The layered double hydroxides (LDH), hydrotalcite (HT) was modified through ion-exchange method with two different organic short chain anionic surfactants in the presence and absence of ultrasound (US). Hydroxy ethane sulphonic acid (HESA) modified HT prepared in the presence of US showed increase of peak intensity in XRD analysis. US assisted sulphoacetic acid (SAA) ion-exchanged HT exhibited completely delaminated/degraded amorphous HT structure. This was authenticated by XRD profiles. The presence of anionic surfactants in the LDH structure is evidenced by FTIR spectroscopy.