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Method for removing free chlorine from solution after cobalt electrolysis
CN102745793A
China
Worldwide applications
2012
CN
Application CN2012102479172A events
2012-07-17
2012-10-24
Status
Pending
Description
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Technical field
The present invention relates in the metallurgy industry liquid dechlorination process after the cobalt chloride solution electrolysis, specifically a kind of method that removes liquid Free Chlorine after the cobalt electrolysis with the ydrogen peroxide 50 reduction method of purification.
Background technology
Contain higher free chlorine in the liquid after the cobalt electrolysis that obtains after the cobalt chloride solution electrolysis; Can not cause heavy corrosion to follow-up equipment if do not remove; And when carrying out back extraction with cobalt chloride solution, can powder blue extraction agent P507 (its chemistry own ester of 2-ethylhexyl phosphonic acid single 2-ethyl by name) or Cyanex272 (its chemistry by name two (2,4; The 4-tri-methyl-amyl) phospho acid), causes the loss of extraction agent.Adopt at present and add method dechlorinations such as activated carbon, S-WAT reduction method and vacuum dechlorination method.Adopt gac to remove the free chlorine of liquid after the cobalt electrolysis, this dechlorination process possible in theory, but can exist the gac consumption bigger in the actual production process, and gac can only use once, the gac after the use becomes waste residue shortcoming such as need handle.The dechlorination of S-WAT reduction method then can be introduced sodium sulfate salt in cobalt liquid, the 7-8 that chemical dechlorination S-WAT actual amount is the Theoretical Calculation consumption has doubly polluted solution; And the facility investment of vacuum dechlorination is higher, and pH control is strict, the most important thing is vacuum tightness is required height, and its control difficulty is big, and energy consumption is bigger.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned prior art to have defectives such as supplementary product onsumption is big, cost is higher, the control difficulty is big; A kind of method of utilizing the ydrogen peroxide 50 reduction method of purification to remove liquid Free Chlorine after the cobalt electrolysis is provided; It not only can realize effectively separating cobalt chloride solution and free chlorine; Can also realize removing liquid free chlorine after the cobalt electrolysis with ydrogen peroxide 50 reduction; Produce pollution-free tail gas oxygen, to reach the preparation high-purity cobalt, remove after the cobalt electrolysis liquid free chlorine and to generate purpose such as recycle acid.
For this reason; The present invention adopts following technical scheme: a kind of method that removes liquid Free Chlorine after the cobalt electrolysis; Its step is following: will contain after the cobalt electrolysis of free chlorine liquid and transfer solution temperature to 30～50 ℃ through heat-exchanger rig earlier; Get in the gas-liquid separation equipment after the temperature adjustment and carry out chlorine and solution initial gross separation, behind gas-liquid separation 30～100min, add an amount of concentrated hydrochloric acid regulator solution pH value between 1.0～3.0; Then solution behind the adjust pH and ydrogen peroxide 50 are fed in the first step dechlorination groove of a multistage dechlorination device continuously, the volume ratio of ydrogen peroxide 50 and solution is 1:500～1:700; Then with solution other dechlorination grooves in the multistage dechlorination device of flowing through successively; In other dechlorination grooves, feed ydrogen peroxide 50 more continuously and carry out dechlorination; The volume ratio of ydrogen peroxide 50 and solution is 1:200～1:300; Open pump, make the cobalt electrolysis after liquid in multistage dechlorination device, fully circulate, disperse and react, the dechlorination grooves at different levels in the multistage dechlorination device are connected successively.The present invention measures the solution Free Chlorine with the free chlorine determinator; Thereby the reduction of the strong oxidizing property atmosphere after the electrolysis of completion cobalt in the liquid; Neither introduce new impurity and pollutent and produce, the hydrochloric acid of dechlorination reaction generation simultaneously also can be used for the P507 back extraction, realizes the recycle free chlorine; And energy consumption is low, and the dioxygen water content consumption is few.
Operational path of the present invention is: the multistage dechlorination of liquid after the cobalt electrolysis → ydrogen peroxide 50 one-level dechlorination → ydrogen peroxide 50 → dechlorination back liquid → P507 back extraction.
The principle that the present invention adopts ydrogen peroxide 50 to remove free chlorine is:
A. under sour environment, ydrogen peroxide 50 can be reduced into HCl with the free chlorine of liquid after the cobalt electrolysis, thereby can reach the effect that removes free chlorine, and its reaction formula is following:
H
2O
2+Cl
2==2HCl+O
2 （1）
H
2O+Cl
2==HCl+?HClO （2）
H
2O
2+2HClO==2HCl+O
2+H
2O （3）
Utilize the both sexes of ydrogen peroxide 50; Chlorine and hypochlorous acid are reduced into oxygen and hydrochloric acid respectively; The liquid Free Chlorine removes after making the cobalt electrolysis, thereby the strong oxidizing property atmosphere of free chlorine is removed, can reduce by free chlorine cause to the corrosion of follow-up equipment and the oxidational losses of extraction agent;
B. the liquid Free Chlorine removes the oxygen entering exhaust treatment system of generation, entering atmosphere, not atmosphere pollution after handling after utilizing ydrogen peroxide 50 to the cobalt electrolysis; The water and steam that generates gets into system, does not introduce impurity, and simultaneously, the hydrochloric acid of generation can be used to regulator solution pH, helps reducing the hydrochloric acid content that the P507 back extraction adds.
As further technical scheme, confirm the progression of multistage dechlorination device according to the volume of the free chlorine content in the liquid after the cobalt electrolysis, solution flow, dechlorination groove.
As further technical scheme, in gas-liquid separation equipment, the gas-liquid separation time is preferably 20～40min.
As further technical scheme, described dechlorination groove top is provided with and is used for liquid and ydrogen peroxide 50 blended line mixer after the cobalt electrolysis, and there is the sparging unit that is communicated with it below of this line mixer, and described sparging unit is installed on the dechlorination groove.Line mixer makes after the cobalt electrolysis liquid and ydrogen peroxide 50 cross thorough mixing, gets into after the mixing in the corresponding dechlorination groove again; Sparging unit guarantees that ydrogen peroxide 50 is dispersed in after the cobalt electrolysis in the liquid.
As further technical scheme, described dechlorination groove is provided with barometric control unit, and it is used for balance dechlorination groove pressure.
Compare with existing method, the present invention not only can obviously reduce the free chlorine in the liquid after the cobalt electrolysis, reduces the oxidizing atmosphere in the liquid after the cobalt electrolysis, reaches the purpose that removes free chlorine, obtains high purity low oxidative cobalt chloride solution, and has the following advantages:
1) speed of response is fast, but accomplishes dechlorination within a short period of time;
2) inclusion-free generates, and the oxygen of generation can be overflowed, contamination-free;
3) running cost is low, and liquid only need consume ydrogen peroxide 50 3L-6L after every cube of cobalt electrolysis;
4) hydrochloric acid of reaction generation, the hydrochloric acid content that adds in the time of can reducing the solution back extraction.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Fig. 2 is the used equipment flowsheet of technology of the present invention.
Among Fig. 2,1-cobalt electrolyzer, 2-heat-exchanger rig, 3-ydrogen peroxide 50 Preparation tank, 4-gas-liquid separation equipment; 5-first step dechlorination groove, 6-first step dechlorination pump, 7-second stage dechlorination groove, 8-second stage dechlorination pump; 9-contains liquid after the cobalt electrolysis of free chlorine, 10-water coolant water inlet (from cooling tower), and 11-advances the tail gas absorption system, 12-dechlorination post chlorization cobalt liquor; 13-returns cooling tower, A-air, B-sparging unit, C-line mixer.
Embodiment
Below in conjunction with Figure of description the present invention is further described.
The employing ydrogen peroxide 50 as shown in Figure 2 reduction method of purification removes the equipment of liquid free chlorine after the cobalt electrolysis; Whole process is mainly carried out in two-stage dechlorination device; Two-stage dechlorination device by first step dechlorination groove 5, second stage dechlorination groove 7, corresponding dechlorination pump and the pipeline that is used between the equipment connecting usefulness form, first step dechlorination groove is connected with second stage dechlorination groove.Liquid at first carries out temperature adjustment through heat-exchanger rig to solution after the cobalt electrolysis, makes the solution of squeezing in the dechlorination groove reach the required temperature of dechlorination.The first step dechlorination groove top of two-stage dechlorination device adds line mixer and sparging unit.Second stage dechlorination groove top adds line mixer, sparging unit and barometric control unit, and barometric control unit is used for balance dechlorination groove pressure.Second stage dechlorination groove barometric control unit valve does not allow chlorine to overflow for closing under the normal circumstances, and when two-stage dechlorination groove communication loop, the barometric control unit valve is an open mode.After two-stage dechlorination groove is realized running balance, can realize removing of free chlorine behind the reaction certain hour, finally send extracting system to carry out the P507 back extraction.
The method that removes the free chlorine in the liquid after the cobalt electrolysis with the ydrogen peroxide 50 reduction method of purification as shown in Figure 1; Its step is following: liquid passes through heat-exchanger rig earlier after will containing the cobalt electrolysis of free chlorine; Regulator solution temperature to 30～50 ℃; Get in the gas-liquid separation equipment after the temperature adjustment and carry out chlorine and solution initial gross separation, behind gas-liquid separation 30～100min, add an amount of concentrated hydrochloric acid regulator solution pH value between 1.0～3.0; Then solution behind the adjust pH and ydrogen peroxide 50 are mixed in the first step dechlorination groove of the continuous feeding in back two-stage dechlorination device, the volume ratio of ydrogen peroxide 50 and solution is 1:500～1:700; Switch first step dechlorination pump line road outlet valve then; Solution is squeezed into the dechlorination groove to the second stage; Feed ydrogen peroxide 50 more continuously and carry out dechlorination, solution and ydrogen peroxide 50 feed in the second stage dechlorination groove after mixing again, and the volume ratio of ydrogen peroxide 50 and solution is 1:200～1:300; Open second stage dechlorination pump; Liquid fully circulates, disperses, reacts in first step dechlorination groove and second stage dechlorination groove after making the cobalt electrolysis; With the free chlorine determinator solution Free Chlorine is measured at last, thus the reduction of the strong oxidizing property atmosphere in the liquid after the electrolysis of completion cobalt.
Liquid after the cobalt electrolysis of aforesaid method, free chloro concentration are 500 ~ 600 mg/L, and after with ydrogen peroxide 50 solution being carried out reduction dechlorination, the Co concentration in the solution remains unchanged basically, and the decreasing ratio of free chlorine is more than 90%.
Some processing condition wherein require: (1) ydrogen peroxide 50 massfraction is 15 ~ 20%.(2) the dechlorination reaction time is 30 ~ 80min.
The above only is preferred embodiment of the present invention.Every foundation technical spirit of the present invention all falls in protection scope of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (5)
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Claims (5)
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1. method that removes liquid Free Chlorine after the cobalt electrolysis; Its step is following: will contain after the cobalt electrolysis of free chlorine liquid and transfer solution temperature to 30～50 ℃ through heat-exchanger rig earlier; Get in the gas-liquid separation equipment after the temperature adjustment and carry out chlorine and solution initial gross separation; Behind gas-liquid separation 30～100min, add an amount of concentrated hydrochloric acid regulator solution pH value between 1.0～3.0; Then solution behind the adjust pH and ydrogen peroxide 50 are fed in the first step dechlorination groove of a multistage dechlorination device continuously, the volume ratio of ydrogen peroxide 50 and solution is 1:500～1:700; Then with solution other dechlorination grooves in the multistage dechlorination device of flowing through successively; In other dechlorination grooves, feed ydrogen peroxide 50 more continuously and carry out dechlorination; The volume ratio of ydrogen peroxide 50 and solution is 1:200～1:300; Open pump, make the cobalt electrolysis after liquid in multistage dechlorination device, fully circulate, disperse and react, the dechlorination grooves at different levels in the multistage dechlorination device are connected successively.
2. the method that removes liquid Free Chlorine after the cobalt electrolysis according to claim 1 is characterized in that, confirms the progression of multistage dechlorination device according to the volume of the free chlorine content in the liquid after the cobalt electrolysis, solution flow, dechlorination groove.
3. the method that removes liquid Free Chlorine after the cobalt electrolysis according to claim 1 and 2 is characterized in that in gas-liquid separation equipment, the gas-liquid separation time is 20～40min.
4. the method that removes liquid Free Chlorine after the cobalt electrolysis according to claim 1 and 2; It is characterized in that; Described dechlorination groove top is provided with and is used for liquid and ydrogen peroxide 50 blended line mixer after the cobalt electrolysis; There is the sparging unit that is communicated with it below of this line mixer, and described sparging unit is installed on the dechlorination groove.
5. the method that removes liquid Free Chlorine after the cobalt electrolysis according to claim 1 and 2 is characterized in that described dechlorination groove is provided with barometric control unit.