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Preparation method and application of hollow-fiber solvent-resisting nanofiltration membranes

A solvent-resistant, nanofiltration membrane technology, applied in the field of membrane separation, to achieve the effect of shortening the crosslinking time, stable and reliable operation, and good industrial application prospects

Active Publication Date: 2018-01-30
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the hollow fiber membrane prepared by the phase inversion method in the prior art needs a follow-up cross-linking step to enhance the solvent resistance of the membrane, and proposes a core liquid and a gel bath in the phase inversion membrane making process. At the same time, a cross-linking agent is added to implement two-way synchronous cross-linking inside and outside, so that the preparation method of solvent-resistant hollow fiber nanofiltration membrane can be directly obtained in one step on the dry-wet spinning production line. This preparation method has the advantages of simple process, stable and reliable production, and required The advantages of less equipment and less consumption of chemical reagents, and the prepared solvent-resistant nanofiltration membrane has good solvent resistance and separation performance, thus solving the technical bottleneck of the hollow fiber SRNF membrane, making the hollow fiber SRNF membrane industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] The difference from the comparative example: 5% hexamethylenediamine was added to the core liquid, and 2.5% hexamethylenediamine was added to the gel bath as a crosslinking agent for simultaneous crosslinking during dry and wet spinning; There is no post-crosslinking step of step four in the comparative example.

[0067] Core liquid preparation: Mix hexamethylenediamine, the first solvent and deionized water at a mass ratio of 5:15:80 to prepare the core liquid.

[0068] Gel bath preparation: Dissolve hexamethylenediamine in deionized water to prepare a 2.5% by mass solution as a gel bath.

[0069] The steps of preparing the spinning solution, spinning the hollow fiber membrane, and post-treatment steps are the same as those of the comparative example.

[0070] At room temperature and a transmembrane pressure difference of 1.0 MPa, the hollow fiber solvent-resistant nanofiltration membrane prepared in Example 1 is −1 The retention rate of rose bengal RB in the rose be...

Embodiment 2

[0073] The difference from the comparative example: adjust the mass ratio of the first solvent and the first co-solvent in the spinning solution to (3:2); add hexamethylenediamine with a mass percentage concentration of 5% in the core solution; in the gel bath Add ethylenediamine with a concentration of 2.5% by mass as a crosslinking agent; dry-wet spinning simultaneous crosslinking; no post-crosslinking step in step 4 in the comparative example.

[0074] Preparation of spinning solution: Dissolve the dried polyimide in the mixed solvent of the first solvent and the first co-solvent (mass ratio 3:2), stir at room temperature for 24 hours to prepare spinning solution (polyimide mass 100% Min concentration is 22%).

[0075] Core liquid preparation: Mix hexamethylenediamine, the first solvent and deionized water at a mass ratio of 5:15:80 to prepare the core liquid.

[0076] Gel bath preparation: Dissolve hexamethylenediamine in deionized water to prepare a 2.5% by mass solution...

Embodiment 3

[0081] The difference from the comparative example: adjust the mass ratio of the first solvent and the first co-solvent in the spinning solution to 3:2; adjust the first non-solvent and the second solvent in the core solution to be diethylene glycol (DG) and NMP ( The mass ratio is 1:1), while adding hexamethylenediamine with a mass percentage concentration of 5% as a crosslinking agent; adding ethylenediamine with a mass percentage concentration of 2.5% as a crosslinking agent in the gel bath; no comparative example The post-crosslinking step in Step 4.

[0082] Preparation of spinning solution: Dissolve the dried polyimide in the mixed solvent of the first solvent and the first co-solvent (mass ratio 3:2), stir at room temperature for 24 hours to prepare spinning solution (the mass concentration of polyimide 22%).

[0083] Preparation of the core liquid: Mix hexamethylenediamine, the first solvent and the first non-solvent uniformly at a mass ratio of 5:47.5:47.5 to prepare...

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Abstract

A preparation method of hollow-fiber solvent-resisting nanofiltration membranes includes step 1, preparing solvents; step 2, filtering and defoaming spinning solutions, removing the spinning solutionsto spinning solution bottles, extruding the spinning solutions and core liquid from spinning nozzles after standing to form nascent-state membranes, and allowing the nascent-state membranes to entergel bath through air gaps at a certain distance to achieve curing and film formation; step 3, sufficiently rinsing the cured hollow-fiber membranes in deionized water for a certain time, soaking the hollow-fiber membranes in activation reagents at a certain temperature for a certain time, soaking the solvent-activated hollow-fiber membranes in glycerin liquors for a certain time, and drying the hollow-fiber membranes in the air before storing. The preparation method has the advantages that hollow-fiber membrane filaments are subjected to bisynchronous crosslinking before curing by crosslinkingagents in the core liquid and the gel bath, crosslinking reaction speeds of the crosslinking agents are increased effectively, the solvent-resisting hollow-fiber nanofiltration membranes can be produced in a large scale, and accordingly, the preparation method has wide application prospect in the field of organic solvent system separation.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and in particular relates to a preparation method and application of a hollow fiber solvent-resistant nanofiltration membrane. Background technique [0002] As a pressure-driven membrane separation technology between reverse osmosis and ultrafiltration, nanofiltration is widely used in many fields such as water treatment, food, medicine, textile, metallurgy, petrochemical and biochemical. However, a large number of organic solvents are used in industrial production, and the existing commercial nanofiltration membranes will swell when used in organic solvent systems, resulting in a decrease in separation performance, or even dissolution, resulting in complete loss of separation performance. Facing this technical problem that needs to be solved urgently, it is particularly critical to develop solvent-resistant nanofiltration (SRNF) membranes with high separation performance. [0003] S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/08B01D63/02B01D69/02C02F1/44C02F101/30
Inventor 苏保卫王振远许胜杰李树轩
Owner OCEAN UNIV OF CHINA
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