Method for purifying dianhydrides
View Patent ↗A method for purifying dianhydrides is provided. In one aspect, purified oxybisphthalic anhydrides, intermediates useful in the preparation of polyetherimides are provided. In one embodiment, a first solution containing a dianhydride compound, a solvent, and a phase transfer catalyst is contacted with a solid inorganic adsorbent material having a total pore volume of about 0.5 milliliters/gram or greater and a cumulative pore volume distribution of about 20 percent or greater of particles having a pore diameter in a range between about 3 nanometers and about 20 nanometers. The solution containing the dianhydride compound is then separated from the solid inorganic adsorbent material to provide a purified dianhydride compound which is substantially free of the phase transfer catalyst. The purification technique is especially valuable for preparing high purity oxybisphthalic anhydrides, such as 4,4′-oxybisphthalic anhydride (4,4′-ODPA), which are substantially free of residual phase transfer catalyst.
1. A method of purifying a dianhydride, said method comprising the steps of:
a. providing a first solution comprising at least one dianhydride, at least one solvent, and at least one organic phase transfer catalyst; and
b. contacting the first solution with a solid inorganic adsorbent material, said solid inorganic adsorbent material having a total pore volume of about 0.5 milliliters/gram or greater, and a cumulative pore volume distribution of about 20 percent or greater of particles having a pore diameter in a range between about 3 nanometers and about 20 nanometers; to provide a second solution of the dianhydride, which is substantially free of the organic phase transfer catalyst, wherein the solid inorganic adsorbent material is selected from the group consisting of silica, alumina, zeolites, inorganic ion exchange compounds and mixtures thereof.
2. The method of claim 1 , wherein the phase transfer catalyst is selected from the group consisting of hexaalkylguanadinium salts, pyridinium salts, and phosphazenium salts.
3. The method of claim 1 , wherein the phase transfer catalyst is a bisguanadinium salt.
4. The method of claim 1 wherein the adsorbent is a silica-based adsorbent.