In this study, 2-phenyl ethanol (2-PEA) was microencapsulated with natural and semisynthetic carbohydrate polymers as the wall material. The wall material components methylcellulose (MC), alginate sodium (ALG), and carboxymethyl chitosan were optimized according to the results of microscopy images, zeta potential, and 2-PEA content. The combination of MC/ALG/MC was selected as the best wall components. Cobalt chloride (CoCl2) was used as the core material to prepare microcapsules whose color was measured with a colorimeter to intuitively express the water absorption of the microcapsules. The absorbed water mass and b* were related to one variable quadratic equation. The rapid release properties and the natural long-term release properties of 2-PEA microcapsules were measured.