2021/11/1 11:48:02
Dextran sulfate sodium salt production method
Hydrolysis watered Dextran sulfate sodium salt, heated and dissolved into 200g/L (20%), then hydrochloric acid to make 0.3%-0.4%, reflux hydrolysis 3h, slightly colder, neutralized with 100g/L (10%) NaOH liquid to pH6-6.5, hydrolysis solution. Cooling, adding ethanol up to 40%, at 30 degrees C static 24h, take liquid vacuum concentrated to 1/4 of the original volume, add ethanol up to 70%, static 4-6h, dry, collect sediment, micromolecules Dextran sulfate salt. Viscosity (η) - 0.03-0.04, yield of about 60%. Dextran sulfate sodium salt (HCl, NaOH) → s3h, pH6-6.5 s hydrolyzed liquid s/he → micromolecules Dextran sulfate salt esterification by micromolecules Dextran sulfate sodium sodium (m): v): chlorosulfonic acid (V) s1:6:1.48 ratio cast. Take the radon (or replace it with methylamine) into the reaction tank, stir under 25 degrees C to drop chlorinated sulfonate, heat to 45-65 degrees C, put into the micromolecules Dextran sulfate salt powder, insulation 2.5-4h, static layering, pour the upper layer of radon, paste esteride. Micromolecules Dextran sulfate sodium salt (chlorpyrifos, chlorosulfonic acid) → (45-65 degrees C, 2.5-4h) paste esteride (Dextran sulfate sodium salt ester) Sulfur trioxide compound salt) neutralized and dried the paste esteride to cool, add the right amount of water at about 30 degrees C, neutralize to pH10-11 with 400g/L (40%) NaOH liquid, and leave to layer, The lower layer liquid is added to the appropriate amount of water and ethanol to make its mass concentration reach 455g/L (45.5%), stirred and washed 30min at 37 oC insulation, left to rest, the lower layer liquid is removed, repeat the above operation washing twice. sodium glyceride solution. Then add the appropriate amount of water, medicinal activated carbon, decolorization at 50 degrees C, pressure filter, filter liquid added the appropriate amount of water and ethanol, so that ethanol up to 47.5%, 37 degrees C insulation stirring 30min, static, sub-layer liquid, and then the lower layer of liquid with ethanol dump dehydration, drying, 50 degrees C dry, sodium glycerides. For Dextran sulfate sodium salt, the total yield is 54%. Paste esterides (water, naOH) → the lower layer liquid (ethanol) → sodium glyceride solution (water, activated carbon) → filter solution (ethanol) → sodium glyceride preparations are made according to the tablet requirements of sodium glycerides intestinal sodium dextran sulfate salt → Dextran sulfate sodium salt tablets.