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Multi-arm [ps-b-pma(11c)az]x liquid crystal block copolymer, preparation method and application thereof

A block copolymer, ps-b-pma technology, applied in liquid crystal materials, chemical instruments and methods, membrane technology, etc., can solve the problem of single performance, high price, difficult and efficient separation of microfiltration membrane materials and high membrane flux And other issues

Active Publication Date: 2022-07-19
HUBEI ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these microfiltration membrane materials are difficult to achieve high-efficiency separation and high membrane flux at the same time, and they are expensive and have single performance.

Method used

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  • Multi-arm [ps-b-pma(11c)az]x liquid crystal block copolymer, preparation method and application thereof
  • Multi-arm [ps-b-pma(11c)az]x liquid crystal block copolymer, preparation method and application thereof
  • Multi-arm [ps-b-pma(11c)az]x liquid crystal block copolymer, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Arms [PS 11 -b-PMA(11C)Az 5 ] 2 The preparation method of liquid crystal block copolymer comprises the following steps:

[0069] 1) Synthesis of double-arm small molecule initiator 1,4-phenylene-bis-2-bromoisobutyrate:

[0070] 5 g of hydroquinone and 250 mL of tetrahydrofuran after dewatering were sequentially added to a clean single-necked bottle and stirred evenly, and then placed in an ice bath at 0°C and stirred for 30 min. Then use a syringe to draw 1.1 equivalents of 7.0 mL of triethylamine acid binding agent and add it to the above system, and continue to stir evenly in an ice bath at 0 °C. Finally, use a syringe to draw 1.1 equivalents of 6.2 mL of 2-bromoisobutyryl bromide into a dry constant pressure dropping funnel, and slowly drop it into the above reaction flask. After the dropwise addition, remove the constant pressure dropping funnel and plug it tightly. The rubber stopper continued to react for 16 hours.

[0071] After the reaction time was reached...

Embodiment 2

[0079] Arms [PS 16 -b-PMA(11C)Az 5 ] 2 The preparation method of the liquid crystal block copolymer is the same as that in Example 1, except that:

[0080] In step 2), initiator: St: ligand: catalyst=1:40:2:2 (molar ratio). The dosage of each substance is: initiator 0.5g, ligand 512μL, CuCl 243.0mg, St 5.7mL, and reaction solvent chlorobenzene 6.0mL. Finally, [PS with a block number of 16 is obtained 16 ] 2 Macromolecular initiator 5.0g;

[0081] In step 3), take the arms [PS 16 ] 2 is a macromolecular initiator, and macromolecular initiator: MA(11C)Az: ligand: CuCl=1:40:2:2 (molar ratio), the dosage of each substance is: initiator 0.5g, monomer MA (11C) Az is 3.0 g, ligand 62.7 μL, CuCl 30.0 mg; reaction solvent chlorobenzene 4 mL, DMF 2 mL. The resulting product double-arm [PS 16 -b-PMA(11C)Az 5 ] 2 of 1 H NMR chart see figure 1 , see GPC diagram image 3 .

Embodiment 3

[0083] Three Arms [PS 11 -b-PMA(11C)Az 5 ] 3 The preparation method of the liquid crystal block copolymer is the same as that in Example 1, except that:

[0084] In step 1), phloroglucinol is used as the substrate of a small molecular hydroxy compound, and phloroglucinol: 2-bromoisobutyryl bromide: triethylamine=1:1.7:1.7 (molar ratio). The dosage of each substance is respectively: phloroglucinol 5g, 2-bromoisobutyryl bromide 8.4mL, triethylamine 9.4mL, and the reaction solvent is anhydrous tetrahydrofuran 250mL. Finally, 20.0 g of 1,3,5-phenylene-tri-2-bromoisobutyrate, a three-arm small molecule initiator, was obtained.

[0085] In step 2), the three-arm small molecule initiator 1,3,5-phenylene-tri-2-bromoisobutyrate is used as the small molecule initiator, and the initiator: St: ligand: CuCl=1: 60:3:3 (molar ratio). The dosage of each substance is: initiator 0.5 g, ligand 548 μL, CuCl 260.0 mg, St 6.0 mL, and reaction solvent chlorobenzene 6 mL. Finally, a three-arm w...

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Abstract

The present invention provides multi-arm [PS‑b‑PMA(11C)Az] x Liquid crystal block copolymer and its preparation method and application, wherein, [PS‑b‑PMA(11C)Az] x The liquid crystal block copolymer has the following structure: wherein, x is 2 or 3, m is 2-600, and n is 2-300. In the present invention, multi-arm [PS-b-PMA(11C)Az] is synthesized by small molecule acylation reaction and two-step ATRP method x liquid crystal block copolymer, and obtain a certain thickness of the liquid crystal block copolymer (BCP) honeycomb microporous film by dropping into a film. The membrane has potential application value in the fields of microfiltration separation, high-efficiency catalytic material preparation, and microelectronics.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to multi-arm [PS-b-PMA(11C)Az] x Liquid crystal block copolymer and its preparation method and application. Background technique [0002] Since the 21st century, with the continuous improvement of people's living standards and the rapid development of modern industries, a steady stream of domestic sewage and industrial wastewater has been discharged into the sea, which has resulted in the inability to guarantee the quality of human drinking water sources. The core technology of wastewater resource utilization is the research and development of high-performance separation membranes. Therefore, it is urgent to explore excellent separation membrane materials and gradually optimize the preparation process to achieve convenient, fast and efficient pretreatment of sewage. [0003] At present, commercialized high-efficiency separation membranes include flat, roll, tubular, holl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F220/36C09K19/38B01D67/00B01D71/80C02F1/44
CPCC08F293/005C08F220/36C09K19/3809B01D71/80B01D67/0002C02F1/444C08F2438/01
Inventor 屈婷郭荣刘海钟菲龚春丽胡富强汪杰郑根稳
Owner HUBEI ENG UNIV
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