CN115747497A - Nickel-containing hazardous waste recycling system and method - Google Patents
Nickel-containing hazardous waste recycling system and method Download PDFInfo
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- CN115747497A CN115747497A CN202211467473.3A CN202211467473A CN115747497A CN 115747497 A CN115747497 A CN 115747497A CN 202211467473 A CN202211467473 A CN 202211467473A CN 115747497 A CN115747497 A CN 115747497A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 194
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 96
- 239000002920 hazardous waste Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000004064 recycling Methods 0.000 title claims abstract description 18
- 238000002386 leaching Methods 0.000 claims abstract description 132
- 238000000605 extraction Methods 0.000 claims abstract description 114
- 238000003825 pressing Methods 0.000 claims abstract description 54
- 239000000706 filtrate Substances 0.000 claims abstract description 39
- 239000012535 impurity Substances 0.000 claims abstract description 27
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 24
- 238000002425 crystallisation Methods 0.000 claims description 20
- 230000008025 crystallization Effects 0.000 claims description 20
- 238000001704 evaporation Methods 0.000 claims description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 17
- 238000011085 pressure filtration Methods 0.000 claims description 15
- 230000008020 evaporation Effects 0.000 claims description 13
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 11
- 239000011790 ferrous sulphate Substances 0.000 claims description 11
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 11
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000009713 electroplating Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000010802 sludge Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007747 plating Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 9
- 239000002699 waste material Substances 0.000 abstract description 9
- 150000002815 nickel Chemical class 0.000 abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 5
- 239000011574 phosphorus Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 24
- 239000012071 phase Substances 0.000 description 16
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a nickel-containing hazardous waste recycling system and method, which comprises a primary leaching tank, an impurity-removing extraction tank and a secondary leaching tank, wherein a primary filter press, a phosphorus removal tank and a secondary filter press are sequentially arranged between the primary leaching tank and the impurity-removing extraction tank, liquid leached by the primary leaching tank enters the phosphorus removal tank after being subjected to filter pressing by the primary filter press, filtrate subjected to filter pressing by the secondary filter press is treated by the impurity-removing extraction tank, raffinate is treated to obtain nickel sulfate, extract phase is reversely extracted, then the extract phase enters the secondary leaching tank, and filtrate subjected to filter pressing by a third filter press enters the primary leaching tank. According to the invention, the nickel-containing waste is sequentially leached, and then subjected to primary and secondary filter pressing, impurity removal extraction is carried out, the extracted extract phase is added into the strip acid for back extraction, and then the filtrate is conveyed to the primary leaching tank for treatment through tertiary filter pressing after secondary leaching, so that the treatment effect of the nickel-containing hazardous waste is improved, the recovery rate is improved, and the purity of the recovered nickel salt is improved.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a nickel-containing hazardous waste recycling system and method.
Background
At present, the electroplating industry in China develops rapidly, nickel plating is used as a main mode for metal surface modification, a large amount of nickel-containing wastewater is generated in the process, according to incomplete statistics, a large amount of electroplating wastewater is discharged every year, pollutants in the electroplating wastewater are difficult to biodegrade and easy to accumulate in organisms, and the pollutants discharged into the environment can cause serious threats to environmental mankind.
At present, the nickel resource recovery of electroplating wastewater is mainly realized by changing nickel-containing wastewater into nickel-containing sludge, recovering on line or recovering by adopting resin adsorption and other modes, the recovery rate is low, the purity of the recovered nickel salt is poor, and the purification cannot be achieved and the due benefit is brought. Therefore, the invention provides a nickel-containing hazardous waste recycling system and method to improve the problems.
Disclosure of Invention
The invention aims to solve the technical problems of low recovery rate, poor purity of recovered nickel salt and incapability of purifying in the prior art, and provides a recycling treatment system and method for nickel-containing hazardous waste.
In order to solve the above problems, the present invention provides a nickel-containing hazardous waste resourceful treatment system, comprising:
the device comprises a primary leaching tank, an impurity removal extraction tank and a secondary leaching tank, wherein the primary leaching tank, the impurity removal extraction tank and the secondary leaching tank are sequentially connected through pipelines;
the primary leaching tank leaches nickel-containing hazardous wastes, a primary filter press, a dephosphorization tank and a secondary filter press are sequentially arranged between the primary leaching tank and the impurity removal extraction tank, and liquid leached by the primary leaching tank is subjected to filter pressing by the primary filter press to obtain primary filter-pressed filtrate; after the primary filter-pressing filtrate enters the dephosphorization tank for dephosphorization, the secondary filter-pressing filtrate enters the secondary filter press for secondary filter pressing to obtain secondary filter-pressing filtrate; the secondary filter pressing filtrate enters the impurity removal extraction box for extraction treatment to obtain raffinate and an extraction phase; the raffinate is nickel sulfate solution, and the extract phase enters the secondary leaching tank after being subjected to back extraction;
and a third pressure filter is arranged between the secondary leaching box and the primary leaching box, leachate treated by the secondary leaching box is subjected to pressure filtration by the third pressure filter, and obtained third pressure filtration filtrate enters the primary leaching box.
Preferably, the primary filter press is further connected with the secondary leaching tank, and filter residues obtained through filter pressing by the primary filter press enter the secondary leaching tank.
Preferably, the filter press further comprises a curing workshop, and filter residues obtained through filter pressing of the secondary filter press and the third filter press enter the curing workshop for treatment.
Preferably, the edulcoration extraction box still pipeline connection has extraction nickel extraction case, deoiling device, evaporating kettle, crystallization kettle and desiccator in proper order, the raffinate gets into the extraction nickel extraction case back extract in the extraction nickel extraction case obtains the strip liquor, the strip liquor gets into deoiling in the deoiling device, later pass through in proper order the evaporating kettle the crystallization of crystallization kettle is followed the desiccator obtains nickel sulfate.
The invention also provides a resource treatment method of nickel-containing hazardous waste, which comprises the nickel-containing hazardous waste resource treatment system, and comprises the following steps:
s1, conveying nickel-containing hazardous waste into the primary leaching tank for leaching, then feeding filtrate subjected to pressure filtration by the primary pressure filter into a dephosphorization tank, and feeding filter residue into the secondary leaching tank;
s2, adding hydrogen peroxide and a ferrous sulfate solution into the dephosphorization tank, and conveying the mixture into the secondary filter press after the reaction is finished;
s3, conveying the filtrate subjected to filter pressing by the secondary filter press to the impurity removal extraction box, and conveying the filter residue subjected to filter pressing by the secondary filter press to the curing workshop for treatment;
s4, conveying raffinate extracted by the impurity removal extraction box to the nickel extraction box;
s5, carrying out oil removal, evaporation, crystallization and drying on the strip liquor obtained by back extraction of the nickel extraction box to obtain nickel sulfate;
s6, adding back extraction acid into the extraction phase extracted by the impurity removal extraction box in the step S4, then conveying to the secondary leaching box, and adding sulfuric acid and water into the secondary leaching box to obtain secondary leaching solution;
and S7, conveying the secondary leachate obtained in the step S6 to the third pressure filter, conveying the filtrate subjected to pressure filtration by the third pressure filter to the primary leaching box again, and conveying the filter residue subjected to pressure filtration by the third pressure filter to a curing workshop for treatment.
Preferably, the pretreatment before leaching of the primary leaching tank in step S1 is:
adjusting the pH value to 3.5-4; adjusting the Ni2+ content to 70-80 g/L; regulating the TP content to be less than or equal to 100mg/L; regulating COD content to be less than 500mg/L.
Preferably, in the step S1, the primary leaching standard is that nickel in the primary leaching residue is 4-6%, and the secondary leaching standard is that nickel in the secondary leaching residue is less than or equal to 0.5%.
Preferably, in step S2, the concentration range of the hydrogen peroxide is 27 to 32%, the concentration of the ferrous sulfate solution is 5 to 20%, and the molar ratio of the added amounts of the hydrogen peroxide and the ferrous sulfate solution is 2.
Preferably, the nickel-containing hazardous waste in step S1 is at least any one of an electroless plating solution, an electroplating solution, and a nickel-containing sludge.
Preferably, the liquid-solid ratio of the extraction phase to the stripping acid in the step S6 is 1;
the concentration of the sulfuric acid is 95-98%.
The nickel-containing hazardous waste recycling system and method provided by the invention have the following beneficial effects:
according to the invention, the nickel-containing waste is sequentially leached, then primary and secondary filter pressing is carried out, impurity removal and extraction are carried out, the extracted extraction phase is added into the back extraction acid for back extraction, then secondary leaching is carried out, and the filtrate is conveyed into the primary leaching tank for treatment through tertiary filter pressing, so that the treatment effect of the nickel-containing hazardous waste is improved, the resources are saved, the recovery rate and the purity of the recovered nickel salt are improved, and the nickel-containing hazardous waste is purified.
Drawings
FIG. 1 is a schematic flow diagram of a nickel-containing hazardous waste recycling system of the present invention;
FIG. 2 is a schematic flow chart of a resource treatment method of nickel-containing hazardous waste.
The reference numerals are represented as:
1. primary leaching tank; 2. a primary filter press; 3. a phosphorus removal tank; 4. a secondary filter press; 5. removing impurities and extracting; 6. extracting a nickel extraction box; 7. evaporating the kettle; 8. a crystallization kettle; 9. a dryer; 10. a secondary leaching tank; 11. a third pressure filter; 12. and (5) curing workshop.
Detailed Description
As shown in fig. 1-2, the present invention provides a nickel-containing hazardous waste recycling system, which comprises:
the device comprises a primary leaching tank 1, an impurity removal extraction tank 5 and a secondary leaching tank 10, wherein the primary leaching tank 1, the impurity removal extraction tank 5 and the secondary leaching tank 10 are sequentially connected through a pipeline;
the nickel-containing hazardous waste is leached by the primary leaching tank 1, a primary filter press 2, a dephosphorization tank 3 and a secondary filter press 4 are sequentially arranged between the primary leaching tank 1 and the impurity removal extraction tank 5, and liquid leached by the primary leaching tank 1 is subjected to filter pressing by the primary filter press 2 to obtain primary filter-pressing filtrate; the primary filter-pressing filtrate enters the dephosphorization tank 3 for dephosphorization and then enters the secondary filter press 4 for secondary filter-pressing to obtain secondary filter-pressing filtrate; the secondary filter-pressing filtrate enters the impurity-removing extraction box 5 for extraction treatment to obtain raffinate and an extraction phase; the raffinate is a nickel sulfate solution, and the extract phase enters the secondary leaching tank 10 after being back-extracted;
a third pressure filter 11 is arranged between the secondary leaching tank 10 and the primary leaching tank 1, leachate treated by the secondary leaching tank 10 is subjected to pressure filtration by the third pressure filter 11, and obtained third pressure filtration filtrate enters the primary leaching tank 1.
As shown in figure 1-2, a nickel-containing hazardous waste recycling system comprises a primary leaching tank 1, an impurity-removing extraction tank 5 and a secondary leaching tank 10, wherein the primary leaching tank 1, the impurity-removing extraction tank 5 and the secondary leaching tank 10 are sequentially connected through a pipeline, the pH value is adjusted to 3.5-4 by immersing nickel-containing hazardous waste into the nickel-containing hazardous waste, a primary filter press 2, a phosphorus removal tank 3 and a secondary filter press 4 are sequentially arranged between the primary leaching tank 1 and the impurity-removing extraction tank 5, liquid leached by the primary leaching tank 1 enters the phosphorus removal tank 3 after being filtered by the primary filter press 2, wherein the primary filter press 2 is a plate-and-frame filter press, filtrate filtered by the secondary filter press 4 is treated by the impurity-removing extraction tank 5, and the secondary filter press 4 is also a plate-and-frame filter press, the method comprises the steps of treating raffinate treated by an impurity-removing extraction box 5 to obtain nickel sulfate, performing back extraction on an extract phase treated by the impurity-removing extraction box 5 by using back extraction acid, then entering a secondary leaching box 10 to perform secondary leaching, further arranging a third-time filter press 11 between the secondary leaching box 10 and the primary leaching box 1, enabling filtrate subjected to filter pressing by the third-time filter press 11 to enter the primary leaching box 1 again to perform secondary leaching, sequentially leaching nickel-containing waste, performing primary and secondary filter pressing, performing impurity-removing extraction, adding back extraction acid into the extract phase after extraction, performing back extraction, and then conveying the filtrate into the primary leaching box 1 to perform treatment by using the third-time filter pressing, so that the treatment effect of the nickel-containing hazardous waste is improved, resources are saved, the recovery rate and the purity of recovered nickel salt are improved, and the nickel-containing hazardous waste is purified.
In some embodiments, the primary filter press 2 is further connected to the secondary leaching tank 10, and filter residue obtained by filter pressing of the primary filter press 2 enters the secondary leaching tank 10. As shown in fig. 1, the primary filter press 2 is further connected to a secondary leaching tank 10 through a pipeline, and the filter residue from the primary filter press 2 enters the secondary leaching tank 10 and is directly subjected to secondary leaching treatment.
In some embodiments, a curing plant 12 is further included, and filter residues obtained by pressure filtration through the secondary filter press 4 and the tertiary filter press 11 enter the curing plant 12 for treatment. As shown in figure 1, the nickel-containing hazardous waste recycling system also comprises a curing workshop 12, and filter residues obtained by the secondary filter press 4 and the tertiary filter press 11 enter the curing workshop 12 for treatment and harmless landfill.
In some embodiments, the impurity-removing extraction box 5 is further sequentially connected with a nickel extraction box 6, an oil removing device, an evaporation kettle 7, a crystallization kettle 8 and a dryer 9 through pipelines, the raffinate enters the nickel extraction box 6, a strip liquor is obtained by strip extraction in the nickel extraction box 6, the strip liquor enters the oil removing device to remove oil, and then the strip liquor sequentially passes through the evaporation kettle 7 and the crystallization kettle 8 after evaporation and crystallization to obtain nickel sulfate in the dryer 9. As shown in fig. 1, the impurity-removing extraction box 5 is further sequentially connected with a nickel extraction box 6, an oil removal device, an evaporation kettle 7, a crystallization kettle 8 and a dryer 9 through pipelines, raffinate enters the nickel extraction box 6, strip liquor is obtained in the nickel extraction box 6 through strip extraction, strip liquor enters the oil removal device for oil removal, oil removal resin is placed in the oil removal device, oil removal resin oil uses oleophylic hydrophobicity of oil-removing high-temperature resin to separate emulsified oil molecules and dissolved oil molecules from water and can be timely discharged on line, a resin bed is arranged in the oil removal device, the oleophylic hydrophobicity of the high-temperature resin is used to separate the emulsified oil molecules and the dissolved oil molecules from the water, emulsion breaking, catching and enrichment are automatically performed, the oil molecules in condensed water are timely collected on the surface of the resin, and then are evaporated and crystallized through the evaporation kettle 7 and the crystallization kettle 8 respectively to obtain nickel sulfate in the dryer 9, and dangerous nickel-containing waste is treated.
The invention also provides a resource treatment method of nickel-containing hazardous waste, which comprises the resource treatment system of nickel-containing hazardous waste, and comprises the following steps:
s1, conveying nickel-containing hazardous waste into a primary leaching tank 1 for leaching, then feeding filtrate subjected to pressure filtration by a primary pressure filter 2 into a dephosphorization tank 3, and feeding filter residues into a secondary leaching tank 10;
s2, adding hydrogen peroxide and a ferrous sulfate solution into the dephosphorization tank 3, and conveying the mixture into the secondary filter press 4 after the reaction is finished;
s3, conveying the filtrate subjected to filter pressing by the secondary filter press 4 to the impurity removal extraction box 5, and conveying the filter residue subjected to filter pressing by the secondary filter press 4 to the curing workshop 12 for treatment;
s4, conveying raffinate extracted by the impurity-removing extraction box 5 to the nickel extraction box 6;
s5, carrying out oil removal, evaporation, crystallization and drying on the strip liquor back extracted by the nickel extraction box 6 to obtain nickel sulfate;
s6, adding back extraction acid into the extraction phase extracted by the impurity removal extraction box 5 in the step S4, then conveying the extraction phase to the secondary leaching box 10, and adding sulfuric acid and water into the secondary leaching box 10 to obtain secondary leachate;
and S7, conveying the secondary leachate obtained in the step S6 to the tertiary filter press 11, conveying filtrate subjected to filter pressing by the tertiary filter press 11 to the primary leaching box 1, and conveying filter residues subjected to filter pressing by the tertiary filter press 11 to a curing workshop 12 for treatment.
In some embodiments, the pre-leaching pretreatment of the primary leaching tank 1 in step S1 is:
adjusting the pH value to 3.5-4; adjusting Ni 2+ The content is 70-80 g/L; regulating the TP content to be less than or equal to 100mg/L; regulating COD content to be less than 500mg/L.
In some embodiments, the primary leaching criterion in step S1 is that the primary leaching residue contains nickel in the range of 4 to 6%, and the secondary leaching criterion is that the secondary leaching residue contains nickel less than or equal to 0.5%.
In some embodiments, the concentration of the hydrogen peroxide solution in step S2 ranges from 27 to 32%, and the concentration of the ferrous sulfate solution ranges from 5 to 20%, wherein the molar ratio of the added amounts of the hydrogen peroxide solution and the ferrous sulfate solution is 2.
In some embodiments, the nickel-containing hazardous waste in step S1 is at least any one of an electroless plating solution, an electroplating solution, and a nickel-containing sludge.
In some embodiments, the liquid-to-solid ratio of the extract phase to the stripping acid in step S6 is 1 to 1.2;
the concentration of the sulfuric acid is 95-98%.
As shown in fig. 2, the nickel-containing waste is leached in sequence, and then subjected to primary and secondary filter pressing, impurity removal and extraction, the extracted extract phase is added to strip acid for back extraction, and then subjected to secondary leaching, and then filtrate is conveyed to a primary leaching tank 1 for treatment through tertiary filter pressing, so that the treatment effect of the nickel-containing hazardous waste is improved, resources are saved, the recovery rate and the purity of recovered nickel salt are improved, and the nickel-containing hazardous waste is purified;
the specific method comprises the following steps: conveying the nickel-containing hazardous waste into a primary leaching tank 1 for leaching, then conveying filtrate subjected to pressure filtration by a primary pressure filter 2 into a dephosphorization tank 3, conveying filter residues into a secondary leaching tank 10, then adding hydrogen peroxide and a ferric sulfate solution into the dephosphorization tank 3, and conveying the reacted product into a secondary pressure filter 4; the filtrate after filter pressing by the secondary filter press 4 is conveyed to an impurity removal extraction box 5, the filter residue after filter pressing by the secondary filter press 4 is conveyed to a curing workshop 12 for treatment, raffinate after extraction by the impurity removal extraction box 5 is conveyed to a nickel extraction box 6, and strip liquor after back extraction by the nickel extraction box 6 is subjected to oil removal, evaporation, crystallization and drying to obtain nickel sulfate; wherein, back extraction acid is added into the extraction phase extracted by the impurity removal extraction box 5, and then the extraction phase is conveyed to a secondary leaching box 10, sulfuric acid and water are added into the secondary leaching box 10 to obtain secondary leaching solution, the obtained secondary leaching solution is conveyed to a third filter press 11, filtrate which is subjected to filter pressing by the third filter press 11 is conveyed to a primary leaching box 1, and filter residue which is subjected to filter pressing by the third filter press 11 is conveyed to a curing workshop 12 for treatment.
Before primary leaching, dangerous waste containing nickel is scattered, chemical nickel plating waste liquid, nickel electroplating waste liquid and secondary leaching filtrate are added into a primary leaching tank 1 according to a liquid-solid ratio of 1-1.2, leaching reaction is carried out, the pH = 3.5-4 is adjusted, so that 70-80 g/L of nickel is contained in the primary leaching tank 1, then solid-liquid separation is carried out by a primary filter press 2, the obtained filtrate is discharged to a dephosphorization tank 3, and filter residues are discharged to a secondary leaching tank 10.
In the secondary leaching, a back-extraction acid solution is added according to the solid-to-liquid ratio of 1-1.2%, wherein the back-extraction acid solution is 200g/L sulfuric acid solution, the secondary leaching is carried out at normal temperature, concentrated sulfuric acid with the concentration of 95-98% is added as necessary, the leaching is carried out for 2-3 hours, so that the nickel content of the leached slag is less than or equal to 0.5%, water washing slag is introduced into the filter residue after filter pressing by a three-time filter press 11 until washing water is colorless, the washing slag water and the filter pressing liquid of the three-time filter press 11 are mixed and discharged to a primary leaching box 1, and the filter residue is treated in a curing workshop 12.
In the dephosphorization process, according to the Fenton reaction, the mixed solution of hydrogen peroxide and ferrous ions has strong oxidizing property, many known organic compounds such as carboxylic acid, alcohol and ester can be oxidized into inorganic state, the oxidizing effect is very obvious, hydrogen peroxide with the concentration range of 27-32% and ferrous sulfate solution with the concentration range of 5-20% are added according to 1.2-1.5 times of the primary leachate, wherein the molar ratio of the adding amount of the hydrogen peroxide to the ferrous sulfate solution is 2, the reaction is carried out for 1.5-2 hours at normal temperature, TP is controlled to be less than or equal to 100mg/L, COD is less than 500mg/L, after the liquid-solid separation by a secondary filter press 4, the amount of the filter-pressing residue iron phosphate is little, the filter-pressing residue is periodically washed and discharged to a curing workshop 12 and then is treated and then filled into a landfill, and the filter-pressing liquid is discharged to an impurity removal extraction box 5 for further extraction and impurity removal.
Wherein in the extraction process, a 20g/L nickel sulfate solution is prepared from standard nickel sulfate so that the organic phase ratio is 20% 2 O 4 +80% sulfonated kerosene, according to the proportion of O/A =1, fully stirring for 10 minutes to carry out nickel saponification, carrying out 26-36 levels of back extraction on an organic phase after nickel saponification according to the proportion of O/A = 1.
In the evaporative crystallization process, after oil removal treatment, the nickel sulfate solution is discharged into an evaporation kettle 7, the pH value is adjusted to 3.8-4.1 for evaporative concentration, after the concentration reaches the required specific gravity, the nickel sulfate solution can be transferred into a crystallizer for cooling crystallization, when the crystals are discharged, the crystals are centrifugally dried to obtain a nickel sulfate product, and the mother solution can be completely collected into a clean container, is recrystallized once and centrifugally dried to prepare nickel soap;
wherein the concentration of evaporation concentration is controlled to be 120-150 g/L of nickel, the temperature of evaporation discharge is controlled to be 85-100 ℃, and the temperature of the material is reduced to 55-65 ℃ after the material is discharged into a crystallization tank so as to generate enough supersaturation;
and discharging the materials after the crystallization is finished, feeding the materials into a centrifugal machine, centrifugally dewatering the materials, feeding the materials into a vibrating fluidized bed dryer for drying, weighing, packaging and warehousing.
To sum up, through carrying out once, secondary filter-pressing after leaching nickeliferous waste in proper order, carry out the edulcoration extraction, add the extraction phase after extracting and strip sour back-extraction and carry out the back-extraction, carry the filtrating to once leaching case 1 through cubic filter-pressing after later carrying out the secondary leaching and handle for improve the treatment effect, resources are saved of nickeliferous hazardous waste, promote the nickel salt purity of recovery rate and recovery, so that nickeliferous hazardous waste reaches the purification.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention. The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A nickel-containing hazardous waste resourceful treatment system is characterized by comprising:
the device comprises a primary leaching tank, an impurity removal extraction tank and a secondary leaching tank, wherein the primary leaching tank, the impurity removal extraction tank and the secondary leaching tank are sequentially connected through pipelines;
the primary leaching tank leaches nickel-containing hazardous wastes, a primary filter press, a dephosphorization tank and a secondary filter press are sequentially arranged between the primary leaching tank and the impurity removal extraction tank, and liquid leached by the primary leaching tank is subjected to filter pressing by the primary filter press to obtain primary filter-pressed filtrate; after the primary filter-pressing filtrate enters the dephosphorization tank for dephosphorization, the secondary filter-pressing filtrate enters the secondary filter press for secondary filter pressing to obtain secondary filter-pressing filtrate; the secondary filter pressing filtrate enters the impurity removal extraction box for extraction treatment to obtain raffinate and an extraction phase; the raffinate is nickel sulfate solution, and the extract phase enters the secondary leaching tank after being subjected to back extraction;
and a third pressure filter is arranged between the secondary leaching tank and the primary leaching tank, the leachate treated by the secondary leaching tank is subjected to pressure filtration by the third pressure filter, and the obtained third pressure filtration filtrate enters the primary leaching tank.
2. The nickel-containing hazardous waste recycling system according to claim 1, wherein:
the primary filter press is further connected with the secondary leaching tank, and filter residues obtained by filter pressing of the primary filter press enter the secondary leaching tank.
3. The nickel-containing hazardous waste recycling system according to claim 1, wherein:
and the filter residue obtained by the filter pressing of the secondary filter press and the third filter press enters the curing workshop for treatment.
4. The nickel-containing hazardous waste recycling system according to claim 1, wherein:
the edulcoration extraction box still pipeline connection has extraction nickel extraction box, deoiling device, evaporating kettle, crystallization kettle and desiccator in proper order, the raffinate gets into the extraction nickel extraction box back extraction obtains strip liquor in the extraction nickel extraction box, strip liquor gets into deoiling in the deoiling device, later process in proper order the evaporating kettle after the crystallization kettle evaporation crystallization obtains nickel sulfate in the desiccator.
5. A method for recycling nickel-containing hazardous waste, which is characterized in that the nickel-containing hazardous waste recycling system according to any one of claims 1 to 4 is adopted, and comprises the following steps:
s1, conveying nickel-containing hazardous waste into the primary leaching tank for leaching, then feeding filtrate subjected to pressure filtration by the primary pressure filter into a dephosphorization tank, and feeding filter residue into the secondary leaching tank;
s2, adding hydrogen peroxide and a ferrous sulfate solution into the dephosphorization tank, and conveying the mixture into the secondary filter press after the reaction is finished;
s3, conveying the filtrate subjected to filter pressing by the secondary filter press to the impurity removal extraction box, and conveying the filter residue subjected to filter pressing by the secondary filter press to the curing workshop for treatment;
s4, conveying raffinate extracted by the impurity-removing extraction box to the nickel extraction box;
s5, carrying out oil removal, evaporation, crystallization and drying on the strip liquor obtained by back extraction of the nickel extraction box to obtain nickel sulfate;
s6, adding back extraction acid into the extraction phase extracted by the impurity removal extraction box in the step S4, then conveying to the secondary leaching box, and adding sulfuric acid and water into the secondary leaching box to obtain secondary leaching solution;
and S7, conveying the secondary leachate obtained in the step S6 to the third pressure filter, conveying the filtrate subjected to pressure filtration by the third pressure filter to the primary leaching box, and conveying the filter residue subjected to pressure filtration by the third pressure filter to a curing workshop for treatment.
6. The resource treatment method for nickel-containing hazardous waste according to claim 5, characterized in that:
the pretreatment before leaching of the primary leaching tank in the step S1 comprises the following steps:
adjusting the pH value to 3.5-4; adjusting Ni 2+ The content is 70-80 g/L; regulating the TP content to be less than or equal to 100mg/L; regulating COD content to be less than 500mg/L.
7. The nickel-containing hazardous waste recycling method according to claim 5, characterized in that:
in the step S1, the primary leaching standard is that nickel in primary leaching slag is 4-6%, and the secondary leaching standard is that nickel in secondary leaching slag is less than or equal to 0.5%.
8. The resource treatment method for nickel-containing hazardous waste according to claim 5, characterized in that:
in the step S2, the concentration range of the hydrogen peroxide is 27-32%, the concentration of the ferrous sulfate solution is 5-20%, and the molar ratio of the added amount of the hydrogen peroxide to the added amount of the ferrous sulfate solution is 2.
9. The resource treatment method for nickel-containing hazardous waste according to claim 5, characterized in that:
the nickel-containing hazardous waste in the step S1 is at least one of chemical plating solution, electroplating solution and nickel-containing sludge.
10. The nickel-containing hazardous waste recycling method according to claim 5, characterized in that:
the liquid-solid ratio of the extract phase to the strip acid in the step S6 is 1-1.2;
the concentration of the sulfuric acid is 95-98%.
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