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L-proline immobilized temperature-sensitive hairy polymer microsphere and preparation method thereof

A proline temperature-sensitive, polymer technology, applied in the preparation of organic compounds, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of large amount of hybrid microspheres, L - Problems such as low proline immobilization amount achieve short catalytic time, increase rate and selectivity, and reduce production cost

Active Publication Date: 2020-04-14
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the hybrid microspheres prepared by the "click chemistry" method have the problem that the amount of L-proline immobilized on the surface of the microspheres is small (0.0551mmol / g), and the amount of hybrid microspheres used in the catalytic process is large.

Method used

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  • L-proline immobilized temperature-sensitive hairy polymer microsphere and preparation method thereof
  • L-proline immobilized temperature-sensitive hairy polymer microsphere and preparation method thereof
  • L-proline immobilized temperature-sensitive hairy polymer microsphere and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Measure monomer HEMA 1.2mL, EGDMA 0.8mL, and initiator AIBN 0.04g (0.244mmol), add them together into a 250mL round bottom flask, continue to add 80mL acetonitrile and stir until the mixture is uniform. Install a fractionation column, a condenser and a receiving flask, heat the round-bottomed flask slowly to bring the temperature of the reaction system to boiling within 25 minutes, control the time to distill 40 mL of acetonitrile within 1.5 hours, and then end the reaction. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 40 - co -HEMA) microspheres, referred to as PE 40 H.

[0035] Weigh PE 40 Add 0.3g of H, 0.272g (0.001mol) of BSPA, and 0.252g (0.002mol) of DMAP into a round bottom flask filled with 10mL of dichloromethane, and let stand in an ice-water bath for 20min. Weigh 0.036g (0.018mmol) of DCC in the above-mentioned round bottom...

Embodiment 2

[0045] Measure 0.8mL of monomer HEMA, 1.2mL of EGDMA, and 0.04g (0.16mmol) of initiator ABVN, add them together into a 250mL round bottom flask, continue to add 80mL of methanol and stir until the mixture is uniform. Install a fractionation column, a condenser tube and a receiving flask, heat the round-bottomed flask slowly to bring the temperature of the reaction system to boil within 15 minutes, control the time to distill 40 mL of methanol within 1 hour, and then end the reaction. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 60 - co -HEMA) microspheres, referred to as PE 60 H.

[0046] Weigh PE 60 Add 0.35g of H, 0.218g (0.6mmol) of DDMAT, and 0.384g (0.003mol) of DMAP into a round-bottomed flask filled with 20mL of dichloromethane, and let stand in an ice-water bath for 25min. Take DCC 0.042g (0.204mmol) in the above-mentioned round-botto...

Embodiment 3

[0051] Measure monomer HEMA 0.4mL, EGDMA 1.6mL, and initiator AIBN 0.04g (0.244mmol), add them together into a 250mL round bottom flask, continue to add 80mL tetrahydrofuran and stir until well mixed. Install a fractionation column, a condenser and a receiving flask, heat the round-bottomed flask slowly to bring the temperature of the reaction system to boil within 30 minutes, control the time to distill 40 mL of tetrahydrofuran within 2 hours, and then end the reaction. The product was separated by centrifugation, washed 3 times with ethanol, and dried to obtain a white powdery solid, that is, P(EGDMA) containing hydroxyl groups on the surface. 80 - co -HEMA) microspheres, referred to as PE 80 H.

[0052] Weigh PE 80 Add 0.4g of H, 0.272g (0.001mol) of BSPA, and 0.48g (0.004mol) of DMAP into a round-bottomed flask filled with 25mL of dichloromethane, and let stand in an ice-water bath for 30min. Weigh 0.053g (0.253mmol) of DCC in the above-mentioned round bottom flask, re...

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Abstract

The invention relates to a temperature-sensitive hairy polymer microsphere immobilized with L-proline. According to the preparation method, a P(EGDMA-co-HEMA) polymer microsphere is used as a core, atrithioester-based RAFT reagent is grafted, a polymer chain formed by copolymerizing NIPAM, N-boc-L-PolyA and MMA as monomers through a surface-initiated RAFT polymerization method to serve as a hairpart, and tert-butyloxycarboryl protection on the N-boc-L-PolyA is removed to obtain the polymer microsphere. According to the present invention, the L-proline immobilization amount on the temperature-sensitive polymer microsphere is large, the good catalysis effect is provided in direct catalysis of an asymmetric Aldol reaction in an aqueous phase environment, the catalysis reaction time is short, and the polymer microsphere can be separated from the catalysis system through simple centrifugal separation.

Description

technical field [0001] The invention belongs to the technical field of polymer catalyst preparation, and relates to an L-proline polymer catalyst, in particular to a hair-like polymer microsphere immobilized with L-proline, and the hair-like polymer microsphere preparation and application. Background technique [0002] The L-proline organic small molecule catalyst has the advantages of simple structure, cheap and easy to obtain, and can be used to catalyze direct asymmetric Aldol reaction without modification. However, when L-proline is directly used as a catalyst, there are disadvantages such as large dosage, difficulty in separating from the product and recycling, and the need for catalysis in an organic medium, which limits the application and development of L-proline. [0003] Using carrier materials to modify and immobilize L-proline is an effective method to solve the above problems. At present, substances that can be used as carrier materials mainly include inorgani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F267/06C08F265/06C08F220/54C08F220/14C08F220/36C08F220/20C08F222/14B01J31/06C07C205/45C07C201/12
CPCC08F267/06C08F265/06C08F220/20C08F222/10B01J31/063C07C201/12C08F2438/03B01J2231/4205C07C2601/14C08F220/54C08F220/14C07C205/45Y02P20/55
Inventor 申迎华王琴雅张光旭靳雯唐娱王文静吴乐轩戴胜
Owner TAIYUAN UNIV OF TECH
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