, coatingand forming the membrane casting solution on a glass plate through a flow casting method; finally, dipping into prepared coagulating bath to finish a phase separation process to obtain a modified polysulfone ultrafiltration membrane. The water flux of the GO-SBA-15 / PSF ultrafiltration membrane prepared by the preparation method disclosed by the invention is remarkably improved; meanwhile, antifouling property of the GO-SBA-15 / PSF ultrafiltration membrane is obviously enhanced; the GO-SBA-15 / PSF ultrafiltration membrane has good thermal stability, is suitable for rigorous industrialized application environments and can be hopefully applied to industrial water treatment.

Description

technical field [0001] The invention belongs to the technical field of material preparation and separation, and relates to a preparation method and application of a graphene oxide / mesoporous silicon dioxide composite ultrafiltration membrane. Background technique [0002] In recent years, ultrafiltration technology has been widely used in the concentration, purification and separation of various products in food, medical, paper products, bioindustry and other fields, or as a pretreatment technology before reverse osmosis, and has received more and more attention. focus on. However, most of the commercial ultrafiltration membranes currently on the market are made of hydrophobic polymers, such as polysulfone (PSF); polyethersulfone (PES); polypropylene (PP); polyvinylidene fluoride (PVDF) Wait. On the one hand, limited by the hydrophilicity of the surface, the flux they are used in ultrafiltration technology is generally low, and the low flux of the membrane will greatly inc...

Claims

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Application Information

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IPC IPC(8): B01D71/68B01D69/02B01D61/14B01D67/00C07K14/765C07K1/34
CPCB01D61/145B01D67/0011B01D67/0013B01D67/0016B01D69/02B01D71/68B01D2325/22B01D2325/24B01D2325/36C07K14/765
Inventor 刘建益刘燕李宇龙倪良
Owner JIANGSU UNIV
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