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Polymer catalytic membrane containing palladium metal active functional layer and preparation method thereof

A metal active and catalytic membrane technology, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the complex modification process and difficult to control the loading of nano-metal particles and other problems, to achieve the effect of convenient preparation, stable performance and high catalytic stability

Inactive Publication Date: 2014-10-22
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the modification process of the above method is relatively complicated, and it is not easy to control the loading amount of nano-metal particles.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. The preparation method of polyacrylonitrile flat base film is as follows:

[0030] (1) Dissolve the mass fraction of 2wt% PEG (molecular weight 2000) and 0.5wt% PVP in a certain amount of DMF solvent under the condition of 50°C water bath, and fully stir to dissolve. Then dissolve 20wt% polyacrylonitrile (PAN) powder in the above solvent, put it in a water bath at 50°C for about 24 hours to remove microbubbles, and obtain a casting solution;

[0031] (2) Pour the casting solution on a clean flat glass plate, and scrape it evenly to form a film with a stainless steel metal rod;

[0032] (3) Place the film scraped on the glass plate in the air for about 30s, then immerse the glass plate in deionized water to solidify into a flat film;

[0033] (4) Soak the prepared flat base film in absolute ethanol for 12 hours to remove the residual solvent in the film.

[0034] 2. The preparation method of metal-containing palladium catalytic membrane is as follows:

[0035] (1) ...

Embodiment 2

[0042] The difference between this embodiment and Example 1 is that during the preparation of the metallic palladium-containing catalytic membrane, the prepared flat base membrane is taken out from absolute ethanol, put into a NaOH solution with a concentration of 1.5mol / L, and heated at 45°C Stand still for 1.5h under water bath conditions, and carry out charging treatment.

[0043] Catalytic performance measurement: Put the assembled catalytic membrane into a flat membrane separation device. Prepare 0.1mmol / L p-nitrophenol solution, then add KBH 4 Solution, make its concentration in the solution reach 10mmol / L, and adjust the pH to 10 with NaOH solution. Place the above mixed solution in a water bath and control the temperature to 45°C and enter the membrane separation device with a working pressure of 0.05Mpa. Take the permeated membrane solution and analyze and measure the concentration of p-nitrophenol with a UV-visible spectrophotometer to measure the concentration of t...

Embodiment 3

[0045] The difference between this embodiment and Example 1 is that during the preparation of the metallic palladium-containing catalytic membrane, the prepared flat base membrane is taken out from absolute ethanol, put into a NaOH solution with a concentration of 1.5mol / L, and heated at 45°C Stand still for 1.5h under water bath conditions, and carry out charging treatment. The molar ratio of PEI and Pd(II) ions in the coordination solution of PEI and Pd(II) ions is 15:2. The treated plate basement membrane was soaked in PEI-Pd(II) solution for 10 minutes, fully cleaned the surface with deionized water after taking it out, gently blotted the water on the surface of the membrane with filter paper, then put it in PSS solution and soaked it for 10 minutes, and took it out with Fully wash the surface with deionized water, and gently blot the moisture on the surface of the membrane with filter paper, thus completing the assembly of one layer. Follow the above steps to assemble 8 ...

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Abstract

The invention relates to a polymer catalytic membrane containing a palladium metal activity functional layer prepared based on the technology of layer-by-layer self assembly and a preparation method thereof, which belongs to the field of catalytic membranes. According to the invention, polyacrylonitrile (PAN) powder, polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP) are dissolved in N,N-dimethyl formamide (DMF), and a PAN flat base membrane is prepared by using a phase inversion process; then the PAN membrane is soaked in a NaOH solution for treatment, which allows surface of the membrane to hydrolyze so as to produce carboxyl groups, thereby enabling the surface of the membrane to carry negative electric charges; a polyethyleneimine (PEI) solution and a potassium chloropalladate K2PdCl4 solution are fully mixed and react for a certain period of time so as to obtain a coordination compound of polyethyleneimine-palladium (PEI-Pd(II)); the treated flat base membrane is alternatively soaked in a solution containing the PEI-Pd(II) coordination compound and a polystyrene sulfonate (PSS) solution for self-assembly of functional layers on the surface of the membrane, and the amount of the assembled layers is controlled; and finally, the membrane obtained after assembly is soaked in a potassium borohydride KBH4 solution, Pd(II) is reduced to be Pd0, and the PAN catalytic membrane containing the palladium metal particle active layer is prepared.

Description

technical field [0001] The invention belongs to the field of catalytic separation membranes, and in particular relates to a palladium-containing catalytic membrane prepared based on a layer-by-layer self-assembly technology. The catalytic membrane can be used for the catalytic conversion of low-concentration p-nitrophenol in environmental water. Background technique [0002] Nanoscale noble metal catalysts have a large specific surface area and high surface reactivity, and play a huge role in the field of environmental catalysis. However, the reaction performance is reduced due to the fact that nanoscale metals are prone to agglomeration or oxidation. In the process of degrading pollutants in water by using the catalytic performance of nano-metal particles, nanoparticles can be fixed on some carriers to ensure good dispersion and reactivity of nanoparticles. Solid supports that can disperse particles include activated carbon, metal oxides, zeolites, or polymer membranes. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/42B01J31/28C07C215/76C07C213/02
Inventor 张环麻晓越郑莹雪张潮
Owner TIANJIN POLYTECHNIC UNIV
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