The cleaning production technology for N,N-Dibenzyl hydroxylamine(Referred to as DBHA)was studied. Using benzyl chloride and hydroxylamine hydrochloride as raw material，triethylamine as proton acceptor，DBHA was synthesized in organic solvents after the two-phase reaction. The optimal conditions of synthesis were as following：the molar ratio of hydroxylamine hydrochloride and benzyl chloride was 1：2.3，the first-phase reaction was carried at 50 ℃ for 80 min，while the second-phase reaction at 80 ℃ for 220 min. Under the above optimum conditions，the yield of the product was 81.3％ with the melting point of 123.6～125.3 ℃. The structure of product was confirmed by IR、1H RMR、13C NMR、MS. This technology was adopted to resolve the problem of sewage including salt and organic solvents which were generated by traditional technology. Compared with traditional technology，this new one was suitable for industrial production.