The invention discloses a novel photodegradation surfactant and preparation thereof, belonging to the field of surfactants. The novel photodegradation surfactant is synthesized through the following three reaction steps: (1) with diethylene triamine pentacetic acid as a raw material and acetic anhydride as a dehydrating agent, carrying out dehydration under the catalysis of pyridine so as to produce diethylene triamine pentacetic dianhydride; (2) with an o-nitrobenzyl bromide derivative as a raw material, carrying out acylating chlorination on the derivative and then reacting an acylating chlorination product with secondary amine so as to obtain an intermediate, i.e., para-position double-long-chain carbomite o-nitrobenzyl bromide; and (3) subjecting double-long-chain benzyl bromide in the intermediate and middle carboxyl groups of diethylene triamine pentacetic dianhydride to nucleophilic substitution under the catalysis of a catalyst in a solvent so as to obtain surfactant molecules containing o-nitrobenzyl ester light-operated groups. According to the invention, four terminal carboxyl groups are protected by ingeniously utilization of dehydration of diethylene triamine pentacetic acid into anhydride, the middle carboxyl groups are selectively utilized and form ester under the catalysis of organic base DBU, so the o-nitrobenzyl ester photodegradation surfactant is prepared. Compared with traditional methods, the method provided by the invention has the advantages that reaction flow is shortened and efficiency is greatly improved.