Chain extender, and preparation method and application of chain extender
A technology of chain extender and catalyst, applied in the field of chain extender and its preparation, can solve the problems of high cost of chain extender, complex synthesis method, low yield and the like, and achieve high yield, simple synthesis method and simple synthesis. Effect
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[0023] The present invention also provides a kind of preparation method of chain extender, wherein, this method can also comprise the following steps:
[0024] (1) dissolving the caprolactam derivative shown in formula (I) and / or its salt and the catalyst in an anhydrous solvent,
[0025]
[0026] (2) adding diacyl halide or acid anhydride to the solution obtained in step (1) to carry out the synthesis reaction;
[0027] (3) Filtering, concentrating, extracting and drying the reaction liquid after the synthesis reaction in step (2).
[0028] According to the present invention, in step (1), the salt of the caprolactam derivative represented by the formula (I) is not specifically limited, and may be any one or more of the organic acid salts of the caprolactam derivative represented by the formula (I) species; preferably, the salt of the caprolactam derivative shown in formula (I) can be one or more of hydrochloride, carbonate and sulfate; more preferably, the caprolactam der...
Embodiment 1
[0050] In a 500ml three-neck flask, dissolve 12.7 grams (0.1mol) of caprolactam derivatives represented by formula (I) in 150 grams of acetone, add 10.1 grams of triethylamine, and lower the solution to 0°C, and pass high-purity nitrogen 30 minutes.
[0051] Under the condition of nitrogen protection, 6.3 g (0.05 mol) of oxalyl chloride (oxalyl chloride) was added to the mixed solution obtained above, and then the temperature was slowly raised to 25° C., and the reaction was continued for 6 hours to terminate the reaction.
[0052] The insoluble matter in the reaction liquid of the above synthesis reaction was filtered and concentrated, and the mass of the concentrated reaction liquid was 10% of that before concentration, 50ml of chloroform was added, dissolved, and extracted three times with 100ml of deionized water to remove unreacted matter. The organic phase was dried and the solvent was removed to obtain 15.0 g of a white solid product with a yield of 96%.
Embodiment 2
[0054] In a 500ml three-neck flask, dissolve 16.4 grams of caprolactam derivative hydrochloride shown in formula (I) in 200 grams of chloroform, add 20 grams of N,N-dimethylaminopyridine, and reduce the solution to 4 °C, flow high-purity nitrogen for 20 minutes.
[0055] Under the condition of nitrogen protection, 9.5 g (0.48 mol) of terephthaloyl chloride was added to the mixed solution obtained above, and then the temperature was slowly raised to 27 degrees Celsius, and the reaction was continued for 5 hours to terminate the reaction.
[0056] Filter and concentrate the insoluble matter in the reaction liquid of the above synthesis reaction, and make the mass of the concentrated reaction liquid 10% of that before concentration, add 50ml of chloroform, dissolve, extract three times with 100ml10% sodium hydroxide aqueous solution, and then use 100ml deionized Water extracted three times to remove unreacted materials. The organic phase was dried and the solvent was removed to ...
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