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Composite molecular sieve carbon film based on phenolic resin-based carbon tube as support body, preparation method and application thereof

A composite molecular sieve and phenolic resin technology, applied in separation methods, oxygen preparation, chemical instruments and methods, etc.

Active Publication Date: 2021-04-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the technical problems of existing high molecular polymers in membrane thermal stability, acid and alkali resistance and pollution resistance in separation applications, the purpose of the present invention is to provide a composite molecular sieve carbon membrane based on a phenolic resin-based carbon tube as a support and Its preparation method and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Prepare the support precursor with an inner diameter of 5mm and a thickness of 1.5mm: add 6wt% HMA to the thermoplastic phenolic resin with an average particle size of 58μm, mix well and place it in an oven at 150°C for pre-curing for 120min; then crush it to an average particle size of 40μm, add 5wt% % methylcellulose, 10wt% water, 3.0wt% HMA, kneaded, extruded into a tubular body with inner diameter ID = 5mm, wall thickness 1.5mm, dried at room temperature for 48h, and pre-cured at 150°C for 120min to obtain a porous support precursor body;

[0073]Prepare mixed coating solution: dissolve thermoplastic phenolic resin and 0.5wt% HMA ethanol solution in DMAc to obtain mixed solution I; dissolve PVDF in DMA to form mixed solution II, add mixed solution I to II, and stir for 40 hours 1. After ultrasonication for 2 hours, a mixed coating solution of thermoplastic phenolic resin and PVDF was obtained. The mass of thermoplastic phenolic resin and PVDF accounted for 15% of th...

Embodiment 2

[0078] Prepare the support precursor with an inner diameter of 8mm and a thickness of 1.8mm: add 7wt% HMA to the thermoplastic phenolic resin with an average particle size of 55μm, mix well and place it in an oven at 150°C for pre-curing for 90min; then crush it to an average particle size of 38μm, add 6wt% % methyl cellulose, 15wt% water, 2.0wt% HMA, kneaded, extruded into a tubular body with inner diameter ID = 8mm, wall thickness 1.8mm, dried at room temperature for 72h, and pre-cured at 150°C for 90min to obtain a porous support precursor body;

[0079] All the other are with embodiment 1.

[0080] The bubble point method test shows that the maximum pore size of the porous tubular support is 0.85 μm, the average pore size is 0.37 μm, and the porosity is 45%. %; SEM shows: the support body and the separation layer are closely combined without obvious defects, and the thickness of the separation layer is about 42 μm.

Embodiment 3

[0082] Prepare ID=10mm, wall thickness 1.9mm porous support precursor as described in Example 1;

[0083] The ethanol solution of 20wt% thermoplastic phenolic resin that is dissolved with 0.5wt% HMA, called coating solution I, is added in the spray gun, with nitrogen as carrier gas, it is sprayed onto the outer surface of the porous support precursor to form a uniform The polymer layer is then dried at 80°C for 24 hours and cured at 150°C for 100 minutes to obtain a porous support precursor I evenly coated with a phenolic resin organic film;

[0084] The DMAC solution that will be dissolved with 12wt% PVDF, is called coating solution II and joins in the spray gun, with nitrogen as carrier gas, it is sprayed onto the outer surface of the porous support precursor I that has been sprayed with phenolic resin to form a uniform The polymer layer was then dried at 80° C. for 24 hours to obtain a porous support uniformly coated with phenolic resin and PVDF and its uniform coating II. ...

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Abstract

The invention discloses a composite molecular sieve carbon film based on a phenolic resin-based carbon tube as a support body and a preparation method thereof. The composite molecular sieve carbon membrane comprises a carbon tube support body and a carbon membrane separation layer, the carbon membrane separation layer is attached to the outer surface or the inner surface of the carbon tube support body, the carbon tube support body is of a carbon-containing porous tubular structure, the average pore diameter is 0.05-0.5 micron, the porosity is 20-80%, the average pore diameter of the carbon membrane separation layer is smaller than 10nm, and the porosity is 20-40%. And the carbon tube support body and the carbon membrane separation layer are both made of a carbon material. As a carbon tube support body precursor and a separation layer precursor are jointly subjected to curing and carbonization treatment to obtain the support body and the separation layer which are both made of carbon materials, the problem that the membrane performance is reduced due to a two-phase gap in a composite carbon membrane in the prior art is solved, the preparation process is simple, the process parameters are controllable, the preparation cost is saved by about 50%, and the permeation flux of the membrane performance is improved by more than 20%.

Description

technical field [0001] The invention relates to membrane preparation in membrane separation technology and its application field, in particular to a composite molecular sieve carbon membrane based on a phenolic resin-based carbon tube as a support and its preparation method and application. Background technique [0002] A carbon film is usually a porous film formed from an organic precursor through appropriate methods (such as spin coating, scraping, dipping, extrusion, deposition) film formation, carbonization, activation and other steps. In terms of separation mechanism, carbon membranes and organic membranes are different. For organic membranes, traditional dissolution-diffusion mechanisms are often used to explain their separation properties. The separation of gases or liquids in carbon membranes is generally considered to be accomplished by utilizing the different mass transfer characteristics of the components. Because gases, liquids and their mixtures have different...

Claims

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Application Information

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IPC IPC(8): B01D69/12B01D69/10B01D71/02B01D67/00B01D53/22C01B13/02
CPCB01D69/12B01D69/10B01D71/021B01D67/0067B01D53/228C01B13/0255
Inventor 吴历斌王月梅孔德金
Owner CHINA PETROLEUM & CHEM CORP
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