Inorganic-organic hybrid materials, a class of probable candidates for combining two counterparts into one structure could be beneficial for improving or combing the excellent electronic, magnetic, rigidity and thermal stability, and optical feathers of inorganic frameworks with diverse structure, processability, flexibility and good geometric controllability of organic molecules. Anchoring inorganic-organic hybrid materials with cocatalysts is a usually used strategy for enhancing their catalytic performance. However, noble metal cocatalysts always limit their practical application. Herein, we report that noble metal free cocatalyst of Ni2P decorated CdS-diethylenetriamine (CdS-DETA) can effectively overcome this limitation to achieve highly photocatalytic hydrogen production. The rapid microwave solvothermal synthesis of CdS-DETA (MCdS-DETA) process shortens reaction time, saves energy and lead to achieve highly photocatalytic activity due to its low crystallinity. When Ni2P decorated MCdS-DETA, The 0.4%Ni2P/MCdS-DETA exhibited the highest photocatalytic hydrogen evolution activity (6836 mu mmol h(-1)g(-1)), which is 4.14 times, 2.06 times and 1.34 times higher than traditional solvothermal CdS-DETA(TCdS-DETA), MCdS-DETA and Pt cocatalysted MCdS-DETA, respectively. The method reported here can be extended to other inorganic-organic hybrid materials, and develops new strategies for exploring inorganic-organic hybrid-based photocatalysts.