Method for recovering toluenediamine from waste slag emitted from production of toluene diisocyanate
A technology of toluene diisocyanate and toluene diamine, which is applied in the field of toluene diisocyanate industrial residue recycling and environmental protection, can solve the problems of high production cost, low yield, long time consumption and the like, and achieves low production cost and product yield. High, time-consuming effect
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Embodiment 1
[0034] Weigh 12g of crushed TDI residue and 80g of triethylenetetramine and add them to a 200mL reactor equipped with a reflux condenser, stirrer and thermometer and heat. When the temperature rises to 100°C, add 8g of TDI residue and heat To 292 ° C until the system boils, keep reflux for 30 minutes. Afterwards, 20 g of 50% NaOH aqueous solution was added at a flow rate of 20 mL / h. During the dropwise addition, the system temperature gradually dropped to 160° C., and the reaction was continued for 1 h after the dropwise addition was completed. Stop heating afterwards, cool down and discharge. The obtained product is filtered to remove the residue to obtain a dark brown filtrate, and the obtained filtrate is salted out with a saturated sodium chloride solution. The filtrate was extracted, and the amount of dichloromethane was 2 times by weight of the filtrate after salting out, and extracted 4 times in 4 equal portions.
[0035] Finally, the solvent (dichloromethane) was re...
Embodiment 2
[0037]Weigh 12g of the crushed TDI distillation residue and 40g of triethylenetetramine and add it to a reactor equipped with a reflux condenser, agitator and a thermometer and heat it. When the temperature rises to 100°C, add 8g of the TDI residue and heat it to 292°C until the system boils, keep reflux for 30min. Afterwards, 20 g of 50% NaOH aqueous solution was added at a flow rate of 20 mL / h. During the dropwise addition, the system temperature gradually dropped to 144°C. All the other steps are the same as in Example 1. The TDA yield was 65.1% of the added TDI residue.
Embodiment 3
[0039] Weigh 12g of the crushed TDI distillation residue and 80g of triethylenetetramine and add them to a reactor equipped with a reflux condenser, a stirrer and a thermometer and heat them. When the temperature rises to 100°C, add 8g of TDI residues and heat to 292°C until the system boils, keep reflux for 40min. All the other steps are the same as in Example 1. The TDA yield was 69.3% of the added TDI residue.
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