CN110668533A - Method and system for treating alkaline chemical nickel plating wastewater - Google Patents
Method and system for treating alkaline chemical nickel plating wastewater Download PDFInfo
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- CN110668533A CN110668533A CN201911062295.4A CN201911062295A CN110668533A CN 110668533 A CN110668533 A CN 110668533A CN 201911062295 A CN201911062295 A CN 201911062295A CN 110668533 A CN110668533 A CN 110668533A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 281
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 133
- 239000002351 wastewater Substances 0.000 title claims abstract description 123
- 239000000126 substance Substances 0.000 title claims abstract description 58
- 238000007747 plating Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 34
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000011574 phosphorus Substances 0.000 claims abstract description 51
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 51
- 238000005086 pumping Methods 0.000 claims abstract description 24
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 238000004070 electrodeposition Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000005844 autocatalytic reaction Methods 0.000 claims abstract description 6
- 239000003999 initiator Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 38
- 239000006228 supernatant Substances 0.000 claims description 32
- 238000004062 sedimentation Methods 0.000 claims description 30
- 239000002244 precipitate Substances 0.000 claims description 27
- 238000005189 flocculation Methods 0.000 claims description 24
- 230000016615 flocculation Effects 0.000 claims description 24
- 239000012716 precipitator Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 17
- 238000001556 precipitation Methods 0.000 claims description 17
- 239000000701 coagulant Substances 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 9
- 238000005868 electrolysis reaction Methods 0.000 claims description 8
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 8
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 239000012028 Fenton's reagent Substances 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 239000001509 sodium citrate Substances 0.000 claims description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- 239000004809 Teflon Substances 0.000 claims description 4
- 229920006362 Teflon® Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 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 claims description 4
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000009388 chemical precipitation Methods 0.000 abstract description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003456 ion exchange resin Substances 0.000 abstract description 3
- 229920003303 ion-exchange polymer Polymers 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract description 3
- 238000003541 multi-stage reaction Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000011550 stock solution Substances 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 3
- 239000005955 Ferric phosphate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- 229940032958 ferric phosphate Drugs 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000011272 standard treatment Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 230000001235 sensitizing effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C02F1/722—Oxidation by peroxides
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Abstract
A method and a system for treating alkaline chemical nickel-plating wastewater, which can reduce the treatment cost of nickel-containing wastewater, improve the recycling rate of nickel resources and enable nickel in the alkaline chemical nickel-plating wastewater to reach the standard. The method comprises the following steps of 1) pumping the wastewater with the pH value of 8.0-10 into a collecting tank; 2) heating the wastewater to 80-90 ℃; 3) carrying out electrolytic reaction by adopting an electrodeposition reactor; 4) the metallic nickel generated by reduction on the cathode is used as an initiator, and nickel ions released after anodic oxidation in a nickel-containing complex state are rapidly reduced and generated on the cathode in the form of metallic nickel simple substances through an autocatalytic reaction. The system adopts multistage reaction equipment, so that the alkaline chemical nickel plating wastewater with high nickel and phosphorus content can be quickly treated, and the treated wastewater reaches the discharge standard specified by the national standard, wherein the nickel content is less than 0.1ppm, and the TP is less than 0.5 ppm. The method can replace the existing chemical precipitation method, ion exchange resin method, membrane separation technology and other processes.
Description
Technical Field
The invention relates to the technical field of electroplating wastewater treatment, in particular to a standard treatment method and a standard treatment system for nickel in alkaline chemical nickel plating wastewater.
Background
The chemical nickel plating technology is to utilize a reducing agent to reduce and deposit nickel ions in a solution on a surface with catalytic activity to form a plating layer, and the chemical nickel plating technology is rapidly developed in China due to the advantages of no need of an external power supply and uniform plating layer. The chemical nickel plating can be divided into acid chemical nickel plating and alkaline chemical nickel plating, wherein the alkaline chemical nickel plating mainly uses sodium hypophosphite as a reducing agent, the plating solution also contains sodium citrate, ammonium chloride, ammonium hydroxide and other components, and the pH value of the plating solution is about 10. In the production process, after the alkaline chemical nickel plating solution is used for 4-6 periods, a large amount of by-products such as sodium phosphite and the like are accumulated in the plating solution, so that the quality of the plating solution is reduced, the nickel plating speed is reduced, the plating performance of a plated piece is reduced, and the plating solution is aged and scrapped to form chemical nickel plating wastewater and is discharged. The waste water has complex components and usually contains 4000-6000 mg.L-1Nickel and nickel belong to the first class of pollutants and have carcinogenic and sensitizing effects, and if the nickel and the nickel are directly discharged without treatment, the nickel and the nickel seriously pollute the environment and threaten the health of human bodies.
The nickel-containing wastewater treatment technology mainly comprises a chemical precipitation method, an ion exchange resin method, a solvent extraction method, an adsorption method, a membrane separation technology and the like. At present, the emission requirements of table 3 in the emission Standard of electroplating pollutants (GB21900-2008) are strictly implemented in most areas, wherein the emission limit of nickel is as follows<0.1mg·L-1. The prior art is adopted to treat the alkaline chemical nickel plating wastewater, on one hand, the reclamation of nickel can not be realized, meanwhile, the treatment of nickel does not reach the standard, nickel ions in the alkaline chemical nickel plating wastewater are all complexed with organic matters, and the standard and reclamation of nickel can not be realized by a single treatment method. .
Disclosure of Invention
The invention aims to solve the technical problem of providing a method and a system for treating alkaline chemical nickel plating wastewater, which can reduce the treatment cost of the nickel-containing wastewater, improve the recycling rate of nickel resources and enable nickel in the alkaline chemical nickel plating wastewater to reach the standard.
In order to solve the technical problems, the invention adopts the technical scheme that:
the method for treating the alkaline chemical nickel plating wastewater comprises the following steps:
1) pumping the wastewater containing sodium hypophosphite, sodium citrate, ammonium chloride, ammonium hydroxide and nickel sulfate and having a pH value of 8.0-10 into a collecting tank;
2) heating the wastewater to 80-90 ℃;
3) using an electrodeposition reactor at 100A/m2-500A/m2The current density of the anode is subjected to electrolytic reaction, nickel ions in the wastewater are reduced on the cathode to generate a metallic nickel simple substance, and meanwhile, the anode oxidizes hypophosphite and a complex compound and continuously releases the complexed nickel ions;
4) the metallic nickel generated by reduction on the cathode is used as an initiator, and nickel ions released after anodic oxidation in a nickel-containing complex state are rapidly reduced and generated on the cathode in the form of metallic nickel simple substances through an autocatalytic reaction.
The steps for removing the residual trace nickel and phosphorus are as follows:
1) after the nickel content in the wastewater is reduced to be within 10 percent, cooling the residual wastewater liquid to room temperature by a cooler and pumping the residual wastewater liquid into a No. 1 pH adjusting tank;
2) adjusting the pH value of the waste water residual liquid to 10-11 by adopting one of sodium hydroxide, calcium hydroxide and potassium hydroxide;
3) pumping the waste water residual liquid with the well adjusted pH value into a chemical nickel/phosphorus removal sedimentation tank, and adding a nickel precipitator and a phosphorus precipitator to ensure that residual nickel and phosphorus in the waste water residual liquid form large colloidal particles to form phosphate precipitation and nickel sulfide precipitation;
4) pumping the waste water residual liquid containing the large colloidal particles into a No. 1 flocculation tank, adding a coagulant aid, and reacting for 10-30min to form precipitates of the large colloidal particles and suspended particles;
5) and discharging the waste water residual liquid containing the precipitate into a No. 1 sedimentation tank, and settling for 60-120min for sludge-water separation so as to remove the residual nickel and phosphorus in the waste water residual liquid in a precipitation form.
The steps for removing the residual phosphorus are as follows:
1) pumping the supernatant of the wastewater without the precipitate into a No. 2 pH adjusting tank, and adjusting the pH value to 2-4;
2) pumping the wastewater supernatant with the well adjusted pH value into a Fenton oxidation tank, adding a Fenton reagent, and oxidizing for 60-120min to convert non-precipitated hypophosphite into orthophosphate, wherein the orthophosphate and iron ions form precipitates;
3) pumping the supernatant of the wastewater into a No. 3 pH adjusting tank, adjusting the pH value to 7-8, and forming iron phosphate precipitate under the condition of the pH value;
4) pumping the wastewater supernatant with the well adjusted pH value into a No. 2 flocculation tank, adding a coagulant aid, and reacting for 10-30min to generate iron phosphate precipitate;
5) and pumping the supernatant of the wastewater flocculated in the No. 2 flocculation tank into a No. 2 sedimentation tank to settle phosphorus-containing suspended matters in the supernatant.
The temperature of the wastewater is 75-80 ℃, and the electrodeposition reaction time is 60-300 min.
The nickel precipitator is sodium sulfide or potassium sulfide which is added according to the volume ratio, and the ratio of the nickel precipitator to the waste water residual liquid is (0.1-0.5): 100; the phosphorus precipitator is calcium chloride, and the ratio of the phosphorus precipitator to the waste water residual liquid is (1.0-0.5): 10.
The Fenton reagent is hydrogen peroxide and ferrous sulfate, and 10-30mL of hydrogen peroxide and 40-70g of ferrous sulfate are added into each liter of wastewater supernatant.
The coagulant aid is polyaluminium chloride or ferric sulfate.
The invention discloses a system for treating alkaline chemical nickel plating wastewater, which is characterized in that: comprises a collecting tank for storing waste water and an electro-deposition reactor, wherein,
a collecting pool for storing alkaline chemical nickel plating wastewater which contains 50-5000mg/L of nickel, 200-30000mg/L of phosphorus and 400-50000mg/L of COD, contains sodium hypophosphite, sodium citrate, ammonium chloride, ammonium hydroxide and nickel in a complex state and has a pH value of 8.0-10;
an electrodeposition reactor comprising an electrolysis vessel, a cathode, an anode, and a DC power supply, and a heater, wherein,
the cathode is a titanium basket filled with reticular carbon fibers; the anode is an iridium coated titanium anode;
the heater is a Teflon heater and is used for heating the wastewater to 80-90 ℃;
the current density during electrolysis was 100A/m2-500A/m2；
The electrodeposition reactor reduces nickel ions in the wastewater in the form of metallic nickel simple substances to generate nickel ions on a cathode, and meanwhile, an anode oxidizes a nickel-containing complex state and continuously releases free nickel ions;
and then, taking the metallic nickel generated by reduction on the cathode as an initiator, and quickly reducing the nickel ions released by anodic oxidation in a nickel-containing complex state in the form of metallic nickel simple substances through an autocatalytic reaction to generate the nickel ions on the cathode.
The system for treating alkaline chemical nickel plating wastewater also comprises a cooler, a No. 1 pH adjusting tank, a chemical nickel/phosphorus removal sedimentation tank, a No. 1 flocculation tank and a No. 1 sedimentation tank, wherein,
the cooler is used for cooling the waste water residual liquid with the nickel content reduced to be within 10 percent;
the No. 1 pH adjusting tank is used for adjusting the pH value of the cooled waste water residual liquid to 10-11 so as to generate the precipitation of phosphate and the precipitation of nickel sulfide;
the chemical nickel/phosphorus removal sedimentation tank is used for adding a nickel precipitator and a phosphorus precipitator to ensure that residual nickel and phosphorus in the residual liquid of the wastewater form large colloidal particles;
the flocculation tank No. 1 is used for adding coagulant aids to enable large colloidal particles and suspended particles to form precipitates;
and a No. 1 sedimentation tank for removing residual nickel and phosphorus in the waste water residual liquid in a sedimentation mode.
The system for treating the alkaline chemical nickel plating wastewater further comprises a 2# pH adjusting tank, a Fenton oxidation tank, a 3# pH adjusting tank, a 2# flocculation tank and a 2# sedimentation tank, wherein the 2# pH adjusting tank is connected with the Fenton oxidation tank through a pipeline
The No. 2 pH adjusting tank is used for storing the supernatant of the wastewater from which the precipitate is removed and adjusting the pH value of the supernatant of the wastewater to 2-4;
the Fenton oxidation tank is used for oxidizing the wastewater supernatant with the well-adjusted pH value to convert the non-precipitated hypophosphite into orthophosphate, and simultaneously the orthophosphate and iron ions form precipitates;
the 3# pH adjusting tank is used for storing the supernatant of the wastewater after the oxidation treatment in the Fenton oxidation tank and adjusting the pH value of the supernatant;
2# flocculation tank, use up and add coagulant aid;
and 2, settling phosphorus-containing suspended matters in the sedimentation tank.
The invention adopts multi-stage reaction (electro-deposition reaction, Fenton reaction, multiple flocculation and precipitation) equipment, so that the alkaline chemical nickel plating wastewater with high nickel and phosphorus content can be quickly treated, and the treated wastewater reaches the discharge standard specified by the national standard, wherein the nickel content is less than 0.1ppm, and the TP is less than 0.5 ppm. The method can replace the chemical precipitation method, ion exchange resin method, solvent extraction method, adsorption method, membrane separation technology and other processes in the prior art.
Drawings
FIG. 1 is a block diagram of a processing system of the present invention.
Detailed Description
As shown in figure 1, the method and system for treating alkaline chemical nickel plating wastewater of the invention are composed of the following devices, namely an alkaline chemical nickel collecting tank, an electrodeposition reactor, a No. 1 pH adjusting tank, a chemical precipitation nickel/phosphorus removal reactor, a No. 1 flocculation tank, a No. 1 sedimentation tank, a No. 2 pH adjusting, a Fenton oxidation reactor, a No. 3 pH adjusting tank, a No. 2 flocculation tank and a No. 2 sedimentation tank, wherein the devices play the following roles:
1. an alkaline chemical nickel collecting pool, wherein the content of collected nickel is 50-5000 mg/L; the phosphorus content is 200-30000 mg/L; the COD of the alkaline chemical nickel plating wastewater stock solution is 400-50000mg/L, and the components of the wastewater stock solution mainly comprise sodium hypophosphite, sodium citrate, ammonium chloride, ammonium hydroxide and nickel sulfate. The pH value is 8.0-10.
2. And (3) electrodeposition, namely, in the alkaline chemical nickel plating wastewater stock solution, the nickel exists in a form of complex mostly, and the nickel is recovered in a form of nickel metal by electrodeposition.
The electrodeposition reactor mainly comprises an electrolysis reactor, a cathode and an anode, a direct current power supply and a Teflon heater;
the alkaline chemical nickel plating wastewater stock solution is heated by a Teflon heater, so that the wastewater stock solution is maintained in a temperature range of 80-90 ℃, not only can normal electrolysis be performed at the temperature, but also nickel metal can be reduced by using a reducing agent sodium hypophosphite which is not completely converted in the wastewater, the nickel concentration in the wastewater is rapidly reduced, meanwhile, the hypophosphite is oxidized into orthophosphate radical, the preferred temperature is 75-85 ℃, and the electrodeposition reaction time is 60-300 min.
Through electrodeposition, metal nickel is generated at a cathode, the initially generated metal nickel serves as an initiator to trigger other nickel ions in the wastewater to be continuously reduced on the cathode to generate the metal nickel, the electrolytic reduction of the metal nickel and the metal nickel generated by autocatalysis have double effects to accelerate the precipitation of the nickel, and simultaneously, due to the oxidation effect of an anode, a complexing agent in the complex nickel is continuously oxidized, so that nickel ions are released.
An electrolysis process:
anode: h2O＝4H++02+4e-Eo＝1.229V，
Cathode: ni2++2e-＝Ni Eo＝0.25V
2H++2e-＝H2Eo＝0V
Eo is potential
In the process, more than 90 percent of nickel ions in the alkaline chemical nickel plating wastewater stock solution can be deposited on the cathode in the form of simple substances.
In the electrolytic process, the adopted cathode is a titanium basket filled with reticular carbon fibers (the shape of the reticular carbon fibers can be spherical, square or elliptical), and the anode is an anode with an iridium coating layer arranged outside a titanium core.
The current density during electrolysis is 100A/m2-500A/m2。
The bottom of the tank body of the electrolytic reactor is provided with a wastewater stock solution inlet pipe which is S-shaped and extends from one end of the tank body to the opposite end along the bottom surface of the tank body. The extension direction of the water inlet pipe is vertical to the cathode plate and the anode plate (the cathode plate and the anode plate are suspended in the tank body in parallel).
The water inlet pipe is provided with a plurality of water outlet holes, the aperture of each water outlet hole is 10mm-15mm, and the water outlet direction and the bottom surface of the groove body form a 45-degree included angle. This arrangement has the following benefits:
1) ensuring that the effluent flows in the tank body without dead angles, thereby leading the nickel reaction to be more thoroughly removed.
2) The water body flows fast and enters the water tank at an included angle of 45 degrees, so that the washing of water flow to the cathode can be reduced, and the quality of cathode nickel is improved.
3. 1# pH adjusting tank: cooling the waste water residual liquid with the nickel content less than 10 percent after the electrolytic reaction treatment to the room temperature by a cooler, pumping the waste water residual liquid into the regulating tank, and regulating the pH value of the waste water residual liquid to 10-11 by adopting one of sodium hydroxide, calcium hydroxide and potassium hydroxide.
4. Chemical nickel/phosphorus removal sedimentation tank: adding a nickel precipitator and a phosphorus precipitator, and removing residual nickel and phosphorus in the waste water residual liquid in a precipitation mode, wherein the nickel precipitator is sodium sulfide or potassium sulfide, the addition amount is added according to the volume ratio, and the nickel precipitator: the ratio of the waste water to the residual liquid is (0.1-0.5): 100; the phosphorus precipitator is calcium chloride, and the ratio of the phosphorus precipitator to the waste water residual liquid is (1.0-0.5): 10.
In the sedimentation tank, the residual nickel and phosphorus in the waste water residual liquid can form nickel sulfide and calcium phosphate with large colloid particles:
Ca2++PO4 3-→Ca3(PO4)2↓
Ni2++S2-＝NiS↓
phosphorus is precipitated in the form of calcium phosphate by adding a phosphorus precipitant, and nickel is precipitated in the form of nickel sulfide by adding a nickel precipitant, both of which achieve treatment under the same process condition. The removal of phosphorus not only reduces the complexing probability of nickel and phosphorus, is convenient for nickel and sulfide to form precipitate, but also increases the floc of the precipitate, is beneficial to the complete precipitation of nickel sulfide, and achieves the synergistic effect, so that the nickel reaches the standard (Ni <0.1 ppm).
5. And a No. 1 flocculation tank, wherein the treated wastewater (namely the wastewater residual liquid containing the large colloidal particles) is discharged into the flocculation tank for flocculation treatment.
Adding coagulant aid, reacting for 10-30min to make the large colloidal particles and suspended particles form precipitate, i.e. to accelerate the speed of the colloidal impurities and/or suspended particles to form precipitate containing ferric hydroxide, nickel hydroxide and/or phosphate.
The coagulant aid is one or more of polyaluminium chloride and ferric sulfate as main coagulant aids.
6. 1# sedimentation tank: and discharging the waste water containing the precipitate (namely the precipitate containing the ferric hydroxide, the nickel hydroxide and/or the phosphate) into the sedimentation tank for mud-water separation, wherein the sedimentation time is 60-120min, namely the residual nickel and phosphorus in the waste water residual liquid are removed in a precipitation form.
7. 2# pH adjusting tank: pumping the supernatant without precipitate into the regulating tank, adding acid solution such as sulfuric acid and hydrochloric acid, and regulating the pH value of the supernatant to 2-4.
8. A Fenton oxidation pond: and adding a Fenton reagent, wherein the Fenton reagent comprises hydrogen peroxide and ferrous sulfate, 10-30mL of the hydrogen peroxide is added into each liter of the supernatant, 40-70g of the ferrous sulfate is added into each liter of the supernatant, and the oxidation time is 60-120min, so that non-precipitated hypophosphite is converted into orthophosphate, and meanwhile, the orthophosphate and iron ions form precipitates.
By Fenton reaction, under acidic environment H2O2With Fe2+The reaction generates OH with strong oxidizing power, the hypophosphite is oxidized and orthophosphate sediment (ferric phosphate) is formed, and the total phosphorus is deeply removed, thereby the total phosphorus in the alkaline chemical nickel plating waste liquid reaches the standard and is discharged. On the other hand, using Fe (OH)3The colloidal flocculation adsorbs the iron phosphate precipitate particles, which are removed by precipitation.
9. 3# pH adjusting tank: pumping the supernatant into the regulating tank, and regulating the pH value to 7-8.
Under the condition of the pH value, the precipitation of the ferric phosphate is facilitated.
10. 2# flocculation tank: pumping the wastewater supernatant with the adjusted pH value into the flocculation tank, adding one or more of coagulant aids mainly comprising polyaluminium chloride and ferric sulfate, and reacting for 10-30 min.
11. 2# sedimentation tank: pumping the supernatant of the wastewater flocculated by the No. 2 flocculation tank into the sedimentation tank, so that suspended matters (iron phosphate) in the supernatant are easy to settle, and the total phosphorus is removed in a form of sedimentation and reaches the standard, wherein the content of nickel is less than 0.1ppm, and the content of total phosphorus is less than 0.5 ppm.
See Table 1 below for examples
Claims (10)
1. A method for treating alkaline chemical nickel plating wastewater comprises the following steps:
1) pumping the wastewater containing sodium hypophosphite, sodium citrate, ammonium chloride, ammonium hydroxide and nickel sulfate and having a pH value of 8.0-10 into a collecting tank;
2) heating the wastewater to 80-90 ℃;
3) using an electrodeposition reactor at 100A/m2-500A/m2The current density of the anode is subjected to electrolytic reaction, nickel ions in the wastewater are reduced on the cathode to generate a metallic nickel simple substance, and meanwhile, the anode oxidizes hypophosphite and a complex compound and continuously releases the complexed nickel ions;
4) the metallic nickel generated by reduction on the cathode is used as an initiator, and nickel ions released after anodic oxidation in a nickel-containing complex state are rapidly reduced and generated on the cathode in the form of metallic nickel simple substances through an autocatalytic reaction.
2. A method for treating alkaline chemical nickel plating wastewater according to claim 1, characterized in that: the steps for removing the residual trace nickel and phosphorus are as follows:
1) after the nickel content in the wastewater is reduced to be within 10 percent, cooling the residual wastewater liquid to room temperature by a cooler and pumping the residual wastewater liquid into a No. 1 pH adjusting tank;
2) adjusting the pH value of the waste water residual liquid to 10-11 by adopting one of sodium hydroxide, calcium hydroxide and potassium hydroxide;
3) pumping the waste water residual liquid with the well adjusted pH value into a chemical nickel/phosphorus removal sedimentation tank, and adding a nickel precipitator and a phosphorus precipitator to ensure that residual nickel and phosphorus in the waste water residual liquid form large colloidal particles to form phosphate precipitation and nickel sulfide precipitation;
4) pumping the waste water residual liquid containing the large colloidal particles into a No. 1 flocculation tank, adding a coagulant aid, and reacting for 10-30min to form precipitates of the large colloidal particles and suspended particles;
5) and discharging the waste water residual liquid containing the precipitate into a No. 1 sedimentation tank, and settling for 60-120min for sludge-water separation so as to remove the residual nickel and phosphorus in the waste water residual liquid in a precipitation form.
3. A method for treating alkaline chemical nickel plating wastewater according to claim 2, characterized in that: the steps for removing the residual phosphorus are as follows:
1) pumping the supernatant of the wastewater without the precipitate into a No. 2 pH adjusting tank, and adjusting the pH value to 2-4;
2) pumping the wastewater supernatant with the well adjusted pH value into a Fenton oxidation tank, adding a Fenton reagent, and oxidizing for 60-120min to convert non-precipitated hypophosphite into orthophosphate, wherein the orthophosphate and iron ions form precipitates;
3) pumping the supernatant of the wastewater into a No. 3 pH adjusting tank, adjusting the pH value to 7-8, and forming iron phosphate precipitate under the condition of the pH value;
4) pumping the wastewater supernatant with the well adjusted pH value into a No. 2 flocculation tank, adding a coagulant aid, and reacting for 10-30min to generate iron phosphate precipitate;
5) and pumping the supernatant of the wastewater flocculated in the No. 2 flocculation tank into a No. 2 sedimentation tank to settle phosphorus-containing suspended matters in the supernatant.
4. A method for treating alkaline chemical nickel plating wastewater according to any of the claims 1-3, characterized in that: the temperature of the wastewater is 75-80 ℃, and the electrodeposition reaction time is 60-300 min.
5. A method for treating alkaline chemical nickel plating wastewater according to claim 2 or 3, characterized in that: the nickel precipitator is sodium sulfide or potassium sulfide which is added according to the volume ratio, and the ratio of the nickel precipitator to the waste water residual liquid is (0.1-0.5): 100; the phosphorus precipitator is calcium chloride, and the ratio of the phosphorus precipitator to the waste water residual liquid is (1.0-0.5): 10.
6. A method for treating alkaline chemical nickel plating wastewater according to claim 3, characterized in that: the Fenton reagent is hydrogen peroxide and ferrous sulfate, and 10-30mL of hydrogen peroxide and 40-70g of ferrous sulfate are added into each liter of wastewater supernatant.
7. A method for treating alkaline chemical nickel plating wastewater according to claim 2 or 3, characterized in that: the coagulant aid is polyaluminium chloride or ferric sulfate.
8. A system for treating alkaline chemical nickel plating wastewater is characterized in that: comprises a collecting tank for storing waste water and an electro-deposition reactor, wherein,
a collecting pool for storing alkaline chemical nickel plating wastewater which contains 50-5000mg/L of nickel, 200-30000mg/L of phosphorus and 400-50000mg/L of COD, contains sodium hypophosphite, sodium citrate, ammonium chloride, ammonium hydroxide and nickel in a complex state and has a pH value of 8.0-10;
an electrodeposition reactor comprising an electrolysis vessel, a cathode, an anode, and a DC power supply, and a heater, wherein,
the cathode is a titanium basket filled with reticular carbon fibers; the anode is an iridium coated titanium anode;
the heater is a Teflon heater and is used for heating the wastewater to 80-90 ℃;
the current density during electrolysis was 100A/m2-500A/m2；
The electrodeposition reactor reduces nickel ions in the wastewater in the form of metallic nickel simple substances to generate nickel ions on a cathode, and meanwhile, an anode oxidizes a nickel-containing complex state and continuously releases free nickel ions;
and then, taking the metallic nickel generated by reduction on the cathode as an initiator, and quickly reducing the nickel ions released by anodic oxidation in a nickel-containing complex state in the form of metallic nickel simple substances through an autocatalytic reaction to generate the nickel ions on the cathode.
9. A system for treating alkaline electroless nickel plating wastewater according to claim 8, characterized in that: also comprises a cooler, a No. 1 pH adjusting tank, a chemical nickel/phosphorus removal sedimentation tank, a No. 1 flocculation tank and a No. 1 sedimentation tank, wherein,
the cooler is used for cooling the waste water residual liquid with the nickel content reduced to be within 10 percent;
the No. 1 pH adjusting tank is used for adjusting the pH value of the cooled waste water residual liquid to 10-11 so as to generate the precipitation of phosphate and the precipitation of nickel sulfide;
the chemical nickel/phosphorus removal sedimentation tank is used for adding a nickel precipitator and a phosphorus precipitator to ensure that residual nickel and phosphorus in the residual liquid of the wastewater form large colloidal particles;
the flocculation tank No. 1 is used for adding coagulant aids to enable large colloidal particles and suspended particles to form precipitates;
and a No. 1 sedimentation tank for removing residual nickel and phosphorus in the waste water residual liquid in a sedimentation mode.
10. A system for treating alkaline electroless nickel plating wastewater as claimed in claim 9, wherein: also comprises a 2# pH adjusting tank, a Fenton oxidation tank, a 3# pH adjusting tank, a 2# flocculation tank and a 2# sedimentation tank, wherein
The No. 2 pH adjusting tank is used for storing the supernatant of the wastewater from which the precipitate is removed and adjusting the pH value of the supernatant of the wastewater to 2-4;
the Fenton oxidation tank is used for oxidizing the wastewater supernatant with the well-adjusted pH value to convert the non-precipitated hypophosphite into orthophosphate, and simultaneously the orthophosphate and iron ions form precipitates;
the 3# pH adjusting tank is used for storing the supernatant of the wastewater after the oxidation treatment in the Fenton oxidation tank and adjusting the pH value of the supernatant;
2# flocculation tank, use up and add coagulant aid;
and 2, settling phosphorus-containing suspended matters in the sedimentation tank.
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