Polyester, polyurethane and methods for producing same
A kind of manufacturing method, technology of polyester, applied in the field of ester of polyurethane and 3-carboxymuconolactone
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Embodiment 1
[0068] Example 1: 2-(2-methoxy-2-oxoethyl)-5-oxo-2,5-dihydrofuran-3-carboxylic acid Manufacture of methyl esters
[0069]
[0070] 3-Carboxymuconolactone (1.69 g, 9.00 mmol) was put in a 25 ml flask, and 10 ml (excess) of methanol was added, stirred, and dissolved. 3-Carboxymuconolactone was obtained according to the method described in Japanese Patent Application No. 2006-218524. After completely dissolving 3-carboxymuconolactone, several drops of concentrated sulfuric acid were added as an acid catalyst, and the mixture was refluxed and stirred at 100° C. under atmospheric atmosphere for 9 hours. The obtained solution was dissolved in an aqueous sodium bicarbonate solution, chloroform was added, and the organic layer was extracted (×2). The obtained organic layer was dried over magnesium sulfate, and the organic layer was distilled off under reduced pressure to obtain 1.43 g of the target compound (yield 73.6%).
[0071] 1 H-NMR (500MHz, CDCl 3 )δ (ppm): 2.77 (1H ...
Embodiment 2
[0074] Embodiment 2: the manufacture of polyester
[0075]
[0076] Put 3-carboxymuconolactone (3.57 g, 19.2 mmol) in a 25 ml flask, add tetrahydrofuran (7 mL), and dissolve while stirring. After completely dissolving 3-carboxymuconolactone, ethylene glycol (1.19 g, 19.2 mmol) was added thereto, and after stirring for 5 minutes, several drops of concentrated hydrochloric acid were added as an acid catalyst, and stirred at 100° C. for several days. The obtained solution was dried at 60° C. under vacuum to obtain 3.72 g (yield: 71.3%) of polyester of the general formula (I) as a viscous solution.
[0077] 1 H-NMR (500MHz, CDCl 3 ) δ (ppm): 2.7 (1H q), 3.2 (1H q), 4.4 (4H m), 5.6 (1H m), 6.7 (1H d).
[0078] 13 C-NMR (500MHz, CDCl 3 ) δ (ppm): 37.3 (5-position α of lactone ring), 62.1 (alkyl), 78.3 (lactone ring), 127.9 (lactone ring), 155.4 (lactone ring), 161.2 (carboxyl), 170.9 ( lactone ring), 172.7 (carboxyl).
[0079] IR(v / cm -1 ): 2962 (alkyl chain), 1736 (lac...
Embodiment 3
[0083] Embodiment 3: the manufacture of polyurethane
[0084]
[0085] Take 0.87 g of the polyester obtained in Example 2, add 7 ml of tetrahydrofuran, stir and dissolve. After the polyester was completely dissolved, 0.03 g of hexamethylene diisocyanate (equal molar amount to the polyester) was added, and after stirring for 1 minute, several drops of tin 2-ethylhexanoate were added as a catalyst, and stirred for 24 hours. The reaction solution was dropped into methanol, and after stirring, methanol was distilled off.
[0086] IR(v / cm -1 ): 1730 (urethane carbonyl), 1750 (-lactone carbonyl).
[0087] Weight average molecular weight: more than 200,000 (dimethylformamide).
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