MXene based compositing nanofiltration membrane and corresponding preparation method

Abstract

The present invention belongs to the membrane separation area, which provides an MXene material based composite nanofiltration membrane and corresponding method. The mentioned membrane is flat membrane, which has supporting layer and functional separation layer and supporting layer is under the functional separation layer. The functional separation layer is a kind of dense ultra-thin layer, no more than 50 m, prepared with MXene and crosslinking agent. This invention is about a flat composite nanofiltration membrane which has excellent separation performance, thermal resistance and chemical stability because of the novel MXene in the functional separation layer. It can be used in the treatment of the waste water with heavy metal ions, organic solvents or other highly oxidizing solution.

Claims

1. An MXene based composite nanofiltration membrane, wherein the composite nanofiltration membrane is a flat structure, comprising a supporting layer below a separation functional layer; the functional layer is a dense thin membrane made of the MXene and a crosslinking agent below 50 m; the crosslinking agent is glutaraldehyde, epoxy chloropropane, epoxy propyl trimethylammonium chloride, trimesoyl chloride, phthaloyl chloride, isophthaloyl dichloride, paraphthaloyl chloride, or hexanedioyl chloride; the supporting layer is made of cellulose derivative, polysulfone, polyether sulfone, polyethylene sulfone, polyacrylonitrile, polyvinyl chloride, polyvinylidene chloride, polyimide, polyetherimide, or a combination thereof; a thickness of the supporting layer is between 50-500 m with pores about 100 nm.

2. The MXene based composite nanofiltration membrane according to claim 1, wherein the dense thin functional layer also has inorganic and/or organic additives.

3. The MXene based composite nanofiltration membrane according to claim 2, wherein the inorganic additives are one or a mixture of nanosized silica, alumina, titanium oxide, ferriferrous oxide, lanthanum strontium cobalt iron, zeolite, graphene and inorganic salt; the organic additives are one or a mixture of chitosan quaternary ammonium salt, cellulose quaternary ammonium salt, cellulose acetate, polyvinyl alcohol, polyethylene glycol, carboxymethylcellulose, polyvinylidene fluoride, polydimethyl diallyl ammonium chloride and sodium polyacrylate.

4. The MXene based composite nanofiltration membrane according to claim 3, wherein the supporting layer is made of polymer or inorganic porous membrane.

5. A preparation method of the MXene based composite nanofiltration membrane of claim 2, comprising steps as follows: (1) separation of MXene Ti.sub.3AlC.sub.2 is slowly dissolved in 50 wt. % HF solution with strong stirring, and a disperse solution A is obtained after 12 h; the concentration of Ti.sub.3AlC.sub.2 is between 5-20 wt. %; the disperse solution A is centrifugal separated, washed, filtered and dried to obtain the MXene material; the prepared MXene is added into the dimethyl sulfoxide solution and peeled off with ultrasonication; then inorganic and/or organic additives are added in to form a disperse solution B; the ultrasonication time is between 2-12 hours and the concentration of MXene is between 1-5 wt. % while the additive concentration is 2 wt. %; (2) separation of functional layer of the composite nanofiltration membrane the supporting layer is used as a filter membrane; disperse solution B is diluted with water and filtered with the supporting layer with pressure or evacuation; the formed functional layer is 50 m in thickness; the concentration of MXene is between 0.1-2 wt. % in the diluted disperse solution B; the inorganic additive and/or organic additive concentration is below 2 wt. %; the MXene based composite nanofiltration membrane is formed with the filtered membrane being air-dried, blown or dried at high temperature; (3) the prepared MXene based composite membrane is immersed in the crosslinking agent solution with 0.1-2 wt. % concentration; then the membrane is post treated at 20-100 C. for 2-30 min to form stable MXene based composite nanofiltration membrane.

Description

DETAILED DESCRIPTION

(1) Follow technology process is used to further explain the method.

Example 1

(2) 1. Preparation of Disperse Solution

(3) Prepared MXene is added into dimethyl sulfoxide solution and peeled off with ultrasonication. Then additives are added form disperse solution B. The ultrasonication time is between 2-12 h and the concentration of MXene is 1 wt. % while the additive concentration of nanosized silica and carboxymethylcellulose is 0.5 wt. %.

(4) 2. Preparation of Functional Layer of Composite Nanofiltration Membrane

(5) Polymer or porous inorganic membrane is used as filter membrane. Disperse solution B is diluted with water and filtered with filter membrane to form functional layer with fixed thickness. Then the membrane is air-dried, blown or dried at high temperature.

(6) Then the membrane is soaked in the 1 wt. % glutaraldehyde solution for 10 seconds, and dried at 60 C. for 5 min.

(7) 3. Application

(8) The membrane is used to treat 1 g/L MgCl.sub.2 solution, under 0.3 MPa, the rejection to MgCl.sub.2 is 96% with a flux of 10 L/m.sup.2 h.

Example 2

(9) 1. Preparation of Disperse Solution

(10) Prepared MXene is added into dimethyl sulfoxide solution and peeled off with ultrasonication. Then additives are added form disperse solution B. The ultrasonication time is between 2-12 h and the concentration of MXene is 3 wt. %.

(11) 2. Preparation of Functional Layer of Composite Nanofiltration Membrane

(12) Polymer or porous inorganic membrane is used as filter membrane. Disperse solution B is diluted with water and filtered with filter membrane to form functional layer with fixed thickness. Then the membrane is air-dried, blown or dried at high temperature.

(13) Then the membrane is soaked in the 0.5 wt. % isophthaloyl dichloride solution for 10 seconds, and dried at 60 C. for 5 min.

(14) 3. Application

(15) The membrane is used to treat 1 g/L MgCl.sub.2 solution, under 0.3 MPa, the rejection to MgCl.sub.2 is 92% with a flux of 12 L/m.sup.2 h.