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Method for preparing polylactone

A polylactone and cyclic lactone technology, applied in the field of polylactone preparation, can solve the problems of unfavorable material stability, uncontrollable reaction process, low molecular weight of the product, etc., and achieve narrow molecular weight distribution index and no monomer residue , high catalytic efficiency

Active Publication Date: 2019-06-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method of preparing polyester is mainly polycondensation method. This method usually requires high temperature, consumes a lot of energy, and the obtained product has a low molecular weight and a wide molecular weight distribution. The reaction process is uncontrollable, which is not conducive to the stability of the material.

Method used

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  • Method for preparing polylactone
  • Method for preparing polylactone
  • Method for preparing polylactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] In a 10mL polymerization tube, add δ-valerolactone (0.27ml, 3mmol), hydantoin derivative (7) (0.016g, 0.1mmol), DBU (14.94ul, 0.1mmol), benzyl alcohol (10.34μL, 0.1mmol), stirred magnetically for 4 hours at 90°C, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, then slowly dropped the resulting solution into cold methanol, a white polymer was precipitated, and was centrifuged and vacuum-dried 0.38 g of the product was obtained, the conversion rate was 95.2%, the number average molecular weight Mn of polyvalerolactone was 3612 g / mol, and the molecular weight distribution PDI was 1.07. The hydrogen spectrum of polyvalerolactone is as follows figure 1 As shown, ( 1 H NMR (CDCl 3 ):δ(ppm),1.67–1.70(m,4H×n,(-CH 2 CH 2 CH 2 O-)n and (-COCH 2 CH 2 CH 2 -)n), 1.95(q, 2H, J=7.2Hz, ArCH 2 CH 2 CH 2 -),2.34(t,2H×n,J=6.9Hz,(-OCOCH 2 CH 2 -)n), 2.68(t, 2H, J=7.7Hz, ArCH 2 CH 2 -),3.65(t,2H,J=6.5Hz,-CH 2 CH ...

Embodiment 2

[0057] In a 10 mL polymerization tube, add D-lactide (0.072 g, 0.5 mmol), hydantoin derivative (3) (0.002 g, 0.01 mmol), 2-tert-butyl-1,1,3,3- Tetramethylguanidine (20.4ul, 0.1mmol), pentaerythritol (9.7μL, 0.1mmol), magnetically stirred at 200°C for 24 hours, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, and then dissolved the resulting solution Slowly drop into cold methanol, a white polymer precipitated, centrifuged and vacuum dried to obtain 0.034g of the product, the conversion rate was 67.9%, the number average molecular weight Mn of poly-D-lactide was 1310g / mol, and the molecular weight distribution PDI was 1.19.

Embodiment 3

[0059] In a 10mL polymerization tube, add L-lactide (7.2g, 50mmol), hydantoin derivative (4) (0.017g, 0.1mmol), tetramethylguanidine (12.55ul, 0.1mmol), benzyl alcohol ( 10.0 μL, 0.1 mmol), stirred magnetically at 130°C for 8 hours, stopped the reaction, added a small amount of dichloromethane dropwise to the resulting mixture to dissolve, then slowly dropped the resulting solution into cold methanol, a white polymer was precipitated, and centrifuged , Vacuum drying to obtain 5.9 g of the product, the conversion rate is 98.4%, the number average molecular weight Mn of poly-L-lactide is 37100 g / mol, and the molecular weight distribution PDI is 1.20. The hydrogen spectrum of polylactide is as image 3 As shown, ( 1 H NMR (400MHz, CDCl 3 ),δ(ppm),1.57-1.59(m,3H×n,(–CH 3 )n),4.34(m,1H,–CH(CH 3 )OH),5.13–5.21(q,1H×(n-1),–CH(CH 3 )O–; 2H, ArCH 2 O–), 7.33–7.34 (m, 5H, aryl).); Its size exclusion chromatography analysis spectrum is as Figure 4 As shown, it can be seen from th...

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Abstract

The invention discloses a method for preparing polylactone, and relates to the technical field of polymer materials. An initiator alcohol or amine is used to initiate ring opening of a cyclic lactonemonomer or a cyclic lactide monomer or a cyclic carbonate monomer, ring-opening polymerization of a small molecule monomer is initiated under the catalysis of an organic catalyst to obtain polylactone, and the organic catalyst is a hydantoin derivative and tertiary amine catalyst system. The method has the advantages of high catalytic efficiency, mild reaction, and high-efficiency synthesis of pure polylactone, and the product has the advantages of no metal residue, narrow molecular weight distribution, high product yield, no monomer residue and white color.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of polylactone. Background technique [0002] Among many synthetic polymer materials, aliphatic polyester occupies an important position due to its excellent biodegradability, bioabsorbability and biocompatibility, and has become a research hotspot in recent years. Due to the easily hydrolyzed ester group in the molecular structure of this kind of polyester, it is easy to gradually decompose into oligomers or monomers in the presence of water and microorganisms, and then be metabolized into carbon dioxide and water, so it can show certain biodegradability. Compatibility, which has great application potential in biomedicine, tissue engineering and other fields. [0003] The traditional method of preparing polyester is mainly polycondensation method. This method usually requires high temperature, consumes a lot of energy, and the obtained product has...

Claims

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Application Information

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IPC IPC(8): C08G63/87C08G63/08C08G64/02C08G64/30
Inventor 郭凯李振江张婵李洁姚志威刘博
Owner NANJING UNIV OF TECH
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