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Preparation method of filled gradient hole separation membrane

A gradient hole and separation membrane technology, which is applied in the direction of semipermeable membrane separation, chemical instruments and methods, membranes, etc., can solve the limitations of pressure resistance, high temperature resistance, corrosion resistance and solvent resistance, the limited range of pore gradient changes, and the influence of gradient Porous film application and other issues, to achieve the effect of low cost, excellent chemical stability and thermal stability, excellent mechanical strength

Inactive Publication Date: 2019-04-05
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained gradient pore membrane is limited by the preparation material and preparation method, the range of the pore gradient is limited, and the flux increase is not obvious
Moreover, there are great limitations in terms of pressure resistance, high temperature resistance, corrosion resistance and solvent resistance.
However, the gradient pore membrane prepared by compounding multiple layers of films with different pore diameters has drastic changes in the pore gradient, which is likely to cause concentration polarization in the separation process, and due to the difference in physical and chemical properties of different layers of materials, the membrane layer has poor bonding force and is easy to fall off. , thus affecting the application of the entire gradient pore membrane

Method used

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  • Preparation method of filled gradient hole separation membrane
  • Preparation method of filled gradient hole separation membrane
  • Preparation method of filled gradient hole separation membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Mix 1.0g phenolic resin prepolymer with 1.0g P123 (EO 20 -PO 70 -EO 20 ), 5.0g of zinc chloride dissolved in 21.0g of water, fully stirred, to obtain a filling solution; take 300μL to coat on 5cm 2 The surface of the PVDF base film is placed at 75°C, the solution spontaneously spreads on the surface of the base film, penetrates into the membrane pores and is accompanied by solvent volatilization. After the solvent is completely volatilized, continue to heat and cure at this temperature for 15 hours to obtain a composite film; The composite membrane was placed in 30wt% sulfuric acid and heat-treated at 100°C for 6h.

[0035] figure 1 It is the SEM image of the surface of the filled gradient pore separation membrane prepared in this example. It can be seen from the figure that the phenolic resin can evenly fill the pores of the basement membrane, and the pore size of the membrane surface is uniform.

[0036] figure 2 is a cross-sectional SEM image of the filled grad...

Embodiment 2

[0042] Mix 1.0g phenolic resin prepolymer with 0.5g P104 (EO 27 -PO 61 -EO 27 ), 2.0g of zinc chloride were dissolved in 10.5g of ethanol, and stirred thoroughly to obtain a filling solution; take 100μL and apply it on 5cm 2 The surface of the PVDF base film is placed at 100°C, the solution spontaneously spreads on the surface of the base film, penetrates into the membrane pores and is accompanied by solvent volatilization. After the solvent is completely volatilized, continue to heat and cure at this temperature for 6 hours to obtain a composite film; The composite membrane was placed in 60wt% sulfuric acid and heat-treated at 80°C for 2h.

[0043] The analysis results of the surface SEM image, cross-sectional SEM image, molecular weight cut-off performance graph, inorganic nanoparticle separation performance graph and pressure resistance performance graph of the filled gradient pore separation membrane obtained in this example are similar to those described in Example 1. ...

Embodiment 3

[0046] Mix 1.0g phenolic resin prepolymer with 1.0g F127 (EO 106 -PO 70 -EO 106 ), 10.0g of zinc chloride were dissolved in 36.0g of methanol and stirred thoroughly to obtain a filling solution; take 500μL and coat it on 5cm 2 The surface of the PVDF base film is placed at 100°C, the solution spontaneously spreads on the surface of the base film, penetrates into the membrane pores and is accompanied by solvent volatilization. After the solvent is completely volatilized, continue to heat and cure at this temperature for 6 hours to obtain a composite film; The composite membrane was placed in 45wt% sulfuric acid and heat-treated at 100°C for 10h.

[0047] The analysis results of the surface SEM image, cross-sectional SEM image, molecular weight cut-off performance graph, inorganic nanoparticle separation performance graph and pressure resistance performance graph of the filled gradient pore separation membrane obtained in this example are similar to those described in Example ...

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Abstract

The invention belongs to the technical field of porous material separation membranes, and discloses a preparation method of a filled gradient pore separation membrane. The preparation method includesthe steps of filling liquid preparation, coated filling and pore-forming. Mixture of a phenolic resin prepolymer, zinc chloride and an amphiphilic copolymer serves as a filling medium, and a polyvinylidene fluoride micro-filtration membrane serves as a base membrane for preparing a filled composite membrane. The phenolic resin prepolymer is subjected to hot polymerization in a pore passage of thebase membrane under the synergistic action of the zinc chloride and the copolymer to form closely stacked phenolic resin nano-particles with particle sizes gradually increased from top to bottom, thecopolymer and the zinc chloride are removed by sulfuric acid treatment to form the pore passage with a pore diameter in gradient change, and the filled gradient pore membrane is prepared. The gradientpore membrane is large in flux and high in selectivity and has good high-temperature resistance, corrosion resistance and organic solvent resistance. Needed raw materials are low in price and easy toobtain, the preparation process is simple and convenient, and the obtained gradient pore membrane has a good application prospect in the fields of substance separation, refinement, purification and the like.

Description

technical field [0001] The invention belongs to the technical field of porous material separation membranes, and in particular relates to a preparation method of a filled phenolic resin gradient pore separation membrane. Background technique [0002] Gradient pore membrane is one of the most ideal membrane materials, and its pore size changes step by step from the surface of the membrane to the bottom of the membrane. The pore size on the surface of the membrane is small and evenly distributed, which plays a role of separation; the pore size below the surface of the membrane gradually increases, which is beneficial to reduce the mass transfer resistance and plays a supporting role. Due to these structural features, the gradient pore membrane can obtain high flux while maintaining high rejection. Gradient pore membranes are often prepared by phase inversion of polymer materials or by compounding multiple layers of membranes with different pore sizes. The phase inversion met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/34B01D67/00B01D69/10
CPCB01D67/00B01D69/10B01D71/34B01D2325/24B01D2325/30
Inventor 汪勇兰倩倩
Owner NANJING UNIV OF TECH