Process for producing high quality ionomers
View Patent ↗A reactive extrusion process for producing an ionomer is disclosed. The process comprising adding a polymer containing a carboxyl functionality to an extruder, then homogenously melting the polymer in a melting zone of the extruder. A first melt seal zone of the extruder is formed to separate the melting zone from an injection zone where an aqueous solution of metallic ions are added to the molten polymer. The first melt seal zone is formed by increasing the pressure in the melt seal zone to a pressure which is higher than the vapor pressure of the water at any point in the injection zone and the reaction zone. The aqueous solution of metallic ions is then mixed with the polymer containing the carboxyl functionality in a reaction zone of the extruder under conditions such that the metallic ions are substantially reacted with the carboxyl functionality. A pressure build-up zone is formed in the extruder, wherein the pressure build-up zone is located no earlier than at the end of the reaction zone wherein the pressure build-up zone is formed by increasing the pressure to a level such that the aqueous solution of metallic ions remains in the liquid phase for a time sufficient to allow for the desired reaction between the metallic ions and the carboxyl functionality of the polymer.
1. A reactive extrusion process for producing an ionomer comprising the steps of:
a. adding a polymer containing a carboxyl functionality to an extruder;
b. homogenously melting the polymer in a melting zone of the extruder;
c. forming a first melt seal zone of the extruder;
d. adding an aqueous solution of metallic ions to the molten polymer in an injection zone of the extruder, wherein the injection zone is located after the first melt seal zone of the extruder;
e. mixing the aqueous solution of metallic ions with the polymer containing the carboxyl functionality in a reaction zone of the extruder under conditions such that the metallic ions are substantially reacted with the carboxyl functionality;
f. forming a pressure build-up zone in the extruder, wherein the pressure build-up zone is located no earlier than at the end of the reaction zone;
wherein the first melt seal zone is formed by increasing the pressure in the melt seal zone to a pressure which is higher than the vapor pressure of the water at any point in the injection zone and the reaction zone; and wherein the pressure build-up zone is formed by increasing the pressure to a level such that the aqueous solution of metallic ions remains in the liquid phase for a time sufficient to allow for the desired reaction between the metallic ions and the carboxyl functionality of the polymer.
2. The process of claim 1 further comprising:
g. removing at least a portion of the water in one or more devolatilization zones of the extruder, wherein the devolatilization zone is located after the pressure build-up zone.
3. The process of claim cm 1 wherein the pressure in the first seal zone is developed using non-pumping elements or reverse pumping elements.
4. The process of claim 1 wherein the aqueous metallic solution is heated thereby increasing the solubility of the ionic species.
5. The process of claim 1 wherein a volatile co-solvent is added.
6. The process of claim 1 wherein the resin is an ethylene—ester copolymer and wherein a portion of the ester functionality is convened into a carboxylic acid functionality prior to entering the first melt seal.
7. The process of claim 1 wherein there are one or more additional reaction zones in the extruder profile.
8. The process of Claim 1 wherein the pressure build-up zone is at a pressure which is higher than the vapor pressure of the water at any point in the injection zone and the reaction zone.
9. The process of claim 1 wherein the metallic ions are selected from the group consisting of the mono-, di-, and trivalent ions of metals in Groups I, II, and III of the periodic table of Elements and combinations thereof.
10. The process of claim 9 wherein the metallic ion is an alkali metal.
11. The process of claim 10 wherein the metallic ion is lithium.
12. The process of claim 1 wherein the aqueous solution is in the form of a slurry.