A kind of preparation method of poly(ethylene glycol monomethyl ether-polylactic acid block copolymer)
A technology of polyethylene glycol monomethyl ether and block copolymer, which can be applied to medical preparations without active ingredients, medical preparations containing active ingredients, and pharmaceutical formulas, etc. Impurities and other problems, to achieve the effect of wide reduction of molecular weight distribution, improved moisture absorption, and good fluidity
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Embodiment 1
[0036] Reaction stage: put 192g of polyethylene glycol monomethyl ether into the reactor, replace it with nitrogen, and dry it in vacuum at 120°C for 3 hours, then put 1.2g of the catalyst stannous octoate into the reactor, replace it with nitrogen, and continue vacuum drying for 1 hour; put in lactide 208g, evacuate for 1.5min, airtight, after the lactide is completely melted, then evacuate for 5min, heat up to 140°C, react for 12h, after the reaction is completed, cool down to obtain a light yellow clear liquid;
[0037] The first crystallization: dilute with 400ml of dichloromethane, slowly add to 8L of ether, stir and crystallize for 1h, and filter with suction;
[0038] The second crystallization: dilute the filter cake with 1600ml of dichloromethane, wash with 800ml of purified water, dry with 200g of anhydrous magnesium sulfate, filter with suction, remove the dichloromethane by rotary evaporation of the mother liquor, add 200ml of dichloromethane to dissolve, add to 6L ...
Embodiment 2
[0043] Reaction stage: put 192g of polyethylene glycol monomethyl ether into the reactor, replace it with nitrogen, and dry it in vacuum at 120°C for 3 hours, then put 1.2g of the catalyst stannous octoate into the reactor, replace it with nitrogen, and continue vacuum drying for 1 hour; put in lactide 208g, evacuate for 1.5min, airtight, after the lactide is completely melted, then evacuate for 5min, heat up to 140°C, react for 12h, after the reaction is completed, cool down to obtain a light yellow clear liquid;
[0044] The first crystallization: add 3L of dichloromethane to the reaction solution for dilution, wash with 1.5L of purified water, dry with 300g of anhydrous magnesium sulfate, filter with suction, remove the dichloromethane by rotary evaporation of the mother liquor, add 200ml of dichloromethane to dissolve, add to In 6L of ether at 0±5°C, stir and crystallize for 1h, and filter with suction;
[0045] The second crystallization: add 200ml of dichloromethane to t...
Embodiment 3
[0049] Reaction stage: put 192g of polyethylene glycol monomethyl ether into the reactor, replace it with nitrogen, and dry it in vacuum at 120°C for 3 hours, then put 1.2g of the catalyst stannous octoate into the reactor, replace it with nitrogen, and continue vacuum drying for 1 hour; put in lactide 208g, evacuate for 1.5min, airtight, after the lactide is completely melted, then evacuate for 5min, heat up to 140°C, react for 12h, after the reaction is completed, cool down to obtain a light yellow clear liquid;
[0050] The first crystallization: add 200ml of dichloromethane to dilute, slowly add to 6L 0±5°C ether, stir and crystallize for 1h, and filter with suction; the second crystallization: add 1000ml of dichloromethane to dissolve the filter cake, wash with 500ml of purified water, Dry 200g of anhydrous magnesium sulfate, filter with suction, remove dichloromethane by rotary evaporation of the mother liquor, then add 200ml of dichloromethane to dissolve, add to 6L of e...
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