There are three important parts in the present thesis. In first part, it studies the way about fully collecting value metallic ions, such as Ni2+, Co2+, Mn2+ etc. from acid washing waste solution and making the waste water reach the permit state discharging standard. In second part, it develops how separating Ni2+ from Co2+, Mn2+ in relative solution. In third part, it pays a great attention to research of fitting electrolysis process parameters in which make nickel power from the solution, and explores the methods attaining cobalt power and manganese compound.Difficulty in the course of taking the way at the first part into consideration exists in bigger discharge, lower value metallic ion concentrations and stronger acidity in the acid washing waste solution. The present thesis compares the way separating by precipitation with by ion exchange, and believe that it is very difficult to retrieve purer value products from precipitation in the former way while the latter way has advantages as follows: high collective rate of value metallic ions, satisfactory results disposing of the waste water and relative easy in the way attaining purer products though the former is simpler than the latter. So the thesis puts emphasis on the way of the latter and researches the law of ion exchange, as result of finding out optimum parameters of ion exchange as well as better reprocessing way of ion exchange resin.In view of the difficult point in hydrometallurgy-separation of Ni2+ and Co2+, on the basis of analyzing and knowing that the way by chemical precipitation has certain difficulty in this case, the thesisadvances the way separating Ni2+ from Co2+ and Mn2+ in relative solution by means of cationic-exchange resin of high-selectivity for nickel ion, and performs experimental research as well as getting better findings.After above process, deep-going experimental research works are put on making nickel power by electrolysis from electrolyte composing of resin reprocessing solution. Findings are that it is necessary to maintain pH value of the solution at 4-5, control current density ic at 4 or so, span of plate at 25mm and initial concentration of nickel ion at 25-30 without stir, in order to attain finer nickel power and higher electrolytic efficiency. In addition to it, the thesis also discusses to get purer cobalt power and manganese sulfate separately by means of reduce under high temperature or method of precipitation at first, then dissolve, evaporate and crystallization after separation of Co2+ and Mn2+ by chemical precipitation.Not only does this thesis perform the above experimental researches, but also develop mechanisms of ion exchange and electrodepositing metallic power, emphatically analyses phenomena in the experiments and reaches correspond conclusions.