A reactive distillation device with an external circulation system and its application
A technology of reactive distillation and reaction kettle, which is applied in the field of polymer material synthesis equipment and technology, can solve the problems of increased energy consumption, increased system viscosity, time-consuming, etc., and achieve the effect of avoiding interference and improving production efficiency
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Embodiment 1
[0058] In the present embodiment, the mass percent of carbonate contained in the preset rectification cut is 32%, and the product hydroxyl value preset value is 112.2mgKOH / g (molecular weight 1000), calculates the amount of dimethyl carbonate addition accordingly.
[0059] Weigh 15.7kg of 1,5-pentanediol, 17.9kg of 1,6-hexanediol, 31.5kg of dimethyl carbonate, 3.42g of isopropyl titanate, and 20g of pyridine, and add them to the above-mentioned 100L stainless steel reaction kettle. Evacuate and pass nitrogen three times. Under the protection of nitrogen, the temperature was raised to the reaction temperature of 96°C. Start timing since the temperature rise at the top of the tower is observed. First, the total reflux is 0.5h, and then the fraction is continuously extracted at a reflux ratio of 1.7:1. The temperature fluctuation at the top of the rectification column is 61.8-62.2°C. During the reaction, methanol: DMC in the fraction The ratio is around 68.0:32.0 (wt%). After a...
Embodiment 2
[0062]In this embodiment, the preset value of the mass percentage of carbonate contained in the rectification fraction is 32%. The default value of the hydroxyl value of the product is 56.1mgKOH / g (molecular weight 2000), and the amount of dimethyl carbonate added is calculated accordingly.
[0063] Weigh 16.3kg of 1,5-pentanediol, 18.4kg of 1,6-hexanediol, and 3.45g of tetrabutyl titanate, and add them to the above-mentioned 100L stainless steel reaction kettle. Vacuumize and pass nitrogen three times to maintain normal pressure. Under the protection of nitrogen, the temperature was raised to a reaction temperature of 145° C., and 35.0 kg (the total amount of carbonate feeds predetermined by stoichiometry) of dimethyl carbonate was slowly added dropwise to the system at a rate of 7 kg / h. Since observing that the tower top temperature rises, at first suspend adding dimethyl carbonate, open the circulation pump low valve, open the circulation pump, flow 20L / h, full reflux 0.5h...
Embodiment 3
[0066] In this embodiment, the preset value of the mass percentage of carbonate contained in the rectification fraction is 32%. The default value of the hydroxyl value of the product is 112.2 mgKOH / g (molecular weight 1000), and the caprolactone content is 50%, based on which the amount of dimethyl carbonate added is calculated.
[0067] Weigh 27.1 kg of 1,6-hexanediol, 31.4 kg of caprolactone, and 5.65 g of tetrabutyl titanate, and add them to the above-mentioned 100 L stainless steel reaction kettle. Vacuumize and pass nitrogen three times to maintain normal pressure. Under nitrogen protection, the temperature was raised to a reaction temperature of 145° C., and 20.0 kg (the total amount of carbonate feeds predetermined by stoichiometry) of dimethyl carbonate was slowly added dropwise to the system at a rate of 4 kg / h. From the observation that the tower top temperature rises, first suspend the addition of dimethyl carbonate, full reflux for 0.5h, then continue to add dimet...
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Abstract
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