Preparation method of carboxylated graphene oxide nanofiltration membrane with controllable flux

A carboxylation and nanofiltration membrane technology, applied in the field of composite membrane materials, can solve the problems such as the flux is not greatly improved, the preparation method is complicated, and the effect of low production cost, simple preparation process and good separation performance is achieved.

Active Publication Date: 2021-06-01
WUHAN INSTITUTE OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although the above method has a relatively high rejection rate, the flux has not been greatly improved, and the preparation method is relatively complicated.

Method used

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  • Preparation method of carboxylated graphene oxide nanofiltration membrane with controllable flux
  • Preparation method of carboxylated graphene oxide nanofiltration membrane with controllable flux

Examples

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Effect test

Embodiment 1

[0023] First, 15mL of hydrobromic acid (HBr) was added to 90mL of graphene oxide (GO) solution, stirred continuously for 12h, then 8g of oxalic acid was added to the above mixture, stirred continuously for 4h, and dialyzed for 1 week to obtain CFGO solution (5mg / mL), take 0.5mL of the prepared CFGO solution in a 50mL volumetric flask, add 1mL of 1mol / L MXDA aqueous solution, dilute to 50mL with deionized water, the molar concentration of MXDA in the mixed solution is 0.02mol / L, vacuum pump Filter the mixture of CFGO and MXDA on the surface of the PES base membrane. After rinsing, soak in 20ml 0.1mol / L TMC / n-hexane solution to obtain a composite membrane. The molar concentration ratio of MXDA aqueous solution to TMC / n-hexane solution is 0.2 , the interlayer distance (d-spacing) of the obtained composite membrane is 0.856nm, and the pure water flux (Water Flux) is 134L / m under the pressure of 0.5Mpa 2 h, for calcium chloride (CaCl 2 ) The rejection rate (Salt Rejection) is 82%...

Embodiment 2

[0025] First, 15mL of hydrobromic acid (HBr) was added to 90mL of graphene oxide (GO) solution, stirred continuously for 12h, then 8g of oxalic acid was added to the above mixture, stirred continuously for 4h, and dialyzed for 1 week to obtain CFGO solution (5mg / mL), take 0.5mL of the prepared CFGO solution in a 50mL volumetric flask, add 2mL of 1mol / L MXDA aqueous solution, dilute to 50mL with deionized water, the molar concentration of MXDA in the mixed solution is 0.04mol / L, and vacuum Filter the mixture of CFGO and MXDA on the surface of the PES base membrane. After rinsing, soak in 20ml 0.1mol / L TMC / n-hexane solution to obtain a composite membrane. The molar concentration ratio of MXDA aqueous solution to TMC / n-hexane solution is 0.4 , the interlayer distance (d-spacing) of the obtained composite membrane is 0.912nm, and the pure water flux is 178L / m under the pressure of 0.5MPa 2 h, for CaCl 2 The rejection rate is 88%.

Embodiment 3

[0027] First, 15mL of hydrobromic acid (HBr) was added to 90mL of graphene oxide (GO) solution, stirred continuously for 12h, then 8g of oxalic acid was added to the above mixture, stirred continuously for 4h, and dialyzed for 1 week to obtain CFGO solution (5mg / mL), take 0.5mL of the prepared CFGO solution in a 50mL volumetric flask, add 4mL of 1mol / L MXDA aqueous solution, use deionized water to set the volume to 50mL, the molar concentration of MXDA in the mixed solution is 0.08mol / L, vacuum pump Filter the mixture of CFGO and MXDA on the surface of the PES base membrane. After rinsing, soak in 20ml 0.1mol / L TMC / n-hexane solution to obtain a composite membrane. The molar concentration ratio of MXDA aqueous solution to TMC / n-hexane solution is 0.8 , the interlayer distance (d-spacing) of the obtained composite membrane is 0.965nm, and the pure water flux is 200L / m under the pressure of 0.5Mpa 2 h, for CaCl 2 The rejection rate is 96%.

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Abstract

The invention discloses a preparation method of a carboxylated graphene oxide nanofiltration membrane with controllable flux. Add m-xylylenediamine to the carboxylated graphene oxide solution, and ultrasonically obtain a uniform mixed solution; the mixed solution is plated on the surface of the polyethersulfone base membrane by the method of auxiliary pressure vacuum self-assembly to obtain a composite membrane, and deionized water is used to Cleaning several times; the auxiliary pressure vacuum self-assembly is to place the polyethersulfone base membrane on a sand core funnel to vacuum filter the mixed solution; immerse the obtained composite membrane in the solution of trimesoyl chloride / n-hexane After the m-xylylenediamine on the carboxylated graphene oxide sheet fully reacts with trimesoyl chloride, the membrane is washed several times with n-hexane solution and dried to obtain the required composite nanofiltration membrane. The selective layer of the composite nanofiltration membrane uses polyamide cross-linked carboxylated graphene oxide sheets, and the chain length and structure of the polyamide are controlled by adjusting the monomer ratio. The distance between the carboxylated graphene oxide sheets of the selective layer is controllable. The flux is controllable.

Description

technical field [0001] The invention belongs to the technical field of composite membrane materials, and in particular relates to a preparation method of a carboxylated graphene oxide nanofiltration membrane with controllable flux. Background technique [0002] Since the 21st century, with the gradual increase of the population on the earth, domestic wastewater and industrial wastewater have also been increasing, and the problem of shortage of clean water resources needs to be solved urgently. The emergence of membrane separation technology has given great help to the treatment of this serious problem. The technology aims to remove pollutants from wastewater to address global water scarcity. Polyamide (PA) nanofiltration membrane is the most commercially used recently. PA membrane can be used as a selective layer to increase the flux of pure water and increase the salt rejection rate. The method used in the preparation of PA is interfacial polymerization, which is mainly t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/56B01D69/12B01D69/02B01D67/00B01D61/00
CPCB01D61/027B01D67/0079B01D69/02B01D69/125B01D71/56B01D2323/50B01D2325/36
Inventor 熊芸彭俊龙刘生鹏孙国锋吴晓宇蔡师
Owner WUHAN INSTITUTE OF TECHNOLOGY
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