The synthesis, electronic spectral and photophysical properties of a new bithiophene derivative, (2,2′-bithiophene)-3,5,5′-trisulfonic acid, a2-SO 3H, were investigated in organic or aqueous solution, in neat oil form, and in the solid state by cointercalation with different amounts of the surfactant 1-heptanesulfonate (HS) into a layered double hydroxide (LDH). In solution the fluorescence quantum yield (fF) of a2-SO 3H increases by one order of magnitude when compared to the unsubstituted bithiophene (a2) counterpart. However, the most dramatic change is obtained when a2-SO 3H is incorporated with HS into a Zn,Al-LDH, where values of fF up to 58% are obtained in comparison with values of 4% for neat a2-SO 3H (as an oil) and 2% for an LDH containing only a2-SO 3H. In the solid state (LDH), in addition to the monomeric form of a2-SO 3H, H-and other types of aggregates are present, which are found to be dependent on the percentage HS content. Time-resolved fluorescence studies further rationalize this behaviour with single and double exponential decays mirroring the contributions of monomers and aggregates. The study validates a strategy of increasing fluorescence in the solid state by introduction of electrodonating groups and isolation of the a2-SO 3H units within the LDH structure with an appropriate surfactant (HS).