Polymerization with strong alkali phosphazene compound as catalyst

A polymerization reaction and compound technology, applied in the field of polymer synthesis, can solve problems such as difficult to use biomedical materials, difficult removal of metal ions, adverse effects of drugs and human body, etc., and achieve the effect of easy removal and mild reaction conditions

Inactive Publication Date: 2011-09-07
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the metal ions of this type of catalyst are not easy to be removed and have adverse ef

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0024] Example 1

[0025] In a dry 50mL three-necked flask with a stirrer and a thermometer, add 2.0g acrylamide, 20mL N,N-dimethylacetamide (DMAc), and add 100μL t-BuP 4 After reacting at 80 °C for 48 h, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction, and nylon 3 was washed, and then 2 × 100 mL of methanol was used to fully wash the polymer with rapid stirring to remove unreacted monoliths. bulk, (protonated) t-BuP 4 and N,N-dimethylacetamide, filtered, and dried under vacuum at 50°C for 12h, the calculated yield was 90%, and the molecular weight was 1.0×10 4 g / mol. Different from the polymerization of acrylamide initiated by the traditional strong base, the nylon 3 synthesized by the polymerization method does not contain double bond polymerization units, and does not need to add any free radical polymerization inhibitor.

Example Embodiment

[0026] Example 2

[0027] Add 1.0g β-lactam to a 25mL sealed tube, stir with a magnetic bar and 10mL N,N-dimethylacetamide (DMAc) solution containing 10wt% LiCl, freeze with liquid nitrogen, replace nitrogen three times and inject under nitrogen atmosphere 7 μL of t-BuP 4 The n-hexane solution was melted and sealed, and the reaction was carried out at 25 °C. After 2 hours, the system was difficult to stir, and then the reaction was continued at this temperature for 10 hours. After adding 2 mL of 10 wt% hydrochloric acid solution and 100 mL of methanol, the reaction was terminated and the nylon 3 was washed. 2 × 100 mL of methanol was thoroughly washed with rapid stirring to remove unreacted monomers, (protonated) t-BuP4 and N,N-dimethylacetamide, filtered, and dried under vacuum at 50 °C for 12 h. Calculate the yield. The rate is 94% and the molecular weight is 1.1×10 5 g / mol.

Example Embodiment

[0028] Example 3

[0029] In a 25 mL sealed tube, add 1.0 g β-lactam, 0.005 g activator N-benzoyl β lactam (NBL), a stirring magnet, and 10 mL N,N-dimethylacetamide (N,N-dimethylacetamide) containing 10 wt% LiCl ( DMAc) solution, frozen in liquid nitrogen, replaced with nitrogen three times, and quickly injected 70 μL of t-BuP4 in n-hexane solution under nitrogen atmosphere, sealed the tube, and reacted at 25 °C for 12 h. After the reaction, 2 mL of 10 wt% hydrochloric acid solution and 100 mL of methanol were added to terminate the reaction and wash nylon 3, and then the polymer was thoroughly washed with 2 × 100 mL of methanol under rapid stirring to remove unreacted monomers, (protonated) t-BuP4 and N,N-dimethylacetamide, filtered, vacuum dried at 50°C for 12h, the calculated yield was 95%, and the molecular weight was 1.2×10 4 g / mol

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PUM

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Abstract

The invention discloses polymerization with strong alkali phosphazene compound as catalyst. The phosphazene compound used as the catalyst is a strong alkali compound with double bonds of P=N, and monomers comprise lactam, lactone, cyclosiloxane, trioxymethylene, ring carbonate, cyclic ether and cyclic phosphate monomers. The condition of the polymerization disclosed by the invention is mild, and the polymerization is suitable for industrial production. The used catalyst has strong alkalinity and good dissolubility and contains no metal ions. The prepared material has good application prospect.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a polymerization reaction using a phosphazene strong base compound as a catalyst. Background technique [0002] Ring-opening polymerization is an important class of polymerization reactions besides stepwise polymerization and chain polymerization. Many cyclic monomers, such as caprolactone, glycolide, lactide, and carbonate, can be polymerized by ring-opening polymerization. These polymers often have excellent biocompatibility, biodegradability, and absorbability, and thus are widely used as various biomedical materials such as drug carriers, tissue engineering matrices, and surgical sutures. However, in general, the ring-opening polymerization of these monomers mostly uses an initiating catalyst system of an organoaluminum compound, a tin salt compound or a rare earth metal compound. Because the metal ions of this type of catalyst are not easy to be removed, it is ea...

Claims

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Application Information

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IPC IPC(8): C08F4/00C08F20/56C08G69/20C08G63/08C08G63/87C08G77/08C08G65/10C08G65/18C08G65/24C08G64/30C08G79/04C08G2/10C08G2/06
Inventor 张广照杨宏军
Owner SOUTH CHINA UNIV OF TECH
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