Process for preparing of aromatic oligomers
View Patent ↗This invention relates to a process for preparing high-purity aromatic oligomers by effectively separating an organic layer containing aromatic oligomers or the reaction products of a polycyclic aromatic compound with formaldehyde from an aqueous layer containing an acid catalyst in a simplified manner, hitherto regarded difficult to accomplish, and obtaining high-purity aromatic oligomers from the organic layer containing a reduced amount of impurities. In separating the aqueous layer containing the acid catalyst and the organic layer containing the oligomers from the reaction mixture formed by the condensation of a polycyclic aromatic compound and formaldehyde, the emulsion phase is broken by adding a nonionic or cationic surfactant in an effective amount and an alkali in an amount sufficient to neutralize 1–70% of the acid in the acid catalyst, the organic and aqueous layers are separated and the aromatic oligomers are recovered from the organic layer.
1. A process for preparing aromatic oligomers comprising
reacting an aromatic compound with formaldehyde in the presence of an acid catalyst to obtain a reaction mixture,
adding a surfactant, and a water-soluble alkali in an amount to neutralize 1–70% of the acid catalyst in the reaction mixture to improve the separability of the organic and aqueous layer in the reaction mixture,
transferring the acid catalyst to the aqueous layer, and followed by
separating the aqueous layer from the organic layer to remove the acid catalyst.
2. A process for preparing aromatic oligomers as described in claim 1 wherein the water-soluble alkali is sodium hydroxide.
3. A process for preparing aromatic oligomers as described in claim 1 wherein the aromatic compound is at least one selected from the group consisting of xylene, naphthalene, methylnaphthalene, dimethylnaphthalene, biphenyl, anthracene, phenanthrene and pyrene.
4. A process for preparing aromatic oligomers as described in claim 1 wherein the surfactant is a nonionic surfactant.
5. A process for preparing aromatic oligomers as described in any one of claims 1 to 4 , which process further comprises
dispersing an adsorbent in the organic layer separated from the aqueous layer, and
filtering the dispersion of the organic layer to remove minute amounts of acids, water and metals remaining in the organic layer.
6. A process for preparing aromatic oligomers as described in claim 2 wherein the aromatic compound is at least one selected from the group consisting of xylene, naphthalene, methylnaphthalene, dimethylnaphthalene, biphenyl, anthracene, phenanthrene and pyrene.
7. A process for preparing aromatic oligomers as described in claim 2 wherein the surfactant is a nonionic surfactant.
8. A process for preparing aromatic oligomers as described in any one of claims 6 or 7 , which process further comprises
dispersing an adsorbent in the organic layer separated from the aqueous layer, and
filtering the dispersion of the organic layer to remove minute amounts of acids, water and metals remaining in the organic layer.
9. A process for preparing aromatic oligomers as described in claim 5 wherein the adsorbent is calcium carbonate or calcium hydroxide.
10. A process for preparing aromatic oligomers as described in claim 5 wherein the metal is sodium.
11. A process for preparing aromatic oligomers as described in claim 8 wherein the adsorbent is calcium carbonate or calcium hydroxide.
12. A process for preparing aromatic oligomers as described in claim 8 wherein the metal is sodium.
13. A process for preparing aromatic oligomers as described in claim 1 wherein the alkali is added in an amount to neutralize 5–50% of the acid catalyst in the reaction mixture.