Polyamide (PA) nanofiltration (NF) membrane, and preparation method thereof by regeneration from scrapped microfiltration (MF) membrane

Patent metadata

Field	Value
Publication number	US-11628405-B2
Application number	US-202117325236-A
Country	US
Kind code	B2
Filing date	May 20, 2021
Priority date	Feb 24, 2021
Publication date	Apr 18, 2023
Grant date	Apr 18, 2023

Abstract

A polyamide (PA) nanofiltration (NF) membrane and a preparation method thereof by regeneration from a scrapped microfiltration (MF) membrane are provided. The method adopts a cleaning-repairing-interfacial polymerization upgrading strategy, where, sodium hypochlorite and oxalic acid are used for deeply cleaning a scrapped MF membrane. PDA is used as a repairing agent to construct a reaction platform on the membrane surface, and finally a reaction system of piperazine and trimesoyl chloride (TMC) are used to form a PA NF membrane with a PA active layer. The repairing can construct a coating with a given thickness and prominent hydrophilicity on the membrane surface, which provides favorable base membrane conditions for upgrading and preparing an NF membrane.

First claim

What is claimed is:

1. A preparation method of a polyamide (PA) nanofiltration (NF) membrane by a regeneration from a scrapped microfiltration (MF) membrane, comprising the following steps:
1) subjecting the scrapped MF membrane to a preliminary hydraulic cleaning for 10 min to 30 min to remove large mud cakes attached to a surface of the scrapped MF membrane to obtain a first cleaned MF membrane;
2) performing a deep cleaning on the first cleaned MF membrane by a chemical cleaning, wherein, the first cleaned MF membrane is placed in a cup-shaped reaction vessel and reacted with a solution A for a first reaction for 1 h to 3 h to obtain a second cleaned MF membrane; after the first reaction is completed, the solution A is poured out; and then the second cleaned MF membrane is reacted with a solution B for a second reaction for 1 h to 3 h to obtain a third cleaned MF membrane;
3) placing the third cleaned MF membrane cleaned in step 2) in a cylindrical reaction vessel, pouring a solution C into the cylindrical reaction vessel to obtain a resulting mixture, and subjecting the resulting mixture to a third reaction at 25° C. to 30° C. for 12 h to 36 h under a shaking to obtain a repaired MF membrane, wherein the solution C is a polydopamine (PDA) solution with a concentration of 1 g/L to 5 g/L, a solvent in the solution C is a mixture of an aqueous tris(hydroxymethyl)aminomethane (THAM) solution and an aqueous hydrochloric acid solution with a mass fraction of 36%, and THAM has a concentration of 0.5 g/L to 1.5 g/L in the aqueous THAM solution; and
4) at a porous side of the repaired MF membrane obtained in step 3), preparing an active layer by an interfacial polymerization, wherein preparation steps specifically include: dissolving imine monomer in water to obtain a solution D, soaking the repaired MF membrane in the solution D as a support layer for 1 min to 5 min and then taking out the repaired MF membrane to obtain a resulting composite, and removing excess liquid droplets on a surface of the resulting composite with a rubber roller; soaking the resulting composite in a solution E for the interfacial polymerization for 30 s to 90 s to obtain a membrane product; and finally drying the membrane product in an oven at 60° C. to 80° C. for 1 min to 10 min to obtain the PA NF membrane.

2. The preparation method of the PA NF membrane by the regeneration from the scrapped MF membrane according to claim 1 , wherein the solution A is an aqueous sodium hypochlorite solution with a mass concentration of 1.05% to 8.39%.

3. The preparation method of the PA NF membrane by the regeneration from the scrapped MF membrane according to claim 1 , wherein the solution B is an aqueous oxalic acid solution with a mass fraction of 0.5% to 4.0%.

4. The preparation method of the PA NF membrane by the regeneration from the scrapped MF membrane according to claim 1 , wherein the imine monomer in the solution D is piperazine, and the solution D is an aqueous piperazine solution with a mass volume fraction of 0.04% to 0.4%.

5. The preparation method of the PA NF membrane by the regeneration from the scrapped MF membrane according to claim 1 , wherein the solution E is a solution of trimesoyl chloride (TMC) in n-hexane with a mass volume fraction of 0.04% to 0.4%.

6. The preparation method of the PA NF membrane by the regeneration from the scrapped MF membrane according to claim 1 , wherein the scrapped MF membrane is a scrapped polyvinylidene fluoride (PVDF) MF membrane or a scrapped polyethersulfone (PES) MF membrane.

Assignees

• Univ Tongji

Inventors

• Wang Zhiwei
• Han Hongyi
• Dai Ruobin
• Wang Tianlin
• Tian Chenxin

Classifications

• B01D67/0095

  Drying · CPC title

• B01D2321/168

  Use of other chemical agents · CPC title

• B01D61/027 Primary

  Nanofiltration · CPC title

• B01D71/56

  Polyamides, e.g. polyester-amides · CPC title

• B01D65/108

  Repairing membranes · CPC title