Preparation of Dextran sulfate sodium salt

Preparation of Dextran sulfate sodium salt

2021/11/9 11:02:09

Preparation of Dextran sulfate sodium salt

(1) Hydrolysis:

Add water to the right-handed sugar, heat and dissolve into 200g/L (20%), then add hydrochloric acid to make 0.3%-0.4%, reflux hydrolysis 3h, slightly cold, with 100g/L (10%) NaOH liquid neutralized 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 right-handed sugar. Viscosity (η) - 0.03-0.04, yield of about 60%.
Right-handed glycerides (HCl, NaOH) → (3h, pH6-6.5) hydrolysates (ethanol) → micromolecules to right-handed glycerides

(2) Esterification:
By micromolecules right-handed glycosine (m): pyridine (V): chlorosulfonic acid (V) - 1:6:1.48 ratio of the feed. Take the radon (or replace with methylamine) into the reaction tank, stir under 25 degrees C to add chlorinated sulfonate, heating to 45-65 degrees C, into the micromolecules right-handed sugar powder, insulation 2.5-4h, static layering, pouring the upper layer of radon, paste esterifier.

Micromolecules right-handed glycerine (chlorpyrifos, chlor-sulfonate) → (45-65 degrees C, 2.5-4h) paste esteride (right-handed glycerides, sulfur trioxide compound salt)

(3) Neutral and dry:
Stir the paste ester to cool, add the right amount of water at around 30 degrees C, neutralize to pH10-11 with 400g/L (40%) NaOH liquid, static layering, lower layering The appropriate amount of water and ethanol to its mass concentration of 455g/L (45.5%), insulation at 37 degrees C stirring washing 30min, static, sub-layer liquid, 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 the right-handed glycosin meter, the total yield was 54%.

Paste esterides (water, NaOH) → the lower layer of liquid (ethanol) → sodium glyceride solution (water, activated carbon) → filter solution (ethanol) → sodium 37 degrees C, 30min

Intestinal soluble icing sheets made of sodium glycerides as required by the tablets

Sodium glycerides → sodium sodium saccharide tablets.