Method for preparing diisocyanate by heat decomposition
A diisocyanate and thermal decomposition technology, which is applied in the field of preparation of aliphatic or alicyclic diisocyanate, can solve the problems of inapplicability to large-scale industrial production, high price of reaction medium, and non-recyclable catalyst, etc., achieving remarkable catalytic effect and simple equipment , good catalytic activity effect
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Embodiment 1
[0039] Weigh 130 mg (0.5 mmol) of ethyl 1,6-hexanedicarbamate and 10.4 mg of zinc powder (200 mesh) into a 5 mL reaction tube. Open the reaction tube, stir it electromagnetically, heat it to 190°C in a sand bath, and keep it warm for 2 hours. Then it was cooled to room temperature, chromatographic analysis was performed after adding 1 mL of dichloromethane and an internal standard substance (dodecane), and the yield of 1,6-hexamethylene diisocyanate was 10%.
Embodiment 2
[0041] Weigh 130 mg (0.5 mmol) of ethyl 1,6-hexanedicarbamate and 10.4 mg of nickel powder (200 mesh) into a 5 mL reaction tube. Open the reaction tube, stir it electromagnetically, heat it to 190°C in a sand bath, and keep it warm for 2 hours. Then it was cooled to room temperature, 1 mL of dichloromethane and an internal standard substance (dodecane) were added and chromatographic analysis was performed, and the yield of 1,6-hexamethylene diisocyanate was 8%.
Embodiment 3
[0043] Weigh 130 mg (0.5 mmol) of ethyl 1,6-hexanedicarbamate, 10.4 mg of nickel powder (200 mesh) and 45 mg of methyl p-toluate, respectively, and add them into a 5 mL reaction tube. Open the reaction tube, stir it electromagnetically, heat it to 190°C in a sand bath, and keep it warm for 1 hour. Then it was cooled to room temperature, 1 mL of dichloromethane and an internal standard substance (dodecane) were added and chromatographic analysis was performed, and the yield of 1,6-hexamethylene diisocyanate was 8%.
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