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Preparation method of superhydrophobic super-lipophilic nanofiber membrane based on layer-by-layer self-assembly technology for oil-water mixture separation

An oil-water separation membrane, layer-by-layer self-assembly technology, applied in separation methods, membrane technology, liquid separation, etc., can solve problems such as lack of mechanical integrity, and achieve the effect of improving oil-water separation performance

Inactive Publication Date: 2018-11-09
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] A common disadvantage of electrospun superhydrophobic porous microsphere / nanofiber membranes is the lack of mechanical integrity

Method used

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  • Preparation method of superhydrophobic super-lipophilic nanofiber membrane based on layer-by-layer self-assembly technology for oil-water mixture separation
  • Preparation method of superhydrophobic super-lipophilic nanofiber membrane based on layer-by-layer self-assembly technology for oil-water mixture separation
  • Preparation method of superhydrophobic super-lipophilic nanofiber membrane based on layer-by-layer self-assembly technology for oil-water mixture separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] equipped with mechanical stirrer, thermometer, N 2 Add BPDA and PDA to the dry four-necked flask leading out the inlet and outlet tubes, and mix well. Under vigorous mechanical stirring, DMAc was added. After reacting at -5°C for 12 hours, the phenomenon of rod climbing began to appear, and then the reaction was terminated by exposing the reaction to air.

[0021] The preparation of polyamic acid (PAA) fiber film uses the DMAc solution of 3wt%PAA, contains the hexadecyltrimethylammonium bromide (increasing electrical conductivity) of 1‰ (wt%), at voltage 25kV (+15, Spinning in a high-voltage electrostatic field of -10kV), the distance from the needle point to the drum is about 15cm, the collector is a grounded flywheel with adjustable speed, the speed is 2000 rpm, and the speed of electrospinning is 0.35ml / h, such as figure 1 shown. The electrospun polyamic acid fiber membrane was subjected to 150°C / 1h, 200 / 1h, 250°C / 1h, 300°C / 1h, 350°C / 30mim in a tube furnace protec...

Embodiment 2

[0023] (1) Accurately weigh 2.7029g of ferric chloride hexahydrate solid, dissolve it in deionized water, and set the volume to 0.1mol / L solution.

[0024] (2) Take 1 mL of 70% phytic acid solution and dissolve it with 99 mL of deionized water.

[0025] (3) Octadecyltrimethoxysilane was dissolved in tetrahydrofuran to prepare a solution with a mass concentration of 1% for later use.

[0026] (4) Immerse the membrane in the PA solution for 2 minutes, take it out, wash it with deionized water, and dry it in the air

[0027] (5) Immerse the dried film in ferric chloride solution for 2 minutes, take it out and wash it with deionized water, and dry it in the air

[0028] (6) Repeat this 5 times to ensure that the self-assembly effect can reach the expected goal

[0029] (7) Vacuum drying and curing for 2 hours at 80°C

[0030] (8) Take it out and soak it in the TMOS solution for 2 hours, take it out, and dry it in vacuum for 2 hours at 80° C. to obtain the superhydrophobic oil-w...

Embodiment 3

[0032] The oil-water mixture is separated by a graduated cylinder filter, and the separation efficiency is calculated by recording the liquid mass before and after separation. The filter is mainly composed of 3 parts, the upper and lower two measuring cylinder filter cups, and the FeCl prepared by the present invention is placed in the middle frosted interface. 3 -PA / TMOS modified layer-by-layer self-assembly structure PI-based oil-water separation fiber membrane, after fixing with clips, fix the whole device on the iron stand. Mix 10mL oil and 10Ml water evenly and pour it from the top of the separation device. The liquid mixture contacts the membrane at the junction, the oil phase flows into the beaker below through the membrane, and the water phase is trapped above the membrane to achieve the purpose of separation. By testing, the FeCL prepared by the present invention 3 - PA / TMOS modified layer-by-layer self-assembly structure PI-based oil-water separation fiber membrane...

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Abstract

The invention discloses a preparation method of superhydrophobic oil-water separation membrane. The membrane has excellent oil-water separation effect, and can quickly separate oil-water mixture, andhas no pollution to the environment and good tolerance, and can be recycled. Polydiformyl biphthalate p-phenylenediamine (BPPAA) can be obtained by reacting biphenyltetracarboxylic dianhydride (BPDA)and p-phenylenediamine (PDA) as monomers at -5 DEG C for 12 hours. The polymer is a precursor for synthesizing high molecular weight polyimide (PI), and a PAA nanofiber membrane is prepared by an electrospinning technique and imidized at 300 DEG C to form a PI membrane. The layer-by-layer self-assembly of the PI membrane is performed by using ferric chloride (FeCI3) and phytic acid (PA) for initially modifying the PI membrane, and then trimethoxyoctadecylsilane (TMOS) is used for the modification of the membrane to obtain the core material. Various analytical testing methods are used for characterizing the material, and the efficacy of the super-hydrophobic oil-water separation membrane can be verified.

Description

technical field [0001] The invention relates to a layer-by-layer self-assembly technology, which is used to prepare a super-hydrophobic and super-oleophilic oil-water mixture separation membrane based on an electrospinning membrane. Background technique [0002] Oil-water separation has become a global problem, especially after the oil spill in the Gulf of Mexico. Oil spills often occur in the process of oil extraction, transportation, storage and use, which not only lead to energy loss and waste of resources, but also pose a threat to the ecological environment on which our long-term survival depends. Oily wastewater has become the most common pollutant in many industries such as crude oil production, petroleum refining, lubricants, metallurgy, food and textile processing. Furthermore, for oil transportation by sea, even a trace amount of water in the oil may threaten the safety of the transportation. [0003] Membrane separation technology has been proven to be the best ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/02B01D71/56B01D17/022
CPCB01D17/02B01D17/085B01D67/0002B01D69/02B01D71/56B01D2323/04B01D2325/38
Inventor 黄超伯张梦洁吕丹
Owner NANJING FORESTRY UNIV
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