Mixed matrix membrane with heat resistance and solvent resistance and preparation method and application thereof

A mixed-matrix membrane and mixed-matrix technology, applied in the field of membrane separation technology and new materials, can solve the problems of poor solvent resistance and heat resistance of membranes, reduced permeation flux, and reduced porosity, and achieve excellent solvent resistance and Effects of heat resistance, permeation separation performance improvement, and membrane separation performance improvement

Active Publication Date: 2017-11-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many problems in the application process of the mixed matrix membrane prepared by the in situ synthesis method, such as the membrane structure is relatively dense, the membrane separation performance is not high due to the uneven pore structure; the membrane stability is caused by the poor solvent resistance and heat resistance of the membrane. Poor sex, etc.
Generally speaking, the pore structure of the membrane can be controlled by controlling the phase inversion process of the polymer, and the solvent resistance and heat resistance of the polymer membrane can be improved by thermally crosslinking the original membrane, but simply controlling the phase inversion process, It is impossible to make the membrane have rich sponge-like pores and uniform finger-like pores at the same time; and during the thermal oxidation crosslinking process, due to the intense thermal movement of the polymer chain segment, the pore structure of the membrane collapses and melts, the permeation flux decreases, and the pores rate decrease

Method used

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  • Mixed matrix membrane with heat resistance and solvent resistance and preparation method and application thereof
  • Mixed matrix membrane with heat resistance and solvent resistance and preparation method and application thereof
  • Mixed matrix membrane with heat resistance and solvent resistance and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]PAA, GO, TIPT, HAc, and DMF were configured as film-forming liquids, and a liquid film with a thickness of 200 μm was prepared, wherein the mass fraction of PAA was 12wt.%, the mass fraction of GO was 0.003wt.%, and the mass fraction of TIPT The fraction is 0.2wt.%, and the mass fraction of HAc is 0.4wt.%. After the liquid film is placed in the air for 40s, it is immersed in an acidic gel bath with a pH value of 5 at 80°C for 10min; It was soaked in deionized water for 24 hours, and then vacuum-dried at 60° C. for 12 hours to obtain a mixed matrix original film. The mixed matrix original film was placed in a thermal oxidation crosslinking device, the temperature was raised from room temperature, and thermal oxidation crosslinking was carried out in the air; the heating rate was 3°C / min, the air flow rate was 1L / min, and the thermal oxidation crosslinking temperature The temperature is 400°C, and the thermal oxidation crosslinking time is 2h. After reaching the final tem...

Embodiment 2-10

[0034] Selected polymer in the following table 3, select the most polar DMSO as the solvent resistance test solvent to repeat the method of embodiment 1, carry out the solvent resistance test, the test results are listed in the following table 3; according to the following table 1 The method of Example 1 was repeated with the polymers specified in Table 4, and the test results are listed in Table 1 and Table 4.

[0035] Table 1

[0036]

[0037]

[0038] Table 2

[0039]

[0040] table 3

[0041]

[0042]

[0043] Table 4

[0044]

Embodiment 11-16

[0046] Selected metal alkoxide in following table 5, select the method for repeating embodiment 1 of DMSO with the strongest polarity, carry out solvent resistance test, listed test result in following table 5; Press in following table 4 and table 6 The method of Example 1 was repeated for specified metal alkoxides, and the test results are listed in Table 4 and Table 6.

[0047] Table 4

[0048]

[0049]

[0050] table 5

[0051] Example

metal alkoxide

Membrane mass loss after immersion in DMSO for one week

Membrane morphology after soaking in DMSO for one week

11

TEOS

no loss

no change

12

TIPS

no loss

no change

13

TET

no loss

no change

14

TIPT

no loss

no change

15

TBT

no loss

no change

16

TIOT

no loss

no change

[0052] Table 6

[0053]

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Abstract

The invention relates to a mixed matrix membrane with heat resistance and solvent resistance and a preparation method and an application thereof and belongs to the field of membrane separation technologies and novel materials. The preparation method of the mixed matrix membrane with heat resistance and solvent resistance comprises the steps of preparing an original membrane of the mixed matrix membrane and performing thermal oxidative crosslinking, wherein the step of preparing an original membrane of the mixed matrix membrane comprises the following steps: preparing a membrane preparation liquid from graphene oxide, metal alkoxide, acetic acid, a polymer and an organic solvent and preparing the membrane; and performing in-situ synthesis of the mixed matrix membrane by means of a non-solvent phase inversion method. The original membrane has a lot of spongy holes and vertical dactylopore structures and meanwhile has a relatively high permeating separating property. The original membrane is subjected to thermal oxidative crosslinking to prepare the mixed matrix membrane with solvent resistance and thermal stability. The mixed matrix membrane not only can keep the porous structure and the high permeating separating property, but also has excellent solvent resistance and heat resistance.

Description

technical field [0001] The invention relates to a heat-resistant and solvent-resistant mixed matrix membrane and its preparation method and application, belonging to the field of membrane separation technology and new materials. Background technique [0002] Polymer membrane is an important part of membrane separation materials. Due to its simple manufacturing method and easy availability of raw materials, it is the most mature and one of the earliest widely used membrane materials. Mixed matrix membrane refers to a composite membrane prepared by filling inorganic materials as a dispersed phase in a polymer continuous phase. This type of membrane combines the excellent properties of organic and inorganic materials, and can improve the structure and separation performance of polymer membranes. Among the various preparation methods of mixed matrix membranes, the in situ synthesis method has attracted extensive attention because it can better uniformly disperse the inorganic p...

Claims

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Application Information

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IPC IPC(8): B01D71/56B01D71/64B01D71/42B01D71/68B01D71/26B01D71/34B01D71/16B01D69/02B01D67/00B01D61/14B01D61/02
CPCB01D61/027B01D61/145B01D67/0079B01D69/02B01D71/16B01D71/26B01D71/34B01D71/42B01D71/56B01D71/64B01D71/68B01D2325/22
Inventor 李琳刘峤金鑫徐瑞松王春雷王同华
Owner DALIAN UNIV OF TECH
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