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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 effects on drugs and the human body, it is difficult to be used as an ideal biomedical material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

[0027] Add 1.0g of β-lactam into a 25mL sealed tube, stirrer and 10mL of 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 n-hexane solution, melted and sealed, and reacted at 25°C. After 2 hours, the system was difficult to stir, and then placed at this temperature to continue the reaction for 10 hours. After adding 2mL of 10wt% hydrochloric acid solution and 100mL of methanol to terminate the reaction and wash nylon 3, 2 × 100mL methanol fully washed the polymer under rapid stirring to remove unreacted monomers, (protonated) t-BuP4 and N, N-dimethylacetamide, filtered, vacuum dried at 50°C for 12h, and calculated the product The ratio is 94%, and the molecular weight is 1.1×10 5 g / mol.

Embodiment 3

[0029] Add 1.0g β-lactam, 0.005g activator N-benzoyl β-lactam (NBL), stirring magnet, and 10mL N,N-dimethylacetamide containing 10wt% LiCl to a 25mL sealed tube ( DMAc) solution, frozen with liquid nitrogen, replaced nitrogen three times, and then quickly injected 70 μL of t-BuP4 n-hexane solution under nitrogen atmosphere, sealed the tube, and reacted at 25° C. for 12 hours. After the reaction, add 2mL of 10wt% hydrochloric acid solution and 100mL of methanol to terminate the reaction and wash the nylon 3, then use 2×100mL of methanol to fully wash the polymer 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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