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Topological structure polymer, and preparation method and application thereof

A topology and polymer technology, applied in the preparation of organic compounds, carboxylic acid ester preparation, drilling composition, etc., can solve the adverse effects of polymer physical and chemical properties, dithioester group or xanthate The group is not easy to remove, the polymer is not easy to low molecular weight, etc.

Inactive Publication Date: 2015-03-11
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to overcome the polymer prepared by the reversible addition-fragmentation chain transfer polymerization method in the prior art is difficult to reach low molecular weight (such as number average molecular weight between 500~10000) and the polymer containing The dithioester group or xanthate group of the disulfide group or the xanthate group is not easy to remove the defect that brings adverse effects on the physical and chemical properties of the polymer, and provides a topological structure polymer and its preparation method and application

Method used

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  • Topological structure polymer, and preparation method and application thereof
  • Topological structure polymer, and preparation method and application thereof
  • Topological structure polymer, and preparation method and application thereof

Examples

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Embodiment 1

[0111] Step a), take tris(hydroxymethyl)ethane (5.4g), chloroform (50ml), pyridine (8ml) in the reactor, place the reactor in an ice-water bath, slowly add 2-bromopropionyl bromide ( 29.1 g), remove the ice-water bath after the dropwise addition, seal the reactor, and stir and react at room temperature for 48-72 hours. The organic phase was washed with 50ml of 25vt% dilute hydrochloric acid and 100ml of 10wt% sodium bicarbonate solution and dried over anhydrous magnesium sulfate for several hours. The solvent was distilled off under reduced pressure to obtain a white solid powder.

[0112] Step b). Take the three-arm brominated precursor (20g), chloroform (100ml) and excess potassium ethyl xanthate (40g) in the reactor at room temperature and stir for 72h to 96h, then filter The excess suspended potassium ethyl xanthate was washed 5 times with 100 ml of chloroform, and the solvent was distilled off under reduced pressure. Obtain 8.7g three-arm topology xanthates (its structu...

Embodiment 2

[0114] Step a), take pentaerythritol (5.72g), chloroform (50ml), and pyridine (8ml) in the reactor, place the reactor in an ice-water bath, slowly add 2-bromopropionyl bromide (30.0g), dropwise Finally, the ice-water bath was removed, the reactor was sealed, and the reaction was stirred at room temperature for 48-72h. The organic phase was washed with 60ml of 25vt% dilute hydrochloric acid and 120ml of 10wt% sodium bicarbonate solution and dried over anhydrous magnesium sulfate for several hours. The solvent was distilled off under reduced pressure to obtain a white solid powder.

[0115] Step b), take the product four-arm brominated precursor (20g) of the above step a), chloroform (10ml), excess potassium ethyl xanthate (4g) in the reactor at room temperature and stir for 72h-96h, filter the excess The suspended potassium ethyl xanthate was washed 6 times with 120 ml of chloroform, and the solvent was distilled off under reduced pressure. Obtain 9.2g four-arm topology xanth...

Embodiment 3

[0117] Take vinyl acetate (18ml), tetrahydrofuran (4ml), helium diisobutyronitrile (0.6065g) and 1.5g of the three-arm topoxanthate prepared in Example 1, and mix them uniformly. Before the reaction, the reactor was evacuated and dry nitrogen was introduced three times, and the reactor was sealed. The reactor was stirred and reacted at a constant temperature of 60°C for 30 minutes, and the product obtained from the reaction was dissolved in 5ml of tetrahydrofuran, precipitated in 200ml of ice-n-hexane, filtered with suction, and the precipitate was vacuum-processed in a 40°C oven for 48 hours to obtain 2.8g with a molecular weight of 956 and a molecular weight distribution of 1.04 polyvinyl acetate.

[0118] Take polyvinyl acetate (2.46mmol), tetrahydrofuran (3ml), isopropanol (6ml) and dilauroyl peroxide (8mmol) synthesized in the previous step reaction in the reactor, vacuumize and feed dry nitrogen repeatedly three times, seal reactor. React at 70°C for 6 hours, dissolve ...

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Abstract

The invention discloses a topological structure polymer, and a preparation method and application thereof. The invention provides a topological structure polymer disclosed as Formula 2 or Formula 2', wherein n represents polymerization degree, and n=10-250. The preparation method of the topological structure polymer is simple to operate, has wide monomer application range, can remove bis thioester group or xanthate group on the polymer, enhances the physicochemical properties of the polymer, and widens the application prospects of the polymer. The topological structure polymer without the terminal bis thioester group or terminal xanthate group has the advantages of lower molecular weight and narrow molecular weight distribution. Compared with the traditional high-molecular-weight topological structure polymer or linear polymer, the topological structure polymer disclosed by the invention has special physicochemical properties. For example, the topological structure polymer has higher solubility in carbon dioxide, and thus, is suitable for application as a carbon-dioxide-philic chain segment in related aspects (for preparing a carbon dioxide thickener, for preparing a carbon dioxide aqueous emulsion or the like).

Description

technical field [0001] The present invention specifically relates to topological structure polymers and their preparation methods and applications. Background technique [0002] Topological polymers with star-shaped and hyperbranched structures have unique properties different from those with linear chain structures. They are a new type of functional polymer materials with important application prospects in the fields of material modification, nanotechnology and biomedicine. , has received increasing attention. For example: hyperbranching of spherical structures, dendritic and star-shaped macromolecules have higher aggregated unit density than linear macromolecules, have ultra-low viscosity in solution, and have a large number of end groups available. Star-shaped block polymers exhibit better solubility and stronger viscoelasticity than linear polymers, and can form complex self-assembled morphologies under specific solvent conditions. [0003] For a polymer with a relativ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F118/08C08F2/38C08F8/00C08F222/14C08F218/08C07C67/317C07C69/73C09K8/588C09K8/594
Inventor 刘涛苏媚胡冬冬孙少俊张颖娜赵玲
Owner EAST CHINA UNIV OF SCI & TECH
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