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A kind of nh2-mil-125/pod-cooh ultra-thin homogeneous hybrid forward osmosis membrane and preparation method thereof

A technology of NH2-MIL-125 and POD-COOH, applied in chemical instruments and methods, semi-permeable membrane separation, permeation/dialysis water/sewage treatment, etc., can solve damage, poor mechanical strength, and eliminate concentration difference in the support layer Polarization and other issues, to achieve the effect of broad application prospects, high water permeability, excellent water permeability and salt retention performance

Active Publication Date: 2021-08-03
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the forward osmosis membranes with the above characteristics often have poor mechanical strength, are easily damaged during use, and have not fundamentally eliminated the internal concentration polarization phenomenon of the support layer.

Method used

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  • A kind of nh2-mil-125/pod-cooh ultra-thin homogeneous hybrid forward osmosis membrane and preparation method thereof
  • A kind of nh2-mil-125/pod-cooh ultra-thin homogeneous hybrid forward osmosis membrane and preparation method thereof
  • A kind of nh2-mil-125/pod-cooh ultra-thin homogeneous hybrid forward osmosis membrane and preparation method thereof

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preparation example Construction

[0035] The invention provides a kind of NH 2 -The preparation method of MIL-125 / POD-COOH ultra-thin homogeneous hybrid forward osmosis membrane, specifically comprising:

[0036] Step 1: Add butyl titanate and 2-amino-terephthalic acid to a mixed solution of N,N-dimethylformamide (DMF) and methanol, stir at room temperature for 3 to 5 hours, then transfer to 40 ml In a polytetrafluoroethylene-lined stainless steel reaction kettle, place it in a temperature-programmed oven at 140-150°C for 24-48 hours. After naturally cooling to room temperature, wash with N,N-dimethylformamide (DMF) for 3 to 5 times and then with methanol for 3 to 5 times, each solution is 20 to 30 ml, and the time is 2 to 3 hours , to obtain MOFs material NH 2 -MIL-125;

[0037] Step 2: Hydrazine sulfate (N 2 h 4 ·H 2 SO 4 ) and polyphosphoric acid (PPA) were added to a three-neck flask equipped with a mechanical stirrer, a nitrogen vent, a thermometer, a Dean-Stark water dispenser and a condenser tube...

Embodiment 1

[0054] 1) Butyl titanate (0.84 mL, 0.75 mmol) and 2-amino-terephthalic acid (1.5 g, 3 mmol) were added to 10 mL of N,N-dimethylformamide (DMF) and methanol in the mixed solution (V (DMF) :V (甲醇) 1:1), stirred at room temperature for 3 hours, transferred to a 40 ml polytetrafluoroethylene-lined stainless steel reaction kettle, and placed in a temperature-programmed oven at 150°C for 24 hours. After naturally cooling to room temperature, wash with N,N-dimethylformamide (DMF) for 3 times and then with methanol for 3 times, each solution is 20 ml for 2 hours, and then put into Dry in a vacuum oven at 150°C for 12 hours to obtain the MOFs material NH 2 -MIL-125. figure 2 The MOFs material NH prepared for Example 1 of the present invention 2 -XRD pattern of MIL-125, such as figure 2 As shown, the five peaks at 6.8°, 9.8°, 11.6°, 16.6°, 17.6° and 17.9° in the XRD pattern of the synthesized MOF particles are respectively attributed to (101), (200), (211) , (222) and (312) crys...

Embodiment 2

[0061] 1) the method described in 1) of embodiment 1 makes NH 2 -MIL-125 material.

[0062] 2) Polyoxadiazole material (POD) was prepared by the method described in 2) of Example 1.

[0063] 3) The method described in 3) of Example 1 makes carboxyl-containing polyoxadiazole material (POD-COOH)

[0064] 4) Dissolve the above-mentioned carboxyl-containing polyoxadiazole material (0.5 g, 0.002 mole) in 30 ml of anhydrous DMF solvent. After the polymer is completely dissolved, it is added dropwise to the solution containing EDC (0.068 g, 0.355 mmol) , NHS (0.0035 g, 0.03 mmol) and NH 2 -In 5 milliliters of anhydrous DMF of MIL-125 material (0.05 g), about 2 hours after the dropwise addition is completed, continue to stir at room temperature for 72 hours, and discharge in n-hexane to obtain 10% NH 2 - MIL-125 / POD-COOH hybrid material.

[0065] 5) The 10% NH prepared above 2 -The MIL-125 / POD-COOH hybrid material was dissolved in DMF solvent to ensure that the mass fraction of t...

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Abstract

The invention provides a method for preparing an NH2-MIL-125 / POD-COOH ultra-thin homogeneous hybrid forward osmosis membrane, which belongs to the technical field of polymer materials. The present invention first prepared MOFs material (NH 2 ‑MIL‑125), polyoxadiazole (POD) materials and carboxyl-containing polyoxadiazole (POD‑COOH) materials, NH 2 ‑MIL‑125 material was introduced into the molecular structure of carboxyl-containing polyoxadiazole material through chemical bonding, and a series of NH 2 ‑MIL‑125 / POD‑COOH hybrid forward osmosis membrane material, as shown in Figure 1, and then use the above material to prepare ultra-thin homogeneous hybrid forward osmosis membrane by solution casting method. Finally, a preparation method of NH2‑MIL‑125 / POD‑COOH hybrid forward osmosis membrane is provided. Since there is no support layer in this type of forward osmosis membrane, the internal concentration polarization phenomenon in the process of forward osmosis separation operation can be eliminated, and the efficiency of forward osmosis water treatment can be greatly improved. In addition, the introduction of porous hydrophilic MOFs materials with high efficient sieving performance for water and salt enhanced the water permeability and desalination performance of the hybrid membrane during the forward osmosis separation operation. In summary, this type of material will have broad application prospects in the fields of seawater desalination and brackish water treatment.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a NH 2 -MIL-125 / POD-COOH ultra-thin homogeneous hybrid forward osmosis membrane and its preparation method. Background technique [0002] In recent years, water security issues and the development of low-energy water treatment technologies have received great attention. Among many water treatment technologies, membrane method is considered to be a very promising type of water treatment technology. Forward Osmosis (FO) membrane separation technology is an emerging membrane water treatment technology. This technology uses the osmotic pressure difference of the solution on both sides of the membrane as the driving force for water separation operation. It has high water recovery rate, low pollution tendency, With the advantages of low energy requirement and easy operation, it has shown good development prospects in the fields of food concentration, drug release, and seawa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/62B01D67/00B01D61/00C02F1/44C02F103/08
CPCB01D61/002B01D67/0006B01D71/62C02F1/445C02F2103/08Y02A20/131
Inventor 耿直何男刘威杨霞赵永杰刘楚汉刘倩梁世强
Owner NORTHEAST NORMAL UNIVERSITY