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A method for rapid and efficient separation of stimuli-responsive star and linear polymers

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

Active Publication Date: 2022-07-12
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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  • A method for rapid and efficient separation of stimuli-responsive star and linear polymers
  • A method for rapid and efficient separation of stimuli-responsive star and linear polymers
  • A method for rapid and efficient separation of stimuli-responsive star 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 to OEGMA is 99:1 by mole, and the star polymer (Star-P (MEO 2 MA-co-OEGMA)) with a grafting degree of 6 as an example:

[0073] 1) Add 10 mL of solvent N,N'-dimethylformamide (DMF), two monomers 2-(2-methoxyethoxy) ethyl methacrylate (MEO) to a 50 mL Schlenk tube 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 uniformly, the oxygen in the system is removed by the refrigerated pumping operation three times. After reacting at 90° C. for 8 h, the reaction system was vented to the atmosphere to stop the reaction. Next, the product...

Embodiment 2

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

[0078] 1) In a 50mL Schlenk tube, add 10mL 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)sulfanylvaleric acid (DTTCP) 0.0645g, and initiator azobicyclohexylmethyl Nitrile (ACCN) 0.0039 g. After the system was evenly mixed, the oxygen in the system was removed by refrigerating and pumping three times. After reacting at 90° C. for 8 h, the reaction system was vented to the atmosphere to stop the reaction. Next, the product was transferred out and dialyzed through a 3000MW molecular weight dialysis bag for 48 hours to obtain LCST type linear homopolymer Linear-PMEO with a degree of polymerization of 100 2 MA, and then place the dialysis product in a freeze dryer to dry for...

Embodiment 3

[0082] Take the design of UCST type zwitterionic linear homopolymer Linear-PDDMAS with a polymerization degree of 80 and a star polymer Star-PDDMAS with a grafting 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-bottomed flask, and acetone (90ml) was used as a solvent to react for 24 hours at 50°C, After suction filtration with a vacuum diaphragm pump, the product was placed in an oven for 24 hours to obtain 3-(2-methacryloyloxyethyldimethylamino)propanesulfonate (DMAPS) as a white solid powder product.

[0084] 2) 8mL of laboratory-made 0.5M sodium chloride solvent was added to the 25mL Schlenk polymerization tube, 2.0g of the self-made monomer DMAPS in step 1, and ECT 4-cyano-4-( ((Ethylthio)thiocarbonyl)thio)valeric acid (ECT) 0.024g and initiator azobicyclohexylcarbonitrile (ACCN) 0.0044g, after the system was evenly mixed, they were refrigerated and extrac...

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Abstract

The invention discloses a method for purifying the target star-shaped polymer by utilizing the stimuli-response characteristics of the star-shaped polymer and combining with centrifugal operation. In the initial design, the synthetic technology route of "arm first, core later" and the polymerization method of reversible addition-fragmentation chain transfer polymerization were used to synthesize stimuli-responsive polymers with temperature-responsive (UCST and LCST) and pH-responsive arms. For the UCST type, we chose DMAPS as the monomer, and the RAFT reagent ECT. For LCST type, we will MEO 2 MA and OEGMA monomers were copolymerized or homopolymerized with the RAFT reagent DTTCP. The linear polymers Linear-PDMAPS and Linear-P (MEO 2 MA‑co‑OEGMA) and then cross-linked into star polymers. Due to the problem of conversion rate and the drawbacks of the synthetic route, it is difficult to remove the unconverted linear polymer mixed in the obtained product, and the molecular weight distribution of the star polymer product is wide. The method utilizes the response difference of linear and star polymers, adopts centrifugation method, and removes the linear polymer quickly and efficiently, and obtains a product with extremely narrow molecular weight distribution.

Description

technical field [0001] The invention relates to a method for rapidly and efficiently separating star-shaped and linear polymers by means of centrifugation by utilizing the synergistic effect of temperature response and pH response. Background technique [0002] Star-shaped polymer refers to a complex topology polymer with three or more branches of the same or different composition (branch chains are not divided into primary and secondary), 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 their relatively simple synthesis that they have been widely used in drug carriers, polymer films, interface stabilizers and nano-imaging in recent years. However, with the rapid development and application of star polymers, researchers ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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