A kind of pentamethylenediamine succinate terephthalic acid eutectic salt and preparation method thereof
A technology of pentamethylene diamine succinic acid and terephthalic acid salt, which is applied in the field of pentamethylene diamine succinic acid terephthalic acid co-crystal salt and preparation thereof, and can solve the problem that it is difficult to obtain high-quality crystals and easy to coalesce oil. It has the advantages of convenient storage and transportation, avoiding yellowing of crystals and improving solubility.
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Embodiment 1
[0061] Example 1: 15.00 g of pentamethylenediamine was added to 200 g of 90% aqueous ethanol by mass fraction, and fully stirred to form an aqueous solution of pentamethylenediamine in ethanol. 10.00g of succinic acid solid and 5.00g of terephthalic acid were added to the solution to form a succinic acid-terephthalic acid ethanol aqueous solution, the temperature was raised to 40°C to completely dissolve the solid, and then the three were mixed in In a 500mL crystallizer, keep stirring at 40°C for 2h at a speed of 400-500r / min, then quickly cool down to 10°C, add 0.5g of seed crystals, and keep stirring at the original speed for 48h, a white crystal substance appears, put it into the tank, Suction filtration, wash the solid with 100mL ethanol, and then vacuum dry the solid for 10h, maintaining the temperature at 45-60°C to obtain 5 2 4T eutectic salt crystallization powder, the thermogravimetric analysis spectrum of the product is as follows Figure 5 Shown: The DSC spectrum ...
Embodiment 2
[0075]Example 2: 20.00 g of pentamethylenediamine was added to 100 g of acetone, and fully stirred to form a pentamethylenediamine acetone solution. Dissolve 15.00g of succinic acid and 11.00g of terephthalic acid in 350g of methanol, drop them into the pentamethylenediamine acetone solution at a flow rate of 1mL / min at 25°C, crystallize while stirring, and monitor the process pH changes, when the pH is around 10.3, add 0.15g of seed crystals, suspend feeding, after crystal growth for 1 hour, drop the remaining succinic acid-terephthalic acid methanol solution into the crystallization system at a flow rate of 0.2mL / min, wait until completely After feeding, continue to stir for 2 hours, put it into the tank, carry out solid-liquid separation of crystal slurry by suction filtration, then wash with 80-100mL methanol, and then vacuum blow dry at 55°C for 8 hours to obtain 5 2 4T eutectic salt crystalline powder, its powder X-ray pattern and Figure 4 Basically the same. When it ...
Embodiment 3
[0076] Example 3: 10.00g of succinic acid and 9.00g of pentamethylenediamine were dissolved in 100mL of methanol to generate 54 salt, 15.00g of terephthalic acid and 10.00g of pentamethylenediamine were dissolved in 100mL of methanol to generate 5T salt, and The obtained two crystalline salts were mixed together, then moved to a 250mL crystallizer, and 100mL of 70% methanol aqueous solution (methanol volume fraction accounted for 70%) was added, and methanol-water was used as a solvent to mediate crystal transformation. Stir for 4-10 hours at a temperature of 35°C and a rotation speed of 200-600rpm, put it in a tank for solid-liquid separation, then wash the filter cake with 200mL of absolute ethanol, and vacuum-dry it at 35-45°C for 8 hours to obtain 5 2 4T eutectic salt crystalline powder, its powder X-ray pattern and Figure 4 Basically the same. When it is prepared as an aqueous solution with a mass fraction of 5%, the pH value of the system is 6.0. The powder has good ...
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