Pentanediamine ethanedioate and crystal thereof
A technology of pentamethylenediamine oxalate and oxalic acid, which is applied in the field of monomer crystallization of bio-based materials, which can solve the problems of inconvenient transportation and use, affecting the purity of pentamethylenediamine itself, and unpleasant pungent smell
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Embodiment 1
[0084] Add 10.00 g of pentamethylenediamine into 100 g of ethanol and stir well to form a pentamethylenediamine ethanol solution. Dissolve 8.81g of oxalic acid in 150g of ethanol, drop it into the ethanol solution of pentamethylenediamine at a flow rate of 0.5mL / min at 35°C, crystallize under stirring, and monitor the pH changes in the process, at pH 10.0 Add 0.2g of seed crystals, suspend feeding, and after 2.5 hours of crystal growth, pump the oxalic acid ethanol solution into the crystallization system at a flow rate of 0.2mL / min. Vacuum suction filtration, and wash the filter cake layer with 50-100mL ethanol, and then vacuum blast drying at 70°C for 12 hours to obtain pentamethylenediamine oxalate crystalline powder, which does not contain crystal water, and its powder X-ray diffraction pattern is as follows: Figure 6 As shown, the specific diffraction data are as Figure 11 shown. When the obtained crystalline salt is formulated into an aqueous solution with a mass fra...
Embodiment 2
[0086] Add 10.00 g of pentamethylenediamine into 60 mL of 90% methanol aqueous solution (methanol volume fraction is 90%), and stir well to form an aqueous solution of pentamethylenediamine methanol. Add 8.81g of oxalic acid solid into 250mL of 80% methanol aqueous solution (methanol volume fraction is 90%), form the methanol aqueous solution of oxalic acid, then the two are mixed in 500mL crystallizer, control temperature at 20 ℃, Stir for 56 hours, a white crystal substance appears, put it into the tank, filter it with suction, wash the solid with 60-80mL of 95% ethanol, then dry the solid under vacuum for 8 hours, and keep the temperature at 45-50°C to obtain crystallization of pentamethylenediamine oxalate Powder, containing 3 waters of crystallization, the water content of the powder is 22wt%, the TG analysis spectrum of the product is as follows Figure 7 , Figure 8 Shown: the product starts to melt at 138.58°C, loses water of crystallization at 159.12°C, loses two wat...
Embodiment 3
[0089] Dissolve 26.00 g of pentamethylenediamine in 300 mL of absolute ethanol to form a uniform pentamethylenediamine ethanol solution. Dissolve 20.10 g of oxalic acid in 450 g of 90% methanol-water binary solvent by volume fraction to form a uniform oxalic acid methanol aqueous solution, and then transfer it into a 1000 mL crystallizer. At 45°C, drop into the pentamethylenediamine ethanol solution at a flow rate of 0.8mL / min, carry out crystallization under stirring, and monitor the pH change during the process. After 1.5 hours of crystallization, drop methanol solution of oxalic acid into the crystallization system at a flow rate of 0.5mL / min. Wash with 100-150mL of acetone, and then vacuum-dry at 50°C for 24 hours to obtain pentamethylenediamine oxalate crystalline powder, which contains 2 crystal waters, and the water content of the powder is 15.5wt%. The powder X-ray diffraction pattern is as follows: Figure 5 As shown, the specific diffraction data are as Figure 10 ...
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