A kind of rifampicin crystal and preparation method thereof
A rifampicin and crystal technology, applied in the field of chemical engineering industrial crystallization, can solve the problems of small particle size, low bulk density, unable to meet the needs of users for high bulk density of medicine, etc., and achieves large crystal size, uniform distribution, and easy drying. Effect
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Embodiment 1
[0031] Take 198g of crude product of crystal form I rifampicin with a purity of 90%, take 1000mL of acetone, and prepare a rifampicin solution; stir and heat up to 55°C to dissolve the rifampicin solid, then add 100ml of water; with a cooling rate of 8°C / h When the temperature is lowered to 45.7°C, the crystals are precipitated, and then the temperature is lowered to 5°C at a cooling rate of 2°C / h, and the crystal is grown for 30 minutes; the crystal slurry is filtered and washed, and the filter cake is dried at 30°C and vacuum degree of 0.08MPa for 2 hours to obtain new The crystalline form of rifampicin product was 144.5g, and the yield was 73%.
[0032] The powder X-ray diffraction pattern of the product is as image 3 As shown, there are characteristic peaks at diffraction angles (2θ) of 5.81, 7.02, 9.09, 12.23, 14.02, 15.48, 16.46, 17.61, 19.62, 20.13, 22.38 and 24.31 degrees. IR Figure 4 Shown at 768, 892, 971, 1057, 1156, 1233, 1371, 1431, 1646, 1716, 2938, 3428, 360...
Embodiment 2
[0034] Take 100g of crude product of crystal form I rifampicin with a purity of 92%, take 1000mL of acetone, and prepare a rifampicin solution; stir and heat up to 53°C to dissolve the rifampicin solid, then add 150ml of water; When the temperature is lowered to 43°C, the crystals are precipitated, and then the temperature is lowered to 5°C at a cooling rate of 1°C / h, and the crystal is grown for 30 minutes; the crystal slurry is filtered and washed, and the filter cake is dried at 40°C and a vacuum of 0.07MPa for 1.5h. 78.8 g of the new crystal form rifampicin was obtained, with a yield of 79%.
[0035] As shown in the powder X-ray diffraction pattern of the product, there are characteristic peaks at diffraction angles (2θ) of 5.80, 7.12, 9.11, 12.18, 14.13, 15.48, 16.31, 17.52, 19.58, 20.02, 22.31 and 24.22 degrees. Infrared spectra at 767, 894, 971, 1058, 1157, 1236, 1370, 1432, 1646, 1719, 2936, 3426, 3607, 3722, 3755, 3817 and 3838cm -1 There are characteristic absorptio...
Embodiment 3
[0037] Get 200g of crude product of crystal form I rifampicin with a purity of 91%, take 1000ml of acetone, and prepare a rifampicin solution; stir and heat up to 57°C to dissolve the rifampicin solid, then add 200ml of water; Crystals precipitated when the temperature was lowered to 45.2°C, and then cooled to 5°C at a rate of 6°C / h, and the crystals were grown for 30 minutes; the crystal slurry was filtered and washed, and the filter cake was dried at 50°C and a vacuum of 0.1MPa for 0.5h to obtain The new crystal form rifampicin product is 136g, and the yield is 68%.
[0038] As shown in the powder X-ray diffraction pattern of the product, there are characteristic peaks at diffraction angles (2θ) of 5.81, 7.02, 9.23, 12.09, 14.12, 15.47, 16.53, 17.58, 19.40, 20.01, 22.32 and 24.28 degrees. Infrared spectra at 767, 893, 970, 1057, 1156, 1235, 1370, 1432, 1646, 1717, 2936, 3428, 3604, 3725, 3755, 3818 and 3836cm -1 There are characteristic peaks. The DSC spectrum has an endot...
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