Conventional　nanomaterials　are　met　with　the　bottleneck　problem　of　difficult　recycling　and　reuse　when　applied　to　water　treatment.　Carbon　aerogel　with　three-dimensional　structure　can　effectively　solve　the　problem　of　recycling,　however,　the　preparation　of　efficient　and　recyclable　aerogel　catalyst　is　still　an　urgent　technical　problem.　Here,　an　NH2-MIL-88B(Fe)/agarose　carbon　aerogel　(MGA-x)　was　synthesized　at　different　calcination　temperatures　(x　=　100,　150,　200　and　300　°C)　and　their　changes　in　structures　and　photo-electrochemical　properties　were　investigated.　As　a　photo-Fenton　catalyst,　the　aerogel　could　efficiently　activate　H2O2　to　ultrafast　degrade　mitoxantrone　in　water.　Within　2　min,　the　removal　efficiency　of　mitoxantrone　in　the　MGA-200/H2O2/Light　system　was　97.6%,　which　was　85.3　times　greater　than　that　in　the　agarose　aerogel/H2O2/Light　system.　Notably,　the　aerogel　catalyst　could　be　directly　recovered　and　recycled　without　additional　treatments,　and　the　microstructure　and　degradation　performance　were　maintained　even　after　five　cycles,　demonstrating　excellent　sustainability　for　applications　in　practical　aquatic　environment.　The　primary　active　radicals　involved　in　the　photocatalytic　degradation　process　were　•OH,　h+　and　•O2-,　which　were　confirmed　through　free　radical　quenching　experiments　and　electron　paramagnetic　resonance　analysis.　Additionally,　possible　degradation　pathways　for　mitoxantrone　were　proposed　based　on　the　results　of　liquid　chromatography-mass　spectrometry.　This　study　presents　a　photocatalytic　aerogel　with　highly　efficient　degradation　ability　along　with　recycling　and　reuse　capacity,　exhibiting　great　potential　for　application　in　the　remediation　of　water　pollution.　©　2024　Elsevier　Ltd