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Organic-inorganic three-layer composite film and preparation method thereof

An inorganic membrane and layer composite technology, which is applied in the field of membrane materials, can solve the problems of poor bonding between the surface dense layer and the inorganic base membrane, preparation of pore-clogging composite membranes, and large pore size of the inorganic base membrane, so as to achieve enhanced permeability and impermeability. Leakage, the effect of high separation factor

Inactive Publication Date: 2018-04-20
NANJING JIUSI HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problem of poor bonding between the surface dense layer and the inorganic base film in the existing inorganic / organic composite film, which is easy to fall off, or the pore size of the inorganic base film is large, and the coating film is prone to pore seepage and pore blocking, resulting in difficulties in the preparation of the composite film. In order to solve such problems, an organic-inorganic three-layer composite membrane and its preparation method are proposed. Using organic polymers as the intermediate transition layer can modify and regulate the surface pore size of the inorganic base membrane, and solve the problems of leakage and pore blocking when the surface membrane is coated. At the same time, it can also strengthen the bonding strength between the separation layer membrane and the base membrane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Pretreatment of the support layer: a single-tube inorganic membrane prepared by sintering zirconia on the surface of alumina was selected as the support layer, the average pore diameter of the surface was 10 nm, and the washing solution was a combination of hydrochloric acid-sodium hydroxide solution, namely Soak in 0.5mol / L hydrochloric acid and 0.5mol / L sodium hydroxide for 12 hours in turn, then rinse the inorganic membrane with deionized water until the surface of the membrane is neutral, and finally dry it in vacuum at 30°C for 12 hours;

[0036] (2) Middle layer coating solution configuration: The middle layer material is polyethersulfone (PES), which is dissolved by adding solvent N,N-dimethylacetamide, and prepared into a coating solution with a mass concentration of 10%. Reserve after soaking;

[0037] (3) Coating the intermediate film layer: seal both ends of the pretreated tubular inorganic film in step (1), and apply the coating solution prepared in step...

Embodiment 2

[0043] (1) Pretreatment of the support layer: select the mullite-based multi-channel inorganic membrane prepared by low-temperature sintering as the support layer, and its surface pore size is 800 nm. Soak in mol / L hydrochloric acid and 0.8mol / L sodium hydroxide for a total of 8 hours, then rinse the inorganic membrane with deionized water until the surface of the membrane is neutral, and finally dry it in vacuum at 60°C for 8 hours;

[0044] (2) Middle layer coating liquid configuration: The middle layer material is polyvinylidene fluoride (PVDF), adding solvent N,N-dimethylformamide to dissolve, and preparing a coating liquid with a mass concentration of 8%, filtering, Standby after defoaming;

[0045] (3) Coating the intermediate film layer: seal both ends of the pretreated inorganic film in step (1), and apply the coating liquid prepared in step (2) to the pretreated inorganic film by dipping coating method On the outer surface of the film, the coating time is 20s. After ...

Embodiment 3

[0050] (1) Support layer pretreatment: select Al 2 o 3 -SiO 2 The hollow fiber inorganic membrane is used as the support layer, and its surface pore size is 200nm. The membrane washing solution is a combination of hydrochloric acid-sodium hydroxide solution, that is, soaked in 1mol / L hydrochloric acid and 0.2mol / L sodium hydroxide for 12 hours, and then Rinse the inorganic membrane with deionized water until the surface of the membrane is neutral, and finally dry it in vacuum at 30°C for 12 hours;

[0051] (2) Coating solution configuration for the middle layer: polysulfone (PSF) is used as the material for the middle layer, and the solvent N-methylpyrrolidone is added to dissolve it, and a coating solution with a mass concentration of 5% is prepared, which is filtered and defoamed for later use;

[0052] (3) Coating the intermediate film layer: seal both ends of the pretreated inorganic film in step (1), and apply the coating liquid prepared in step (2) to the pretreated in...

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Abstract

The invention discloses an organic-inorganic three-layer composite film and a preparation method thereof, and belongs to the field of the preparation of film materials. The composite film comprises asupporting layer, a middle transition layer and a surface active layer, wherein the supporting layer adopts an inorganic film, with the surface average pore size being 10 to 800 nm; the middle transition layer adopts organic polymer, with the mass fraction being 1 to 10 percent, and the surface average pore size being 5 to 80 nm; the surface active layer adopts silicone rubber PDMS, with the filmlayer thickness being 1 to 10 micrometers. The organic-inorganic three-layer composite film takes an organic polymer film with controllable thickness and surface pore size as a middle transition layer, can optimally regulate the uniformity and thickness of the surface active layer of the composite film and the bonding strength between the dense surface active layer and the middle transition layerand between the inorganic film supporting layer and middle transition layer by controlling the viscosity of PDMS coating fluid. The composite film is large in permeation flux and high in separation factor, and the surface active layer is not easy to peel off, so that the composite film is applicable to organic solvent recovery and organic gas separation in pervaporation.

Description

technical field [0001] The invention belongs to the technical field of membrane materials, and in particular relates to an organic-inorganic three-layer composite membrane and a preparation method thereof. Background technique [0002] In the production process of chemical, biological, pharmaceutical and other industries, organic solvents are usually required as the reaction medium or reactant. When the reaction is incomplete or the product is desolvated, a large amount of organic tail gas is usually produced, which will also cause waste of resources. Recycling these solvents is of great significance to reduce production costs, sustainable economic development and environmental protection. Biomass fuel separation industry, food natural aroma separation, azeotropic system separation industry and other processes all involve the separation of organic matter, but most of the currently used separation methods such as distillation and evaporation have high energy consumption, high...

Claims

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Application Information

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IPC IPC(8): B01D71/70B01D67/00B01D69/12B01D71/02
CPCB01D67/0079B01D69/12B01D69/125B01D71/024B01D71/70
Inventor 丁晓斌孙雪飞沈春香
Owner NANJING JIUSI HIGH TECH
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