A kind of polyglycolic acid material and its preparation method and application
A technology of polyglycolic acid and diethyl oxalate, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of decreased mechanical properties of materials, decreased molecular weight of ester polymers, etc.
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Embodiment 1
[0051] In a 500mL three-neck flask, add 15mL diethyl oxalate, 200mL ethanol, 9mL ethanolamine, and 6mL n-propylamine, react at 50°C for 24h, filter to obtain the solid component, wash with ethanol several times, and then dry in a vacuum oven for 24h to obtain terminal functional groups Compound Intermediate A: N 1 -(2-Hydroxyethyl)-N 2 - Propyloxamide, namely:
[0052]
[0053] Weigh glycolide and N at a mass ratio of 100:1 1 -(2-Hydroxyethyl)-N 2 - Propyl oxalamide, add 0.5wt% stannous octoate, melt reaction at 135° C. for 24 hours under vacuum and reduced pressure atmosphere to obtain a white solid, and obtain a new polyglycolic acid material after drying (yield 86.8%).
[0054] figure 1 It is the proton nuclear magnetic spectrum of the terminal functional group compound intermediate product A of the gained of the present embodiment, and its data are as follows: 1 H NMR (400MHz, DMSO) δ8.65–8.50 (m, 2H), 4.76 (t, 1H), 3.45 (q, 2H), 3.21 (q, 2H), 3.08 (q, 2H), 1.54-1....
Embodiment 2
[0058] In a 500mL three-neck flask, add 50mL diethyl oxalate, 200mL ethanol, and 10mL ethylenediamine, react at 50°C for 24h, filter to obtain the solid component, wash with ethanol several times, and then dry it in a vacuum oven for 24h to obtain intermediate product B , Weigh the intermediate product B, ethanolamine and n-propylamine at a molar ratio of 10:1:1.1, slowly add the intermediate product B / chloroform solution dropwise to the tetrahydrofuran solution containing excess ethanolamine and n-propylamine using a constant pressure dropping funnel, heat and stir, Reflux for 24h to obtain a white suspension, filter, wash and dry to obtain the compound intermediate product C:N 1 -(2-Hydroxyethyl)-N 2 -(2-(2-Oxo-2-(propylamino)acetamido)ethyl)oxamide, namely:
[0059]
[0060] Weigh glycolide and N at a mass ratio of 100:1 1 -(2-Hydroxyethyl)-N 2 -(2-(2-Oxo-2-(propylamino)acetamido)ethyl)oxalamide, add 0.5wt% stannous octoate, and melt at 135°C for 24 hours under vacuum...
Embodiment 3
[0074] Example 3 explores the influence of different primary amine compounds on the prepared polyglycolic acid material
[0075] Referring to Example 1, the n-propylamine was replaced by the primary amine compound shown in Table 2, and other process conditions remained unchanged to prepare the corresponding polyglycolic acid material.
[0076] The performance results of the obtained materials are shown in Table 2.
[0077] The performance result of the polyglycolic acid material that table 2 different primary amine compounds make
[0078]
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