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Preparation method of functionalized multiwalled carbon nanotube blended ultrafiltration membrane

A multi-walled carbon nanotube and functionalized technology, applied in chemical instruments and methods, ultrafiltration, membranes, etc., can solve the problems of ineffective blend membrane preparation process, poor pollutant retention effect, and high production cost, and achieve and The effect of enhanced mechanical properties, enhanced pollution resistance, and production cost savings

Active Publication Date: 2016-04-13
成都恒固新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of functionalized multi-wall carbon nanotube blended ultrafiltration membrane, aiming to solve the problem that the existing blended membrane preparation process cannot effectively solve the dispersibility of nanomaterial MWCNT in the casting liquid , high production cost, and poor pollutant interception effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Mix concentrated sulfuric acid and concentrated nitric acid at a mass ratio of 3:1 to obtain a mixed acid solution, place 1 g of MWCNT in 50 ml of mixed acid solution for acidification for 1 h, take out the MWCNT, and obtain acidified modified MWCNT;

[0016] Put 1g of acidified and modified dry MWCNT into 15mL of thionyl chloride, heat and stir at 70°C, react for 7h, and remove excess thionyl chloride by distillation under reduced pressure;

[0017] (2) After the product is dried, add it to 200ml ethanol water (mixture of ethanol and water volume ratio 1:1), after ultrasonication for 20min, then add 12ml3-aminopropyltriethoxysilane, and continue ultrasonication for 20-30min After that, it was transferred to a three-necked flask, and refluxed at 80° C. for 1 h, then filtered, and dried to obtain functionalized multi-walled carbon nanotubes F-MWCNT.

Embodiment 2

[0019] (1) Mix concentrated sulfuric acid and concentrated nitric acid at a mass ratio of 3:1 to obtain a mixed acid solution, place 2 g of MWCNT in 50 ml of mixed acid solution for acidification for 2 hours, take out the MWCNT, and obtain acidified modified MWCNT;

[0020] Put 2g of acidified and modified dry MWCNT into 15mL of thionyl chloride, heat and stir at 70°C, react for 8h, and remove excess thionyl chloride by distillation under reduced pressure;

[0021] (2) After the product is dried, add it to 200ml of ethanol water, after ultrasonication for 30min, then add 8ml of 3-aminopropyltriethoxysilane, continue ultrasonication for 20min, transfer to a three-necked flask, and reflux at 80°C 1h, followed by filtration and drying to obtain functionalized multi-walled carbon nanotubes F-MWCNT.

Embodiment 3

[0023] (1) Add 0.2g of functionalized multi-walled carbon nanotubes F-MWCNT to a beaker containing 80g of N,N-dimethylacetamide solution, ultrasonically disperse for 30min, then add 2g of polyvinylpyrrolidone and 18g of polyvinylidene fluoride , and heated and stirred at 70°C for 12 hours; after the solution was cooled, it was placed in a vacuum drying oven for degassing for 24 hours to obtain a casting solution;

[0024] (2) Slowly pour the film casting solution on a clean glass plate, and scrape it into a film with a thickness of 0.2mm with a film scraper; pre-evaporate in the air for 15s and then immerse in pure water; after the film completely falls off from the glass plate, take it out After soaking in deionized water for 24 hours and drying for 2 hours, the functionalized blend ultrafiltration membrane F-MWCNT / PVDF was obtained.

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Abstract

The invention provides a preparation method of a functionalized multiwalled carbon nanotube blended ultrafiltration membrane, comprising the following steps: putting dried MWCNT after acidized modification into thionyl chloride for reaction for 7-8h; drying a product and then adding the dried product into ethanol water, carrying out ultrasonic dispersion and then adding 3-aminopropyl triethoxy silane, continuing to carry out ultrasonic dispersion and then carrying out backflow for 1h at the temperature of 80 DEG C, filtering and drying to obtain the functionalized multiwalled carbon nanotube; adding the functionalized multiwalled carbon nanotube to an N, N-dimethylacetamide solution, carrying out ultrasonic dispersion and then adding polyvinylpyrrolidone and polyvinylidene fluoride, heating and stirring, cooling and then defoaming to prepare a casting film solution; pouring the casting film solution to a glass plate and scraping to form a membrane; pre-evaporating in air and then immersing into pure water; and taking out after the membrane falls out and then soaking with deionized water, and drying to obtain the functionalized blended ultrafiltration membrane. The hydrophilia, the anti-fouling performance and the mechanical performance of the functionalized multiwalled carbon nanotube blended ultrafiltration membrane are all enhanced, and the manufacture cost is low.

Description

technical field [0001] The invention belongs to the field of petrochemical materials, and in particular relates to a preparation method of a functionalized multi-walled carbon nanotube blended ultrafiltration membrane. Background technique [0002] In the prior art, the preparation process of the blend film is generally as follows: the nanomaterial MWCNT (multi-walled carbon nanotube), polymer matrix and organic solvent are composed of a ternary blend system, and stirred at 60 ° C for 24 hours to prepare the casting film; After defoaming, use a spatula to scrape it into a film of 0.15-0.3 mm, then immerse it in a gel bath, and soak it in distilled water for several days after it falls off. [0003] It can be seen from the above existing technical solutions that the preparation process of the blend film cannot effectively solve the dispersion problem of the nanomaterial MWCNT in the casting liquid, so that the excellent performance of the MWCNT cannot be utilized to a greater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/02B01D71/02B01D71/38B01D71/34B01D67/00B01D61/14
CPCB01D61/145B01D69/02B01D71/021B01D71/34B01D71/38B01D2325/24B01D2325/36
Inventor 何毅曾广勇余宗学潘洋杨稀石恒第海辉詹迎青
Owner 成都恒固新材料科技有限公司
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