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Realizing the reversible transformation of the supramolecular hydrogels is essential for their application as smart materials. The reversible sol‐gel transition of the polypseudorotaxane (PPR) hydrogels is achieved through adding a CO2‐switchable guest molecule into the PPR hydrogel of poly(ethylene glycol) (PEG) and α‐cyclodextrins (α‐CDs). Alternating treatments with CO2 and heating drive such reversible transition due to the competitive complexation as evidenced by 2D NOESY 1H NMR and isothermal titration calorimetry as well as X‐ray diffraction. The present work describes a straightforward way to obtain switchable PPR hydrogels triggered by a compatible stimulus of CO2. These stimuli‐responsive PPR hydrogels have potential applications as biomaterials.

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