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Tetrahydrofuran-glycidol random hyperbranched copolyether and preparation method thereof

A technology of tetrahydrofuran and glycidol, which is applied in the field of tetrahydrofuran-glycidol random hyperbranched copolyether and its preparation, can solve the problems of high degree of branching of products and difficulty in controlling the degree of branching of polymers , to achieve the effect of wide sources, simple and easy methods, and easy access to raw materials

Inactive Publication Date: 2013-01-23
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods are difficult to control the degree of branching of the polymer, and the prepared products often have a higher degree of branching.

Method used

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  • Tetrahydrofuran-glycidol random hyperbranched copolyether and preparation method thereof
  • Tetrahydrofuran-glycidol random hyperbranched copolyether and preparation method thereof
  • Tetrahydrofuran-glycidol random hyperbranched copolyether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 10mL of tetrahydrofuran and 3mL of glycidol into a 100ml round bottom flask. After stirring for 10 minutes in an ice-water mixed bath, 0.1 mL of boron trifluoride tetrahydrofuran complex was added to react for 2 hours. Finally, 10 mL of water was added to terminate the reaction, and after stirring for 15 minutes, the mixture was evaporated to dryness to obtain a crude product. The crude product was purified by dialysis with a molecular weight cut-off of 300, and a colorless viscous liquid was obtained after drying. The product was characterized by Gel Permeation Chromatography-Laser Light Scattering-Viscosity Detector (such as figure 1 shown): Mn=8195, Mw=11640, Mw / Mn=1.42; the parameters of the Mark-Houwink-Sakurada equation are:

[0022] K:(5.639±0.078)×10 -1 mL / g

[0023] a:0.334±0.001

[0024] Where a is less than 0.5, indicating that the prepared polymer product has typical hyperbranched structure characteristics.

[0025] Proton nuclear magnetic spectrum...

Embodiment 2

[0027] 10 mL of tetrahydrofuran and 2 mL of glycidol were added to a 100 ml round bottom flask. After stirring for 15 minutes in an ice-water mixed bath, 0.18 g of phosphotungstic acid was added and reacted for 3 hours. Finally, 10 mL of 2% sodium hydroxide solution was added to terminate the reaction, stirred for 15 minutes and then evaporated to dryness to obtain a crude product. The crude product was characterized by gel permeation chromatography-laser light scattering (SEC-MALLS): Mn=6689, Mw=12200, Mw / Mn=1.824. From the elution curve of the test, it can be found that the product contains some oligomers of small molecules. The crude product was purified by dialysis for 36 hours in a dialysis bag with a molecular weight cut-off of 300. After drying, a colorless viscous product was obtained. Characterized by SEC-MALLS: Mn=11610, Mw=14540, Mw / Mn=1.196.

Embodiment 3

[0029] 10 mL of tetrahydrofuran and 3 mL of glycidyl alcohol were added to a 100 ml round bottom flask. After stirring for 15 minutes at minus 10°C, add 1 mL of acetic anhydride and 0.15 mL of perchloric acid. After reacting for 3 hours, add 10 mL of water to terminate the reaction. After stirring for 15 minutes, evaporate to dryness to obtain a colorless thick product. The crude product was dissolved in water and purified by dialysis with a dialysis bag with a molecular weight cut-off of 300. After drying, a colorless viscous liquid was obtained, characterized by SEC-MALLS: Mn=2266, Mw=2887, Mw / Mn=1.274).

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Abstract

The invention relates to a tetrahydrofuran-glycidol random hyperbranched copolyether and a preparation method of the tetrahydrofuran-glycidol random hyperbranched copolyether. The preparation method comprises the steps of selecting tetrahydrofuran as the linear monomer, and carrying out cationic ring opening polymerization to glycidol and tetrahydrofuran, so as to obtain the random hyperbranched copolyether, wherein ternary cyclic ether in the glycidol structure is to form ternary cyclic oxonium ion first in the chain initiation process during polymerizing; the highly-active ternary cyclic oxonium ion can synchronously initiate ring opening polymerization between the tetrahydrofuran and the glycidol, so as to achieve random copolymerization; once the ternary cycle of the glycidol is opened and enters the molecular chain, the contained alcoholic hydroxyl group is subjected to chain transfer reaction to generate new active points which initiate the lengthening of the chain, so that novel random hyperbranched copolyether is prepared. The preparation method provided by the invention is simple, convenient and easy to implement; the raw materials are easy to obtain; and initiating agents are available.

Description

technical field [0001] The invention belongs to the field of polymer material synthesis, and relates to a tetrahydrofuran-glycidyl alcohol random hyperbranched copolyether and a preparation method thereof. Background technique [0002] Hyperbranched polymers are a new class of polymer materials developed in recent decades. Their special three-dimensional topological structure makes the molecular chains less entangled, so they have superior physical properties such as low viscosity, difficult crystallization and easy film formation. chemical properties. At the same time, this highly branched structure can have a large number of active functional groups through chemical modification, and has important application value in the fields of nanomaterials, optoelectronic materials, biomedical materials, and supramolecular materials. Polyether polyols (referred to as polyether) are usually cyclic ether monomers such as ethylene oxide (EO), propylene oxide (PO), butylene oxide (BO), ...

Claims

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Application Information

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IPC IPC(8): C08G65/28
Inventor 范晓东范伟伟张万斌白阳王罡
Owner NORTHWESTERN POLYTECHNICAL UNIV
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