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Preparation method of polyvinylidene fluoride/TiO2 nano-sol composite ultrafiltration membrane

A polyvinylidene fluoride and nanosol technology, applied in ultrafiltration, chemical instruments and methods, membrane technology, etc., can solve problems such as uneven distribution of nanometers, achieve overall uniformity and stability, overcome the phenomenon of agglomeration and precipitation, and facilitate uniform dispersion. Effect

Active Publication Date: 2016-07-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcomings of conventional nano-modified film preparation methods, to provide a method that can minimize the problem of uneven nano-distribution of blended films caused by nano-agglomeration, and ensure the stability of the casting film solution by using nano-sol Improve the filtration performance and anti-pollution performance of nanocomposite membranes

Method used

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  • Preparation method of polyvinylidene fluoride/TiO2 nano-sol composite ultrafiltration membrane
  • Preparation method of polyvinylidene fluoride/TiO2 nano-sol composite ultrafiltration membrane
  • Preparation method of polyvinylidene fluoride/TiO2 nano-sol composite ultrafiltration membrane

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Embodiment 1

[0029](a) Tetrabutyl titanate and absolute ethanol were mixed and stirred at a ratio of 1:12 for 30 min to obtain a transparent and uniform reaction precursor. The mixed solution composed of absolute ethanol and deionized water at a ratio of 6:1 was mechanically stirred for 30 minutes, and the pH value was adjusted to 2 with dilute nitric acid or dilute hydrochloric acid, and the obtained uniform transparent solution was the reaction medium. Add the reaction precursor dropwise to the reaction medium in a water bath at 50°C, stir and sonicate for 60 minutes to obtain a light yellow emulsion, which is TiO 2 Sol solution, TiO 2 The ratio of tetrabutyl titanate to deionized water in the sol solution is 1:1.

[0030] (b) Add 8% polyvinylidene fluoride to a mixed solution containing 10% pore-forming agent and 62% organic solvent and mechanically stir at 80°C for 4 days to form a homogeneous precast film solution. Then ultrasonically dispersed 30min containing 0.15%TiO 2 The mixed...

Embodiment 2

[0033] (a) Tetrabutyl titanate and absolute ethanol were mixed and stirred at a ratio of 1:12 for 30 min to obtain a transparent and uniform reaction precursor. The mixed solution composed of absolute ethanol and deionized water at a ratio of 6:1 was mechanically stirred for 30 minutes, and the pH value was adjusted to 2 with dilute nitric acid or dilute hydrochloric acid, and the obtained uniform transparent solution was the reaction medium. Add the reaction precursor dropwise to the reaction medium in a water bath at 45°C, stir and sonicate for 60 minutes to obtain a light yellow emulsion, which is TiO 2 Sol solution, TiO 2 The ratio of tetrabutyl titanate to deionized water in the sol solution is 1:0.9.

[0034] (b) Add 7% polyvinylidene fluoride to a mixed solution containing 11% pore-forming agent and 64% organic solvent and mechanically stir at 80°C for 5 days to form a homogeneous precast film solution. Then ultrasonically dispersed for 30 min containing 1% TiO 2 The...

Embodiment 3

[0037] (a) Tetrabutyl titanate and absolute ethanol were mixed and stirred at a ratio of 1:15 for 30 minutes to obtain a transparent and uniform reaction precursor. The mixed solution composed of absolute ethanol and deionized water at a ratio of 9:1 was mechanically stirred for 30 minutes, and the pH value was adjusted to 1.5 with dilute nitric acid or dilute hydrochloric acid, and the obtained uniform transparent solution was the reaction medium. Add the reaction precursor dropwise to the reaction medium in a 60°C water bath, stir and ultrasonically for 20 minutes to obtain a light yellow emulsion, which is TiO 2 Sol solution, TiO 2 The ratio of tetrabutyl titanate to deionized water in the sol solution is 1:0.8.

[0038] (b) Add 10% polyvinylidene fluoride to a mixed solution containing 8% pore-forming agent and 60% organic solvent and mechanically stir at 80°C for 4 days to form a homogeneous precast film solution. Then ultrasonically dispersed 30min containing 0.5%TiO ...

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Abstract

The invention relates to a preparation method of a polyvinylidene fluoride / TiO2 nano-sol composite ultrafiltration membrane. The preparation method comprises the following steps: preparation and mixing of a nano-sol liquid reaction precursor and a reaction medium, dispersion of nano-sol, preparation of a membrane pre-casting solution and a membrane casting solution, membrane coating, solvent leaching and subsequent treatment of the membrane to obtain the composite ultrafiltration membrane. A sol solution containing nano TiO2 primary particles is prepared by a sol-gel method, and then is fully mixed and dispersed with an organic solvent, so as to be blended into a polymer membrane pre-casting solution, and the composite ultrafiltration membrane uniformly dispersed nano is prepared by an immerged phase-inversion process. According to the process disclosed by the invention, a uniformly dispersed and stable sol solution replaces powdered nano TiO2 particles, so that the phenomenon that the powdered nano particles are united after being added into the membrane casting solution and make the membrane casting solution unstable is effectively avoided; the obtained composite ultrafiltration membrane is high in strength, high in flux, anti-pollution, easy to clean and low in production cost.

Description

technical field [0001] The invention relates to a polyvinylidene fluoride / TiO 2 The preparation method of nano sol composite ultrafiltration membrane involves three stages of preparation of nano sol, film casting liquid and film formation, and the prepared film is suitable for membrane wastewater treatment process, especially the application in membrane bioreactor. Background technique [0002] Membrane sewage treatment process is a new process developed by applying membrane separation technology to the field of sewage treatment. It is favored because of its advantages of low energy consumption and stable effluent quality. Among them, membrane bioreactor technology is a new wastewater treatment process that combines membrane separation technology and sewage biological treatment technology. It has the advantages of good effluent quality, compact equipment, small footprint, impact load resistance, and convenient operation and management. It has broad application prospects in ...

Claims

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Application Information

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IPC IPC(8): B01D71/34B01D69/12B01D67/00B01D61/14C02F1/44
CPCB01D61/145B01D67/0002B01D69/12B01D71/34C02F1/444
Inventor 王志伟张杰王巧英曾豪陈妹郑君健潘辰张星冉王煊博吴志超
Owner TONGJI UNIV
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