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Preparation method of microporous molecular sieve filled solvent resistant composite film

A microporous molecular sieve and solvent-resistant technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of unsuitable industrial application, poor stability of mixed oil, high retention rate of soybean oil, etc., and achieve separation performance maintenance Stable, good anti-swelling performance, excellent separation effect

Active Publication Date: 2015-03-04
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most membrane materials have poor separation performance for mixed oils, high flux but low rejection of soybean oil, high rejection of soybean oil but too low flux, or low flux and rejection of soybean oil
A small amount of membrane materials with good separation performance have also been found, such as polydimethylsiloxane, but its swelling in hexane is severe, and its stability to mixed oil is poor, and the separation performance is less than 100 hours in mixed oil that starts to decline rapidly, which makes it unsuitable for industrial applications

Method used

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  • Preparation method of microporous molecular sieve filled solvent resistant composite film
  • Preparation method of microporous molecular sieve filled solvent resistant composite film
  • Preparation method of microporous molecular sieve filled solvent resistant composite film

Examples

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Effect test

Embodiment 1

[0032] Crush the ZSM-5 molecular sieve with a silicon-aluminum ratio of 300 to a particle size of less than 2 microns, add toluene to form a suspension with a mass concentration of 20% and ultrasonically disperse it for 1 hour, and then add octyltrichlorosilane with a mass concentration of 10% of ZSM-5 , and stirred at 80°C for 12 hours. After filtering, washing and drying, octyltrichlorosilane-modified ZSM-5 was obtained. Take 10 grams of fluorosilicone oil whose γ-trifluoropropyl side chain segments account for 50% of the total number of segments, dissolve it in 20 grams of methyl ethyl ketone, add 2 grams of modified ZSM-5, stir and ultrasonically disperse for 1 hour, and then add 1 1 gram of phenyltrimethoxysilane and 0.3 gram of dibutyltin diacetate were stirred evenly to obtain the casting solution, and the PVDF ultrafiltration membrane was used as the base film, and the film was scraped on the base film. After standing at room temperature for 24 hours, it was heated in...

Embodiment 2

[0037] Crush the ZSM-5 molecular sieve with a silicon-aluminum ratio of 300 to a particle size of less than 2 microns, add toluene to form a suspension with a mass concentration of 20% and ultrasonically disperse it for 1 hour, and then add octyltrimethoxy with 50% of the mass of ZSM-5 Silane, stirred at room temperature for 1 hour. After filtering, washing and drying, octyltrimethoxysilane-modified ZSM-5 was obtained. Take 10 grams of fluorosilicone oil whose γ-trifluoropropyl side chain segments account for 30% of the total number of segments, dissolve it in 90 grams of toluene, add 3 grams of modified ZSM-5, stir and ultrasonically disperse for 2 hours, then add 1 g Phenyltrimethoxysilane and 0.2 gram of dibutyltin dilaurate were stirred evenly to obtain a casting solution, and the PVDF ultrafiltration membrane was used as the base film, and the film was scraped on the base film. After standing at room temperature for 24 hours, it was heated in an oven at 120° C. for 12 ho...

Embodiment 3

[0040]The silicate-1 molecular sieve was crushed to a particle size of less than 2 microns, and toluene was added to prepare a suspension with a mass concentration of 15% for ultrasonic dispersion for 2 hours, then dodecyltrichlorosilane with a silicate mass of 20% was added, and stirred at 50 °C for 12 hours. After filtering, washing and drying, silicate-1 modified with dodecyltrichlorosilane was obtained. Dissolve 14 grams of fluorosilicone oil whose γ-trifluoropropyl side chains account for 50% of the total number of segments in 6 grams of methyl ethyl ketone, add 0.7 grams of modified silicate-1, stir and ultrasonically disperse for 5 hours, and then add 1.5 grams of octyltrimethoxysilane and 0.4 grams of dibutyltin diacetate were stirred evenly to obtain a casting solution. Use the PVDF ultrafiltration membrane as the bottom membrane, and scrape the membrane on the bottom membrane. After standing at room temperature for 24 hours, it was heated in an oven at 120 °C for 24...

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Abstract

The invention discloses a preparation method of a microporous molecular sieve filled solvent resistant composite film. The preparation method comprises the following steps: preparing fluorosilicone oil, a microporous molecular sieve, a crosslinking agent, a catalyst and a solvent into a film casting solution, uniformly coating the film casting solution on a base film by using a solvent resistant ultra-filtration film as the base film, further heating to enable the film casting solution to deeply crosslink with the base film after the solvent is evaporated and solidified so as to obtain the microporous molecular sieve filled solvent resistant composite film. Through the composite film prepared by using the method disclosed by the invention, the molecular sieve is uniformly dispersed in a separation layer, and meanwhile, the separation layer is tightly combined with a support layer; the composite film has good swelling resistance in the organic solvent, and is excellent in separation effect and high in stability when being used for recycling low-molecular weight solvent from an oil mixture, and the separation performance can be stably maintained in long-term operation.

Description

technical field [0001] The invention relates to the technical field of solvent-resistant composite membranes, in particular to a preparation method of a microporous molecular sieve filled solvent-resistant composite membrane suitable for recovery of low-molecular-weight organic solvents. Background technique [0002] In production fields such as the chemical industry, there are a large number of separation processes involving vaporization such as rectification and distillation. Due to the generally high latent heat of vaporization, these processes consume a lot of energy. 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 evaporation process. [0003] The current industrial oil production processes mainly include pressing method and solvent extraction method. Solvent leaching method includes thre...

Claims

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Application Information

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IPC IPC(8): B01D69/12B01D71/34B01D71/64B01D67/00
Inventor 李继定蔡卫滨夏阳郑冬菊李祥房满权朱慎林
Owner TSINGHUA UNIV
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