The present invention discloses a preparation method of a nanometer iron-copper-carbon micro electrolysis material for organic waste water treatment. The preparation method comprises: mixing acrylic acid and water; adding copper-iron hydrotalcite particles to the acrylic acid solution, wherein per g of the copper-iron hydrotalcite particles is corresponding to 3-5 mmol of the acrylic acid, and the copper-iron hydrotalcite particles are screened through a 20-50 mesh sieve; adding ammonium persulfate, heating, washing with deionized water, drying, grinding, and screening through a 20-40 mesh sieve to obtain powder; heating the obtained powder under a vacuum condition to 600-700 DEG C, and carrying out calcination for 2-4 h; adding 2-4 g of the resulting product into a flask, adding 20 ml of deionized water, introducing N2 to carry out protection, stirring, then adding a KBH4 solution, and carrying out continuous stirring; and carrying out centrifugation separation, and carrying out constant temperature drying for 5-6 h at a temperature of 60-70 DEG C under N2 protection to obtain the nanometer iron-copper-carbon micro electrolysis material for organic waste water treatment, wherein an activated surface area can be increased, pollutants can be absorbed, a nanometer effect of the nano-scale iron-copper-carbon can be provided, and oxidation efficiency can be improved.