A kind of hydrophilic graft multi-walled carbon nanotube modified polyvinylidene fluoride membrane and preparation method thereof

A multi-wall carbon nanotube and polyvinylidene fluoride membrane technology is applied in the field of multi-wall carbon nanotube modified separation membrane and its preparation, which can solve the problem that carbon tubes are easy to agglomerate, affect membrane strength, separation performance and pollution resistance, The modification effect is not obvious and other problems, to achieve the effect of facilitating distribution, improving anti-pollution ability, and improving hydrophilicity

Inactive Publication Date: 2017-04-05
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent 201310014691.6 discloses a preparation method of hydrophilic polyvinylidene fluoride modified separation membrane, which is to add graphene oxide, carbon nanotubes and porogen into PVDF at the same time, and the oxygen-containing functional groups on the filler can strengthen the separation membrane Hydrophilicity, and carbon nanotubes and graphene mutually inhibit their respective agglomeration, but the modification effect of these two modification methods is not significant, due to the large specific surface area of ​​nanoscale graphene and carbon nanotubes, Simple oxidation treatment cannot fully and uniformly disperse carbon tubes and is easier to agglomerate, which in turn affects membrane strength, separation performance and pollution resistance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 1.0g±0.001g of the above-mentioned carboxylated multi-walled carbon nanotubes and 200mL±1mL of thionyl chloride, add them into a three-necked flask, stopper them, and after ultrasonication in a water bath at 20°C for 40min, assemble a condensation reflux device and start stirring at the same time And heating, slowly warming up to 65°C, reflux for 10h, then stop heating and slowly lower the temperature to room temperature, after stirring for 3h, turn on the heating again and raise the temperature to 65°C, reflux for 40h while stirring, then filter the mixture at room temperature and dry to obtain black Powder, that is, acyl chloride carbon nanotubes. Then add the obtained acyl chloride carbon nanotubes and 150mL ± 1mL polyethylene glycol (200g / mol) into a three-necked flask, start stirring and heating, raise the temperature to 130°C for 36h, and suction filter the suspended mixture after the reaction at room temperature , washing with ethanol and drying to obtain P...

Embodiment 2

[0039] Add 0.02 g of the hydrophilic grafted multi-walled carbon nanotubes prepared in Example 1 to 23 g of N-N dimethylacetamide, heat and stir in a water bath at 60° C. for 2 h, and then ultrasonically disperse in an ultrasonic cleaner for 1 h. Finally, add 2g of polyvinylidene fluoride, heat and stir in a water bath at 60°C for 8 hours until it is completely dissolved, then apply strong ultrasonic (100W) for 30 minutes, let it stand at room temperature for defoaming, and use a scraping rod to control a certain film thickness on a clean glass Scrape the film on the board, so that the casting solution after the scraping is pre-volatilized for 30s, and then quickly immersed in the deionized water coagulation bath. Water-grafted carbon nanotube-modified polyvinylidene fluoride membrane.

[0040]In order to characterize the change of hydrophilicity of the modified separation membrane, the above-mentioned hydrophilic graft modified polyvinylidene fluoride membrane was vacuum-drie...

Embodiment 3

[0042] Add 0.04g of the hydrophilic grafted carbon nanotubes prepared in Example 1 to 24g of N-N dimethylacetamide, heat and stir in a water bath at 55°C for 3h, then place in an ultrasonic cleaner for ultrasonic dispersion for 1h, and then add 2g of polyvinylidene fluoride, heated and stirred in a water bath at 55°C for 8 hours until completely dissolved, then subjected to strong ultrasonic (100W) for 30 minutes, left at room temperature for defoaming, and used a scraping rod to control a certain film thickness on a clean glass plate Scrape the film, make the casting solution after scraping the film pre-volatilized for 30s, then quickly immerse in the deionized water coagulation bath, after the film is formed, change the water repeatedly to remove the solvent N-N dimethylacetamide, and finally obtain a hydrophilic adhesive Carbon nanotube modified polyvinylidene fluoride film.

[0043] The above-mentioned hydrophilic graft modified polyvinylidene fluoride film was vacuum-drie...

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Abstract

The invention provides a hydrophilic grafted multiwalled carbon nanotube modified polyvinylidene fluoride film and a preparation method thereof. The preparation method comprises the steps of grafting polyethylene glycol molecules with low polymerization degree to multiwalled carbon nanotubes, evenly dispersing hydrophilic grafted multiwalled carbon nanotubes into a PVDF (Polyvinylidene Fluoride) casting solution, and filming with an immersion precipitated phase conversion method. When being used as a hydrophilic group, the polyethylene glycol chain with low polymerization degree, grafted on the carbon nanotubes, can improve the hydrophilcity of the film so as to improve the anti-pollution capacity of the film; when being used as polymers, the polyethylene glycol chain can be well compatible with the PVDF matrix, the carbon nanotubes can be well dispersed in the matrix, the contact area between the carbon nanotubes and the matrix is increased, and the film strength is improved. In addition, the preparation process is simple, has strong operability and is easy to realize.

Description

technical field [0001] The invention belongs to the technical field of separation membrane modification, in particular to a separation membrane modified by hydrophilic grafted multi-walled carbon nanotubes and a preparation method thereof. Background technique [0002] Polyvinylidene fluoride (PVDF) is a semi-crystalline polymer. Due to the short C-F bond length and large bond energy (486kJ / mo1), it has good thermal stability, chemical stability, radiation resistance and high mechanical strength. It is a kind of separation membrane material with excellent comprehensive performance. However, as a polymer material with strong hydrophobicity, when PVDF is applied, it is easy to breed microorganisms on the membrane surface and in the pores, adsorb inorganic substances, colloidal particles, proteins, etc., resulting in some irreversible changes in membrane performance, such as membrane Membrane permeation flux decreases, selectivity decreases, and service life shortens due to po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/34B01D69/02B01D67/00
Inventor 王文一李艳玲高宁宁刘正鑫
Owner TIANJIN POLYTECHNIC UNIV
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