Preparation method of solvent resistant nanofiltration membrane

A nanofiltration membrane and solvent-resistant technology, which is applied in the field of solvent-resistant nanofiltration membrane preparation, can solve the problems of rapid decline in separation performance, poor separation performance of mixed oil, low flux and rejection rate, etc., and achieve stable separation performance , large industrial application potential, and the effect of simple and easy methods

Inactive Publication Date: 2015-03-25
TSINGHUA UNIV
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Problems solved by technology

However, most nanofiltration membranes have poor separation performance for mixed oils, with large flux but low rejection rate, or high rejection rate but too low flux, or both flux and rejection rate are low
At present, a small amount of membrane materials with good separation performance have also been found, such as polydimethylsiloxane, but its swelling in hexane is serious, and its stability to mixed oil is poor, and it can be separated in less than 100 hours in mixed oil. Performance begins to degrade rapidly, making it unsuitable for widespread use in industry

Method used

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  • Preparation method of solvent resistant nanofiltration membrane
  • Preparation method of solvent resistant nanofiltration membrane
  • Preparation method of solvent resistant nanofiltration membrane

Examples

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Effect test

Embodiment 1

[0023] (1) Preparation of polyvinylidene fluoride (PVDF) base film: the PVDF raw material was dehydrated in an oven, and then a solution with a PVDF mass concentration of 15% was prepared with triethyl phosphate (TEP) as a solvent, and stirred at 100 °C for 24 h; After filtration and vacuum defoaming, use water as a gel bath, and use the immersion precipitation phase inversion method to scrape the film on the non-woven fabric to obtain a PVDF film, and finally fully wash off the solvent with deionized water, and dry it to obtain PVDF Ultrafiltration membrane, that is, the bottom membrane of fluorosilicone rubber solvent-resistant nanofiltration membrane.

[0024] （ 2) Prepare fluorosilicone rubber casting solution: mix fluorosilicone oil containing γ-trifluoropropyl side chains accounting for 50% of the total number of side chains, phenyltrimethoxysilane, dibutyltin diacetate and butanone, and stir well , filtered, and defoamed to obtain a fluorosilicone rubber casting soluti...

Embodiment 2

[0033] (1) Preparation of polyetherimide (PEI) base film: Dehydrate PEI raw materials in an oven, use dimethylacetamide (DMAC) as solvent and N-methylpyrrolidone as additive, and prepare PEI with a mass concentration of 15% solution, stirred for 24 h; after filtration and vacuum defoaming, water was used as the gel bath, and the film was scraped on the non-woven fabric by immersion precipitation phase inversion method to obtain the PEI film. The obtained membrane is fully washed with deionized water to remove the solvent, and dried to obtain the PEI ultrafiltration membrane, which is the bottom membrane of the fluorosilicone rubber solvent-resistant nanofiltration membrane.

[0034] (2) Preparation of fluorosilicone rubber casting solution: Mix fluorosilicone oil containing γ-trifluoropropyl side chains accounting for 50% of the total number of side chains, octyltrimethoxysilane, dibutyltin diacetate and pentanone, and stir Uniform, filtered, and defoamed to obtain the fluoros...

Embodiment 3

[0041] (1) Preparation of polyvinylidene fluoride (PVDF) base film: the method is the same as step (1) in Example 1.

[0042] (2) Preparation of fluorosilicone rubber casting solution: Mix fluorosilicone oil, hydrogen silicone oil, dibutyltin dilaurate and butanone containing γ-trifluoropropyl side chains accounting for 50% of the total number of side chains, stir well, and filter , after defoaming, the fluorosilicone rubber casting liquid is obtained, wherein the mass ratio of fluorosilicone oil:hydrogen silicone oil:dibutyltin dilaurate:butanone is 10:0.3:0.3:50.

[0043] (3) Preparation of fluorosilicone rubber nanofiltration membrane: Coat the fluorosilicone rubber casting solution obtained in step (2) on the PVDF bottom membrane prepared in step (1), and place it at room temperature for 24 hours until the solvent volatilizes and initially solidifies Afterwards, heat treatment in an oven at 120°C for 36 hours to prepare a fluorosilicone rubber solvent-resistant nanofiltrat...

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Abstract

The invention discloses a preparation method of a solvent resistant nanofiltration membrane. The preparation method comprises the steps of dissolving fluorosilicone oil, a cross-linking agent and a catalyst in a solvent, fully stirring to prepare a casting solution, filtering, defoaming, controlling the thickness, uniformly coating a base membrane by the casting solution, placing at room temperature until the solvent is volatized and solidified preliminarily, and further crosslinking at certain room temperature to obtain the fluorinated silicone rubber solvent resistant nanofiltration membrane. The prepared solvent resistant nanofiltration membrane is used for recycling hexane from soybean oil/hexane mixed oil, has excellent separation property, can overcome the disadvantage that the common silicone rubber has organic solvent intolerance, has excellent swelling resisting behavior, and can keep stable separating property after long-time operation.

Description

technical field [0001] The invention belongs to the technical field of organic membrane separation, and in particular relates to a preparation method of a solvent-resistant nanofiltration membrane. Background technique [0002] Organic solvent leaching is the mainstream process in the current vegetable oil processing process. The leaching solvent mainly uses hexane or No. 6 solvent oil mainly based on hexane. The leaching solvent and oil are contacted in the leaching device to obtain vegetable oil containing more The mixed oil, in which the vegetable oil content is generally between 20% and 30%. The existing process usually adopts the evaporation method to recover the solvent and obtain the vegetable oil, which consumes a lot of energy. [0003] Nanofiltration is a membrane separation process that uses pressure as the driving force to separate the solvent from the solution. Using nanofiltration to recover solvent from mixed oil can save a lot of energy because there is no ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/70B01D69/02B01D67/00
Inventor 李继定蔡卫滨夏阳郑冬菊房满权李祥朱慎林
Owner TSINGHUA UNIV
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