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A preparation method of a polymer organic ligand, a preparation method of a polymer metal-organic framework, an ion separation membrane and a preparation method thereof

A metal-organic framework and ion separation technology, which is applied in the preparation of polymer metal-organic frameworks, ion separation membranes and their preparation, and the preparation of polymer organic ligands, can solve the problem of long-term stability of polymer metal-organic frameworks that needs to be improved and other problems, to achieve the effect of simple and effective construction, simplified preparation, and improved stability

Active Publication Date: 2020-05-01
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the above two approaches basically combine polymer materials with MOF materials in the form of physical blending, and the long-term stability of polymer metal-organic frameworks has been to be improved.
However, there are no relevant reports on PolyMOF materials with soluble properties. The soluble properties can greatly expand the application range of PolyMOF and make the preparation of PolyMOF thin layers easier.

Method used

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  • A preparation method of a polymer organic ligand, a preparation method of a polymer metal-organic framework, an ion separation membrane and a preparation method thereof
  • A preparation method of a polymer organic ligand, a preparation method of a polymer metal-organic framework, an ion separation membrane and a preparation method thereof
  • A preparation method of a polymer organic ligand, a preparation method of a polymer metal-organic framework, an ion separation membrane and a preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Preparation of polymeric organic ligands:

[0059] Diethyl 2,5-dihydroxyterephthalate (1.2 g, 4.7 mmol), 1,10-dibromodecane (4.7 mmol) and potassium carbonate (2.6 g, 19.0 mmol) were mixed and added to 33 mL A suspension was formed in DMSO, and the reaction was stirred at 100 °C for 24 h.

[0060] After the above reaction system was cooled down to room temperature, 50 mL of water was added to the reaction system, and the obtained reaction product was separated by centrifugation, and then the product was washed three times with methanol and acetone, each time with 35 mL of detergent.

[0061] The products of the above steps were collected by centrifugation, and dried overnight at 60°C. The obtained dry product (1.0g) was added to a total of 30mL of a mixed solution of water and DMSO with a volume ratio of 1:1, and 4.0g of KOH was added, and the mixed solution was heated to 80°C and reacted for 8h to obtain a clear solution until.

[0062] The resulting clear solution ...

Embodiment 2

[0075] The polymer organic ligand, polymer metal organic framework and ion separation membrane were prepared according to the method described in Example 1, the difference from Example 1 was that 1,9-dibromononane was used.

[0076] The nuclear magnetic resonance detection result of the macromolecular organic ligand prepared in Example 2 of the present invention is as follows image 3 shown. Depend on image 3 It can be seen that there is an obvious strong peak of carboxyl hydroxyl hydrogen near 12.8ppm, indicating that the hydrolysis reaction is relatively complete, the original carboxylate has been hydrolyzed into carboxylic acid, and the polymer organic ligand can be used for coordination. At the same time, near 7.26ppm, there is a characteristic peak of methylene group shifted due to the connection with oxygen atom, indicating that the original hydroxyl group has been replaced by an alkoxy group. From this, it can be determined that the synthesis of polymeric organic lig...

Embodiment 3

[0081] The polymer organic ligand, polymer metal organic framework and ion separation membrane were prepared according to the method described in Example 1, the difference from Example 1 was that 1,11-dibromoundecane was used.

[0082] The nuclear magnetic resonance detection result of the macromolecular organic ligand prepared in Example 3 of the present invention is as follows Figure 4 shown. Depend on Figure 4 It can be seen that there is an obvious strong peak of carboxyl hydroxyl hydrogen near 12.8ppm, indicating that the hydrolysis reaction is relatively complete, the original carboxylate has been hydrolyzed into carboxylic acid, and the polymer organic ligand can be used for coordination. At the same time, near 7.26ppm, there is a characteristic peak of methylene group shifted due to the connection with oxygen atom, indicating that the original hydroxyl group has been replaced by an alkoxy group. From this, it can be determined that the synthesis of polymeric organi...

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Abstract

The invention provides a preparation method of a high-molecular organic ligand. The preparation method comprises the following steps: enabling diester of terephthalic acid, a dibromoalkane compound and potassium carbonate to react in a solvent to obtain a reaction product; enabling the reaction product to react with a base to obtain an intermediate product; enabling the intermediate product to react with an acid to obtain the high-molecular organic ligand. In the invention, the surface of a porous substrate is coated with a high-molecular organic metal framework layer, and a function of selective ion separation is effectively realized by use of an aperture sieving effect; moreover, the high-molecular organic metal framework is applied to the surface of the porous substrate in a solution state, thus the acting force between the high-molecular organic metal framework and the substrate is remarkably enhanced, and the applicability of an ion separation membrane is improved. The invention also provides a preparation method of the high-molecular organic metal framework and an ion separation membrane and a preparation method of the ion separation membrane.

Description

technical field [0001] The invention relates to the technical field of ion separation, in particular to a preparation method of a polymer organic ligand, a preparation method of a polymer metal organic framework, an ion separation membrane and a preparation method thereof. Background technique [0002] Metal-organic frameworks, as an emerging porous material, have attracted attention due to their wide range of applications. Metal-organic framework (MOF) materials have outstanding performance in the fields of gas separation and storage, drug delivery, ion separation, etc., because of the various forms of pores in their structure, which is an advantage that other materials do not have. However, MOF materials are transition metal ions or metal clusters and organic ligands using molecular assembly and crystal engineering methods to obtain cavity coordination polymers with a certain pore size and framework, and contain free anions to neutralize charges. Due to the irregularity o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C08G65/40B01D67/00B01D69/10
CPCB01D67/0088B01D69/10C08G65/4006C08G83/008
Inventor 徐铜文葛亮王鑫伍斌徐婷婷
Owner UNIV OF SCI & TECH OF CHINA
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