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Method for rapidly and efficiently separating stimuli-responsive star-shaped and linear polymers

A stimuli-responsive, star-shaped polymer technology, applied in the field of rapid and efficient separation of star-shaped and linear polymers, can solve the problems of low operational flexibility, low separation power, incomplete separation, etc., and achieves high operational flexibility and requirements. The effect of small, shortened operation time

Active Publication Date: 2021-04-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The dialysis method is very simple to operate, but it takes a long time, the separation power is small, and the separation is not complete. Moreover, this method is limited by the commercially available dialysis bags, and the operation flexibility is very low.
The precipitation method takes a short time to operate, but it often requires fractional precipitation, and often requires post-treatment of the product, which is cumbersome to operate

Method used

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  • Method for rapidly and efficiently separating stimuli-responsive star-shaped and linear polymers
  • Method for rapidly and efficiently separating stimuli-responsive star-shaped and linear polymers
  • Method for rapidly and efficiently separating stimuli-responsive star-shaped and linear polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] To design LCST type linear copolymer Linear-P (MEO 2 MA-co-OEGMA) degree of polymerization is 100, monomer MEO 2 The ratio of MA and OEGMA is 99:1 by mole, star polymer (Star-P(MEO 2 MA-co-OEGMA)) degree of grafting is 6 as an example:

[0073] 1) In a 50mL Schlenk tube, add solvent N,N'-dimethylformamide (DMF) 10mL, two monomers 2-(2-methoxyethoxy) ethyl methacrylate (MEO 2 MA) 0.08g and oligo(ethylene glycol) methyl ether methacrylate (OEGMA, M n =500g·mol -1 ) 2.92g, a total of 3g (the molar ratio of the two monomers is 99:1). Oil-soluble carboxyl-terminated RAFT reagent 4-cyano-4-(dodecylsulfanylthiocarbonyl)sulfanylvaleric acid (DTTCP) 0.063g and initiator azobicyclohexylcarbonitrile (ACCN) 0.008 g. After the system is mixed evenly, the oxygen in the system is removed by freezing and pumping three times. After reacting at 90° C. for 8 h, the reaction system was aired to stop the reaction. Next, the product is transferred out, and after 48 hours of dialysis t...

Embodiment 2

[0077] To design LCST type linear homopolymer Linear-PMEO 2 The degree of polymerization of MA is 100, and the star polymer Star-PMEO 2 MA grafting degree is 6 as an example:

[0078] 1) In a 50mL Schlenk tube, add 10mL of solvent N,N'-dimethylformamide (DMF), monomer 2-(2-methoxyethoxy) ethyl methacrylate (MEO 2 MA) 3g, oil-soluble carboxyl-terminated RAFT reagent 4-cyano-4-(dodecylsulfanylthiocarbonyl)sulfanylpentanoic acid (DTTCP) 0.0645g, and initiator azobicyclohexylmethyl Nitrile (ACCN) 0.0039 g. After the system was mixed evenly, the oxygen in the system was removed by freezing and pumping three times. After reacting at 90° C. for 8 h, the reaction system was aired to stop the reaction. Next, the product is transferred out and dialyzed through a 3000MW molecular weight dialysis bag for 48 hours to obtain the LCST type linear homopolymer Linear-PMEO with a polymerization degree of 100 2 MA, and then the dialysis product was dried in a freeze dryer for 72 h to consta...

Embodiment 3

[0082] Take the design of the UCST type zwitterionic linear homopolymer Linear-PDMAPS with a polymerization degree of 80 and the star-shaped polymer Star-PDMAPS with a graft degree of 6 as an example:

[0083] 1) At the beginning, 10.89g of dimethylaminoethyl methacrylate (DMAEMA) and 8.461g of propane sultone were added to a 250ml round bottom flask, and acetone (90ml) was used as a solvent to react at 50°C for 24 hours. After suction filtration by a vacuum diaphragm pump, it was placed in an oven for 24 hours to obtain a white solid powder product 3-(2-methacryloyloxyethyldimethylamino)propanesulfonate (DMAPS).

[0084] 2) Add 8 mL of laboratory-made 0.5M sodium chloride solvent into a 25 mL Schlenk polymerization tube, use 2.0 g of self-made monomer DMAPS in step 1 as the monomer, and water-soluble carboxyl-terminated RAFT reagent ECT 4-cyano-4-( ((Ethylthio) thiocarbonyl) thio) valeric acid (ECT) 0.024g and initiator azobicyclohexylcarbonitrile (ACCN) 0.0044g, after mixing...

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Abstract

The invention discloses a method for purifying a target star-shaped polymer by utilizing stimulus response characteristics of the star-shaped polymer and combining centrifugal operation. In the initial design, an 'arm-first and core-second' synthesis technical route and a reversible addition fragmentation chain transfer polymerization method are selected, and stimulus-responsive polymers with different arm numbers and temperature response (UCST and LCST) and pH response are synthesized. For a UCST type, DMAPS is selected as a monomer, and an RAFT reagent ECT is selected. For an LCST type, MEO2MA and OEGMA monomers are subjected to copolymerization or homopolymerization by using an RAFT reagent DTTCP. The linear polymer Linear-PDMAPS and the linear polymer Linear-P (MEO2MA-co-OEGMA) are obtained, and then are cross-linked to form a star-shaped polymer. Due to the problem of conversion rate and the defects of a synthetic route, unconverted linear polymers mixed in the obtained product are difficult to remove, and the molecular weight distribution of the star-shaped polymer product is wide. According to the method, linear and star polymer response differences are utilized, a centrifugation method is adopted, the linear polymer is rapidly and efficiently removed, and a product with extremely narrow molecular weight distribution is obtained.

Description

technical field [0001] The invention relates to a method for rapidly and efficiently separating star-shaped and linear polymers in a centrifugal manner by utilizing the synergistic effect of temperature response and pH response. Background technique [0002] A star polymer refers to a complex topological polymer that has three or more branched chains with the same or different composition (the branched chains are not divided into primary and secondary chains), which are connected to the same central core through chemical bonds. Compared with other polymers, star polymers have a unique dense spatial structure, lower diffusion coefficient, melt viscosity, crystallinity and hydrodynamic volume. It is precisely because of the special advantages of star polymers and the relatively simple synthesis that they have been widely used in drug carriers, polymer films, interface stabilizers, and nanoimaging in recent years. However, with the rapid development and wide application of sta...

Claims

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Application Information

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IPC IPC(8): C08F265/06C08F220/28C08F222/38C08F6/00C08L51/00
Inventor 冯岸超李昊李智张立群
Owner BEIJING UNIV OF CHEM TECH